CN112730495A - Test method for improving characteristic X-ray intensity value - Google Patents
Test method for improving characteristic X-ray intensity value Download PDFInfo
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- CN112730495A CN112730495A CN202011406792.4A CN202011406792A CN112730495A CN 112730495 A CN112730495 A CN 112730495A CN 202011406792 A CN202011406792 A CN 202011406792A CN 112730495 A CN112730495 A CN 112730495A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
- G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
Abstract
The invention discloses a test method for improving a characteristic X-ray intensity value, which comprises the following steps: forming a test system of the element to be tested by utilizing a plurality of spectral crystals on different spectrometers of the electronic probe, and simultaneously testing the same element to be tested; acquiring the total net count of the elements to be detected in the standard sample; acquiring the total net count of elements to be detected in a sample to be detected; calculating the concentration of the element to be detected in the sample to be detected according to the total net count of the element to be detected in the standard sample, the total net count of the element to be detected in the sample to be detected and the concentration of the element to be detected in the standard sample; and acquiring the total background intensity of the elements to be detected in the sample to be detected according to the background intensity of the elements to be detected in the sample to be detected on each spectral crystal, and further calculating the detection limit of the elements to be detected. The invention can improve IunkValue, lowering the detection limit of the test, or without changing IunkOn the premise of the value, the test current is reduced to avoid the phenomenon that the sample to be tested is damaged to cause element migration.
Description
Technical Field
The invention relates to the technical field of electronic probe test. More particularly, the present invention relates to a test method for improving characteristic X-ray intensity values.
Background
The electronic probe is used as a micro-area in-situ analysis means, can quickly and accurately analyze the element concentration of a solid sample, is widely applied to the fields of geology, material science and the like, and is mainly applied to the analysis and test of major elements. Compared with other micro-area in-situ analysis and test means, the electronic probe has the characteristics of small spatial resolution, no damage and accurate test, so that the electronic probe is increasingly paid more attention to the analysis of micro-area in-situ trace elements.
The basic principle of the electron probe is that an electron beam bombards a sample to generate X rays, and the percentage concentration of elements in the sample is obtained through matrix correction according to the comparison between the intensity of the characteristic X rays of the elements of the tested sample and the intensity of the characteristic X rays of the elements of a standard sample, and the formula is as follows:
wherein, CunkRepresenting the concentration of the test element in the test sample, CstdRepresenting the concentration of the element to be measured in the standard sample, IunkRepresenting the intensity of the test element of the test sample, IstdRepresenting the intensity of the element to be measured of the standard sample, GZAFRepresents a stromal correction factor. When the electron probe is used for quantitative analysis, a spectroscopic crystal on a spectrometer is used for testing the characteristic X-ray intensity of elements.
When the trace elements are tested by using the electronic probe, the tested I is low in element concentrationunkThe value is very low. To improve the accuracy of the test, I must be increasedunkThe value is obtained. At present, I is increasedunkThe methods of the value include changing the accelerating voltage, increasing the electron beam current and prolonging the testing time, and the methods are easy to cause the tested sample to be damaged and cause element migration, thereby causing the testing result to be inaccurate.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
It is still another object of the present invention to provide a method for improving the characteristic X-ray intensity by using a plurality of spectroscopic crystals on different spectrometers using an electron probe, and simultaneously testing the characteristic X-ray intensity of the same element using each of the spectroscopic crystals, such methodThe method can increase I without increasing test currentunkMeanwhile, the phenomenon that elements migrate because the sample to be detected is damaged due to the use of large current is avoided.
To achieve these objects and other advantages in accordance with the purpose of the invention, there is provided a test method for improving characteristic X-ray intensity values, comprising:
forming a test system of the element to be tested by utilizing a plurality of spectral crystals on different spectrometers of the electronic probe, and simultaneously testing the same element to be tested;
acquiring the total net count of the elements to be detected in the standard sample;
acquiring the total net count of elements to be detected in a sample to be detected;
calculating the concentration of the element to be detected in the sample to be detected according to the total net count of the element to be detected in the standard sample, the total net count of the element to be detected in the sample to be detected and the concentration of the element to be detected in the standard sample;
and acquiring the total background intensity of the elements to be detected in the sample to be detected according to the background intensity of the elements to be detected in the sample to be detected on each spectral crystal.
Preferably, the detection limit of the element to be detected is calculated according to the total background intensity of the element to be detected in the sample to be detected.
Preferably, the spectrographic crystals on different spectrometers are homogeneous spectrographic crystals.
Preferably, the spectroscopy crystals on different spectrometers are different spectroscopy crystals.
Preferably, the specific method for obtaining the total net count of the elements to be detected in the standard sample comprises the following steps: and testing the characteristic X-ray total intensity and the background intensity of the element to be detected in the standard sample, calculating the net count of the element to be detected obtained by each light splitting crystal, and then calculating the total net count of the element to be detected in the standard sample.
Preferably, the specific method for obtaining the total net count of the elements to be detected in the sample to be detected is as follows: and testing the characteristic X-ray total intensity and the background intensity of the elements to be tested in the sample to be tested, calculating the net count of the elements to be tested obtained in each light splitting crystal, and then calculating the total net count of the elements to be tested in the sample to be tested.
