CN101070248A - Method for synthesizing aluminium-titanium carbonate ceramic powder - Google Patents

Abstract

This invention relates to a synthetic method of aluminium carbide titanium ceramic powder. The invention takes TiH2 powder, Al powder and TiC powder as raw material, add Sn as accessory ingredient, dyr mix the raw materials acoording to mol ratio of TiH2:TiC:Al:Sn=1:1:1:0.1 for 10 hours, execute piece under 30 to 50 pressure, then put at high temperature furnace, under vacuum atmosphere rise the furnace temperature to 1350 to 1550 deg by rate of 15 to 40 deg per minute, holding time for 5 to 15min, execute low cost high-purity Ti3AlC2 powder.

Description

A kind of synthetic method of aluminium-titanium carbonate ceramic powder

Technical field

The present invention relates to a kind of synthetic method of aluminium-titanium carbonate ceramic powder, particularly low-cost aluminium-titanium carbonate Ti ₃AlC ₂The atmospheric synthesizing method of ceramic powder belongs to ceramic materials preparation technology field.

Background technology

Aluminium-titanium carbonate Ti ₃AlC ₂With its high conductivity, anti-oxidant, heat shock resistance, corrosion-resistant, self-lubricating, easy premium properties such as processing, become the preferred material of parts such as bearing, high-temperature structural components, the charged friction of high speed.The various parts that preparation engineering is used not only need in enormous quantities Ti cheaply ₃AlC ₂Powder, and Ti ₃AlC ₂The necessary purity height of powder especially can not contain TiC impurity phase.Because the existence of impurity phase is to Ti ₃AlC ₂Excellent specific properties such as the high conductivity of material, self-lubricating and easy processing all have disadvantageous effect.So mass production low-cost high-purity Ti ₃AlC ₂Powder has crucial meaning in practical application.

At present, synthetic Ti ₃AlC ₂Powder is a raw material with Ti powder, Al powder and C powder usually, according to Ti: Al: C=3: and 1: 2 molar ratio ingredient, by normal pressure synthesis method (Chinese invention patent ZL200510011650.7), combustion synthesis method (Chinese invention patent ZL03146390.8; J.Eur.Ceram.Soc.2003,23:567; Rare Metals Materials and engineering .2003,32 (7): 56 1.), mechanical activation low temperature synthesis method (Ceramics International, 2007; 33:169) wait preparation Ti ₃AlC ₂Powder.

But with the Ti powder, Al powder and C powder are feedstock production Ti ₃AlC ₂Can there be following problem in powder:

1) have Ti powder and C powder in the batching, both react acutely, emit a large amount of heat, " thermal explosion " phenomenon occurs, cause system temperature sharply to raise, and cause simple substance Al volatilization loss serious, thereby have changed the reaction ratio of each constituent element in the system, influence Ti ₃AlC ₂Purity.

2) occur " thermal explosion " phenomenon in the reaction process and can cause temperature rapid fluctuation in the stove, the temperature parameter in the building-up process is wayward.

3) there is TiC impurity phase in the product usually, influenced Ti ₃AlC ₂The purity of powder and performance;

4) used Ti powder content is more in the especially above-mentioned batching, and Ti powder price is higher at present, causes synthetic Ti ₃AlC ₂The powder cost is too high.

For addressing the above problem, Chinese invention patent (application number: 200610114335.1) open report, directly adopt the TiC powder to replace part Ti and whole C in the above-mentioned raw materials, according to Ti: Al: TiC: Sn=1: 1: 1: 0.1 molar ratio ingredient, synthesized high purity Ti ₃AlC ₂Powder.This method not only efficiently solves the thermal explosion problem, and the corresponding Ti that reduced ₃AlC ₂The cost of powder.

But still used a certain amount of Ti powder in the above-mentioned batching, be called as the Ti of ' aerial metal ', along with the development of aerospace, it is had a sudden rise in social status.If synthetic Ti ₃AlC ₂Powder does not use the Ti powder, can not only further reduce Ti ₃AlC ₂Synthetic cost, and Ti resource that can saves valuable.

