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X-RAY SPECTROMETRY

X-Ray Spectrom. 28, 396–398 (1999)

High-Resolution X-Ray Spectrometry Using


Iridium–Gold Phase Transition Thermometers†

J. Höhne,* M. Altmann, G. Angloher, P. Hettl, J. Jochum, T. Nüssle, S. Pfnür, J. Schnagl,


M. L. Sarsa, S. Wänninger and F. v. Feilitzsch
Technische Universität München, Physik Department E15, 85748 Garching, Germany

Cryogenic detectors based on iridium–gold phase transition thermometers are being developed for various
applications in astroparticle physics, aiming at high energy resolution, low energy threshold and moderate
count rates. A microcalorimeter with an energy resolution of 15.5 eV (FWHM) for the 55 Mn Ka1 x-ray line
for tentative use in an analytical x-ray system (e.g. SEM, TRFA) is presented. Copyright  1999 John Wiley
& Sons, Ltd.

INTRODUCTION to lower temperatures, this detector concept is most sen-


sitive at operating temperatures below 100 mK. These
temperatures are reached with standard 3 He/4 He dilution
Cryogenic detectors with excellent energy resolution and or adiabatic demagnetization refrigerators.
low energy threshold far beyond the level of semicon-
ducting detectors open up a variety of new applications
in physics, including the search for dark matter in the SUPERCONDUCTING PHASE TRANSITION
universe,2 neutrino physics3 and IR, UV and x-ray astro- THERMOMETERS (SPTs)
physics.4 Interdisciplinary fields where cryogenic detectors
have already shown promising results are the detection of Our phase transition thermometers are thin superconduct-
biomolecules5 and x-ray spectrometry at synchrotron beam ing films (ca 150 nm) with areas ranging from µm2 to
lines6 and in scanning electron microscopes (SEMs).7 For cm2 depending on the application. The film is stabilized
both astrophysical and analytical use we started the devel- in the region between the normal conducting and the
opment of high-resolution microcalorimeters based on irid- superconducting state, where the resistance shows a strong
ium–gold phase transition thermometers for use in a mobile dependence on temperature. Fig. 1 shows an example of a
detector system. transition curve of an iridium–gold proximity effect phase
transition thermometer at Tc D 39.5 mK. The width of the
transition region is about 2 mK. A typical temperature rise
MICROCALORIMETER due to absorption of a 6 keV x-ray is in the µK range.
The readout arrangement is shown in the inset of
Fig. 1. A constant current I0 is passed through both the
Our microcalorimeters consist of an absorber, a ther- thermometer RT and a shunt resistor RS placed in parallel.
mometer and a coupling to a heat sink. An incoming par- A resistance change of the thermometer due to the heating
ticle or x-ray photon deposits an energy E in the absorber. from energy deposition in the absorber causes a change
The corresponding temperature rise T is then measured in current in the SQUID input coil. Assuming linearity
using an iridium–gold superconducting phase transition of the transition curve and a calorimetric operating mode
thermometer (SPT). After the particle interaction, the sys- of the detector, the signal height is directly proportional
tem relaxes to its operating temperature via the coupling to the deposited energy.
to the heat sink. In a simple model the temperature rise Our SPTs, consisting of a bilayer of iridium and gold,
T of the thermometer can be described as T D E/C, make use of the proximity effect. The critical temperature
where C is the heat capacity of the thermometer–absorber of the iridium film (bulk Tc D 112 mK) is reduced
system. Since heat capacities become smaller on going by the gold film depending on the film thicknesses of
both films.8 This bilayer technique permits us to fabricate
* Correspondence to: J. Höhne, CSP Crgogenic Spectrometers Gmb4,
thermometers with operating temperatures between 20 and
Bahnhofstr. 18A, D-857371 smaning, Germany. 112 mK. The reproducibility of the transition temperature
E-mail address: jens.hoehne@csp-munich.com is about š5 mK above 40 mK. Fabrication is done under
† Presented at the European Conference on EDXRS, Bologna, Italy, UHV conditions in a dedicated system.
7–12 June 1998.
Contract/grant sponsor: Deutsche Forschungsgemeimschaft.
Contract/grant sponsor: Sonderforschungsbereich Astro/Teilchen-
physik; Contract/grant number: SFB 375. EXPERIMENTAL
Contract/grant sponsor: European Community; Contract/grant num-
ber: ERB; Contract/grant number: CHRX CT93-0341 ERB FMRX
CT98-0167. Figure 2 shows the experimental setup for a microcalori-
Contract/grant sponsor: Beschleuniger-Laboratorium Garching. meter consisting of a gold absorber (250 ð 250 ð 1 µm3 )

CCC 0049–8246/99/050396–03 $17.50 Received 13 October 1998


Copyright  1999 John Wiley & Sons, Ltd. Accepted 4 June 1999
HIGH-RESOLUTION XRS USING Ir–Au PHASE TRANSITION THERMOMETERS 397

The gold absorber was irradiated through a 100 µm


diameter copper collimator with a rate of about 50 cps.
The SQUID signal was recorded using a 12-bit transient
recorder and a 50 kHz anti-aliasing filter.