Preferably, the calculation formula of the concentration of the element to be detected in the sample to be detected is as follows:
wherein CY1 and CY2 … CYn (n is an integer more than or equal to 2) are a plurality of spectral crystals on different spectrometers respectively,
respectively the net count of the elements to be measured obtained in each spectroscope when the standard sample is tested,
respectively the net count of the elements to be tested, C, obtained in each spectroscopic crystal when testing the sample to be testedstdRepresenting the concentration of the element to be measured in the standard sample, GZAFRepresents the stromal correction factor, CunkThe concentration of the element to be detected in the sample to be detected is shown.
Preferably, the calculation formula of the total background intensity of the elements to be detected in the sample to be detected is as follows:
Preferably, the calculation formula of the detection limit of the element to be detected is as follows:
wherein CY1 and CY2 … CYn (n is an integer more than or equal to 2) are a plurality of spectral crystals respectively,
respectively, the net count of the elements to be measured of each spectroscopic crystal when testing the standard sample, CstdRepresents the concentration of the element to be measured in the standard sample,
respectively the background intensity, t, of the sample to be tested on each spectroscopic crystal when the sample to be tested is testedbackTest time for background, GZAFRepresents a matrix correction factor, and D.L. is a detection limit.
The invention at least comprises the following beneficial effects:
by utilizing the plurality of the spectral crystals on the different spectrometer of the electronic probe, when the plurality of the spectral crystals are used for testing the same element, the total intensity of the characteristic X-ray is improved, the phenomenon that the element is migrated because a sample to be tested is damaged due to high current and long time is avoided, and the detection limit is effectively reduced.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a flow chart of a testing method for improving characteristic X-ray intensity values according to one embodiment of the present invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
The invention provides a test method for improving a characteristic X-ray intensity value, which comprises the following steps:
installing a plurality of spectral crystals on a spectrometer of an electronic probe to form a test system of an element to be tested; the plurality of spectral crystals on different spectrometers can be the same type of spectral crystal, and the plurality of spectral crystals on different spectrometers can be different types of spectral crystals; the spectral crystals are respectively marked as CY1, CY2, … and CYn (n is an integer more than or equal to 2). In the embodiment of the invention, the plurality of the spectroscopies are three spectroscopies, namely PETL1, PETL2 and PETL3, which are arranged on three different spectrometers.
The method for acquiring the total net count of the elements to be detected in the standard sample comprises the following steps: testing the characteristic X-ray total intensity and the background intensity of the element to be tested in the standard sample, calculating the net count of the element to be tested obtained by each light splitting crystal, and respectively recording the net count as
Then calculating the total net count of the elements to be measured in the standard sample and recording the total net count as
In the embodiment of the invention, the standard sample is rutile, the element to be detected is Ti, the net counts of Ti in the standard samples obtained by the three spectrographic crystals are 3311020, 2927275 and 3663455 cps/muA respectively, and the total net count I of the element to be detected Ti in the standard samplestd＝9901750cps/μA。
The method for acquiring the total net count of the elements to be detected in the sample to be detected comprises the following steps: testing the characteristic X-ray total intensity and the background intensity of the element to be tested in the sample to be tested, calculating the net count of the element to be tested obtained in each light splitting crystal, and respectively recording the net count as
Then calculating the total net count of the elements to be detected in the sample to be detected and recording the total net count as
In the embodiment of the invention, the sample to be detected is quartzThe element to be detected is Ti, net counts of Ti in the sample to be detected obtained by the three spectrographic crystals are 303.0, 255.0 and 299.8 cps/muA respectively, and the total net count I of the element to be detected in the sample to be detected isunk＝857.8cps/μA。
Calculating the concentration of the element to be detected in the sample to be detected according to the total net count of the element to be detected in the standard sample, the total net count of the element to be detected in the sample to be detected and the concentration of the element to be detected in the standard sample; the calculation formula of the concentration of the element to be detected in the sample to be detected is as follows:
wherein CY1 and CY2 … CYn (n is an integer more than or equal to 2) are a plurality of spectral crystals on different spectrometers respectively,
respectively the net count of the elements to be measured obtained in each spectroscope when the standard sample is tested,
respectively the net count of the elements to be tested, C, obtained in each spectroscopic crystal when testing the sample to be testedstdRepresenting the concentration of the element to be measured in the standard sample, GZAFRepresents the stromal correction factor, CunkThe concentration of the element to be detected in the sample to be detected is shown. In the embodiment of the invention, the concentration of the element Ti to be measured in the rutile of the standard sample is 59.9 wt.%, and the matrix correction factor GZAF1.1127, calculating to obtain the concentration of the element Ti to be measured in the quartz sample to be measured to be 57.7 mug/g (consistent with the content of Ti in the quartz sample to be measured to be 57 +/-4 mug/g)
Obtaining the total background intensity of the elements to be detected in the sample to be detected and the total back of the elements to be detected in the sample to be detected according to the background intensity of the elements to be detected in the sample to be detected on each spectroscopeThe scene intensity is calculated by the formula
Wherein the content of the first and second substances,
