CN102530945A - Method for preparing high-purity Ti3SiC2 powder - Google Patents

Method for preparing high-purity Ti3SiC2 powder Download PDF

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Publication number
CN102530945A
CN102530945A CN2011104211243A CN201110421124A CN102530945A CN 102530945 A CN102530945 A CN 102530945A CN 2011104211243 A CN2011104211243 A CN 2011104211243A CN 201110421124 A CN201110421124 A CN 201110421124A CN 102530945 A CN102530945 A CN 102530945A
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China
Prior art keywords
powder
sic
purity
organic solvent
polycarbosilane
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CN2011104211243A
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Chinese (zh)
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杨金山
董绍明
张翔宇
王震
何平
高乐
胡建宝
胡志辉
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention discloses a method for preparing high-purity Ti3SiC2 powder, which includes the following steps: first, dissolving polycarbosilane in organic solvent, then, adding titanium hydride powder, and evenly mixing in an ultrasonic mode; heating while mixing until the organic solvent is fully volatilized to enable solution to be thick, and then drying in a vacuum mode; processing at a low temperature under the protection of inert atmosphere; and processing at a high temperature under the protection of inert atmosphere. The method for preparing high-purity Ti3SiC2 powder has the advantages of being high in purity, high in degree of crystallization, small in powder particle size, and the like. In addition, the method for preparing high-purity Ti3SiC2 powder is simple in process, easy to operate, less in energy consumption and capable of meeting large-scale and economic requirements of industrial production of Ti3SiC2 powder, and has wide application value.

