PIXE-TES results from Jyväskylä

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LARGE AREA TRANSITION-EDGE SENSOR

ARRAY FOR PARTICLE INDUCED X-RAY

EMISSION SPECTROSCOPY

M Palosaari 1 , K Kinnunen 1 , I Maasilta 1 , C Reintsema 2 , D Schmidt 2 , J Fowler 2 , R

Doriese 2 , J Ullom 2 , M Käyhkö 1 , J Julin 1 , Mikko Laitinen 1 , T Sajavaara 1

1 Department of Physics, University of Jyväskylä, P.O. Box 35, Jyväskylä 40014, Finland

2 National Institute of Standards and Technology, Boulder CO 80305, United States email: mikko.i.laitinen@jyu.fi

INTRODUCTION to TES

Superconducting Transition-Edge Sensor

Transition-Edge Sensor (TES)

 TES as a calorimeter

– Measures the energy of incident radiation

Schematics of a calorimeter

Typical pulse from a calorimeter

TES Operation

Operates between superconducting and normal state

Extremely sensitive R(T)

Excellent energy resolution

Wide energy range

Detects radiation, in our case X-rays

Particles also possible

Normal state

Superconducting state

Typical transition of a TES

TES basics

TES thin film device is made of normal metal superconducting metal bilayer.

The absorber details depend on the desired energy range.

TESs are usually fabricated on thin SiN membranes to limit the thermal conductivity G.

Photograph of a 256 pixel

TES array made in VTT, Finland.

In typical TES array, all pixels different

-> automated calibration essential

PIXETES SETUP IN JYVÄSKYLÄ

PIXE-TES Setup in Jyväskylä

Details inside the instrument

~15 mm

~300 m m

Jyväskylä TES specifications

160 pixels from NIST, upgradable to 256 (from VTT)

Total area with 160 pixels ~16 mm 2

Single pixel count rate limited to <20 Hz, typical value 10 Hz

2 m m thick Bi absorber with Mo/Cu superconducting juction

Detection efficiencies with 100 um of Be:

80 % at 5 keV,

20 % at 10 keV,

5 % at 30 keV

Low energies limited by

MeV particle absorber, probably not needed

PIXE-TES MEASUREMENTS

From a single pixel to many…

PIXETES results from Jyväskylä

Roughly one year ago: 12 pixels

Mn Kα from Fe-55 source

Best pixel

Instrumental resolution for the best pixel with 55 Fe source was 3.06 eV

PIXETES results from Jyväskylä

Now: 160 pixels…

• But, Computer interface and I/O cards cannot handle all pixels simultaneously

• I/O card + PC update coming from NIST to finally secure the function of all 256 possible channels, simultaneously.

This month: data with Fe-55 source

Resolution around 5 eV for combined 40 pixels,

Improvement seen by better data analysis

PIXETES results from Jyväskylä

SRM-611, trace elements in glass

All TES data shown was analyzed last week, 1 eV / bin

Analysis resolution for all of these plots ~10 eV

PIXETES results from Jyväskylä

SRM-611, trace elements in glass

PIXETES results from Jyväskylä

SRM-611, trace elements in glass

Differences between pixels which are not only statistics

PIXETES results from Jyväskylä

SRM-1157, speciality tool steel

No Si escape peak

Bi escape peaks

Single measurement, wide energy range

PIXETES results from Jyväskylä

SRM-1157, speciality tool steel

V, Cr, Mn, Fe separated

In the Near Future

Read-out upgraded to full scale.

Modification of PIXE setup to be able to measure samples in atmosphere.

Study art samples in a project that just started

X-ray measurements with our own detector array fabricated by VTT.

Study the satellite peaks with different ions and energies.

->> Chemical information from wide energy/elemental range ???

Conclusions

Instrumental resolution of 3 eV demonstrated

Combined pixel resolution of ~5 eV looks realistic

Wide energy scale (“0” to tens of keV)

Reasonable count rates available

(10 Hz/pixel, 256 pixels)

Active detector area about 16 mm 2

No liquid He needed for ADR cryo cooler

Largish instrument: ~5 cm sample-to-detector

Data handling and analysis: automation necessary

Is the chemical information achievable, after all ?

