JP2002235129A - Method for producing metal - ceramics composite material having reduced gas releasabiltiy - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing a metal-ceramics composite material, by which the composite material having reduced gas releasability can be obtained. SOLUTION: The method for producing the metal - ceramics composite material having reduced gas releasability comprises forming a preform by using ceramics powder or a ceramic fiber subjected to heat treatment at 500 to 1,500 deg.C under the atmosphere or a nitrogen atmosphere, then infiltrating aluminum or a aluminum alloy melted in an electric furnace into the preform at 700 to 900 deg.C under a nitrogen atmosphere without pressurizing the aluminum or the aluminum alloy and cooling the infiltrated material to form a composite material, and after that, heat treating the cooled composite material at 300 to 600 deg.C under vacuum.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a method for producing a metal-ceramic composite material, and more particularly to a method for producing a metal-ceramic composite material used in a semiconductor or liquid crystal film forming process.

[0002]

2. Description of the Related Art Recently, a metal-ceramic composite material using a ceramic powder or a ceramic fiber as a reinforcing material and aluminum or an aluminum alloy as a matrix has begun to be used in a semiconductor manufacturing apparatus, a liquid crystal manufacturing apparatus and the like.

[0003] As a method for producing this composite material, particularly a method for producing a composite material using aluminum as a matrix as a metal, methods such as powder metallurgy, high pressure casting, and vacuum casting have been conventionally known. However, in these methods, the content of the ceramics as a reinforcing material cannot be increased, or a large-sized pressing device is required, or it is difficult to form a near net, and the cost is extremely high. It was not satisfactory.

[0004] Recently, as a manufacturing method for solving the above problem, there is a non-pressurized metal infiltration method (Primex ^™ ) developed by Rankside Co., USA. This method uses SiC
, Al ₂ O _3, or the ceramic powder preforms formed by the contacting the aluminum alloy containing Mg, such as, to which the permeate of aluminum was melted by heating to a temperature of 700 to 900 ° C. in a N ₂ atmosphere furnace in the alloy Is the way. This has the feature that the wettability between the ceramic powder and the molten metal is improved by utilizing the chemical reaction of Mg, and that it can penetrate into the preform without performing mechanical pressing.
This is an excellent method that does not require a pressurizing device.

[0005]

However, since the composite material produced by this method contains a large amount of hydrocarbon-based or carbon-dioxide-based gas, a large amount of such gas is released from the composite material, and the temperature is high. As the temperature rises, the release of those gases further increases, and there is a problem that it is difficult to use them in a film forming process for semiconductors and liquid crystals used in a heated atmosphere.

The present invention has been made in view of the problems of the above-described method for producing a metal-ceramic composite material, and has as its object to produce a metal-ceramic composite material capable of obtaining a composite material with reduced gas emission. It is to provide a method.

[0007]

Means for Solving the Problems The present inventors have conducted intensive studies to achieve the above object, and as a result, specified a ceramic powder or ceramic fiber as a reinforcing material and aluminum or an aluminum alloy as a matrix to form a composite material. The inventor has found that a composite material with reduced gas emission can be obtained by manufacturing and subjecting the manufactured composite material to vacuum heat treatment, thereby completing the present invention.

That is, the present invention relates to (1) a preform formed from ceramic powder or ceramic fiber heat-treated at a temperature of 500 to 1500 ° C. in the air or a nitrogen atmosphere, and aluminum or aluminum melted in an electric furnace on the preform. Aluminum alloy 700-9 in nitrogen atmosphere
After infiltration at a temperature of 00 ° C. under no pressure and cooling to produce a composite material, the composite material is placed in a vacuum at 300 to 600 ° C.
A method for producing a metal-ceramic composite material with reduced outgassing, characterized by performing a heat treatment at a temperature of at least one.
(2) 500 to 15 in the air or nitrogen atmosphere
A preform is formed from ceramic powder or ceramic fiber heat-treated at a temperature of 00 ° C., and aluminum or an aluminum alloy melted in an electric furnace is penetrated into the preform at a temperature of 700 to 900 ° C. in a nitrogen atmosphere without pressure. After producing the composite material by cooling, the composite material is heat-treated in a vacuum at a temperature of 300 to 600 ° C., and further heat-treated in the air at a temperature of 300 to 1000 ° C. The gist of the present invention is to provide a method for producing a reduced metal-ceramic composite material (claim 2). This will be described in more detail below.

