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We have checked the contents of this manual for agreement with the hardware and software described. Since deviations cannot
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necessary corrections are included in subsequent editions. Suggestions for improvement are welcome.
In case you need more information than this user's manual can supply, you can get additional help from our service group in one
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Order no. M89-E01005. Version 1. Issue: Jan 07, 2004.
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Printed in the Federal Republic of Germany.
NanoSTAR SAXS System
User Manual Vol. 2
1
NanoSTAR SAXS-Systems User Manual Vol. 2:
Operating Instructions and Alignment
Table of Contents
1
NanoSTAR SAXS-Systems User Manual Vol. 2: Operating Instructions and
Alignment..........................................................................................................1-1
Safety Instructions .................................................................................................1-1
General Remarks......................................................................................................................... 1-1
Radiation Safety .......................................................................................................................... 1-3
Introduction ............................................................................................................1-6
Interaction of X-rays With Matter ..........................................................................1-7
Diffraction .................................................................................................................................... 1-8
Scattering..................................................................................................................................... 1-9
SAXS – Small Angle X-Ray Scattering...................................................................................... 1-9
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Components of the SAXS System...................................................................... 1-14
X-ray Optics ............................................................................................................................... 1-14
Göbel Mirrors Optics ............................................................................................................ 1-14
Pinhole Collimation System ................................................................................................. 1-17
Combination of ccGMs With Pinhole Collimation................................................................. 1-17
Design of the Instrument .......................................................................................................... 1-18
X-ray Parallel Beam Source (PBS) ...................................................................................... 1-21
X-ray Tube With Mount ........................................................................................................ 1-22
4DOF .................................................................................................................................... 1-23
ccGM (cross coupled Göbel Mirrors) ................................................................................... 1-23
Mirror Shape and d-spacing................................................................................................. 1-23
Intrinsic Divergence.............................................................................................................. 1-24
0-Pinhole .............................................................................................................................. 1-24
Absorber Holder ................................................................................................................... 1-25
1st Pinhole or Divergence Pinhole ........................................................................................ 1-25
X-ray Labyrinth Flange......................................................................................................... 1-26
Primary Beam Path Tube System........................................................................................ 1-26
Entrance Window ................................................................................................................. 1-26
Exit Window.......................................................................................................................... 1-26
Beam Defining Pinhole......................................................................................................... 1-26
Antiscatter Pinhole ............................................................................................................... 1-27
Sample Chamber ................................................................................................................. 1-27
Chamber............................................................................................................................... 1-27
Automatic Sample Changer and 2D Scanning Stage.......................................................... 1-27
Sample Holder...................................................................................................................... 1-28
Reference Sample Changer................................................................................................. 1-28
Vacuum Cone....................................................................................................................... 1-28
Vacuum System ................................................................................................................... 1-28
Cooling Water System ......................................................................................................... 1-28
Security Circuit ..................................................................................................................... 1-29
Secondary Scattering Beam Path Tubes............................................................................. 1-29
Primary Beam Stop .............................................................................................................. 1-29
Measurements...................................................................................................... 1-30
2D-Detector ................................................................................................................................ 1-30
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Bias Settings ........................................................................................................................ 1-32
Flood Field Correction.......................................................................................................... 1-33
Spatial or Fiducial Correction (Brass Plate Correction) ....................................................... 1-34
Samples...................................................................................................................................... 1-36
Glassy Carbon Transmission............................................................................................... 1-36
Sample Transmission .......................................................................................................... 1-36
Absolute Calibration............................................................................................................. 1-37
Determination of Sample to Detector Distance ................................................................... 1-39
Determination of Sample Position ....................................................................................... 1-39
Alignment Overview NanoSTAR U SAXS System .............................................1-40
NanoSTAR U, Compact, Long Version, One Tube or …? What’s That ?............................... 1-40
Which Components of the NanoSTAR U Systems Have to be Aligned? ............................ 1-41
What Degrees of Freedom are Available for Alignment........................................................ 1-41
What will be the Result After the Alignment Procedures? ................................................... 1-43
Which Alignment Steps Have to be Done? ............................................................................ 1-43
SAXS Operation Modes ............................................................................................................ 1-45
Alignment Details NanoSTAR U SAXS System .................................................1-47
Some Remarks .......................................................................................................................... 1-47
Quick Alignment Overview ...................................................................................................... 1-48
Alignment in Detail.................................................................................................................... 1-49
Alignment Overview NanoSTAR C SAXS System .............................................1-69
NanoSTAR C, Long Version, One Tube or …? What’s That ?.............................................. 1-69
Which Components of the NanoSTAR C Systems Have to be Aligned? ............................ 1-70
What Degrees of Freedom are Available for Alignment........................................................ 1-70
What will be the Result After the Alignment Procedures? ................................................... 1-72
Which Alignment Steps Have to be Done? ............................................................................ 1-72
SAXS Operation Modes ............................................................................................................ 1-74
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Alignment Details NanoSTAR C SAXS System ................................................. 1-75
Some Remarks........................................................................................................................... 1-75
Quick Alignment Qverview ....................................................................................................... 1-76
Alignment in Detail .................................................................................................................... 1-76
Figure Captions ................................................................................................... 1-92
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Safety Instructions
General Remarks
Read this manual completely and carefully before you use the SAXS system! You will find notices and
hints which are very important for your own personal safety, as well as to protect the system and all
connected devices.
Installation, alignment and rebuilding procedures or any changes of the system may only be carried
out by authorized and qualified personnel who are familiar with the installation instructions and have a
technical and scientific education with enough experience, know how and technical and scientific
background.
Bruker AXS warrants the proper functioning of the SAXS system only, if no unauthorized adjustments
have been made in mechanical and electronic parts and software.
Follow all hints, warnings and instructions contained in this manual to ensure the correct and safe
functioning of the SAXS system.
Never use the instrument for any purpose other than described in the manual.
Never operate the SAXS system if a malfunction is suspected, or damages, injuries or loss of life cannot be excluded under all circumstances.
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Repair procedures may only be carried out by authorized personnel from Bruker AXS. Do not use any
components, accessories or spare parts other than those supplied or approved by Bruker AXS.
Service procedures which involve removing covers and working with power on may only be performed
by authorized service personnel from Bruker AXS.
This SAXS system is not an explosion proofed instrument, and therefore must not be operated at explosion hazardous places.
Due to the nature of the measurement, measuring results do not only depend on the correct use and
functioning of the SAXS system, but may also be influenced by other factors. Therefore it is advised
that the analysis results are checked and tested by other methods before consequential actions are
taken.
The instrument may be operated only by qualified personnel who are familiar with the safety precautions and have a technical and scientific education.
Ensure that all operators are fully trained in the correct use of this instrument and its safe operation.
Make sure that the operation is supervised sufficiently.
Follow the precautions below for handling and measurement of inflammable samples and cleaning
materials:
-
Do not store inflammable material near the SAXS system
-
Do not leave sample containers uncovered.
-
Clean all spills immediately.
-
Ensure that the SAXS system is located in a sufficiently ventilated area with air conditioning, free
from inflammable gases and vapours.
-
Connect this SAXS system to the mains via a safety switch located in a safe distance from the
system. In an emergency, turn off the power using this switch. Do not use the NanoSTAR’s power
switch.
-
Keep a fire extinguisher at hand.
-
Do not leave the SAXS system unattended while in use.
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Radiation Safety
DANGER
Never bridge any security switches or contacts during the alignment procedures and measurements! If you follow all alignment and adjustment steps as described here the radiation which
leaves the system will be always lower than the maximum legal level (German law). If you are unsure
whether your electrical and radiation safety system is running correctly and if you suspect that there is
any faulty inside the system, please switch off the complete SAXS system and contact Bruker AXS
service at once.
DANGER
The primary and secondary X-ray beam path is completely surrounded with closed housings and
meets the requirements for fully protected instruments with single acceptance (“Vollschutzgerät mit
Einzelabnahme”) as written in the last valid German X-ray regulations (Röntgenschutzverordnung).
Please read carefully the safety instructions of this system! Danger! Do never bridge the security
switches and do never any changes of this security protection system!
For servicing and alignment reasons by authorized service personnel it is necessary to disable safety
precautions. This can be done by turning the ‘SERVICE MODE’ key switch to position ‘ON’.
As long as the ‘SERVICE MODE’ key switch is set to ‘SERVICE MODE’ position the control software
modules will indicate this by a flashing warning message over the sample chamber.
The SAXS system is designed so that the X-ray source, the complete primary beam path, the irradiated samples and the complete secondary scattered radiation including the detector is surrounded
with a closed housing. Under normal operation, the materials selected ensure that no radiation escapes.
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WARNING
Read this carefully if you use the vacuum set A10-D15/A10-D16 for “sample chamber under air operation mode”. The radiation protection circuit (safety circuit) is provided for the safety of operating personnel and for meeting the prerequisites for a fully protected device with single acceptance (“Vollschutzgerät mit Einzelabnahme”) according to German law. The protection circuit shuts down the Xray generator (off) if a safety switch on the connected equipment is open, or if the two safety circuits
give different results, or if the high-voltage cable is not connected (ripcord not inserted). Especially
both vacuum switches are part of the safety circuit, and X-ray generation is only possible if both
switches are active simultaneously (vacuum mode). In case of sample chamber under air operation
mode the sample chamber is filled with air and hence not integrated in the security system via the
vacuum switches.
NOTE
The status “sample chamber under air operation mode” means:
1. The primary beam path is evacuated, closed by an X-ray window to the chamber inlet flange and
watched by one vacuum switch.
2. The secondary beam path is closed with a cone (including an X-ray window) to the chamber outlet
flange and watched by another vacuum switch.
3. The sample chamber is under air (no hose to the vacuum pump). X-ray generation is possible
because both vacuum switches are active and indicate identical result. It is also possible to open
the shutter and start measurements.
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WARNING
In this status it is possible that personnel might be exposed to radiation if one or more blanking flanges
of the NanoSTAR sample chamber are removed. This state cannot be detected by the safety circuit.
Use only this “sample chamber under air operation mode” when it is necessary to measure samples
under air. Never use this system setup for convenience.
WARNING
X-rays are dangerous and harmful. Make sure that you always work according to the locally valid Xray laws and regulations and that the X-ray penetration of personnel is always as low as reasonably
achievable. Only professional X-ray experts especially trained on a NanoSTAR are allowed to carry
out maintenance and alignment work.
Bruker-AXS is not responsible if personnel get hurt by X-ray while the radiation protection circuit is not
able to watch the sample chamber under air with one or more blanking flanges removed.
NOTE
Personnel who wants to measure in the ‘samples under air measurement mode’ have to sign a document that assures that:
-
they received the extended vacuum set including a second X-ray window and the cone,
-
they will never remove one or more blanking flanges of the sample chamber with the X-ray generator “on”,
-
they will always act according to the valid locally X-ray law,
-
they read and understood the meaning of the text in the document mentioned above.
All components that can be detached during normal operation are protected via safety switches.
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Introduction
A small angle X-ray scattering (SAXS) system, as the NanoSTAR, is the ideal tool for the examination
of structures which have dimensions typically in the range between 1nm to several 100nm.
Structural investigations in the nanometer range with scattering (X-rays and neutrons) methods have
several advantages compared to electron microscopy. They require virtually no sample preparation
and the measured parameters as sample size, orientation or shape are mean values from the complete irradiated sample region.
The range of properties of these nanoparticles is broad and includes not only microstructures in materials, but also microemulsions, polymer chain properties and many others. SAXS is used in many scientific areas of material- and biophysical sciences.
The main feature of the NanoSTAR SAXS system is that not only isotropic materials, such as liquids
or polycrystals can be studied, but also more complex samples, especially anisotropic ones, such as
fibrous or layered structures. The use of a two dimensional detector and the possibility of several different sample to detector distances gives the NanoSTAR SAXS system a wide variety in setups.
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Interaction of X-rays With Matter
Here some basic physics concerning interaction of X-rays with matter is explained. Because this is a
user’s manual and not a scientific text book not all aspects can be illuminated. If there is a need to get
more information about basic X-ray physics please read additional scientific literature.
There are three main processes of interaction of X-rays with matter:
•
elastic X-ray scattering
•
inelastic X-ray scattering
•
X-ray absorption
Using X-rays in the range of approx. wavelength 1Å small angle X-ray scattering can be treated as
elastic coherent scattering. The electrons in the sample which interact with the X-rays often can be
considered as free. In this case the X-ray energy has to be far away from the photo absorption edges
of the sample elements.
Excited by the incoming electromagnetic wave the electrons of the sample oscillate with the same
frequency and phase. These charged and accelerated electrons themselves emit radiation with an
intensity:
1 + cos 2 (2ϑ )
I e (ϑ ) = 2 I 0
2
r
re2
I0 is the intensity of the incoming beam, r the distance to the detector, 2ϑ the scattering angle and re
the classical electron radius. The last term is the polarization factor and is practically equal to
1 (2ϑ→0) Incoherent Compton scattering can be neglected for small angles.
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In general the intensity I(q) is the square of the modulus of the scattering amplitude A(q). This can be
expressed as:
I (q ) = A(q ) = I 0 ∫ ρ (r ) exp(i q ⋅ r )d 3 r
2
2
V
This is the Fourier transformation of the object which is ‘seen’ by X-rays - the electron density of the
specimen ρ(r). q is the scattering vector, the difference of kin and kout - the incoming and scattered
wavevector, with
q= q =
4π
λ
sin ϑ
2ϑ is the angle between kin and kout and V is the volume of the sample which is irradiated by kin. I0 is a
constant which is necessary so that energy conservation remains fulfilled.
For typical wavelengths of approx. 1Å electron density variations in the order of 1nm to several 100nm
can be observed.
Depending on the arrangement of the scattering objects the interference of the scattered waves
shows a characteristic pattern. In general we have to distinguish scattering- from diffractionprocesses:
Diffraction
The origin of this process is a periodically arranged set of identical scatterers. This structure may appear in form of one, two or three dimensional lattices.
The scattering results are sharp interference maxima and are well known from crystallographic investigations. These patterns deliver not only information about the basic lattice but also about the content
of one lattice cell - the smallest unit in the lattice which is periodically manifold.
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Scattering
In this general case the presence of a lattice is not a must. The scattering objects may be arranged in
a statistical way. In general the resultant interference pattern consists of broad diffuse intensity distributions. The scattering intensity distribution contains information about particle size and its distributions, particle shapes, their arrangements, orientations and others.
As structure and scattering/diffraction pattern are related to each other by a reciprocal law, small angle
X-ray scattering (SAXS) means scattering of relatively large objects which are mostly statistically isotropic and no long range order exists. Nevertheless SAXS does not exclude diffraction processes.
In general SAXS scatterers are embedded in a matrix which means a homogeneous medium with
electron density ρ0 (particles in a solution).
These processes give information on the internal crystalline structure within the sample and can be
found in most cases at larger angles. At very small angles the scattering signal gives information on
the arrangement of the scatterer whereas in the mid range of angles shape and size of the scatterer
can be seen.
SAXS – Small Angle X-Ray Scattering
If electron density variations are arranged more or less randomly, diffuse scattering is observed in the
vicinity of the direct X-ray beam. This effect is called SAXS. Now some examples will be described
how SAXS patterns are affected by the properties of the scattering objects.
Assuming that the sample is composed of two separate phases A and B with different electron densities
ρ A (r ) = ρ A = const.
ρ B (r ) = ρ B = const.
then it can be described in a simple two phase model. Let χA(r) be a weighting function which is
χ A (ri ) = 1
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ρ (ri ) = ρ A
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and
if
ρ (ri ) ≠ ρ A
then the intensity which is scattered by the sample volume V can be written:
I (q) = I 0 ( ρ A − ρ B ) ∫ χ A (r )exp(i q r )d 3 r
2
2
V
As one can see the result for I(q) remains unchanged when ρA is replaced by ρB. If the scattering objects are totally randomly oriented then the scattered intensity has spherical symmetry, i.e. I(q) = I(q).
∆ρ is the contrast of the two phases, i.e. the difference of ρA and ρB. Let S be the total surface between
the two phases of the sample then the spherically averaged intensity I(q) can be written following
Porod’s law:
I (q) = I 0 ∆ρ 2
2πS
q4
This means that the intensity is proportional to the surface area and decreases as 1/q4. In this case
the assumption of widely separated particles is not necessary.
In the next example we suppose a dilute system with widely separated small particles. The sample
should consist ideally of a large number of identical particles distributed randomly with no interference
between them, similar to gas scattering. The intensity of radiation by an ensemble of widely separated
particles is identical to the mean intensity scattered by one isolated particle.
At very small angles, the shape of the scattering in the so-called Guinier region can be used to give us
an idea of the radius of gyration of any distinct structures that are on this type of lengthscale.
Following Guinier’s law for small q-values the observed intensity can be approximated as:
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(
I ≈ I 0 exp − KR 2 (2ϑ )
2
)
with
2
(
2π / λ )
K=
3
or written as a q-formula:
⎛ q2R2 ⎞
⎟⎟
I (q ) ≈ I 0 exp⎜⎜ −
3 ⎠
⎝
with
q≈
4πϑ
λ
ϑ
for small
Here R is the radius of gyration for the scattering process which depends on the geometrical shape. R
is defined in analogy to the radius of inertia; the difference is that the electrons take place of the mass
elements.
2
(
)
ρ
r
r
dVi
i
i
∫
R2 = V
∫ ρ (r )dV
i
i
V
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It is possible to determine the average particle size if the shape of the particles is known. In a first step
produce a so called Guinier plot, i.e. a plot of ln(I) vs. q2 then determine the slope in its innermost part
from which R can be derived:
q2 R2
ln (I ) = ln (I 0 ) −
3
The geometric radius r for spherical objects can be obtained from the Guinier radius R (radius of gyration)
r2 =
5 2
R
3
In the case of objects which have a shape similar to needles the Guinier formula becomes:
⎛ q2R2 ⎞
1
⎟⎟
I (q ) = I 0 exp⎜⎜ −
3
q
⎝
⎠
with the Guinier plot ln(qI) vs. q2
q2R2
ln (qI ) = ln (I 0 ) −
3
and objects with flat plate shape objects Guinier’s formula is
⎛ q2R2 ⎞
1
⎟⎟
I (q ) = 2 I 0 exp⎜⎜ −
q
3 ⎠
⎝
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The slope, and hence R2, can be obtained by plotting ln(q2I) vs. q2
q2 R2
ln (q I ) = ln(I 0 ) −
3
2
It is found that widely different particle shapes give curves which are only slightly different. This means
practically that one needs extra information such as volume etc. or sometimes one gets only vague
indications on the shapes of the particles.
In the case of a sample which contains a group of non-identical particles, we have
⎛ q2 2 ⎞
I = I 0 ∑ g n exp⎜⎜ − Rk ⎟⎟
k
⎝ 3
⎠
2
k k
with nk is the number of electrons for the particle of the k-th group, Rk is the radius of gyration of group
k and gk is the proportion. The resulting curve is not an exponential any more.
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Components of the SAXS System
X-ray Optics
The complete primary optical system which conditions the parallel primary X-ray beam consist of an
active crossed multilayer monochromator system and a passive pinhole collimation system. The
crossed multilayer monochromator - the Göbel mirror - has two functions:
•
Selection of the characteristic Kα-radiation from the continuous white spectrum that means
monochromatisation of the X-ray radiation.
•
Conditioning of the two dimensional divergent beam to a two dimensional parallel beam.
In general this beam is good enough for standard scattering and diffraction experiments. However,
this monochromatic and parallel beam is not ideal concerning SAXS critical properties as beam size
and shape, cleanness and divergence, especially around the direct primary beam.
A pinhole collimation system conditions the beam and its direct vicinity in such a way that SAXS
measurements can be done with highest resolution by lowest background.
In the next sections the basics of the multilayer optics system is described, then the principal function
of the pinhole collimation system, followed by the coupled function of both and the function of other
components.
Göbel Mirrors Optics
As shown in the schematic drawings of Fig. 1-58/Fig. 1-123/Fig. 1-126/Fig. 1-127 a Göbel mirror (GM)
is a multilayer of approx. 100 pairs of layers with a large scattering contrast. The layer has a gradient
in d-spacing (Fig. 1-123). Further the layer’s surface is bent to the shape of a parabola (Fig. 1-123).
The d-spacing, its gradient and the multilayer’s surface shape are fit to each other so that each Kα-ray
which comes from the source (the anode) in the focus of the parabola is diffracted on the multilayer
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according to Bragg’s law into one direction. In this way a divergent beam is directed into a parallel
beam (Fig. 1-123).
A crossed coupled Göbel mirror (ccGM) means two mirrors which are arranged perpendicular to each
other as shown in the schematic drawing of Fig. 1-58 and Fig. 1-124. The foci of both mirrors must
coincide with the focus of the X-ray source which is a line focus source F (Fig. 1-124).