Acknowledgements

t

38. July, 2016, in Jyväskylä, Finland

Pixel calibration

Single pixel shows Si peaks nicely but without good calibration, sum spectrum useless

No/bad calibration regime

Sample: SRM-611 good calibration

TES-PIXE data calibration

Raw pulse height data where sample was changed.

Sample 1 Sample 2

Substrate was Si for both samples

Measurement time/duration

TES-PIXE data

Making selection to single (example) emission line

• Before liner fit

Straight line to guide the eye

TES-PIXE data

• After linear fit

Si

Straight line to guide the eye

Si

Nitride hits

PIXE Mn vs.

55

Fe

Mn Kα from Fe55 source same pixel

What is the origin of the hump?

Detector performance: PIXE Mn vs. 55 Fe source

Instrumental resolution for the best pixel with 55 Fe source was 3.06 eV.

For 2 MeV protons and Mn sample resolution was 4.20 eV.

M. Palosaari et. al J. Low Temp.

DOI 201310.1007/s10909-013-1004-5

PIXE applications

Traditional PIXE applications

– Archaeology

– Geology

– Filters in industry

– Old paintings

With better detectors one could see the chemical environment of the sample.

Rev. Sci. Instrum. 78, 073105 (2007)

J. Hasegawa et. al

TES vs. SDD

Impurities in the Cu sample resolved better with TES detector

Stainless steel example

PIXE Mn vs.

55

Fe

Mn Kα from Fe55 source same pixel

FWHM broadens less than 1eV.

TES vs. SDD

TES circuit diagram

Example: Thin film with high mass element

Atomic layer deposited Ru film on HF cleaned Si

Scattered beam, 35 Cl, used for Ru deph profile

Monte Carlo simulations needed for getting reliable values for light impurities at the middle of the film

Si

Ru

SiO

2

Poor E resolution

Low energy heavy ion ERDA – See posters!

Example

: Diamond-like carbon films

2.3 µm thick diamond-like-carbon film on Si, measured with 9 MeV 35 Cl

All isotopes can be determined for light masses

Light elements can be well quantified (N content 0.05

± 0.02 at.%)

Low energy heavy ion ERDA

ALD 8.6 nm Al

2

O

3

/Si

Atomic layer deposited Al

2

O

3 film on silicon (Prof. Ritala, U. of Helsinki)

Density of 2.9 g/cm 3 and thickness of 8.6 nm determined with XRR (Ritala)

Elemental concentrations in the film bulk as determined with TOF ERDA are O 60 ± 3 at.%, Al 35 ± 2 at.%, H 4 ± 1 at.%. and C 0.5

± 0.2 at.%

10 nm CN

x

on silicon

TOF-ERDA results from sputter deposited 10 nm thick CN x hard coating on

Si. Measured with 6 MeV 35 Cl beam and extreme glancing angle of 3 °

A density of 2.0 g/cm 3 was used in converting areal densities to nm

Effect of stripper gas pressure

13.6 MeV 63 Cu 7+ CaPO (hydroxyapatite)

Gas ionization detector

Thin (~100 nm) SiN window

Electrons for T2 timing signal emitted from the membrane

Future improvements: Gas ionization detector

TOFE results from ETH Zürich

Incident ion 12 MeV 127 I and borosilicate glass target

Nucl. Instr. and Meth. B 248 (2006) 155-162

200 nm thick SiN membrane from Aalto

University, Finland, on 100 mm wafer

Gas ionization detector to replace

Si-energy detector

Why try to fix a well working system?

Greatly improved energy resolution for low energy heavy ions → heavier masses can be resolved

Gas detector is 1D position sensitive by nature → possibility for kinematic correction and therefore larger solid angles possible

Gas detector does not suffer from ion bombardment

Recoil ranges in isobutane

10.2 MeV 79 Br 8.5 MeV 35 Cl

Gas ionization detector develoment – See posters!

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