CN1958514A

CN1958514A - Method for preparing Ti2AlC ceramic material

Info

Publication number: CN1958514A
Application number: CN 200610104816
Authority: CN
Inventors: 朱建锋; 王芬; 罗宏杰; 杨海波; 陈平
Original assignee: Shaanxi University of Science and Technology
Current assignee: Shaanxi University of Science and Technology
Priority date: 2006-10-30
Filing date: 2006-10-30
Publication date: 2007-05-09
Anticipated expiration: 2026-10-30
Also published as: CN100396650C

Abstract

This invention discloses a method for preparing Ti2AlC ceramic material. The method comprises: (1) preparing a mixture of Ti, Al and C, adding sodium stearate dispersant into the mixture, performing dry ball-milling for mechanically alloying and obtained fine powder of TiAl, TiC, and minor Ti and Al, and vacuum-drying; (2) loading the dried powder into a graphite mold, and hot-pressing sintering in Ar or vacuum. After ball-milled, Ti, Al and C powder can perform in situ reaction to form TiC intermediate phase, which is then hot-pressing sintered to form processable ceramic material with Ti2AlC as the major crystalline. The method has such advantages as simple process and low sintering temperature. The prepared Ti2AlC ceramic material is uniform and compact.

Description

A kind of Ti 2The preparation method of AlC stupalith

Technical field

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

Background technology

Titanium aluminium carbon (Ti ₂AlC) 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 two kinds, in-situ hot pressing sintering and HIP sintering.These two kinds of methods all are to utilize Ti, Al, C to be raw material, directly prepare titanium aluminium carbon block material by reaction sintering.But the purity of this method is difficult to control, and impurity is mutually more, comprises reactant residue and intermediate product, and Ti is also arranged ₃AlC ₂The thing phase can't large-scale industrialized production.

Summary of the invention

This purpose is to overcome the shortcoming of above-mentioned prior art, and provide a kind of and need not atmosphere protection, technology is simple, is easy to industrialization, and the Ti of low cost of manufacture ₂The preparation method of AlC 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: at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C are made mixture; The sodium stearate dispersion agent that adds mixture quality 0.2-0.5% in mixture adopts dry ball milling, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling at 70-80 ℃ of following vacuum-drying 4-5 hour; Dried powder is packed in the graphite grinding tool, and with 1200 ℃-1300 ℃, the pressure hot pressed sintering of 10-35MPa got final product in 1-2 hour under argon gas or vacuum condition.

The present invention utilizes Ti powder, Al powder, C powder and a small amount of additive behind high-energy ball milling, and reaction in generates TiC intermediate phase, and this composite granule forms principal crystalline phase again behind hot pressed sintering be Ti ₂The processable ceramics material of AlC, not only cost is low in the present invention, technology is simple, and 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, Al powder, C powder, the XRD analysis result of sample, and wherein X-coordinate is that XRD tests 2 θ angles, ordinate zou is a diffraction peak intensity;

Fig. 2 is the XRD analysis result of 1200 ℃ of sintered specimens, and wherein X-coordinate is that XRD tests 2 θ angles, and ordinate zou is a diffraction peak intensity.

Embodiment

Below in conjunction with accompanying drawing the present invention is described in further detail

Embodiment 1, at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.2%, the employing dry ball milling is 730 rpms planetary ball mill with rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 6 hours, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling 70 ℃ of following vacuum-dryings 5 hours; Dried powder is packed in the graphite grinding tool, and with 1300 ℃, the pressure hot pressed sintering of 10MPa got final product in 1 hour under the argon gas condition.

Embodiment 2, at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.4%, the employing dry ball milling is 700 rpms planetary ball mill with rotating speed, pellet matter is than being 1: 10, the ball milling time is 7 hours, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling 76 ℃ of following vacuum-dryings 4.5 hours; Dried powder is packed in the graphite grinding tool, and with 1270 ℃, the pressure hot pressed sintering of 20MPa got final product in 2 hours under vacuum condition.

Embodiment 3, at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.3%, the employing dry ball milling is 760 rpms planetary ball mill with rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 8 hours, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling 72 ℃ of following vacuum-dryings 4.2 hours; Dried powder is packed in the graphite grinding tool, and with 1220 ℃, the pressure hot pressed sintering of 26MPa got final product in 1.4 hours under the argon gas condition.

Embodiment 4, at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.5%, the employing dry ball milling is 800 rpms planetary ball mill with rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 8 hours, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling 80 ℃ of following vacuum-dryings 4 hours; Dried powder is packed in the graphite grinding tool, and with 1200 ℃, the pressure hot pressed sintering of 35MPa got final product in 1.8 hours under vacuum condition.

Referring to Fig. 1, principal crystalline phase is TiC and a spot of TiAl as seen from Figure 1 ₃

Referring to Fig. 2, as seen from Figure 2, this material principal crystalline phase is Ti ₂AlC and a spot of TiC.

Claims

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

1) at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C are made mixture;

2) add the sodium stearate dispersion agent of mixture quality 0.2-0.5% in mixture, adopt dry ball milling, making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium;

3) with the powder behind the ball milling at 70-80 ℃ of following vacuum-drying 4-5 hour;

4) dried powder is packed in the graphite grinding tool, with 1200 ℃-1300 ℃, the pressure hot pressed sintering of 10-35MPa got final product in 1-2 hour under argon gas or vacuum condition.

2, a kind of Ti according to claim 1 ₂The preparation method of AlC stupalith is characterized in that: said dry ball milling employing rotating speed is 700-800 rpm a planetary ball mill, and the pellet mass ratio is 1: 10, and the ball milling time is 6-8 hour.

3, a kind of Ti according to claim 1 ₂The preparation method of AlC stupalith is characterized in that: at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C are made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.2%, the employing dry ball milling is 730 rpms planetary ball mill with rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 6 hours, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling 70 ℃ of following vacuum-dryings 5 hours; Dried powder is packed in the graphite grinding tool, and with 1300 ℃, the pressure hot pressed sintering of 10MPa got final product in 1 hour under the argon gas condition.

4, a kind of Ti according to claim 1 ₂The preparation method of AlC stupalith is characterized in that: at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C are made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.4%, the employing dry ball milling is 700 rpms planetary ball mill with rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 7 hours, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling 76 ℃ of following vacuum-dryings 4.5 hours; Dried powder is packed in the graphite grinding tool, and with 1270 ℃, the pressure hot pressed sintering of 20MPa got final product in 2 hours under vacuum condition.

5, a kind of Ti according to claim 1 ₂The preparation method of AlC stupalith is characterized in that: at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C are made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.3%, the employing dry ball milling is 760 rpms planetary ball mill with rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 8 hours, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling 72 ℃ of following vacuum-dryings 4.2 hours; Dried powder is packed in the graphite grinding tool, and with 1220 ℃, the pressure hot pressed sintering of 26MPa got final product in 1.4 hours under the argon gas condition.

6, a kind of Ti according to claim 1 ₂The preparation method of AlC stupalith is characterized in that: at first by mass percentage 71.11% Ti, 20.00% Al and 8.89%C are made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.5%, the employing dry ball milling is 800 rpms planetary ball mill with rotating speed, the pellet mass ratio is 1: 10, the ball milling time is 8 hours, and making its mechanical alloying form principal crystalline phase is TiAl, TiC and a little amount of titanium, the tiny powder of aluminium; With the powder behind the ball milling 80 ℃ of following vacuum-dryings 4 hours; Dried powder is packed in the graphite grinding tool, and with 1200 ℃, the pressure hot pressed sintering of 35MPa got final product in 1.8 hours under vacuum condition.