furnacemar345
Handbook
total outer
length of
fibres: 4-5mm
distance crystalalumina-tube: 3mm
distance crystal - brass-tube:
min: 20.5mm
max: 21.5mm
alumina-tube:
fl 0.5mm, length: 26mm
brass-tube:
fl 3mm, length: 8mm
furnacemar345
Handbook
for the high temperature furnace attachment to the mar345
imaging plate detector system
Version 1.6
November 2000
Copyright © November 2000
by Michael Estermann, Roman Gubser, Monika Krichel, Katja Lemster, Hans Reifler,
Stefan Scheidegger, Walter Steurer.
Laboratory of Crystallography
Eidgenössische Technische Hochschule ETH
ETH Zentrum
CH-8092 Zürich
Switzerland
http://www.kristall.ethz.ch/LFK
Contact
Michael Estermann
Laboratory of Crystallography
Eidgenössische Technische Hochschule ETH
ETH Zentrum
CH-8092 Zürich
Switzerland
Phone
+ 41 (0)1 632 64 04
Fax
+ 41 (0)1 632 11 33
Email
michael.estermann@kristall.erdw.ethz.ch
furnacemar345
Contents
INTRODUCTION ............................................................... 5
Synopsis .................................................................................................... 5
Documentation .......................................................................................... 5
FURNACE ......................................................................... 7
Components .............................................................................................. 7
Furnace housing ..............................................................................................................7
Heating core .....................................................................................................................7
Transformer ..................................................................................................................... 7
Power controller ...............................................................................................................7
Temperature controller .....................................................................................................7
Thermocouple ..................................................................................................................7
Crystal mounting ..............................................................................................................7
Computer control (Silicon Graphics) ................................................................................7
Preparing the mar345 base ...................................................................... 8
Helium beam path (optional) .................................................................. 15
Attach the furnace base ..........................................................................16
Place furnace onto furnace base ............................................................18
Connect furnace to supplies .................................................................. 21
Sample change .........................................................................................21
Changing the heating rods ......................................................................24
CRYSTAL MOUNTING ................................................... 25
High Temperature Crystal Holding Devices ......................................... 25
Building the crystal holding device with alumina fibres ..................................................25
Alumina fibre crystal holder, mounting the crystal ......................................................... 26
Building the crystal holding device with two quartz glass capillaries ............................. 27
Components .............................................................................................29
Alumina tubes ............................................................................................................... 29
Alumina fibres ............................................................................................................... 29
furnacemar345
High temperature cement .............................................................................................. 29
Goniometer head .......................................................................................................... 29
Quartz glass capillaries ................................................................................................. 29
TEMPERATURE CONTROL .......................................... 30
Programmable PID controller, Eurotherm EPC900 ...............................30
Back panel, connections ...............................................................................................
Front panel, fuses .........................................................................................................
Front panel keys, EPC900 Controller ............................................................................
Graphic display, EPC900 Controller ..............................................................................
Setting limits, EPC900 Controller ..................................................................................
Activate Setpoint rate limit SRL, EPC900 Controller .....................................................
Auto Tune (AT), EPC900 Controller ..............................................................................
Initiate Auto Tune ..........................................................................................................
Instrum. Conf.-Level, EPC900 Controller ......................................................................
30
30
31
31
31
32
33
33
34
Temperature calibration.......................................................................... 34
Calibration reference thermocouple RTC ...................................................................... 34
Calibration furnace ........................................................................................................ 34
COMPUTER CONTROL ................................................. 35
Hardware at the Swiss-Norwegian Beamline at ESRF ..........................35
EPC900 Controller, Silicon Graphics OCTANE ............................................................. 35
Silicon Graphics OCTANE ............................................................................................ 35
Wiring EPC900 - Silicon Graphics OCTANE ................................................................. 35
EPC900 supervisory program .................................................................36
In situ diffraction at 900 ºC ......................................................................36
furnacemar345
INTRODUCTION
Synopsis
This handbook describes the installation and operation of the high-temperature furnace attachment for the
mar345 imaging plate detector system (X-ray Research GmbH, Norderstedt, Germany). The helium beam
path for the mar345 system is also described.
Both the high-temperature attachment and the helium beam path were developed at the Laboratory of
Crystallography, ETH Zürich, Switzerland.
The heating core was developed in collaboration with the Professur für Nichtmetallische Werkstoffe, ETH
Zürich, Switzerland.
Documentation
•
The marresearch Imaging Plate System Owner’s Guide, X-ray Research GmbH
http://www.marresearch.com
•
High-temperature furnace for an imaging-plate data-acquisition system.
J. Schreuer, A. Baumgarte, M. A. Estermann, W. Steurer and H. Reifler.
Journal of Applied Crystallography (1996) 29, 365-370.
•
A helium beam path for an imaging plate detector system.
M. A. Estermann, S. Scheidegger, H. Reifler and W. Steurer.
Journal of Applied Crystallography (1998) 30, 1165-1166.
•
Diffuse scattering data acquisition techniques.
M. A. Estermann and W. Steurer.
Phase Transitions (1988) 67, 165-196.
•
A high-temperature furnace for X-ray diffraction with directly machined α-Al2O3 ceramic parts.
