Hole filling slurry for aluminum nitride electrostatic chuck and preparation method thereof

Abstract

The invention discloses pore-filling slurry for an aluminum nitride electrostatic chuck and a preparation method of the pore-filling slurry, and belongs to the technical field of electrostatic chucks, the pore-filling slurry comprises powder and an organic phase, the powder comprises carbide and inorganic matter, the carbide is WC or Mo2C or a mixture of the carbide and the inorganic matter, and the organic phase is a mixture of the carbide and the inorganic matter. The carbide comprises powder in different particle size ranges according to the following mass ratios: 1-15% of WC carbide powder or Mo2C carbide powder or a mixture of the WC carbide powder and the Mo2C carbide powder, and the particle size of the WC carbide powder and the Mo2C carbide powder is 0.1-1 [mu] m; wC carbide powder or Mo2C carbide powder or a mixture of the WC carbide powder and the Mo2C carbide powder accounts for 70-90% by mass, and the particle size of the WC carbide powder or the Mo2C carbide powder is 1-3 microns; the particle size of the WC carbide powder or the Mo2C carbide powder or the mixture of the WC carbide powder and the Mo2C carbide powder is 3-5 microns; the inorganic matter is any one or a mixture of two or more than two of Y2O3, MgO and CaO. The pore-filling slurry can avoid the phenomenon that the resistance is unstable due to metal carbonization caused by residual C existing during sintering of the aluminum nitride electrostatic chuck.

Description

Technical Field

[0001] The invention relates to the technical field of electrostatic chucks, and in particular to a hole-filling slurry for an aluminum nitride electrostatic chuck and a preparation method thereof. Background Art

[0002] At present, the hole filling process used for aluminum nitride electrostatic chucks is mainly based on HTCC high-temperature co-firing. The purpose of the hole filling is to make electrode columns. The electronic slurries used are mostly W slurry and Mo / Mn slurry. However, the hole filling of electrostatic chucks is more particular than that of conventional HTCC products: the size of the filled holes is larger in both horizontal and thickness directions, that is, more slurry is required to be filled.

[0003] As mentioned above, the electrostatic chuck has certain defects after sintering due to its special hole filling properties: W, Mo, and Mn are easy to react with the atmosphere or residual C in the product during high-temperature sintering to generate WC and Mo. 2 C. Mn 2 C, resulting in changes in the resistance of the electrode column made by filling the hole, and the resistance value will vary with the degree of carbonization, and its stability cannot be controlled. Summary of the invention

[0004] The technical problem to be solved by the present invention is to provide a hole-filling slurry for an aluminum nitride electrostatic chuck and a preparation method thereof, so as to solve the problem in the prior art that the resistance of the hole-filling slurry of the aluminum nitride electrostatic chuck changes and is unstable after sintering.

[0005] In order to solve the above technical problems, the technical solution of the present invention is:

[0006] The present invention discloses a hole-filling slurry for an aluminum nitride electrostatic chuck. The hole-filling slurry comprises a powder and an organic phase. The powder comprises a carbide and an inorganic substance. The carbide is WC or Mo. 2 C or a mixture of the two, wherein the carbide comprises powders within different particle size ranges in the following mass ratio:

[0007] WC carbide powder or Mo with a mass percentage of 1% to 15% 2 C carbide powder or a mixture of the two, with a particle size of 0.1 to 1 μm;

[0008] WC carbide powder or Mo with a mass percentage of 70% to 90% 2 C carbide powder or a mixture of the two, with a particle size of 1 to 3 μm;

[0009] WC carbide powder or Mo with a mass percentage of 1% to 15% 2 C carbide powder or a mixture of the two, with a particle size of 3 to 5 μm;

[0010] The inorganic substance is Y2 O 3 , MgO, CaO or a mixture of two or more.

[0011] Preferably, the organic phase comprises the following mass ratio:

[0012] Binder: The binder is any one of ethyl cellulose, acrylic resin, PVB, or a mixture of any two or more thereof, accounting for 10% to 50% by weight;

[0013] Solvent: The solvent is any one of terpineol, butyl carbitol, butyl carbitol acetate, dibutyl phthalate, and alcohol ester twelve, and the mass proportion thereof is 30% to 60%;

[0014] Dispersant: The dispersant is lecithin or castor oil, and its mass proportion is 5% to 20%.

[0015] Preferably, the mass fractions of the components in the pore-filling slurry are: 70 to 95 parts of carbide, 0.1 to 10 parts of inorganic matter, and 5 to 30 parts of organic phase.

[0016] Another aspect of the present invention discloses a method for preparing a hole-filling slurry for an aluminum nitride electrostatic chuck, the method for preparing the hole-filling slurry comprising:

[0017] In a planetary ball mill, carbide, inorganic matter and organic phase are added according to the proportion, and ball milling is performed for more than 1 hour using a ball mill with a diameter of 3 to 5 mm at a rotation speed greater than or equal to 300 rpm to produce a slurry, which is then rolled 3 to 6 times using a three-roll rolling machine with a roller gap of 10 to 50 μm until the fineness reaches less than 5 μm, thereby producing the pore-filling slurry.

