CN101423215B

CN101423215B - Method for preparing Al4SiC4 powder

Info

Publication number: CN101423215B
Application number: CN2008102310952A
Authority: CN
Inventors: 王刚; 王来稳; 周继伟; 周军; 王龙庆; 李代兵
Original assignee: Sinosteel Luoyang Institute of Refractories Research Co Ltd
Current assignee: Sinosteel Luoyang Institute of Refractories Research Co Ltd
Priority date: 2008-11-27
Filing date: 2008-11-27
Publication date: 2010-12-01
Anticipated expiration: 2028-11-27
Also published as: CN101423215A

Abstract

The invention belongs to the technical fields of ceramic and fireproof material, providing a method used for preparing Al4SiC4 powder. The method comprises the specific processes as follows: metal Al powder, Si powder, carbon black or graphite are taken as raw materials; the metal Al powder, Si powder and carbon black or graphite are uniformly mixed according to the molar ratio of 4:1:4.2-4.5; the mixture of the metal Al powder, Si powder and carbon black or graphite is arranged in the ball-grinding tank of a high-energy ball-grinder where aluminum stearate used as a dispersant is added; the ball material ratio is 10-15:1; the ball-grinding is carried out for 20-40 hours under a vacuum argon state, the rotation speed is 800-1000r/min; therefore, the Al4SiC4 powder is gained. The method has simple preparation process, stable process parameter, easy controlling, high ball-grinding efficiency and complete raw material reaction, and can prepare the high-purity powder containing no Al3C4 phase.

Description

A kind of Al 4SiC 4The preparation method of powder

Technical field

The present invention relates to the synthetic method of pottery, refractory materials, be specifically related to a kind of Al ₄SiC ₄The preparation method of powder.

Background technology

Al ₄SiC ₄Powder has high-melting-point (about 2037 ℃), than low density (3.03g/cm ³), the characteristics such as aggressiveness of thermal conductive resin and high temperature resistance melt, slag, and Al ₄SiC ₄Generate mullite and corundum protective layer at material surface when material at high temperature is oxidized,, good prospects for application is arranged at aspects such as functional refractory such as slide plate, the mouths of a river so its antioxidant property is good.The material supplier author of Japan and Britain has utilized Al ₄SiC ₄Excellent oxidation-resistance has a better effect in carbon containing refractory.Yet because Al ₄SiC ₄The synthetic difficulty of powder, relevant all the time Al ₄SiC ₄The synthetic report is very limited.Generally be the synthetic Al of method that adopts solid state reaction, slowly heats up at present both at home and abroad ₄SiC ₄Powder.There is complex process in this method, shortcomings such as long reaction time, energy consumption height, and the Al that synthesizes ₄SiC ₄Unavoidably there is the Al of easy aquation in powder ₃C ₄Phase.

Summary of the invention

The purpose of this invention is to provide a kind of Al ₄SiC ₄The preparation method of powder promptly adopts high-energy ball milling technology to synthesize Al ₄SiC ₄The method of powder; High-energy ball milling method equipment and synthesis technique are simple, can prepare high purity and not contain Al ₃C ₄The Al of phase ₄SiC ₄Powder.

Preparation method's of the present invention concrete technology is: with metal A l powder, Si powder and carbon black or graphite is raw material, and metal A l powder, Si powder and carbon black or graphite are mixed 4:1:4.2～4.5 in molar ratio; The compound of metal A l powder, Si powder and carbon black or graphite is packed in the ball grinder of high energy ball mill, add aluminum stearate as dispersion agent, ratio of grinding media to material is 10～15:1, and ball milling is 20～40 hours under vacuum argon gas state, rotating speed is 800～1000 rev/mins, obtains Al ₄SiC ₄Powder.

The granularity of described metal A l powder≤10 μ m, purity 〉=99%; The granularity of described Si powder≤10 μ m, purity 〉=99%; The granularity of described carbon black or graphite≤1 μ m, purity 〉=98%, fugitive constituent≤0.2%.

Described aluminum stearate add-on is 0.2～0.5% of metal A l powder, Si powder and carbon black or a graphite mixture quality.

Metal A l powder, Si powder and carbon black or graphite put into by additional proportion that urethane jar ball milling is dried to be mixed evenly, and ratio of grinding media to material is 3:1, ball milling 3～5 hours.

The mill ball of high energy ball mill is a Ceramic Balls.

Substantive distinguishing features of the present invention is:

1) preparation technology is simple, and processing parameter is stable, easy to control;

2) grinding efficiency height, raw material reaction is complete, prepared Al ₄SiC ₄Powder purity height, and do not contain easy aquation

Al ₃C ₄Phase can be widely used in pottery, refractories industry;

3) energy consumption is low, and is pollution-free, environmentally friendly.

