CN102621176B - The analytical approach of nitrogen content in a kind of Ti (C, N) - Google Patents
The analytical approach of nitrogen content in a kind of Ti (C, N) Download PDFInfo
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- CN102621176B CN102621176B CN201110029239.8A CN201110029239A CN102621176B CN 102621176 B CN102621176 B CN 102621176B CN 201110029239 A CN201110029239 A CN 201110029239A CN 102621176 B CN102621176 B CN 102621176B
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Abstract
The invention discloses the analytical approach of nitrogen content in a kind of Ti (C, N), is add N in 1:1 ratio in the sample to which
2releasing agent tungsten powder, grinding evenly, after carrying out pre-treatment, adopts inert gas fusion-thermal conductivity method to measure to sample.Because nitrogen release not exclusively causes the problem of Lower result and poor stability when measuring nitrogen content in Ti (C, N) with inert gas fusion-thermal conductivity method when the invention solves sample not pre-service, improve analysis result accuracy.Present invention reduces analysis result RSD, by original be not less than 3.0% to be reduced to≤0.7%, greatly meet research and production quality control requirements.
Description
Technical field
The present invention relates to the analytical approach of nitrogen content in Ti (C, N) based ceramic metal, particularly relate to the analytical approach that inert gas fusion-thermal conductivity method measures nitrogen content.
Background technology
Ti (C, N) is the continuous solid solution of TiC and TiN, and its molecular formula also can be expressed as Ti (C
1-x, N
x) form (0 < x < 1), it has the advantages such as good elevated temperature strength, high-melting-point, high rigidity, stable chemical nature, enhancing hard alloy and metal material wear-resisting, corrosion-resistant, high temperature resistant etc. in be widely applied.Ti (C, N) stability has a strong impact on sintering processing and final products performance, and S. Kang is by the stability study to Ti (C, the N) solid solution of different C/N ratio, the stability of discovery Ti (C, N) and C/N form close relationship.Therefore realize Ti (C, N) in, the accurate analysis of nitrogen content is measured, and not only has great directive significance to Ti (C, N) powder preparation, and be conducive to when enhancing hard alloy or preparation Ti (C, N) metallic ceramics raw-material selection.
Based on the nitrogen oxygen analyzer of inert gas fusion-thermal conductivity method, due to its distinctive characteristic fast and efficiently, be used to more and more widely in the analysis detect delay work of nitrogen content in compound.But the present inventor by nitrogen oxygen analyzer to Ti(C, N) in nitrogen content analyte detection process in, find all to be difficult to realize N in compound by optimizing instrument parameter and test condition
2release completely, and test result poor stability, also have embodiment in the test of this point nitrogen content in the new layer of stone etc. is to Ti and titanium alloy, the standard deviation (RSD) of method test N reaches the height of 7.5%.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art, provide a kind of inert gas fusion-thermal conductivity method to measure Ti(C, N) the method for nitrogen content, improve analysis result accuracy.
The technical scheme that the present invention solves its technical matters used is:
The analytical approach of nitrogen content in a kind of Ti (C, N), be adopt inert gas fusion-thermal conductivity method to measure, wherein: carried out pre-treatment to sample, its process comprises the steps:
After being mixed with tungsten powder in 1:1 ratio by sample, accurately take a certain amount of (0.015g to 0.025g is accurate to 0.0001 gram) compound sample, load in the nickel foil prepared, make length and be about no more than the granular of 4mm.
Described tungsten powder: more than granularity 20nm, purity is more than 99.9%, and nitrogen content is less than 0.002%.
After adopting such scheme, concrete grammar of the present invention is: will add the Ti(C after nitrogen releasing agent tungsten powder, N) sample is placed on the melting of pulse stove high-temperature heating in graphite crucible after nickel foil parcel, and generate the alloy of low melting point with flux and become the melt of flowing, the nitrogen in sample is with N
2the form of molecule discharges, and removes wherein CO, CO through gas washing
2, H
2after O, take thermal conductivity detector (TCD) to by carrier gas (helium) and detect.
The present invention is at Ti(C, N) nitrogen content test in, introduce a certain amount of tungsten powder as N
2releasing agent promotes the release of N in powder, because W is as the good dissolubility in the nickel of lapping, melt body can be caused to reduce the affinity of N, thus causes having relatively many N in melting process
2discharge from melt body, improve stability and the accuracy of inert gas fusion-thermal conductivity method test.