The first mirror GM1 has a focal length of D1 and the second GM2 has D1 + D2. GM1 conditiones the
divergent beam parallel in the drawing plane and GM2 does it perpendicular to this plane.
All what was described up to now was the ideal situation. The first deviation from the ideal state in
reality concerns the shape of the X-ray source. Each real X-ray source - even when it is called point
focus - has finite dimensions.
The SAXS system uses a point focus source (sealed tube or rotating anode). This means that a
source with line focus F is arranged in such a way that the multilayer mirror system ‘sees’ a point focus (Fig. 1-124). The line shaped focused electron beam hits the anode and generates X-rays which
are illuminating the half sphere with solid angle 2π over the anode surface.
If the mirror system is arranged in the line direction and the take off angle α (Fig. 1-124) is small then
the active source shape is the projection of the line and hence similar to a point; in the projection the
line is shortened by a factor sin(α). In general α is approx. 6° so that the factor is approx. 0,1 ≈ sin(6°).
As an example the fine focus tube which is used in the SAXS system has a line focus of 0,4mm x
8mm. This means if it is arranged in point focus mode that the size of the point focus is 0,4mm x
sin(6°) . 8mm = 0,4mm x 0,8mm.
The other non ideal property comes from the Göbel mirrors. Since the multilayer has a finite number of
layer pairs it cannot work as a perfect crystal with approx. infinite diffracting lattice planes. The mirror
accepts the characteristic Kα-radiation coming from the X-ray source within a small range ∆ϑ (Fig. 1126).
The expression ‘accepts’ means that Bragg’s law is fulfilled for Kα-radiation and hence incoming and
outgoing angle - the Bragg angle ϑ - must be equal. The consequence is that there remains a retained
divergence of the outgoing beam and the beam is not ideally parallel (Fig. 1-126) depending on the
amount of ∆ϑ which is also called ‘intrinsic divergence’.
A typical value of ∆ϑ (FWHM) for multilayer mirrors is approx. 0,5 mrad (compare to the intrinsic divergence of perfect crystals which is approx. 0,05 mrad).
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The Göbel mirrors GM1 and GM2 of the SAXS system have focal lengths of D1 = 90mm and D1+D2 =
150mm. This means that the ccGM diffracts Kα-radiation from an area of the source which is approx.
45µm x 75µm.
From the complete radiation which is generated from a fine focu tube within the area of 0,4mm x
0,8mm only a very small part of approx. 45 µm x 75 µm ist diffracted (Kα-radiation) into the direction of
the primary beam!
If ∆ϑ is larger, the effective focus size and the intensity increases but the quality of the parallel beam
would decrease because of higher divergence. The values which were given here are a compromise
which lead to a maximum of intensity with tolerable divergence in the beam.
Another effect will deteriorate the quality of a parallel beam for SAXS applications. As mentioned
above the ‘point’ focus source size (0,4mm x 0,8mm) is larger than necessary (45µm x 75µm). This
means that not only characteristic Kα-radiation is diffracted into the parallel primary beam but also
other wavelengths (Fig. 1-28 and Fig. 1-127) of the white spectrum from the border of the point focus.
This parasitic radiation is divergent and only appears in the direct vicinity of the primary beam and
hence it does not disturb normal XRD measurements. Further the intensity is low because it comes
from the continuous white bremsstrahlung near the Kα-line. This radiation is not too different from Kα,
so it cannot be discriminated with a gas counter as the HiStar and increases the background around
the direct Kα primary beam.
For the first mirror GM1 which has a length of 40mm the additional divergence caused by the parasitic
non-monochromatic radiation is several mrad in maximum (the monochromatic ‘parallel’ beam remains at 0.5mrad). The second mirror GM2 has a length of 60mm and leads to an additional divergence of some mrad of non-monochromatic parasitic radiation (also here the monochromatic ‘parallel’
beam remains at 0.5mrad).
The result of this discussion shows the limits of high end X-ray optics and sources: The ‘parallel’ beam
of a ccGM without any pinhole collimation system has an intrinsic divergence FWHM of Kα-radiation
(property of the X-ray mirror), additional there is a part of divergent non-monochromatic parasitic radiation of several mrad (property of the ‘point’ focus X-ray source) if no collimators, piholes and slits
are used (nevertheless the monochromatic ‘parallel’ beam remains at 0.5mrad).
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Pinhole Collimation System
From the discussion above it is clear that an additional conditioning of the beam is desirable. If an
ideal parallel beam is used one pinhole P1 (Fig. 1-31, Fig. 1-121) is sufficient to condition a small Xray beam with defined round cross section. This pinhole must consist of strongly absorbing material.
This simple arrangement has the disadvantage that the pinhole emits secondary radiation S (Fig. 1121), parasitic scattering or edge scattering from its edge. This radiation can be WAXS, SAXS or fluorescent radiation of the pinhole material.
If the sample under investigation has very strong small angle scattering and very small angles are of
no interest then the measured results can be satisfactory. As shown in Fig. 1-31/Fig. 1-32/Fig. 1-121 a
second pinhole P2 leads to a considerable improvement. The size of P2 must be a little bit larger than
that of P1 so that it is not hit by the primary beam PB2 (Fig. 1-121).
In this arrangement P2 is placed as close as possible to the beam PB2 (Fig. 1-122), defined by P1.
Let us investigate the effect of P2 by considering the parasitic scattering emitted from the edge of P1.
This radiation covers from 1 to 1´. All scattering at larger angles is absorbed by P2.
Between 2 and 2’ the parasitic radiation is more intense than between 1 and 2 and 1’ and 2’ because
the lower and upper edges (in this two dimensional representation) contribute simultaneously.
It is not recommend to measure in the range between 2 and 2’, while within the ranges 1-2 and 1’-2’
give often reasonable results especially with strongly scattering samples.
In the next section the combination of ccGM and pinhole collimation system is discussed. The more
simpler case is the pinhole collimation system of compact SAXS systems which conditions a very
small beam for scanning SAXS measurements (Fig. 1-31).
The more complex one is the 3-pinhole collimation SAXS system (Fig. 1-30). In this case the diameter
of the parallel beam is larger, hence the volume of the irradiated sample is larger and hence the surrounding of the beam must be very ‘clean’ in order to measure at small angles of a relatively large
beam.
Combination of ccGMs With Pinhole Collimation
According to the discussion above, the parallel beam which comes only from a ccGM is not ideal. For
scanning measurements a small beam diameter is needed in order to get a good spacial resolution.
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At least one pinhole is necessary in order to reduce the diameter of the original ccGM beam which is
approx. 0,8mm base width (GM exit) to a size of 100µm. The distance between X-ray focus (source)
and this pinhole is approx. 270mm (Fig. 1-31). This reduces the divergence of the non-monochromatic
parasitic radiation from horizontal and from vertical to some mrad.
As described in the section before this 100µm pinhole produces additional parasitic radiation which is
removed mostly by a second 300µm pinhole at a distance of approx. 130mm from the first one.
The divergence of the additional pinhole edge scattering is limited from the 300µm pinhole to approx.
3mrad.
Design of the Instrument
The functional important components of the NanoSTAR U SAXS system (Fig. 1-1, Fig. 1-3) are:
•
X-ray parallel beam system (PBS) (Fig. 1-6 and Fig. 1-10)
- X-ray tube with mount
- 4DOF
- ccGM (cross coupled Göbel mirrors)
- 0-Pinhole
- Absorber slit holder
- 1st pinhole
- X-ray labyrinth flange
•
Primary beam path tubes (Fig. 1-12)
- Entrance window
- First and second beam path tube
- Exit window
•
Beam defining pinhole (Fig. 1-12 and Fig. 1-26)
- X-ray labyrinth flanges
- Pinhole unit
- 2DOF
- Vacuum flanges
•
Antiscatter pinhole (Fig. 1-27 and Fig. 1-71)
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•
Sample Chamber (Fig. 1-7 and Fig. 1-27)
- Chamber
- Sample holder
- Automatic sample changer
- Scanning stage
- Reference sample changer
- Vacuum cone
•
Vacuum system (Fig. 1-125, Fig. 1-26, Fig. 1-116, Fig. 1-117, Fig. 1-128-Fig. 1-130)
- Vacuum control panel
- Vacuum pump
- Vacuum switches
- Vacuum gauges
•
Security system (Fig. 1-44, Fig. 1-52-Fig. 1-55, Fig. 1-133)
- Beam path control line
- Sample chamber window
•
Scattering tubes (Fig. 1-43, Fig. 1-61, Fig. 1-135, Fig. 1-139)
- Two tubes for extended SAXS
- One tube for SAXS
- No tube for WAXS
- No tube with extender for extended WAXS
•
Primary beam stop (Fig. 1-15, Fig. 1-8)
- Beam stop unit with strings
- Beam stop ring
- Security plug
- X- and y-translation micrometer head screws
•
2D-Detector (Fig. 1-8, Fig. 1-63, Fig. 1-75, Fig. 1-140)
- Detector
- Controller
- Frame buffer PC with software
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The functional important components of the NanoSTAR C SAXS (Fig. 1-4, Fig. 1-5) system are:
•
X-ray parallel beam system (PBS) (Fig. 1-6 and Fig. 1-10)
- X-ray tube with mount
- 4DOF
- ccGM (cross coupled Göbel mirrors)
- 0-Pinhole
- Absorber slit holder
- 1st pinhole (beam defining pinhole)
- X-ray labyrinth flange
•
Antiscatter pinhole (Fig. 1-27 and Fig. 1-71)
•
Sample Chamber (Fig. 1-13)
- Entrance window
- Chamber
- Sample holder
- Automatic sample changer
- Scanning stage
- Reference sample changer
- Vacuum cone
•
Vacuum system (Fig. 1-128, Fig. 1-116, Fig. 1-117)
- Vacuum pump
- Vacuum switches
- Vacuum gauges
•
Security system (Fig. 1-44, Fig. 1-52-Fig. 1-55, Fig. 1-133)
- Beam path control line
- Sample chamber window
•
Scattering tubes (Fig. 1-43, Fig. 1-61, Fig. 1-135, Fig. 1-139)
- Two tubes for extended SAXS
- One tube for SAXS
- No tube for WAXS
- No tube with extender for extended WAXS
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•
Primary beam stop (Fig. 1-15, Fig. 1-8)
- Beam stop unit with strings
- Beam stop ring
- Security plug
- X- and y-translation micrometer head screws
•
2D-Detector (Fig. 1-8, Fig. 1-63, Fig. 1-75, Fig. 1-140)
- Detector
- Controller
- Frame buffer PC with software
Operating Instructions and Alignment
X-ray Parallel Beam Source (PBS)
The parallel beam source system (PBS system) is the component from which a well defined and conditioned parallel and monochromatic X-ray beam comes from. X-ray source can be a fine focus sealed
tube (ST) with high power density.
The X-rays which are emitted from the anode are monochromatized by two multilayer optics with high
spectral purity (Kα-radiation). In addition the rays which leave the multilayers form a beam which is
parallel in two dimensions (Fig. 1-124, Fig. 1-141).
In order to remove all other radiation which leaves the multilayer optics a pinhole collimation system
‘cleans’ the surrounding area of the monochromatic parallel beam and defines a symmetric round two
dimensional profile (Fig. 1-30, Fig. 1-31).
This pinhole collimation system (long U system) consists of 3 pinholes from which one - the first pinhole - is part of the PBS (Fig. 1-48). Directly at the Göbel mirror’s housing exit an additional pinhole 0
(Fig. 1-21) is positioned (exit pinhole). This exit pinhole removes most of the disturbing radiation before the main Kα beam reaches the 1st pinhole.
This beam is used for further conditioning by other pinholes. The mechanical interface from the beam
exit to the primary beam path tube system is realized with a radiation safe labyrinth flange e (Fig. 140).
This beam can be aligned to the rest of the SAXS system by an alignment stage with four degrees of
freedom (4DOF).
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X-ray Tube With Mount
The X-ray tube which is used (KFFCu2K-90 or KFFCo2K-90) is a ceramic diffraction tube (KF-type) on
which a 90° cooling head (K-90-type) is mounted to operate it in point focus orientation. The focus is a
fine focus (F-type) on a Cu- or Co-anode. The beam exit window is made of Beryllium.
WARNING
Never touch the Beryllium windows of the tube and do not clean them. Fumes or the dust from Beryllium and its compounds can be hazardous if inhaled! During use corrosion of beryllium may occur.
Beryllium must not be cut, machined or handled in any way. Disposal of parts containing beryllium
must comply with all applicable national regulation.
The tube is water cooled with an internal water cooling system and a water temperature of approx.
30°C. This cooling concept avoids condensation of water on the tube and optics and guarantees a
constant water quality in the primary water cooling system.
The size of the point focus under 6° take off angle is 0,4mm x 0,8mm. The maximum power of the
tube may never exceed 1,5kW for Cu and 1,2kW for Co. You should set your generator to parameters
40kV / 35mA for Cu and 40kV / 30mA for Co only for test purposes. For normal use please set to 20%
less power.
Use the max. values not for normal measurement modes because these parameters decrease lifetime. In normal measurement mode we recommend 80% of max. power, this is 40kV and 30mA for Cu
and 40kV and 25mA for Co radiation.
The tube is mounted on a stable and precise XY-stage (Fig. 1-64, Fig. 1-67) and the optics is directly
fixed onto the tube mount via a knife edge adapter (Fig. 1-19, Fig. 1-38, Fig. 1-39). The cover (Fig. 123) of the radiation housing is integrated into the security circuit to guarantee maximum security during the optics alignment. The radiation safety housing is mounted onto an additional support (Fig. 1142) which gives an optimum degree of stability.
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4DOF
The 4DOF carries the parallel beam source system and allows the alignment of the beam relative to
the SAXS system. Two perpendicular rotation axes, one in x- and the other in y-direction enable the
adjustment of the parallel beam perpendicular to the detector (Fig. 1-64, Fig. 1-95-Fig. 1-98).
With the two translation stages in y- and x-direction the X-ray beam can be aligned to the centre of the
detector. This is the final orientation of the parallel beam relative to the detector. All other components
as sample, pinholes, primary beam stop etc. use this line (the oriented beam) as reference position.
After the alignment of the degrees of freedom is finished, these must be fixed with screws (Fig. 1-64,
Fig. 1-67) and the alignment has to be checked again because of the small backlash of the 4DOF.
ccGM (cross coupled Göbel Mirrors)
The main components of the X-ray optics are two bent gradient multilayer X-ray mirrors (Fig. 1-58,
Fig. 1-123, Fig. 1-124, Fig. 1-126). One mirror is 40mm long and has a focal length of 90mm (distance
from X-ray source focus to mid of mirror). The other one is 60mm long and has a focal length of
150mm. Both mirrors are arranged perpendicular to each other.
Mirror Shape and d-spacing
The multilayers consist of approx. 100 pairs of layers A and B. They must have a large difference in
electron density to give a significant contrast for Kα X-rays.
The shape of the mirror’s multilayer is a part of a parabola with focus at position of the X-ray source
(Fig. 1-58, Fig. 1-123, Fig. 1-124, Fig. 1-126). This shape diffracts the rays into one direction as is
known from parabola mirrors for visible light.
The d-spacing of the multilayer is typically some nm and has a gradient along the mirror. This is necessary because the angle ϑ between the incoming ray (from the focus) and the mirror’s surface depends on its position along the mirror’s length l. So ϑ is a ϑ (l) and in order to fulfil Bragg’s law
1 2 sin (ϑ )
λ
=
→ d (l ) =
d
λ
2 sin (ϑ (l ))
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the d-spacing must change along the mirror’s length.
The multilayer optics are optimized to the Kα-radiation of the anode material. This means that the
multilayer material combination A and B, the d-spacing gradient and the curvature are optimized to the
radiation. This means practically that a Co-mirror cannot be used for Cu-radiation.
Intrinsic Divergence
A multilayer mirror is an artificial one dimensional crystal with limited periodicity. This means that the
constructive interference of this lattice which forms the Bragg peaks has also a limited width. In contrast to this situation a nearly perfect crystal with practically infinite periodicity makes practically infinite
sharp Bragg peaks (Darwin’s reflection width is some 0.001°).
The reflection width ∆ϑ of our mirrors is typically 0.03° and is also called intrinsic divergence (Fig. 1126). This means that the 2 dimensional parallel beam diverges 0.03° in each dimension and hence
becomes broader at large distance.
If x is the focal length relative to the mid of the mirror and p is the parabola parameter then the 2ϑangle in the middle of the multilayer mirrors can be calculated
⎛ 2p ⎞
⎟
2ϑ = arctan⎜⎜
⎟
⎝ x ⎠
For Cu-Kα pCu = 0.075mm, x1 = 90mm for the first mirror with length l1 = 40mm and x2 = 150mm for
the second mirror with l2 = 60mm. Co mirrors have a p-value of pCo = 0.1mm because p is approx.
proportional to λ2.
0-Pinhole
This 0-pinhole removes most of the disturbing radiation before the main Kα beam (d) reaches the 1st
pinhole. All in all there are 4 main beams coming from the ccGM housing which can also be seen on
the detector (Fig. 1-91).
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The 0-pinhole selects the beam d. Most of a, b and c are blocked by the absorber of the pinhole but
not all because the local separation of the different beams is not enough at the pinhole position. This
0-pinhole or exit pinhole can be adjusted by the dove tail screws.
Absorber Holder
In some cases it may be necessary to absorb the radiation to avoid an overexposure of the detector.
We recommend always to run the X-ray source with the same parameters of power (kV and mA) as
you aligned the Göbel mirror optics. If the system was aligned with max. power, please use at least
10% less.
1st Pinhole or Divergence Pinhole
The first pinhole with a diameter of 750µm is mounted in an XY-translation stage with micrometer adjustment screws for ±6mm setting range in x- and y-direction. The pinhole is very precise in a Pt-slice
which is mounted in a holder with thread.
The 1st pinhole with XY-translation stage is a part of the PBS system (parallel beam source). It is directly mounted onto the radiation safety shielding of the X-ray optics. With this concept it is easier to
align the pinhole collimation system. The alignment steps are:
•
Align the first GM.
•
Align the second GM and insert slit between 1st and 2nd one.
•
Move the 0-pinhole to the twice reflected parallel beam and reduce disturbing radiation.
•
Move the 1st pinhole to the parallel beam.
•
After these steps you have a ‘clean’ monochrome and parallel beam which can be aligned by
the 4DOF perpendicular into the centre of the detector.
The detailed description of the alignment will follow in another section of this manual.
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X-ray Labyrinth Flange
The first X-ray labyrinth flange ensures the radiation safe connection to the first X-ray beam path tube.
In order to avoid that radiation comes out between this mechanical connection also these components
are saved by beam path control line.
Only when both sides of the labyrinth interface are positioned narrow enough together, the safety system allows to switch on the generator. If the slit is too broad and a risk for radiation damages exists
the generator will switch off or remains off.
Primary Beam Path Tube System
The beam path tubes are made of steel and give radiation safety for all user’s works. The complete
primary beam path has to be evacuated. An evacuation is necessary because the absorption and
background scattering is too high in air.
Additionally to the beam path control line the vacuum is controlled by the safety system. If there is
anything not adapted correctly a proper vacuum is not possible and the safety system avoids to switch
on the generator.
Entrance Window
The vacuum tight entrance window which is placed directly to the X-ray labyrinth of the 1st pinhole has
a special low absorbing X-ray window and is screwed in with a screw thread into the end of the tube
(Fig. 1-45). The tube end is supported by a stable support foot.
Exit Window
The exit window of the primary beam path tube system is only necessary when the sample chamber is
under air (Fig. 1-47). In this case the primary beam path tube system and the secondary beam path
system (with inserted cone, Fig. 1-106) are both evacuated. The exit window is identical to the entrance window and is screwed in into the 3rd pinhole component (Fig. 1-71).
Beam Defining Pinhole
The beam defining pinhole is the 2nd pinhole with 400µm in diameter and is positioned between the
two beam path tubes. The pinhole carrier is fixed inside with a magnet. The access to the pinhole is
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via the cover. Also this pinhole is on a XY-translation stage with micrometer adjustment screws for
±6mm setting range in x- and y-direction. The pinhole is very precise in a Pt-slice which is mounted in
a holder with thread.
Antiscatter Pinhole
The antiscatter pinhole is the 3rd pinhole in a 3-pinhole system or the 2nd pinhole in the 2-pinhole system. This pinhole cuts away the edge scattering of the 2nd (1st) pinhole. The antiscatter pinhole is positioned in the chamber an can be aligned with 2 degrees of freedom from outside.
Sample Chamber
The sample chamber has several flanges and a transparent X-ray safe window in the front door.
There is a built-in automatic sample changer which can also be used as a 2D-scanning stage with
sample holder. Additional there is a reference sample wheel with glassy carbon sample and other
sample positions.
