Query: X-ray microanalysis with transition edge sensors

Candidate papers:

abstract: In current experiments and technical applications the demand for new and advanced concepts for the detection of radiation and particle is increasing. Low temperature detectors such as Transition Edge Sensors (TES) have been developed as ultrahigh resolution radiation and particle detectors offering advantages in manifold applications. They were designed primarily for astrophysical experiments such as the dark matter search. In material analysis they have been introduced to revolutionize mass spectroscopy of biological molecules and Energy Dispersive X ray Spectroscopy (EDS) EDS is the determination of the elemental constitution of samples in scanning electron microscopes (SEMs) with characteristic X ray radiation excited by the electron beam. The use of TES detectors improves the EDS analysis of small volumes such as particles or thin layers. This is especially important for the semiconductor industry because of the continual shrinking of device size. Current structure sizes of 65 nm are already demanding new approaches in analytic methodology. In this thesis the introduction and improvement of a fully automated TES detector system in the industrial environment of a semiconductor failure analysis lab is described. This system, marketed under the trade name of 'Polaris' by the manufacturer, is based on a mechanical pulse tube cooler in combination with an adiabatic demagnetization refrigerator (ADR) for cooling the TES detector to its operating temperature. Several large improvements had to be made to the system during the total system integration. The energy resolution could be improved significantly thus enabling a better peak separation and the measurement of chemical shifts. Due to the small area of TES detectors compared with conventional EDS detectors the efficiency of the system proved to be too low for everyday use. A polycapillary X ray lens was added to the system in order to solve this problem. The application of the lens, however, brought its own problems and appropriate and practicable adjustment methods had to be developed. With the lens the count rate could be increased by more than two orders of magnitude. In order to identify X ray peaks correctly, an accurate energy calibration correcting the nonlinear behavior of the TES detector is absolutely necessary. A new approach to the linearization of TES has been developed and enables a calibration accuracy for TES spectra fulfilling all the needs of material analysis. This linearization method is also easy to handle for the future user of the system. With the achieved degree of automation and extended analysis possibilities such as a superior peak separation, a lower element detection limit and easy peak identification, TES EDS spectrometers hold the potential to replace conventional Si(Li) detectors in the near future.
author_names: C Hollerith
title: X Ray Microanalysis with Transition Edge Sensors
year: 2006

abstract: We have developed superconducting calorimeters using transition edge sensors (TESs) for industrial X ray microanalysis. To obtain high count rate, high reliability, and high energy resolution, a large format array of the sensors and an integration of a TES calorimeter and a SQUID amplifier are required. A novel calorimeter fabrication process has been established, in which a micro machining technology using a silicon on insulator wafer was applied. A 4 pixel Au/Ti TESs calorimeter was fabricated using this process. SQUID amplifiers suitable for the calorimeter have also been designed and fabricated. It is expected to achieve a count rate per pixel of 7.1 kcps. The expected energy resolution including the SQUID contribution was estimated at 17 21 eV. It has been confirmed that the SQUID contribution for the current noise of our calorimeter can almost be ignored. It has also been confirmed that an array of 14 or more pixel are required that to achieve an effective count rate of more than 100 kcps.
author_names: Toshimitsu Morooka

Keiichi Tanaka

Satoshi Nakayama

Atsushi Nagata

Kazuo Chinone

Masahiro Ukibe

Fuminori Hirayama

Masataka Ohkubo

Masao Koyanagi

Taku Mizuki

Tomotaka Hikosaka

Ushio Kawabe

Toshio Nemoto
title: Fabrication and characterization of superconducting X ray calorimeters with transition edge sensors
year: 2001

abstract: We have developed high performance X ray microcalorimeters based on superconducting transition edge sensors. These superconducting detectors, which are cooled by a compact adiabatic demagnetization refrigerator mounted on a scanning electron microscope, provide significant new capabilities for X ray microanalysis. The performance characteristics of these detectors are nearly ideal for many applications in X ray microanalysis, attaining an energy resolution of 3 4 eV at a counting rate of 500 s/sup and an effective collection area of 4 mm/sup 2/ The excellent energy resolution enables measurements of chemical shifts in X ray spectra caused by changes in electron binding energy due to chemical bonding. Another important application of these detectors is analysis of contaminant particles and defects for the semiconductor industry. We present data demonstrating the analysis of particles on Si wafers, including 0.3 /spl mu/m tungsten particles and 0.1 /spl mu/m alumina particles.
author_names: G C Hilton

David A Wollman

Kent D Irwin

L L Dulcie

Norman F Bergren

John M Martinis
title: Superconducting transition edge microcalorimeters for X ray microanalysis
venue: IEEE Transactions on Applied Superconductivity
year: 1999

abstract: The combination of high energy resolution spectrometers with high spatial resolution scanning electron microscopes provides a powerful tool for material analysis. X ray spectrometers based on superconducting transition edge sensors combine the advantages of commonly used energy and wavelength dispersive spectrometers, i.e. a fast spectrum acquisition and a high energy resolution over a wide energy range. While the energies of the characteristic lines present in a spectrum contain the qualitative composition of the analyzed material, the corresponding mass fractions can be obtained from their intensities. In this work first quantitative measurements performed with the POLARIS spectrometer system are presented.
author_names: C Isaila

