JPH1171184A - Binder for aln sintered product, its production and binding of aln sintered product therewith - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a binder for AlN sintered products, capable of highly enhancing the air tightness and binding strength of a bound portion by mixing YAG powder with AlN powder, calcining the mixture and subsequently crushing the calcination product into particles having particle diameters of a specific value or less. SOLUTION: This binder for AlN sintered products is obtained by mixing 100 pts.wt. of YAG (Y3 Al5 O12 ) powder having an average particle diameter of <=50 μm with 30-150 pts.wt. of AlN(aluminum nitride) powder in a solvent, drying the mixture, granulating the dried mixture, calcining the granules at a temperature of 1,500-1,850 deg.C in the atmosphere of nitrogen gas and subsequently crushing the calcined granules into particles having particle diameters of <=100 μm. The AlN sintered products are bound to each other by kneading the binder in an organic solvent, coating the obtained paste on the binding portions of the AlN sintered products, or forming the binder into a sheet-like product, disposing the sheet-like product on the binding portions of the AlN sintered products, and subsequently thermally treating the superposed AlN sintered products at a temperature exceeding 1,850 deg.C in the atmosphere of nitrogen gas. The binding of the AlN sintered products with the binder gives a volume contraction coefficient of <=10% on the sintering, a porosity of <=5% in the bound portion, and a binding strength of >=50 Mpa.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a bonding agent for AlN sintered bodies used for bonding AlN (aluminum nitride) sintered bodies, a method for producing the same, and a method for bonding AlN sintered bodies using the same.

[0002]

2. Description of the Related Art In recent years, in an etcher or a CVD apparatus which is a semiconductor manufacturing apparatus, a susceptor or a clamp ring for holding a wafer is required to have high thermal conductivity, high rigidity at high temperature, or high thermal shock resistance against a rapid rise and fall temperature. Al
Forming with an N sintered body is performed. Conventionally,
To make the above susceptor and clamp ring,
As a bonding agent for bonding a component having a complicated shape made of an N sintered body, the same component as a grain boundary phase component of an AlN sintered body fired using a sintering aid such as Y ₂ O ₃ (yttria) is used. Alternatively, a powder comprising this and an additive for lowering the melting point is known. This bonding agent is applied as a paste to the joint portion of the AlN sintered body, and at or below the firing temperature of the AlN sintered body,
Heat treatment in the same atmosphere as the firing
It is used for joining sintered bodies.

[0003]

However, the conventional AlN
The bonding agent for a sintered body causes a dimensional difference from the AlN sintered body due to its sintering shrinkage, and a gap is generated in the joint of the AlN sintered body, so that the hermeticity and the joint strength of the joint are reduced. . Therefore, an object of the present invention is to provide a bonding agent for an AlN sintered body capable of significantly improving the airtightness and bonding strength of a bonded portion, a method for producing the same, and a method for bonding an AlN sintered body using the same. .

[0004]

In order to solve the above-mentioned problems, a bonding agent for an AlN sintered body of the present invention comprises a YAG powder or a mixed powder of Y ₂ O ₃ and Al ₂ O _{3 having} a YAG composition.
0 parts by weight and 30 to 150 parts by weight of AlN powder are mixed, calcined, and pulverized to form a powder having a particle diameter of 100 μm or less. In the method of manufacturing the AlN sintered body for a bonding agent is a YAG powder or YAG composition Y ₂ O ₃ and Al ₂
100 parts by weight of a mixed powder of O ₃ and 30 to 150 AlN powders
The mixture is dried, granulated, and calcined at a temperature of 1500 to 1850 ° C. in a nitrogen gas atmosphere, and then pulverized to a particle diameter of 100 μm or less. Further, in the method of joining the AlN sintered body, an organic solvent is added to the above-mentioned bonding agent for the AlN sintered body to form a paste, which is applied to the joint of the AlN sintered body or formed into a sheet. And a heat treatment at a temperature exceeding 1850 ° C. in a nitrogen gas atmosphere.

