CN102180673A - Preparation method of Ti3SiC2 powder with hexagonal layer structure - Google Patents

Abstract

The invention discloses a preparation method of Ti3SiC2 powder with a hexagonal layer structure. The preparation method comprises the following steps: mixing titanium powder, silicon powder and graphite powder which have a certain grain size as raw materials in a proportion; and successively carrying out ball-milling, solvent removal, sintering and the like so as to prepare the Ti3SiC2 powder with the hexagonal layer structure. The method has the advantages of simple process, easily controlled parameters, short production period, less energy consumption and no environment pollution, and is suitable for industrial production; and the obtained Ti3SiC2 powder has the characteristics of small density, large strength, high temperature resistance, oxidization resistance, good conductivity and heat conducting property and the like, and has a wide application prospect and huge potential economic benefits in the fields of engineering technology, space technology, defense industry, micro-electronics and the like.

Description

A kind of six side's laminate structure Ti 3SiC 2The preparation method of powder

Technical field

The present invention relates to a kind of preparation method of carbon titanium silicide of ad hoc structure, more specifically, is a kind of six side's laminate structure Ti ₃SiC ₂The preparation method of powder.

Background technology

Carbon titanium silicide (Ti ₃SiC ₂, Titanium silicon carbide) and be a kind of comprehensive stupalith, both had high temperature resistant, anti-oxidant, high-intensity characteristics, have the characteristic such as conduction, heat conduction, workability, plasticity of metallic substance again.The seventies in 20th century, since tougheners such as fiber, whisker develop requirement with the high thrust-weight ratio engine of aviation rapidly, ceramic matric composite becomes the research focus, adopting fiber, whisker to strengthen can make the toughness of material improve, but because preparation cost height and poor reliability, the application of ceramic matric composite is restricted.Therefore, people such as material supply section scholar Jeitschko W. begin to explore the high-temperature material that has metal and ceramic character concurrently, find a kind of silicon titanium-carbide (Ti finally in the Ti-Si-C system ₃SiC ₂), this respect is reported referring to " Monatash Chem " 1967 the 98th phase 329-333 pages or leaves.Ti ₃SiC ₂The characteristic of existing metal, good heat conductivility and conductivity are arranged at normal temperatures, relatively low Vickers' hardness and higher modulus of elasticity have ductility at normal temperatures, can process as metal, at high temperature also has plasticity, simultaneously, it has the performance of stupalith again, i.e. high-yield strength, high-melting-point, high thermal stability and good antioxidant property, at high temperature can keep high strength, this respect is reported referring to " investigation of materials journal " 2005 the 19th phase 457-463 pages or leaves.More meaningfully it also has than lower frictional coefficient of traditional solid lubricant graphite, molybdenumdisulphide and good self-lubricating property.But the technology of above-mentioned research is all very complicated, and the production cycle is long, energy consumption is big, simultaneously environment is had to a certain degree pollution, therefore is very restricted on using, and numerous inherent advantages of carbon titanium silicide material fully can't be utilized for the mankind.

Summary of the invention

The object of the invention is to provide a kind of six side's laminate structure Ti ₃SiC ₂The preparation method of powder has that technology is simple, parameter is easy to control, with short production cycle a, less energy consumption, eco-friendly characteristics.

The present invention realizes by following technique means: can not react and the characteristics volatile, that surface tension is little, cheap with titanium valve, silica flour and Graphite Powder 99 at alcohol, liquid medium as titanium valve, silica flour and Graphite Powder 99 mixing and ball milling provides a kind of preparation six side's laminate structure Ti ₃SiC ₂The method of powder has that technology simply is easy to control, with short production cycle a, less energy consumption, characteristics that cost is low.

Preparation six side's laminate structure Ti of the present invention ₃SiC ₂The method of powder may further comprise the steps:

(1) preparation raw material mixture: get the Graphite Powder 99 of 300 purpose titanium valves, 200 purpose silica flours and the particle diameter＜20 μ m of analytical pure specification, the three is according to 3: (1～1.2): after 2 mixed in molar ratio is even, obtain raw mix;

(2) ball milling: the above-mentioned raw materials mixture is placed ball mill, add 10ml alcohol, under argon shield, after 12 hours, send into the vibration drying device with 200 rev/mins rotating speed ball milling;

Affiliated alcohol is as liquid medium, and its selection is very crucial, must satisfy following three conditions: one, in titanium valve, silica flour and Graphite Powder 99 chemical reaction does not take place, can guarantee not introduce impurity in raw material; Two, have lower boiling point, can send out by meeting at a lower temperature and remove, thereby avoid high temperature can make the situation that chemical reaction takes place between powdered alloy generation oxidation and the metal-powder; Three, surface tension is little, can prevent that powders is agglomerating.In addition, affiliated liquid medium has cheap characteristics the most carefully, thereby helps reducing production costs.Alcohol has above condition concurrently, and can be recycled, and therefore, is that the ideal of liquid medium among the present invention is selected, but satisfies the also replaceable alcohol of material of above-mentioned condition as liquid medium of the present invention for him.

