CN101289222A - Method for preparing high-pure and superfine titanium-aluminum-nitrogen powder - Google Patents
Method for preparing high-pure and superfine titanium-aluminum-nitrogen powder Download PDFInfo
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- CN101289222A CN101289222A CNA2008101145163A CN200810114516A CN101289222A CN 101289222 A CN101289222 A CN 101289222A CN A2008101145163 A CNA2008101145163 A CN A2008101145163A CN 200810114516 A CN200810114516 A CN 200810114516A CN 101289222 A CN101289222 A CN 101289222A
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- 239000000843 powder Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 24
- -1 titanium-aluminum-nitrogen Chemical compound 0.000 title claims description 5
- 239000000463 material Substances 0.000 claims abstract description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims description 45
- 230000015572 biosynthetic process Effects 0.000 claims description 11
- 238000003786 synthesis reaction Methods 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 238000013467 fragmentation Methods 0.000 claims description 7
- 238000006062 fragmentation reaction Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000009837 dry grinding Methods 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 238000001599 direct drying Methods 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 229910052718 tin Inorganic materials 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 238000001272 pressureless sintering Methods 0.000 description 3
- 241000209456 Plumbago Species 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 229910009594 Ti2AlN Inorganic materials 0.000 description 1
- IWBUYGUPYWKAMK-UHFFFAOYSA-N [AlH3].[N] Chemical compound [AlH3].[N] IWBUYGUPYWKAMK-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The invention relates to a preparation method of superfine Ti2AlN2 powder with high purity, which pertains to the field of ceramic materials. The raw materials and mole ratio thereof adopted by the method is that TiN:Ti:Al is equal to 1:(0.9 to 1.2):(0.9 to 1.2); after the steps such as ball milling, mixing, vacuum filtration or direct drying, baking and sieving, and the like, being carried out, the raw materials react to synthesize in a vacuum firing furnace under the conditions of floating argon protection, 1200 DEG C to 1350 DEG C of resultant temperature and heat preservation for 10min to 120min; the obtained material is further finely milled and then dried and sieved, so as to obtain the Ti2AlN2 powder with content being more than 97 percent and granularity being in micron or submicron. After an XRD test, the main component of the powder is Ti2AlN2 and the main impurity is TiN with the content being 3 to 0wt percent. The method of the invention has the advantages of simple and easy operation, high productivity, high purity and high efficiency, which is applicable to industrialized mass production.
Description
Technical field
The present invention relates to the stupalith field, a kind of high-pure and superfine titanium-aluminum-nitrogen (Ti is provided
2AlN) the pressureless sintering preparation method of powder.
Background technology
Ti
2AlN is a kind of novel material with special performance.The advantage that this material has been concentrated metal and pottery, as conduction, heat conduction, can process, very peculiar over-all propertieies such as high temperature resistant, anti-thermal shock, self-lubricating, in a lot of fields such as high-temperature structural components, Chemical Preservation material, electrode brush material very wide application prospect is arranged.
The method that the existing at present document of publishing prepares this material mainly contains two kinds: adopting Ti, Al and N simple substance powder is raw material, and original position hot isostatic pressing reaction sintering prepares Ti
2The AlN block materials (document 1:Metall.Mater.Trans.A, 2000,31[7]: be raw material with adopting Ti, Al, TiN 1857-1865), the in-situ hot pressing sintering prepares Ti
2The AlN block materials (document 2:Trans.Nonferrous Met.Soc.China, 2008,18:80-85).These two kinds of methods all are to utilize reaction in agglomerating method directly to prepare Ti
2AlN block materials, its main drawback are that the purity of Ti2AlN material is difficult to control, and can't be fit to large-scale application.According to the manufacturing mode of the stupalith of routine, generally all is earlier synthetic high-purity ceramic powder, and then prepares ceramic component by the powder design.Therefore, Ti
2Synthesizing of AlN powder, this material is used widely in the future, have great importance.
