CN102175557B - Method for testing trace impurities in ultrahigh-purity graphite - Google Patents
Method for testing trace impurities in ultrahigh-purity graphite Download PDFInfo
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- CN102175557B CN102175557B CN201110056199A CN201110056199A CN102175557B CN 102175557 B CN102175557 B CN 102175557B CN 201110056199 A CN201110056199 A CN 201110056199A CN 201110056199 A CN201110056199 A CN 201110056199A CN 102175557 B CN102175557 B CN 102175557B
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- 238000012360 testing method Methods 0.000 title claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000012535 impurity Substances 0.000 title claims abstract description 19
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 17
- 239000010439 graphite Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 16
- 230000008774 maternal effect Effects 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 abstract description 5
- 239000010432 diamond Substances 0.000 abstract description 5
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 8
- 238000010998 test method Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for testing trace impurities in ultrahigh-purity graphite. The method comprises the following steps of: A, enlarging the quantity of female parents of a sample to 4-5 times that of the female parents of the sample specified in GB/T8133.17-1999; B, testing the fluctuation ratio k before high-temperature calcination and after calcination of a ceramic crucible for accommodating the sample, wherein the value of the fluctuation ratio k is tested by using a sample cup, and the temperature is controlled at 800-850 DEG C; and C, adding a fluctuation ratio factor, i.e., A=(G1-G2*k)/GX100% into a calculation formula of a test result, wherein A refers to ash content or impurity content; G is the quantity of the female parents of the sample; G1 is the total weight of the ceramic crucible and sample residues after calcination; G2 is the weight of the ceramic crucible for accommodating the sample; and K is the fluctuation ratio of the sample cup of the ceramic crucible before and after calcination. The method is practicable, simple in equipment, convenient to operate, and suitable for testing the impurity content of purified graphite powder for synthesizing diamond and graphite with the purity of over 99.99 percent.
Description
Technical field
The present invention relates to carbon element industry technology field; The method of testing that more specifically relates to the trace impurity content in a kind of ultra-high purity graphite; Can be widely used in diamond synthesis and be higher than the mensuration of the impurity content of 4 graphite more than 9 (99.99%), especially in the sample analysis of impurity content, test result accurately is provided less than 20ppm with purifying dag and purity.
Background technology
The goods of carbon and graphite and the ash content of material thereof are called the analytical test of impurity content again, in general, all are to carry out according to the analytical test method of standard GB/T8133.17-1999 regulation.But; For the test of the trace impurity content in the ultra-high purity graphite, for example diamond synthesis is used the purifying dag, the graphite for reactor of nuclear power station; The monocrystalline silicon thermal field is with graphite etc.; According to said method analyze, will feel that the test findings error is too big, the layman often is difficult to according to said method provide analytical test result accurately. draw the test findings that numerical value is negative sometimes even.
It is unexpected that principal element have 2 points, and the one, the impurity content in the sample is small especially, and for example diamond synthesis is used the purifying dag, domestic standard requirement≤30ppm; American-European standard-required≤20ppm; West standard-required≤the 10ppm of Cree Inc.; The graphite for reactor of nuclear power station, its technical standard requirement≤5ppm; The monocrystalline silicon thermal field is with the technical standard requirement≤50ppm of graphite; Second it be that the test error of analytical test method of GB/T8133.17-1999 regulation is bigger.
The ceramic crucible of the splendid attire sample that is adopted in this analytical test method,, before high temperature sintering, the weight differential after the calcination is bigger.And each weight behind high temperature sintering, all can change irregular seeking because of residing environment temperature in the cooling procedure is different with humidity.In order to lower its rate of change before and after the high temperature sintering as far as possible, professional scientific research institution can adopt that expensive rare metal---platinum is made the crucible of splendid attire sample, but as the common engineering manufacturing industry, it is obviously too high that it detects cost.
Summary of the invention
The objective of the invention is to be to provide a kind of method of testing of ultra-high purity graphite trace impurity content, method is easy, and is fast, accurately with low cost, solved the too big problem of test findings error of the analytical test method of GB/T8133.17-1999 regulation.
In order to reach above-mentioned purpose, the present invention adopts following technical measures:
The maternal quantity of sample is strengthened, the ceramic crucible of test splendid attire sample before high temperature sintering with calcination after rate of change k, in the computing formula of test findings, add the rate of change factor, thus greatly the raising of degree measuring accuracy.
A kind of method of testing of ultra-high purity graphite trace impurity comprises the following steps:
A, the maternal quantity of sample is increased to 4～5 times of maternal quantity of the sample of GB/T8133.17-1999 regulation;
The ceramic crucible of B, test splendid attire sample before high temperature sintering with calcination after rate of change k, its value by the appearance cup test it, temperature is controlled at 800～850 ℃;
C adds the rate of change factor in the computing formula of test findings, specific as follows:
A = (G1－G2*k)?/?G?X?100%
In the formula: A---ash content or impurity content;
The maternal weight of G---sample;
G1---the ceramic crucible after the calcination and the weight of sample residue;
G2---the weight of the ceramic crucible of splendid attire sample;
The rate of change of the ceramic crucible appearance cup before and after K---the calcination.