(3) desolventize: with 5 ℃/minute heat-up rates the vibration drying device is warming up to 50 ℃, vibration drying naturally cooled to room temperature in 60 minutes to the thorough volatilization of alcohol, cross 300 mesh sieves, obtained the ball milling powder;

(4) sintering: above-mentioned ball milling powder is put into vacuum sintering furnace, be evacuated to 5.0 * 10 ^-3Pa is warmed up to 200 ℃ with 15 ℃/minute speed, is incubated 0.5 hour, is warming up to 1400-1500 ℃ with 10 ℃/minute speed then, is incubated after 1 hour, cools to room temperature with the furnace, can obtain the Ti of six side's laminate structures ₃SiC ₂Powder.

Utilize the present invention to prepare six side's laminate structure Ti ₃SiC ₂Powder adopts mechanical alloying method and vaccum sintering process combination, technology is simple, parameter with control, with short production cycle, energy consumption is few, environmentally safe, is suitable for suitability for industrialized production; Gained Ti ₃SiC ₂The particle diameter of powder is between 1～10 μ m, have that density is little, intensity is big, good characteristic such as high temperature resistant, anti-oxidant and electrical and thermal conductivity performance is good, be with a wide range of applications and huge potential economic benefit in fields such as engineering, spationautics, national defense industry and microelectronics.

Description of drawings

Fig. 1 is the Ti of the embodiment of the invention 1 described six side's laminate structures ₃SiC ₂The X-ray diffraction analysis figure of powder 1;

Fig. 2 is the Ti of the embodiment of the invention 2 described six side's laminate structures ₃SiC ₂The scanning electron microscope analysis figure of powder 2;

Fig. 3 is the Ti of the embodiment of the invention 3 described six side's laminate structures ₃SiC ₂The scanning electron microscope analysis figure of powder 3.

Embodiment

Below further describe the present invention by embodiment, as known by the technical knowledge, the present invention also can describe by other the scheme that does not break away from the technology of the present invention feature, thus all within the scope of the present invention or the change that is equal in the scope of the invention all be included in the invention.

Embodiment 1:

Be prepared as follows six side's laminate structure Ti ₃SiC ₂Powder:

(1) preparation raw material mixture: get 300 purpose titanium valve 21.741g, the 300 purpose silica flour 4.227g of analytical pure specification and the Graphite Powder 99 3.624g of particle diameter＜20 μ m, obtain raw mix after mixing;

(2) ball milling: the ball grinder that the above-mentioned raw materials mixture is placed planetary high-energy ball mill, add 10ml alcohol, in airflow rate is that 0.5L/min, air pressure are under the argon gas stream protection of 0.2MPa, adopt diameter to be respectively each 50 of three kinds of steel balls of 10mm, 6mm, 4mm, under the 110V voltage raw mix being carried out ball milling after 12 hours, send into the vibration drying device with 200 rev/mins rotating speeds;

(3) desolventize: with 5 ℃/minute heat-up rates the vibration drying device is warming up to 50 ℃, vibration drying naturally cooled to room temperature in 60 minutes to the thorough volatilization of alcohol, cross 300 mesh sieves, obtained the ball milling powder;

(4) sintering: above-mentioned ball milling powder is put into vacuum sintering furnace, be evacuated to 5.0 * 10 ^-3Pa is warmed up to 200 ℃ with 15 ℃/minute speed, is incubated 0.5 hour to remove steam, is warming up to 1400 ℃ with 10 ℃/minute speed then, is incubated after 1 hour, and furnace cooling can obtain the Ti of six side's laminate structures to room temperature in 10 hours ₃SiC ₂Powder 1, sealing is preserved.

Ti to above-mentioned six side's laminate structures ₃SiC ₂Powder 1 carries out X-ray diffraction analysis, the result as shown in Figure 1, its crystallization phases is Ti basically ₃SiC ₂, its primary particle size is about 5～15 μ m.

