CN111175324A - application of analysis line start-stop angle in measuring α -quartz phase content - Google Patents
application of analysis line start-stop angle in measuring α -quartz phase content Download PDFInfo
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- CN111175324A CN111175324A CN202010012184.9A CN202010012184A CN111175324A CN 111175324 A CN111175324 A CN 111175324A CN 202010012184 A CN202010012184 A CN 202010012184A CN 111175324 A CN111175324 A CN 111175324A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 229910021489 α-quartz Inorganic materials 0.000 title claims abstract description 92
- 238000004458 analytical method Methods 0.000 title claims description 23
- 238000000034 method Methods 0.000 claims abstract description 33
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052802 copper Inorganic materials 0.000 claims abstract description 31
- 239000010949 copper Substances 0.000 claims abstract description 31
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 28
- 238000005259 measurement Methods 0.000 claims abstract description 22
- 239000011449 brick Substances 0.000 claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 14
- 238000004364 calculation method Methods 0.000 claims description 21
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000011068 loading method Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052710 silicon Inorganic materials 0.000 abstract description 7
- 239000010703 silicon Substances 0.000 abstract description 7
- 239000013077 target material Substances 0.000 abstract description 6
- 239000011819 refractory material Substances 0.000 abstract description 4
- 238000004445 quantitative analysis Methods 0.000 abstract description 3
- 239000010453 quartz Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 11
- 235000012239 silicon dioxide Nutrition 0.000 description 10
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 2
- 229910016523 CuKa Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910021427 silicon allotrope Inorganic materials 0.000 description 1
- 238000010998 test method Methods 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth 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 avoids the diffraction peak of non- α -quartz phase existing between 26.3 DEG and 27.4 DEG in the α -quartz phase quantitative analysis and measurement of the actual silicon brick sample, so as to obviously improve the accuracy of the α -quartz phase content calculated by measurement, and improves the accuracy of the copper target material X-ray diffraction method for measuring the α -quartz phase content from the test principle, therefore, the domestic standard α -quartz sample is adopted in the actual silicon brick sample test process to replace the α -quartz standard sample produced by the existing American refractory material standard sample Association, and better test results can be obtained, thereby greatly reducing the cost of the actual silicon brick sample test.
Description
Technical Field
the invention relates to application of quantitative phase analysis X-ray diffraction method for measuring α -quartz phase content in silicon bricks in metallurgical industry, in particular to application of an analysis line start-stop angle in measurement of α -quartz phase content.
Background
the silica brick is one of important compositions of refractory materials, the silica brick generally contains tridymite, cristobalite, α -quartz (commonly called residual quartz) and amorphous phase, the tridymite, the cristobalite and the α -quartz are allotropes of silicon dioxide, the content of the α -quartz phase is an important index of the silica brick and directly influences the high-temperature use performance of the silica brick, the quality technology of the silica brick requires that the α -quartz phase is transformed as much as possible, the domestic general design requires that the content of the residual α -quartz phase is not more than 1 percent, so the quantitative analysis of the content of the α -quartz phase in the silica brick is particularly important, the YB172/2000 standard specifies an analysis method of the content of the α -quartz phase, and the analysis lines are selected from 101 surfaces for the α -quartz, namely a CoKa cobalt target material of 30.5 to 31.5 degrees and a CuKa copper target material of 26.0 to 27.0 degrees.
however, in the actual measurement, when the copper target material X-ray diffraction method is used for measuring the alpha-quartz phase, the standard sample only has the characteristic peak of the alpha-quartz phase between 26 degrees and 27 degrees, but when the actual silica brick sample is tested, a diffraction peak which is not α -quartz phase exists between 26.3 degrees and 27.4 degrees, when the integral method is used for calculating the intensity of the alpha-quartz phase diffraction peak, the analysis line integral calculation angle adopts 26.0 degrees to 27.0 degrees to calculate the diffraction peak of the non-alpha-quartz phase, so that the calculated alpha-quartz phase content is higher, and the accuracy of the measurement result of the residual alpha-quartz phase in the silica brick is influenced.
Disclosure of Invention
in order to overcome the defects in the background art, the invention discloses the application of the start and stop angles of an analysis line in measuring α -quartz phase content, the initial angle of the integral calculation of the diffraction peak intensity is 26.5 degrees, and the end angle of the integral calculation of the diffraction peak intensity is 27.0 degrees.
in order to achieve the purpose, the invention adopts the following technical scheme that the starting angle and the stopping angle of an analysis line are applied to measuring α -quartz phase content, the starting angle of the peak integral calculation in the alpha-quartz phase diffraction pattern is 26.5 degrees, and the stopping angle of the peak integral calculation in the alpha-quartz phase diffraction pattern is 27.0 degrees.
