CN101624287A

CN101624287A - Preparation method for Ti3SiC2 ceramic material

Info

Publication number: CN101624287A
Application number: CN200910023534A
Authority: CN
Inventors: 王芬; 刘波波; 朱建锋; 杨志波; 许红娅; 薛小霜; ***
Original assignee: Shaanxi University of Science and Technology
Current assignee: Shaanxi University of Science and Technology
Priority date: 2009-08-07
Filing date: 2009-08-07
Publication date: 2010-01-13

Abstract

The invention relates to a preparation method for a Ti3SiC2 ceramic material, which comprises the following steps of: firstly, preparing Ti, Si and C into mixture, adding sodium stearate dispersing agent and little amount of A1 into the mixture for enhancing sintering, adopting a dry method for ball milling to lead the mixture to be mechanically alloyed to form main phases such as Ti, Si and little amount of SiC as well as Ti5Si3 fine powder, using an alcohol wet method to take materials from the ball-milled powder, and vacuum-drying; putting the dried powder into a graphite grinding tool, and carrying out hot-pressing and sintering under the condition of argon or vacuum. The preparation method uses Ti powder, Si powder, C powder and little amount of additives for high-energy ball milling, fining crystalline grain, simultaneously carrying out in situ reaction to generate little amount of SiC, Ti5Si3 intermediate phase. The compound powder forms a machinable ceramic material with the main phases of Ti3SiC2 after hot-pressed and sintered. The preparation method has simple technique and low firing temperature, and the prepared material has even and compact structure.

Description

A kind of Ti 3SiC 2The preparation method of stupalith

Technical field

The invention belongs to stupalith and make the field, be specifically related to a kind of Ti ₃SiC ₂The preparation method of stupalith.

Background technology

Titanium silicon-carbon (Ti ₃SiC ₂) be a kind of new ceramic material with special performance.The advantage that the performance of this material has been concentrated metallic substance and stupalith, as conduction, heat conduction, can process, high temperature resistant, anti-thermal shock, the very peculiar over-all properties of self-lubricating, have broad application prospects in fields such as high-temperature structural components, Chemical Preservation material, electrode materials and machinable materials.

At present, the main preparation methods of this material has multiple, in-situ hot pressing sintering, HIP sintering, discharge plasma sintering method, solid-state displacement reaction in synthesis method, chemical vapour deposition reaction method, self propagating high temperature method, mechanical alloying method, arc-melting method.Having only in-situ hot pressing sintering, HIP sintering, discharge plasma sintering method in this several different methods is to utilize Ti, Si, C to be raw material, directly prepares titanium silicon-carbon block materials by reaction sintering.But the purity of this method is difficult to control, and impurity is mutually more, comprises reactant residue and intermediate product SiC and Ti ₅Si ₃, TiC thing phase is also arranged, can't large-scale industrialized production.

Summary of the invention

The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of to need vacuum protection, technology simple, and the Ti of low cost of manufacture ₃SiC ₂The preparation method of stupalith, according to the material purity height that preparation method of the present invention makes, foreign matter content is low.

For achieving the above object, the preparation method that the present invention adopts is:

1) at first, by mass percentage 66.6～68.5% Ti powder, 19.5～20.1% Si powder and 11.4～13.9% C powder are made mixture;

2) secondly, in mixture, add the sodium stearate dispersion agent and the 2.698% aluminium powder dry ball milling 18-24h of mixture quality 0.5%, earlier the ball milling cylinder is fed argon gas before the ball milling and discharge air in the ball milling cylinder;

3) then, get material with the powder wet method of alcohol after, at 50-80 ℃ of vacuum-drying 20-30 hour to ball milling;

4) with dried powder, dry-pressing formed in the graphite grinding tool of packing into, with 1200 ℃-1300 ℃, the pressure hot pressed sintering of 10-25MPa obtained Ti in 1-2 hour under vacuum condition ₃SiC ₂Stupalith.

Dry ball milling of the present invention adopts the QM-ISP2 planetary ball mill of rotating speed 400r/min, and the pellet mass ratio is 1: 10, and the ball milling time is 18 hours, makes crystal grain thinning after its mechanical alloying, and reaction in generates a small amount of SiC, Ti simultaneously ₅Si ₃The intermediate phase; What wet method was got the material employing is ethanolic soln.

The present invention utilizes Ti powder, Si powder, C powder and a small amount of additive behind high-energy ball milling, crystal grain thinning, and reaction in generates a small amount of SiC, Ti simultaneously ₅Si ₃The intermediate phase.This composite granule forms principal crystalline phase again behind hot pressed sintering be Ti ₃SiC ₂Processable ceramics material, not only cost is low in the present invention, technology is simple, firing temperature is low, and the material structure even compact that makes.

Description of drawings

Fig. 1 is the high-energy ball milling process of Ti powder, Si powder, C powder, the XRD analysis result of sample, and wherein X-coordinate is 2 θ, ordinate zou is a diffraction peak intensity.

Fig. 2 is the XRD analysis result of 1300 ℃ of sintered specimens, and wherein X-coordinate is that XRD tests 2 θ angles, and ordinate zou is a diffraction peak intensity.

Fig. 3 is the SEM picture of 1300 ℃ of sintered specimens.

Embodiment

Below in conjunction with drawings and Examples the present invention is described in further detail.