The present invention confirms through many experiments, when introducing tungsten powder makes N
2after releasing agent, by EMGA-620W type oxygen nitrogen instrument to self-produced and external Ti(C, N) when sample carries out analysis of nitrogen content, the Stability and veracity of method is greatly improved, reduce analysis result RSD, its RSD by original be not less than 3.0% to be reduced to≤0.7%, greatly meet research and production quality control requirements.
The invention has the beneficial effects as follows, realization inert gas fusion-thermal conductivity method is measured the accurate analysis of nitrogen content in Ti (C, N).
Embodiment
Below the Comparison study on example is measured:
1, experiment parameter
Experiment material:
Sample A, Ti(C, N), certain famous foreign brand, nitrogen content is reported as: 11.04%
Sample B, self-produced, nitrogen content is unknown
Lapping: nickel foil, nitrogen content is lower than 0.002%
Analyze power: 5.5KW
Analysis time: 80 seconds
2, record analysis result, all analysis results calculate all automatically
After Sample A sample adopts and adds tungsten powder pre-treatment, analysis result is 11.02%, RSD is 0.39%
When Sample A sample does not carry out pre-treatment, analysis result is 10.56%, RSD is 3.0%
After sample B sample adopts and adds tungsten powder pre-treatment, analysis result is 9.11%, RSD is 0.53%
When sample B sample does not carry out pre-treatment, analysis result is 8.27%, RSD is 12.69%
Show that through many experiments pre-treating method of the present invention improves N in analytic process
2release completeness, greatly improve analysis precision.
Claims (3)
1. an analytical approach for the middle nitrogen content of Ti (C, N), be adopt inert gas fusion-thermal conductivity method to measure, it is characterized in that: carried out pre-treatment to sample, its process comprises the steps:
After being mixed with tungsten powder in 1:1 ratio by sample, accurately take compound sample, load in the nickel foil prepared, make length and be about no more than the granular of 4mm.
2. the analytical approach of the middle nitrogen content of a kind of Ti (C, N) according to claim 1, it is characterized in that: more than the granularity 20nm of described tungsten powder, purity is more than 99.9%, and nitrogen content is less than 0.002%.
3. the analytical approach of the middle nitrogen content of a kind of Ti (C, N) according to claim 1, is characterized in that: the described compound sample accurately taken is 0.015g to 0.025g.
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| CN201110029239.8A CN102621176B (en) | 2011-01-27 | 2011-01-27 | The analytical approach of nitrogen content in a kind of Ti (C, N) |
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| CN102621176B true CN102621176B (en) | 2015-08-26 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458802A (en) * | 2014-12-17 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for measuring nitrogen content of rare earth permanent magnetic material neodymium-iron-boron alloy by using thermal conductivity method |
| CN105784530A (en) * | 2014-12-19 | 2016-07-20 | 北京有色金属研究总院 | Method for measuring contents of oxygen and nitrogen in neodymium iron boron (NdFeB) material |
| CN104764695A (en) * | 2015-03-26 | 2015-07-08 | 中国船舶重工集团公司第七二五研究所 | Method for determining oxygen/nitrogen/hydrogen content in interalloy for titanium alloys |
| CN108508176A (en) * | 2018-02-06 | 2018-09-07 | 太原重工股份有限公司 | The analysis determining method of nitrogen content in alloy |
| CN110133041A (en) * | 2019-05-14 | 2019-08-16 | 包头钢铁（集团）有限责任公司 | The rapid analysis method of nitrogen content in a kind of production of silicon steel |
| CN111855349A (en) * | 2020-07-21 | 2020-10-30 | 湖南华菱涟源钢铁有限公司 | Sample preparation method and nitrogen content detection method for HiB steel decarburization and nitridation annealing coil |
| CN112834310B (en) * | 2020-12-31 | 2023-03-24 | 山东天岳先进科技股份有限公司 | Pretreatment method and device for measuring nitrogen content in nitrogen-doped sample |
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| CN1413268A (en) * | 1999-12-22 | 2003-04-23 | H.C.施塔克股份有限公司 | Powder mixture or composite powder, method for production thereof and use thereof in composite materials |
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| JP5063129B2 (en) * | 2007-02-08 | 2012-10-31 | 京セラ株式会社 | cermet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413268A (en) * | 1999-12-22 | 2003-04-23 | H.C.施塔克股份有限公司 | Powder mixture or composite powder, method for production thereof and use thereof in composite materials |
Non-Patent Citations (2)
| Title |
|---|
| 化学法测定碳氮化钛中氮含量;钟华;《钢铁钒钛》;20050331;第26卷(第1期);65-68 * |
| 惰气熔融-热导法测定钛铁中氮;王伟等;《冶金分析》;20101231;第30卷(第9期);62-64 * |
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