Quantitative EPMA of nitrogen : A tricky element in the electron-probe microanalyzer

Author(s):  
G.F. Bastin ◽  
H.J.M. Heijligers

Among the ultra-light elements B, C, N, and O nitrogen is the most difficult element to deal with in the electron probe microanalyzer. This is mainly caused by the severe absorption that N-Kα radiation suffers in carbon which is abundantly present in the detection system (lead-stearate crystal, carbonaceous counter window). As a result the peak-to-background ratios for N-Kα measured with a conventional lead-stearate crystal can attain values well below unity in many binary nitrides . An additional complication can be caused by the presence of interfering higher-order reflections from the metal partner in the nitride specimen; notorious examples are elements such as Zr and Nb. In nitrides containing these elements is is virtually impossible to carry out an accurate background subtraction which becomes increasingly important with lower and lower peak-to-background ratios. The use of a synthetic multilayer crystal such as W/Si (2d-spacing 59.8 Å) can bring significant improvements in terms of both higher peak count rates as well as a strong suppression of higher-order reflections.

1999 ◽  
Vol 5 (S2) ◽  
pp. 78-79
Author(s):  
C. Merlet ◽  
X. Llovet ◽  
F. Salvat

Studies of x-ray emission from thin films on substrates using an electron probe microanalyzer (EPMA) provide useful information on the characteristics of x-ray generation by electron beams. In this study, EPMA measurements of multilayered samples were performed in order to test and improve analytical and numerical models used for quantitative EPMA. These models provide relatively accurate results for samples consisting of layers with similar average atomic numbers, because of their similar properties regarding electron transport and x-ray generation. On the contrary, these models find difficulties to describe the process when the various layers have very different atomic numbers. In a previous work, we studied the surface ionization of thin copper films of various thicknesses deposited on substrates with very different atomic numbers. In the present communication, the study is extended to the case of multilayered specimens.The studied specimens consisted of thin copper films deposited on a carbon layer which, in turn, was placed on a variety of single-element substrates, ranging from Be to Bi.


2009 ◽  
Vol 24 (8) ◽  
pp. 2638-2643 ◽  
Author(s):  
Kai-Jheng Wang ◽  
Yan-Zuo Tsai ◽  
Jenq-Gong Duh ◽  
Toung-Yi Shih

An Sn-patch formed in Ni(V)-based under bump metallization during reflow and aging. To elucidate the evolution of the Sn-patch, the detailed compositions and microstructure in Sn–Ag–Cu and Ti/Ni(V)/Cu joints were analyzed by a field emission electron probe microanalyzer (EPMA) and transmission electron microscope (TEM), respectively. There existed a concentration redistribution in the Sn-patch, and its microstructure also varied with aging. The Sn-patch consisted of crystalline Ni and an amorphous Sn-rich phase after reflow, whereas V2Sn3 formed with amorphous an Sn-rich phase during aging. A possible formation mechanism of the Sn-patch was proposed.


2010 ◽  
Vol 160-162 ◽  
pp. 1787-1790
Author(s):  
Jing Cao ◽  
Yong Feng Wang ◽  
Chun Xue Wei

1J79 alloy was prepared by vacuum electric arc smelting.The crystal growth and the content of impurity was observed by electron probe microanalyzer,and magnetic properties were measured by vibrating sample magnetometer(VSM).Experimental results show that inclusions in the alloy are fewer and fewer, composition becomes more uniform with the increases of the Mo content, and grain size also becomes larger and larger with the increases of Mo content, to reduce coercivity. The small amount of Mo addition is useful to improve the saturation magnetization and reduce coercivity.


2021 ◽  
Vol 2 (446) ◽  
pp. 22-28
Author(s):  
Z. Bagova ◽  
K. Zhantasov ◽  
G. Turebekova ◽  
B. Sapargaliyeva ◽  
Javier Rodrigo-Ilarri

The article presents the analysis and results of the study of technogenic slag waste of lead-zinc production. Slags of lead-zinc production contain a large number of toxic compounds: lead, zinc, osmium, cadmium, which are dangerous sources of environmental pollution. Due to the open storage of slags, it was found that the maximum permissible concentrations of lead were exceeded. Utilization of man-made slag waste is of great importance for reducing the negative impact on the safety of life and improving the environmental situation in the region. At the same time, slags are valuable raw materials containing compounds of non-ferrous and rare-earth metals. The article shows the results of laboratory studies of slags to determine the qualitative and quantitative composition of valuable components in the waste of lead production and the possibility of their further processing and disposal. Studies of the material of the heavy slag fraction were carried out on an electron probe microanalyzer of the JEOL IXA-8230 Electron Probe microanalyzer brand. X-ray diffractometric analysis of the average slag sample was performed on a DRON-4 diffractometer with Cu radiation, graphite monochromator. Samples were selected heavy fraction and manufactured artificial polished sections (briquettes). The sections were studied under the microscope of the brand LEICA DM 2500P and immersion in liquids. According to the results of research, it was found that lead slags contain a sufficiently high amount of non-ferrous metal compounds: lead oxide up to 0.7 % and zinc oxide up to 8.5 % of the weight amount of slag, which makes the process of recycling toxic waste from lead production technically and economically feasible.


1996 ◽  
Vol 69 (12) ◽  
pp. 834-839
Author(s):  
Osamu WATANABE ◽  
Hiroshi SAITOH ◽  
Yasuhito MARUYAMA

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