Summary of the invention

The objective of the invention is to utilize titanium hydride TiH ₂Replace titanium Ti, adopt TiH ₂: Al: TiC: Sn=1: 1: 1: 0.1 synthetic Ti of new prescription ₃AlC ₂Powder, new prescription not only has Ti: Al: TiC: Sn=1: advantages such as the supression thermal explosion that 1: 1: 0.1 batching is had, synthetic powder purity height, and further reduced Ti ₃AlC ₂Synthetic cost because TiH ₂Price be 1/3 of Ti.

The present invention adopts TiH ₂Powder, Al powder and TiC powder are raw material, interpolation Sn is an auxiliary agent, in wide temperature range, in the short period of time, realizes high purity, low-cost Ti with the normal pressure synthesis technology ₃AlC ₂The batch of powder is synthetic.

The objective of the invention is to be achieved through the following technical solutions:

A kind of synthetic method of aluminium-titanium carbonate ceramic powder: contain following steps;

(1) with TiH ₂Powder, Al powder and TiC powder are raw material, interpolation Sn is an auxiliary agent, presses TiH ₂: TiC: Al: Sn=1: 1: 1: 0.1 molar ratio ingredient;

(2) above-mentioned batching and agate ball are put into ball grinder, on ball mill, do and mixed 10 hours;

(3) with the above-mentioned batching that mixes briquetting under 30～50MPa pressure;

(4) above-mentioned briquetting is placed High Temperature Furnaces Heating Apparatus, under the vacuum atmosphere, with the temperature rise rate of 15～40 ℃/min furnace temperature is risen to 1350～1550 ℃, soaking time is 5～15min, makes low-cost high-purity Ti ₃AlC ₂Powder.

The invention has the beneficial effects as follows:

The first, the TiH that the present invention adopts ₂: Al: TiC: Sn=1: 1: 1: 0.1 batching, effectively restrained and occurred the thermal explosion problem in the reactive system, reduce the system temperature big ups and downs and caused the high temperature loss problem of Al, help system components to generate by design proportion, guarantee high purity Ti ₃AlC ₂Synthetic.

The second, the TiH that the present invention adopts ₂: Al: TiC: Sn=1: 1: 1: 0.1 batching, adopt TiH ₂Powder and TiC powder replace whole Ti powder and the C powder in the batching, because TiH ₂With the price of TiC powder be respectively 1/3 of Ti powder, therefore with Ti: Al: C=3: batching was compared in 1: 2, still and Ti: Al: TiC: Sn=1: batching was compared in 1: 1: 0.1, synthesized Ti ₃AlC ₂The cost of powder reduces.

The 3rd, technical process of the present invention is simple, in the vacuum oven of routine, and under the vacuum atmosphere, synthetic Ti ₃AlC ₂Powder purity height, the synthesis temperature wide ranges, the used time is short, and sintering process parameter is stable, is suitable for large-scale production.

Description of drawings

Fig. 1 is that normal pressure synthesis legal system of the present invention is equipped with Ti ₃AlC ₂The process flow sheet of powder;

Fig. 2 is the Ti of normal pressure synthesis method preparation of the present invention ₃AlC ₂The X-ray diffraction of powder (XRD) collection of illustrative plates.

Embodiment

Below as shown in Figure 1, the present invention is further elaborated in conjunction with embodiment:

Embodiment 1: a kind of synthetic method of aluminium-titanium carbonate ceramic powder, contain following steps;

1) presses TiH ₂: Al: TiC: Sn=1: 1: 1: 0.1 molar ratio ingredient takes by weighing Ti powder 16.8 grams, Al powder 9.1 grams, TiC powder 20.1 grams, Sn powder 4.0 grams;

2) as shown in Figure 1 above-mentioned batching is put into ball grinder and placed on the ball mill batch mixing 10 hours;

3) batching that will mix is pressed into block under the pressure of 30MPa.

