High-resolution microcalorimeter energy-dispersive spectrometer for x-ray microanalysis and particle analysis

Wollman, David A.; Hilton, G. C.; Irwin, K. D.; Dulcie, L L.; Bergren, Norman F.; Newbury, Dale E.; Woo, Keung‐Shan; Liu, Benjamin Y. H.; Diebold, Alain C.; Martinis, John M.

doi:10.1063/1.56867

Cited by 7 publications

(4 citation statements)

References 2 publications

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“…As a result, especially high energy satellites may make determination of chemical bonding states, as proposed in [15], doubtful even by WDXS and microcalorimeter EDS. If, it will work only with pure substances, or when a standard extremely close in composition to the unknown can be found.…”

Section: Mass Absorption Coef®cientsmentioning

confidence: 97%

Low Voltage EDXS and Elements of the First Transition Series

Poelt

2000

Mikrochim Acta

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Use of the L-lines in connection with the elements of the ®rst transition series entails a lot of problems. The corresponding X-ray peaks are composed of contributions of a group of several lines. Because of the incompletely ®lled 3d-shells, the intensity ratios of the lines and thus the overall peak shapes of the X-ray peaks vary with the type of bonding of the respective element. A special problem posed is that of high energy satellites, which could be strongly absorbed even by use of low electron energies. Crucial for reliable quantitative results is a careful choice of reference spectra for peak deconvolution and peak ®t.Nevertheless, with appropriate care results with an accuracy of around 10 ± 15 wt7 relative may be obtained. This has been tested by performing quantitative analysis on a haematite and magnetite specimen by use of the Fe-L lines.Key words: SEM; low voltage; X-ray analysis; elements of the ®rst transition series.Low voltage scanning electron microscopy (E 0 7 keV) offers both high spatial resolution and a greatly reduced X-ray generation depth. This enables the analysis of particles and phases with diameters in the submicrometer range. Although thin ®lm analysis generally can be performed with great success by use of higher energies and conventional thin ®lm analysis programs [1], low voltages may be preferable in case of non¯at specimens or specimens with several common elements in the ®lm and the substrate.While with the advent of ®eld emission scanning electron microscopy imaging at low voltages has become commonplace, use of low voltages in X-ray analysis is still rather rare. Whereas its advantages have been recognized early [2 ± 6], also its limitations have always been emphasized, and quantitative low voltage X-ray analysis is still regarded as applicable in special cases only [7,8]. Special ProblemsQuantitative analysis with the L-lines of the elements of the ®rst transition series has always been regarded as extremely dif®cult. The corresponding peaks are composed of the contributions of the L , L , L 1 and L and additional non-diagram lines. Because of the incompletely ®lled 3d-shells, the intensities of the L 1 and L lines are no longer negligible, but can be as high as that of the L and L lines. Measurable L 1 and L peaks entail an overlap with the L , -peak in case of energy dispersive spectra (see Fig. 1) and generally more frequent peak overlaps with the X-ray peaks of other elements.Other problems are caused by bonding effects. The occupation number of the 3d-shell and thus the intensity ratios of the lines and the overall peak shapes of the EDXS peaks will vary with the bonding of the respective element. As a consequence, simple peak integration could give wrong results in case of different type of bonding of the speci®c element in the unknown and the standard. Additionally, the choice of an appropriate standard is also important for the recording of reference spectra for peak deconvolution. This will require some preknowledge about the specimen. In fact, the errors caused by ...

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Section: Mass Absorption Coef®cientsmentioning

confidence: 97%

Low Voltage EDXS and Elements of the First Transition Series

Poelt

2000

Mikrochim Acta

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“…A difficult microanalysis challenge facing the semiconductor industry is the chemical identification of the small particles and defects that occur in the, manufacture of integrated circuits [12]. As circuit dimensions continue to shrink, it be- comes impossible to perform this task efficiently with either EDS or WDS systems.…”

Section: B Particle Identijicationmentioning

confidence: 99%

Superconducting transition-edge microcalorimeters for X-ray microanalysis

Hilton¹,

Wollman²,

Irwin³

et al. 1999

IEEE Trans. Appl. Supercond.

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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-' and an effective collection area of 4 m m ' . 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 pm tungsten particles and 0.1 pm alumina particles.

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“…The range of problems that can be solved with the NIST microcalorimeter EDS is demonstrated in the examples presented in Figures 3∼7 [8][9][10].…”

Section: Increasing Sensitivity By Improving P/b: High Spectral Rmentioning

confidence: 99%

Improving the Sensitivity of Electron Beam Microanalytical Techniques by Enhanced X-ray Spectrometry: X-ray Microcalorimetry, Silicon Drift Detector Energy Dispersive X-ray Spectrometry, and Polycapillary X-ray Optics

Newbury

2003

e-J. Surf. Sci. Nanotechnol.

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The microcalorimeter energy dispersive x-ray spectrometer, the silicon drift detector (SDD), and polycapillary x-ray optics are recent developments that have significantly advanced analytical x-ray spectrometry for electron beam instruments. The microcalorimeter EDS is capable of high resolution operation (∼ 5 eV wide peaks) over a wide range of photon energies (250 eV ∼ 10 keV). The microcalorimeter EDS can be successfully applied to peak interference problems that are not accessible with the conventional semiconductor EDS such as TiN and BaTiO3. Polycapillary x-ray optics can augment the collection angle of the microcalorimeter EDS to increase its sensitivity. The SDD is capable of extremely high count rates, up to 1 MHz, and is especially useful for high speed x-ray mapping.

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High-resolution microcalorimeter energy-dispersive spectrometer for x-ray microanalysis and particle analysis

Cited by 7 publications

References 2 publications

Low Voltage EDXS and Elements of the First Transition Series

Low Voltage EDXS and Elements of the First Transition Series

Superconducting transition-edge microcalorimeters for X-ray microanalysis

Improving the Sensitivity of Electron Beam Microanalytical Techniques by Enhanced X-ray Spectrometry: X-ray Microcalorimetry, Silicon Drift Detector Energy Dispersive X-ray Spectrometry, and Polycapillary X-ray Optics

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