Chamber
The chamber has a KF40, a DN ISO-K 63, a KF 16 and a vacuum connection on the rear side. Further
on the left hand side is a KF40 mount for the primary tubes. On the right hand side is a DN ISO-K 160
flange for the secondary tubes and on the top there is a KF25 which can be used to run individual
tests.
In the chamber the antiscatter pinhole is mounted on the left hand side with an XY-alignment stage.
The chamber door is made of transparent plexiglass with a radiation safe lead glass window.
Automatic Sample Changer and 2D Scanning Stage
The automatic sample changer allows sample positioning over distances of 100mm in y- and 80mm in
x-direction with an accuracy of better than 10µm each. All movements can be done with high speed
and maximum reproducibility. The stepper motor is controlled by the measurement software and can
be used in sample changer or scanning mode.
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Sample Holder
The sample holder frame is fixed in the mount with two balls. The sample holder frame can hold up to
18 single samples or 3 sets of 6 samples on a special sample plate.
Reference Sample Changer
The reference sample changer holds several reference samples. One sample, the glassy carbon sample, is built-in from factory. The user can mount samples into the other positions as he likes.
Vacuum Cone
The vacuum cone must be used when the sample is not suitable for vacuum measurements. This
means that the sample under air mode must be active. In this case there must be a vacuum X-ray
window on the primary side chamber entrance window and a vacuum window - the cone - on the secondary side. Both the primary and the secondary tube system must be evacuated during the sample
chamber and the samples remain under air pressure.
Vacuum System
The vacuum system consists of two parts which can be controlled via the vacuum control panel between the two bases. Each vacuum system has a vent valve (small round control knob) and a shut-off
valve. The left shut-off valve shuts off the complete vacuum system from the pump. After activating
this valve one or both vent valves can be opened in order to vent the complete system, i.e. primary
and secondary beam path system and the sample chamber.
If the left shut-off valve remains open and the right one shuts-off then the chamber can be vent by the
right vent valve knob if the chamber is in the sample under air mode. Both, the primary and secondary
beam path tube systems remain under vacuum if the chamber is in the sample under air mode.
Cooling Water System
The cooling unit is located behind the electronic rack. The internal cooling unit enables a relatively
constant temperature of the X-ray source, i.e. the X-ray sealed tube and the temperature sensitive Xray optics.
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Security Circuit
The NanoSTAR SAXS system has two totally independent safety circuits which are implemented by
electro-mechanical components. In case of an error which affects the X-ray radiation safety the two
safety systems will be interrupted and thus the X-ray radiation generation will be switched off. The two
safety circuits control two contactors which are located inside the X-ray generator and enable the generator of high voltage.
Secondary Scattering Beam Path Tubes
The scattering tube is mounted to the sample chamber via an ISO K DN160 flange. The beam stop is
fixed at the rear of the scattering beam path tube. It is possible to mount one or two tubes or remove
all tubes completely. In this case it is possible to measure in WAXS setup. Then the beam stop has to
be fixed directly to the outlet flange of the sample chamber.
Primary Beam Stop
The primary beam stop unit is mounted into a ring with two translation stages which are based on
micrometer head screws. The beam stop unit (small absorbing part which is mounted between the
crossed strings) is made of ‘star metal’ which is a antimony-lead alloy (approx. 87% Pb, 13% Sb).
This material has high absorbing coefficient and low fluorescent rate. The size of the beam stop unit is
matched to the geometry of the system and its beam size. The beam stop unit can be exchanged by
another one with different size in an easy way.
This unit is fixed by two 90° crossed thin strings which are made from capton material. The beam stop
ring is flanged to the detector with quick acting couplings. There are two vacuum O-rings on both
sides of the ring.
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Measurements
2D-Detector
The HiStar area detector is filled with pressurized xenon gas, and is capable of determining the X and
Y position of X-rays which enter its imaging area.
X-rays scatter from the sample and enter the detector through a patented, concave X-ray transparent
entrance window. The curved design of the window reduces parallax by presenting a nearly uniform
distance between the diffracting crystal and the surface of the xenon gas.
Inside, the gas-tight enclosure is pressurized to approximately 4 bar. Because the detector is sealed,
the xenon tube remains stable for years and adjustments to its circuitry are rarely necessary; however,
adjustment of the detector bias is required for use with different X-ray energy sources.
Individual xenon atoms in the enclosure are ionized by incident X-rays, producing a shower of charged
particles each time an X-ray passes through the gas. Inside the detector, these charged particles are
electrically attracted to an electrode assembly, which is a multiwire grid encoded in a proprietary manner to establish optimal spatial resolution of detected events at the detector surface.
The charged particles interact with the electrode assembly to generate electrical signals indicative of
the X-Y position of the original X-ray. From the electrode assembly, electrical signals are routed to a
preamplifier in the detector, then output to the PDC.
The PDC positions a signal, if it falls within a pulse height window. The energy window is fixed and the
signal height is determined by adjusting the detector bias. Because the primary ionization is a function
of X-ray energy, the gain of the detector must be changed when imaging X-rays of different energy.
The detector and PDC produce a 14-bit location (0 to 16,383) in X and Y for each X-ray entering the
imaging area of the detector. This information is coupled to two 16-bit parallel ports in the frame buffer
computer. During data collection, the frame buffer polls the ports for new data.
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When new data is detected, the 14-bit values for X and Y are mapped to a frame pixel (0 to 511 or
1023), which is incremented. The frame buffer combines individual positions and intensity signals from
the PDC into a complete "frame" of information.
Real-time colour display shows the diffraction pattern building up as it is collected. Each frame is typically saved on disk as a single file. The fixed aperture of the detector subtends a large solid angle with
reference to the sample when the detector is close to the sample. When the detector is moved away
from the sample, this solid angle becomes smaller, but the resolution increases.
The diameter of the active area is 10.5 cm with resolutions of 1024 pixel x 1024 pixel and 512 pixel x
512 pixel are possible. Additional to the ‘pixel size’ of 100µm there is a point spread of σ = 200µm
(see chapter about detector resolution) which leads to a spatial resolution of approx. σ = 220µm. The
quantum efficiency for copper Kα radiation is approx. 80% with an energy resolution of approx. 20%.
The HiStar can be used for energies between 3keV and 15keV with a dynamic range of 106.
WARNING
Do not touch the detector window. It is made of Beryllium, a highly toxic metal. Beryllium dust can
cause lung disease if inhaled. Beryllium particles, which penetrate the skin, can cause dermatitis or
ulcers.
WARNING
Severe Beryllium poisoning can be fatal. Though the window has protective coating to prevent contamination, it may not properly protect you if the window gets scratched or otherwise mishandled (creating potential for loose Beryllium particles).
If you touch the window in any manner (gently or otherwise), avoid touching any other body part and
immediately wash the contacted body part. When not using the detector, place a protective cover over
the window.
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CAUTION
Do not manually move the HiStar detector when the PDC BIAS is on. Turn off bias or power off the
PDC before loosening the screws and moving the detector, to avoid damaging the detector grid (a
highly expensive repair item).
When using copper radiation make sure that this is also set in the SAXS software (collect → detector
→ Cu-bias). For installation details please refer to the HiStar reference manual. For software instructions and details refer to the SAXS software manual.
Bias Settings
Please check the following bias adjustment procedure from time to time. Remove the sample holder
frame 2 (Fig. 1-147) from the mounting block inside the sample chamber (Fig. 1-148). Mount the Fe55
source (Fig. 1-143) onto the sample holder via the adapter 1 (Fig. 1-147). Note that the source face
(Fig. 1-143) faces the detector. Insert the sample frame with the radioactive source again and move it
with x- and y-motors to the system axis (where the primary beam position is). Close the door of the
sample chamber and evacuate the chamber.
Activate the following settings in the SAXS software:
• collect → detector → Fe-Bias
• collect → detector → E-vs.-E
• collect → detector → Add
Enter the following parameters in the Add menue:
• Max Seconds 1200
• Pre-Clear Y
• Test Pattern Y
• Max Counts 10000000
• Max Display Counts 20
• Realtime Display Y
• Reset Interval 5
• Open & Close Shutter N
• → OK
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The E vs. E plot is shown as an oval diagonal spot distribution from the top left to the bottom right.
Adjust the detector bias until this distribution is positioned over the first line. Do not forget to switch
back to copper bias and Y vs. X display after this procedure. For details see the HiStar detector manual.
WARNING
55
The Fe sample is a radioactive source! It is possible that personnel might be exposed to radiation.
Use this sample only when it is necessary. After usage put the sample back to the radioactive safe
enclosure. Radioactivity is dangerous and harmful. Make sure that you always work according to the
locally valid X-ray laws and regulations and that the radioactive radiation penetration of personnel is
always as low as reasonably achievable. Only professional radioactive experts especially trained on a
NanoSTAR are allowed to carry out maintenance and alignment work. Bruker-AXS is not responsible
if personnel get hurt by radioactive radiation.
Flood Field Correction
The flood field correction procedure must be done after a change of the geometry (secondary beam
path length) or Bias change. Exchange the beam stop ring by the blank ring. Mount the Fe55 sample
as described in chapter ‘bias setting’ and evacuate the sample chamber. Move the Fe55 sample in
beam position with Cntrl D x- and y-motor settings.
Activate the following settings in the SAXS software and open ‘flood/new options (1024x1024 frames)menu:
• collect → detector → Fe-bias
• process → flood field → new
Enter the following parameters in this menu (Fig. 1-153):
• Max Seconds: as long as possible
• Max Counts: 10 mio
• Lower X: 0
• Lower Y: 0
• Magnification: 1
• Realtime Display Y
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• Open & Close Shutter N
• Output Filename 1024_xxx._fl with xxx the detector distance in cm (or others)
With these settings the SAXS software collects 10 million counts (because this condition is fulfilled first
if the max. seconds value is long enough) and the results do not depend on the age of the Fe55 source
and hence on the intensity decrease of the radioactive source. After this measurement a correction
table is stored automatically on disc and loaded into memory which can be seen at the bottom right
corner of the SAXS software window.
A previously measured correction table can be loaded with process → flood → load or process →
flood → linear (without correction). The sampled frame is not saved automatically on disc. If one wants
to have a look on it later, it must be stored with the file → save command. The flood field correction is
used automatically during the measurements as long as the flood field correction table is loaded. After
a flood field a spatial correction has to be done.
For further details refer to the SAXS software and HiStar manual.
WARNING
The Fe55 sample is a radioactive source! It is possible that personnel might be exposed to radiation.
Use this sample only when it is necessary. After usage put the sample back to the radioactive safe
enclosure. Radioactivity is dangerous and harmful. Make sure that you always work according to the
locally valid radiation laws and regulations and that the radioactive radiation penetration of personnel
is always as low as reasonably achievable. Only professional radiation experts especially trained on a
NanoSTAR are allowed to carry out maintenance and alignment work. Bruker-AXS is not responsible
if personnel get hurt by radioactive radiation.
Spatial or Fiducial Correction (Brass Plate Correction)
A spatial correction must be performed after every flood-field correction. Fig. 1-155 and Fig. 1-156
show two frames recorded with the brass plate. Fig. 1-155 is a measurement without correction and
Fig. 1-156 shows a frame after a spatial correction.
Mount the Fe55 sample as described before (switch to Fe-bias!) and the brass fiducial plate on the
detector face so that the countersunk holes of the plate face the source. Tightly fasten the plate to the
detector face to be sure that the plate is flat and evacuate the chamber.
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Now select process → spatial → new and set the following parameters in the ‘options for process
spatial new’-menue:
• Max Seconds (12 h = 12:00:00) same time as for flood field correction
• Max Counts 10000000
• Output Filename 1024_xxx._br (xxx = distance in cm or use any other name)
• # sigmas spot threshold should be left unchanged (recognition of weak spots)
Click on OK to start collecting spatial correction data. When the system has collected for 12 mio
counts (because this condition is fulfilled first if the max. counts value is long enough), it automatically
builds the spatial correction tables and saves them on disc and loads them into memory. The values
of max. Sec. and max. counts depend on the activity of the Fe55 source!
Previously measured correction tables can be loaded by process → spatial → load and measurements without correction with process → spatial → linear. The measured frame is not saved automatically but can be saved by file → save. The frame itself can be reprocessed with a different value of
‘sigma spot threshold’ by process → spatial → reprocess. View the new spatial file with the extension
._br.
Use ANALYZE → GRAPH → FILE to view the new spatial files with extensions ._ix, ._if, and ._it.
Some “spots” may be missing on the outer edges of the graphs. This is normal and will not affect data
results. The spot patterns should be uniform and not abruptly distorted.
Even if a spatial correction table is loaded, a spatial correction can only be do after a measurement.
Frames can be saved without correction by file → save. To save corrected files use process → spatial
→ unwrap (Fig. 1-157). ‘$frame’ as input file name is the currently displayed frame.
If automated measurements by using collect → scan → multitargets are started and the spatial correction table is loaded, each measurement is saved with the spatial correction. Use process → spatial →
linear in order to save the uncorrected frames.
Switch back the detector bias with collect → detector → Cu-bias when the normal measurement with
Cu is used. Remove the Fe55 sample and the exchange blank ring by the beam stop ring. Caution:
the beam stop position can differ from the one before this change. Before normal measurement operation is started check the correct position of the beam stop with low power (start with 15kV and 10mA).
For further details refer to the detector manual.
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WARNING
The Fe55 sample is a radioactive source! It is possible that personnel might be exposed to radiation.
Use this sample only when it is necessary. After usage put the sample back to the radioactive safe
enclosure. Radioactivity is dangerous and harmful. Make sure that you always work according to the
locally valid radiation laws and regulations and that the radioactive radiation penetration of personnel
is always as low as reasonably achievable. Only professional radiation experts especially trained on a
NanoSTAR are allowed to carry out maintenance and alignment work. Bruker-AXS is not responsible
if personnel get hurt by radioactive radiation.
Samples
Glassy Carbon Transmission
For transmission determination of glassy carbon insert an absorber (1,2,3 or 5 in Fig. 1-149) into the
beam path (e.g. 100 µm to 150µm copper thickness) or 4,2,3 (Fig. 1-149) between the Göbel mirrors.
Determine IABS, the integral over the complete detector area. Move the glassy carbon sample with the
reference sample wheel into beam position while leaving the absorber still inside and start another
measurement. Determine IABS+GC, the integral over the complete detector area. The glassy carbon
transmission factor is then given by:
t GC =
I ABS +GC
I ABS
The integral signal IABS+GC should be at least 10000 counts. If necessary, increase the measuring time.
If the signal is too small (compact setup) reduce the absorber thickness. If possible check transmission factor with different absorbers.
Sample Transmission
Determine four integral signals (cps) over the complete detector area:
• Sample signal: IX
• Glassy carbon with sample: IX+GC
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•
Operating Instructions and Alignment
Glassy carbon signal: IGC
Blank signal without sample and GC: I0
The measurement time depends on the signal strength. The blank measurement and glassy carbon
measurement need only be done once for a complete series of samples. The transmission of the unknown sample is determined by
tx =
I X +GC − tGC ∗ I X
I GC − tGC ∗ I 0
This calculation can be done with analyse → transmission in the SAXS software (Fig. 1-165). Choose
the files for the four measurements then the result is written on the right side as well as the count rates
of all four measurements. Note, that only for solid samples the background is ‘no sample’. For samples in a liquid the correct background is the signal from the liquid. Or if a scotch tape as ‘sample
holder’ is used then the background is the signal from the scotch tape.
Absolute Calibration
The result of the absolute calibration is the number of photons in the direct beam. First determine the
scattering signal (cps) of pure water:
• Determine transmission factor of glass capillary as sample as described before
• Determine transmission factor of glass capillary filled with water as described before
• Determine transmission of water:
t
t H 2O = H 2O +CAP
t CAP
•
•
Start a Chi-Integration from –180° to +180° with the SAXS software for both measurements.
The result is the scattering signal I(q) depending from q-vector. Choose ‘1-Avg pixel’ in the
‘Options for Peaks Integrate Chi’ for field ‘Normalize intensity’ (Fig. 1-151).
If ICAP(q) is the scattering function of the empty capillary and IH2O+CAP(q) is the intensity of capillary filled with water then determine the scattering intensity of water
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I H 2O (q) = I H 2O +CAP (q ) − t H 2O ∗ I CAP (q )
•
Don’t use SAXS for the last calculation because of the low signal of water because this may
result in wrong results.
The result - the scattering signal of pure water vs. the scattering vector q - should be a constant signal
and not depend on q similar to the function which is shown in Fig. 1-152.
Now determine the absolute number of photons I0 which hit the sample:
I0 ⋅ A ⋅ ε =
with:
•
•
•
•
•
I H 20
⋅ 4π
ρ 2 ⋅ b 2 ⋅ k B ⋅ T ⋅ χ T ⋅ d ⋅ τ ⋅ ∆Ω
•
•
•
I0 primary intensity on sample
IH2O as determined before
A beam area on sample
ε detector efficiency
ρ number of molecules per volume unit (from stochastic composition of H20 → ρ = 3.346 *
1022 cm-3)
scattering length of molecule: b = z * re (from no. of electrons and classical electron radius: b =
2.818 * 10-12 cm)
kB = 1.38 * 10-23 JK-1, Boltzmann’s constant
T sample temperature
χ T = 46 * 106 atm-1, isothermal compressibility of water
•
•
•
d sample thickness (determine from transmission)
τ sample transmission
∆Ω solid angle from sample to detector
•
If the detector efficiency and the beam area on the sample are not known then calculate I0 * A * ε for
further use (ε for copper is approx 80%).
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Determination of Sample to Detector Distance
Mount the silver behenate sample (Fig. 1-77) onto the sample frame and insert it into the sample
chamber as shown in Fig. 1-71. Start a measurement with 600s (Fig. 1-159) and choose process →
calibrate. With ‘auto mode’ (Fig. 1-158) the calibration will start automatically. After the first ‘loop’ enter
‘yes’ to update the values. Repeat this several times until the values for beam position and distance
do not change any more.
If one wants to determine the value manually, move the ring structure until it coincides with the measured silver behenate frame. For moving the ring structure use ‘c’ for toggling between position and
size adjustment and the arrow keys. With this procedure also the beam position is determined.
Determination of Sample Position
Mount the samples on the sample carrier (Fig. 1-118) similar to the samples shown in Fig. 1-134.
Mount the sample carrier(s) on the sample frame and insert into the measurement chamber. Then
move the glassy carbon sample with the reference sample wheel into the beam path. Choose collect
→ scan → nanography, enter x- and y-values with interval and a time for seconds/frame (1s or more),
the rest remains unchanged.
After start of the measurement, the sample is moved in x- and y-coordinates according to the values
from above. The count rate is displayed in colours as shown in Fig. 1-161. Analyse this sample transmission image and select the desired measuring coordinates:
•
manually: move mouse to a position and read the coordinates and count rate in the bottom
right corner.
•
automatically: pick the ‘targets’ by left click on the mouse at the desired positions. If one
chooses ‘edit/send targets’ from the menue then the ‘send targets to SAXS/start collecting targets’ (Fig. 1-162) window appears. Enter ‘send’ then ‘collect’, return to SAXS and choose collect → scan → accept-targets. Choose collect → scan → edit-targets then the measurement
positions are shown. Here one can edit it desired (Fig. 1-163).
‘run#’ and ‘frame#’ changes the file names which are generated by the automatic measurements. Now
choose collect → scan → multi-targets and look to the window in Fig. 1-164. Enter a job name and
start measurement. In this example files are generated with name: test0_1_000, test0_2_001,
test0_3_002 and test0_4_003. We recommend to start a measurement additionally without sample in
order to have empty beam and glassy carbon signal.
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Alignment Overview NanoSTAR U SAXS System
NanoSTAR U, Compact, Long Version, One Tube or …? What’s That ?
Fig. 1-1 shows a NanoSTAR U SAXS system. This system has a long primary beam path tube (a) with
a 3-pinhole collimation system (b,c,d) and a fine focus sealed tube (e). Additionally see two secondary
beam path tubes (f). All is mounted on a stable granite (g) and steel table top (h) with two D8-bases
(i,j).
Fig. 1-2 shows a NanoSTAR U in compact setup without long primary beam path tubes. This system
has a 2-pinhole collimation system (k,l) and a fine focus sealed tube (m). Additionally there are two
secondary beam path tubes (n). All is mounted on a stable granite and steel table top with two D8bases as described before.
Fig. 1-3 shows also a NanoSTAR U. This system has a long primary beam path tube with a 3-pinhole
collimation system and a fine focus sealed tube as described before. Additionally there is one secondary beam path tube (o). All is mounted on a stable granite and steel table top with two D8-bases as
described before.
The parallel beam source (PBS) is shown in Fig. 1-6. The PBS is the source, with Göbel mirrors, exit
pinhole and the 1st pinhole and 4DOF. A parallel monochromatic beam comes out from this system
unit.
The parallel beam source (PBS) system with sealed tube (ST) is shown in Fig. 1-6. The PBS is the
source (sealed tube) (w), with Göbel mirrors (x), exit pinhole and the 1st pinhole (y) and the 4DOF (z).