As described above, as the production method of the present invention, by first specifying that the ceramic powder or the ceramic fiber to be used is heat-treated, it is possible to remove hydrocarbon-based gas and the like adhering to the ceramic powder or the ceramic fiber. Next, by specifying the aluminum or aluminum alloy to be infiltrated into the formed preform as the aluminum or aluminum alloy melted in the electric furnace, the gas contained therein is reduced as compared with the aluminum or aluminum alloy melted and formed in the conventional gas furnace. By heat-treating the composite material made using them in a vacuum,
Since gas adhering to the surface of the composite material can be removed,
This is a manufacturing method that can provide a composite material in which the emission of gas is far reduced.

The heat treatment of the ceramic powder or the ceramic fibers is preferably performed in the air or in a nitrogen atmosphere. If the heat treatment is not performed in the air or in a nitrogen atmosphere, organic substances and carbon adhering to the ceramic powder are burned. Not preferred. The processing temperature is preferably from 500 to 1500 ° C.
If the temperature is lower than 00 ° C., the attached gas cannot be reduced,
If the temperature is higher than 00 ° C., the oxidation of the ceramic powder, especially the non-oxide powder proceeds, which is not preferable.

On the other hand, the heat treatment temperature in vacuum is as follows:
If the temperature is lower than 300 ° C., the adhering gas cannot be reduced. If the temperature is higher than 600 ° C., aluminum or an aluminum alloy as a matrix dissolves and spreads on the surface, which is not preferable. .

Another manufacturing method other than the above is a manufacturing method in which the above-mentioned vacuum-processed product is further heat-treated in the air. And the like can also remove organic impurities such as

[0013]

More particularly the method of producing a composite material of the embodiment of the present invention, first, SiC as a ceramic powder or ceramic fiber as reinforcement, Al ₂ O _3, A
A ceramic powder or a ceramic fiber such as 1N is prepared. On the other hand, an ingot of an aluminum alloy containing Mg dissolved in an electric furnace as a metal to be a matrix is also prepared.

The prepared ceramic powder or ceramic fiber is placed in the atmosphere or in a nitrogen atmosphere at 500 to 150
Heat treatment at a temperature of 0 ° C. A preform is formed from the obtained ceramic powder or ceramic fiber. On the other hand, the ingot of the aluminum alloy obtained by melting the prepared electric furnace is melted in a nitrogen atmosphere, and penetrates into the preform formed with the molten aluminum alloy in a nitrogen atmosphere at a temperature of 700 to 900 ° C. without pressure. Let it.

[0015] The resulting composite material is vacuumed for 300 to 60
Heat treatment at a temperature of 0 ° C. to produce a composite material with reduced outgassing. If necessary, add this to the atmosphere for 300 ~
Heat treatment is performed at a temperature of 1000 ° C. to produce a composite material in which organic impurities are also reduced. The degree of vacuum for vacuum processing is 1
The degree of vacuum may be 0 ^-1 to 10 ^-2 torr or more.

When a metal-ceramic composite material is produced by the above method, a composite material with reduced outgassing can be obtained.

[0017]

EXAMPLES Hereinafter, the present invention will be described in more detail by giving specific examples of the present invention together with comparative examples.

(Example 1) (1) Production of metal-ceramic composite material with reduced gas emission Commercially available Si of # 180 (average particle size 66 μm) as a reinforcing material
70 parts by weight of C powder and 30 parts by weight of a commercially available SiC powder of # 500 (average particle size 25 μm) were used.
A heat treatment was performed at a temperature of 200 ° C., and a colloidal silica liquid was added as a binder to the heat-treated SiC powder in an amount such that the silica solid content became 2 parts by weight, and ion-exchanged water was added thereto.
4 parts by weight were added and mixed by a pot mill for 12 hours.