According to the retrieval, about high-purity Ti
2Synthesizing of AlN powder also do not have disclosed bibliographical information at present, do not have commercial Ti on the market yet
2The AlN powder is sold.A kind of high pure and ultra-fine Ti that the present invention proposes
2The pressureless sintering preparation method of AlN powder has filled up the technological gap of this respect just.
Summary of the invention
The purpose of this invention is to provide a kind of high purity titanium aluminium nitrogen (Ti
2AlN) the synthetic and preparation method of powder utilizes pressureless sintering method to prepare Ti
2The AlN powder.The present invention is simple and easy to do, productive rate is high, purity is high, efficient is high, be fit to commercial scale production.
The preparation method of a kind of high-pure and superfine titanium-aluminum-nitrogen powder that the present invention proposes, it is characterized in that: described method contains following steps:
(1) raw material is: nitrogenize titanium valve, titanium valve, aluminium powder;
(2) the material molar ratio proportioning is: TiN: Ti: Al=1: (0.9～1.2): (0.9～1.2);
(3) set by step prescription weigh batching in (2) is put into ball grinder, is abrading-ball with the agate ball, is medium with alcohol, or directly dry grinding, ball mill mixing;
(4) after the discharging, vacuum filtration or convection drying after the oven dry, sieve, and obtain the blended powder;
(5) powder that step (4) is obtained is put into graphite or alumina crucible, reacts synthetic in vacuum oven, the argon shield of flowing, 1200～1350 ℃ of synthesis temperatures, insulation 10min～120min;
(6) product that step (5) is obtained after fragmentation, pulverizing, sieves; Adopt the method for ball milling or stirring mill further levigate again, sieve after the drying, can obtain content greater than 97%, granularity is the Ti of micron or submicron order
2AlN
2Powder.
Utilize the present invention can utilize comparatively cheap raw material and simple production unit, just can synthesize in large quantity high-purity (＞97wt%), the Ti of ultra-fine (micron or submicron)
2AlN
2Powder.Detect through XRD, main component is Ti in the powder
2AlN
2, impurity mainly is TiN, its content is 3～0wt%.
The present invention is simple and easy to do, productive rate is high, purity is high, efficient is high, be fit to commercial scale production.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
(1). raw material:
Titanium valve (Ti ,～300 orders, purity＞99%, weight ratio, down with), aluminium powder (Al ,～300 orders, purity＞98%), nitrogenize titanium valve (TiN, purity＞99%)
(2). proportioning (mol ratio, down together):
Proportioning raw materials is: TiN: Ti: Al=1: (0.9～1.2): (0.9～1.2)
(3). by prescription weigh batching in (2).Putting into ball grinder, is abrading-ball with the agate ball, is medium with alcohol, or directly dry grinding (not adding alcohol is medium), 12～24 hours (material: ball: alcohol=1: (1～2): (0～2), mass ratio) of ball mill mixing.
(4). discharging, vacuum filtration or convection drying after drying 1～4 hour about 80 ℃, are crossed 50～100 mesh sieves, obtain the blended powder.
(5). the powder in the process (4) is put into graphite or alumina crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1200～1350 ℃ of synthesis temperatures, insulation 10min～120min.
(6). with the product that process (5) obtains, after fragmentation, pulverizing, cross 200 sieves; Can adopt ball milling method then or stir the method for mill further levigate, 300～500 mesh sieves are crossed in dry back, can obtain content greater than 97%, and granularity be micron or the Ti of submicron order
2AlN
2Powder.
Embodiment
Embodiment one:
Select for use prescription to be: TiN: Ti: Al=1: 1: 1 (mol ratio), carry out weigh batching, put into ball grinder, in material: agate ball: the ratio of alcohol=1: 2: 1 adds abrading-ball and alcohol, ball milling mixed 12 hours, and discharging final vacuum suction filtration was 80 ℃ of oven dry 2 hours, cross 100 mesh sieves then, obtain the blended powder.Mixed powder is put into plumbago crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1280 ℃ of synthesis temperatures, insulation 30min.With the synthetic product, after fragmentation, pulverizing, cross 200 sieves; Can adopt the method that stirs mill further levigate then, 300 mesh sieves are crossed in dry back, and can obtain main component is Ti
2The powder of AlN.By analysis, Ti in institute's synthetic powder
2The content of AlN is 99.5%, and granularity is 2.4 μ m.
