CN1179916C - Method for preparing single-phase compact silicon titanium carbid block body material by using Al as adjuvant through hot-pressing reaction in situ - Google Patents
Method for preparing single-phase compact silicon titanium carbid block body material by using Al as adjuvant through hot-pressing reaction in situ Download PDFInfo
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- CN1179916C CN1179916C CNB031281818A CN03128181A CN1179916C CN 1179916 C CN1179916 C CN 1179916C CN B031281818 A CNB031281818 A CN B031281818A CN 03128181 A CN03128181 A CN 03128181A CN 1179916 C CN1179916 C CN 1179916C
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Abstract
The present invention relates to a method for making single-phase compact silicon titanium carbide block materials by using Al as an auxiliary agent through hot-pressing reaction in situ. In the method, TiC, Ti, Si and Al with the molar ratio of 2:1:(0.95 to 1.05): (0.15 to 0.25) are used as raw materials; the raw materials are uniformly mixed and then sintered in the atmosphere of Ar in a hot-pressing furnace, the sintering temperature is from 1200 to 1500 DEG C, the heat preservation time is from 1 to 8 hours, and the pressure is from 20 to 80MPa. The product made by the method has the Ti3SiC2 content of 98 wt%, the material density of larger than 99%, the pressure strength of 800MPa, the three-point bending strength sigma b of no smaller than 420MPa and KIC of no smaller than 5MPa. m<1/2>. The present invention has the advantages of simple technology and suitability for industrial production.
Description
Technical field
The present invention relates to the preparation of stupalith, particularly a kind of be the method for the single-phase compact silicon carbide titanium block material of auxiliary agent in-situ hot pressing prepared in reaction with Al.
Background technology
Silicon carbide titanium (Ti
3SiC
2) be a kind of outstanding thermal structure/functional materials, it has electroconductibility, thermal conductivity, high-temp plastic and workability as metal, has the characteristics such as high strength, low density, good high-temperature stability and high-temperature oxidation resistance as pottery again.But, the synthetic difficulty that but compares of silicon carbide titanium, document (1) Monatsh.Fur.Chem.98,1967. with TiH
2, Si and graphite is raw material, under 2000 ℃, carry out chemical reaction and synthesized Ti
3SiC
2Document (2) J.Less.Common Metals.26,1972. documents (3) J.Mater.Sci.29,1994. use SiCl respectively
4, TiCl
4, CCl
4, H
2And TiCl
4, SiCl
4, CH
4, H
2Be raw material, prepared Ti with vapour deposition process
3SiC
2Film.Document (4) J.Eur.Ceram.Soc.5,1989. is raw material with Ti, Si and carbon black, by the synthetic Ti of self propagating high temperature reaction
3SiC
2, have a large amount of impurity phases in the reaction product.Document (5) J.Amer.Ceram.Soc.78,1995. is raw material with Ti, Si and carbon black, with arc-melting method and after annealing Processing of Preparation Ti
3SiC
2Block materials, but reaction product foreign matter content height, temperature of reaction are difficult for accurately control.Document (6) J.Amer.Ceram.Soc.79, No.7,1996. adopt heat and other static pressuring processes, are raw material with Ti, SiC and graphite, have prepared fine and close single-phase Ti
3SiC
2Block materials, but preparation technology is quite complicated.Document (7) Z.Metallkd.91, No.11,2000. is raw material with Ti, Si and graphite, and to add weight be that 4% NaF makes reaction promoter, adopts heat pressing process to prepare Ti
3SiC
2Block materials contains a large amount of TiC in the product.Document (8) J.Eur.Ceram.Soc.22,2002. adopt discharge plasma sintering (SPS) novel process, are raw material with Ti, Si and TiC, have obtained purity and have reached 98% Ti
3SiC
2Block materials, but this technology also is unsuitable for industrial production.
Summary of the invention
The object of the present invention is to provide a kind of Ti of single-phase densification
3SiC
2The preparation method of block materials, this method is fit to industrial scale production.
The invention provides the method for the single-phase compact silicon carbide titanium block material of a kind of in-situ hot pressing prepared in reaction.It is characterized in that: with Al auxiliary agent, and preparation according to the following steps, 1, with the TiC powder, the Ti powder, Si powder and Al powder are raw material, four kinds of raw materials are TiC: Ti: Si: Al=2 in molar ratio: 1: (0.95～1.05): (0.15～0.25) batching; 2, raw material powder is mixed after, place graphite jig, do in the hot pressing furnace of protective atmosphere at Ar gas, be warming up to 1200～1500 ℃ with 20-60 ℃/min speed, in-situ hot pressing 1-8 hour, hot pressing pressure was 20～80MPa.