The obtained slurry is 50 × 50 × 50 mm
Was poured into a rubber mold from which a molded article was obtained, and was allowed to stand for 24 hours to precipitate SiC powder, and the supernatant was removed with a cloth or the like. Then, it was put into a freezing room, frozen for 30 hours, and demolded. . The obtained molded body was fired at a temperature of 1000 ° C. to form a preform having a filling ratio of SiC powder of 70% by volume.

The obtained preform is made of Al-12Si-
An ingot of an aluminum alloy melted in an electric furnace having a 3Mg composition was brought into contact with the ingot, which was heat-treated at a temperature of 825 ° C. in a nitrogen atmosphere. . The obtained composite material was heated at 450 ° C. in a vacuum having a degree of vacuum of 10 ⁻³ torr.
At 24 ° C. for 24 hours to produce a composite material with reduced outgassing.

(2) Evaluation The amount of gas released from the obtained composite material was determined by temperature-programmed desorption gas analysis using a quadrupole mass spectrometer (manufactured by ULVAC). The higher the current value, the greater the emission amount). As a result, the degree of vacuum is 10 ⁻⁷ torr.
under a temperature of 200 ° C., the amount of released H ₂ O gas is 1
× 10 ^-7 amps, N ₂ , CO etc. are 3 × 10 ^-9 amps, O ₂ etc. are 5 × 10 ^-10 amps, C
O _{2 and the} like are 3 × 10 ⁻⁹ amps, and C _n H _m is 1 × 10 ⁻⁹ amps.
^-10 amperes, and the emission of gas was smaller than in any of the comparative examples described below.

(Example 2) The composite material obtained in Example 1 was further heat-treated at 550 ° C for 5 hours in the air, and the reduction of residual carbon and the like was examined by weight change before and after the heat treatment. As a result, the weight after heat treatment was 0.1% as compared with that before heat treatment.
It was confirmed that the residual carbon and the like were reduced by 1%. This is described in connection with Example 1. According to the present invention, when a composite material is manufactured, a composite material with reduced gas emission can be obtained. It is shown that a composite material can be obtained.

Comparative Example Used for comparison in Example 1.
SiC powder that has not been heat treated,
The aluminum alloy ingot used in Example 1 was
Aluminum alloy melted in a furnace
Other than the vacuum-processed composite material
A composite material was prepared and evaluated in the same manner as in Example 1. The result
Fruit, H_TwoO gas is 3 × 10^-7Amps and N_Two, CO
Etc. is 3 × 10^-8Ampere and O_TwoEtc. is 5 × 10^-9A
And CO_TwoEtc. is 1 × 10^-8Ampere,
C _nH_mIs 3 × 10^-TenAnd the gas release from Example 1.
There were many.

[0024]

As described above, according to the method for producing a metal-ceramic composite material of the present invention, a method for producing a composite material with reduced gas emission can be obtained. As a result, a composite material that can be used in a semiconductor or liquid crystal film formation step can be obtained.

Claims (2)

[Claims] 1. 500-1 in the air or nitrogen atmosphere
A preform is formed from ceramic powder or ceramic fiber heat-treated at a temperature of 500 ° C., and aluminum or an aluminum alloy melted in an electric furnace is penetrated into the preform in a nitrogen atmosphere at a temperature of 700 to 900 ° C. without pressure. A method for producing a metal-ceramic composite material with reduced outgassing, characterized in that after cooling to produce a composite material, the composite material is heat-treated in a vacuum at a temperature of 300 to 600 ° C. 2. 500 to 1 in air or nitrogen atmosphere.
A preform is formed from ceramic powder or ceramic fiber heat-treated at a temperature of 500 ° C., and aluminum or an aluminum alloy melted in an electric furnace is penetrated into the preform in a nitrogen atmosphere at a temperature of 700 to 900 ° C. without pressure. After producing a composite material by cooling, the composite material is heat-treated in a vacuum at a temperature of 300 to 600 ° C., and further heat-treated in the air at a temperature of 300 to 1000 ° C. A method for producing a reduced metal-ceramic composite material.