M. Estermann, H. Reifler, W. Steurer, F. Filser, P. Kocher and L. J. Gauckler.
Journal of Applied Crystallography (1999) 32, 833-836.
furnacemar345
•
THERMOCOAX
http://www.thermocoax.fr
•
900 EPC Series Enhanced Programmer Controllers Handbook
900 EPC Handbook Supplement
900 Series Digital Communications Handbook
Eurotherm Controls
http://www.eurotherm.com
•
Helium flow meter, GEC Marconi 40-500, Elliot Process Instruments
1100 series
WISAG Zürich
•
Helium reduction valve, DL230-0.1, SL Gas, 0-0.1 bar
Sauerstoff Werke, Lenzburg AG
WISAG Zürich
furnacemar345
FURNACE
Components
Furnace housing
Integrated water cooling
Entry and exit window (Kapton) for X-ray beam
In-situ observation of crystal specimen by CCD-camera
Heating core
The heating core of the furnace consists of a solid block of sintered aluminium oxide ceramic in which
four heating rods are placed. The heating rods have an embedded 0.5mm Kanthal wire. Inside the
solid ceramic block is a cavity which hosts the crystal specimen. Access to the central cavity is provided
by a number of holes. This includes access for incident and diffracted X-ray beam, optical observation
of the crystal specimen with a CCD-camera system, and thermocouple.
Transformer
Lapp-Textima, 20 volt terminal
Power controller
425S Solid state relay with optional Partial Load failure, Eurotherm Controls
Temperature controller
4900 EPC Series Enhanced Programmer Controllers, Eurotherm Controls
Thermocouple
Thermocouple in furnace:
THERMOCOAX mantle thermocouple, chromel-alumel, type K, thermocouple SKI10/50, compensation
cable 2AB35NN, connector MF7M
Thermocouple at position of crystal specimen:
THERMOCOAX mantle thermocouple, chromel-alumel, type K, thermocouple SKI05/25, compensation
cable 2AB35D, connector MF7M
Crystal mounting
Crystal specimen is clamped between alumina fibres of 0.01 mm thickness
Computer control (Silicon Graphics)
Supervisory program for EPC900 controller via RS232 serial interface
furnacemar345
Preparing the mar345 base
Fig. 2:
Attach two magnetic stands onto the base to keep the mar345 in place during installation, put a piece of
paper in between stand and marbase.
Fig.3 : Remove the connectors from the back of the scanner.
Fig. 4:
Unscrew the scanner from the scanner base plate, remove the screw completely from the scanner (Allen
key, size 2.5mm).
Fig. 5: Lift scanner away from the screw, do not touch the Kapton window of the scanner.
furnacemar345
Fig. 6: Detector base without scanner.
Fig. 7: Remove scanner base plate (Allen key, size 3.0 mm).
Fig. 8: Unscrew the white cover at the back of the detector base.
Fig. 9: Remove cover, cables remain connected.
furnacemar345
Fig. 10: Unscrew the black cover.
Fig. 11: First, move the spindle axis to the end-position in direction of the collimation block. Second, remove
black cover vertically.
Fig. 12: Unscrew white cover at the front of the detector base.
Fig. 13: Remove cover.
furnacemar345
Fig. 14: Re-insert all unused screws for safe keeping.
Fig. 15: Unscrew white side cover.
Fig. 16: Remove white side cover.
Fig. 17: Unscrew side cover on the opposite side.
furnacemar345
Fig. 18: Remove cover.
Fig. 19: Unscrew white front cover.
Fig. 20: Remove white front cover.
Fig. 21: Move white cover at the back, back on.
furnacemar345
Fig. 22: Move back scanner base plate (black).
Fig. 23: Attach supporting elements (three are of the same type, one is different), leave 5 mm freedom
between support element and the table.
Fig. 24: Turn brass screw until it contacts with base plate, then tighten.
Fig. 25: Attach supporting element at the front.
furnacemar345
Fig. 26: Tighten screws.
Fig. 27: First, remove screw which fixes the scanner (if not already done). Second, move scanner back onto
detector base, and fix with the single screw (Allen key, size 2.5 mm).
Fig. 28: Place a sheet of paper onto the detector base (in case a screw falls down), remove beam stop.
Fig. 29: Unscrew spindle axis.
furnacemar345
Fig. 30: Remove bolt which fixes spindle axis, remove spindle axis.
Helium beam path (optional)
Fig. 31: Attach clamp.
Fig. 32: Attach helium beam path at the clamp, insert special collimator.
furnacemar345
Fig. 33: Attach the beam stop.
Fig. 34: Move special spindle axis (brass) into position, insert positioning bolt.
Attach the furnace base
1
2
Fig. 35: Position the clamps before attaching the furnace base, (1) loose, (2) tightened.
Fig. 36:
(a) Attach the furnace base by inserting it in a slightly tilted position into the detector base, insert first clamp
1, then clamp 2.
(b) Tighten the clamps which hold the furnace base on the detector base.
furnacemar345
Fig. 37: Lower clamp.
Fig. 38: Tighten support bolt.
Fig. 39: Remove the four bolts on the translation table of the furnace base.
furnacemar345
Place furnace onto furnace base
Fig. 40:
Move the translation table as far back as possible (service position), place furnace onto translation table
(positioning bolts), tighten the four other bolts.