RESULTS

Since the absorption efficiency of our gold absorber is


about 50% for 6 keV x-rays, two different classes of
events were expected: absorptions in the gold absorber
or in the thermometer and absorptions in the underly-
ing sapphire substrate. For further processing the signals
were fitted using one exponential rise time and one expo-
nential decay time. The two classes of events could be
Figure 1. Transition curve for an iridium–gold phase transition distinguished by analyzing the decay time of the signals:
thermometer. Inset: readout circuit for our SPTs.
absorptions in the gold absorber are described best with
a rise time of 30 µs and a decay time of 630 µs, whereas
absorptions directly underneath the thermometer have a
much longer decay time and can be seen at a much lower
pulse height in the spectrum. Figure 3 shows the spectrum
of a 55 Fe source measured with our microcalorimeter. The
55
Mn K˛ line complex was fitted using two Gaussians of
equal width, fixed intensity ratio and fixed relative energy
difference. The 55 Mn K˛1 line could be resolved with an
energy resolution of 15.5 eV (FWHM) (Fig. 3, inset). Two
features in the structures of the K˛ and Kˇ peaks should
be noticed: there is a small peak with about one tenth of
the intensity immediately below the K˛ and Kˇ peaks,
which might be due to absorption of x-rays in the Ir–Au
thermometer since the ratio of thicknesses of the gold
absorber and the Ir–Au thermometer is in this range. Just
below these lines there is another small peak of unknown
origin.
Our energy resolution is still worse than the theoretical
limit owing to thermodynamic fluctuations for this kind of
detector. One major contribution was the SQUID noise,
being 20 pA Hz 1/2 . The energy threshold of this detector
was measured to be below 30 eV.
Figure 2. Experimental setup for our microcalorimeter.

and an iridium–gold thermometer (1 mm ð 1 mm ð


150 nm). The sapphire substrate underneath served as a
heat sink, being coupled to the thermometer via its sur-
face. Its heat capacity can be neglected for the evaluation
of T since its coupling to the thermometer–absorber
system is slow compared with the heat distribution in
this system. Electrical contact to the thermometer was
made via evaporated aluminum leads from where contact
was made to the SQUID circuit using 25 µm diame-
ter wedge bonded aluminum wires. Detector fabrication
was done in three major steps: evaporation of the irid-
ium–gold thermometer, sputtering of the gold absorber
and evaporation of the aluminum leads. Device patterning
processes were done via photolithography and ion beam
etching.
The readout circuit consisted of a 6 m shunt resis-
tor and a single-stage HYPRES SQUID system. The
microcalorimeter and the SQUID were mounted in a
3 Figure 3. Spectrum of 55 Mn measured with our microcalorime-
He/4 He dilution refrigerator. The microcalorimeter was ter. To the left of the main K˛ peak a satellite peak can be seen
operated at 40 mK with a temperature stability of better which might be due to absorptions in the thermometer. Further
than 100 µK. left an even smaller satellite of unknown origin can be seen.

Copyright  1999 John Wiley & Sons, Ltd. X-Ray Spectrom. 28, 396–398 (1999)
398 J. HÖHNE ET AL.

CONCLUSION applications, where there is a need for high-energy reso-


lution in the energy region below 2 keV to identify low-Z
elements, cryogenic detectors will bring major improve-
With a cryogenic microcalorimeter with an active area of ments in sensitivity.
250 ð 2502 µm and an absorption efficiency of 50% for
6 keV x-rays, an excellent energy resolution of 15.5 eV
(FWHM) for the 55 Mn K˛1 x-ray line could be shown. Acknowledgements
The use of a SQUID system with much lower noise could
further increase the sensitivity of our detector. Techniques We gratefully acknowledge the support of the Deutsche Forschungsge-
for shortening signal lengths are being developed having meinschaft (DFG), the Sonderforschungsbereich Astro/Teilchenphysik
as a goal count rates in the kHz region. A mobile detec- (SFB 375), the European Community under Grants ERB CHRX CT93-
0341 and ERB FMRX CT98-0167 and the Beschleuniger-Laboratorium
tor system is being constructed and will be available for Garching. We are indebted to F. Pröbst and W. Seidel of the Max-
use in various experiments in the field of x-ray spectrome- Planck-Insitut für Physik in Munich for many helpful discussions and
try. Especially for x-ray spectrometry for material analysis practical support.

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Copyright  1999 John Wiley & Sons, Ltd. X-Ray Spectrom. 28, 396–398 (1999)

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