[0005] As a bonding agent for AlN sintered bodies, YAG
(Y ₃ Al ₅ O ₁₂₎ a powder or YAG composition Y ₂ O ₃
If the AlN powder is less than 30 parts by weight with respect to 100 parts by weight of the mixed powder of AlN ₂ and Al ₂ O _3, the volume shrinkage due to sintering exceeds 10%, and a gap is formed in the joint, and It is difficult to control the dimensions of the joined body (control of the thickness dimension of the bonding agent after sintering). On the other hand, if it exceeds 150 parts by weight, the porosity of the bonding agent after sintering exceeds 5%, and open pores are generated, resulting in poor airtightness and insufficient bonding strength.
A more preferable addition amount of the AlN powder is YAG powder or YAG powder.
Mixed powder 100 of Y ₂ O ₃ and Al ₂ O _{3 having} AG composition
It is 80 to 100 parts by weight based on parts by weight. Further, it is important that YAG powder or a mixed powder of Y ₂ O ₃ and Al ₂ O _{3 having} a YAG composition and AlN powder are sequentially mixed, calcined, and pulverized. To control the amount of shrinkage, the calcination treatment is indispensable. Further, when the particle size of the powder exceeds 100 μm, the airtightness of the bonding agent portion is reduced, the bonding strength is reduced, and the coating property is deteriorated. A more preferred particle size is 10 μm or less.
According to the bonding agent for AlN sintered body, the volume shrinkage at the time of sintering is 10% or less, and the porosity of the bonding agent portion after sintering is 5%.
Or less, and the bonding strength is 50 MPa or more. On the other hand, YA
The particle diameter of the G powder or the mixed powder of Y ₂ O ₃ and Al ₂ O _{3 having} a YAG composition is preferably 50 μm or less in average particle diameter. If the average particle size exceeds 50 μm, slurry preparation becomes difficult. A more preferred average particle size is 1 μm. The particle diameter of the AlN powder is 10 μm in average particle diameter.
The following is preferred. When the average particle size exceeds 10 μm, it is similarly difficult to prepare a slurry. A more preferred average particle size is 1 μm.

In the production of a bonding agent for an AlN sintered body, if the calcination temperature is less than 1500 ° C., the volume shrinkage is 10%.
If the temperature exceeds 1850 ° C., the temperature becomes equal to the heat treatment temperature at the time of joining, and substantially no heat diffusion occurs at the time of joining. Therefore, the joining strength becomes less than 50 MPa, and the product cannot withstand practical use. Preferred calcination temperatures are 1800 to 1850
° C.

[0007] In joining AlN sintered bodies using the bonding agent for AlN sintered bodies, butyl carbitol, thermoplastic cellulose ether, dibutyl phthalate and the like are used as organic solvents to be added to the bonding agent. Regarding the bonding heat treatment condition, if the heat treatment temperature is 1850 ° C. or lower, since the temperature is lower than the base material sintering temperature, material diffusion during bonding cannot be performed, and the bonding strength becomes less than 50 MPa.

[0008]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below with reference to specific examples and comparative examples. Examples 1 to 4 and Comparative Examples 1 to 8 First, 100 parts by weight of YAG powder (manufactured by Kojundo Chemical Co., Ltd., yttrium aluminate, average particle size: 50 μm) was mixed with 100 parts by weight of AlN.
Powder (manufactured by Mitsui Toatsu Chemical, product name MAN-2, average particle size 1μ)
m) or a mixed powder obtained by mixing Y ₂ O ₃ and Al ₂ O ₃ (alumina) at a weight ratio of the YAG composition (in Table 1, YO +
Notated as AO. ) Were added at the ratios shown in Table 1, and a mixer (4 liter malon resin pot, 5 mm diameter Al)
Mix using an N ball (250 g) and add a solvent (methanol first grade) to this (500 g of AlN raw material).
, And mixed on a rotary table at 130 rpm for 15 hours to prepare a slurry. Next, each slurry was granulated using a drying device (evaporator (heat-drying device under reduced pressure)), and then sieved to obtain a particle size of 100 μm.
m or less was obtained. Next, each granulated powder (Comparative Example 1,
4 and 8) were placed in a sagger with a lid made of AlN and calcined in an atmosphere of nitrogen gas at atmospheric pressure. The maximum temperature during calcination is lower than the bonding temperature described below, and the heating conditions when the bonding temperature is 1900 ° C. are as follows. Room temperature to 1100 ° C .: 550 ° C./h 1100 to 1500 ° C .: 400 ° C./h 1500 to 1850 ° C .: 200 ° C. 1850 ° C. × 3 h 1850 to 1500 ° C .: 100 ° C./h Next, each calcined body is crushed (AlN The mixture was pulverized using a mortar and an AlN pestle, and then sieved to obtain a powdery binder having a particle size of 50 μm or less.

