A computer programme for an automated electron microprobe to solve X-ray interferences

Armigliato, A.; Garulli, A.; Gavoni, D.; Venturi, Paolo

doi:10.1016/0304-3991(83)90343-1

Cited by 3 publications

(4 citation statements)

References 0 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Our general feeling is that the accuracies for N-Ka are probably in the order of ± 1.5 % for easy cases like BN, AlN and Si3N4 and of 2-3 % for really difficul t cases like ZrN, Nb2N and Mo2N. 27 III.6 Measurements of Inteqral k-ratios between ~ and 30 kV Al though the APF concept has been introduced 1 ' 2 in order to facilitate the conversion of fast (and usually incorrect) peak intensity ratio measurements into correct integral intensity ratio measurements with great savings of time and effort, the concept could only be used in a very limited number of cases in the present work; only for the nitrides of the lighter elements B, Al and Si. The main reasen was the sametimes streng curvature in the backgrounds in the heavier nitrides, which made the routine procedure, consisting of background measurements at equal distances on either side of the peak, impossible to use.…”

Section: Iii5 Measurements Of Area-peak Factorsmentioning

confidence: 86%

“…Moreover, we have verified experimentally that no noticeable losses in N-Ka intens i ty took place during the time required for the integral recording of our Nitrogen spectra. In the past, several methods for peak separation have been proposed 27 • They can be qualified either as ratio methóds or as deconvolution techniques. The ratio methods are based on the assumption that there is a fixed ratio between the integral intensities of either Ti~ï<a and Ti-11 or Ti-La and Ti-11 and that these ratios, oncè they are known from measurements on a pure Ti standard, éan also be applied to the Titanium in the Ti-N compóuhd.…”

Section: Ivl Oxygen Contamination In the Mieroprobementioning

confidence: 99%

See 1 more Smart Citation

Quantitative electron probe microanalysis of nitrogen

Bastin

Heijligers

1991

Scanning

View full text Add to dashboard Cite

Quantitative electron probe microanalysis of nitrogen has been performed on 18 nitride specimens in the voltage range of 4–30 kV. A conventional lead stearate and a new W/Si multilayer analyzer crystal (2d = 5.98 nm) were used simultaneously. The net peak count rates on the latter crystal were approximately 2.8 times higher than on the lead stearate crystal. In addition, significant improvements in the peak to background ratios were achieved, which proved critical when dealing with difficult nitrides such as ZrN, Nb2N, and Mo2N. A most conspicuous feature of the new crystal, however, is its effective suppression of higher‐order reflections in the wavelength range of N‐Kα. As a result, backgrounds are free of interfering lines and spectral artifacts, which facilitates accurate background determination. Two procedures for the analysis of nitrogen in the presence of titanium are also discussed. One procedure is based on the assumption that the area–peak factor (APF, integral k‐ratio/peak k‐ratio) of the N‐Kα peak in Ti–N compounds relative to a nitrogen standard (Cr2N) has a fixed value which can be used in order to separate the Ti‐ll peak from the N‐Kα peak. Extensive tests on a number of compositions in the Ti–N system have shown that it is possible to do quantitative analysis of nitrogen in Ti–N compounds with a relative accuracy of better than 5%. For very low levels of nitrogen (below 15 at%) the APF method was found unsuitable. In such cases, however, the well‐known multiple least‐squares digital‐fitting techniques appeared to do an excellent job. In order to account for the effects of peak shape alterations in the N‐Kα peak, all nitrogen spectra were recorded in integral fashion and compared with those of the Cr2N standard. The shape alterations for the N‐Kα peak were much smaller than for B‐Kα and C‐Kα radiations: The observed values for the area–peak factor relative to Cr2N differed less than 5% from unity. The present work has resulted in a database containing 144 integral k‐ratios for N‐Kα and 149 peak k‐ratios for the x‐ray lines of the metal partners in the nitrides. Our own Gaussian ϕ(pz) matrix correction procedure “PROZA,” used in conjunction with a set of improved mass absorption coefficients, yielded excellent results for the nitrogen data: An average value of kcalc/Kmeas of 1.0051 and a relative root mean square deviation of 3.99%.