Ti in the product of the present invention's preparation
3SiC
2Content can be by internal mark method determination, it is worth up to 98wt%, material density is measured by Archimedes, it is worth greater than 99%.On the omnipotent test machine for mechanism of INSTRON-1195, record the ultimate compression strength 〉=800MPa of material, three-point bending strength σ
b〉=420MPa, K
1C〉=5MPam
1/2
Essence of the present invention is to utilize a kind of reaction hot-pressing to prepare Ti
3SiC
2Material.Because the fusing point of Al is low, at a lower temperature, the Al-Si liquid phase alloy that Al can melt also and Si forms together, promoted reaction is synthetic.
Innovation part of the present invention is to utilize low melting point (660 ℃) and two kinds of similar compound Ti of Al
3SiC
2And Ti
3AlC
2Structure, performance similarity.The promoted reaction of Al-Si liquid phase alloy energy is synthetic can quicken sintering again, and simultaneously, the Al disperse of admixture is solid-solubilized in the matrix, can not produce significantly influence to the structure and the performance of material.Therefore, can obtain the block materials of single-phase densification by hot pressed sintering.
Description of drawings
Fig. 1 is the product Ti of present method preparation
3SiC
2The X-ray diffracting spectrum of sample.
Fig. 2 is the diameter 110mm of present method preparation, and thickness is the Ti of 10mm
3SiC
2The photo of block materials.
Embodiment
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
With mol ratio is TiC: Ti: Si: Al=2: 1: 0.95: 0.25 mixed powder 150 grams, put into graphite jig, sintering under the Ar protective atmosphere.Heat-up rate is 50 ℃/min, and sintering temperature is 1300 ℃, and pressure is 30MPa, is incubated 2 hours.The density of block materials is 99%, Ti
3SiC
2Content is 98.2wt.%.Ultimate compression strength 〉=800MPa, three-point bending strength σ
b〉=420MPa, K
IC〉=5MPam
1/2
Embodiment 2
With mol ratio is TiC: Ti: Si: Al=2: 1: 1.05: 0.15 mixed powder 250 grams, put into graphite jig, sintering under the Ar protective atmosphere.Heat-up rate is 50 ℃/min, and sintering temperature is 1400 ℃, and pressure is 60MPa, is incubated 6 hours.The density of block materials is 99.8%, Ti
3SiC
2Content is 99.5wt.%.Ultimate compression strength 〉=800MPa, three-point bending strength σ
b〉=500MPa, K
IC〉=5MPam
1/2
Claims (1)
1, the method for the single-phase compact silicon carbide titanium block material of a kind of in-situ hot pressing prepared in reaction is characterized in that this method is auxiliary agent with Al, and preparation according to the following steps:
1) with the TiC powder, the Ti powder, Si powder and Al powder are raw material; Mol ratio by four kinds of raw materials is TiC: Ti: Si: Al=2: 1: (0.9 5～1.05): (0.15～0.25); Batching,
2) after raw material powder mixes, place graphite jig, in being connected with the hot pressing furnace of Ar gas as protective atmosphere, rise to 1200～1500 ℃ of in-situ hot pressings 1～8 hour with the temperature rise rate of 20～60 ℃/min, hot pressing pressure is 20～80MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031281818A CN1179916C (en) | 2003-06-20 | 2003-06-20 | Method for preparing single-phase compact silicon titanium carbid block body material by using Al as adjuvant through hot-pressing reaction in situ |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031281818A CN1179916C (en) | 2003-06-20 | 2003-06-20 | Method for preparing single-phase compact silicon titanium carbid block body material by using Al as adjuvant through hot-pressing reaction in situ |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1460658A CN1460658A (en) | 2003-12-10 |
| CN1179916C true CN1179916C (en) | 2004-12-15 |
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|---|---|---|---|
| CNB031281818A Expired - Fee Related CN1179916C (en) | 2003-06-20 | 2003-06-20 | Method for preparing single-phase compact silicon titanium carbid block body material by using Al as adjuvant through hot-pressing reaction in situ |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1300359C (en) * | 2004-11-22 | 2007-02-14 | 武汉理工大学 | Compact titanium carbon silicide-titanium diboride composite block material and producing process thereof |
| CN1296501C (en) * | 2004-11-23 | 2007-01-24 | 武汉理工大学 | In-situ hot pressing process of synthesizing compact composite carbon titanosilicide-titanium diboride bulk material |
| CN103253667B (en) * | 2013-04-16 | 2014-12-03 | 武汉理工大学 | Preparation method of ternary layered carbide Ti2SC (titanium sulfur carbide) material |
| CN108585869B (en) * | 2018-05-10 | 2021-06-11 | 西北工业大学 | Preparation method of in-situ synthesized MAX phase modified composite material |
| CN110156018B (en) * | 2019-06-03 | 2020-11-06 | 蚌埠学院 | Preparation method of high-purity titanium silicon carbon material |
| CN110903091B (en) * | 2019-12-06 | 2021-12-07 | 燕山大学 | SiC-Ti3SiC2Composite material and preparation method thereof |
| CN116143121A (en) * | 2023-02-21 | 2023-05-23 | 东南大学 | Full-component MAX phase A solid solution material and preparation method thereof |
-
2003
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