4) above-mentioned briquetting is put into High Temperature Furnaces Heating Apparatus, vacuum atmosphere rises to 1350 ℃ with the temperature rise rate of 15 ℃/min with furnace temperature, and soaking time is 15min, promptly makes high purity Ti ₃AlC ₂Powder, the X-ray diffraction of powder (XRD) collection of illustrative plates as shown in Figure 2.As seen from Figure 2, the product purity height removes Ti in the XRD figure spectrum ₃AlC ₂Not having other impurity outward, exists mutually.

Embodiment 2: a kind of synthetic method of aluminium-titanium carbonate ceramic powder: contain following steps;

1) presses TiH ₂: Al: TiC: Sn=1: 1: 1: 0.1 molar ratio ingredient takes by weighing Ti powder 16.8 grams, Al powder 9.1 grams, TiC powder 20.1 grams, Sn powder 4.0 grams;

2) above-mentioned batching is put into ball grinder and placed on the ball mill batch mixing 10 hours;

3) batching that will mix is pressed into block under the pressure of 40MPa.

4) above-mentioned briquetting is put into High Temperature Furnaces Heating Apparatus, vacuum atmosphere rises to 1450 ℃ with the temperature rise rate of 30 ℃/min with furnace temperature, and soaking time is 10min, promptly makes high purity Ti ₃AlC ₂Powder, its XRD result is identical with embodiment one.

Embodiment 3: a kind of synthetic method of aluminium-titanium carbonate ceramic powder: contain following steps;

1) presses TiH ₂: Al: TiC: Sn=1: 1: 1: 0.1 molar ratio ingredient takes by weighing Ti powder 16.8 grams, Al powder 9.1 grams, TiC powder 20.1 grams, Sn powder 4.0 grams;

2) above-mentioned batching is put into ball grinder and placed on the ball mill batch mixing 10 hours;

3) batching that will mix is pressed into block under the pressure of 50MPa.

4) above-mentioned briquetting is put into High Temperature Furnaces Heating Apparatus, vacuum atmosphere rises to 1500 ℃ with the temperature rise rate of 40 ℃/min with furnace temperature, and soaking time is 5min, promptly makes high purity Ti ₃AlC ₂Powder, its XRD result is identical with embodiment one.

Embodiment 4: a kind of synthetic method of aluminium-titanium carbonate ceramic powder: contain following steps;

1) presses TiH ₂: Al: TiC: Sn=1: 1: 1: 0.1 molar ratio ingredient takes by weighing Ti powder 33.6 grams, Al powder 18.2 grams, TiC powder 40.2 grams, Sn powder 8.0 grams;

2) above-mentioned batching is put into ball grinder and placed on the ball mill batch mixing 10 hours;

3) batching that will mix is pressed into block under the pressure of 50MPa.

4) above-mentioned briquetting is put into High Temperature Furnaces Heating Apparatus, vacuum atmosphere rises to 1550 ℃ with the temperature rise rate of 30 ℃/min with furnace temperature, and soaking time is 5min, promptly makes high purity Ti ₃AlC ₂Powder, its XRD result is identical with embodiment one.

Claims (1)

1. the synthetic method of an aluminium-titanium carbonate ceramic powder is characterized in that containing following steps;

(1) with TiH ₂Powder, Al powder and TiC powder are raw material, interpolation Sn is an auxiliary agent, presses TiH ₂: TiC: Al: Sn=1: 1: 1: 0.1 molar ratio ingredient;

(2) above-mentioned batching and agate ball are put into ball grinder, on ball mill, do and mixed 10 hours;

(3) with the above-mentioned batching that mixes briquetting under 30～50MPa pressure;

(4) above-mentioned briquetting is placed High Temperature Furnaces Heating Apparatus, under the vacuum atmosphere, with the temperature rise rate of 15～40 ℃/min furnace temperature is risen to 1350～1550 ℃, soaking time is 5～15min, makes Ti ₃AlC ₂Powder.

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