Embodiment 1, at first, by mass percentage 66.6% Ti powder, 20.1% Si powder and 13.3% C powder made mixture; Secondly, the sodium stearate dispersion agent and the 2.698% aluminium powder employing dry ball milling that add mixture quality 0.5% in mixture are the QM-ISP2 planetary ball mill of 400r/min with the rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 18 hours, make crystal grain thinning after its mechanical alloying, reaction in generates a small amount of SiC, Ti simultaneously ₅Si ₃Elder generation is to the air in the ball milling cylinder feeding argon gas discharge ball milling cylinder before the intermediate phase, ball milling; Then, adopt the ethanolic soln wet method to get material to the powder behind the ball milling, then 55 ℃ of vacuum-dryings 28 hours; With dried powder, dry-pressing formed in the graphite grinding tool of packing into, with 1200 ℃, the pressure hot pressed sintering of 10MPa obtained Ti in 1.5 hours under vacuum condition ₃SiC ₂Stupalith.Referring to Fig. 1, principal crystalline phase is Ti, Si and a small amount of SiC, Ti as seen from Figure 1 ₅Si ₃Tiny powder.

Embodiment 2, at first, by mass percentage 68.5% Ti powder, 19.5% Si powder and 12% C powder made mixture; Secondly, the sodium stearate dispersion agent and the 2.698% aluminium powder employing dry ball milling that add mixture quality 0.5% in mixture are the QM-ISP2 planetary ball mill of 400r/min with the rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 20 hours, make crystal grain thinning after its mechanical alloying, reaction in generates a small amount of SiC, Ti simultaneously ₅Si ₃Elder generation is to the air in the ball milling cylinder feeding argon gas discharge ball milling cylinder before the intermediate phase, ball milling; Then, adopt the ethanolic soln wet method to get material to the powder behind the ball milling, then 50 ℃ of vacuum-dryings 30 hours; With dried powder, dry-pressing formed in the graphite grinding tool of packing into, with 1300 ℃, the pressure hot pressed sintering of 15MPa obtained Ti in 2 hours under vacuum condition ₃SiC ₂Stupalith.As seen from Figure 2, this material principal crystalline phase is Ti ₃SiC ₂And a spot of SiC.As seen from Figure 3, this material microstructure is the synusia shape.

Embodiment 3, at first, by mass percentage 68.5% Ti powder, 20.1% Si powder and 11.4% C powder made mixture; Secondly, the sodium stearate dispersion agent and the 2.698% aluminium powder employing dry ball milling that add mixture quality 0.5% in mixture are the QM-ISP2 planetary ball mill of 400r/min with the rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 22 hours, make crystal grain thinning after its mechanical alloying, reaction in generates a small amount of SiC, Ti simultaneously ₅Si ₃Elder generation is to the air in the ball milling cylinder feeding argon gas discharge ball milling cylinder before the intermediate phase, ball milling; Then, adopt the ethanolic soln wet method to get material to the powder behind the ball milling, then 60 ℃ of vacuum-dryings 25 hours; With dried powder, dry-pressing formed in the graphite grinding tool of packing into, with 1250 ℃, the pressure hot pressed sintering of 20MPa obtained Ti in 2 hours under vacuum condition ₃SiC ₂Stupalith.

Embodiment 4, at first, by mass percentage 66.6% Ti powder, 19.5% Si powder and 13.9% C powder made mixture; Secondly, the sodium stearate dispersion agent and the 2.698% aluminium powder employing dry ball milling that add mixture quality 0.5% in mixture are the QM-ISP2 planetary ball mill of 400r/min with the rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 24 hours, make crystal grain thinning after its mechanical alloying, reaction in generates a small amount of SiC, Ti simultaneously ₅Si ₃Elder generation is to the air in the ball milling cylinder feeding argon gas discharge ball milling cylinder before the intermediate phase, ball milling; Then, adopt the ethanolic soln wet method to get material to the powder behind the ball milling, then 70 ℃ of vacuum-dryings 23 hours; With dried powder, dry-pressing formed in the graphite grinding tool of packing into, with 1280 ℃, the pressure hot pressed sintering of 18MPa obtained Ti in 2 hours under vacuum condition ₃SiC ₂Stupalith.

Embodiment 5, at first, by mass percentage 67% Ti powder, 20% Si powder and 13% C powder made mixture; Secondly, the sodium stearate dispersion agent and the 2.698% aluminium powder employing dry ball milling that add mixture quality 0.5% in mixture are the QM-ISP2 planetary ball mill of 400r/min with the rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 21 hours, make crystal grain thinning after its mechanical alloying, reaction in generates a small amount of SiC, Ti simultaneously ₅Si ₃Elder generation is to the air in the ball milling cylinder feeding argon gas discharge ball milling cylinder before the intermediate phase, ball milling; Then, adopt the ethanolic soln wet method to get material to the powder behind the ball milling, then 80 ℃ of vacuum-dryings 20 hours; With dried powder, dry-pressing formed in the graphite grinding tool of packing into, with 1230 ℃, the pressure hot pressed sintering of 13MPa obtained Ti in 1 hour under vacuum condition ₃SiC ₂Stupalith.

Claims

1, a kind of Ti ₃SiC ₂The preparation method of stupalith is characterized in that:

3) then, adopt wet method to get material to the powder behind the ball milling, then at 50-80 ℃ of vacuum-drying 20-30 hour;

2, Ti according to claim 1 ₃SiC ₂The preparation method of stupalith, it is characterized in that: said dry ball milling adopts the QM-ISP2 planetary ball mill of rotating speed 400r/min, and the pellet mass ratio is 1: 10, and the ball milling time is 18 hours, make crystal grain thinning after its mechanical alloying, reaction in generates a small amount of SiC, Ti simultaneously ₅Si ₃The intermediate phase.

3, Ti according to claim 1 ₃SiC ₂The preparation method of stupalith is characterized in that: what said wet method was got the material employing is ethanolic soln.