[0009]

[Table 1]

An organic solvent (solvent 1: butyl carbitol, solvent 2: thermoplastic cellulose ether,
Solvent 3: dibutyl phthalate) was added (solvent 1: 100 g, solvent 1: 45.5 cc, solvent 2: 4.5 cc, solvent 3: 4.0 cc were added), and a mixer (AlN mortar,
(AlN pestle) to obtain a paste. Next, each paste-like bonding agent is applied to an AlN sintered body plate as a body to be bonded by a screen printing machine (the thickness of the bonding agent is set by the number of times of printing), and the two AlN sintered body plates are stacked. After being combined, each of the laminates was heated (elevated temperature 100 ° C./h, maximum temperature 600 ° C. × 1 h) and degreased in an atmosphere of nitrogen gas at atmospheric pressure. Next, heat treatment was performed in the same atmosphere as the degreasing treatment, and the bonding agent was fired to bond the respective laminates. The heating conditions for the heat treatment are as follows. Room temperature to 1100 ° C .: 550 ° C./h 1100 to 1500 ° C .: 400 ° C./h 1500 to 1900 ° C .: 200 ° C./h 1900 ° C. × 3 h 1900 to 1500 ° C .: 100 ° C./h Table 2 shows the volume shrinkage, porosity, bonding strength and the like.

[0011]

[Table 2]

According to Tables 1 and 2, a powder containing 30 to 150 parts by weight of AlN per 100 parts by weight of YAG is mixed, calcined, and pulverized to obtain a powder having a particle diameter of 100 μm or less. Since the porosity is 10% or less, the porosity is 5% or less, and the joining strength is 100 to 200 MPa, it can be seen that the joining of the AlN sintered bodies can be performed well.

In the above-described embodiment, A
In the case of bonding 1N sintered bodies, a case in which a paste-like bonding agent is applied to a bonding portion has been described. However, the present invention is not limited to this. For example, a paste-like bonding agent is formed into a sheet, and It may be interposed between the joints of the AlN sintered body, and the same operation and effect can be obtained.

[0014]

As described above, according to the bonding agent for an AlN sintered body of the present invention, the method of manufacturing the same, and the method of bonding an AlN sintered body using the same, the bonding agent is previously contracted in volume. Therefore, the airtightness and the joint strength of the joint can be greatly increased without generating a gap in the joint of the AlN sintered body.

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[Procedure amendment]

[Submission date] November 21, 1997

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] Claims

[Correction method] Change

[Correction contents]

[Claims]

[Procedure amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0004

[Correction method] Change

[Correction contents]

[0004]

Means for Solving the Problems] To solve the above problems, A1N sintered body for bonding agent of the present invention, YAG Powder 1 0
0 parts by weight and 30 to 150 parts by weight of A1N powder are mixed, calcined, and pulverized to form a powder having a particle diameter of 100 μm or less. The manufacturing method of A1N sintered body for bonding agents, YAG Powder 1 00 parts by weight and the A1N powder 30-150
The mixture is dried, granulated, and calcined at a temperature of 1500 to 1850 ° C. in a nitrogen gas atmosphere, and then pulverized to a particle diameter of 100 μm or less. Further, the joining method of the A1N sintered body is as follows. An organic solvent is added to the joining agent for the A1N sintered body to form a paste, which is applied to the joint of the A1N sintered body or formed into a sheet. And a heat treatment at a temperature exceeding 1850 ° C. in a nitrogen gas atmosphere.

[Procedure amendment 3]

[Document name to be amended] Statement

[Correction target item name] 0005

[Correction method] Change

[Correction contents]