Further, the specific measurement steps are as follows: removing the skin of a sample to be tested and a standard sample, reducing by a quartering method, and grinding to 50 g of 0.045MM powder sample; preparing 5 sample sheets by a back-loading method, wherein the test surfaces of the sample sheets are smooth, the sample loading density is uniform, and the thickness is consistent; scanning the prepared sample sheet by a copper target X-ray diffraction method, wherein the scanning speed is less than 1 degree/min, the divergence slit is 1 degree, and the acceptance slit is 0.3 mm; the initial scanning angle is 19 degrees, and the scanning termination angle is 29 degrees; performing diffraction intensity integral calculation on the diffraction pattern obtained after scanning, wherein the integral calculation starting angle is 26.5 degrees, and the integral calculation ending angle is 27.0 degrees;
the alpha-quartz phase content is calculated by the formula of Wx ═ Ix × (μm)/(Ix) o × (μm) o,
wherein Wx is the content of alpha-quartz phase in the sample to be detected;
ix is the diffraction intensity of α -quartz phase analysis line in the sample to be detected;
(Ix) o is the diffraction intensity of the analytical line of the standard sample;
(mum) is the mass absorption coefficient of the sample to be measured, and the unit is square centimeter/gram;
(mum) o is the standard sample mass absorption coefficient in square centimeters per gram;
wherein the sample to be tested is silica brick, the standard sample is α -quartz standard sample, and if no other phase exists except tridymite, cristobalite and residual quartz in the test sample, (mu m)/(mu m) o is approximately 1.
the method for calculating the difference between α -quartz phase content measured by applying the starting and stopping angles of the analysis lines in the measurement of α -quartz phase content and the alpha 0-quartz phase content specified by the YB172/2000 standard causes diffraction only when the difference between optical paths irradiating two adjacent crystal planes is n times of the wavelength of X-rays through the Bragg equation 2dsin theta of the X-ray diffraction mineral phase, and the alpha 1-quartz phase is used as the alpha 2-quartz in the X-ray diffraction of the copper target, the spacing d of the crystal planes is the integral multiple of the X-ray wavelength lambda under the irradiation of the X-ray wavelength lambda of the copper target, so that the diffraction peak exists between 26.3 DEG and 27.4 DEG of the diffraction map when the copper target is actually measured, and the diffraction peak does not exist between the alpha 4-quartz phase and 27.4 DEG of the diffraction map when the copper target is actually measured, and the diffraction peak exists between 26.3 DEG and 27.4 DEG of the diffraction map when the copper target is actually measured, and the quartz phase is observed, the quartz phase is found to be not the crystal phase when the crystal phase is actually measured, the crystal phase is found to be the crystal phase, the crystal phase diffraction peak, the crystal phase is calculated from the crystal phase diffraction peak of the quartz phase, the crystal phase calculated by applying the standard diffraction index alpha 2-quartz-n DEG, the quartz-crystal diffraction mineral phase, the standard diffraction mineral phase diffraction mineral-quartz.
by applying the method disclosed by the invention and comparing with an analysis method of α -quartz phase content specified by YB172/2000 standard, results of the alpha-quartz phase content in the range of 0-1.0% are analyzed through experimental measurement, and the method is specifically shown in the following table:
the sample with the α -quartz phase content of 0-1.0% is prepared by mixing an α -quartz standard sample and a standard phosphorosilicate sample produced by American refractory material standard sample Association according to a weight ratio, and the comparison in the table shows that the deviation of the experimental measurement result is obviously smaller than the analysis method of the α -quartz phase content specified by YB172/2000 standard when the α -quartz phase content is within the range of 0-1.0%.
in addition, by applying the method disclosed by the invention and comparing with an analysis method of α -quartz phase content specified by the YB172/2000 standard, the test result that α -quartz phase content is 5% is measured and analyzed through experiments, and the method is specifically shown in the following table:
the comparison results in the table show that the average value of the experimental measurement results of the invention is 5.04% and the deviation is 0.8% when the content of the alpha-quartz phase is 5%, and the average value of the experimental measurement results of the analytical method of the content of the alpha-quartz phase specified by the YB172/2000 standard is 5.92% and the deviation is as high as 18.4%.