[0018] The above technical solution has the following beneficial effects:

[0019] Using carbide to make the hole-filling slurry for aluminum nitride electrostatic chuck can avoid the metal carburization and unstable resistance caused by the residual C present during the sintering of the aluminum nitride electrostatic chuck. In addition, the thermal expansion coefficients of carbide ceramics and aluminum nitride materials are closer, and the bonding with the hole wall is better after hole-filling sintering. DETAILED DESCRIPTION

[0020] The specific embodiments of the present invention are further described below. It should be noted that the description of these embodiments is used to help understand the present invention, but does not constitute a limitation of the present invention. In addition, the technical features involved in each embodiment of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0021] Example 1

[0022] A hole-filling slurry for an aluminum nitride electrostatic chuck, the hole-filling slurry comprising a powder and an organic phase, the powder comprising a carbide and an inorganic substance, the carbide being WC or Mo 2 C or a mixture of the two, carbides including powders within different particle sizes in the following mass ratios:

[0023] WC carbide powder or Mo with a mass percentage of 1% to 15% 2 C carbide powder, or WC carbide powder and Mo 2 C carbide powder mixture, if the two are mixed, the two can be determined according to the needs or existing conditions, such as WC carbide powder and Mo 2 The amount of WC carbide powder is equal to that of Mo. 2 The particle size of C carbide powder is between 0.1 and 1 μm, and the total mass proportion is between 1% and 15%;

[0024] WC carbide powder or Mo with a mass percentage of 70% to 90% 2 C carbide powder, or WC carbide powder and Mo 2 C carbide powder mixture, if the two are mixed, the two can be determined according to the needs or existing conditions, such as WC carbide powder and Mo 2 The amount of WC carbide powder is equal to that of Mo. 2 The particle size of C carbide powder is between 1 and 3 μm, and the total mass proportion is between 70% and 90%;

[0025] WC carbide powder or Mo with a mass percentage of 1% to 15% 2 C carbide powder, or WC carbide powder and Mo 2 C carbide powder mixture, if the two are mixed, the two can be determined according to the needs or existing conditions, such as WC carbide powder and Mo 2 The amount of WC carbide powder is equal to that of Mo. 2 The particle size of C carbide powder is between 3 and 5 μm, and the total mass proportion is between 1% and 15%;

[0026] By mixing the carbide powders of different particle sizes, the pore-filling slurry is filled more densely. The powder size is mainly 1-3 μm. In addition, powders with a particle size of 0.1-1 μm and powders with a particle size of 3-5 μm are used to fill the gaps, so that the slurry is filled more densely.

[0027] Inorganic matter is Y 2 O 3, MgO, CaO, any one or a mixture of two or more;

[0028] Wherein, the organic phase comprises according to the following mass ratio:

[0029] Binder: The binder is any one of ethyl cellulose, acrylic resin, PVB, or a mixture of any two or more thereof, and its mass accounts for 10% to 50%;

[0030] Solvent: The solvent is any one of terpineol, butyl carbitol, butyl carbitol acetate, dibutyl phthalate, and alcohol ester twelve, and the mass proportion thereof is 30% to 60%;

[0031] Dispersant: The dispersant is lecithin or castor oil, and its mass proportion is 5% to 20%;

[0032] The mass fractions of the components in the hole filling slurry are: 70-95 parts of carbide, 0.1-10 parts of inorganic matter, and 5-30 parts of organic phase. The mixture of the above mass fractions is used to prepare the slurry;

[0033] In the prior art, the hole filling process used for aluminum nitride electrostatic chucks is mainly based on HTCC high temperature co-firing. The purpose of the hole filling is to make electrode columns. The electronic slurries used are mostly W slurry and Mo / Mn slurry. The aluminum nitride electrostatic chuck ceramic discs are mostly hot pressed and sintered. There is a large amount of residual carbon (C) in the ceramic disc after debinding. During the hot pressing and sintering process, the residual carbon (C) will react with metals such as W, Mo, and Mn to generate their carbides. The present application replaces the metal that is easy to react with carbon with carbides, which can solve the above problems;

[0034] The present application utilizes carbide to prepare the hole-filling slurry of aluminum nitride electrostatic chuck, which can avoid the unstable resistance phenomenon caused by metal carbonization due to residual C existing during the sintering of the aluminum nitride electrostatic chuck, and the thermal expansion coefficient of carbide ceramics is closer to that of aluminum nitride materials, and the bonding with the hole wall is better after the hole-filling sintering, so as to solve the problem of variable and unstable resistance value of the hole-filling slurry of aluminum nitride electrostatic chuck after sintering in the prior art.