Fig. 41:
Remove flange clamp as shown in picture, remove small furnace housing from the rest of the housing and
place fully on a even surface.
2
1
Fig. 42: Unscrew the heat shield, remove heat shield, lower screw 1, upper screw 2.
Fig. 43: Fully open all collimation slits.
furnacemar345
Fig. 44: Reconnect all the cables to the mar345 system.
(a) Open beam shutter (hidden switch underneath the detector base).
(b) Insert brass needle into collimation system.
(c) Close collimation system gently until contact.
(d) Open collimation slits slightly so that needle can be moved.
(e) Move needle as close as possible (without touching) to the heating core.
(f) Close collimation system gently until contact.
(g) Centre the heating core with translation tables (vertical, horizontal).
(h) Centre the CCD-camera observation hole on the TV-screen by translating the spindle axis (and herewith
the CCD camera).
Fig. 45:
(a) Lock the horizontal and vertical translation tables by the black screws.
(b) Remove needle by extracting it through the collimation system.
furnacemar345
Fig. 46:
(a) Set the zero-position on ring of the horizontal translation table.
(b) Move furnace into service position.
(c) Screw on heat shield gently.
Fig. 47:
(a) Move back small furnace case.
(b) Align Kapton exit window vertically.
Fig. 48:
(a) Apply vacuum grease on customised spindle axis (brass).
(b) Place flange over spindle axis.
(c) Attach spindle axis, insert positioning bolt, screw on spindle axis (Allen key, size 3.0 mm).
continue on next page
furnacemar345
Fig. 48: Continued from previous page.
(d) Translate spindle axis into position.
(e) Place goniometer head with needle onto spindle axis.
(f) Centre needle.
(g) Move furnace forward into measurement position.
Connect furnace to supplies
•
•
•
•
•
•
cooling-water supply
thermocouple plug with the compensation cable
electrical heating cable with the terminal clamp
helium gas supply
vacuum tube to pump
vacuum meter
Sample change
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
Set temperature to room temperature (i.e. epc900> SL 25.0)
Turn off thyristor on the temperature controller (for quick cooling)
Close He-valve
Remove clamp between spindle and furnace
Release locking arm and translate furnace back to be able to access sample
Remove sample and put on a new one
If a capillary powder sample is used , orient capillary while checking on monitor (adjust tilt also !)
Translate back furnace to correct position (check position on monitor)
If necessary, put vacuum grease on spindle axis and on furnace side of flange
Start vacuum pump
Open slowly vacuum valve and check that flange between spindle axis and furnace is pulled in
Close vacuum valve when Kapton-window has moved inwards
Insert clamp between spindle and furnace
Check on vacuum meter that vacuum is OK (approx. 1.5 mbar)
Close vacuum valve and check that needle moves only slowly clockwise
Turn off vacuum meter, close vacuum valve
Open slowly He-valve until Kapton window bulges out (He-flow 400 ml/min)
Close He-valve, open slowly vacuum valve and check vacuum
Repeat the above three points a couple of times to wash out furnace (3-4 times)
Finally close vacuum valve, turn off vacuum pump and vacuum meter
Open He-valve and adjust flow to approx. 40 ml/min
Collect an image at room temperature to check that everything is OK
Start heating to desired temperature
furnacemar345
Fig. 49:
(a) Place goniometer head with crystal onto spindle axis.
(b) Move furnace forward into measurement position.
(c) Open vacuum valve and pump.
(d) Move flange on spindle axis towards the flange of the furnace housing.
(e) Check vacuum meter (leaks in vacuum).
Fig. 50: Attach the special flange clamp, tighten with the brass screw.
Fig. 51:
(a) Screw on beam stop.
(b) Setup the helium atmosphere by a sequence of pumping and filling (with helium) of the furnace (helium
reduction valve 0.02 bar).
furnacemar345
Fig. 52: Cooling-water connections.
Fig. 53: Electrical heating wires, thermocouple connections.
Fig. 54: Helium supply and flow meter.
Fig. 55: Overview.
furnacemar345
Changing the heating rods
Follow the instructions from Fig. 40 to 42. Remove the heat shield, exchange the heating rods, replace the
heat shield, and assemble the furnace housing.
Fig. 56 & 57: The heating core with embedded heating elements. Loosen screws and replace the heating
rods.
furnacemar345
CRYSTAL MOUNTING
High Temperature Crystal Holding Devices
Building the crystal holding device with alumina fibres
Alumina tubes of 0.5 mm diameter are cut with a diamond saw to their final length of 26 mm. Five to eight
alumina fibres of 0.01 mm thickness are placed into one tube and fixed with high temperature cement based
on ceramic compounds and water (Polytec 903HP). The free ends of the fibres are then glued together with
cement.
The next step is to heat the cement to harden it by loss of water and organic compounds. The alumina tubes
with the fibres are placed into the furnace, standing in little alumina crucibles. The heat treatment (A) is as
follows:
Room temperature — heating rate 120ºC/h — 120ºC for 2h — heating rate 220 or 340ºC/h — 340ºC for 4h
— cooling to RT.