A parallel monochromatic beam comes out from such a system.
Fig. 1-7 shows the chamber where an X-ray window (a) on the primary side and a cone with X-ray
window (b) on the secondary side can be mounted in order to let the chamber under air during evacuating the secondary and the primary beam path tubes.
Fig. 1-8 shows the detector with mount (c) and beam stop (d). The beam stop unit (d) can be aligned
with two perpendicular micrometer translation units (e,f). (g) is the beam path control line plug.
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Which Components of the NanoSTAR U Systems Have to be
Aligned?
1. Table top with main track system
The granite plate (g) (Fig. 1-9) consists of two smaller plates (h,i) and is mounted between the main
track system (j) and the steel table top (k).
2. Parallel beam source system (PBS) with slit, exit pinhole and 1st pinhole:
• X-ray source (sealed tube l in Fig. 1-10)
• Göbel mirrors GM (n)
• Slit and pinholes (o)
• 4DOF (p)
3. Primary beam path tube with 2nd pinhole
The primary beam path tube system is shown in Fig. 1-12 and leads the beam through the 2nd pinhole
(q) which can be aligned in x- and y-direction by micrometer translation screws (r,s).
4. Sample chamber with 3rd pinhole
The 3rd pinhole (t) is a part of the sample chamber as shown in Fig. 1-13 and Fig. 1-14. It is inside the
chamber but can be aligned from the outer micrometer screws (u) and (v). Here the X-ray window (w)
is mounted when the system shell be used in the sample under air operation mode. In this mode the
cone (x) must also be mounted as shown Fig. 1-14.
5. Secondary beam path tube with beam stop
The beam stop is fixed with 2 strings (y,z) as shows in Fig. 1-15. The small beam stop unit (a) can be
moved via the strings by two micrometer screws (b,c).
What Degrees of Freedom are Available for Alignment
1. NanoSTAR base
• Table top height alignment must be done by 8 screws (d) as shown in Fig. 1-16. Each D8base has 4 screws in its corners under the steel plate.
• Track system line alignment (Fig. 1-17). Each track line consists of 2 shorter tracks (e,f)
which can be aligned by means of a third track (g). The distance of the two parallel tracks
can be aligned by the PBS on the primary side or the detector track mount on the secondary side as shown in Fig. 1-18.
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2. Göbel mirror alignment:
• Bragg screw of the first mirror (1 in Fig. 1-19).
• Tilt screw of the first mirror (2 in Fig. 1-19).
• 3rd screw of the first mirror (3 in Fig. 1-19).
• Bragg screw of the second mirror (5 in Fig. 1-22).
• Tilt screw of the second mirror (6 in Fig. 1-22).
• 3rd screw of the second mirror (7 in Fig. 1-22).
• Knife edge screw at the entrance of the first mirror (4 in Fig. 1-19).
• z and y translation screws of the pinhole at the exit of the second mirror (8 and 9 in Fig. 121).
• z and y translation micrometer head screws (10 and 11 in Fig. 1-23) of the 1st pinhole (divergence pinhole).
3. 4DOF alignment:
• x-translation (Fig. 1-24) of the primary beam.
• y-translation (Fig. 1-24) of the primary beam.
• Φ-rotation (vertical rotation axis) of the primary beam (Fig. 1-25).
• ψ-rotation (horizontal rotation axis) of the primary beam (Fig. 1-25).
4. 2nd pinhole alignment:
• x (b in Fig. 1-26) and y (a in Fig. 1-26) translation micrometer head screws of the 2nd pinhole (beam defining pinhole). The pinhole is under the lid (c in Fig. 1-26).
5. 3rd pinhole alignment:
• x (e in Fig. 1-27) and y (d in Fig. 1-27) translation micrometer head screws of the 3rd pinhole (antiscatter pinhole). This pinhole is inside the sample chamber.
6. Beam stop alignment:
• x (f in Fig. 1-28) and y (g in Fig. 1-28) translation micrometer head screws of the beam
stop.
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What will be the Result After the Alignment Procedures?
1. Göbel mirror with slit and exit pinhole alignment results in a 2-dimensional parallel monochromatic
primary beam (with Kβ but relatively clean of white radiation). The reason of Kβ is the large source
focus as shown in Fig. 1-29. Additionally there is a small amount of non monochromatic radiation
which comes from the white spectrum. The knife edge cuts away the most part of the direct white
beam. The slit between both mirrors selects the single diffracted beam from the first mirror (depends on setting of the knife edge). The exit pinhole (1000µm at U-Systems) selects the double
diffracted Göbel mirror Bragg peak from the rest (depends on setting of knife edge). The 2- and 3pinhole collimation system along the beam path makes a spatial separation of the monochromatic
Kα radiation from the rest, especially the Kβ can totally be removed.
2. 4DOF: Primary beam is perpendicular to the detector plane and hits its centre, i.e. the primary
beam path is on the physical system axis.
3. 3rd pinholes: They have to be also on the physical system axis. The 1st and 2nd pinhole define the
maximum divergency which is accepted by the pinhole collimation system. It is optimized to the
natural or intrinsic divergency of the optical mirror system (Bragg reflections on limitied multilayer
systems). Fig. 1-30 shows the 3-pinhole collimation system. Here P0 is the exit pinhole of the
Göbel mirror which removes most of unwanted signals. The 3rd pinhole of the 3-pinhole collimation
system 2-pinhole collimation system cuts away the edge scattering from the 1st and 2nd pinhole
and reduces the background on the detector significantly (Fig. 1-32 and Fig. 1-33). In a 3-pinhole
collimation system (Fig. 1-32) the size of the 3rd pinhole is a small amount larger than the beam
size. If the 3rd pinhole is not aligned very well then the beam hits the edge of the pinhole and produces parasitic radiation as seen in Fig. 1-33.
4. Beam stop: The direct beam is completely shadowed with a minimum of background noise.
Which Alignment Steps Have to be Done?
1. Table top and track alignment:
• Check that both granite plates are in plane with a water level in all directions. If not,
check alignment of 8 screws (height alignment) as seen in Fig. 1-16.
• Check that the tracks are in line as seen in Fig. 1-17.
• Check on left hand side (primary) with PBS that the first two tracks have the correct
distance. Check on right hand side (secondary) with detector that the second two
tracks have also the correct distance.
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2. Presettings:
• 4DOF:
i. x- and y-translation
ii. Φ-, ψ-rotation
• Crossed Coupled GM ccGM:
i. Tilt and Bragg angle of 1st and 2nd GM,
ii. knife edge,
iii. exit pinhole
• 1st, 2nd and 3rd Pinhole
• Sample Stages
• Beam stop
3. Alignment of the Göbel mirror:
• Optimize 1st mirror in Kα Bragg position
• Optimize 2nd mirror in Kα Bragg position
• Optimize knife edge, tube height, relative position of the GMs
• Set exit pinhole to double diffracted Bragg peak
• Set 1st pinhole to beam
4. 4DOF:
• Set Φ-, ψ-rotation so that the beam does not move on the detector when the detector
sample distance is changed, i.e. that the beam is perpendicular to the detector face.
• Set x- and y-translation so that the beam is in the centre of the detector area.
5. Pinholes:
• Set 2nd pinhole to maximum intensity
• Set 3rd pinhole to maximum intensity
6. Beam stop:
• Set Beam stop to minimum intensity
• Check position of 3rd pinhole and reduce scattering to minimum signal.
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SAXS Operation Modes
In this section all possible measurement modes are described. As the NanoSTAR is very flexible a
wide variety of modes is possible. On the one hand the primary beam path and hence the beam properties can be changed. On the other hand the secondary beam path and hence the diffraction angle
range is variable. Further there is the possibility to measure the sample under vacuum and also under
air pressure if it is a critical sample (burst in vacuum). In some cases it is possible to measure the
sample under He or other gases.
1. Measurements with samples under vacuum
a. NanoSTAR U system (for high intensity applications)
i. High resolution (extended SAXS, 1070mm)
ii. Short beam path (670mm)
iii. Very short beam path (WAXS, 270mm)
iv. Very short beam path and WAXS extender (WAXS, 60mm or less)
b. NanoSTAR U system in Compact setup (scanning SAXS applications)
i. High resolution (extended SAXS, 1070mm)
ii. Short beam path (670mm)
iii. Very short beam path (WAXS, 270mm)
iv. Very short beam path and WAXS extender (WAXS, 60mm or less)
2. Measurements with sample under air mode (or other gases)
The same configurations as described above under ‘Measurements with samples under vacuum’ are
possible. Follow these steps to get a configuration which enables measurements with samples under
air.
a. Insert the primary X-ray window as shown in Fig. 1-46 and Fig. 1-47.
b. Insert the secondary X-ray window cone (Fig. 1-111) as shown in the sequence of Fig. 1103, Fig. 1-104, Fig. 1-105, Fig. 1-106, Fig. 1-107, Fig. 1-108, Fig. 1-109 and Fig. 1-110.
i. Loosen the clamps for secondary tube on chamber flange as shown in Fig. 1-103
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ii. Move back tube system with detector as shown in Fig. 1-104. Attention! Do not
forget to switch off the detector bias before moving the detector
iii. Insert the cone as shown in Fig. 1-105. Take care of collision with sample holder
etc.
iv. Try to fix the cone or hold it carefully in correct position (Fig. 1-106)
v. Now move the tube carefully to the cone (Fig. 1-107)
vi. If the cone is not stable in its position and it is impossible to move the tube to the
cone without tilting it hold the cone from inside the chamber as shown in Fig. 1108.
vii. Now move the tube that it contacts the sealing rubber ring in the correct way (Fig.
1-109).
viii. Check from inside the chamber whether the cone’s position is stable (Fig. 1-110).
ix. Close the vacuum valve (position ‘shut’ of right valve) of the chamber and vent it
(right knob counter clockwise) (Fig. 1-125).
x. Open the vacuum valve (position ‘opent’ of left valve) of the tube system and
close vent valve (left knob clockwise) (Fig. 1-125).
xi. We recommend to evacuate the system first before fixing the tubes with the
clamps again (Fig. 1-103)
xii. When the vacuum reaches good values and you are sure that the cone sealing
ring does not leak then fix the clamps.
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Alignment Details NanoSTAR U SAXS System
Some Remarks
•
It is time consuming to get a beam through a pinhole or a slit proceeding step by step like
i. Turn pinhole translation a small amount
ii. Start measurement und read intensity
iii. If intensity is not satisfactory goto i)
•
The beam can be found quickly, if the measurement parameters are configured as follows:
•
Press Ctrl Shift A to start options for collect add. “Pre-clear” means that after each “Reset interval” of 1 sec. the image is cleared and the measurement is displayed in realtime for 5000
measurements. This is similar to a “ratemeter” where knobs and screws can be turned by directly observing what happens until the beam is found passing through the pinhole or slit (Fig.
1-34).
•
Tools settings: Start Tools, press online status and initialize x-, y- and sample wheel motors.
Before changing to the SAXS software, close Tools or press offline button otherwise communication problems can block during both programs be active.
•
Flood field and spatial correction: See HiStar detector manual, where the procedure is described in detail.
•
SAXS Software settings: Set SAXS to level 3 with Cntrl + 3 and set “Admin settings” (Fig. 1-35)
as seen in screenshot for Cu-radiation (Fig. 1-36) and for Co-radiation (Fig. 1-37).
•
We recommend to use generator settings for normal measurements of 40kV and 30mA for Cu
and 40kV and 25mA for Co tubes (= approx. 80% of max. power). During alignment procedure
max. settings can be used in order to reach the min. and max. specs of the system: 40kV and
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37mA for Cu and 40kV and 30mA for Co tubes (= 100% power). But note that max. parameters
reduce the lifetime of the tube significantly.
•
Before beginning with the alignment procedures always check whether all relevant degrees of
freedoms are stable, especially check the grub screws (1 in Fig. 1-20 and 2 in Fig. 1-21) of the
dove tails whether they are inserted with moderate force so that the crossed Göbel mirrors are
stable. Also check the fixing screws of the 4DOF (c in Fig. 1-67 and 3, 3’, 4, 5 and 6 in Fig. 164) whether they are fixed and the 4DOF is stable and also check other screws which fix the
positions of relevant units as detector, beam stop, X-ray source (Fig. 1-115), etc.
•
All alignment work concerning table, tracks etc. as shown in Fig. 1-9, Fig. 1-16, Fig. 1-17 and
Fig. 1-18 should be finished before starting the ‘alignment in detail’ which describes Göbel mirrors, pinholes, 4DOF, dove tails etc.
Quick Alignment Overview
•
Rebuilt NanoSTAR to Compact setup (short system) without vacuum windows and without
beam stop (service mode activated)
•
Set presettings and set Göbel mirrors to Bragg position
•
Align exit pinhole and 1st pinhole (divergence pinhole)
•
Set beam perpendicular to the centre of the detector
•
Move PBS back and insert primary beam path tubes (long system) without pinholes but with Xray windows, deactivate service mode and evacuate system.
•
Check again whether the beam is perpendicular at the detector’s centre and align if necessary.
•
Insert 2nd pinhole and optimize
•
Insert 3rd pinhole and optimize
•
Insert beam stop and optimize to beam
•
Insert silver behenate sample and optimize beam stop
•
Evacuate system and optimize 3rd pinhole
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Alignment in Detail
1. The presettings of degrees of freedom guarantee that the optics is near the diffraction position of
the Göbel mirrors and the beam is approx. on the system axis. Only relatively small translations
and inclinations are necessary to find the optimum settings:
•
Set NanoSTAR U system to Compact setup:
i. Move back PBS a (Fig. 1-40) back on tracks so that primary tubes d (Fig. 1-40)
can be removed.
ii. Remove primary beam path tubes a (Fig. 1-41 and Fig. 1-42)
iii. Insert two secondary beam path tubes (Fig. 1-43)
iv. Remove all X-ray windows from the PBS (Fig. 1-48), from the chamber entrance
window (Fig. 1-46) with the special tool as seen in Fig. 1-47 and Fig. 1-50 and
from the primary beam path tube system (Fig. 1-45) for later alignment.
v. Move PBS b (Fig. 1-42) along the track to the entrance flange of chamber until the
beam path control line is closed (Fig. 1-44)
vi. Remove slit between the two Göbel mirrors (Fig. 1-20)
vii. Remove exit pinhole and absorber if present (Fig. 1-21)
viii. Remove 1st pinhole as seen in Fig. 1-48
ix. Remove 3rd pinhole in the chamber (Fig. 1-49). Remove the 2nd pinhole
(NanoSTAR U system) under the lid a (in Fig. 1-51) of the primary beam path system. This is needed later but can be done now, before it is forgotten.
x. Check that beam path control line is connected completely (Fig. 1-52, Fig. 1-53,
Fig. 1-54, Fig. 1-55).
•
Presettings for Cu:
xi. Setting of screw 1 (Fig. 1-19): 2.2mm
xii. Setting of screw 2 (Fig. 1-19): 2.2mm
xiii. Setting of screw 3 (Fig. 1-19): 2.2mm
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xiv. Translation dove tail between the mirrors should be flush (p in Fig. 1-20)
xv. Setting of screw 5 (Fig. 1-22): 1.8mm
xvi. Setting of screw 6 (Fig. 1-22): 0.8mm
xvii. Setting of screw 7 (Fig. 1-22): 0.8mm
xviii. Setting of screw 9 (Fig. 1-21): +0.8mm (Fig. 1-56 shows what ‘+’ means, ‘-‘ is the
opposite direction)
xix. Setting of screw 8 (Fig. 1-21): +4.8mm (Fig. 1-56 shows what ‘+’ means, ‘-‘ is the
opposite direction)
xx. Setting a (Fig. 1-24): 32.6mm
xxi. Setting b (Fig. 1-24): 3.9mm
xxii. Setting c (Fig. 1-25): 6.3mm
xxiii. Setting d (Fig. 1-25): 4.1mm
xxiv. Setting j (Fig. 1-24): 0.3mm, mount with force in direction k. This value should be
flush but with force k the value can be between 0mm and approx. 0.35mm.
xxv. Setting y (Fig. 1-87): 2.3mm
•
Presettings for Co:
xxvi. Setting of screw 1 (Fig. 1-19): 0.68mm
xxvii. Setting of screw 2 (Fig. 1-19): 1.3mm
xxviii. Setting of screw 3 (Fig. 1-19): 1.3mm
xxix. Translation dove tail between the mirrors should be flush (Fig. 1-20)
xxx. Setting of screw 5 (Fig. 1-22): 1.6mm
xxxi. Setting of screw 6 (Fig. 1-22): 0.49mm
xxxii. Setting of screw 7 (Fig. 1-22): 0.49mm
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xxxiii. Setting of screw 9 (Fig. 1-21): -1.1mm (Fig. 1-56 shows what ‘+’ means, ‘-‘ is the
opposite direction)
xxxiv. Setting of screw 8 (Fig. 1-21): +1.65mm
xxxv. Setting a (Fig. 1-24): 32.7mm
xxxvi. Setting b (Fig. 1-24): 9.7mm
xxxvii. Setting c (Fig. 1-25): 7.8mm
xxxviii. Setting d (Fig. 1-25): 5.5mm
xxxix. Setting j (Fig. 1-24): 0.3mm, mount with force in direction k. This value should be
flush but with force k the value can be between 0mm and approx. 0.35mm.
xl. Setting y (Fig. 1-87): 2.5mm
•
Set pinhole micrometer screws to mid position (approx. 6) 10,11 in Fig. 1-23 and d,e in Fig. 127 (is needed later!)
•
Remove beam stop from centre position. This means set f,g in Fig. 1-28 in min. or max. position.
•
Remove sample holder (Fig. 1-49)
•
Remove sample translation stage from beam position
2. Set tube to 15kV and 5mA and insert 1 Cu (100µm) absorber (Cu-radiation) or 50µm Cu absorber
for Co radiation (Fig. 1-56) and 1 Ni absorber (Cu-radiation) in order to avoid Kβ-radiation (Fe for
Co radiation). Use Cu-absorber without slit aperture otherwise use a 6mm slit with Cu-absorber
plate and clamp (Fig. 1-149).
3. Switch on detector (bias on in Fig. 1-63) and check intensity of the double diffracted Göbel mirror
beam. Fig. 1-58 shows the principle of a single Göbel mirror and a crossed couple Göbel mirror
(ccGM). A ccGM optics generates 4 beams as shown in Fig. 1-57 or Fig. 1-90. One beam is the
single Bragg reflection (monochromatic radiation) from the first mirror (short mirror) as shown in c
in Fig. 1-91, another is the beam from the tube which hits the second mirror and gives a single
Bragg reflection (monochromatic radiation) from the second mirror (long one) as shown in a in Fig.
1-91. The third beam is the double diffracted beam (monochromatic radiation) from the first and
then the second mirror (d in Fig. 1-91). This is the 2D-parallel monochromatic beam which is
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needed. The fourth beam (polychromatic or ‘white’ radiation) is the direct beam which passes the
housing without being reflected (b in Fig. 1-91). Additionally Fig. 1-91 shows the shadow f of the
tube system inside the pinhole XY-alignment unit and the shadow of the Göbel mirror’s knife edge
e which separates the direct beam b from c and d from a, respectively.
•
In general reflection condition should appear with the presettings of the Göbel mirrors and 4DOF
•
Measure the count rate of d (Fig. 1-91) with a small rectangular box (F5) to avoid
white radiation counts.
•
Move box to reflection d and read “I” and optimize this value
4. If Intensity is not on optimum turn Bragg screw from 1st GM (screw 1 in Fig. 1-19)
•
Move screw in amounts of a ¼ of a complete turn (clockwise or counterclockwise)
•
Check intensity on detector (F5)
•
The reflection of the first mirror c (Fig. 1-91) should have a width of approx. 1 turn
of the Bragg screw.
5. Then check whether tilt screw from 1st GM is on optimum (screw 2 in Fig. 1-19)
•
Move screw in amounts of a ¼ of a complete turn (clockwise or counterclockwise)
•
Check intensity on detector (F5)
6. In the next step check Intensity and optimize Bragg screw from 2nd GM (5 in Fig. 1-22)
7. If Intensity is not on optimum optimize tilt screw from 2nd GM (screw 6 in Fig. 1-22)
1-52
•
Move screw in amounts of a ¼ of a complete turn (clockwise or counterclockwise)
•
The reflection should have a width of less than 1 turn of screw 5 (Fig. 1-22).
•
Check intensity of d (Fig. 1-91) on detector (F5)
•
If the double diffracted Bragg reflection is on optimum insert a 1mm slit with Cuabsorber between the two mirrors (s. Fig. 1-20) and try to improve intensity by repeating the alignment steps of the first and second mirror. The 1mm slit separates
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a and d (Fig. 1-91) from the four beams so that the greatest parts of c and b (Fig.
1-91) are removed (Fig. 1-92).