Embodiment two:
Select for use prescription to be: TiN: Ti: Al=1: 1: 1.1 (mol ratio), carry out weigh batching, put into ball grinder, in material: the ratio of agate ball=1: 2 adds abrading-ball, and dry ball milling mixed 24 hours, after the discharging, 80 ℃ of oven dry 1 hour, cross 100 mesh sieves then, obtain the blended powder.Mixed powder is put into alumina crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1250 ℃ of synthesis temperatures, insulation 45min.With the synthetic product, after fragmentation, pulverizing, cross 200 sieves; Can adopt the method that stirs mill further levigate then, 300 mesh sieves are crossed in dry back, and can obtain main component is Ti
2The powder of AlN.By analysis, Ti in institute's synthetic powder
2The content of AlN is 99.0%, and granularity is 1.8 μ m.
Embodiment three:
Select for use prescription to be: TiN: Ti: Al=1: 1.1: 0.95 (mol ratio), carry out weigh batching, put into ball grinder, in material: agate ball: the ratio of alcohol=1: 2: 1 adds abrading-ball and alcohol, ball milling mixed 24 hours, and discharging final vacuum suction filtration was 80 ℃ of oven dry 2 hours, cross 60 mesh sieves then, obtain the blended powder.Mixed powder is put into plumbago crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1325 ℃ of synthesis temperatures, insulation 60min.With the synthetic product, after fragmentation, pulverizing, cross 200 sieves; Can adopt the method that stirs mill further levigate then, 300 mesh sieves are crossed in dry back, and can obtain main component is Ti
2The powder of AlN.By analysis, Ti in institute's synthetic powder
2The content of AlN is 98.4%, and granularity is 3.18 μ m.
Embodiment four:
Select for use prescription to be: TiN: Ti: Al=1: 0.9: 1.15 (mol ratio), carry out weigh batching, put into ball grinder, in material: the ratio of agate ball=1: 2 adds abrading-ball, and dry ball milling mixed 12 hours, after the discharging, 80 ℃ of oven dry 1 hour, cross 100 mesh sieves then, obtain the blended powder.Mixed powder is put into alumina crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1300 ℃ of synthesis temperatures, insulation 90min.With the synthetic product, after fragmentation, pulverizing, cross 200 sieves; Can adopt the method that stirs mill further levigate then, 300 mesh sieves are crossed in dry back, and can obtain main component is Ti
2The powder of AlN.By analysis, Ti in institute's synthetic powder
2The content of AlN is 97.3%, and granularity is 1.76 μ m.
Claims (5)
1, a kind of preparation method of high-pure and superfine titanium-aluminum-nitrogen powder is characterized in that: described method contains following steps:
(1) raw material is: nitrogenize titanium valve, titanium valve, aluminium powder;
(2) the material molar ratio proportioning is: TiN: Ti: Al=1: (0.9～1.2): (0.9～1.2);
(3) set by step prescription weigh batching in (2) is put into ball grinder, is abrading-ball with the agate ball, is medium with alcohol, or directly dry grinding, ball mill mixing;
(4) after the discharging, vacuum filtration or convection drying after the oven dry, sieve, and obtain the blended powder;
(5) powder that step (4) is obtained is put into graphite or alumina crucible, reacts synthetic in vacuum oven, the argon shield of flowing, 1200～1350 ℃ of synthesis temperatures, insulation 10min～120min;
(6) product that step (5) is obtained after fragmentation, pulverizing, sieves; Adopt the method for ball milling or stirring mill further levigate again, sieve after the drying, can obtain content greater than 97%, granularity is the Ti of micron or submicron order
2AlN
2Powder.
