CN114047362A - Silicate ceramic composition detection method - Google Patents
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- CN114047362A CN114047362A CN202111312303.3A CN202111312303A CN114047362A CN 114047362 A CN114047362 A CN 114047362A CN 202111312303 A CN202111312303 A CN 202111312303A CN 114047362 A CN114047362 A CN 114047362A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 57
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000000203 mixture Substances 0.000 title claims abstract description 35
- 238000001514 detection method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000003822 epoxy resin Substances 0.000 claims abstract description 30
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 30
- 239000011707 mineral Substances 0.000 claims abstract description 30
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 30
- 238000001228 spectrum Methods 0.000 claims abstract description 15
- 239000011148 porous material Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 238000005498 polishing Methods 0.000 claims abstract description 3
- 238000005507 spraying Methods 0.000 claims abstract description 3
- 238000005259 measurement Methods 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 13
- 238000004814 ceramic processing Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000000113 differential scanning calorimetry Methods 0.000 description 4
- 229910052634 enstatite Inorganic materials 0.000 description 4
- BBCCCLINBSELLX-UHFFFAOYSA-N magnesium;dihydroxy(oxo)silane Chemical compound [Mg+2].O[Si](O)=O BBCCCLINBSELLX-UHFFFAOYSA-N 0.000 description 4
- 238000004445 quantitative analysis Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 238000003991 Rietveld refinement Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052604 silicate mineral Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010813 internal standard method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 238000011895 specific detection Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 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
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- CVPJXKJISAFJDU-UHFFFAOYSA-A nonacalcium;magnesium;hydrogen phosphate;iron(2+);hexaphosphate Chemical compound [Mg+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Fe+2].OP([O-])([O-])=O.OP([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O CVPJXKJISAFJDU-UHFFFAOYSA-A 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000000547 structure data Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052591 whitlockite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/02—Non-SPM analysing devices, e.g. SEM [Scanning Electron Microscope], spectrometer or optical microscope
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Radiology & Medical Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention belongs to the technical field of analysis and detection, and particularly discloses a method for detecting the composition of silicate ceramics. Firstly, cutting a silicate ceramic sample into blocks, then carrying out epoxy resin inlaying treatment on the block sample, and curing to obtain an epoxy resin polished section; polishing and spraying carbon on the epoxy resin polished section, and then measuring by adopting an MLA system to obtain a newly-built X-ray energy spectrum chart list; and (3) arranging and naming the newly-built X-ray energy spectrogram list, then carrying out phase classification on the measured data, and then calculating to obtain the mass percentage content of each crystalline phase mineral, amorphous phase and pore in the silicate ceramic sample. The method can evaluate the performance of the silicate ceramic by measuring the composition of the silicate ceramic, and provides theoretical basis and support for optimizing the ceramic processing technology.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to a method for detecting the composition of silicate ceramics.
Background
Silicate ceramics are a widely used inorganic non-metallic material, and the phase structure of the silicate ceramics mainly comprises a crystal phase, an amorphous phase and pores. The crystalline phase and the amorphous phase are the main composition phases of the silicate ceramic, and the content and the structure of the crystalline phase and the amorphous phase determine the main properties and the application of the silicate ceramic. The method for measuring the phase composition of the silicate ceramic, such as the mass content and the structural characteristics of the crystalline phase and the amorphous phase in the silicate ceramic, has important significance for evaluating the performance of the silicate ceramic, optimizing the ceramic processing technology and the like.
At present, the conventional methods for measuring the contents of crystalline phase and amorphous phase in silicate ceramics mainly comprise a micro lithofacies analysis method, an X-ray diffraction method, a differential scanning calorimetry method and the like. Wherein, the micro lithofacies analysis method is used for identifying the crystalline mineral and the structure thereof in the silicate ceramic according to the light transmission property of the crystalline mineral. The method can meet certain qualitative and quantitative requirements, but the identification of the crystalline phase and the amorphous phase depends on human vision, and has strong subjectivity and larger error. The X-ray diffraction method is a method for identifying the crystal phase of a ceramic sample widely applied at present, and can be combined with a K value method, an internal standard method, a Rietveld method and other methods to quantitatively analyze the crystal phase and the amorphous phase under certain conditions. However, the main components of the ceramic include a large amount of glassy substances and a small amount of pores in addition to a crystalline phase, the glassy phase in the ceramic is amorphous, there is no regular atomic array inside, only a wide amorphous peak is shown in an X-ray diffraction pattern, and the ratio of the crystalline peak to the amorphous peak area is used to calculate the crystallinity of the sample, which is relatively rough. The Rietveld method is to obtain fine structure data or quantitative information of a powder sample by least squares fitting of measured diffraction patterns, which is mainly applied to crystalline phases of known structure; although the Rietveld method can be combined with other techniques to determine the content of amorphous or unidentified phases, such as internal or external standard methods, the determination method is cumbersome and the error in the determination of low content phases is large. Differential Scanning Calorimetry (DSC) is a thermal analysis method that measures various thermodynamic and kinetic parameters, such as crystallization rate, crystallinity, etc., depending on the rate of heat absorption or release from a sample. The sintering temperature of the silicate ceramic sample is higher and usually exceeds the scanning temperature of DSC, and the DSC adopts an estimation method, so that the result error is large.