•
If necessary increase the tube kV a little bit, for example from 15kV to 20kV. If you
are not satisfied with intensity try not to exceed 20kV because of disturbing white
radiation. It is better to increase the milliamps to get more intensity.
8. If intensity is not satisfactory (remove 1mm slit) move first or/and second mirror by simultaneously
turning the screws 1, 2, 3 and 5, 6, 7, respectively (steps of approx. ¼ turn). Try to start alignment
once more and check whether the intensity has increased, otherwise move mirrors in the opposite
direction. With this procedure try to find the optimum “take off angle” relative to the surface of the
anode.
9. If optimum setting with low power (15kV to 20kV and 5mA or more) is found, insert a second Cuabsorber, increase the power to maximum (or to values which are used later for measurements)
and find again maximum intensity (don’t remove the Kβ filter) by optimizing the Bragg screws.
10. Alignment of exit pinhole at the ccGM
•
Insert a 1mm slit aperture at the position of the exit pinhole (right hand side position in Fig. 1-21)
•
Search the double diffracted Göbel mirror beam by translation the slit in ydirection (screw 9 in Fig. 1-21)
•
Exchange the slit by the 1mm pinhole
•
Search the double diffracted Göbel mirror beam by translation of the pinhole in xdirection (screw 8 in Fig. 1-21)
•
Optimize the intensity by translating the pinhole in x- and y-direction in smaller
steps. Measure intensity with F5 box in order to avoid disturbing signals.
•
(a) cannot be removed (Fig. 1-91) completely because the angle between a and d
(Fig. 1-91) is small and the distance of the exit pinhole to the Göbel mirrors is also
too small. a (Fig. 1-91) can be decreased a small amount (Fig. 1-93) by closing
the knife edge but check whether the intensity of the double diffracted beam d
(Fig. 1-91) does not suffer.
11. Alignment of 1st pinhole
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•
Insert the slit (pinhole holder with slit) into the holder of the 1st pinhole horizontally
(Fig. 1-94). Fig. 1-59 shows a set of apertures. c and d are pinholes for the 2nd
pinhole position. h is the alignment slit for the 3rd pinhole position and a for the 2nd
pinhole position. g, e and f are regular pinholes for the 1st and 3rd pinhole position.
•
Translate the slit vertically with screw 10 in Fig. 1-23 and check with the detector
until the double reflected beam passes the slit. Search maximum of intensity.
•
Turn the slit (pinhole holder with slit) vertically (Fig. 1-94).
•
Translate the slit horizontally with screw 11 in Fig. 1-23 and check with detector
until the double reflected beam passes the slit. Search maximum of intensity.
•
Insert the 750µm pinhole into the holder of the 1st pinhole. Use the tool with the
two pins similar to that as shown in Fig. 1-112, Fig. 1-113 and Fig. 1-114.
•
search maximum intensity with detector in x- and y-translation direction with screw
10 and 11 in Fig. 1-23.
12. Check whether the beam is perpendicular to the detector (short compact setup of NanoSTAR U
system)
1-54
•
Measure beam with two secondary tubes (Fig. 1-43) and find coordinates
XCntroid and YCntroid with F5 (small box)
•
Remove 2nd secondary tube b (Fig. 1-60) and move detector c (Fig. 1-61) until
safety circuit is closed again (Fig. 1-62).
•
Measure beam with one sec. tube (Fig. 1-62) and find coordinates XCntroid and
YCntroid with F5 (small box)
•
Attention: Don’t forget, during moving the detector along the track to switch off
the bias of the detector (Fig. 1-63).
•
Move Φ- (b rotation around axis b in Fig. 1-64) and ψ-rotation (a rotation around
axis a in Fig. 1-64) so that x- and y-coordinates of the beam do not differ more
than 3 pixels comparing the beam positions of one and two secondary tubes. Note
to loosen the fixing screws 4,5,6 (Fig. 1-64) for the Φ-rotation and 3 and the opposite screw (3’) for the ψ-rotation (fix it again after rotation).
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•
Operating Instructions and Alignment
In these 1-4 in Fig. 1-65 ‘a’ is the near position of the detector (one secondary
tube) and ‘b’ the far position (two secondary tubes). One line is perpendicular to
the detector (system axis) the other one shows the unaligned beam which is not
perpendicular to the detector face.
1) In this case the beam hits the detector in ‘a’-position at x1 and in ‘b’position at x2 with x1 < x2. The difference of x in ‘a’- and ‘b’-position is x2-x3
= x2-x1.
2) In this case the beam hits the detector in ‘a’-position at x1 and in ‘b’position at x2 with x1 > x2. The difference of x in ‘a’- and ‘b’-position is x2-x3
= x2-x1, the value is negative.
3) The same as 1) for y.
4) The same as 2) for y.
•
It is possible to calculate the shift which has to be done in x- and y-direction (Fig.
1-65 and Fig. 1-66 for NanoSTAR U systems and Fig. 1-99 for Compact-setup of
U systems) by Φ and ψ. Doing this leads to a reduction of the alignment steps
(one tube ↔ two tubes).
1) Shift the beam in the long distance (two tubes) setup in the following
way: Measure x1 and x2 and calculate the difference δ = x2 - x1. Take x1
and x2 in pixel and multiply with 10, this is the shift δ in mm. Then the following equation is valid: δ/400mm = (x2 - x4)/1500mm = ∆/1500mm (Fig.
1-99). ∆ is the value in mm the beam has to be shifted until it is perpendicular to the detector face in the two tubes setup: ∆ = δ * 3.75. Divide ∆
by 10 to get the result in pixel. See Fig. 1-65 and decide in which direction
the beam has to be shifted by rotation of Φ or ψ.
i. Rotate screw a (Fig. 1-95) counterclockwise in order to increase
the beam’s y coordinate in direction b (Fig. 1-95).
ii. Rotate screw a (Fig. 1-96) clockwise in order to decrease the
beam’s y coordinate in direction b (Fig. 1-96).
iii. Rotate screw c (Fig. 1-97) counterclockwise in order to increase
the beam’s x coordinate in direction d (Fig. 1-97).
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iv. Rotate screw c (Fig. 1-98) clockwise in order to decrease the
beam’s x coordinate in direction d (Fig. 1-98).
2) Shift the beam in the short distance (one tube) setup in the following way:
Measure x1 and x2 and calculate the difference δ = x2 - x1. Take x1 and x2
in pixel and multiply with 10 to get the shift δ in mm. Then the following
equation is valid: δ/400mm = (x1 - x4)/1100mm = ∆/1100mm (Fig. 1-99). ∆
is the value in mm the beam has to be shifted until it is perpendicular to
the detector face in the one tube setup: ∆ = δ ∗ 2.75. Divide ∆ by 10 to get
the result in pixel. See Fig. 1-65 and decide in which direction the beam
has to be shifted by rotation of Φ or ψ.
i. Rotate screw a (Fig. 1-95) counterclockwise in order to increase
the beam’s y coordinate in direction b (Fig. 1-95).
ii. Rotate screw a (Fig. 1-96) clockwise in order to decrease the
beam’s y coordinate in direction b (Fig. 1-96).
iii. Rotate screw c (Fig. 1-97) counterclockwise in order to increase
the beam’s x coordinate in direction d (Fig. 1-97).
iv. Rotate screw c (Fig. 1-98) clockwise in order to decrease the
beam’s x coordinate in direction d (Fig. 1-98).
•
Move x- and y-translation of 4DOF so that the beam is approx. at 512 in x and 512
in y. Do this with one secondary tube or two tubes.
•
Now the beam is approximately parallel on the system axis and it can pass the
long primary tubes which are inserted in the next steps.
13. Insert primary beam path pinhole collimation system
1-56
•
Close shutter, open door and switch off generator
•
Move the PBS system back on track
•
Check whether the X-ray window ‘a’ at the chamber is removed (s. Fig. 1-47)
•
Insert primary beam path pinhole collimation system (Fig. 1-42 → Fig. 1-41)
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•
Check that the primary beam path has an X-ray window (Fig. 1-45) at its end (at
PBS)
•
Check whether the lid c (Fig. 1-26) at the 2nd pinhole is closed (but without pinhole)
•
Move the PBS a (Fig. 1-40) to the pinhole collimation system d in order to close
the beam path line b-c completely
•
Switch on the generator again and set to 40kV 30mA (25mA f. Co)
•
Insert 2 (1) Cu absorber
14. Fine alignment of beam to the system axis (long NanoSTAR U)
•
Measure beam with two sec. tubes (Fig. 1-43) and find coordinates XCntroid and
YCntroid with F5 (small box)
•
Measure beam with one sec. tube (Fig. 1-28) and find coordinates XCntroid and
YCntroid with F5 (small box)
•
Attention: Don’t forget, to switch off the bias of the detector (Fig. 1-63) before
moving it along the track.
•
Move Φ- (b rotation around axis b in Fig. 1-64) and ψ-rotation (a rotation around
axis a in Fig. 1-64) so that x- and y-coordinates of the beam do not differ more
than +/-1 pixel comparing the beam positions of one and two secondary tubes.
Note to loosen the fixing screws 4,5,6 (Fig. 1-64) for the Φ-rotation and screw 3
and the opposite one 3’ for the ψ-rotation (fix it again after rotation).
•
In these figures 1-4 in Fig. 1-65 ‘a’ is the near position of the detector (one secondary tube) and ‘b’ the far position (two secondary tubes). One line is perpendicular
to the detector (system axis) the other one shows the unaligned beam which is not
perpendicular to the detector face.
1) In this case the beam hits the detector in ‘a’-position at x1 and in ‘b’position at x2 with x1 < x2. The difference of x in ‘a’- and ‘b’-position is x2-x3
= x2-x1.
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2) In this case the beam hits the detector in ‘a’-position at x1 and in ‘b’position at x2 with x1 > x2. The difference of x in ‘a’- and ‘b’-position is x2-x3
= x2-x1, the value is negative.
3) The same as 1) for y.
4) The same as 2) for y.
•
It is possible to calculate the shift which has to be done in x- and y-direction (Fig.
1-65 and Fig. 1-66) by Φ and ψ. Doing this leads to a reduction of the alignment
steps (one tube ↔ two tubes).
1) Shift the beam in the long distance (two tubes) setup in the following
way: Measure x1 and x2 and calculate the difference δ = x2 - x1. Take x1
and x2 in pixel and multiply with 10 to get the shift δ in mm. Then the following equation is valid: δ/400mm = (x2 - x4)/2800mm = ∆/2800mm (Fig.
1-66). ∆ is the value in mm to shift the beam until it is perpendicular to the
detector face in the two tubes setup: ∆ = δ * 7. Divide ∆ by 10 then to get
the result in pixel. See Fig. 1-65 and decide in which direction the beam
has to be shifted by rotation of Φ or ψ.
i. Rotate screw a (Fig. 1-95) counterclockwise in order to increase
the beam’s y coordinate in direction b (Fig. 1-95).
ii. Rotate screw a (Fig. 1-96) clockwise in order to decrease the
beam’s y coordinate in direction b (Fig. 1-96).
iii. Rotate screw c (Fig. 1-97) counterclockwise in order to increase
the beam’s x coordinate in direction d (Fig. 1-97).
iv. Rotate screw c (Fig. 1-98) clockwise in order to decrease the
beam’s x coordinate in direction d (Fig. 1-98).
2) Shift the beam in the short distance (one tube) setup in the following way:
Measure x1 and x2 and calculate the difference δ = x2 - x1. Take x1 and x2
in pixel and multiply with 10 to get the shift δ in mm. Then the following
equation is valid: δ/400mm = (x1 - x4)/2400mm = ∆/2400mm (Fig. 1-66). ∆
is the value in mm the beam must be shifted until it is perpendicular to the
detector face in the one tube setup: ∆ = δ ∗ 6. Divide ∆ by 10 to get the re-
1-58
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sult in pixel. See Fig. 1-65 and decide in which direction the beam must
be shifted by rotation of Φ or ψ.
i. Rotate screw a (Fig. 1-95) counterclockwise in order to increase
the beam’s y coordinate in direction b (Fig. 1-95).
ii. Rotate screw a (Fig. 1-96) clockwise in order to decrease the
beam’s y coordinate in direction b (Fig. 1-96).
iii. Rotate screw c (Fig. 1-97) counterclockwise in order to increase
the beam’s x coordinate in direction d (Fig. 1-97).
iv. Rotate screw c (Fig. 1-98) clockwise in order to decrease the
beam’s x coordinate in direction d (Fig. 1-98).
•
Move x- and y-translation of 4DOF (a and b Fig. 1-67) so that the beam is between 509 and 515 (512+/-3) in x and 509 and 515 (512+/-3) in y or better. Do not
forget to loosen the screws c (Fig. 1-67) for translation and fixing them again afterwards. Check alignment again after fixing.
•
Now the beam is parallel to the system axis and for all practical measurements in
the centre of the detector.
15. Alignment of 2nd pinhole (beam defining pinhole)
•
Open lid c (Fig. 1-26) of the 2nd pinhole
•
Insert slit unit (a in Fig. 1-59) horizontally and close pinhole chamber again (Fig. 126).
•
Move slit in y-direction (a in Fig. 1-26) and search for the beam with the detector
•
Optimize to maximum in y-direction
•
Open lid c (Fig. 1-26) of the 2nd pinhole again
•
Turn slit unit (a in Fig. 1-59) to vertical position and close pinhole chamber again
(Fig. 1-26)
•
Move slit in x-direction (b in Fig. 1-26) and search for the beam with the detector
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•
Optimize to maximum in x-direction
•
Open lid of the 2nd pinhole again
•
Remove slit unit
•
Insert 2nd pinhole c (Fig. 1-59) (450µm) and close pinhole chamber again
•
Move pinhole in x- and y-direction (a and b in Fig. 1-266) and search for the beam
with the detector
•
Search maximum in x- and y-direction
•
Increase measurement time and optimize maximum intensity
16. Alignment of 3rd pinhole
1-60
•
Open sample chamber
•
Insert slit unit in horizontal direction (a in Fig. 1-69) and close chamber
•
Move slit in y-direction (Fig. 1-70) and search for the beam with the detector
•
Optimize to maximum in y-direction (Fig. 1-70)
•
Open sample chamber again
•
Turn slit to vertical direction (b in Fig. 1-68) and close chamber again
•
Move slit in x-direction (Fig. 1-70) and search for the beam with the detector
•
Optimize to maximum in x-direction (Fig. 1-70)
•
Open sample chamber again
•
Remove slit unit
•
Insert 3rd pinhole (1000µm) (d in Fig. 1-71) and close chamber again
•
Move pinhole in x- and y-direction and search for the beam with the detector (Fig.
1-70)
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•
Search maximum in x- and y-direction (Fig. 1-70)
•
Increase measurement time and optimize maximum intensity
•
The beam in Fig. 1-72 was zoomed by a factor of 8
•
Now check the centre of the beam with F5 and determine XCntroid and YCntroid.
•
Enter Cntrl C (edit configure user settings) and enter “Direct beam X” and Yvalues from XCntroid and YCntroid, then OK as shown in Fig. 1-73.
•
Now check photon flux and analyze beam profile vertically and horizontally:
a. Under the following conditions the min. photon flux should be reached:
i. Cu systems with 3-pinhole collimation (NanoSTAR U systems)
optics: Cflux = 1.1 * 106 cps
ii. Cu systems with 2-pinhole collimation (compact-systems) optics:
Cflux = 1.2 * 105 cps
iii. Co systems with 3-pinhole collimation (NanoSTAR U systems)
optics: Cflux = 1.1 * 106 cps
iv. Co systems with 2-pinhole collimation (compact-systems) optics:
Cflux = 1.2 * 105 cps
b. For flux determination and profile analysis a vacuum of at least 1.0 * 10-1
mbar is necessary (no absorption).
c.
Generator settings (max. seetings of sealed X-ray tubes):
i. Cu: 40kV, 37mA
ii. Co: 40kV, 30mA
d. Pinholes and slits:
i. Systems with 3-pinhole collimation (NanoSTAR U systems) optics:
1. 1mm slit between the Göbel mirrors
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2. Exit pinhole 1mm
3. 1st pinhole (divergence pinhole) 750µm
4. 2nd pinhole (defining pinhole) 400µm
5. 3rd pinhole (antiscatter pinhole) 1000µm
6. 2 secondary beam path tubes
e. Use two Cu-absorber (Cu-radiation) with known absorption factor.
f.
No Kβ filter, no samples
g. Measure direct beam without beam stop at least 60s and check intensity
with F5 box with approx. 30 px * 30 px. Take counts (Total Cts), measurement time and absorption factors, calculate the flux in cps and compare with the values which are given above.
h. With the same conditions which are given above a beam profile analysis
should result in the following numbers:
i. Cu/Co systems with 3-pinhole collimation (NanoSTAR U systems)
optics:
•
•
1-62
Beam widths:
o Min. FWHMhor:
o Min. FW10%Mhor:
7 pixels
14 pixels
o
o
Min. FWHMvert:
Min. FW10%Mvert:
7 pixels
14 pixels
o
o
Max. FWHMhor:
Max. FW10%Mhor:
12 pixels
22 pixels
o
o
Max. FWHMvert:
Max. FW10%Mvert:
12 pixels
22 pixels
Beam symmetry:
o Min. FWHMhor / FWHMvert:
0.80
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o
Max. FWHMhor / FWHMvert:
1.25
o
o
Min. FW10%Mhor / FW10%Mvert:
Max. FW10%Mhor / FW10%Mvert:
0.80
1.25
17. Beam stop alignment
•
Start measurement with Cntrl Shft A as described under “Remark” at the beginning of the alignment procedure. Don’t remove the absorbers.
•
Move x- and y-translation (Fig. 1-75) until the beam disappears. x and y should be
approx. between 5 and 7 of the micrometer screw scale. Compare with Fig. 1-76
where an asymmetric beam stop is shown (note that this is a 50000s measurement!). Normally check the alignment with approx. 30 to 100s.
•
After optimizing the intensity to minimum remove the absorber(s). Now the full
beam photon flux hits the beam stop before the detector! Be sure that the beam
stop shadows the beam completely, otherwise the detector will be damaged!
Compare with Fig. 1-76 where an asymmetric beam stop is shown (note that this
is a 50000s measurement!). Normally check the alignment with approx. 30 to
100s.
•
Attention! Be sure that the intensity is low and completely shadowed by the
beam stop.
18. Insert a Silver-Behenate sample (Fig. 1-77) into diffraction position
•
Mount the Silver-Behenate sample e onto the sample frame carrier as shown in
Fig. 1-71 (example). Close the shutter press “door open” button (Fig. 1-74), open
the door of the sample chamber and mount the sample into the sample chamber
•
Move y- and x- motor until the sample powder is in the beam. Enter Ctrl Shft D to
enter the x- and y-value.
•
Start a measurement. The diffraction pattern should look similar to the screen shot
in Fig. 1-78. A more or less symmetrical corona around the beam stop shadow
should be seen with one or more rings around it.
19. Beam stop fine alignment
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•
With full flux, there should be a asymmetric or symmetric intensity ring around the
beam stop shadow (corona scattering from silver behenate). Fig. 1-78 shows a
symmetric corona.
•
Take a measurement of at least 120 sec or more.
•
Analyse the measurement and press Cntrl V to start settings of “graph vector”
•
Check horizontally whether the corona is symmetrical (Fig. 1-79)
•
If both “peaks” (Fig. 1-80) have not the same peak height, move the beam stop in
x direction a small amount and repeat this measurement until both peaks have the
same height. If necessary then increase the measurement time.
•
Analyse the same measurement in vertical direction and press Cntrl V to start settings of “graph vector”.
•
Check vertically whether the corona is symmetrical
•
If both “peaks” have not the same peak height, move the beam stop a small
amount in y direction and repeat this measurement until both peaks have same
height. If necessary then increase the measurement time.
•
If the intensity of the silver behenate pattern rings is high enough (measurement
time approx. 600s - 1000s) then calibrate the sample to detector distance (Fig. 182)
•
Chose process → calibrate
•
Enter calibration filename, sample to detector distance (first guess 105cm), detector x and y-centre as determined before (Fig. 1-83).
•
Move theoretical rings to measured ones and start evaluation with left mouse button.
•
The result is the real sample to detector distance.
•
Enter this value into the “admin settings” menue (Fig. 1-37)
20. Background and parasitic scattering reduction and analysis
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•
Remove the silver behenate sample so that the beam can pass the complete path
to the beam stop
•
Be sure that all absorbers are removed and there is a good vacuum value (typ.
1.5 x 10-2 mbar but not more than 2.5 x 10-2 mbar) in order to reduce the scattering on air molecules (O2 and N2).
•
Start a “blank”-measurement with at least 10000 sec. measurement time and
check background.
•
Two things are important:
a. If there are “streaks” beginning at the shadow of the beam stop (b in Fig.
