CN112748142A - Method for quantitatively analyzing beryllium content in-situ micro-area - Google Patents
Method for quantitatively analyzing beryllium content in-situ micro-area Download PDFInfo
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- 229910052790 beryllium Inorganic materials 0.000 title claims abstract description 49
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000523 sample Substances 0.000 claims abstract description 80
- 229910001767 beryllium mineral Inorganic materials 0.000 claims abstract description 26
- 230000003287 optical effect Effects 0.000 claims abstract description 20
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 18
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 238000004458 analytical method Methods 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims description 7
- PWOSZCQLSAMRQW-UHFFFAOYSA-N beryllium(2+) Chemical compound [Be+2] PWOSZCQLSAMRQW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 5
- 239000011707 mineral Substances 0.000 claims description 5
- 238000012113 quantitative test Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 238000004451 qualitative analysis Methods 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000010894 electron beam technology Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000007123 defense Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000000095 laser ablation inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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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]
-
- 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
- G01N23/2202—Preparing specimens therefor
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention belongs to the technical field of beryllium ore analysis and test, and particularly relates to a method for quantitatively analyzing beryllium content in an in-situ micro-area, which is used for collecting a beryllium ore sample; manufacturing a beryllium ore sample into a probe sheet or a light sheet; identifying beryllium minerals, and thermally evaporating a carbon film on the surface of a probe sheet or an optical sheet sample; and quantitatively analyzing the beryllium mineral in situ micro area. By configuring the light splitting crystal aiming at the large-size interplanar spacing of the ultra-light element and configuring the pulse height analyzer, the in-situ micro-area quantitative analysis of the beryllium mineral can be realized, the micron-level nondestructive analysis can be performed on the beryllium mineral, the acquisition of the component information of the beryllium mineral in the micro-area scale is facilitated, and by applying the testing method technology, the method has the advantages of no complex sample preparation process, in-situ micro-area, no damage, real-time performance, simplicity and convenience in operation, high sensitivity and the like.
Description
Technical Field
The invention belongs to the technical field of beryllium ore analysis and test, and particularly relates to a method for quantitatively analyzing beryllium content in an in-situ micro-area.
Background
Beryllium is the lightest alkaline earth element. The metallic beryllium and series products thereof are indispensable functional materials, structural materials and key raw materials in high-tech fields such as atomic energy, national defense and military industry, aerospace, metallurgical industry, automotive electronic equipment, high-end electrical appliances, telecommunication infrastructure, computers, new energy automobiles, medical treatment, oil and gas exploitation and the like, so that the metallic beryllium and series products thereof are known as 'space metal', 'top metal', 'super metal', 'nuclear reactor protection spirit'. Beryllium is in an extremely important position in systematic construction and strategic development of national defense and military core capacity and is an absolutely important strategic material because beryllium cannot be replaced by other materials; meanwhile, beryllium as a high-technology mineral product is a guarantee resource for the development of high and new industries, and the importance of beryllium is increasingly remarkable! Currently, beryllium production is concentrated in a few countries, and supply risks are increasing, so that people start to look at the resources more from the perspective of economic safety and national defense safety.
Beryllium is an ultra-light metal element, and quantitative testing of light and ultra-light elements has been an important and complex problem. At present, the beryllium detection method mainly comprises a wet chemical analysis method, a spectrophotometry method, an atomic absorption spectrometry, an electrochemical method, a secondary ion mass spectrometry, a laser ablation inductively coupled plasma mass spectrometry and the like, but the methods have larger defects. If the sample needs to Be dissolved and damaged, the requirement on the purity of the sample is higher, the determination method is complicated, the standard sample is lacked, the analysis error of the Be main quantity analysis is influenced by the substrate effect, and the like.
Disclosure of Invention
The invention aims to provide a method for quantitatively analyzing beryllium content in an in-situ micro-area, which can be used for rapidly and quantitatively analyzing the beryllium content in the in-situ micro-area in a lossless and real-time manner.