Based on the disadvantages of the prior art methods for measuring the phase composition of silicate ceramics, it is necessary to provide a method for measuring the phase composition of silicate ceramics in order to more accurately analyze the phase composition.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for detecting the composition of silicate ceramics so as to more accurately and conveniently detect and analyze the composition of silicate ceramics.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for detecting the composition of silicate ceramics comprises the following steps:
(1) cutting a silicate ceramic sample into blocks with the particle size of less than 10mm, then carrying out epoxy resin inlaying treatment on the block samples, and then curing to obtain epoxy resin polished sections;
(2) polishing the cured epoxy resin polished section, spraying carbon, and measuring by adopting an MLA system to obtain a newly-built X-ray energy spectrum chart list;
(3) arranging and naming the newly-built X-ray energy spectrogram list, wherein the naming of the crystalline phase minerals is completed in a database in an automatic matching way, and the naming of the amorphous phase minerals is completed by manual processing; because the X-ray energy spectrum of the amorphous phase is different from the spectrum of the crystalline phase mineral, the components of the amorphous phase are usually between several main silicate mineral raw materials, and the amorphous phase is usually filled between crystalline phases, the naming of the amorphous phase needs to be finished by manual treatment;
(4) and after the X-ray energy spectrum chart list is named, the measured data are subjected to phase classification, and then the mass percentage content of each crystalline phase mineral, amorphous phase and pore in the silicate ceramic sample is calculated according to the classification result.
In a preferred embodiment of the present invention, the MLA system model is MLA 650.
As a preferred embodiment of the present invention, the measurement conditions of the MLA system are: the SEM accelerating voltage is 20KV, and the beam spot is 7.0 nm.
In a preferred embodiment of the present invention, when the MLA system measures, the contrast and brightness of SEM are adjusted by selecting epoxy resin and metallic copper as gray scale samples in BSE mode, respectively, so that the gray value of epoxy resin is adjusted to 10 and the gray value of metallic copper is adjusted to 255.
In a preferred embodiment of the present invention, when the MLA system measures, a representative rectangular region is selected, a grid-type measurement mode is adopted, the image resolution is 500 × 500, the X-ray acquisition resolution is 2 × 2, the energy spectrometer residence time is 50ms, and the total time is not more than 30 minutes.
In a preferred embodiment of the present invention, the epoxy resin embedding process is a cold embedding process using an epoxy resin.
The invention provides a method for detecting the composition of silicate ceramics, which mainly measures the mass contents of a crystal phase, an amorphous phase and air holes in the silicate ceramics to obtain the mass percentage contents of minerals, the amorphous phase and the air holes of each crystal phase and obtain the microstructure characteristics of the silicate ceramics, namely the microstructure characteristics of three phases of the crystal phase, the amorphous phase and the air holes. By accurately measuring the phase composition of the silicate ceramic, the performance of the silicate ceramic can be evaluated, and a theoretical basis and support are provided for optimizing the ceramic processing technology, so that the method has important significance for improving the ceramic processing technology.
When the method is used for detection, the epoxy resin is used for cold-embedding treatment, and the prepared test sample can be effectively separated from the embedding agent background, so that the detection accuracy is ensured. During detection, in a BSE mode, epoxy resin and metal copper are respectively selected as gray scale samples to adjust the contrast and brightness of an SEM, the gray value of the epoxy resin is adjusted to 10, the gray value of the metal copper is adjusted to 255, and accurate detection can be achieved. By adopting the grid scanning measurement mode, the phases with extremely small gray difference can be distinguished, and when the gray difference between the silicate ceramic crystal phase and the amorphous phase is extremely small, particularly when the amorphous phase contains a fine crystalline phase, the accurate measurement of the three phases of the silicate ceramic can be realized by the grid scanning measurement mode.
Drawings
FIG. 1 is an MLA phase composition of a silicate ceramic sample of example 1 of the present invention;
FIG. 2 is a MLA phase composition of a silicate ceramic sample of example 2 of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail by the following specific examples.
Example 1
The embodiment detects a daily silicate ceramic sample, and the specific detection process is as follows:
the method comprises the following steps: cutting the ceramic sample into blocks with the diameter of less than 10mm, drying, and then carrying out cold embedding by using epoxy resin to prepare epoxy resin polished sections.