show abstract

Section: Iii5 Measurements Of Area-peak Factorsmentioning

confidence: 86%

Section: Ivl Oxygen Contamination In the Mieroprobementioning

confidence: 99%

Quantitative electron probe microanalysis of nitrogen

Bastin

Heijligers

1991

Scanning

View full text Add to dashboard Cite

show abstract

“…[35] For the determination of the characteristic X-ray emission peak of nitrogen, a correction procedure had to be applied because of severe overlap of the N-K a and Ti-L l X-ray emission peaks. The correction procedure, known as the ratio method, is as follows [36] :…”

Section: F Electron Probe Microanalysis (Epma)mentioning

confidence: 99%

Nitride Formation and Excess Nitrogen Uptake After Nitriding Ferritic Fe-Ti-Cr Alloys

Jung

Meka

Schacherl

et al. 2011

Metall Mater Trans A

View full text Add to dashboard Cite

The microstructure of the nitrided zone of Fe-Ti-Cr alloys, containing a total of 0.30 at. pct (Ti + Cr) alloying elements, with varying Ti/Cr atomic ratio (0.45, 0.87, and 1.90), was investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The stable TiN and CrN nitrides did not precipitate after nitriding. Instead, ultrafine, metastable, mixed Ti 1-x Cr x N nitride precipitates developed in the nitrided zone: The precipitates were of platelet morphology (length £30 nm and thickness £3 nm) and of cubic, rock-salt, crystal-structure type. The misfit strain around the nitride platelets in the ferrite matrix increases with increasing Ti/Cr atomic ratio. As a consequence, most pronouncedly for the highest Ti/Cr atomic ratio, a tetragonally distorted ferrite matrix surrounds the precipitates, as evidenced both by XRD and TEM. The amount of nitrogen taken up was determined quantitatively by measuring the so-called nitrogen-absorption isotherms. It follows that the absorbed amount of so-called excess nitrogen dissolved in the matrix and adsorbed at the nitride-platelet faces increases distinctly with increasing Ti/Cr atomic ratio. The results were discussed in terms of the dependence of misfit strain on the Ti/Cr atomic ratio and the higher chemical affinity of Ti for N than of Cr for N.

show abstract

“…[43] To determine the characteristic X-ray emission peak of nitrogen, a correction procedure had to be applied because of severe overlap of the N-K a and Ti-L l X-ray emission peaks. The correction procedure known as ratio method [44] was applied.…”

Section: Epma Analysismentioning

confidence: 99%

The Kinetics of the Nitriding of Ternary Fe-2 at pct Cr-2 at pct Ti Alloy

Jung

Schacherl

Bischoff

et al. 2011

Metall Mater Trans A

View full text Add to dashboard Cite

The mechanism and the kinetics of growth of the nitrided zone of ternary Fe-2 at pct Cr-2 at pct Ti alloy was investigated by performing gaseous nitriding experiments at temperatures of 833 K and 853 K (560°C and 580°C) and at nitriding potentials r N = 0.004 atm À1/2 and 0.054 atm À1/2 . The microstructure of the nitrided zone was investigated by transmission electron microscopy and the elemental compositional variation with depth was determined by employing electron probe microanalysis. Fine platelet-type mixed Cr 1 -x Ti x N nitride precipitates developed in the nitrided zone. To describe the evolution of the nitrogen concentration depth profile, a numerical model was developed with the following parameters: the surface nitrogen content, the solubility product(s) of the alloying elements and dissolved nitrogen in the ferrite matrix, and a parameter defining the composition of the inner nitride precipitates. These parameters were determined by fitting model-calculated nitrogen depth profiles to the corresponding experimental data. The results obtained demonstrate that the type of nitride formation (i.e., whether Cr and Ti precipitate separately, as CrN and TiN, or jointly, as mixed Cr 1 -x Ti x N) as well as the amounts of mobile and immobile excess nitrogen taken up by the specimen considerably influence the shape and extent of the nitrogen concentration profiles.

show abstract

A computer programme for an automated electron microprobe to solve X-ray interferences

Cited by 3 publications

References 0 publications

Quantitative electron probe microanalysis of nitrogen

Quantitative electron probe microanalysis of nitrogen

Nitride Formation and Excess Nitrogen Uptake After Nitriding Ferritic Fe-Ti-Cr Alloys

The Kinetics of the Nitriding of Ternary Fe-2 at pct Cr-2 at pct Ti Alloy

Contact Info

Product

Resources

About