Embodiment 2:

Be prepared as follows six side's laminate structure Ti ₃SiC ₂Powder:

(1) preparation raw material mixture: get 300 purpose titanium valve 21.741g, the 300 purpose silica flour 4.650g of analytical pure specification and the Graphite Powder 99 3.624g of particle diameter＜20 μ m, obtain raw mix after mixing;

(2) ball milling: the ball grinder that the above-mentioned raw materials mixture is placed planetary high-energy ball mill, add 10ml alcohol, in airflow rate is that 0.5L/min, air pressure are under the argon gas stream protection of 0.2MPa, adopt diameter to be respectively each 50 of three kinds of steel balls of 10mm, 6mm, 4mm, under the 110V voltage raw mix being carried out ball milling after 12 hours, send into the vibration drying device with 200 rev/mins rotating speeds;

(3) desolventize: with 5 ℃/minute heat-up rates the vibration drying device is warming up to 50 ℃, vibration drying naturally cooled to room temperature in 60 minutes to the thorough volatilization of alcohol, cross 300 mesh sieves, obtained the ball milling powder;

(4) sintering: above-mentioned ball milling powder is put into vacuum sintering furnace, be evacuated to 5.0 * 10 ^-3Pa is warmed up to 200 ℃ with 15 ℃/minute speed, is incubated 0.5 hour to remove steam, is warming up to 1400 ℃ with 10 ℃/minute speed then, is incubated after 1 hour, and furnace cooling can obtain the Ti of six side's laminate structures to room temperature in 10 hours ₃SiC ₂Powder 2, sealing is preserved.

Ti to above-mentioned six side's laminate structures ₃SiC ₂Powder 2 carries out scanning electron microscope analysis, the result as shown in Figure 2, powder presents six squares of clear rule, marginal surface is also relatively slicker and more sly, the obvious refinement of particle reaches micron order, and some big coacervate surface arrangement some tiny particles, and these short grained sizes are observed under scanning electron microscope, diameter is approximately 0.5～5 μ m, also has some less than 300nm.

Embodiment 3:

Be prepared as follows six side's laminate structure Ti ₃SiC ₂Powder:

(1) preparation raw material mixture: get 300 purpose titanium valve 21.741g, the 300 purpose silica flour 4.650g of analytical pure specification and the Graphite Powder 99 3.624g of particle diameter＜20 μ m, obtain raw mix after mixing;

(2) ball milling: the ball grinder that the above-mentioned raw materials mixture is placed planetary high-energy ball mill, add 10ml alcohol, in airflow rate is that 0.5L/min, air pressure are under the argon gas stream protection of 0.2MPa, adopt diameter to be respectively each 50 of three kinds of steel balls of 10mm, 6mm, 4mm, under the 110V voltage raw mix being carried out ball milling after 12 hours, send into the vibration drying device with 200 rev/mins rotating speeds;

(3) desolventize: with 5 ℃/minute heat-up rates the vibration drying device is warming up to 50 ℃, vibration drying naturally cooled to room temperature in 60 minutes to the thorough volatilization of alcohol, cross 300 mesh sieves, obtained the ball milling powder;

(4) sintering: above-mentioned ball milling powder is put into vacuum sintering furnace, be evacuated to 5.0 * 10 ^-3Pa is warmed up to 200 ℃ with 15 ℃/minute speed, is incubated 0.5 hour to remove steam, is warming up to 1450 ℃ with 10 ℃/minute speed then, is incubated after 1 hour, and furnace cooling can obtain the Ti of six side's laminate structures to room temperature in 10 hours ₃SiC ₂Powder 3, sealing is preserved.

Ti to above-mentioned six side's laminate structures ₃SiC ₂Powder 3 carries out scanning electron microscope analysis, the result as shown in Figure 3, Ti ₃SiC ₂Powder presents tangible laminated structure, and the thin slice comparatively homogeneous that distributes, and every layer thickness is about 50nm.

In sum, the Ti that utilizes the present invention to prepare ₃SiC ₂Powder has six side's laminate structures, and particle diameter is little, production technique is simple, parameter is easy to control, with short production cycle, energy consumption is few, is suitable for suitability for industrialized production.

Claims (1)

1. side's laminate structure Ti ₃SiC ₂The preparation method of powder is characterized in that, may further comprise the steps:

(1) preparation raw material mixture: get the Graphite Powder 99 of 300 purpose titanium valves, 200 purpose silica flours and the particle diameter＜20 μ m of analytical pure specification, the three is according to 3: (1～1.2): after 2 mixed in molar ratio is even, obtain raw mix;

(2) ball milling: the above-mentioned raw materials mixture is placed ball mill, add 10ml alcohol, under argon shield, after 12 hours, send into the vibration drying device with 200 rev/mins rotating speed ball milling;

(3) desolventize: with 5 ℃/minute heat-up rates the vibration drying device is warming up to 50 ℃, vibration drying naturally cooled to room temperature in 60 minutes to the thorough volatilization of alcohol, cross 300 mesh sieves, obtained the ball milling powder;

(4) sintering: above-mentioned ball milling powder is put into vacuum sintering furnace, be evacuated to 5.0 * 10 ^-3Pa is warmed up to 200 ℃ with 15 ℃/minute speed, is incubated 0.5 hour, is warming up to 1400-1500 ℃ with 10 ℃/minute speed then, is incubated after 1 hour, cools to room temperature with the furnace, can obtain the Ti of six side's laminate structures ₃SiC ₂Powder.

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