Step two: the cured epoxy resin sheets were polished, carbon-blasted, and then measured by an MLA system (model: MLA 650). Setting the accelerating voltage of the SEM to be 20KV, the beam spot to be 7.0nm, and respectively selecting epoxy resin and metal copper as gray scale samples in a BSE mode to adjust the contrast and brightness of the SEM, so that the gray scale value of the epoxy resin is adjusted to be 10, and the gray scale value of the metal copper is adjusted to be 255. Selecting a representative rectangular area, measuring the frame number to be 25, adopting a grid type measuring mode, wherein the image resolution is 500 × 500, the X-ray acquisition resolution is 2 × 2, the energy spectrometer residence time is 50ms, and the total time is not more than 30 minutes.
Step three: after MLA measurement is completed, a newly-built X-ray energy spectrogram list is sorted and named, the naming of crystalline phase minerals is automatically matched in a database, the X-ray energy spectrogram of an amorphous phase and the spectrogram of the crystalline phase minerals have differences, the components of the amorphous phase are usually between several main silicate mineral raw materials, the amorphous phase is usually filled between crystalline phases, and the naming is completed by manual processing.
Step four: after the X-ray energy spectrum chart lists are arranged and named, the phase classification is carried out on the measured data, each crystalline phase mineral, each amorphous phase and each pore are separated, and the accurate mass percentage content and the microstructure characteristics of each crystalline phase mineral, each amorphous phase and each pore in the ceramic sample are obtained through calculation according to the classification result. Among them, the MLA phase composition chart of the obtained ceramic sample is shown in FIG. 1, and the MLA phase composition analysis data is shown in Table 1 below.
TABLE 1
| Mineral composition | Mass content (wt%) | Mineral composition | Mass content (wt%) |
| Quartz | 23.00 | Hematite (iron ore) | 0.11 |
| Mullite | 17.98 | Air hole | 9.44 |
| Corundum | 0.35 | Others | 0.37 |
| Amorphous phase | 48.73 | Total up to | 100.00 |
| Rutile type | 0.03 |
Meanwhile, the ceramic sample is subjected to X-ray diffraction full-spectrum fitting quantitative analysis, and the analysis result is shown in Table 2.
TABLE 2 ceramic sample XRD full spectrum fit phase quantitative composition
| Mineral composition | Mass content (wt%) | Mineral composition | Mass content (wt%) |
| Quartz | 32.50 | Glass phase | 53.23 |
| Mullite | 14.26 | Total up to | 100.00 |
The ceramic samples were also chemically analyzed and compared to the MLA test results, which are shown in table 3. The MLA test results in Table 3 are obtained by converting the measurement results of the MLA phase composition.
TABLE 3 comparison of ceramic sample MLA test results with chemical analysis
| Mineral composition | MLA test (wt%) | Chemical analysis (wt%) |
| SiO2 | 69.98 | 71.10 |
| Al2O3 | 20.13 | 19.45 |
| K2O | 4.11 | 3.99 |
| Na2O | 2.16 | 2.33 |
The comparison shows that the method for measuring the whole minerals of the ceramic sample is adopted to measure the whole minerals, and the measurement result is closer to the chemical analysis result after conversion, so that the result is superior to the XRD full-spectrum fitting quantitative analysis method, which shows that the MLA test method of the invention has accurate result.
Example 2
In this embodiment, a silicate ceramic sample is detected, and the specific detection process is as follows:
the method comprises the following steps: cutting the ceramic sample into blocks with the diameter of less than 10mm, drying, and then carrying out cold embedding by using epoxy resin to prepare epoxy resin polished sections.
Step two: the cured epoxy resin sheets were polished, carbon-blasted, and then measured by an MLA system (model: MLA 650). Setting the accelerating voltage of the SEM to be 20KV, the beam spot to be 7.0nm, and respectively selecting epoxy resin and metal copper as gray scale samples in a BSE mode to adjust the contrast and brightness of the SEM, so that the gray scale value of the epoxy resin is adjusted to be 10, and the gray scale value of the metal copper is adjusted to be 255. Selecting a representative rectangular area, measuring the frame number to be 25, adopting a grid type measuring mode, wherein the image resolution is 500 × 500, the X-ray acquisition resolution is 2 × 2, the energy spectrometer residence time is 50ms, and the total time is not more than 30 minutes.
Step three: after MLA measurement is completed, a newly-built X-ray energy spectrogram list is sorted and named, the naming of crystalline phase minerals is automatically matched in a database, the X-ray energy spectrogram of an amorphous phase and the spectrogram of the crystalline phase minerals have differences, the components of the amorphous phase are usually between several main silicate mineral raw materials, the amorphous phase is usually filled between crystalline phases, and the naming is completed by manual processing.
