CN1356291A - Non-pressure sinter process for compact ZrB2 or TiB2 ceramic material - Google Patents

Non-pressure sinter process for compact ZrB2 or TiB2 ceramic material Download PDF

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Publication number
CN1356291A
CN1356291A CN 01143480 CN01143480A CN1356291A CN 1356291 A CN1356291 A CN 1356291A CN 01143480 CN01143480 CN 01143480 CN 01143480 A CN01143480 A CN 01143480A CN 1356291 A CN1356291 A CN 1356291A
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sintering
powder
tib2
ceramic material
tib
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CN1132801C (en
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龙冲生
邹从沛
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Nuclear Power Institute of China
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Nuclear Power Institute of China
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Abstract

A non-pressure sinter process for preparing compact ZrB2-TiB2 ceramic includes mixing ZrB2 powder, TiB2 powder and ZrH2 (or TiH2) as assistant, shaping and vacuum sinter. Its desntiy can reach 94-96% T.D.

Description

The method of zirconium diboride or the pressureless sintering of TiB2 dense ceramic material
Technical field
The invention belongs to a kind of preparation method of stupalith, specifically a kind of zirconium diboride (ZrB 2) or TiB2 (TiB 2) method of dense ceramic material pressureless sintering.
Background technology
Zirconium diboride and TiB2 not only have the erosion resistance and the oxidation-resistance of high-melting-point, high rigidity, excellence, and have good electrical conductivity and thermal conductivity, and therefore very application prospects is arranged.Because ZrB 2And TiB 2Be the extremely strong covalent linkage compound of bond energy, be difficult to obtain highdensity sintered compact.Prepare ZrB at present 2And TiB 2Dense ceramic material method commonly used is hot pressing, and typical hot pressing parameters is that pressure is 1-2GPa; Temperature is 1600-1800 ℃; Press time is 1-2h.In order to improve ZrB 2And TiB 2The hot pressing performance, add some sintering aids, sintering aid commonly used is the boride of transition metal such as CoB, FeB, Ni 3B 4, VB 2, CrB 2, NbB 2Deng.By hot pressing, ZrB 2And TiB 2The density of stupalith can reach 95-99%T.D..
At present at ZrB 2And TiB 2The normal atmosphere sintering method that stupalith adds sintering aid has also carried out some researchs.The sintering aid that adds is oxide-based, as ZrO 2, Al 2O 3, Y 2O 3Deng, add-on is more than 30wt%.When sintering temperature more than 1900 ℃ the time, sintered density can reach about 90%.There is following problem in aforesaid method: 1. adopt hot pressing, production efficiency is low, and cost is high.2. the sintering aid content in normal pressure-sintered is too many, greatly sinking ZrB 2And TiB 2Performance, as specific conductivity etc., and sintered density is lower, thereby has influenced ZrB 2And TiB 2The use of material.
Summary of the invention
The objective of the invention is to solve ZrB 2And TiB 2The problem of the normal pressure-sintered difficulty of stupalith provides the method for a kind of zirconium diboride and the pressureless sintering of TiB2 dense ceramic material, reduces production costs.
The present invention is achieved in that the ZrB with median size 1 μ m-2 μ m 2Powder or TiB 2Powder is a raw material, adopts ZrH 2Or TiH 2Make sintering aid, ZrH 2Or TiH 2Add-on be ZrB 2Powder or TiB 2The 3-5wt% of powder stock, routinely after technology batch mixing, the moulding, sintering in vacuum, vacuum tightness requires to be better than 5 * 10 -2Pa, sintering temperature is 1700-1900 ℃, sintering time is 2-3 hour, can obtain the fine and close ZrB that sintered density reaches 94-96%T.D. 2Or TiB 2Stupalith.
Effect of the present invention is: because sintering aid is at ZrB 2Powder or TiB 2Content in the powder stock is few, does not influence ZrB 2And TiB 2The performance of material is as fusing point, hardness etc.And be pressureless sintering, the production efficiency height, cost descends.
Embodiment
Embodiment one.
1. with the ZrB about mean particle size 1 μ m 2Powder is a raw material, adds sintering aid ZrH 2, ZrH 2Add-on be ZrB 2The 3wt% of powder stock behind the thorough mixing, at the 500Mpa forming under the pressure, reaches more than the 60%T.D. green density.
2. sintering in vacuum atmosphere, vacuum tightness is 3 * 10 -2Pa, sintering temperature is 1900 ℃, sintering time is 2h, ZrB 2The density of sintered compact reaches more than the 94%T.D..
Embodiment two.
1. with the ZrB about mean particle size 1 μ m 2Powder is a raw material, adds sintering aid ZrH 2, ZrH 2Add-on be ZrB 2The 3wt% of powder stock behind the thorough mixing, at the 500Mpa forming under the pressure, reaches more than the 60%T.D. green density.
2. sintering in vacuum atmosphere, vacuum tightness is 4 * 10 -2Pa, sintering temperature is 1800 ℃, sintering time is 2.5h, ZrB 2The density of sintered compact reaches more than the 94%T.D..
Embodiment three.
1. with the TiB of mean particle size about 2 μ m 2Powder is a raw material, adds sintering aid TiH 2, TiH 2Add-on be TiB 2The 4wt% of powder stock behind the thorough mixing, at the 500Mpa forming under the pressure, reaches more than the 60%T.D. green density.
2. sintering in vacuum atmosphere, vacuum tightness is 3 * 10 -2Pa, sintering temperature is 1700 ℃, sintering time is 2h, TiB 2The density of sintered compact reaches more than the 94%T.D..
Embodiment four.
1. with the TiB of mean particle size about 2 μ m 2Powder is a raw material, adds sintering aid TiH 2, TiH 2Add-on be TiB 2The 5wt% of powder stock behind the thorough mixing, at the 500Mpa forming under the pressure, reaches more than the 60%T.D. green density.
2. sintering in vacuum atmosphere, vacuum tightness 4 * 10 -2Pa, sintering temperature is 1900 ℃, sintering time is 3h, TiB 2The density of sintered compact reaches more than the 94%T.D..