1-85) realign the 3rd pinhole in very small amounts of 3-5µm (approx. ½
unit or less) vertically or horizontally (Fig. 1-32 and Fig. 1-33). In general
the beam stop is aligned good enough with the silver behenate corona, so
the last alignment step is a very fine alignment of the 3rd pinhole. The origin of these streaks are the edge scattering of the 3rd pinhole as shown in
Fig. 1-33.
b. Sometimes if the “corona” of the beam stop is asymmetric align the beam
stop in amounts of approx. 10-30µm. d in Fig. 1-84 shows a symmetric
corona. Sometimes a streak can be so broad that it seems to be an asymmetric shadow of the beam stop. In general try to optimize the 3rd pinhole
first. A “good” blank measurement should look similar to Fig. 1-84.
•
The homogeneous background is all what there is around the beam stop (c in Fig.
1-84). It should be homogeneous and the overall intensity should not exceed a
certain level.
•
Fig. 1-88 shows a streak (e) after 1000 sec. measurement time.
•
Fig. 1-86 is a better alignment as shown in Fig. 1-85. Both, the beam stop and the
3rd pinhole have been moved slightly, but the alignment of the 3rd pinhole is not yet
perfect (note this is a 60000s measurement!).
•
Fig. 1-89 shows a “perfectly” aligned system after a long alignment procedure
(several measurements with more than 40000s) and very small alignment steps of
the 3rd pinhole (approx. 2µm or 1/5 of one unit or less). After some training one
can get nearly perfect results in faster times.
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•
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Under the following conditions reach at least the following numbers for
NanoSTAR U systems concerning the background:
a. Detector dark noise: D = max. 10cps (for Cu/Co/)
i. No samples, no filters, no absorbers
ii. Aligned system, measurement at least 600 sec.
iii. Measurement with closed shutter (Fig. 1-100). Don’t mark ‘open &
close shutter’ as shown in Fig. 1-34.
iv. Set kV and mA to min. values
v. Determine counts integral over the complete detector area
(‘counts’) and calculate cps per 1024 px * 1024 px. Calculate also
Dbox = D / 105, this is the detector’s dark noise in a 100 px * 100
px box. This value is important because it is needed later for
background analysis.
b. Homogeneous background: H = max. 0.5 cps per 100 px * 100 px (Cu/Co
for NanoSTAR U systems)
i. Same conditions as under flux and profile analysis with no filters,
no absorbers, no samples and aligned beam stop.
ii. Set kV and mA to max. values
iii. Measurement time at least 10000 sec.
iv. Vacuum must be better than 2.5 * 10-2 mbar
v. Measure background counts in a 100 px * 100 px box (F5) at 8
positions, determine the arithmetical median (example see Fig. 1101) and divide by measurement time.
c.
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Parasitic scattering background: P = max. 0.8 cps per 100 px * 100 px
(Cu/Co for NanoSTAR U systems). Measure with F5 as shown in Fig. 1102.
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i. Conditions identical to measurement of homogeneous background. Evaluate the same frame as for homogeneous background.
d. Calculate Peff = max. 0.5 cps per 100 px * 100 px
i. Peff = (P – H) / (Cflux / 1.6 * 106 cps) - Dbox
ii. Values Cflux and Dbox as determined above.
21. After all alignment steps are finished and one is satisfied with the performance of the system, note
all parameters for the future:
c.
First Göbel mirror:
i. Bragg screw 1 in Fig. 1-19 (1st 40mm mirror) :.........................................................
ii. Tilt screw 2 in Fig. 1-19 (1st 40mm mirror):...............................................................
iii. Third screw 3 in Fig. 1-19 (1st 40mm mirror): ...........................................................
iv. Knife edge screw 4 in Fig. 1-19 (1st 40mm mirror): ...................................................
d. Second Göbel mirror:
i. Bragg screw 5 in Fig. 1-22 (2nd 60mm mirror) : .........................................................
ii. Tilt screw 6 in Fig. 1-22 (2nd 60mm mirror): ...............................................................
iii. Third screw 7 in Fig. 1-22 (2nd 60mm mirror): ...........................................................
e. Dove tail p in Fig. 1-20 between the mirrors :.........................................................................
f.
Hor. dove tail 8 in Fig. 1-21:....................................................................................................
g. Vert. dove tail 9 in Fig. 1-21:...................................................................................................
h. 1st pinhole:
i. micrometer head screw 11 in Fig. 1-23: ....................................................................
ii. micrometer head screw 10 in Fig. 1-23: ....................................................................
i.
4DOF-Parameters for x-, y-translation, Φ-, ψ-rotation
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i. Parameter a in Fig. 1-24: ..........................................................................................
ii. Parameter b in Fig. 1-24: ..........................................................................................
iii. Parameter c in Fig. 1-25: ..........................................................................................
iv. Parameter d in Fig. 1-25: ..........................................................................................
j.
2nd pinhole:
i. micrometer head screw a in Fig. 1-26: .....................................................................
ii. micrometer head screw b in Fig. 1-26: .....................................................................
k.
rd
3 pinhole:
i. micrometer head screw d in Fig. 1-27: .....................................................................
ii. micrometer head screw e in Fig. 1-27: .....................................................................
l.
Beam stop:
i. micrometer head screw g in Fig. 1-28: .....................................................................
ii. micrometer head screw f in Fig. 1-28: ......................................................................
m. Detector bias setting: .............................................................................................................
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Alignment Overview NanoSTAR C SAXS System
NanoSTAR C, Long Version, One Tube or …? What’s That ?
Fig. 1-4 shows a NanoSTAR C system. This system has a short primary beam path with a 2-pinhole
collimation system and a fine focus sealed tube as described before. Additionally here is one secondary beam path tube, but the system with two secondary tubes is the standard Compact system. All is
mounted on a stable granite and steel table top with only one D8-base (r).
The parallel beam source (PBS) is shown in Fig. 1-6. The PBS is the source, with Göbel mirrors, exit
pinhole and the 1st pinhole and 4DOF. A parallel monochromatic beam comes out from this system
unit.
The parallel beam source (PBS) system with sealed tube (ST) is shown in Fig. 1-6. The PBS is the
source (sealed tube) (w), with Göbel mirrors (x), exit pinhole and the 1st pinhole (y) and the 4DOF (z).
A parallel monochromatic beam comes out from such a system.
Fig. 1-7 shows the chamber where an X-ray window (a) on the primary side and a cone with X-ray
window (b) on the secondary side can be mounted in order to let the chamber under air during evacuating the secondary and the primary beam path tubes.
Fig. 1-8 shows the detector with mount (c) and beam stop (d). The beam stop unit (d) can be aligned
with two perpendicular micrometer translation units (e,f). (g) is the beam path control line plug.
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Which Components of the NanoSTAR C Systems Have to be
Aligned?
1. Table top with main track system
The granite plate (Fig. 1-4) is one single plate and is mounted between the main track system and the
steel table top.
2. Parallel beam source system (PBS) with slit, exit pinhole and 1st pinhole:
• X-ray source (sealed tube l in Fig. 1-10)
•
Göbel mirrors GM
•
Slit and pinholes
•
4DOF
3. Sample chamber with 2nd pinhole
The 2nd pinhole is a part of the sample chamber as shown in Fig. 1-13 and Fig. 1-14. It is inside the
chamber but can be aligned from the outer micrometer screws (u) and (v). Here the X-ray window (w)
is mounted when the system shell be used in the sample under air operation mode. In this mode the
cone (x) must also be mounted as shown in Fig. 1-14.
4. Secondary beam path tube with beam stop
The beam stop is fixed with 2 strings (y,z) as shows in Fig. 1-15. The small beam stop unit (a) can be
moved via the strings by two micrometer screws (b,c).
What Degrees of Freedom are Available for Alignment
1. NanoSTAR base
• Table top height alignment must be done by 4 screws (d) as shown in Fig. 1-16. The D8-base
has 4 screws in its corners under the steel plate.
•
Track system line alignment (similar to Fig. 1-17 of U system). The distance of the two parallel
tracks can be aligned by the PBS on the primary side or the detector track mount on the secondary side similar as shown in Fig. 1-18 for U sytems.
2. Göbel mirror alignment:
• Bragg screw of the first mirror (1 in Fig. 1-19).
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•
•
Tilt screw of the first mirror (2 in Fig. 1-19).
3rd screw of the first mirror (3 in Fig. 1-19).
•
•
•
Bragg screw of the second mirror (5 in Fig. 1-22).
Tilt screw of the second mirror (6 in Fig. 1-22).
3rd screw of the second mirror (7 in Fig. 1-22).
•
Knife edge screw at the entrance of the first mirror (4 in Fig. 1-19).
•
z and y translation screws of the pinhole at the exit of the second mirror (8 and 9 in Fig. 1-21).
•
z and y translation micrometer head screws (10 and 11 in Fig. 1-23) of the 1st pinhole (divergence pinhole).
3. 4DOF alignment:
• x-translation (Fig. 1-24) of the primary beam.
•
y-translation (Fig. 1-24) of the primary beam.
•
Φ-rotation (vertical rotation axis) of the primary beam (Fig. 1-25).
•
ψ-rotation (horizontal rotation axis) of the primary beam (Fig. 1-25).
4. 2nd pinhole alignment:
• x (similar to e in Fig. 1-27 for U systems) and y (similar to d in Fig. 1-27 for U systems) translation micrometer head screws of the 2nd pinhole (antiscatter pinhole). This pinhole is inside the
sample chamber.
5. Beam stop alignment:
• x (f in Fig. 1-28) and y (g in Fig. 1-28) translation micrometer head screws of the beam stop.
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What will be the Result After the Alignment Procedures?
1. Göbel mirror with slit and exit pinhole alignment results in a 2-dimensional parallel monochromatic
primary beam (with Kβ but relatively clean of white radiation). The reason of Kβ is the large source
focus as shown in Fig. 1-29. Additionally there is a small amount of non monochromatic radiation
which comes from the white spectrum. The knife edge cuts away the most part of the direct white
beam. The slit between both mirrors selects the single diffracted beam from the first mirror (depends on setting of the knife edge). The exit pinhole (200µm at C-Systems) selects the double diffracted Göbel mirror Bragg peak from the rest (depends on setting of knife edge). The 2-pinhole
collimation system along the beam path makes a spatial separation of the monochromatic Kα radiation from the rest, especially the Kβ can totally be removed.
2. 4DOF: Primary beam is perpendicular to the detector plane and hits its centre, i.e. the primary
beam path is on the physical system axis.
3. 2nd pinholes: They have to be also on the physical system axis. The 1st and 2nd pinhole define the
maximum divergence which is accepted by the pinhole collimation system. It is optimized to the
natural or intrinsic divergence of the optical mirror system (Bragg reflections on limited multilayer
systems). Fig. 1-31 shows the 2-pinhole collimation system. Here P0 is the exit pinhole of the
Göbel mirror which removes most of unwanted signals. The 2nd pinhole of the 2-pinhole collimation system cuts away the edge scattering from the 1st pinhole and reduces the background on
the detector.
4. Beam stop: The direct beam is completely shadowed with a minimum of background noise.
Which Alignment Steps Have to be Done?
1. Table top and track alignment:
• Check that the granite plate is in plane with a water level in all directions. If not, check alignment of 4 screws (height alignment) as seen in Fig. 1-16.
• Check that the tracks are in line similar to Fig. 1-17 for U systems.
• Check on left hand side (primary) with PBS that the tracks have the correct distance. Check on
right hand side (secondary) with detector that the tracks have also the correct distance.
2. Presettings:
• 4DOF:
xli. x- and y-translation
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xlii. Φ-, ψ-rotation
•
Crossed Coupled GM ccGM:
xliii. Tilt and Bragg angle of 1st and 2nd GM,
xliv. knife edge,
xlv. exit pinhole
•
•
•
1st and 2nd Pinhole
Sample Stages
Beam stop
3. Alignment of the Göbel mirror:
• Optimize 1st mirror in Kα Bragg position
• Optimize 2nd mirror in Kα Bragg position
• Optimize knife edge, tube height, relative position of the GMs
• Set exit pinhole to double diffracted Bragg peak
• Set 1st pinhole to beam
4. 4DOF:
• Set Φ-, ψ-rotation so that the beam does not move on the detector when the detector sample
distance is changed, i.e. that the beam is perpendicular to the detector face.
• Set x- and y-translation so that the beam is in the centre of the detector area.
5. Pinholes:
• Set 2nd pinhole to maximum intensity
6. Beam stop:
• Set Beam stop to minimum intensity
• Check position of 2nd pinhole and reduce scattering to minimum signal.
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SAXS Operation Modes
In this section all possible measurement modes are described. As the NanoSTAR is very flexible a
wide variety of modes is possible. On the one hand the primary beam path and hence the beam properties can be changed. On the other hand the secondary beam path and hence the diffraction angle
range is variable. Further there is the possibility to measure the sample under vacuum and also under
air pressure if it is a critical sample (burst in vacuum). In some cases it is possible to measure the
sample under He or other gases.
1. Measurements with samples under vacuum
1. Compact system (scanning SAXS applications)
i. High resolution (extended SAXS, 1070mm)
ii. Short beam path (670mm)
iii. Very short beam path (WAXS, 270mm)
iv. Very short beam path and WAXS extender (WAXS, 60mm or less)
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Alignment Details NanoSTAR C SAXS System
Some Remarks
•
It is time consuming to get a beam through a pinhole or a slit proceeding step by step like
i. Turn pinhole translation a small amount
ii. Start measurement und read intensity
iii. If intensity is not satisfactory goto i)
•
The beam can be found quickly, if the measurement parameters are configured as follows:
Press Cntrl Shft A to start options for collect add. “Pre-clear” means that after each “Reset interval”
of 1 sec. the image is cleared and the measurement is displayed in realtime for 5000 measurements. This is similar to a “ratemeter” where knobs and screws can be turned by directly observing
what happens until the beam is found passing through the pinhole or slit (Fig. 1-34).
•
Tools settings: Start Tools, press online status and initialize x-, y- and sample wheel motors.
Before changing to the SAXS software, close Tools or press offline button otherwise communication problems can block during both programs be active.
•
Flood field and spatial correction: See HiStar detector manual, where the procedure is described in detail.
•
SAXS Software settings: Set SAXS to level 3 with Cntrl + 3 and set “Admin settings” (Fig. 1-35)
as seen in screenshot for Cu-radiation (Fig. 1-36) and for Co-radiation (Fig. 1-37).
•
We recommend to use generator settings for normal measurements of 40kV and 30mA for Cu
and 40kV and 25mA for Co tubes (= approx. 80% of max. power). During alignment procedure
max. settings can be used in order to reach the min. and max. specs of the system: 40kV and
37mA for Cu and 40kV and 30mA for Co tubes (= 100% power). But note that max. parameters
reduce the lifetime of the tube significantly.
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•
Before beginning with the alignment procedures always check whether all relevant degrees of
freedoms are stable, especially check the grub screws (1 in Fig. 1-20 and 2 in Fig. 1-21) of the
dove tails whether they are inserted with moderate force so that the crossed Göbel mirrors are
stable. Also check the fixing screws of the 4DOF (c in Fig. 1-67 and 3, 3’, 4, 5 and 6 in Fig. 164) whether they are fixed and the 4DOF is stable and also check other screws which fix the
positions of relevant units as detector, beam stop, X-ray source (Fig. 1-115), etc.
•
All alignment work concerning table, tracks etc. similar to as shown in Fig. 1-9, Fig. 1-16, Fig.
1-17 and Fig. 1-18 for U systems should be finished before starting the ‘alignment in detail’
which describes Göbel mirrors, pinholes, 4DOF, dove tails etc.
Quick Alignment Qverview
•
Set NanoSTAR C system without vacuum windows and without beam stop (service mode activated)
•
Set presettings and set Göbel mirrors to Bragg position
•
Align exit pinhole and 1st pinhole (divergence pinhole)
•
Set beam perpendicular to the centre of the detector
•
Insert 2nd pinhole and optimize
•
Insert beam stop and optimize to beam
•
Insert silver behenate sample and optimize beam stop
•
Evacuate system and optimize 2nd pinhole
Alignment in Detail
1. The presettings of degrees of freedom guarantee that the optics is near the diffraction position of
the Göbel mirrors and the beam is approx. on the system axis. Only relatively small translations
and inclinations are necessary to find the optimum settings:
•
1-76
Set NanoSTAR C system:
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i. Insert two secondary beam path tubes (Fig. 1-60)
ii. Remove all X-ray windows from the PBS (Fig. 1-46), from the chamber entrance
window (Fig. 1-46) with the special tool as seen in Fig. 1-47 and Fig. 1-50.
iii. Remove 1st pinhole as seen in Fig. 1-48
iv. Move PBS b (Fig. 1-42) along the track to the entrance flange of chamber until the
beam path control line is closed (Fig. 1-44)
v. Remove slit between the two Göbel mirrors (Fig. 1-20)
vi. Remove exit pinhole and absorber if present (Fig. 1-21)
vii. Remove 2nd pinhole in the chamber (Fig. 1-49).
viii. Check that beam path control line is connected completely (Fig. 1-52, Fig. 1-53,
Fig. 1-54, Fig. 1-55).
•
Presettings for Cu:
i. Setting of screw 1 (Fig. 1-19): 2.2mm
ii. Setting of screw 2 (Fig. 1-19): 2.2mm
iii. Setting of screw 3 (Fig. 1-19): 2.2mm
iv. Translation dove tail between the mirrors should be flush (p in Fig. 1-20)
v. Setting of screw 5 (Fig. 1-22): 1.8mm
vi. Setting of screw 6 (Fig. 1-22): 0.8mm
vii. Setting of screw 7 (Fig. 1-22): 0.8mm
viii. Setting of screw 9 (Fig. 1-21): +0.8mm (Fig. 1-56 shows what ‘+’ means, ‘-‘ is the
opposite direction)
ix. Setting of screw 8 (Fig. 1-21): +4.8mm (Fig. 1-56 shows what ‘+’ means, ‘-‘ is the
opposite direction)
x. Setting a (Fig. 1-24): 32.6mm
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xi. Setting b (Fig. 1-24): 3.9mm
xii. Setting c (Fig. 1-25): 6.3mm
xiii. Setting d (Fig. 1-25): 4.1mm
xiv. Setting j (Fig. 1-24): 0.3mm, mount with force in direction k. This value should be
flush but with force k the value can be between 0mm and approx. 0.35mm.
xv. Setting y (Fig. 1-87): 2.3mm
•
Presettings for Co:
i. Setting of screw 1 (Fig. 1-19): 0.68mm
ii. Setting of screw 2 (Fig. 1-19): 1.3mm
iii. Setting of screw 3 (Fig. 1-19): 1.3mm
iv. Translation dove tail between the mirrors should be flush (Fig. 1-20)
v. Setting of screw 5 (Fig. 1-22): 1.6mm
vi. Setting of screw 6 (Fig. 1-22): 0.49mm
vii. Setting of screw 7 (Fig. 1-22): 0.49mm
viii. Setting of screw 9 (Fig. 1-21): -1.1mm (Fig. 1-56 shows what ‘+’ means, ‘-‘ is the
opposite direction)
ix. Setting of screw 8 (Fig. 1-21): +1.65mm
x. Setting a (Fig. 1-24): 32.7mm
xi. Setting b (Fig. 1-24): 9.7mm
xii. Setting c (Fig. 1-25): 7.8mm
xiii. Setting d (Fig. 1-25): 5.5mm
xiv. Setting j (Fig. 1-24): 0.3mm, mount with force in direction k. This value should be
flush but with force k the value can be between 0mm and approx. 0.35mm.
xv. Setting y (Fig. 1-87): 2.5mm
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•
Set pinhole micrometer screws to mid position (approx. 6) 10,11 in Fig. 1-23 and d,e in
Fig. 1-27 (is needed later!)
•
Remove beam stop from centre position. This means set f,g in Fig. 1-28 in min. or max.
position.
•
Remove sample holder (Fig. 1-49)
•
Remove sample translation stage from beam position
1. Set tube to 15kV and 5mA and insert 1 Cu (100µm) absorber (Cu-radiation) or 50µm Cu absorber
for Co radiation (Fig. 1-56) and 1 Ni absorber (Cu-radiation) in order to avoid Kβ-radiation (Fe for
Co radiation). Use Cu-absorber without slit aperture otherwise use a 6mm slit with Cu-absorber
plate and clamp (Fig. 1-149).
2. Switch on detector (bias on in Fig. 1-63) and check intensity of the double diffracted Göbel mirror
beam. Fig. 1-58 shows the principle of a single Göbel mirror and a crossed couple Göbel mirror
(ccGM). A ccGM optics generates 4 beams as shown in Fig. 1-57 or Fig. 1-90. One beam is the
single Bragg reflection (monochromatic radiation) from the first mirror (short mirror) as shown in c
in Fig. 1-91, another is the beam from the tube which hits the second mirror and gives a single
Bragg reflection (monochromatic radiation) from the second mirror (long one) as shown in a in Fig.