respectively the background intensity, I, of the sample to be tested on each spectroscopic crystal when the sample to be tested is testedunk-bgIs the total background intensity of the elements to be measured. In the embodiment of the invention, the background intensity of Ti in the sample to be detected obtained by the three spectroscopic crystals is 4278.8, 3941.8 and 5047.3 cps/muA respectively, and the total background intensity I of element Ti to be detected in the sample to be detectedunk-bg＝13267.9cps/μA。
Calculating the detection limit of the element to be detected according to the total background intensity of the element to be detected in the sample to be detected, wherein the calculation formula of the detection limit of the element to be detected is as follows:
wherein CY1 and CY2 … CYn (n is an integer more than or equal to 2) are a plurality of spectral crystals on different spectrometers respectively,
respectively, the net count of the elements to be measured of each spectroscopic crystal when testing the standard sample, CstdRepresents the concentration of the element to be measured in the standard sample,
respectively the background intensity, t, of the sample to be tested on each spectroscopic crystal when the sample to be tested is testedbackMeasuring time for background, GZAFRepresents a matrix correction factor, and D.L. is a detection limit. In an embodiment of the invention, the background measures time tback200s, the calculated limit of detection d.l. 0.7 μ g/g (1 δ)
Compared with other micro-area in-situ analysis and test means, the electronic probe has the characteristics of small spatial resolution, no damage and accurate test, so that the electronic probe is increasingly paid more attention to the analysis of micro-area in-situ trace elements. According to the content, when the plurality of spectral crystals are used for testing the same element at the same time, the total intensity of characteristic X-rays is improved, sample damage caused by high current and long time is avoided, and the detection limit is effectively reduced.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (9)
1. A test method for improving a characteristic X-ray intensity value, comprising:
forming a test system of the element to be tested by utilizing a plurality of spectral crystals on different spectrometers of the electronic probe, and simultaneously testing the same element to be tested;
acquiring the total net count of the elements to be detected in the standard sample;
acquiring the total net count of elements to be detected in a sample to be detected;
calculating the concentration of the element to be detected in the sample to be detected according to the total net count of the element to be detected in the standard sample, the total net count of the element to be detected in the sample to be detected and the concentration of the element to be detected in the standard sample;
and acquiring the total background intensity of the elements to be detected in the sample to be detected according to the background intensity of the elements to be detected in the sample to be detected on each spectral crystal.
2. The method as claimed in claim 1, wherein the detection limit of the element to be detected is calculated according to the total background intensity of the element to be detected in the sample to be detected.
3. The method of claim 1, wherein the plurality of nanocrystals on different spectrometers are the same type of nanocrystal.
4. The method of claim 1, wherein the plurality of spectroscopy crystals on different spectrometers are different spectroscopy crystals.
5. The method for improving characteristic X-ray intensity value according to claim 1, wherein the specific method for obtaining the total net count of the elements to be measured in the standard sample is as follows: and testing the characteristic X-ray total intensity and the background intensity of the element to be detected in the standard sample, calculating the net count of the element to be detected obtained by each light splitting crystal, and then calculating the total net count of the element to be detected in the standard sample.
6. The method for improving characteristic X-ray intensity as claimed in claim 1, wherein the specific method for obtaining the total net count of the elements to be measured in the sample to be measured is as follows: and testing the characteristic X-ray total intensity and the background intensity of the elements to be tested in the sample to be tested, calculating the net count of the elements to be tested obtained in each light splitting crystal, and then calculating the total net count of the elements to be tested in the sample to be tested.
7. The method as claimed in claim 1, wherein the concentration of the test element in the sample is calculated by the following formula:
wherein CY1 and CY2 … CYn (n is an integer more than or equal to 2) are a plurality of spectral crystals on different spectrometers respectively,
respectively the net count of the elements to be measured obtained in each spectroscope when the standard sample is tested,
respectively the net count of the elements to be tested, C, obtained in each spectroscopic crystal when testing the sample to be testedstdRepresenting the concentration of the element to be measured in the standard sample, GZAFRepresents the stromal correction factor, CunkThe concentration of the element to be detected in the sample to be detected is shown.
8. The method as claimed in claim 1, wherein the calculation formula of the total background intensity of the elements to be measured in the sample to be measured is:
wherein the content of the first and second substances,
respectively the background intensity, I, of the sample to be tested on each spectroscopic crystal when the sample to be tested is testedunk-bgIs the total background intensity of the elements to be measured.
9. The method as claimed in claim 2, wherein the detection limit of the element to be detected is calculated by the following formula:
wherein CY1 and CY2 … CYn (n is an integer more than or equal to 2) are multiple spectrocrystals on different spectrometers respectivelyThe body is provided with a plurality of grooves,
respectively, the net count of the elements to be measured of each spectroscopic crystal when testing the standard sample, CstdRepresents the concentration of the element to be measured in the standard sample,
the background intensity t of each spectroscopic crystal of the sample to be tested is measuredbackTest time for background, GZAFRepresents a matrix correction factor, and D.L. is a detection limit.
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