The maternal quantity that adds bulk specimen, the ceramic crucible of test splendid attire sample before high temperature sintering with calcination after the rate of change; Thereby in the computing formula of test findings, add the rate of change factor. greatly the raising of degree measuring accuracy.Test error by original ± 25% narrow down to ± 5% in.
The present invention compares with the analytical test method of existing GB/T8133.17-1999 regulation, has the following advantages and effect:
The inventive method is prone to row, and equipment is simple, and is easy to operate, is applicable to that diamond synthesis is higher than the mensuration of the impurity content of 4 graphite more than 9 (99.99%) with purifying dag and purity.No matter be that professional or other staff can both learn very soon, especially for the test findings error rate, will drop to ± 5% in.Greatly the raising of degree measuring accuracy.
Embodiment
Embodiment1:
The maternal quantity of sample is increased to 4～5 times of maternal quantity of the sample of GB/T8133.17-1999 regulation; The ceramic crucible of test splendid attire sample before high temperature sintering with calcination after rate of change k, its value by the appearance cup test it; In the computing formula of test findings, add the rate of change factor.
A kind of method of testing of ultra-high purity graphite trace impurity comprises the following steps:
A, the maternal quantity of sample is increased to 4～5 times of maternal quantity of the sample of GB/T8133.17-1999 regulation;
The ceramic crucible of B, test splendid attire sample before high temperature sintering with calcination after rate of change k, its value by the appearance cup test it; Temperature is controlled at 800 or 810 or 815 or 822 or 829 or 834 or 838 or 842 or 847 or 850 ℃;
C, in the computing formula of test findings, add the rate of change factor, specific as follows:
A=?(G1－G2*k)?/?G?X?100%
In the formula: A---ash content or impurity content;
The maternal weight of G---sample;
G1---the ceramic crucible after the calcination and the weight of sample residue;
G2---the weight of the ceramic crucible of splendid attire sample;
The rate of change of the ceramic crucible appearance cup before and after K---the calcination.Thereby greatly the raising of degree measuring accuracy.Test error by original ± 25% narrow down to ± 5% in.
Claims (1)
1. the method for testing of a ultra-high purity graphite trace impurity the steps include:
A, the maternal quantity of sample is increased to 4～5 times of maternal quantity of the sample of JB/T8133.17-1999 regulation;
The ceramic crucible of B, test splendid attire sample before high temperature sintering with calcination after rate of change k, its value by the appearance cup test it, temperature is controlled at 800～850 ℃;
C, in the computing formula of test findings, add the rate of change factor:
A=?(G1－G2*k)?/?G?×?100%
Wherein: A---ash content or impurity content;
The maternal weight of G---sample;
G1---the ceramic crucible after the calcination and the weight of sample residue;
G2---the weight of the ceramic crucible of splendid attire sample;
The rate of change of the ceramic crucible before and after k---the calcination.
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| CN201110056199A CN102175557B (en) | 2011-03-09 | 2011-03-09 | Method for testing trace impurities in ultrahigh-purity graphite |
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| CN201110056199A CN102175557B (en) | 2011-03-09 | 2011-03-09 | Method for testing trace impurities in ultrahigh-purity graphite |
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| CN102175557A CN102175557A (en) | 2011-09-07 |
| CN102175557B true CN102175557B (en) | 2012-09-19 |
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| CN201110056199A Expired - Fee Related CN102175557B (en) | 2011-03-09 | 2011-03-09 | Method for testing trace impurities in ultrahigh-purity graphite |
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| CN107102096B (en) * | 2017-06-12 | 2019-12-13 | 常州第六元素材料科技股份有限公司 | Method for detecting ash content of graphene oxide |
| CN108872004A (en) * | 2018-06-04 | 2018-11-23 | 中钢集团新型材料（浙江）有限公司 | A kind of measuring method for ultra-pure graphite ash content |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329242A (en) * | 2008-08-05 | 2008-12-24 | 株洲硬质合金集团有限公司 | Method for analyzing and detecting free carbon in chromium carbide |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2659876B2 (en) * | 1991-11-27 | 1997-09-30 | 信越半導体株式会社 | Impurity analysis method for high purity graphite used in semiconductor manufacturing process |
| JP2007101400A (en) * | 2005-10-05 | 2007-04-19 | Toyota Motor Corp | Method of quantitative determination of impurity in carbon nanotube |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101329242A (en) * | 2008-08-05 | 2008-12-24 | 株洲硬质合金集团有限公司 | Method for analyzing and detecting free carbon in chromium carbide |
Non-Patent Citations (3)
| Title |
|---|
| 侯列奇.核纯石墨中微量杂质元素ICP/AES法测定的研究.《中国核科技报告》.1996,(第S1期),1-6. * |
| 国家机械工业局.电炭制品物理化学性能试验方法 灰分含量.《中华人民共和国机械行业标准 JB/T 8133.17- 1999》.2000,66-67. * |
| 高水凤等.小麦粉灰分测定结果不确定度的评定.《现代农业科学》.2008,第15卷(第6期),36-38. * |
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Address after: 436056 Diamond Industrial Park, Hubei Yan Road, Hubei, Ezhou Patentee after: HUBEI EXIN DIAMOND TECHNOLOGY Co.,Ltd. Address before: 436056 Diamond Industrial Park, Hubei Yan Road, Hubei, Ezhou Patentee before: HUBEI EXIN DIAMOND MATERIAL Co.,Ltd. |
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