Another step (B) is a temperature treatment for better stability of the fibres to avoid - or at least minimize distortion and excessive movements once the crystal is clamped in. The alumina tubes with the fibres are
heated up to 1000ºC and are held at this temperature for about an hour. It is useful to carry out this step
directly after the cement treatment to save time and energy.
total outer
length of
fibres: 4-5mm
distance crystalalumina-tube: 3mm
distance crystal - brass-tube:
min: 20.5mm
max: 21.5mm
alumina-tube:
Ø 0.5mm, length: 26mm
brass-tube:
Ø 3mm, length: 8mm
Fig. 58: High temperature crystal holding device - dimensions.
furnacemar345
The heat-treated tube then is cemented into the brass tube. It is necessary to straighten the tubes extremely
well, otherwise there could be problems with the centring of the crystal in the high temperature furnace later.
The freshly cemented tubes have to dry for about an hour and then are treated again as mentioned above
(A).
Fig. 59: The fibres holding a crystal
Alumina fibre crystal holder, mounting the crystal
To mount the crystal, it is necessary to fix a “Crystal Mounting Device” to the microscope (Nikon SMZ-2T).
This mounting device consists of two goniometer head holders (Enraf-Nonius).
Fig. 60: Crystal attached to a small piece of bee wax.
Fig. 61: Crystal clamped between fibres, detached from the bee wax.
One holder is fixed to the microscope and the other one to the desk. They are perpendicular to each other.
The Huber goniometer head with the prepared crystal holding device is placed onto the first holder, a
furnacemar345
goniometer head with a preparation needle is placed onto the other. The difficulty now is to insert the tip of
the preparation needle between the fibres of the crystal holding device. This needs several attempts, because
of the height adjustment between the two goniometer heads. Once the tip of the preparation needle holds
the fibres apart, actual mounting of the crystal can begin. The operator takes a second preparation needle,
fixes a very small piece of bees wax on it and picks up the crystal. Now you need a steady hand to put the
crystal between the fibres. If the position of the crystal is right, the second goniometer head with the first
preparation needle has to be moved back, so that the crystal will be clamped between the fibres. It is useful
to check the strength of hold with several light hits against the goniometer head holder which carries the
Huber goniometer head with the clamped crystal. If the crystal does not move any more, mounting has been
successful.
Building the crystal holding device with two quartz glass capillaries
Alternatively, a single crystal may be placed onto the end of a small inner capillary, which in turn is placed
into the larger outer capillary. Both capillaries are placed into the brass-tube. The measures from Fig. 59a
apply. The capillary enters the heating core via a hole with a diameter of 2.5 mm, preferably one should use
capillaries of 1.5 mm or less in diameter. We used the Huber, Eucentric Goniometer Head 1005, for all the
applications.
Do not touch the quartz glass capillary without gloves, the capillary could crystalise at high
temperatures.
1 Mount the crystal onto the inner glass capillary with cement
Break capillary at desired length (> 20 mm) so that it still can be handled (scratch capillary at breaking point
with sandpaper to ease breaking).
In order to close the capillary opening, insert cement into the capillary opening, let it dry a bit.
Use cement with a lot of water, and place a drop of cement onto the dried cement on the capillary. Place the
crystal onto a waxed needle. Place crystal immediately onto the cement drop. Leave it to dry.
crystal
4 mm ± 2 mm
cement
inner capillary
(Ø 0.2-0.3 mm)
cement
glue
24 mm ± 2 mm
approx. 36 mm
outer capillary
filled with argon
(Ø 0.5-1.0 mm)
brass tube
8 mm
Ø 1-2 mm
Fig. 59a: Schematic drawing of the mount of a single crystal with double capillaries (prevents
recristallisation at high temperatures). The measures also apply for a single capillary mount.
2 Temper the cement to remove water from cement
Place capillary into a alumina crucible, and place it into a furnace.
Heat at 120°C for one hour
furnacemar345
3 Place outer capillary over inner capillary
Break outer capillary at desired length (20 mm). If both ends are open, flame-seal one opening (use gas/
oxygen mixture because cigarette lighter flame is not hot enough).
Carefully insert inner into outer capillary, crystal should not touch the end of the outer capillary (danger of
recrystallisation), 2mm distance.
Fix the inner to the outer capillary with glue (Cellit) for further handling.
4 Fill capillaries with argon gas
Place the capillaries, open end upside, into the alumina crucible and place into the glove box pass-through.
Evacuate the pass-through three times and carefully fill with argon.
5 Flame-seal second capillary opening
Remove capillaries from the glove box pass-through, keep capillaries upright, and flame-seal capillaries.
6 Place capillaries into brass tube
Place some glue (e.g. Araldit rapid) into the brass tube. Depending on the experiment, the glue should
withstand heat.
Place capillaries into the brass tube, and align them along the axis of the brass tube.
Apply cement at the upper end of the brass tube to seal off brass tube and glue from the high temperatures
at the experiment.
Fig. 59b: Single-crystal mounted with double capillary technique.
furnacemar345
Components
Alumina tubes
Degussit AL23 insulating tube D 0.5/0.2mm.
http://www.friatec.de
Email info@friatec.de
Alumina fibres
Goodfellow AL605725, filament diameter 0.01mm.
http://www.goodfellow.com
High temperature cement
Cement 903 HP, Polytec.
Polytec GmbH, Polytec-Platz 1-7, 76337 Waldbronn, Germany.
http://www.polytec.com Email info-vi@polytec.de
Goniometer head
Huber, Eucentric Goniometer Head 1005, 49mmm.