Step four: after the X-ray energy spectrum chart lists are sorted and named, the phase classification is carried out on the measured data, and the accurate mass percentage content and the microstructure characteristics of crystalline phase minerals, amorphous phases and air holes in the sample are obtained through calculation according to the classification result. Among them, the MLA phase composition chart of the obtained ceramic sample is shown in FIG. 2, and the MLA phase composition analysis data is shown in Table 4 below.
TABLE 4
| Mineral composition | Mass content (wt%) | Mineral composition | Mass content (wt%) |
| Quartz | 9.44 | Brown curtain stone | 0.06 |
| Enstatite (enstatite) | 4.01 | Amorphous phase | 77.37 |
| Whitlockite | 0.31 | Air hole | 8.48 |
| Rutile type | 0.02 | Others | 0.23 |
| Ilmenite | 0.04 | Total up to | 100.00 |
Meanwhile, the ceramic sample is subjected to X-ray diffraction full-spectrum fitting quantitative analysis, and the analysis result is shown in Table 5.
TABLE 5 ceramic sample XRD full spectrum fit phase quantitative composition
| Mineral composition | Mass content (wt%) | Mineral composition | Mass content (wt%) |
| Quartz | 7.34 | Glass phase | 87.34 |
| Enstatite (enstatite) | 6.03 | Total up to | 100.00 |
The ceramic samples were also chemically analyzed and compared to the MLA test results, which are shown in table 6. The MLA test results in Table 6 were obtained by converting the measurement results of the MLA phase composition.
TABLE 6 comparison of ceramic sample MLA test results with chemical analysis
Similarly, it can be seen from the comparison that when the method of the present invention is used for carrying out the all-mineral determination on the ceramic sample, the determination result is closer to the chemical analysis result after conversion, so that the result is superior to the XRD full-spectrum fitting quantitative analysis method, which shows that the MLA test method of the present invention has accurate result.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (6)
1. A method for detecting the composition of silicate ceramics is characterized by comprising the following steps:
(1) cutting a silicate ceramic sample into blocks with the particle size of less than 10mm, then carrying out epoxy resin inlaying treatment on the block samples, and then curing to obtain epoxy resin polished sections;
(2) polishing the cured epoxy resin polished section, spraying carbon, and measuring by adopting an MLA system to obtain a newly-built X-ray energy spectrum chart list;
(3) arranging and naming the newly-built X-ray energy spectrogram list, wherein the naming of the crystalline phase minerals is completed in a database in an automatic matching way, and the naming of the amorphous phase minerals is completed by manual processing;
(4) and after the X-ray energy spectrum chart list is named, performing phase classification on the measured data, and calculating to obtain the mass percentage content of each crystalline phase mineral, amorphous phase and pore in the silicate ceramic sample.
2. The detection method according to claim 1, wherein the MLA system model is MLA 650.
3. The detection method according to claim 2, wherein the measurement conditions of the MLA system are: the SEM accelerating voltage is 20KV, and the beam spot is 7.0 nm.
4. The detection method as claimed in claim 3, wherein during measurement of the MLA system, epoxy resin and copper metal are respectively selected as gray scale samples in BSE mode to adjust contrast and brightness of SEM, so that the gray value of epoxy resin is adjusted to 10 and the gray value of copper metal is adjusted to 255.
5. The detection method according to claim 4, wherein when the MLA system measures, a representative rectangular region is selected, a grid-type measurement mode is adopted, the image resolution is 500 × 500, the X-ray acquisition resolution is 2 × 2, the spectrometer residence time is 50ms, and the total time is not more than 30 minutes.
6. The detection method according to any one of claims 1 to 5, wherein the epoxy resin embedding treatment is a cold embedding treatment using epoxy resin.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108226199A (en) * | 2016-12-14 | 2018-06-29 | 北京有色金属研究总院 | The method for quantitatively determining of tin anode mud material composition |
| JP2020153738A (en) * | 2019-03-19 | 2020-09-24 | 住友金属鉱山株式会社 | Method for acquiring data related to abundance ratio of mineral contained in sample |
| CN112557429A (en) * | 2020-12-15 | 2021-03-26 | 广东省科学院资源综合利用研究所 | Quantitative determination method for all minerals in graphite ore and sample preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108226199A (en) * | 2016-12-14 | 2018-06-29 | 北京有色金属研究总院 | The method for quantitatively determining of tin anode mud material composition |
| JP2020153738A (en) * | 2019-03-19 | 2020-09-24 | 住友金属鉱山株式会社 | Method for acquiring data related to abundance ratio of mineral contained in sample |
| CN112557429A (en) * | 2020-12-15 | 2021-03-26 | 广东省科学院资源综合利用研究所 | Quantitative determination method for all minerals in graphite ore and sample preparation method |
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