Accurate determinations of Ge atom fractions in SiGe semiconductor chips using high performance ICP-OES

Rabb, Savelas A.; Yu, Lee L.

doi:10.1039/b715148a

Cited by 3 publications

(4 citation statements)

References 20 publications

(29 reference statements)

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“…HP-ICP-OES is used routinely for the certification of elemental mass fraction in the 3100 series of elemental standard solution SRMs 22,25 and has also been used in other NIST measurements. [26][27][28][29] involving ICP-OES procedures that are similar to the highperformance protocol have been reported by other laboratories. [30][31][32][33][34] It is important to emphasize that for the certification of Be mass fraction in SRM 1877, HP-ICP-OES was modified somewhat from the way it has been described previously.…”

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confidence: 80%

“…Relative expanded uncertainties, expressed as 95% confidence intervals, are typically on the order of 0.1%. HP-ICP-OES is used routinely for the certification of elemental mass fraction in the 3100 series of elemental standard solution SRMs , and has also been used in other NIST measurements. − Measurements involving ICP-OES procedures that are similar to the high-performance protocol have been reported by other laboratories. − …”

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confidence: 99%

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Certification of Beryllium Mass Fraction in SRM 1877 Beryllium Oxide Powder Using High-Performance Inductively Coupled Plasma Optical Emission Spectrometry with Exact Matching

et al. 2009

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High-performance inductively coupled plasma optical emission spectrometry (HP-ICP-OES) was used to certify the Be mass fraction in National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) 1877 Beryllium Oxide Powder. The certified value and expanded uncertainty expressed at a 95% confidence level is (0.3576 +/- 0.0024) g/g. To obtain best results, the Be mass fractions, Mn (internal standard) mass fractions, and matrix compositions of the calibration solutions were carefully matched to those of the sample solutions for each individual HP-ICP-OES analysis. This "exact matching" approach was used because experience at NIST has shown that it often affords improved accuracy and precision in HP-ICP-OES analysis. NIST has never published these observations. Due to the toxicity of BeO and the difficulty of containing the very fine powder material, sets of solutions for HP-ICP-OES analysis were prepared by laboratories collaborating with NIST who have the experience and equipment needed to work with the material safely. Each laboratory utilized a unique digestion protocol(s). After preparing the sets of solutions, the collaborating laboratories shipped them to NIST for HP-ICP-OES analysis. NIST provided the collaborating laboratories with solution preparation kits and spreadsheets to help establish traceability of the HP-ICP-OES results to the International System of Units (SI) and to allow exact matching to be accomplished. The agreement observed among the four individual Be mass fraction values determined from the sets of solutions prepared by the collaborating laboratories was 0.074% relative (1s of mean). The excellent agreement provides a measure of confidence in the robustness of each of the digestion procedures, as well as in the certified Be mass fraction value. The analytical benefits of using exact matching for this particular certification were investigated. Results show that exactly matching the matrix compositions of the standards to the samples for each HP-ICP-OES analysis was critical to obtaining the excellent agreement observed among the individual Be mass fraction values and also helped to minimize bias and uncertainty in the certified value. Unlike previous NIST studies, exactly matching the Be and Mn mass fractions of the standards to the samples for this particular certification appears to have had little effect on the data.

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Certification of Beryllium Mass Fraction in SRM 1877 Beryllium Oxide Powder Using High-Performance Inductively Coupled Plasma Optical Emission Spectrometry with Exact Matching

et al. 2009

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“…Inductively coupled plasma optical emission spectroscopy (ICP-OES) was one technique used for bulk quantification of Ge in the Si 0.86 Ge 0.14 bulk alloy as described by Rabb et al (2008). Two randomly selected 2 mm × 2 mm × 2 mm chips that had been cut from the alloy were analyzed.…”

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confidence: 99%

Characterization of SiGe Films for Use as a National Institute of Standards and Technology Microanalysis Reference Material (RM 8905)

et al. 2009

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Bulk silicon-germanium (SiGe) alloys and two SiGe thick films (4 and 5 microm) on Si wafers were tested with the electron probe microanalyzer (EPMA) using wavelength dispersive spectrometers (WDS) for heterogeneity and composition for use as reference materials needed by the microelectronics industry. One alloy with a nominal composition of Si0.86Ge0.14 and the two thick films with nominal compositions of Si0.90Ge0.10 and Si0.75Ge0.25 on Si, evaluated for micro- and macroheterogeneity, will make good microanalysis reference materials with an overall expanded heterogeneity uncertainty of 1.1% relative or less for Ge. The bulk Ge composition in the Si0.86Ge0.14 alloy was determined to be 30.228% mass fraction Ge with an expanded uncertainty of the mean of 0.195% mass fraction. The thick films were quantified with WDS-EPMA using both the Si0.86Ge0.14 alloy and element wafers as reference materials. The Ge concentration was determined to be 22.80% mass fraction with an expanded uncertainty of the mean of 0.12% mass fraction for the Si0.90Ge0.10 wafer and 43.66% mass fraction for the Si0.75Ge0.25 wafer with an expanded uncertainty of the mean of 0.25% mass fraction. The two thick SiGe films will be issued as National Institute of Standards and Technology Reference Materials (RM 8905).

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“…The HP-ICP-OES technique has become a method of choice for many NIST measurements. − These include certification measurements for NIST reference materials (RMs) and Standard Reference Materials (SRMs). For example, the technique has been used recently for the certification of the Be mass fraction in SRM 1877 Beryllium Oxide Powder .…”

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Improving the High-Performance Inductively Coupled Plasma Optical Emission Spectrometry Methodology through Exact Matching

Butler

Turk

2010

Anal. Chem.

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Exact matching is investigated as a means of improving high-performance inductively coupled plasma optical emission spectrometry (HP-ICP-OES), a technique developed at the National Institute of Standards and Technology (NIST) to enable elemental determinations with relative expanded uncertainty of approximately 0.2% expressed at 95% confidence. "Exact matching" refers to the very careful matching of analyte mass fractions, internal standard mass fractions, and matrix compositions among the calibration and unknown sample solutions prepared for an analysis. Computer spreadsheet modeling results and laboratory data involving 16 pairs of analyte and internal standard wavelengths show that exact matching of analyte and internal standard mass fractions mitigates imprecision and bias that can be caused by even subtle nonlinearity in the ICP-OES instrument response. Laboratory experiments also demonstrate matrix effects caused by small variations in acid composition and by mass fractions of Na less than 4 mg kg(-1), emphasizing the need for exact matching of matrix compositions. HP-ICP-OES analyses performed at NIST with and without exact matching illustrate that exact matching enables relative expanded uncertainties to be halved to approximately 0.1%.

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Accurate determinations of Ge atom fractions in SiGe semiconductor chips using high performance ICP-OES

Cited by 3 publications

References 20 publications

Certification of Beryllium Mass Fraction in SRM 1877 Beryllium Oxide Powder Using High-Performance Inductively Coupled Plasma Optical Emission Spectrometry with Exact Matching

Certification of Beryllium Mass Fraction in SRM 1877 Beryllium Oxide Powder Using High-Performance Inductively Coupled Plasma Optical Emission Spectrometry with Exact Matching

Characterization of SiGe Films for Use as a National Institute of Standards and Technology Microanalysis Reference Material (RM 8905)

Improving the High-Performance Inductively Coupled Plasma Optical Emission Spectrometry Methodology through Exact Matching

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