The technical scheme of the invention is as follows:
a method for quantitatively analyzing beryllium content in an in-situ micro-area comprises the following steps:
step 1) collecting a beryllium ore sample;
step 2), manufacturing a beryllium ore sample into a probe sheet or an optical sheet;
step 3) identifying beryllium minerals, and thermally evaporating a carbon film on the surface of a probe sheet or optical sheet sample;
step 4), quantitatively analyzing the beryllium mineral in-situ micro area;
4.1) selecting an analytical instrument and setting working conditions;
4.2) placing the probe sheet or optical sheet sample processed in the step 3) on a probe worktable for testing;
4.3) carrying out full spectrum qualitative analysis on the probe to judge each element KaWhether the peak shape affects the quantitative test of beryllium or not;
4.4) filtering other elements, high-beryllium high-order wire and beryllium element KαInterference of peaks
4.5) adopting a data processing method of subtracting the background counting intensity from the peak position counting intensity to quantitatively analyze the element concentration.
In the step 1), the specification of the sample is 2cm × 5cm × 8cm or 3cm × 6cm × 9 cm; the number of samples is 1-3.
In the step 2), the collected beryllium ore sample is mechanically ground and polished to be made into a probe piece or a light slice, and the specification of the probe piece is 2cm multiplied by 1 cm; the optical sheet specification was 2 cm. times.3 cm. times.0.3 mm.
In the step 3), the probe sheet or the optical sheet is subjected to mineral phase identification, suspected beryllium minerals are identified and defined, and then a carbon film is thermally evaporated on the surface of the probe sheet or the optical sheet sample.
In the step 4), an instrument is selected as an Shimadzu electronic probe EPMA-1720.
In the step 4), the ambient temperature is 18-28 ℃, and the humidity is 30-60% RH; the X-ray detection angle is 52.5 degrees; the accelerating voltage is 10-15 kV; the beam current is 50-200 nA; the test time is background 50s, element 100s, and peak shape analysis is 1 s/point; the beam spot diameter was 1 μm.
In the step 4), the pulse height analyzer is used for filtering and eliminating K of the high-order pairs of the silicon elements to the berylliumαPeak-shaped interference.
In the step 4.5), the electron probe uses a fine focused electron beam to enter the surface of the sample to excite the characteristic X-ray of the sample element, the type of the element contained in the sample can be known by analyzing the wavelength of the characteristic X-ray, and the content of the corresponding element in the sample can be known by analyzing the intensity of the X-ray.
And in the step 4.5), beryllium element peak searching is carried out on each test point in the quantitative test process.
The invention has the following remarkable effects:
by applying a modern electronic probe, the in-situ micro-area quantitative analysis of the beryllium mineral can be realized by configuring the light splitting crystal aiming at the large-size crystal face spacing of the ultra-light element and configuring the pulse height analyzer, the micron-level nondestructive analysis can be performed on the beryllium mineral, the acquisition of the component information of the beryllium mineral in the micro-area scale is facilitated, and the method has important theoretical and practical significance for identifying the type of the beryllium mineral, knowing the geochemistry property of the beryllium mineral, determining or optimizing the beryllium mineral mining scheme, researching the mineral-forming mechanism and exploring the resource distribution. Meanwhile, the testing method technology has no complex sample preparation process, and has the advantages of in-situ, micro-area, no damage, real-time, simple and convenient operation, high sensitivity and the like.
Drawings
FIG. 1 is a flow chart of the method.
Detailed Description
The invention is further illustrated by the accompanying drawings and the detailed description.
Step one, collecting a beryllium ore sample;
beryllium ore samples were collected by field geological investigation or investigation. The sample specification is 2cm multiplied by 5cm multiplied by 8cm or 3cm multiplied by 6cm multiplied by 9 cm; the number of samples is 1-3; due to the in-situ micro-area quantitative analysis, one beryllium mineral (i.e. one sample) can meet the test requirement. In order to prevent the influence of unforeseeable factors (such as sample breakage in the sample preparation process, diversity of beryllium mineral types, statistical requirements and the like), more than two samples are recommended to be collected.
Step two, manufacturing a probe sheet or an optical sheet;
and (3) mechanically grinding and polishing the beryllium ore sample collected in the step one to prepare a probe sheet or an optical sheet. The specification of the probe sheet is 2cm multiplied by 1 cm; the optical sheet specification was 2 cm. times.3 cm. times.0.3 mm.