F v Feilitzsch

J Hohne

C Hollerith

K Phelan

B Simmnacher

R Weiland

Doreen Wernicke
title: X ray microanalysis with microcalorimeters
year: 2006

abstract: Cryogenic microcalorimeter X ray detectors based on superconducting transition edge sensors (TES) offer up to a roughly 60 fold improvement in energy resolution as compared with conventional detectors for energy dispersive spectrometry. The best energy resolutions demonstrated to date are 2.0 eV full width at half maximum (FWHM) at 1.5 keV (Al K) and 2.4 eV FWHM at 5.9 keV (Mn K) The energy resolution of state of the art microcalorimeter detectors rivals the resolution of spectrometers for wavelength dispersive spectrometry (WDS) yet microcalorimeters offer all the advantages of EDS detectors ease of use, long term stability, and the ability to quickly provide qualitative as well as quantitative chemical analysis.
author_names: Robin Cantor

Mark P Croce

George J Havrilla

Matthew H Carpenter

Kathryn G Mcintosh

Ad Hall

Stosh Anthony Kozimor

Hideo Naito

Michael William Rabin

Daniel Schmidt

Daniel S Swetz

J N Ullom
title: Oxidation State Determination from Chemical Shift Measurements using a Cryogen Free Microcalorimeter X Ray Spectrometer on an SEM
venue: Microscopy and Microanalysis
year: 2016

abstract: Improving x ray spectral energy resolution in conventional scanning electron microscopes (SEM) can be achieved by using microcalorimeters. Although improvements to microcalorimeter design are still being studied, several research groups have developed fabrication techniques that result in consistent devices [1] Here we discuss the fabrication techniques we use to make microcalorimeters using superconducting transition edge sensors (TES) as thermometers.
author_names: K L Nelms

D Liu

Dan Mccammon

Lindsay Rocks

Wilton T Sanders

Ping Tan

John E Vaillancourt
title: Transition Edge Sensor Fabrication
venue: Microscopy and Microanalysis
year: 2002

abstract: The development of time domain SQUID multiplexers enables the integration of superconducting transition edge sensors (TES) into arrays with thousands of elements while maintaining a manageable number of readout channels. The applications for detector arrays range from highcount rate x ray microanalysis systems to focal plane arrays for imaging at wavelengths from the submillimeter to gamma ray. We present results from recent measurements of a twodimensional TES array. The measurements focus on the heatpulse response of a TES measured with multiplexed read out and show no degradation of energy resolution with eight detectors multiplexed. We describe the system architecture, including the cryogenic SQUID amplifier chain, the analog interface electronics, and the digital feedback electronics.
author_names: Carl D Reintsema

J A Beall

Steven W Deiker

William Bertrand Doriese

G C Hilton

Kent D Irwin

Sae Woo Nam

L R Vale

J N Ullom

Y Xu

Joern Beyer

Martin E Huber
title: A Time Domain SQUID Multiplexer System for Read Out of Superconducting Transition Edge Sensor Arrays
year: 2003

abstract: We have been developing cryogenic detectors for astro particle physics applications including search for Dark Matter, neutrino physics and x ray astronomy. Most recently we started the development of high resolution x ray detectors based on superconducting tunnel junctions and superconducting phase transition thermometers/transition edge sensors for microanalysis applications. Both types of sensors are being investigated as well as the cryogenic setup for applications on a scanning electron microscope.
author_names: Jens Hoehne

Michael Altmann

Godehard Angloher

Matthias Buehler

F v Feilitzsch

Torsten Frank

Paul Hettl

Theo Hertrich

Josef Jochum

Tobias Nuessle

Stefan Pfnuer

Johann Schnagl

Stefanie Waenninger
title: Cryogenic microcalorimeters and tunnel junctions for high resolution energy dispersive x ray spectrometry
venue: Other Conferences
year: 1999

abstract: Low temperature microcalorimeter x ray detectors based on transition edge sensors (TESs) integrated with scanning electron microscopes (SEMs) can combine the resolution of wavelength dispersive spectroscopy (WDS) instruments with a broad energy range and efficiency comparable to energydispersive spectroscopy (EDS) instruments [1] With recent developments in microwave multiplexing of hundreds of TES pixels [2] and the availability of lower cost, reliable dilution refrigerator cryostats, it is now becoming practical to measure chemical speciation in the SEM via subtle peak shifts in the emission spectrum [3] Microcalorimeters can also improve sensitivity for elemental composition. Due to the Bremsstrahlung background and ~100 eV energy resolution of the Si drift detector (SDD) standard EDS has detection limits of order 0.1 wt% while WDS has of order 0.01 wt% detection limit owing to its higher resolution ~5 15 eV FWHM) [4,5] With even higher energy resolution than typical WDS instruments, microcalorimeters have the potential to further improve detection limits especially when spectral interferences are present.
author_names: Matthew H Carpenter

Mark P Croce

Chandler M Smith

K E Koehler
title: High Resolution Chemical state Mapping and Analysis for Nuclear Safeguards with Microcalorimeter SEM EDS
venue: Microscopy and Microanalysis
year: 2020

abstract: Thermal Equilibrium Calorimeters An Introduction. Semiconductor Thermistors. Transition Edge Sensors. Metallic Magnetic Calorimeters. Quantum Giaever Detectors. Electron Probe Microanalysis. Dark Matter Direct Detection. X Ray Astronomy and Astrophysics. Optical/UV Astrophysics Applications of Cryogenic Detectors Beta Decay Experiments. Heavy Ion Physics. Index.
author_names: Christian Enss
title: Cryogenic particle detection
year: 2005