Claims (5)

1. the method for zirconium diboride or the pressureless sintering of TiB2 dense ceramic material is with ZrB 2Powder or TiB 2Powder is a raw material, adds sintering aid, and technology batch mixing, moulding, sintering are made zirconium diboride (ZrB routinely 2) or TiB2 (TiB 2) dense ceramic material, it is characterized in that: described sintering aid is ZrH 2Or TiH 2, and under vacuum condition sintering.
2. the method for zirconium diboride as claimed in claim 1 or the pressureless sintering of TiB2 dense ceramic material is characterized in that: sintering aid ZrH 2Or TiH 2Add-on be ZrB 2Powder or TiB 2The 3-5wt% of powder stock.
3. the method for zirconium diboride as claimed in claim 1 or 2 or the pressureless sintering of TiB2 dense ceramic material is characterized in that: vacuum tightness requires to be better than 5 * 10 -2Pa.
4. the method for zirconium diboride as claimed in claim 3 or the pressureless sintering of TiB2 dense ceramic material is characterized in that: sintering temperature is 1700-1900 ℃, and sintering time is 2-3 hour.
5. as the method for claim 1 or 2 or 4 described zirconium diborides or the pressureless sintering of TiB2 dense ceramic material, it is characterized in that: ZrB 2Powder or TiB 2The powder median size is at 1-2 μ m.
CN 01143480 2001-12-29 2001-12-29 Non-pressure sinter process for compact ZrB2 or TiB2 ceramic material Expired - Lifetime CN1132801C (en)

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CN1132801C CN1132801C (en) 2003-12-31

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100336723C (en) * 2005-05-23 2007-09-12 哈尔滨工业大学 Combustion synthesis method of zirconium diboride micro-powder
CN101182212B (en) * 2007-11-06 2010-04-07 武汉理工大学 YAG/ZrB2 series multi-phase ceramics and preparation method thereof
CN102190495A (en) * 2010-03-18 2011-09-21 中国科学院上海硅酸盐研究所 Preparation method for promoting to sinter zirconium boride or zirconium carbide ceramics by using reaction aids
CN102557644A (en) * 2010-12-09 2012-07-11 中国科学院金属研究所 Method for preparing titanium diboride ceramic with titanium aluminum carbon as sintering aid
CN103833286A (en) * 2014-03-11 2014-06-04 山东理工大学 Method for preparing low-density oil well cement test block by using zirconium diboride ceramic micro-beads
CN103833287A (en) * 2014-03-11 2014-06-04 山东理工大学 Method for preparing low-density oil well cementation cement test block through titanium diboride ceramic beads
CN108997020A (en) * 2018-06-25 2018-12-14 广东工业大学 A kind of high-performance zirconium boride ceramic and its preparation method and application

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100336723C (en) * 2005-05-23 2007-09-12 哈尔滨工业大学 Combustion synthesis method of zirconium diboride micro-powder
CN101182212B (en) * 2007-11-06 2010-04-07 武汉理工大学 YAG/ZrB2 series multi-phase ceramics and preparation method thereof
CN102190495A (en) * 2010-03-18 2011-09-21 中国科学院上海硅酸盐研究所 Preparation method for promoting to sinter zirconium boride or zirconium carbide ceramics by using reaction aids
CN102190495B (en) * 2010-03-18 2013-10-30 中国科学院上海硅酸盐研究所 Preparation method for promoting to sinter zirconium boride or zirconium carbide ceramics by using reaction aids
CN102557644A (en) * 2010-12-09 2012-07-11 中国科学院金属研究所 Method for preparing titanium diboride ceramic with titanium aluminum carbon as sintering aid
CN103833286A (en) * 2014-03-11 2014-06-04 山东理工大学 Method for preparing low-density oil well cement test block by using zirconium diboride ceramic micro-beads
CN103833287A (en) * 2014-03-11 2014-06-04 山东理工大学 Method for preparing low-density oil well cementation cement test block through titanium diboride ceramic beads
CN103833286B (en) * 2014-03-11 2015-10-21 山东理工大学 Zirconium diboride ceramics microballon prepares the method for low density oil well cementing cement briquette
CN103833287B (en) * 2014-03-11 2015-11-11 山东理工大学 Titanium diboride ceramic microballon prepares the method for low density oil well cementing cement briquette
CN108997020A (en) * 2018-06-25 2018-12-14 广东工业大学 A kind of high-performance zirconium boride ceramic and its preparation method and application

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