Quantitative EPMA and TEM of unsupported films

Dijkstra, Johannes M.; Bastin, G.F.; Heijligers, H.J.M.; Klepper, D.

doi:10.1007/bf01244553

Cited by 8 publications

(4 citation statements)

References 8 publications

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“…This is due to the fact that the X-ray energies of the characteristic lines are positioned in the region lower than 0.7 keV of the energy spectrum, which allows the effective emission of the generated X-rays to take place only in very shallow depth [105,106]. Another difficulty occurs if the emission energy of the analyzed element coincides with the absorption edge of an accompanying element [107][108][109], which makes it necessary to reduce surface contamination caused by long analysis times [105,109]. The surface roughness of technological samples complicates the evaluation of the results, since changes of the take-off angle of 5°can alter the results by 10 % when performing the analysis at the relatively shallow take-off angle of 32° [106,108].…”

Section: Electron Probe Microanalysismentioning

confidence: 99%

Critical evaluation of the state of the art of the analysis of light elements in thin films demonstrated using the examples of SiOXNY and AlOXNY films (IUPAC Technical Report)

Dreer¹,

Wilhartitz²

2004

Pure and Applied Chemistry

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The quantitative analysis of thin films containing light elements is very important in improving the coating processes and technological properties of the products. In order to review the state of the art of modern analytical techniques for such applications, the model systems SiOXNY and AlOXNY were selected. Over 1000 abstracts were screened, and the relevant literature was evaluated to give a comprehensive overview of instruments, analytical procedures and results, film types, deposition methods, and investigation goals. From more than 150 citations, the limitations, drawbacks, and pitfalls of the different methods were extracted and reviewed critically, while in addition, improvements were proposed where possible. These suggestions are combined with the newest results of investigation by the authors of this paper. Recommendations concerning the optimized combination of analytical methods for different analytical problems have been worked out on the basis of all results. Analysis of various multicomponent systems containing light elements demonstrated the applicability of the different methods of analysis in combination to all film systems with related compositions.

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Section: Electron Probe Microanalysismentioning

confidence: 99%

Critical evaluation of the state of the art of the analysis of light elements in thin films demonstrated using the examples of SiOXNY and AlOXNY films (IUPAC Technical Report)

Dreer¹,

Wilhartitz²

2004

Pure and Applied Chemistry

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“…It is furthermore possible to extend this method to the analysis of unsupported layers [7]. The attainable depth resolution has been demonstrated to be, under favorable circumstances, comparable to that of Auger sputter profiling [8,9].…”

Section: Introductionmentioning

confidence: 99%

Progress in the Characterization of Layered Structures by X-Ray Microanalysis

Rickerby

1995

Microsc. Microanal. Microstruct.

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Abstract. 2014 Recent advances in the mathematical description of the depth distribution of X-ray generation, ø(03C1z), have permitted the quantitative analysis of multilayer structures with a precision approaching ±1 nm. A weighted average mass absorption coefficient is proposed for use in analysis with L series radiation when the energy separation of the component lines is less than the spectrometer resolution. This is shown to improve agreement between experimental data and the theoretically calculated X-ray intensities. An example of the application of the Ø(03C1z) method to the analysis of a titanium-boron nitride bilayer is described with special reference to the problem of detection of interfacial diffusion and oxidation phenomena. Microsc. Microanal. Microstruct. 6 (1995) Classification Physics Abstracts

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“…To measure thickness using EDS, we need a reference for the x-ray signal. Dijkstra et al [1] used a bulk target as a reference in TEM but the yield was too high at currents suitable for analysis of a thin sample. Boon [2] devised a beam current monitor linear over 3-4 decades so that a bulk target could be measured at much less current than the specimen and a beam current correction applied.…”

mentioning

confidence: 99%

“…Solutions like tilting the holder as shown in Fig.2 and removing material on the side of the holder facing the detector as in Fig.3 can help alleviate the occlusion [5,6]. Any occlusion alters  in equation (1) and thus influences any method of mass thickness measurement but the reference sample can be used to test what area on the sample is safe to use for measurement. With a 5 degree specimen tilt we have been able to obtain consistent mass thickness measurements in a JEOL JEC 2100 TEM over a region spanning 0.8mm (Fig.4).…”

mentioning

confidence: 99%

Mass Thickness Measurement in TEM: A New Single Standard Method for Convenient Quantification by TEM EDS

Statham¹,

Sagar²,

Holland³

et al. 2016

Microsc Microanal

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The mass thickness, ( t ) sp , of a thin film specimen is needed for absorption corrections in X-ray analysis and the equivalent areal density (atoms/m 2 ) for constituent elements is also useful. To measure thickness using EDS, we need a reference for the x-ray signal. Dijkstra et al [1] used a bulk target as a reference in TEM but the yield was too high at currents suitable for analysis of a thin sample. Boon [2] devised a beam current monitor linear over 3-4 decades so that a bulk target could be measured at much less current than the specimen and a beam current correction applied. Nevertheless, at TEM voltages (e.g. 200 kV) absorption corrections are severe for bulk material and the method still requires the use of many standards. Watanabe's zeta factor method [3] requires thin film standards of known mass thickness and composition and a method of measuring the beam current. However, beam current measurement is not always available, convenient or of sufficient accuracy and there is a dearth of suitable thin film standards.Here we consider a new method that uses a single reference standard and can be used on any TEM. The procedure involves recording an x-ray spectrum from the reference standard before each session of acquisitions on a real specimen. There is no need to measure the beam current; it just needs to be stable for the duration of the session. For a thin specimen with uniform ionization throughout, the counts recorded for the emission line of element A can be written as (4π)) ) from the measurement on the reference standard provided we use the same beam current and kV. When a spectrum is recorded from the specimen, equation (1) can be then be used to determine ( t ) sp . C A for each element. ( t ) sp is then obtained by assuming that the mass fractions sum to unity and iteration can be used to refine f(chi) A . Doing a "beam measurement" on the reference standard at the start of any session thus replaces explicit measurement of beam current.To make this technique accessible requires a suitable well-characterized reference standard to be available. Silicon nitride TEM support films within a standard 3mm diameter disk are now widely available and can be manufactured to have highly uniform thickness over a large area. Although film composition, thickness and density is nominal, we have characterized some samples in an SEM at 30 kV using a transmission holder and pure bulk reference standards so that we can measure ( t ) ref . C ref at a series of points all over the support film. An example shown in Fig.1 shows that the mass thickness 38

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Quantitative EPMA and TEM of unsupported films

Cited by 8 publications

References 8 publications

Critical evaluation of the state of the art of the analysis of light elements in thin films demonstrated using the examples of SiOXNY and AlOXNY films (IUPAC Technical Report)

Critical evaluation of the state of the art of the analysis of light elements in thin films demonstrated using the examples of SiOXNY and AlOXNY films (IUPAC Technical Report)

Progress in the Characterization of Layered Structures by X-Ray Microanalysis

Mass Thickness Measurement in TEM: A New Single Standard Method for Convenient Quantification by TEM EDS

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