HUBER Diffraktionstechnik GmbH, Sommerstraße 4, D-83253 Rimsting, Germany.
http://ourworld.compuserve.com/homepages/xhuber
Email xhuber@compuserve.com
Quartz glass capillaries
Quartzglass capillaries (Mark-Röhrchen).
inner capillaries 0.2 - 0.3 mm diameter, outer capillaries 0.7 - 1.0 mm diameter.
Glass, Technik und Konstruktion, Wolfgang Müller, Glasinstrumentemachermeister,
Germanenweg 13c, D-14621 Schönwalde bei Berlin, Germany.
furnacemar345
TEMPERATURE CONTROL
Programmable PID controller, Eurotherm
EPC900
Back panel, connections
(1)
Fig. 62:
(2)
(3)
(1) RS232 serial communications interface.
(2) Connector thermocouple.
(3) Exit power controller.
(4) Mains 230V.
Front panel, fuses
(1)
Fig. 63:
(2)
(1) Fuse 250V/500mA.
(2) Fuse 600V/20A.
furnacemar345
(4)
Front panel keys, EPC900 Controller
Fig. 64: Front panel EPC900.
The instrument can be operated by means of the front panel keys or via the supervisory communications
port (RS232). The functioning of the instrument may be accessed by operation of the six front panel keys.
The main functions of the instrument are arranged in menu format, which are accessed by the PAGE key,
parameters in the menu can be scrolled by the SCROLL key and entered by the VIEW key.
selects next menu or returns to the previous menu display
SCROLL key, scroll to next parameter or moves highlighted cursor from one
entry to another
accepts highlighted parameter
decrements/increments highlighted numerical parameter
Graphic display, EPC900 Controller
Fig. 65: graphic display
Setting limits, EPC900 Controller
Go to access level 2 ( press
until access levels reached)
Press
until SET POINTS reached
Select with
Proceed to SPLIMITS with
and select with
Enter the following values
SPH = Set Point High= 1000.0
SPL = Set Point low = 0.0
SPR = Set Point Rate / min= 30.0
Move back with
to access level 2 and proceed in an analog way with OUTPUTS and proceed to OPLIMITS
Enter the following values
HO1 = output power high limit = 70 [%]
LO1 = output power low limit= 0.0
OPR = output power rate limit dP/dt = 50.0 [%/s]
(OP = current output power)
furnacemar345
Fig. 66: Limits
Activate Setpoint rate limit SRL, EPC900 Controller
This function allows the working setpoint to be ramped from the current process variable value to the defined
target setpoint. The setpoint rate is in units per minute (unless changed in user configuration menu). The
setpoint rate has to be activated after an Auto Tuning or turning the mains off and on again.
The setpoint rate limit, SRL has to be selected from the parameter scroll list. Press the SCROLL key
until SRL-OFF is displayed and press an up or down key to obtain SRL-ON.
To set the setpoint rate SPR with the front panel keys, press the SCROLL key until SPR is displayed. Press
the up and down keys to set the required value.
The setpoint rate SPR can also be set via the supervisory program located on the Silicon Graphics Octane
computer.
furnacemar345
Auto Tune (AT), EPC900 Controller
The autotune AT is a one-shot algorithm which can be manually initiated at any time to allow the user to retune the instrument control parameters to suit a new setpoint or experimental condition (water pressure,
different heating element). Use the autotune in combination with adaptive tune ADT.
Initiate Auto Tune
&
.
Turn off controller, turn on again and press both
Proceed to Auto Tune page and follow the instructions below.
Fig. 67: Initiate Autotune.
Adaptive tune will be suspended if manual operation is selected but is automatically reinstated
when the instrument is switched back to automatic operation. Ensure that automatic mode is in
operation.
Activate setpoint rate limit SPR.
furnacemar345
Instrum. Conf.-Level, EPC900 Controller
2
1
Fig. 68: Instrument configuration level
no changes are required for normal use
turn off controller, turn on again and press both
&
Temperature calibration
The temperature is calibrated with a reference thermocouple (RTC) placed at the position of the crystal
specimen. The RTC is mounted on a flange which fits onto the corresponding flange of the furnace housing.
The temperature is changed in steps of 50º and the thermovoltage from the RTC is measured with a suitable
instrument. The RTE, the compensation cable and the voltmeter are a calibrated system. If any of these
components are replaced, the complete system has to be re-calibrated.
Calibration reference thermocouple RTC
13-JUN-1997, temperature RTC versus thermovoltage
temperature [ºC] = 32.201747 + thermovoltage RTC [mV]*25.117049
Calibration furnace
17-JUN-1997, ESRF, temperature furnace versus temperature display EPC900
temperature EPC900 [ºC] = - 0.47647 + temperature furnace [ºC] * 0.95201
14-MAY-1998, ESRF, temperature furnace versus temperature display EPC900
temperature EPC900 [ºC] = - 19.46447 + temperature furnace [ºC] * 1.00279
03-JUN-1998, ESRF, temperature furnace versus temperature display EPC900
temperature EPC900 [ºC] = - 20.58268 + temperature furnace [ºC] * 0.96146
12-JUN-1998, ESRF, temperature furnace versus temperature display EPC900
temperature EPC900 [ºC] = - 11.85021 + temperature furnace [ºC] * 0.936624
29-OCT-1998, ESRF, temperature furnace versus temperature display EPC900
temperature EPC900 [ºC] = - 20.2998 + temperature furnace [ºC] * 0.97259
furnacemar345
COMPUTER CONTROL
Hardware at the Swiss-Norwegian
Beamline at ESRF
EPC900 Controller, Silicon Graphics OCTANE
The 900EPC series of controllers and programmer/controllers are high stability, high accuracy, communicating
units designed to cope with a wide range of process needs and environments. The 16-bit 68070
microprocessor delivers the power of a PC; a number of ASICs significantly increase the I/O capability.