Description

A kind of preparation high-purity Ti 3SiC 2The method of powder
Technical field
The present invention relates to a kind of Ti 3SiC 2The preparation method of powder specifically, relates to a kind of preparation high-purity Ti 3SiC 2The method of powder belongs to the material technology field.
Background technology
Ternary layered compound Ti 3SiC 2Be unique real ternary compound in the Ti-Si-C series, belong to hexagonal system, both had the excellent properties of metal, as good heat conduction and conductivity, good heat-shock resistance and workability and high-temp plastic are arranged when the normal temperature; Simultaneously, it has the excellent properties of pottery again, like high ys, and HMP, high and good antioxidant property and the corrosion resistance nature of high thermal stability and hot strength; Having broad application prospects, is the ideal candidates material of high-temperature engine, also can be used as the brush and the electrode materials of a new generation, also is fit to be manufactured on all kinds of anti-attrition members of working under high temperature, the chemical corrosion condition.Ti 3SiC 2Powder removes can be directly as original powder, and preparation has the Ti of excellent properties 3SiC 2Outside the block ceramic, also can it be come the high-temperature self-lubrication stupalith of synthesizing new as additive.
Ti 3SiC 2Excellent properties attracted the lot of domestic and foreign scholar that its preparation method is studied and explored.But because in the Ti-Si-C ternary phase diagrams, single Ti during high temperature 3SiC 2Phase stable range is narrow, and preparation high purity, fully dense Ti are described 3SiC 2Block materials is difficulty very.Prepare Ti at present 3SiC 2Method mainly can be divided into 2 types: gas phase synthesis method and solid-phase synthesis, wherein: gas phase synthesis method has chemical Vapor deposition process, solid-phase synthesis comprises self propagating high temperature synthesis method, pressure sintering, hot isostatic pressing method, impulsive discharge sintering process etc.But above-mentioned preparing method's common defects all is to obtain high purity Ti 3SiC 2Powder, major impurity are carbide and/or the oxide compounds of titanium etc., so that have limited the widespread use of this material in industry member.
In sum, but seek the simple preparation of industrialization high-purity Ti of a kind of technology 3SiC 2The method of powder will be the difficult problem that this area Kei need solve.
Summary of the invention
To the above-mentioned defective and the problem of prior art existence, but the purpose of this invention is to provide the simple preparation of industrialization high-purity Ti of a kind of technology 3SiC 2The method of powder is to satisfy Ti 3SiC 2The industrial application requirement of material.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is following:
A kind of preparation high-purity Ti 3SiC 2The method of powder comprises the steps:
A) at first Polycarbosilane is dissolved in the organic solvent, adds titanium hydride powder then, ultrasonic making mixes;
B) heat while stirring, it is thick until the organic solvent volatilization solution to be become, and carries out vacuum-drying then;
C) under inert atmosphere protection, carry out subzero treatment: 500～1200 ℃ of insulations 0.5～2 hour, temperature rise rate was 1～10 ℃/min;
D) under inert atmosphere protection, carry out pyroprocessing: 1400～1600 ℃ of insulations 0.5～2 hour, temperature rise rate was 1～10 ℃/min; Promptly get described high-purity Ti 3SiC 2Powder.
Described organic solvent is preferably industrial naptha, YLENE or toluene.
The mass ratio of described organic solvent and Polycarbosilane is recommended as 1: 1～and 10: 1, be preferably 3: 1～10: 1.
The mass ratio of described titanium hydride powder and Polycarbosilane is recommended as 0.5: 1～and 2.5: 1, be preferably 1.5: 1～2.5: 1.
Said vacuum drying temperature is recommended as 80～200 ℃, is preferably 100～200 ℃.
The said vacuum drying time is recommended as 0.5～6 hour, is preferably 2～6 hours.
Described inert atmosphere is preferably argon atmospher.
Key point in the technical scheme of the present invention mainly contains following four:
With titanium hydride as the titanium source, release the titanium that H-H reaction generates through titanium hydride and replace titanium valve of the prior art, not only improved the purity in titanium source, and the titanium that generates has higher activity.
2. the mass ratio of titanium hydride and Polycarbosilane.The mass ratio that titanium hydride and Polycarbosilane are suitable is the preparation high-purity Ti 3SiC 2Key.The Polycarbosilane amount more after a little while, split product can not provide enough activeconstituentss, titanium hydride can't complete reaction generates Ti 3SiC 2, can cause existing dephasigns such as TiC; When Polycarbosilane more for a long time, titanium hydride is converted into Ti fully 3SiC 2, but unnecessary Polycarbosilane can be converted into SiC; When having only mass ratio when titanium hydride and Polycarbosilane suitable, titanium hydride can be converted into Ti fully 3SiC 2, and do not have SiC mutually residual, so that form high-purity Ti 3SiC 2Powder;
3. adopt titanium hydride as the titanium source, can reduce the rough handling temperature.
4. pyroprocessing can promote each component after the subzero treatment further to react, and causes titanium elements to be converted into Ti fully 3SiC 2
Compared with prior art, utilize the Ti of the inventive method preparation 3SiC 2Powder has purity height (can reach more than 98%), percent crystallinity is high (is entirely Ti 3SiC 2Phase), Ti 3SiC 2The less advantages such as (being about several microns) of powder granularity, and present method technology is simple, easy handling, and energy consumption is less, can satisfy suitability for industrialized production Ti 3SiC 2The mass-producing of powder and requirement economically have widespread use and are worth.
Description of drawings
The Ti that Fig. 1 makes for embodiment 1 3SiC 2The stereoscan photograph of powder;
The Ti that Fig. 2 makes for embodiment 1 3SiC 2The X ray diffracting spectrum of powder;
The Ti that Fig. 3 makes for embodiment 2 3SiC 2The X ray diffracting spectrum of powder;
The Ti that Fig. 4 makes for embodiment 3 3SiC 2The X ray diffracting spectrum of powder;
The Ti that Fig. 5 makes for embodiment 4 3SiC 2The X ray diffracting spectrum of powder.
Embodiment
Below in conjunction with embodiment and accompanying drawing to the present invention do further in detail, intactly explanation.
Embodiment 1
A) earlier the 10g Polycarbosilane is dissolved in the 30g YLENE, adds the 17.2g titanium hydride powder then, ultrasonic it is mixed;
B) heat while stirring, it is thick until the organic solvent volatilization solution to be become, and carries out vacuum-drying 3 hours at 130 ℃ then;
C) under the argon atmospher protection, carry out subzero treatment: 700 ℃ of insulations 0.5 hour, temperature rise rate was 5 ℃/min;
D) under the argon atmospher protection, carry out pyroprocessing: 1500 ℃ of insulations 0.5 hour, temperature rise rate was 5 ℃/min; Promptly get Ti 3SiC 2Powder.
At low-temperature process, contingent reaction equation is following:
TiH 2→Ti+H 2
PCS→SiC+C
Ti+C→TiC
Ti+SiC→Ti 5Si 3C+C；
At high-temperature process, contingent reaction equation is following:
Ti 5Si 3C+C→Ti 3SiC 2+Si
Ti 5Si 3C+TiC+C→Ti 3SiC 2。
The Ti that Fig. 1 makes for present embodiment 3SiC 2The stereoscan photograph of powder, visible by Fig. 1: the Ti that makes 3SiC 2Powder granularity is less, and median size is 0.95 μ m.
The Ti that Fig. 2 makes for present embodiment 3SiC 2The X ray diffracting spectrum of powder, visible by Fig. 2: the Ti that makes 3SiC 2Powder purity is high, and percent crystallinity is high.
Embodiment 2
The difference of present embodiment and embodiment 1 only is: the subzero treatment temperature is 1100 ℃; All the other contents are all with described in the embodiment 1.
The Ti that Fig. 3 makes for present embodiment 3SiC 2The X ray diffracting spectrum of powder, visible by Fig. 3: the Ti that makes 3SiC 2Powder purity is high, and percent crystallinity is high.
Embodiment 3
The difference of present embodiment and embodiment 1 only is: the quality of titanium hydride powder and Polycarbosilane is respectively 15.2g and 10g; All the other contents are all with described in the embodiment 1.
The Ti that Fig. 4 makes for present embodiment 3SiC 2The X ray diffracting spectrum of powder, visible by Fig. 4: Ti is fully with Ti 3SiC 2Form exist, contain a small amount of SiC impurity; Can learn the Ti that makes in addition 3SiC 2Powder percent crystallinity is high.
Embodiment 4
The difference of present embodiment and embodiment 1 only is: the quality of titanium hydride powder and Polycarbosilane is respectively 15.2g and 10g; The subzero treatment temperature is 1100 ℃; All the other contents are all with described in the embodiment 1.
The Ti that Fig. 5 makes for present embodiment 3SiC 2The X ray diffracting spectrum of powder, visible by Fig. 5: Ti is fully with Ti 3SiC 2Form exist, contain a small amount of SiC impurity; Can learn the Ti that makes in addition 3SiC 2Powder percent crystallinity is high.
Be necessary at last to be pointed out that at this: above embodiment only is used for the present invention is done further explain; Can not be interpreted as the restriction to protection domain of the present invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.

