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Quantitative analysis method for detecting boron content by electron probe

An electronic probe and quantitative analysis technology, which is applied to the use of wave/particle radiation for material analysis, measuring devices, electrical components, etc., can solve problems such as difficult element analysis, poor penetration ability, and high background strength

Inactive Publication Date: 2011-07-20
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the long wavelength of X-rays, ultralight elements with atomic number less than 10 have poor penetrating ability; the fluorescence yield is low, which is several orders of magnitude smaller than that of ordinary elements; The peak position is affected by the combination state; the background intensity is high and changes nonlinearly with the wavelength; it is seriously interfered by the overlapping peaks of heavy elements, so it is difficult to use electronic probes for elemental analysis of these elements

Method used

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  • Quantitative analysis method for detecting boron content by electron probe
  • Quantitative analysis method for detecting boron content by electron probe
  • Quantitative analysis method for detecting boron content by electron probe

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The first step is to prepare the sample zirconium boride (ZrB 2 );

[0024] In the second step, according to the sample injection requirements of the electron probe, the sample zirconium boride (ZrB 2 ) into the sample stage of the electron probe;

[0025] The third step is to set a series of quantitative analysis conditions such as accelerating voltage and electron beam current, among which the accelerating voltage is set to 6KV, 8KV, 10KV, 12KV, 15KV, 18KV, 20KV, and the electron beam current is set to 2×10 -7 A, Quantitative analysis test was carried out, and the test results are listed in Table 1.

[0026] Discussion of test results:

[0027] In the test, multiple acceleration voltage values ​​of 6KV, 8KV, 10KV, 12KV, 15KV, 18KV, and 20KV were used for ultra-light element analysis and peak-finding. The purpose is to find the best acceleration voltage value to obtain the maximum peak count. From figure 1 It can be seen from the experimental data in Table 1 that ...

Embodiment 2

[0031] The first step is to prepare the sample hafnium boride (HfB 2 );

[0032] In the second step, the prepared sample is loaded on the sample stage of the electronic probe according to the sampling requirements of the electronic probe;

[0033] The third step is to set a series of quantitative analysis conditions such as accelerating voltage and electron beam current, among which the accelerating voltage is set to 6KV, 8KV, 10KV, 12KV, 15KV, 18KV, 20KV, and the electron beam current is set to 2×10 -7 A, Quantitative analysis test is carried out, and the maximum peak count obtained is shown in Table 2.

[0034] Table 2 Counting of boron element peaks in hafnium boride under different accelerating voltages

[0035]

[0036] Discussion of test results:

[0037] From the experimental data in Table 2, when the accelerating voltage is 10KV, the peak count is the highest. Therefore, 10KV is the best accelerating voltage value for boron electron probe quantitative analysis. ...

Embodiment 3

[0039] The first step is to prepare the sample nickel boride (Ni 2 B);

[0040] In the second step, according to the sample injection requirements of the electronic probe, the sample nickel boride (Ni 2 B) on the sample stage of loading electron probe;

[0041] The third step is to set a series of quantitative analysis conditions such as accelerating voltage and electron beam current, among which the accelerating voltage is set to 6KV, 8KV, 10KV, 12KV, 15KV, 18KV, 20KV, and the electron beam current is set to 2×10 -7 A, Quantitative analysis test is carried out, and the maximum peak count obtained is shown in Table 3.

[0042] Table 3 Nickel boride (Ni 2 B) Boron element peak count and upper and lower background values

[0043]

[0044] Discussion of Test Results

[0045] From the experimental data in Table 3, when the accelerating voltage is 10KV, the peak count is the highest. Therefore, 10KV is the best accelerating voltage value for boron electron probe quantitati...

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Abstract

Elements, of which the atomic numbers are smaller than 10, are ultralight elements. At present, an electron probe mainly can detect elements such as boron, carbon, nitrogen, oxygen and fluorine. Due to long wavelength of characteristic X-rays, the penetration capacities of these elements are low, the fluorescence yield is low, the background strength is high, and the interference with overlapped peaks of L and M lines of heavy elements is serious. Therefore, it is difficult to analyze the ultralight elements by using the electron probe or scanning electron microscopy / energy dispersive spectrometer. When the method is used for quantitative analysis on a boron sample by the electron probe, quantitative analysis is performed by changing accelerating voltage, reducing electron penetration depth and selecting a 10KV accelerating voltage, so that more satisfactory boron micro area quantitative analysis and element area distribution results can be achieved.

Description

technical field [0001] The invention relates to a quantitative analysis method for detecting the content of boron-containing elements, in particular to a quantitative analysis method for detecting the content of boron-containing elements by an electronic probe. Background technique [0002] Electron probe is the most reliable means of micro-area quantitative analysis with fast analysis speed and relatively accurate quantification. The range of elements analyzed by electron probe is generally from beryllium (Be) to uranium (U). However, due to the long wavelength of X-rays, ultralight elements with atomic number less than 10 have poor penetrating ability; the fluorescence yield is low, which is several orders of magnitude smaller than that of ordinary elements; The peak position is affected by the combination state; the background intensity is high and changes nonlinearly with the wavelength; it is seriously interfered by the overlapping peaks of heavy elements, so it is diff...

Claims

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Application Information

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IPC IPC(8): G01N23/083G01N23/00H01J37/252
Inventor 周莹黄碧兰张冰罗超
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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