2, in accordance with the method for claim 1, it is characterized in that: described step (2) material molar ratio proportioning is: TiN: Ti: Al=1: 1: 1, described step (5) synthesis temperature was 1280 ℃, insulation 30min.
3, in accordance with the method for claim 1, it is characterized in that: described step (2) material molar ratio proportioning is: TiN: Ti: Al=1: 1: 1.1, described step (5) synthesis temperature was 1250 ℃, insulation 45min.
4, in accordance with the method for claim 1, it is characterized in that: described step (2) material molar ratio proportioning is: TiN: Ti: Al=1: 1.1: 0.95, described step (5) synthesis temperature was 1325 ℃, was incubated 60min ℃.
5, in accordance with the method for claim 1, it is characterized in that: described step (2) material molar ratio proportioning is: TiN: Ti: Al=1: 0.9: 1.15, described step (5) synthesis temperature was 1300 ℃, insulation 90min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101145163A CN101289222A (en) | 2008-06-06 | 2008-06-06 | Method for preparing high-pure and superfine titanium-aluminum-nitrogen powder |
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|---|---|---|---|
| CNA2008101145163A CN101289222A (en) | 2008-06-06 | 2008-06-06 | Method for preparing high-pure and superfine titanium-aluminum-nitrogen powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402450A (en) * | 2014-10-13 | 2015-03-11 | 陕西科技大学 | Method for quickly preparing Ti2AlN ceramic powder on the basis of thermal explosion reaction at low temperature |
| CN106830971A (en) * | 2017-04-05 | 2017-06-13 | 河海大学 | A kind of preparation method of MAX phases porous ceramics |
| CN109160520A (en) * | 2018-09-01 | 2019-01-08 | 河南理工大学 | A kind of ball-milling treatment Material synthesis high purity Ti3B2The method of N material |
| WO2019181600A1 (en) * | 2018-03-23 | 2019-09-26 | 日清エンジニアリング株式会社 | Composite particles and method for producing composite particles |
-
2008
- 2008-06-06 CN CNA2008101145163A patent/CN101289222A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402450A (en) * | 2014-10-13 | 2015-03-11 | 陕西科技大学 | Method for quickly preparing Ti2AlN ceramic powder on the basis of thermal explosion reaction at low temperature |
| CN106830971A (en) * | 2017-04-05 | 2017-06-13 | 河海大学 | A kind of preparation method of MAX phases porous ceramics |
| WO2019181600A1 (en) * | 2018-03-23 | 2019-09-26 | 日清エンジニアリング株式会社 | Composite particles and method for producing composite particles |
| CN111867972A (en) * | 2018-03-23 | 2020-10-30 | 日清工程株式会社 | Composite particle and method for producing composite particle |
| KR20200135322A (en) * | 2018-03-23 | 2020-12-02 | 닛신 엔지니어링 가부시키가이샤 | Composite particles and methods of manufacturing composite particles |
| JPWO2019181600A1 (en) * | 2018-03-23 | 2021-04-22 | 日清エンジニアリング株式会社 | Composite particles and methods for producing composite particles |
| JP7159292B2 (en) | 2018-03-23 | 2022-10-24 | 日清エンジニアリング株式会社 | Composite particles and method for producing composite particles |
| US11479674B2 (en) | 2018-03-23 | 2022-10-25 | Nisshin Engineering Inc. | Composite particles comprising TiN powder and method for producing the composite particles |
| KR102639978B1 (en) * | 2018-03-23 | 2024-02-22 | 닛신 엔지니어링 가부시키가이샤 | Composite particles and methods for producing composite particles |
| CN109160520A (en) * | 2018-09-01 | 2019-01-08 | 河南理工大学 | A kind of ball-milling treatment Material synthesis high purity Ti3B2The method of N material |
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Open date: 20081022 |