Claims (6)

1. one kind prepares high-purity Ti 3SiC 2The method of powder is characterized in that, comprises the steps:
A) at first Polycarbosilane is dissolved in the organic solvent, adds titanium hydride powder then, ultrasonic making mixes;
B) heat while stirring, it is thick until the organic solvent volatilization solution to be become, and carries out vacuum-drying then;
C) under inert atmosphere protection, carry out subzero treatment: 500～1200 ℃ of insulations 0.5～2 hour, temperature rise rate was 1～10 ℃/min;
D) under inert atmosphere protection, carry out pyroprocessing: 1400～1600 ℃ of insulations 0.5～2 hour, temperature rise rate was 1～10 ℃/min; Promptly get described high-purity Ti 3SiC 2Powder.
2. preparation high-purity Ti according to claim 1 3SiC 2The method of powder is characterized in that: described organic solvent is industrial naptha, YLENE or toluene.
3. preparation high-purity Ti according to claim 1 3SiC 2The method of powder is characterized in that: the mass ratio of described organic solvent and Polycarbosilane is 1: 1～10: 1.
4. preparation high-purity Ti according to claim 1 3SiC 2The method of powder is characterized in that: the mass ratio of described titanium hydride powder and Polycarbosilane is 0.5: 1～2.5: 1.
5. preparation high-purity Ti according to claim 1 3SiC 2The method of powder is characterized in that: said vacuum-drying is meant at 80～200 ℃, vacuum-drying 0.5～6 hour.
6. preparation high-purity Ti according to claim 1 3SiC 2The method of powder is characterized in that: described inert atmosphere is an argon atmospher.
CN2011104211243A 2011-12-15 2011-12-15 Method for preparing high-purity Ti3SiC2 powder Pending CN102530945A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103849790A (en) * 2014-03-20 2014-06-11 苏州赛菲集团有限公司 In-situ generated homogenous nano ceramic-metal composite material and preparation method thereof
CN104233128A (en) * 2014-05-29 2014-12-24 华东理工大学 Preparation method applicable to secondary heating of semisolid thixotropic cast aluminum alloy
CN115959668A (en) * 2022-12-12 2023-04-14 长安大学 Full-liquid state synthetic Ti 3 SiC 2 Ceramic and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555137A (en) * 2009-05-20 2009-10-14 南京工业大学 (TiB2 plus TiC)/Ti3SiC2 multi-phase ceramic material and prepration method thereof
CN102050448A (en) * 2009-11-06 2011-05-11 中国科学院上海硅酸盐研究所 Method for preparing Ti3SiC2-based powder
CN102241514A (en) * 2011-05-24 2011-11-16 武汉理工大学 Method for synthetizing Ti3SiC2 high-purity powder

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555137A (en) * 2009-05-20 2009-10-14 南京工业大学 (TiB2 plus TiC)/Ti3SiC2 multi-phase ceramic material and prepration method thereof
CN102050448A (en) * 2009-11-06 2011-05-11 中国科学院上海硅酸盐研究所 Method for preparing Ti3SiC2-based powder
CN102241514A (en) * 2011-05-24 2011-11-16 武汉理工大学 Method for synthetizing Ti3SiC2 high-purity powder

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103849790A (en) * 2014-03-20 2014-06-11 苏州赛菲集团有限公司 In-situ generated homogenous nano ceramic-metal composite material and preparation method thereof
CN103849790B (en) * 2014-03-20 2016-04-20 苏州中宝复合材料股份有限公司 A kind of in-situ preparation homogeneous nano level ceramic-metal composite material and preparation method thereof
CN104233128A (en) * 2014-05-29 2014-12-24 华东理工大学 Preparation method applicable to secondary heating of semisolid thixotropic cast aluminum alloy
CN115959668A (en) * 2022-12-12 2023-04-14 长安大学 Full-liquid state synthetic Ti 3 SiC 2 Ceramic and preparation method thereof

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Application publication date: 20120704