[0005] In the bonding agent for A1N sintered body, YAG
To _(Y 3 _Al 5 _{O 12)} powder powder 1 00 parts by weight, A1N
When the amount of the powder is less than 30 parts by weight, the volume shrinkage due to sintering exceeds 10%, a gap is formed in the joint, and A1N
It is difficult to control the dimensions of the joined body of the sintered bodies (control of the thickness of the bonding agent after sintering). On the other hand, if it exceeds 150 parts by weight,
The porosity of the bonding material after sintering exceeds 5%, and open pores are generated, resulting in poor airtightness and insufficient bonding strength. More preferred amount of A1N powder, YAG Powder 1
It is 80 to 100 parts by weight with respect to 00 parts by weight. Also, YA
It is important is obtained by successively mixing, calcining and pulverizing the G Powder and A1N powder, in particular, in controlling the sintering shrinkage of the bonding agent, calcination process is indispensable. Furthermore,
When the particle diameter of the powder exceeds 100 μm, the airtightness of the bonding agent portion is reduced, the bonding strength is reduced, and the coating property is deteriorated. A more preferred particle size is 10 μm or less. According to the bonding agent for A1N sintered body, the volume shrinkage at the time of sintering is 10% or less, the porosity of the bonding agent portion after sintering is 5% or less, and the bonding strength is 50 MPa or more. on the other hand,
Particle size of YAG Powder is preferably an average particle diameter is 50μm or less. If the average particle size exceeds 50 μm, slurry preparation becomes difficult. A more preferred average particle size is 1 μm.
m. The particle size of the A1N powder is 10
It is preferably not more than μm. When the average particle size exceeds 10 μm, it is similarly difficult to prepare a slurry. A more preferred average particle size is 1 μm.

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0008

[Correction method] Change

[Correction contents]

[0008]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below with reference to specific examples and comparative examples. Examples 1 to 4 and Comparative Examples 1 to 8 First, 100 parts by weight of YAG powder (manufactured by Kojundo Chemical Co., Ltd., yttrium aluminate, average particle size: 50 μm) was mixed with 100 parts by weight of A1N.
Powder (manufactured by Mitsui Toatsu Chemicals, flat Hitoshitsubu径1 [mu] m) or _Y 2 _{O 3}
And Al ₂ O ₃ were mixed at a weight ratio of the YAG composition ( Comparative Example 8, described as YO + AO in Table 1) in the proportions shown in Table 1, respectively, and a mixer (4 liter malon resin pot, Mixing was performed using 250 g of A1N balls having a diameter of 5 mm, and a solvent (methanol first grade) was added thereto (450 cc for 500 g of A1N raw material).
) And mixed on a rotating table at 130 rpm for 15 hours to prepare a slurry. Next, each slurry was granulated by using a drying device (evaporator (heat-drying device under reduced pressure)), and then sieved to obtain granulated powder having a particle size of 100 μm or less. Next, each granulated powder (except for Comparative Examples 1, 4, and 8) was A
Each was housed in a 1N lid sagger and calcined in an atmosphere of nitrogen gas at atmospheric pressure. The maximum temperature during calcination is lower than the bonding temperature described below, and the heating conditions when the bonding temperature is 1900 ° C. are as follows. Room temperature to 1100 ° C .: 550 ° C./h 1100 to 1500 ° C .: 400 ° C./h 1500 to 1850 ° C .: 200 ° C. 1850 ° C. × 3 h 1850 to 1500 ° C .: 100 ° C./h Next, each calcined body is crushed (A1N). After crushing using a mortar and an A1N pestle), the mixture was sieved to obtain a powdery binder having a particle size of 50 μm or less.

Continued on the front page (72) Inventor Mitsuhiro Fujita 30 Soya, Hadano-shi, Kanagawa Prefecture Toshiba Ceramics Co., Ltd.

Claims (3)

[Claims] 1. YAG powder or Y ₂ O having a YAG composition
100 parts by weight of mixed powder of Al ₃ and Al ₂ O ₃ and AlN powder 3
0 to 150 parts by weight of mixed, calcined and pulverized particle diameter 10
A bonding agent for an AlN sintered body, comprising a powder having a particle size of 0 μm or less. 2. Y ₂ O to be YAG powder or YAG composition
100 parts by weight of mixed powder of Al ₃ and Al ₂ O ₃ and AlN powder 3
A solvent is added to 0 to 150 parts by weight, mixed, dried and granulated, calcined in a nitrogen gas atmosphere at a temperature of 1500 to 1850 ° C., and then pulverized to a particle diameter of 100 μm or less. A method for producing a bonding agent for binding. 3. An AlN additive is added to the bonding agent according to claim 1 to form a paste, which is applied to a bonding portion of the AlN sintered body or formed into a sheet to bond the AlN sintered body. A method for joining AlN sintered bodies, wherein a heat treatment is performed in a nitrogen gas atmosphere at a temperature exceeding 1850 ° C.