the invention has the advantages that the application of the start-stop angle of the analysis line in measuring α -quartz phase content has the diffraction peak intensity integral calculation start angle of 26.5 degrees and the diffraction peak intensity integral calculation stop angle of 27.0 degrees, avoids the diffraction peak of the non-alpha-quartz phase existing between 26.3 and 27.4 degrees in the actual alpha-quartz phase quantitative analysis and measurement of the silicon brick sample, obviously improves the accuracy of the alpha-quartz phase content calculated by measurement, improves the accuracy of the alpha-quartz phase content by the copper target X-ray diffraction method in the measurement principle, adopts the domestic standard alpha-quartz sample with higher phosphorus quartz phase content in the actual silicon brick sample test process, replaces the alpha-quartz standard sample produced by the existing American refractory material standard sample Association, and can obtain better test results, thereby greatly reducing the cost of the actual silicon brick sample test.
Drawings
FIG. 1 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method of a No. 1 sample copper target;
FIG. 2 is a 2# sample copper target X-ray diffraction method measured alpha-quartz phase diffraction pattern;
FIG. 3 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method of a 3# sample copper target;
FIG. 4 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method of a 4# sample copper target;
FIG. 5 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method of 5# sample copper target;
FIG. 6 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method of a No. 6 sample copper target;
FIG. 7 is a 7# sample copper target material X-ray diffraction method measured alpha-quartz phase diffraction pattern;
FIG. 8 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method of copper target of No. 8 sample;
FIG. 9 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method for copper target 9# sample;
FIG. 10 is a 10# sample copper target X-ray diffraction pattern of alpha-quartz phase;
FIG. 11 is a 11# sample copper target X-ray diffraction pattern for alpha-quartz phase measurement;
FIG. 12 is a 12# sample copper target X-ray diffraction pattern of alpha-quartz phase;
FIG. 13 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method for copper target 13# sample;
FIG. 14 is a 14# sample copper target X-ray diffraction method measured alpha-quartz phase diffraction pattern;
FIG. 15 is a diffraction pattern of a 15# sample copper target measured by X-ray diffraction method for alpha-quartz phase;
FIG. 16 is a 16# sample copper target X-ray diffractometry α -quartz phase diffraction pattern;
FIG. 17 is a 17# sample copper target X-ray diffraction pattern for alpha-quartz phase measurement;
FIG. 18 is a diffraction pattern of alpha-quartz phase measured by X-ray diffraction method for 18# sample copper target;
FIG. 19 is a diffraction pattern of tridymite phase measured by X-ray diffraction method for copper target material;
Detailed Description
The present invention will be explained in detail by the following examples, which are disclosed for the purpose of protecting all technical improvements within the scope of the present invention.
the application of the start and stop angles of the analysis lines in the measurement of the α -quartz phase content is characterized in that the start angle of peak integral calculation in an α -quartz phase diffraction pattern is 26.5 degrees, and the stop angle of peak integral calculation in the α -quartz phase diffraction pattern is 27.0 degrees.
Removing the skin of a sample to be tested and a standard sample, reducing by a quartering method, and grinding to 50 g of 0.045MM powder sample; preparing 5 sample sheets by a back-loading method, wherein the test surfaces of the sample sheets are smooth, the sample loading density is uniform, and the thickness is consistent; scanning the prepared sample sheet by a copper target X-ray diffraction method, wherein the scanning speed is less than 1 degree/min, the divergence slit is 1 degree, and the acceptance slit is 0.3 mm; the initial scanning angle is 19 degrees, and the scanning termination angle is 29 degrees; performing diffraction intensity integral calculation on the diffraction pattern obtained after scanning, wherein the integral calculation starting angle is 26.5 degrees, and the integral calculation ending angle is 27.0 degrees;
the alpha-quartz phase content is calculated by the formula of Wx ═ Ix ([ mu ] m)/(Ix) o [ [ mu ] m ] o [ ]
wherein Wx is the content of alpha-quartz phase in the sample to be detected;
ix is the diffraction intensity of α -quartz phase analysis line in the sample to be detected;
(Ix) o is the diffraction intensity of the analytical line of the standard sample;
(mum) is the mass absorption coefficient of the sample to be measured, and the unit is square centimeter/gram;
(mum) o is the standard sample mass absorption coefficient in square centimeters per gram;
the preparation, test and calculation methods of the sample piece are the same as those of the sample to be tested;
the content of α -quartz phase is in a range of 0-1.0% according to experimental measurement analysis, and alpha-quartz phase content measurement specified by a YB172/2000 standard is compared, wherein a sample with the content of α -quartz phase in a range of 0-1.0% is prepared by mixing an alpha-quartz standard sample and a standard phosphorosilicate sample produced by American refractory standard sample Association in a weight ratio, phases except tridymite, cristobalite and residual quartz are not found in the sample in the test, and the phase (mum)/(mum) o is approximately equal to 1, and specific results are shown in the following table:
in addition, according to the method, the content of α -quartz phase is 5.0 percent through experimental measurement analysis, and α -quartz phase content measurement specified by a comparative YB172/2000 standard is carried out, wherein the sample with the content of α -quartz phase of 5 percent is prepared by mixing an alpha-quartz standard sample produced by American society for fire-resistant materials standard sample and a standard quartz sample in a weight ratio, and phases except tridymite, cristobalite and residual quartz are not found in the sample in the test, and the phase (mum)/(mum) o is approximately equal to 1, and the specific results are shown in the following table:
the present invention is not described in detail in the prior art.