900 EPC Engineers Handbook
900 Series Digital Communications Handbook
Silicon Graphics OCTANE
General info OCTANE
Technical publications and library
Serial communications ports
General terminal interfaces
Wiring EPC900 - Silicon Graphics OCTANE
•
•
•
•
•
EPC900 controller, serial communications port wired to a standard RS232 connector
Silicon Graphics computer OCTANE serial communications port with DB-9 male serial port
connector
connect the back panel of the EPC900 with a standard RS232 cable (no null-modem cable)
connect the OCTANE with a converter from DB-9 to standard RS232
use serial communications port 2 of the OCTANE
Eurotherm controller to female connector at the back panel
EPC900
RS232 female connector
•
X1 TD
pin 3
•
X3 RD
pin 2
•
X5 GND
pin 7
converter cable RS232 to DB-9
RS232 male connector •
pin 2
•
pin 3
•
pin 7
-
DB-9 female connector
pin 3 TD
pin 2 RD
pin 5 GND
furnacemar345
EPC900 supervisory program
A supervisory program (author M. A. Estermann) is installed on the SGI Octane (IRIX 6.4). The program
utilises the Serial Communications Port 2, i.e. the DB-9 connector has to plugged into Port 2. The program
is self-explanatory and has a help section. The most common commands, such as for setting the temperature,
limiting setpoint rate, output power, and setpoint high are always offered. For safety reasons, Auto Tune and
changes of the configuration levels can only be performed from the EPC900 console. Start the supervisory
program from any unix-shell by typing epc900. The program epc900 displays a list of the most used
commands.
Fig. 69 & 70: Screen snap shots from a Silicon Graphics OCTANE
In situ diffraction at 900 ºC
The image was recorded with the mar345 imaging plate detector system and the furnacemar345 at 900ºC.
Swiss-Norwegian Beamline at the European Synchrotron Radiation Facility (ESRF), Grenoble, France,
Experiment 01-02-156, November 1998.
furnacemar345
ETH - Laboratory of Crystallography
> Introduction
> Access Statistics
> Annual Reports
> Equipment
> Links
> Location
> Open positions
> Research
> Seminars
> Software
> Staff
> Teaching
Laboratory of
Crystallography
Swiss Federal Institute of Technology Zürich
ETH Zentrum, Sonneggstr. 5, CH-8092 Zürich,
Switzerland
Phone: +41-1-6323769, FAX: +41-1-6321133, Email:
lfketh@kristall.erdw.ethz.ch
Head: Prof. Dr. Walter Steurer
Radiation safety
Quick Links
> CWW
> DGK
> ETH
> IUCr
> IZA
> SGK
> QDB
http://www.kristall.ethz.ch/LFK/ (1 of 2) [3.11.2000 08:47:49 Uhr]
Scientific Index (Bild der Wissenschaft
9/99):
The Top Ten in Crystal Research in
Austria, Germany and Switzerland.
ETH - Laboratory of Crystallography
© Laboratory of Crystallography (last updated: 30/Aug/99)
http://www.kristall.ethz.ch/LFK/ (2 of 2) [3.11.2000 08:47:49 Uhr]
Laboratory of Crystallography - Teaching
Teaching
The institute is responsible for teaching compulsory introductory courses in crystallography for
students of earth and materials sciences (ca. 50-60 students/course), and various specialised courses
at higher levels for chemistry, physics, earth and materials science students. The lectures aim to
impart the crystallographic-structural way of thinking as basis for professional activities in the
field of materials science. The focus is on real structure of crystals, structure-property correlations,
and methods for the investigation of single-crystalline and polycrystalline materials.
List of courses
06-009
06-101
Röntgenographische Pulvermethoden
Kahr, G., Stahel, A.
Kristallographie II
Steurer, W., Estermann,
M.
06-102
Kristallographisches Grundpraktikum
Schobinger, P,
Fehlmann, M.
06-104
Röntgenographische Einkristallmethoden
Gramlich, V., Fehlmann,
M.
06-110
Quasikristalle
Steurer, W.
06-113
Mineralogische Modelle des Erdmantels und des
Erdkerns.
Kunz, M.
06-130
Kristallographisches Seminar
Steurer, W.
06-131
Kristallographisches Seminar
Steurer, W.
06-134
06-801
09-062
Quasikristall-Seminar
Steurer, W.
Kristallographie I für Physiker
Grimmer, H.
Mineralogie-Petrographie I
Kunz, M., Schmid, R.,
Schreuer, J.
39-226
Kristallographie I
Steurer, W., Haibach, T.
40-009
Chemische Kristallographie II
Dobler, M., McCusker,
L.B.