1-91. The third beam is the double diffracted beam (monochromatic radiation) from the first and
then the second mirror (d in Fig. 1-91). This is the 2D-parallel monochromatic beam which is
needed. The fourth beam (polychromatic or ‘white’ radiation) is the direct beam which passes the
housing without being reflected (b in Fig. 1-91). Additionally Fig. 1-91 shows the shadow f of the
tube system inside the pinhole XY-alignment unit and the shadow of the Göbel mirror’s knife edge
e which separates the direct beam b from c and d from a, respectively.
•
In general reflection condition should appear with the presettings of the Göbel mirrors and 4DOF
•
Measure the count rate of d (Fig. 1-91) with a small rectangular box (F5) to avoid
white radiation counts.
•
Move box to reflection d and read “I” and optimize this value
3. If Intensity is not on optimum turn Bragg screw from 1st GM (screw 1 in Fig. 1-19)
•
Move screw in amounts of a ¼ of a complete turn (clockwise or counterclockwise)
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•
Check intensity on detector (F5)
•
The reflection of the first mirror c (Fig. 1-91) should have a width of approx. 1 turn
of the Bragg screw.
4. Then check whether tilt screw from 1st GM is on optimum (screw 2 in Fig. 1-19)
•
Move screw in amounts of a ¼ of a complete turn (clockwise or counterclockwise)
•
Check intensity on detector (F5)
5. In the next step check Intensity and optimize Bragg screw from 2nd GM (5 in Fig. 1-22)
6. If Intensity is not on optimum optimize tilt screw from 2nd GM (screw 6 in Fig. 1-22)
•
Move screw in amounts of a ¼ of a complete turn (clockwise or counterclockwise)
•
The reflection should have a width of less than 1 turn of screw 5 (Fig. 1-22).
•
Check intensity of d (Fig. 1-91) on detector (F5)
•
If the double diffracted Bragg reflection is on optimum insert a 1mm slit with Cuabsorber between the two mirrors (s. Fig. 1-20) and try to improve intensity by repeating the alignment steps of the first and second mirror. The 1mm slit separates
a and d (Fig. 1-91) from the four beams so that the greatest parts of c and b (Fig.
1-91) are removed (Fig. 1-92).
•
If necessary increase the tube kV a little bit, for example from 15kV to 20kV. If you
are not satisfied with intensity try not to exceed 20kV because of disturbing white
radiation. It is better to increase the milliamps to get more intensity.
7. If intensity is not satisfactory (remove 1mm slit) move first or/and second mirror by simultaneously
turning the screws 1, 2, 3 and 5, 6, 7, respectively (steps of approx. ¼ turn). Try to start alignment
once more and check whether the intensity has increased, otherwise move mirrors in the opposite
direction. With this procedure try to find the optimum “take off angle” relative to the surface of the
anode.
8. If optimum setting with low power (15kV to 20kV and 5mA or more) is found, insert a second Cuabsorber, increase the power to maximum (or to values which are used later for measurements)
and find again maximum intensity (don’t remove the Kβ filter) by optimizing the Bragg screws.
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9. Alignment of exit pinhole at the ccGM
•
Insert a 1mm slit aperture at the position of the exit pinhole (right hand side position in Fig. 1-21)
•
Search the double diffracted Göbel mirror beam by translation the slit in ydirection (screw 9 in Fig. 1-21)
•
Exchange the slit by the 1mm pinhole
•
Search the double diffracted Göbel mirror beam by translation of the pinhole in xdirection (screw 8 in Fig. 1-21)
•
Optimize the intensity by translating the pinhole in x- and y-direction in smaller
steps. Measure intensity with F5 box in order to avoid disturbing signals.
•
(a) cannot be removed (Fig. 1-91) completely because the angle between a and d
(Fig. 1-91) is small and the distance of the exit pinhole to the Göbel mirrors is also
too small. a (Fig. 1-91) can be decreased a small amount (Fig. 1-93) by closing
the knife edge but check whether the intensity of the double diffracted beam d
(Fig. 1-91) does not suffer.
10. Alignment of 1st pinhole
•
Insert the slit (pinhole holder with slit) into the holder of the 1st pinhole horizontally
(Fig. 1-94). Fig. 1-59 shows a set of apertures. h is the alignment slit for the 2nd
pinhole position and g, e and f are regular pinholes for the 1st and 2nd pinhole position.
•
Translate the slit vertically with screw 10 in Fig. 1-23 and check with the detector
until the double reflected beam passes the slit. Search maximum of intensity.
•
Turn the slit (pinhole holder with slit) vertically (Fig. 1-94).
•
Translate the slit horizontally with screw 11 in Fig. 1-23 and check with detector
until the double reflected beam passes the slit. Search maximum of intensity.
•
Insert the 100µm pinhole into the holder of the 1st pinhole. Use the tool with the
two pins similar to that as shown in Fig. 1-112, Fig. 1-113 and Fig. 1-114.
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•
NanoSTAR SAXS System User's Manual Vol. 2
search maximum intensity with detector in x- and y-translation direction with screw
10 and 11 in Fig. 1-23.
11. Check whether the beam is perpendicular to the detector
•
Measure beam with two secondary tubes (Fig. 1-43) and find coordinates
XCntroid and YCntroid with F5 (small box)
•
Remove 2nd secondary tube b (Fig. 1-60) and move detector c (Fig. 1-61) until
safety circuit is closed again (Fig. 1-62).
•
Measure beam with one sec. tube (Fig. 1-62) and find coordinates XCntroid and
YCntroid with F5 (small box)
•
Attention: Don’t forget, during moving the detector along the track to switch off
the bias of the detector (Fig. 1-63).
•
Move Φ- (b rotation around axis b in Fig. 1-64) and ψ-rotation (a rotation around
axis a in Fig. 1-64) so that x- and y-coordinates of the beam do not differ more
than +/-1 pixel comparing the beam positions of one and two secondary tubes.
Note to loosen the fixing screws 4,5,6 (Fig. 1-64) for the Φ-rotation and 3 and the
opposite screw (3’) for the ψ-rotation (fix it again after rotation).
•
In these figures 1-4 in Fig. 1-65 ‘a’ is the near position of the detector (one secondary tube) and ‘b’ the far position (two secondary tubes). One line is perpendicular
to the detector (system axis) the other one shows the unaligned beam which is not
perpendicular to the detector face.
1) In this case the beam hits the detector in ‘a’-position at x1 and in ‘b’position at x2 with x1 < x2. The difference of x in ‘a’- and ‘b’-position is x2-x3
= x2-x1.
2) In this case the beam hits the detector in ‘a’-position at x1 and in ‘b’position at x2 with x1 > x2. The difference of x in ‘a’- and ‘b’-position is x2-x3
= x2-x1, the value is negative.
3) The same as 1) for y.
4) The same as 2) for y.
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•
Operating Instructions and Alignment
It is possible to calculate the shift which has to be done in x- and y-direction (Fig.
1-65 and Fig. 1-99 for NanoSTAR C systems) by Φ and ψ. Doing this leads to a
reduction of the alignment steps (one tube ↔ two tubes).
1) Shift the beam in the long distance (two tubes) setup in the following
way: Measure x1 and x2 and calculate the difference δ = x2 - x1. Take x1
and x2 in pixel and multiply with 10, this is the shift δ in mm. Then the following equation is valid: δ/400mm = (x2 - x4)/1500mm = ∆/1500mm (Fig.
1-99). ∆ is the value in mm the beam has to be shifted until it is perpendicular to the detector face in the two tubes setup: ∆ = δ * 3.75. Divide ∆
by 10 to get the result in pixel. See Fig. 1-65 and decide in which direction
the beam has to be shifted by rotation of Φ or ψ.
i. Rotate screw a (Fig. 1-95) counterclockwise in order to increase
the beam’s y coordinate in direction b (Fig. 1-95).
ii. Rotate screw a (Fig. 1-96) clockwise in order to decrease the
beam’s y coordinate in direction b (Fig. 1-96).
iii. Rotate screw c (Fig. 1-97) counterclockwise in order to increase
the beam’s x coordinate in direction d (Fig. 1-97).
iv. Rotate screw c (Fig. 1-98) clockwise in order to decrease the
beam’s x coordinate in direction d (Fig. 1-98).
2) Shift the beam in the short distance (one tube) setup in the following way:
Measure x1 and x2 and calculate the difference δ = x2 - x1. Take x1 and x2
in pixel and multiply with 10 to get the shift δ in mm. Then the following
equation is valid: δ/400mm = (x1 - x4)/1100mm = ∆/1100mm (Fig. 1-99). ∆
is the value in mm the beam has to be shifted until it is perpendicular to
the detector face in the one tube setup: ∆ = δ ∗ 2.75. Divide ∆ by 10 to get
the result in pixel. See Fig. 1-65 and decide in which direction the beam
has to be shifted by rotation of Φ or ψ.
i. Rotate screw a (Fig. 1-95) counterclockwise in order to increase
the beam’s y coordinate in direction b (Fig. 1-95).
ii. Rotate screw a (Fig. 1-96) clockwise in order to decrease the
beam’s y coordinate in direction b (Fig. 1-96).
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iii. Rotate screw c (Fig. 1-97) counterclockwise in order to increase
the beam’s x coordinate in direction d (Fig. 1-97).
iv. Rotate screw c (Fig. 1-98) clockwise in order to decrease the
beam’s x coordinate in direction d (Fig. 1-98).
•
Move x- and y-translation of 4DOF so that the beam is at 512 +/-3 in x and 512 +/3 in y. Do this with one secondary tube or two tubes.
12. Alignment of 2nd pinhole
1-84
•
Open sample chamber
•
Insert slit unit in horizontal direction (a in Fig. 1-69) and close chamber
•
Move slit in y-direction (Fig. 1-70) and search for the beam with the detector
•
Optimize to maximum in y-direction (Fig. 1-70)
•
Open sample chamber again
•
Turn slit to vertical direction (b in Fig. 1-68) and close chamber again
•
Move slit in x-direction (Fig. 1-70) and search for the beam with the detector
•
Optimize to maximum in x-direction (Fig. 1-70)
•
Open sample chamber again
•
Remove slit unit
•
Insert 2nd pinhole (300µm) (d in Fig. 1-71) and close chamber again
•
Move pinhole in x- and y-direction and search for the beam with the detector (Fig.
1-70)
•
Search maximum in x- and y-direction (Fig. 1-70)
•
Increase measurement time and optimize maximum intensity
•
The beam in Fig. 1-72 was zoomed by a factor of 8
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•
Now check the centre of the beam with F5 and determine XCntroid and YCntroid.
•
Enter Cntrl C (edit configure user settings) and enter “Direct beam X” and Yvalues from XCntroid and YCntroid, then OK as shown in Fig. 1-73.
•
Now check photon flux and analyze beam profile vertically and horizontally:
a. Under the following conditions the min. photon flux should be reached:
i. Cu systems with 2-pinhole collimation (C-systems) optics: Cflux =
1.2 * 105 cps
ii. Co systems with 2-pinhole collimation (C-systems) optics: Cflux =
1.2 * 105 cps
b. For flux determination and profile analysis a vacuum of at least 1.0 * 10-1
mbar is necessary (no absorption).
c.
Generator settings (max. seetings of sealed X-ray tubes):
i. Cu: 40kV, 37mA
ii. Co: 40kV, 30mA
d. Pinholes and slits:
i. Systems with 2-pinhole collimation (compact-systems) optics:
1. 1mm slit between the Göbel mirrors
2. Exit pinhole 200µm
3. 1st pinhole (defining pinhole) 100µm
4. 2nd pinhole (antiscatter pinhole) 300µm
5. 2 secondary beam path tubes
e. Use one Cu-absorber (Cu-radiation) with known absorption factor.
f.
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g. Measure direct beam without beam stop at least 60s and check intensity
with F5 box with approx. 30 px * 30 px. Take counts (Total Cts), measurement time and absorption factors, calculate the flux in cps and compare with the values which are given above.
h. With the same conditions which are given above a beam profile analysis
should result in the following numbers:
i. Cu/Co systems with 2-pinhole collimation (C-systems) optics:
•
•
Beam widths:
o
o
Min. FWHMhor:
Min. FW10%Mhor:
6 pixels
11 pixels
o
o
Min. FWHMvert:
Min. FW10%Mvert:
6 pixels
11 pixels
o
o
Max. FWHMhor:
Max. FW10%Mhor:
10 pixels
18 pixels
o
o
Max. FWHMvert:
Max. FW10%Mvert:
10 pixels
18 pixels
Beam symmetry:
o
o
Min. FWHMhor / FWHMvert:
Max. FWHMhor / FWHMvert:
0.80
1.25
o
o
Min. FW10%Mhor / FW10%Mvert:
Max. FW10%Mhor / FW10%Mvert:
0.80
1.25
13. Beam stop alignment
•
1-86
Start measurement with Cntrl Shft A as described under “Remark” at the beginning of the alignment procedure. Don’t remove the absorbers.
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•
Move x- and y-translation (Fig. 1-75) until the beam disappears. x and y should be
approx. between 5 and 7 of the micrometer screw scale. Compare with Fig. 1-76
where an asymmetric beam stop is shown.
•
After optimizing the intensity to minimum remove the absorber(s). Now the full
beam photon flux hits the beam stop before the detector! Be sure that the beam
stop shadows the beam completely, otherwise the detector will be damaged! Normally check the alignment with approx. 100s.
•
Attention! Be sure that the intensity is low and completely shadowed by the
beam stop.
14. Insert a Silver-Behenate sample (Fig. 1-77) into diffraction position
•
Mount the Silver-Behenate sample e onto the sample frame carrier as shown in
Fig. 1-71 (example). Close the shutter press “door open” button (Fig. 1-74), open
the door of the sample chamber and mount the sample into the sample chamber
•
Move y- and x- motor until the sample powder is in the beam. Enter Ctrl Shft D to
enter the x- and y-value.
•
Start a measurement. The diffraction pattern should look similar to the screen shot
in Fig. 1-78. A more or less symmetrical corona around the beam stop shadow
should be seen with one or more rings around it.
15. Beam stop fine alignment
•
With full flux, there should be a asymmetric or symmetric intensity ring around the
beam stop shadow (corona scattering from silver behenate). Fig. 1-78 shows a
symmetric corona.
•
Take a measurement of at least 120 sec or more.
•
Analyse the measurement and press Cntrl V to start settings of “graph vector”
•
Check horizontally whether the corona is symmetrical (Fig. 1-79)
•
If both “peaks” (Fig. 1-80) have not the same peak height, move the beam stop in
x direction a small amount and repeat this measurement until both peaks have the
same height. If necessary then increase the measurement time.
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•
Analyse the same measurement in vertical direction and press Cntrl V to start settings of “graph vector”.
•
Check vertically whether the corona is symmetrical
•
If both “peaks” have not the same peak height, move the beam stop a small
amount in y direction and repeat this measurement until both peaks have same
height. If necessary then increase the measurement time.
•
If the intensity of the silver behenate pattern rings is high enough (measurement
time approx. 600s - 1000s) then calibrate the sample to detector distance (Fig. 182)
•
Chose process → calibrate
•
Enter calibration filename, sample to detector distance (first guess 105cm), detector x and y-centre as determined before (Fig. 1-83).
•
Move theoretical rings to measured ones and start evaluation with left mouse button.
•
The result is the real sample to detector distance.
•
Enter this value into the “admin settings” menue (Fig. 1-37)
16. Background and parasitic scattering reduction and analysis
•
Remove the silver behenate sample so that the beam can pass the complete path
to the beam stop
•
Be sure that all absorbers are removed and there is a good vacuum value (typ.
1.5 x 10-2 mbar but not more than 2.5 x 10-2 mbar) in order to reduce the scattering on air molecules (O2 and N2).
•
Start a “blank”-measurement with at least 1000 sec. measurement time and check
background.
•
Two things are important:
a. If there are “streaks” beginning at the shadow of the beam stop (b in Fig.
1-85) realign the 2nd pinhole in very small amounts of 3-5µm (approx. ½
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unit or less) vertically or horizontally (Fig. 1-32 and Fig. 1-33). In general
the beam stop is aligned good enough with the silver behenate corona, so
the last alignment step is a very fine alignment of the 2nd pinhole.
b. Sometimes if the “corona” of the beam stop is asymmetric align the beam
stop in amounts of approx. 10-30µm. d in Fig. 1-84 shows a symmetric
corona. Sometimes a streak can be so broad that it seems to be an asymmetric shadow of the beam stop. In general try to optimize the 2nd pinhole
first.
•
The homogeneous background is all what there is around the beam stop in a certain distance. It should be homogeneous and the overall intensity should not exceed a certain level.
•
Under the following conditions reach at least the following numbers for
NanoSTAR C systems concerning the background:
a. Detector dark noise: D = max. 10cps (for Cu/Co/U/C)
i. No samples, no filters, no absorbers
ii. Aligned system, measurement at least 600 sec.
iii. Measurement with closed shutter (Fig. 1-100). Don’t mark ‘open &
close shutter’ as shown in Fig. 1-34.
iv. Set kV and mA to min. values
v. Determine counts integral over the complete detector area
(‘counts’) and calculate cps per 1024 px * 1024 px. Calculate also
Dbox = D / 105, this is the detector’s dark noise in a 100 px * 100
px box. This value is important because it is needed later for
background analysis.
b. Homogeneous background: H = max. 0.1 cps per 100 px * 100 px
(Cu/Co)
i. Same conditions as under flux and profile analysis with no filters,
no absorbers, no samples and aligned beam stop.
ii. Set kV and mA to max. values
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iii. Measurement time at least 10000 sec.
iv. Vacuum must be better than 2.5 * 10-2 mbar
v. Measure background counts in a 100 px * 100 px box (F5) at 8
positions, determine the arithmetical median (example see Fig. 1101) and devide by measurement time.
c.
Parasitic scattering background: P = max. 7 cps per 100 px * 100 px
(Cu/Co). Measure with F5 as shown in Fig. 1-102.
i. Conditions identical to measurement of homogeneus background.
Evaluate the same frame as for homogeneous background.
d. Calculate Peff = max. 0.5 cps per 100 px * 100 px
i. Peff = (P – H) / (Cflux / 2.2 * 105 cps) - Dbox
ii. Values Cflux and Dbox as determined above.
17. After all alignment steps are finished and one is satisfied with the performance of the system, note
all parameters for the future:
n. First Göbel mirror:
i. Bragg screw 1 in Fig. 1-19 (1st 40mm mirror) : ........................................................
ii. Tilt screw 2 in Fig. 1-19 (1st 40mm mirror): ..............................................................
iii. Third screw 3 in Fig. 1-19 (1st 40mm mirror):...........................................................
iv. Knife edge screw 4 in Fig. 1-19 (1st 40mm mirror): ..................................................
o. Second Göbel mirror:
i. Bragg screw 5 in Fig. 1-22 (2nd 60mm mirror) : ........................................................
ii. Tilt screw 6 in Fig. 1-22 (2nd 60mm mirror): ..............................................................
iii. Third screw 7 in Fig. 1-22 (2nd 60mm mirror):...........................................................
p. Dove tail p in Fig. 1-20 between the mirrors : ........................................................................
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q. Hor. dove tail 8 in Fig. 1-21:....................................................................................................
r.
Vert. dove tail 9 in Fig. 1-21:...................................................................................................
s.
1st pinhole:
i. micrometer head screw 11 in Fig. 1-23: ....................................................................
ii. micrometer head screw 10 in Fig. 1-23: ....................................................................
t.
4DOF-Parameters for x-, y-translation, Φ-, ψ-rotation
i. Parameter a in Fig. 1-24: ...........................................................................................
ii. Parameter b in Fig. 1-24: ...........................................................................................
iii. Parameter c in Fig. 1-25: ...........................................................................................
iv. Parameter d in Fig. 1-25: ...........................................................................................
nd
u. 2 pinhole:
i. micrometer head screw a in Fig. 1-26: ......................................................................
ii. micrometer head screw b in Fig. 1-26: ......................................................................
v.
Beam stop:
i. micrometer head screw g in Fig. 1-28: ......................................................................
ii. micrometer head screw f in Fig. 1-28: .......................................................................
w. Detector bias setting: ..............................................................................................................
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Figure Captions
Fig. 1-1:
1-92
Standard NanoSTAR SAXS system (NanoSTAR U) with 3-pinhole collimation system for
high intensity applications, 2 secondary beam path tubes for high resolution and sealed
tube.
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Fig. 1-2:
Operating Instructions and Alignment
NanoSTAR U SAXS system in compact setup with 2-pinhole collimation system for scanning SAXS applications, 2 secondary beam path tubes for high resolution and sealed
tube.
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Operating Instructions and Alignment
Fig. 1-3:
1-94
NanoSTAR SAXS System User's Manual Vol. 2
NanoSTAR U SAXS system with 3-pinhole collimation system for high intensity applications, one secondary beam path tube and sealed tube.