Claims (2)
1. the application of the start-stop angle of an analysis line in measuring α -quartz phase content is characterized in that the start angle of peak integral calculation in an alpha-quartz phase diffraction pattern is 26.5 degrees, and the stop angle of peak integral calculation in the alpha-quartz phase diffraction pattern is 27.0 degrees.
2. the application of the start-stop angle of the analysis line in the measurement of the alpha-quartz phase content of claim 1 is characterized in that a sample to be measured and a standard sample are subjected to surface removal, are subjected to shrinkage by a quartering method and are ground to 50 g of 0.045MM powder sample, 5 sample pieces are prepared by a back-loading method, the test surfaces of the sample pieces are flat, the loading density is uniform, and the thickness is consistent, the prepared sample pieces are subjected to scanning by a copper target X-ray diffraction method, the scanning speed is less than 1 degree/min, a divergent slit is selected to be 1 degree, a receiving slit is selected to be 0.3MM, the initial scanning angle is 19 degrees, the scanning stop angle is 29 degrees, the diffraction intensity integral calculation is performed on the diffraction pattern obtained after scanning, the integral calculation initial angle is 26.5 degrees, and the integral calculation stop angle is 27.0 degrees;
the alpha-quartz phase content is calculated by the formula of Wx ═ Ix ([ mu ] m)/(Ix) o [ [ mu ] m ] o [ ]
wherein Wx is the content of alpha-quartz phase in the sample to be detected;
ix is the diffraction intensity of α -quartz phase analysis line in the sample to be detected;
(Ix) o is the diffraction intensity of the analytical line of the standard sample;
(mum) is the mass absorption coefficient of the sample to be measured, and the unit is square centimeter/gram;
(mum) o is the standard sample mass absorption coefficient in square centimeters per gram;
wherein the sample to be tested is a silica brick to be tested, and the standard sample is an α -quartz standard sample.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4592082A (en) * | 1984-08-10 | 1986-05-27 | The United States Of America As Represented By The United States Department Of Energy | Quantitative determination of mineral composition by powder X-ray diffraction |
| CN1473139A (en) * | 2001-06-27 | 2004-02-04 | 日本碍子株式会社 | Low-temperature fired porcelain and electronic component |
| US20170368486A1 (en) * | 2014-12-19 | 2017-12-28 | Ep Minerals, Llc | Opaline biogenic silica/expanded perlite composite products |
| US20210057778A1 (en) * | 2019-08-19 | 2021-02-25 | Zhejiang The Light Of Heaven-Earth Battery Manufacturing Co., Ltd. | Electrolyte Solution of Lead-Crystal Storage Battery, Preparation Method Thereof, and Lead-Crystal Storage Battery |
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2020
- 2020-01-07 CN CN202010012184.9A patent/CN111175324B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4592082A (en) * | 1984-08-10 | 1986-05-27 | The United States Of America As Represented By The United States Department Of Energy | Quantitative determination of mineral composition by powder X-ray diffraction |
| CN1473139A (en) * | 2001-06-27 | 2004-02-04 | 日本碍子株式会社 | Low-temperature fired porcelain and electronic component |
| US20170368486A1 (en) * | 2014-12-19 | 2017-12-28 | Ep Minerals, Llc | Opaline biogenic silica/expanded perlite composite products |
| US20210057778A1 (en) * | 2019-08-19 | 2021-02-25 | Zhejiang The Light Of Heaven-Earth Battery Manufacturing Co., Ltd. | Electrolyte Solution of Lead-Crystal Storage Battery, Preparation Method Thereof, and Lead-Crystal Storage Battery |
Non-Patent Citations (1)
| Title |
|---|
| 程玉海: "X线衍射法测定粉尘中游离二氧化硅含量", 《中华劳动卫生职业病杂志》 * |
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