40-029
Chemische Kristallographie III
Dobler, M., Gramlich, V.
40-039
Chemische Kristallographie I
Dobler, M., Gramlich, V.
http://www.kristall.ethz.ch/LFK/teaching/ (1 of 2) [3.11.2000 08:47:58 Uhr]
Laboratory of Crystallography - Teaching
© Laboratory of Crystallography (last updated: 11-Apr-99)
http://www.kristall.ethz.ch/LFK/teaching/ (2 of 2) [3.11.2000 08:47:58 Uhr]
Laboratory of Crystallography - Teaching: Course 06-023
Teaching:
Kristallographie II
(W. Steurer, M. Estermann)
Ziel:
Vermittlung kristallographischer Denkweisen und Untersuchungsmethoden als Grundlage
praxisbezogener (erd)materialwissenschaftlicher Tätigkeit.
Inhalt:
Realstruktur von Kristallen, Beziehungen zwischen Struktur und Eigenschaften, Methoden zur
Untersuchung von kristallinem und polykristallinem Material.
Skript:
Vorhanden.
Besonderes:
Die 3-stündige Veranstaltung, die auch von Materialwissenschaftlern gehört wird, beinhaltet
Vorlesungen und Übungen. Erdwissenschaftler nehmen zusätzlich an 2-stündigen erweiterten
Übungen teil, in denen an Hand von praxisbezogenen Fallbeispielen aus dem Erdmaterialbereich
kristallographische Untersuchungsmethoden geübt werden.
Voraussetzungen:
Mineralogie-Petrographie I oder Kristallographie I.
Umfang:
3 (+2) Stunden im WS.
Download:
●
Vorlesungsskript (PDF-Format)
●
Übungsaufgaben (PDF-Format)
Serie [1]
●
Musterlösungen der Übungsaufgaben (PDF-Format)
Serie [1]
© Laboratorium für Kristallographie (last updated: 2. November 2000, M. Estermann)
http://www.kristall.ethz.ch/LFK/teaching/course-06-023.html [3.11.2000 08:48:01 Uhr]
Übungsaufgaben zur Kristallographie II WS 2000/2001
Serie 1, Donnerstag 2. November 2000
Seite 1/4
Lösung
1) Frenkel-Defekte, allgemein
N
Anzahl Gitterplätze
NZ
Anzahl möglicher Zwischengitterplätze
EF
Energie um ein Atom von einem Gitterplatz auf einen Zwischengitterplatz
zu bringen (Frenkel-Defekt)
nF
Frenkel-Defekte
Innere EnergieU = nF EF
Anzahl
Konfigurationenen
nF
identische
Atome
aus
N
Gitterplätzen
herauszunehmen
❶
❷
❸
❹
❺
❻
❼
❽
❾
❿
….
1. Atom
N
Möglichkeiten
2. Atom
N-1
Möglichkeiten
3. Atom
N-2
Möglichkeiten
nF. Atom
N-nF+1
Möglichkeiten
total
M1 = N (N-1) (N-2) (N-3) … (N-nF+1) Möglichkeiten
Betrachten wir die Atome als identisch, dann wird eine Sequenz (1, 2, 3, …, nF)
nicht von der Sequenz (2, 3, …, nF, 1) zu unterscheiden sein.
Beispiel: N=10, nF=4, (❶, ❷, ❸, ❹) ist nicht von (❷, ❸, ❹, ❶) unterscheidbar, letzlich
betrachten wir also nur die Menge {(❶, ❷, ❸, ❹) } und nicht mehr die einzelnen
Permutationen.
Michael Estermann, Laboratorium für Kristallographie, ETH-Zentrum
Übungsassistenten: Antonio Cervellino (NOG59.1, Tel 2 3727), Thilo Scholpp (NOG58, Tel. 2 6130)
Mirsolav Kobas (NOG63, Tel. 2 3774), Stefano Ortelli (NOG63, Tel. 2 3774)
Lösungen:
http://www.kristall.ethz.ch/LFK/teaching/
Übungsaufgaben zur Kristallographie II WS 2000/2001
Serie 1, Donnerstag 2. November 2000
Seite 2/4
Lösung
Da es insgesamt nF! = nF (nF-1) (nF-2) … 1 Permutationen gibt, reduziert sich die
Anzahl der Konfigurationen um den Faktor nF! auf
W1 =
N ( N - 1)( N - 2)( N - nF + 1)
N!
=
nF !
( N - nF )!nF !
analog gilt W2 =
nF
=
N
NZ !
( NZ - nF )!nF !
Ê E ˆ
NZ
expÁ - F ˜
N
Ë 2 kBT ¯
S = kB log W1 + kB log W2 , Näherung von Stirling für grosse N: log N! @ N log N
log W1 = log
N!
@ N log N - ( N - nF ) log( N - nF ) - nF log nF
( N - nF )!nF !
log W2 = log
NZ !
@ N log N Z - ( N Z - nF ) log( N Z - nF ) - nF log nF
( NZ - nF )!nF ! Z
freie Energie F = U - TS soll als Funktion von nF minimal sein, d.h.