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Fig. 1-4:
Operating Instructions and Alignment
NanoSTAR C SAXS system with 2-pinhole collimation system for scanning SAXS applications, one secondary beam path tube and sealed tube.
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Operating Instructions and Alignment
Fig. 1-5:
1-96
NanoSTAR SAXS System User's Manual Vol. 2
NanoSTAR C SAXS system with 2-pinhole collimation system for scanning SAXS applications, one secondary beam path tube and sealed tube.
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Fig. 1-6:
Operating Instructions and Alignment
Parallel beam source (PBS) with sealed tube for high intensity performance. The PBS
consists of a 4DOF with two perpendicular translation stages and two perpendicular rotation stages, the X-ray source (sealed tube), the crossed coupled Göbel mirrors (ccGM)
with slit and exit pinhole and the 1st pinhole of the 2- or 3-pinhole collimation system.
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Operating Instructions and Alignment
Fig. 1-7:
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NanoSTAR SAXS System User's Manual Vol. 2
SAXS sample chamber with primary beam path flanges on the left hand side and secondary beam path flanges on the right hand side. On the top of the chamber there are the
radiation warning lamps.
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Fig. 1-8:
Operating Instructions and Alignment
HiStar area detector with adjustable beam stop ring.
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Operating Instructions and Alignment
Fig. 1-9:
1-100
NanoSTAR SAXS System User's Manual Vol. 2
NanoSTAR SAXS system base with two base units (D8-bases). The left one contains the
electronics components as generator, motor drivers, detector controllers etc. The table is
a very stable steel plate with two granite table units and a precise track system which carries all SAXS components as PBS, primary and secondary beam path tubes and the
chamber and detector.
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Fig. 1-10:
Operating Instructions and Alignment
PBS similar as shown in Fig. 1-6 from the front direction.
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Operating Instructions and Alignment
Fig. 1-11:
1-102
NanoSTAR SAXS System User's Manual Vol. 2
4DOF with two perpendicular rotation stages.
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Fig. 1-12:
Operating Instructions and Alignment
Primary beam path tubes with 2nd pinhole (beam defining pinhole) q and alignment micrometer head screws. The pinhole on the right hand side is integrated into the chamber
(3rd pinhole) as shown in Fig. 1-13.
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Fig. 1-13:
1-104
NanoSTAR SAXS System User's Manual Vol. 2
SAXS sample chamber where the 3rd (2nd for compact systems) pinhole alignment translations can be seen. It is possible to insert an X-ray window on the primary beam path
flange.
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Fig. 1-14:
Operating Instructions and Alignment
SAXS sample chamber with inserted X-ray window cone x for ‘sample under air measurement mode’. Here the XY-sample translation stage and the reference sample wheel is
shown in detail. t is the pinhole in the small tube which can be translated in x- and ydirection by micrometer head screws from outside the chamber.
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Operating Instructions and Alignment
Fig. 1-15:
1-106
NanoSTAR SAXS System User's Manual Vol. 2
Beam stop ring unit with micrometer head screws for XY-translation alignments.
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Fig. 1-16:
Operating Instructions and Alignment
These screws are on each corner of the D8-bases. Align all 8 screws in order to get a
plane surface of the SAXS system’s table top.
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Fig. 1-17:
1-108
NanoSTAR SAXS System User's Manual Vol. 2
Two tracks of one line can be aligned with the third one during assembling and setup
procedure.
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Fig. 1-18:
Operating Instructions and Alignment
The second track line can be set parallel with the PBS on the primary and the detector on
the secondary side.
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Operating Instructions and Alignment
Fig. 1-19:
1-110
NanoSTAR SAXS System User's Manual Vol. 2
First Göbel mirror (40mm long) with alignment screws, Bragg screw 1, tilt screw 2, and
screw 3. 4 is the screw with which the knife edge can be set to correct position (minimum
of direct beam).
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Fig. 1-20:
Operating Instructions and Alignment
Connection dove tail between first and second Göbel mirror.
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Operating Instructions and Alignment
Fig. 1-21:
1-112
NanoSTAR SAXS System User's Manual Vol. 2
Perpendicular exit dove tails at second Göbel mirror. These degrees of freedom translate
the exit pinole to the double diffracted monochromatic beam.
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Fig. 1-22:
Operating Instructions and Alignment
Second Göbel mirror (60mm long) with alignment screws, Bragg screw 5, tilt screw 6,
and screw 7.
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Operating Instructions and Alignment
Fig. 1-23:
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ccGM optics unit with cover and alignment micrometer head screws for the 1st pinhole.
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Fig. 1-24:
Operating Instructions and Alignment
Rotation settings of 4DOF.
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Fig. 1-25:
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Translation settings of 4DOF.
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Fig. 1-26:
Operating Instructions and Alignment
2nd pinhole unit between the two primary beam path tubes with translation micrometer
head screws and lid where the 2nd pinhole can be inserted or changed. Behind this unit
there is a vacuum switch which is integrated in the security and safety system.
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Fig. 1-27:
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SAXS sample chamber with 3rd pinhole flange and adapted primary beam path tubes.
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Fig. 1-28:
Operating Instructions and Alignment
Secondary beam path tube adapted to the SAXS sample chamber with detector and
beam stop ring.
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Fig. 1-29:
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Principle of a mutilayer Göbel mirror optics by using it with a point focus source. Because
the relatively large focus not only Kα radiation is Bragg-reflected by the mirror but also a
small wavelength interval from the generated X-ray spectrum.
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Fig. 1-30:
Operating Instructions and Alignment
Schematic drawing of the geometrical conditions of a 3-pinhole SAXS system. The first
pinhole (750µm) is the divergence pinhole, the second pinhole (400µm) is the beam defining pinhole. Both, the divergence and the definging pinhole limit the maximum divergence of the ‘nearly’ parallel beam. The third pinhole (1000µm) is the antiscatter pinhole
which shadows all edge scattering from the 2nd one. P0 is the Göbel mirror exit pinhole
which shadows most of the disturbing radiation. The secondary distance of 1070mm is
for 2 beam path tubes.
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Fig. 1-31:
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Schematic drawing of the geometrical conditions of a 2-pinhole SAXS system. The first
pinhole (100µm) is the beam defining pinhole. The 2nd pinhole (300µm) is the antiscatter
pinhole which shadows all edge scattering from the 1st one. P0 is the Göbel mirror exit
pinhole which shadows most of the disturbing radiation. The secondary distance of
1070mm is for 2 beam path tubes.
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Fig. 1-32:
Operating Instructions and Alignment
Geometrical principle of the 3-pinhole collimation system. The first two pinholes limit the
divergence and the 3rd shadows the edge scattering of the 2nd one.
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Fig. 1-33:
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Geometrical principle of the 3-pinhole collimation system. The first two pinholes limit the
divergence and the 3rd shadows the edge scattering of the 2nd one. This figure shows
what happens when the 3rd pinhole is not aligned correctly. Rays with maximum divergence of the ‘parallel’ beam hit the antiscatter pinhole and generate disturbing parasitic
radiation which can be seen as streaks on detector frameas.
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Fig. 1-34:
Operating Instructions and Alignment
“Options for collect add” settings if using the detector for directly observing what happens
when screws are turned during the alignment procedures.
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Fig. 1-35:
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Find the “Admin settings” menu in the SAXS software.
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Fig. 1-36:
Operating Instructions and Alignment
Example for “Admin settings” for Cu radiation.
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Fig. 1-37:
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Example for “Admin settings” for Co radiation.
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Fig. 1-38:
Operating Instructions and Alignment
Setting the screw of the knife edge.
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Fig. 1-39:
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Mount knife edge to tube mount with force in direction k. Normally the knife edge is flush
to the tube mount or some 100µm deeper.
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Fig. 1-40:
Operating Instructions and Alignment
PBS a and primary beam path system d with open beam path safety system b-c
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Fig. 1-41:
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Between compact and U setup remove the primary beam path tube system completely.
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Fig. 1-42:
Operating Instructions and Alignment
After removing the primary beam path tube system from the track system move the PBS
to the SAXS sample chamber.
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Fig. 1-43:
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The long secondary beam path system (1070mm) with beam stop ring unit and vacuum
display unit
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Fig. 1-44:
Operating Instructions and Alignment
Closed beam path safety system in compact setup without the primary beam path tube
system.
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Fig. 1-45:
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Insert the X-ray vacuum window into the left primary tube end and turn with force in direction of the tube axis.
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Fig. 1-46:
Operating Instructions and Alignment
Insert X-ray window at the X-ray inlet flange of the SAXS sample chamber when the
compact setup or U-setup and sample under air operation mode shell be used
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Fig. 1-47:
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Insert X-ray window at the X-ray inlet flange of the SAXS sample chamber when the
compact setup or U-setup and sample under air operation mode shell be used. Fix the
window with special X-ray window tool.
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Fig. 1-48:
Operating Instructions and Alignment
Insert 1st pinhole, turn and fix with special pinhole tool
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Fig. 1-49:
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Inner part of SAXS sample chamber with XY-stage, mounting block, sample frame, a
silver behenate powder and a string shaped sample mounted. On the left hand side the
tube with the 3rd pinhole (compact → 2nd pinhole) is shown which can be set from micrometer head screws from outside the chamber.
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Fig. 1-50:
Operating Instructions and Alignment
Pinhole with mounting tool.
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Fig. 1-51:
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Pinhole chamber for the 2nd pinhole between the two primary beam path tubes. The pinhole is under the cover which is mounted with two screws.
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Fig. 1-52:
Operating Instructions and Alignment
Closed beam path safety system between chamber and secondary beam path tubes.
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Fig. 1-53:
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Closed beam path safety system between secondary beam path tubes and detector unit.
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Fig. 1-54:
Operating Instructions and Alignment
Closed beam path safety system between first and second secondary beam path tubes.
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Fig. 1-55:
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Closed beam path safety system plug connecting beam stop ring unit.
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Fig. 1-56:
Operating Instructions and Alignment
Inserting the Cu absorber.
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Fig. 1-57:
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Detector frame with four beams resulting from crossed coupled Göbel mirrors. A detailed
description is done in another figure.
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Fig. 1-58:
Operating Instructions and Alignment
This drawing shows how crossed coupled multilayer mirrors work. The first mirror 5 conditions the divergent beam 10 parallel in the x-z-plane and the second mirror in XY-plane,
respectively. 1, 2 and 4 are the alignment screws of the first mirror. 6 is the knife edge
with setting screw 3.
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Fig. 1-59:
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Set of slits and pinholes. d and c are pinholes for the 2nd pinhole position, a and b are
slits which can be used for alignment. a is for the 2nd pinhole position and can be inserted
in two orientations, horizontally and vertically, respectively. h is an alignment slit for the
1st and 3rd (compact: 2nd) pinhole position and can also be rotated by 90°. e, f and g are
pinholes with different sizes.
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Fig. 1-60:
Operating Instructions and Alignment
Remove the second secondary beam path tube after loosen the screws and clamps and
move back the detector unit.
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Fig. 1-61:
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Move the detector to the secondary beam path tube carefully.
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Fig. 1-62:
Operating Instructions and Alignment
Fix the detector with the clamps to the beam path tube.
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Fig. 1-63:
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Attention! Switch off the detector’s bias (high voltage) with the switch in the controller
before moving it.
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Fig. 1-64:
Operating Instructions and Alignment
b is Φ-rotation (vertical rotation axis), a is ψ-rotation (horizontal rotation axis). 3, 3’, 4, 5
and 6 are fixing screws.
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Fig. 1-65:
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Shifts in x- and y-direction when the beam is not perpendicular to the detector face. Here
the position of the inclined beam is shown in two detector positions, with one (a) and two
(b) secondary beam path tubes, respectively. Check whether x1 < x2 or x2 < x1 and y1 <
y2 or y2 < y1 in order to decide in which direction the beam has to be rotatet.
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Fig. 1-66:
Operating Instructions and Alignment
These are the approx. distances between the rotation axes and the detector positions
with one (a) and two (b) detector tubes, valid for the NanoSTAR U version with 3-pinhole
collimation system.
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Fig. 1-67:
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Translations screws of the 4DOF in x- and y-direction with fixing screws c.
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Fig. 1-68:
Operating Instructions and Alignment
Vertical alignment slit at 3rd pinhole position inside the sample chamber.
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Fig. 1-69:
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Horizontal alignment slit at 3rd pinhole position inside the sample chamber.
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Fig. 1-70:
Operating Instructions and Alignment
X- and y- translation micrometer head screws on primary side of the sample chamber.
The 3rd pinhole inside the chamber can be set from outside.
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Fig. 1-71:
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3rd pinhole (d) inside the sample chamber with silver behenate powder sample (e) on
translation stage
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Fig. 1-72:
Operating Instructions and Alignment
Example of beam profile of primary beam.
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Fig. 1-73:
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Options for edit configure user settings
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Fig. 1-74:
Operating Instructions and Alignment
Right column of left D8-base from NanoSTAR U system with on-off-buttons, generator
switch and control lamps.
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Fig. 1-75:
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Micrometer head screws for x- and y-translation of beam stop.
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Fig. 1-76:
Operating Instructions and Alignment
Example of blank measurement with inserted beam stop.
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Fig. 1-77:
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Silver behenate powder sample
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Fig. 1-78:
Operating Instructions and Alignment
Example of silver behenate diffraction frame with corona around the beam stop shadow.
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Fig. 1-79:
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Profile through a beam stop shadow and corona of a silver behenate powder sample.
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Fig. 1-80:
Operating Instructions and Alignment
Profile through a beam stop shadow and corona of a silver behenate powder sample with
plot.
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Fig. 1-81:
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Calibration of detector distance with silver behenate powder sample
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Fig. 1-82:
Operating Instructions and Alignment
How to find the calibrate menue?
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Fig. 1-83:
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Options for process calibrate
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Fig. 1-84:
Operating Instructions and Alignment
Example for good aligned pinholes and beam stop.
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Fig. 1-85:
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Streaks in a blank measurement indicate that the 3rd pinhole is hit from the primary beam.
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Fig. 1-86:
Operating Instructions and Alignment
Same as Fig. 1-85 but better aligned 3rd pinhole.
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Fig. 1-87:
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y-value for opening and closing the knife edge
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Fig. 1-88:
Operating Instructions and Alignment
Blank measurement with streak recorded with short exposure time.
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Fig. 1-89:
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Very good aligned SAXS system with symmetric beam stop shadow and without streaks.
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Fig. 1-90:
Operating Instructions and Alignment
Four beams resulting from two Göbel mirrors perpendicular to each other and pint focus
source. Details are described in Fig. 1-90.
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Fig. 1-91:
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Four beams resulting from two Göbel mirrors perpendicular to each other and pint focus
source. b is the direct beam which passes the mirrors and housing, c is the Bragg reflected beam from the 1st Göbel mirror. a is the Bragg reflection of b from the 2nd mirror
and d is the double diffracted beam by both mirrors. The edge e is the shadow of the
knife edge and f is the shadow of the tube which holds the pinhole.
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Fig. 1-92:
Operating Instructions and Alignment
After inserting a slit aperture between the two Göbel mirrors, c and b from Fig. 1-91 are
shadowed by the slit aperture.
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Fig. 1-93:
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Same as Fig. 1-92 but with different setting of the knife edge.
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Fig. 1-94:
Operating Instructions and Alignment
Inserting the 1st pinhole with special tool.
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Fig. 1-95:
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Turn a anticlockwise to lift source in direction b.
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Fig. 1-96:
Operating Instructions and Alignment
Turn a clockwise to move source in direction b.
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Fig. 1-97:
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Turn c anticlockwise to move source in direction d.
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Fig. 1-98:
Operating Instructions and Alignment
Turn a clockwise to move source in direction d.
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Fig. 1-99:
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Distances of rotation axes from detector positions (one and two tubes, respectively).
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Fig. 1-100: Dark count measurement with Histar detector and closed shutter.
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Fig. 1-101: Blank measurement and determination of average homogeneous background.
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Fig. 1-102: Blank measurement and determination of parasitic background radiation.
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Fig. 1-103: Removing the secondary beam path tube from the sample chamber flange by loosen the
clamps.
1-194
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Fig. 1-104: Moving back the secondary beam path tube.
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Fig. 1-105: Inserting the X-ray window cone.
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Fig. 1-106: Hold the cone in correct position.
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Fig. 1-107: Moving the secondary beam path tube to the sample chamber with X-ray cone.
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Fig. 1-108: Check whether the cone is in correct position before the secondary beam path tube is
fixed again.
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Fig. 1-109: Check whether the cone flange is in plane with the chamber flange and the tube end.
1-200
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Fig. 1-110: Check whether the rubber seal of the cone is in correct position before the secondary
tube is fixed again.
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Fig. 1-111: X-ray window vacuum cone.
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Fig. 1-112: Pinhole with special tool
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Fig. 1-113: Inserting the pins of the tool into the grip holes of the pinhole
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Fig. 1-114: Grip the pinhole with tool
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Fig. 1-115: Fixing screw of one of the supports on the track system
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Fig. 1-116: Pirani vacuum element adapted at sample chamber flange
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Fig. 1-117: Pirani vacuum element adapted at secondary beam path tube (beam stop) system.
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Fig. 1-118: Two 6-pack sample holder
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Fig. 1-119: 6-pack sample holder on sample frame
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Fig. 1-120: Scattering of radiation by sample.
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Fig. 1-121: Parasitic radiation generated by the edge of pinhole P1
1-212
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Fig. 1-122: Geometrical conditions with two pinholes.
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Fig. 1-123: Göbel mirror X-ray optics with X-ray source in focus of parabola.
1-214
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Fig. 1-124: Two crossed couple Göbel mirror optics conditioning a parallel beam in two dimensions.
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Fig. 1-125: Vacuum system: left shut-off valve closes the complete system (i.e. primary beam path
system + secondary beam path system + sample chamber) and right one only closes the
chamber evacuation. In this case the sample chamber can be vent separately if it is
separated from the primary and secondary tubes with X-ray windows or X-ray cone, respectively.
1-216
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Fig. 1-126: Intrinsic divergence of a multilayer X-ray optics.
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Fig. 1-127: If the X-ray source is larger than the ‘monochromatic eye’ of the mirror then other than
Kα radiation is Bragg reflected by the mirrors multilayer.
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Fig. 1-128: Pump wit oil filter and hose.
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Fig. 1-129: Connection of evacuation hose on 2nd pinhole chamber.
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Fig. 1-130: Connection of vacuum switch on 2nd pinhole chamber.
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Fig. 1-131: Connection of pirani gauge and vacuum switch on secondary beam path side.
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Fig. 1-132: Connection of pirani gauge and vacuum switch on secondary beam path side.
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Fig. 1-133: Door closing and security system for the door chamber.
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Fig. 1-134: Samples on sample carrier.
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Fig. 1-135: Long NanoSTAR system in compact setup and WAXS setup.
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Fig. 1-136: 2nd pinhole chamber with support and part of the track system.
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Fig. 1-137: Samples on sample carrier mounted on sample frame.
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Fig. 1-138: Samples on sample carrier mounted on sample frame.
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Fig. 1-139: WAXS extender with sample frame
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Fig. 1-140: User working with SAXS software
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Fig. 1-141: PBS with source (sealed tube), 4DOF, 1st pinhole and ccGM.
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Fig. 1-142: PBS system.
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Fig. 1-143: Radioactive Fe55 source.
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Fig. 1-144: This table shows how the cables have to be connected with frame buffer, detector, PDCcontroller and D8-controller.
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Fig. 1-145: Schematic drawing of detector with Be-window and multi-wire electrode.
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Fig. 1-146: Plugs and control of the detector.
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Fig. 1-147: Sample frame with holder for radioactive Fe55 source.
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Fig. 1-148: Sample frame with Fe55 holder inserted in sample mount of chamber.
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Fig. 1-149: Absorbers, slits and clamp for X-ray optics (ccGM).
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Fig. 1-150: Glass capillary with open ends.
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Fig. 1-151: Settings for Chi-integration.
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Fig. 1-152: Scattering intensity of pure water vs. scattering vector q
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Fig. 1-153: ‘flood/new options’ menue
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Fig. 1-154: ‘options for process calibrate’ menue
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Fig. 1-155: Uncorrected frame with fiducial brass plate
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Fig. 1-156: Spatial corrected frame from fiducial brass plate
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Fig. 1-157: ‘process/spatial/unwarp’ command menue
Fig. 1-158: ‘options for process calibrate’ command menue
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Fig. 1-159: Silver behenate sample frame with several rings and short distance
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Fig. 1-160: ‘options for collect scan radiography’ menue
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Fig. 1-161: Radiography of a sample
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Fig. 1-162: ‘send targets to SAXS/Start collecting targets’ window
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Fig. 1-163: ‘scan multitargets list’ window
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Fig. 1-164: ‘options for collect scan multitargets’ menue
Fig. 1-165: ‘options for analyse transmission’ window
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