Step three, observing under a mirror (identifying mineral phases) and preprocessing samples before testing;
observing the probe sheet or the optical sheet manufactured in the step two under a mirror (identifying the mineral phase), and identifying and delineating suspected beryllium minerals; then, a carbon film (or a gold plating film) is thermally deposited on the surface of the probe sheet or the optical sheet sample.
Fourthly, carrying out quantitative analysis of beryllium mineral in-situ micro-area
And (4) carrying out quantitative analysis on the beryllium mineral in-situ micro-area on the probe sheet or the optical sheet sample processed in the third step.
The method specifically comprises the following steps:
4.1) selecting an analytical instrument and setting working conditions.
Selecting an instrument as an Shimadzu electronic probe EPMA-1720, and simultaneously providing an LSA200/LSA300 spectroscopic crystal and a pulse height analyzer; the working (laboratory) environment temperature is 18-28 ℃, and the humidity is 30-60% RH; the X-ray detection angle is 52.5 degrees; acceleration voltage: 10-15 kV; beam current: 50-200 nA; and (3) testing time: background 50s, element 100s, peak shape analysis 1 s/point; beam spot diameter: 1 μm.
4.2) according to the operation protocol of the Shimadzu electronic probe EPMA-1720, putting the probe sheet or the optical sheet sample processed in the step three into a test bench, and finding out the (suspected) beryllium mineral to be tested.
4.3) before quantitative analysis is carried out, a spectrometer (WDS: wavelet Dispersive Spectrometer), analyzing element composition and each element spectrogram, and determining each element KaWhether the peak shape affects the quantitative measurement of beryllium (line interference is common in electronic probes, especially prominent in ultra-light element analysis, and KaLine is the only line system to choose from in ultralight element spectroscopy).
4.4) filtering other elements, high-beryllium high-order wire and beryllium element KαInterference of peaks.
The beryllium mineral is composed of elements of Si, Al, O, Be, Fe, Mg, Cr, K, Na and Ca, and usually the higher-order line of the Si element is opposite to the K of BeαThe peak shape has interference, and a Pulse Height Analyzer (Pulse Height Analyzer) is used for filtering and eliminating K of the high-order line of the silicon element to berylliumαPeak-shaped interference.
4.5) carrying out qualitative analysis and filtering on K of beryllium by high-order lines of silicon elementsαAnd (4) after the interference of the peak shape, further carrying out element quantitative analysis on the beryllium mineral.
The electron probe uses the fine focusing electron beam to irradiate the surface of the sample, so as to excite the characteristic X ray of the sample element, the kind of the element contained in the sample can be known by analyzing the wavelength of the characteristic X ray (qualitative analysis), and the content of the corresponding element in the sample can be known by analyzing the intensity of the X ray (quantitative analysis). The calculation of the element concentration in the quantitative analysis adopts a data processing method of subtracting the background counting intensity from the peak counting intensity. Meanwhile, beryllium element peak searching is carried out on each test point in the quantitative test process in order to obtain a more accurate test result.
The quantitative analysis result shows that the beryllium mineral in the beryllium ore sample is sapphire. It is mainly composed of O, Si, Al and Be elements, and contains a small amount of Na, K, Fe, Mg, Ca and Cr. SiO 22The content is 65.74-66.13 percent (average is 65.98 percent) and Al2O317.58 to 17.84 percent (average of 17.73 percent), 14.23 to 14.85 percent of BeO (average of 14.49 percent), 0.31 to 0.40 percent of FeO (average of 0.36 percent), 0.14 to 0.17 percent of MgO (average of 0.15 percent), and Na2The content of O is 0.21-0.23 percent (average is 0.22 percent) and K20.01 to 0.04 percent of O (average of 0.03 percent), 0.00 to 0.02 percent of CaO (average of 0.01 percent) and 0.00 to 0.02 percent of CrO (average of 0.01 percent). The content change of each element is small, which shows that the analysis result is accurate.
The present invention has been described in detail with reference to the drawings and examples, but the present invention is not limited to the examples, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. The prior art can be adopted in the content which is not described in detail in the invention.