Ê ∂F ˆ
Ê ∂U ˆ
Ê ∂S ˆ
Á
˜ =Á
˜ - TÁ
˜ =0
Ë ∂nF ¯ T Ë ∂nF ¯ T
Ë ∂nF ¯ T
È Ê N - nF ˆ
Ê N Z - nF ˆ ˘
Ê ∂S ˆ
Á
˜ = kB ÍlogÁ
˜ + logÁ
˜˙
Ë ∂nF ¯
Ë nF ¯ ˚
Î Ë nF ¯
Ê ∂U ˆ
Á
˜ = EF ,
Ë ∂nF ¯
Ê ( N - nF )( N Z - nF ) ˆ
Ê NN Z ˆ
EF = kBT logÁ
˜ @ kBT logÁ 2 ˜ ; nF << N , N Z
2
nF
Ë nF ¯
Ë
¯
Ê E ˆ
nF = NN Z expÁ - F ˜
Ë 2 kBT ¯
Michael Estermann, Laboratorium für Kristallographie, ETH-Zentrum
Übungsassistenten: Antonio Cervellino (NOG59.1, Tel 2 3727), Thilo Scholpp (NOG58, Tel. 2 6130)
Mirsolav Kobas (NOG63, Tel. 2 3774), Stefano Ortelli (NOG63, Tel. 2 3774)
Lösungen:
http://www.kristall.ethz.ch/LFK/teaching/
Übungsaufgaben zur Kristallographie II WS 2000/2001
Serie 1, Donnerstag 2. November 2000
Seite 3/4
Lösung
durch dividieren mit N kann dieser Audruck auf Konzentrationen umgerechnet
werden
nF
=
N
Ê E ˆ
NZ
expÁ - F ˜ .
N
Ë 2 kBT ¯
Siehe die Abbildung 1.1-5 im Skript Seite 7, Einheit der x-Achse 1 / T , Einheit der yÊn ˆ
Achse lnÁ F ˜ ergibt dann einen linearen Verlauf mit
ËN¯
Ê NZ ˆ
E
Ên ˆ
- F
lnÁ F ˜ = lnÁ
˜
ËN¯
Ë N ¯ 2 kB T .
y = a + bx
Beim Abkühlen werden die Punktdefekte ab einer
gewissen
Temperatur
eingefroren, d.h. es kann keine Diffusion mehr stattfinden, und damit auch kein
equilibrieren der Defekte mehr.
2) Frenkel-Defekte, Silberchlorid AgCl
4 Ag+ Ionen pro Einheitszelle
4 Cl- Ionen pro Einheitszelle
8 mögliche
Zwischengitterplätze
(in den
Zentren
der
Achtelswürfel)
pro
Einheitszelle
Für die Berechnung der Konzentrationen können wir uns auf die Einheitszelle
beschränken, da die Konzentration für eine Einheitszelle die gleiche wie für den
ganzen Kristall ist (Translationssymmetrie).
kb = 1.38 E - 23 Joule / K , 1eV = 1.6 E - 19 Joule
nF
= 8 E - 10
N
Michael Estermann, Laboratorium für Kristallographie, ETH-Zentrum
Übungsassistenten: Antonio Cervellino (NOG59.1, Tel 2 3727), Thilo Scholpp (NOG58, Tel. 2 6130)
Mirsolav Kobas (NOG63, Tel. 2 3774), Stefano Ortelli (NOG63, Tel. 2 3774)
Lösungen:
http://www.kristall.ethz.ch/LFK/teaching/
Übungsaufgaben zur Kristallographie II WS 2000/2001
Serie 1, Donnerstag 2. November 2000
Seite 4/4
Lösung
AgCl, F 4/m -3 2/m, a=5.549Å, mit Zwischengitterplätzen
Michael Estermann, Laboratorium für Kristallographie, ETH-Zentrum
Übungsassistenten: Antonio Cervellino (NOG59.1, Tel 2 3727), Thilo Scholpp (NOG58, Tel. 2 6130)
Mirsolav Kobas (NOG63, Tel. 2 3774), Stefano Ortelli (NOG63, Tel. 2 3774)
Lösungen:
http://www.kristall.ethz.ch/LFK/teaching/
marresearch: Home Page
Welcome to Our Home Page
Protein and small molecule crystallographers around the globe know one word for
unsurpassed data quality and reliability of X-ray equipment: mar.
Please come in and get more information about our products:
❍
mar345 Image Plate Detector
❍
marCCD CCD Detector
❍
marCAM X-ray Beam Monitor
❍
Osmic Confocal Max-Flux® Optics
❍
mar Focussing Mirrors
Check out the latest news.
Aug 24, 2000: marHKL and marXDS data processing
packages now available! marFLM updated (version 2.0)!
Our staff members will be glad to help you with more detailed information by email,
phone or FAX.
© 2000 by X-ray Research GmbH
http://www.marresearch.com/ [3.11.2000 08:48:26 Uhr]
1st_page
Welcome on our Web site
Your expert in
thermal devices and
temperature measurement
English - Deutsch
This site is optimized for a
600 x 800 resolution.
Sales International
THERMOCOAX
40 Bld Henri Sellier
92156 SURESNES Cedex - France
Tel: +33 1 41 38 80 50 - Fax: +33 1 41 38 80 58
e-mail : info@thermocoax.fr
http://www.thermocoax.fr/ [3.11.2000 08:48:54 Uhr]
Navigation : best with
NETSCAPE or EXPLORER