Embodiment

Embodiment 1:

With metal A l powder (granularity 10 μ m, purity 〉=99%), Si powder (granularity 10 μ m, purity 〉=99%) and carbon black (granularity≤1 μ m, purity 〉=98%, fugitive constituent≤0.2%) 4:1:4.5 prepares burden in molar ratio, does in the urethane jar with ratio of grinding media to material 3:1 and mixes 3h; Get compound 50 gram then and pack in the ball grinder of high energy ball mill, add the aluminum stearate of mixture quality 0.2%, put into 500 gram corundum balls, vacuumize and make vacuum tightness, feed argon gas less than 1 handkerchief, with 800 change minute ball milling 20 hours.Powder Al after measured behind the ball milling ₄SiC ₄Purity reaches more than 80%, and does not contain Al ₃C ₄Phase.

Embodiment 2:

With metal A l powder (granularity 5 μ m, purity 〉=99%), Si powder (granularity 10 μ m, purity 〉=99%) and carbon black (granularity≤1 μ m, purity 〉=98%, fugitive constituent≤0.2%) 4:1:4.2 batching in molar ratio, do in the urethane jar with ratio of grinding media to material 3:1 and to mix 4h; Get compound 50 gram then and pack in the ball grinder of high energy ball mill, add the aluminum stearate of mixture quality 0.3%, put into 600 gram corundum balls, vacuumize and make vacuum tightness, feed argon gas less than 1 handkerchief, with 900 change minute ball milling 25 hours.Powder is Al after measured behind the ball milling ₄SiC ₄, purity reaches more than 84%, and does not contain Al ₃C ₄Phase.

Embodiment 3:

With metal A l powder (granularity 5 μ m, purity 〉=99%), Si powder (granularity 10 μ m, purity 〉=99%) and graphite (granularity≤1 μ m, purity 〉=98%, fugitive constituent≤0.2%) 4:1:4.2 batching in molar ratio, do in the urethane jar with ratio of grinding media to material 3:1 and to mix 4h; Get compound 50 gram then and pack in the ball grinder of high energy ball mill, add the aluminum stearate of mixture quality 0.3%, put into 600 gram corundum balls, vacuumize and make vacuum tightness, feed argon gas less than 1 handkerchief, with 1000 change minute ball milling 30 hours.Powder is Al after measured behind the ball milling ₄SiC ₄, purity reaches more than 86%, and does not contain Al ₃C ₄Phase.

Embodiment 4:

With metal A l powder (granularity 5 μ m, purity 〉=99%), Si powder (granularity 5 μ m, purity 〉=99%) and graphite (granularity≤1 μ m, purity 〉=98%, fugitive constituent≤0.2%) 4:1:4.3 batching in molar ratio, do in the urethane jar with ratio of grinding media to material 3:1 and to mix 5h; Get compound 50 gram then and pack in the ball grinder of high energy ball mill, add 0.5% aluminum stearate of mixture quality, put into 750 gram corundum balls, vacuumize and make vacuum tightness, feed argon gas less than 1 handkerchief, with 800 change minute ball milling 40 hours.Powder is Al after measured behind the ball milling ₄SiC ₄, purity reaches more than 89%, and does not contain Al ₃C ₄Phase.

Embodiment 5:

With metal A l powder (granularity 5 μ m, purity 〉=99%), Si powder (granularity 5 μ m, purity 〉=99%) and carbon black (granularity≤1 μ m, purity 〉=98%, fugitive constituent≤0.2%) 4:1:4.3 batching in molar ratio, do in the urethane jar with ratio of grinding media to material 3:1 and to mix 5h; Get compound 50 gram then and pack in the ball grinder of high energy ball mill, add 0.3% aluminum stearate of mixture quality, put into 750 gram corundum balls, vacuumize and make vacuum tightness, feed argon gas less than 1 handkerchief, with 1000 change minute ball milling 30 hours.Powder is Al after measured behind the ball milling ₄SiC ₄, purity reaches more than 92%, and does not contain Al ₃C ₄Phase.

Claims

1. Al ₄SiC ₄The preparation method of powder is characterized in that: described Al ₄SiC ₄The concrete technology of powder preparation method is: with metal A l powder, Si powder and carbon black or graphite is raw material, and metal A l powder, Si powder and carbon black or graphite 4: 1: 4.2 in molar ratio～4.5 are mixed; The compound of metal A l powder, Si powder and carbon black or graphite is packed in the ball grinder of high energy ball mill, the aluminum stearate that adds metal A l powder, Si powder and carbon black or graphite mixture quality 0.2～0.50% is as dispersion agent, ratio of grinding media to material is 10～15: 1, vacuumize and make vacuum tightness less than 1 handkerchief, fed the argon gas ball milling 20～40 hours, rotating speed is 800～1000 rev/mins, obtains Al ₄SiC ₄Powder.

2. a kind of Al according to claim 1 ₄SiC ₄The preparation method of powder is characterized in that: the granularity of described metal A l powder≤10 μ m, purity 〉=99%; The granularity of described Si powder≤10 μ m, purity 〉=99%; The granularity of described carbon black or graphite≤1 μ m, purity 〉=98%, fugitive constituent≤0.2%.

3. a kind of Al according to claim 1 ₄SiC ₄The preparation method of powder is characterized in that: the mill ball of high energy ball mill is a Ceramic Balls.