Claims (9)
1. A method for quantitatively analyzing beryllium content in an in-situ micro-area is characterized by comprising the following steps:
step 1) collecting a beryllium ore sample;
step 2), manufacturing a beryllium ore sample into a probe sheet or an optical sheet;
step 3) identifying beryllium minerals, and thermally evaporating a carbon film on the surface of a probe sheet or optical sheet sample;
step 4), quantitatively analyzing the beryllium mineral in-situ micro area;
4.1) selecting an analytical instrument and setting working conditions;
4.2) placing the probe sheet or optical sheet sample processed in the step 3) on a probe worktable for testing;
4.3) carrying out full spectrum qualitative analysis on the probe to judge each element KaWhether the peak shape affects the quantitative test of beryllium or not;
4.4) filtering other elements, high-beryllium high-order wire and beryllium element KαInterference of peaks
4.5) adopting a data processing method of subtracting the background counting intensity from the peak position counting intensity to quantitatively analyze the element concentration.
2. The method for in-situ micro-area quantitative analysis of beryllium content as claimed in claim 1, wherein: in the step 1), the specification of the sample is 2cm × 5cm × 8cm or 3cm × 6cm × 9 cm; the number of samples is 1-3.
3. The method for in-situ micro-area quantitative analysis of beryllium content as claimed in claim 2, wherein: in the step 2), the collected beryllium ore sample is mechanically ground and polished to be made into a probe piece or a light slice, and the specification of the probe piece is 2cm multiplied by 1 cm; the optical sheet specification was 2 cm. times.3 cm. times.0.3 mm.
4. The method for in-situ micro-area quantitative analysis of beryllium content as claimed in claim 3, wherein: in the step 3), the probe sheet or the optical sheet is subjected to mineral phase identification, suspected beryllium minerals are identified and defined, and then a carbon film is thermally evaporated on the surface of the probe sheet or the optical sheet sample.
5. The method for in-situ micro-area quantitative analysis of beryllium content as claimed in claim 4, wherein: in the step 4), an instrument is selected as an Shimadzu electronic probe EPMA-1720.
6. The method for in-situ micro-area quantitative analysis of beryllium content as claimed in claim 4, wherein: in the step 4), the ambient temperature is 18-28 ℃, and the humidity is 30-60% RH; the X-ray detection angle is 52.5 degrees; the accelerating voltage is 10-15 kV; the beam current is 50-200 nA; the test time is background 50s, element 100s, and peak shape analysis is 1 s/point; the beam spot diameter was 1 μm.
7. The method for in-situ micro-area quantitative analysis of beryllium content as claimed in claim 4, wherein: in the step 4), the pulse height analyzer is used for filtering and eliminating K of the high-order pairs of the silicon elements to the berylliumαPeak-shaped interference.
8. The method for in-situ micro-area quantitative analysis of beryllium content as claimed in claim 4, wherein: in the step 4.5), the electron probe uses a fine focused electron beam to enter the surface of the sample to excite the characteristic X-ray of the sample element, the type of the element contained in the sample can be known by analyzing the wavelength of the characteristic X-ray, and the content of the corresponding element in the sample can be known by analyzing the intensity of the X-ray.
9. The method for in-situ micro-area quantitative analysis of beryllium content as claimed in claim 8, wherein: and in the step 4.5), beryllium element peak searching is carried out on each test point in the quantitative test process.
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| CN114295663A (en) * | 2021-12-28 | 2022-04-08 | 自然资源部第二海洋研究所 | Magnesium-based electron probe microbeam component analysis standard sample and preparation method thereof |
| CN118225771A (en) * | 2024-05-23 | 2024-06-21 | 洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所) | High-flux assessment method for non-uniformity of performance of large-wall-thickness structural cast steel |
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| 赵同新等: "电子探针对含Be矿物绿柱石的定量分析", 《矿物学报》 * |
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| CN114295663A (en) * | 2021-12-28 | 2022-04-08 | 自然资源部第二海洋研究所 | Magnesium-based electron probe microbeam component analysis standard sample and preparation method thereof |
| CN118225771A (en) * | 2024-05-23 | 2024-06-21 | 洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所) | High-flux assessment method for non-uniformity of performance of large-wall-thickness structural cast steel |
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