CN102621176A - Method for analyzing content of nitrogen in Ti(C,N) - Google Patents
Method for analyzing content of nitrogen in Ti(C,N) Download PDFInfo
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- CN102621176A CN102621176A CN2011100292398A CN201110029239A CN102621176A CN 102621176 A CN102621176 A CN 102621176A CN 2011100292398 A CN2011100292398 A CN 2011100292398A CN 201110029239 A CN201110029239 A CN 201110029239A CN 102621176 A CN102621176 A CN 102621176A
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Abstract
The invention discloses a method for analyzing the content of nitrogen in Ti(C,N). The method comprises the following steps: adding an N2 releaser tungsten powder to a sample according to a ratio of 1:1, uniformly grinding, preprocessing and postprocessing the sample, and determining through adopting an inert gas fusion-thermal conductivity method. The method which solves problems of low result and bad result stability caused by incomplete release of nitrogen during determination through the inert gas fusion-thermal conductivity method without preprocessing the sample makes the accuracy of the analytic result be improved. The method which makes RSD of the analytic result be reduced to equal to or less than 0.7% from not lower than 3.0% greatly satisfies scientific research and production quality control demands.
Description
Technical field
(C, the N) analytical approach of nitrogen content in the based ceramic metal particularly relate to the analytical approach that inert gas fusion-thermal conductivity method is measured nitrogen content to the present invention relates to Ti.
Background technology
(C N) is the continuous solid solution of TiC and TiN to Ti, and its molecular formula also can be expressed as Ti (C
1-x, N
x) form (0＜x＜1), it has advantages such as good high-temperature intensity, high-melting-point, high rigidity, chemical property are stable, has obtained widespread use at the aspect such as wear-resisting, corrosion-resistant, high temperature resistant of enhancing hard alloy and metal material.Ti (C, N) stability has a strong impact on sintering processing and final products performance, and (C, the N) stability study of solid solution find that (C, stability N) and C/N form has confidential relation to Ti to S. Kang through the Ti to different C/N ratios.Therefore realize to Ti (C, N) in the accurate analysis to measure of nitrogen content, not only to Ti (C, N) powder preparation has great directive significance, and help enhancing hard alloy or preparation Ti (C, N) during metallic ceramics to raw-material selection.
Based on the nitrogen oxygen analyzer of inert gas fusion-thermal conductivity method, because its distinctive characteristic fast and efficiently is used in the analyzing and testing research work of nitrogen content in the compound more and more widely.(C N) in the analyte detection process of middle nitrogen content, finds to be difficult to realize N in the compound through optimizing instrument parameter and test condition to Ti but the inventor is passing through the nitrogen oxygen analyzer
2Release fully, and test result poor stability, this point also has embodiment in the test of nitrogen content at the new layer of stone etc. in to Ti and titanium alloy, the standard deviation (RSD) of method test N has reached 7.5% height.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, (C, the method for nitrogen content N) improve analysis result accuracy to provide a kind of inert gas fusion-thermal conductivity method to measure Ti.
The present invention solves the used technical scheme of its technical matters:
(C, the N) analytical approach of middle nitrogen content are to adopt inert gas fusion-thermal conductivity method to measure to a kind of Ti, and wherein: sample has been carried out pre-treatment, and its process comprises the steps:
After sample mixed in 1:1 ratio and tungsten powder, accurately take by weighing a certain amount of (0.015g to 0.025g is accurate to 0.0001 gram) compound sample, in the nickel foil for preparing of packing into, process length and be no more than the granular of 4mm approximately.
Said tungsten powder: more than the 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: with the Ti (C behind the interpolation nitrogen releasing agent tungsten powder; N) sample is placed on behind nickel foil parcel in the graphite crucible with the fusion of pulse stove heat, generates low-melting alloy and becomes mobile melt with flux, and the nitrogen in the sample is with N
2The form of molecule discharges, and removes wherein CO, CO through gas washing
2, H
2Behind the O, take thermal conductivity detector (TCD) to by carrier gas (helium) and detect.
(C in nitrogen content test N), introduces a certain amount of tungsten powder as N at Ti in the present invention
2Releasing agent promotes the release of N in the powder, because W can cause melting the affinity reduction of body to N, thereby cause that more relatively N is arranged in melting process as the dissolubility preferably in the nickel of lapping
2From melt body, discharge, improve the stability and the accuracy of inert gas fusion-thermal conductivity method test.
The present invention's warp is experiment confirm repeatedly, makes N when introducing tungsten powder
2Behind the releasing agent; Through EMGA-620W type oxygen nitrogen appearance to self-produced and external Ti (C; When N) sample carried out analysis of nitrogen content, the accuracy and the stability of method were greatly improved, and have reduced analysis result RSD; Its RSD by original be not less than 3.0% be reduced to≤0.7%, greatly satisfied research and production quality control demand.
The invention has the beneficial effects as follows, realize with inert gas fusion-thermal conductivity method Ti (C, N) the accurate analysis to measure of middle nitrogen content.
Embodiment
Below be the application contrast on instance is measured:
1, experiment parameter
Experiment material:
Sample A, and Ti (C, N), certain external famous brand name, 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 all calculate automatically
After the Sample A samples using added the tungsten powder pre-treatment, analysis result was 11.02%, and RSD is 0.39%
When the Sample A sample did not carry out pre-treatment, analysis result was 10.56%, and RSD is 3.0%
After the sample B samples using added the tungsten powder pre-treatment, analysis result was 9.11%, and RSD is 0.53%
When the sample B sample did not carry out pre-treatment, analysis result was 8.27%, and RSD is 12.69%
Draw through repeatedly testing, pre-treating method of the present invention has improved N in the analytic process
2The release completeness, greatly improved analysis precision.
Claims (3)
1. (C, the N) analytical approach of middle nitrogen content are to adopt inert gas fusion-thermal conductivity method to measure to a Ti, and it is characterized in that: sample has been carried out pre-treatment, and its process comprises the steps:
After sample mixed in 1:1 ratio and tungsten powder, accurately take by weighing compound sample, in the nickel foil for preparing of packing into, process length and be no more than the granular of 4mm approximately.
2. (it is characterized in that: more than the granularity 20nm of said tungsten powder, purity is more than 99.9%, and nitrogen content is less than 0.002% for C, the N) analytical approach of middle nitrogen content for a kind of Ti according to claim 1.
3. (it is characterized in that: the said compound sample that accurately takes by weighing is 0.015g to 0.025g to a kind of Ti according to claim 1 for C, the N) analytical approach of middle nitrogen content.
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| Application Number | Priority Date | Filing Date | Title |
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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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| 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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| CN102621176A true CN102621176A (en) | 2012-08-01 |
| CN102621176B CN102621176B (en) | 2015-08-26 |
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Cited By (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 |
| 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 |
| 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 |
| 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 |
| CN112834310A (en) * | 2020-12-31 | 2021-05-25 | 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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Cited By (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 |
| CN112834310A (en) * | 2020-12-31 | 2021-05-25 | 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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| CN102621176B (en) | 2015-08-26 |
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