[0035] Example 2

[0036] A hole-filling slurry for an aluminum nitride electrostatic chuck, the hole-filling slurry comprising a powder and an organic phase, the powder comprising a carbide and an inorganic substance, the carbide being WC or Mo 2 C or a mixture of the two, carbides including powders within different particle sizes in the following mass ratios:

[0037] WC carbide powder or Mo with a mass percentage of 1% 2 C carbide powder, the particle size is 0.1μm;

[0038] WC carbide powder or Mo with a mass percentage of 70% 2 C carbide powder, the particle size is 1μm;

[0039] WC carbide powder or Mo with a mass percentage of 1% 2 C carbide powder, the particle size is 3μm;

[0040] By mixing the carbide powders of different particle sizes, the pore-filling slurry can be filled more densely;

[0041] Inorganic matter is Y 2 O 3 , MgO, CaO.

[0042] Wherein, the organic phase comprises according to the following mass ratio:

[0043] Binder: The binder is any one of ethyl cellulose, acrylic resin, PVB, or a mixture of any two or more thereof, accounting for 10% by weight;

[0044] Solvent: The solvent is any one of pineol, butyl carbitol, butyl carbitol acetate, dibutyl phthalate, and alcohol ester twelve, and the mass proportion thereof is 30%;

[0045] Dispersant: The dispersant is lecithin or castor oil, accounting for 5% by mass;

[0046] The mass fractions of each component in the hole filling slurry are: 70 parts of carbide, 0.1 parts of inorganic matter, and 5 parts of organic phase;

[0047] The present application utilizes carbide to prepare the hole-filling slurry of aluminum nitride electrostatic chuck, which can avoid the unstable resistance phenomenon caused by metal carbonization due to residual C existing during the sintering of the aluminum nitride electrostatic chuck, and the thermal expansion coefficient of carbide ceramics is closer to that of aluminum nitride materials, and the bonding with the hole wall is better after the hole-filling sintering, so as to solve the problem of variable and unstable resistance value of the hole-filling slurry of aluminum nitride electrostatic chuck after sintering in the prior art.

[0048] Example 3

[0049] A hole-filling slurry for an aluminum nitride electrostatic chuck, the hole-filling slurry comprising a powder and an organic phase, the powder comprising a carbide and an inorganic substance, the carbide being WC or Mo 2 C or a mixture of the two, carbides including powders within different particle sizes in the following mass ratios:

[0050] WC carbide powder and Mo with a mass percentage of 15% 2 A mixture of C carbide powders, the proportion of each is determined according to needs and actual conditions, and the particle size and total proportion are guaranteed, and the particle size is 1μm;

[0051] WC carbide powder or Mo with a mass percentage of 70% 2 A mixture of C carbide powders, the particle size of which is 3 μm;

[0052] WC carbide powder or Mo with a mass percentage of 15% 2 A mixture of C carbide powders, the particle size of which is 5 μm;

[0053] By mixing the carbide powders of different particle sizes, the pore-filling slurry can be filled more densely;

[0054] Inorganic matter is Y 2 O 3 , MgO, CaO or a mixture of any two or more thereof.

[0055] Wherein, the organic phase comprises according to the following mass ratio:

[0056] Binder: The binder is any one of ethyl cellulose, acrylic resin, PVB, or a mixture of any two or more thereof, accounting for 50% by weight;

[0057] Solvent: The solvent is any one of pineol, butyl carbitol, butyl carbitol acetate, dibutyl phthalate, and alcohol ester twelve, and the mass proportion thereof is 60%;

[0058] Dispersant: The dispersant is lecithin or castor oil, accounting for 20% by weight;

[0059] The mass fractions of each component in the hole filling slurry are: 95 parts of carbide, 10 parts of inorganic matter, and 30 parts of organic phase;

[0060] The present application utilizes carbide to prepare the hole-filling slurry of aluminum nitride electrostatic chuck, which can avoid the unstable resistance phenomenon caused by metal carbonization due to residual C existing during the sintering of the aluminum nitride electrostatic chuck, and the thermal expansion coefficient of carbide ceramics is closer to that of aluminum nitride materials, and the bonding with the hole wall is better after the hole-filling sintering, so as to solve the problem of variable and unstable resistance value of the hole-filling slurry of aluminum nitride electrostatic chuck after sintering in the prior art.

[0061] Example 4

[0062] A method for preparing a hole-filling slurry for an aluminum nitride electrostatic chuck, the method comprising:

[0063] In a planetary ball mill, carbide, inorganic matter and organic phase are added according to the proportion, and ball milling is performed for more than 1 hour at a rotation speed greater than or equal to 300 rpm using a ball mill with a diameter of 3 to 5 mm. Specifically, a ball mill with a diameter of 3 mm or 5 mm can be used. After ball milling, the slurry is produced, and then rolled 3 to 6 times using a three-roll rolling machine at a roller gap of 10 to 50 μm, and the fineness reaches less than 5 μm, thereby preparing a pore-filling slurry.

[0064] The embodiments of the present invention are described in detail above, but the present invention is not limited to the described embodiments. For those skilled in the art, various changes, modifications, substitutions and variations of these embodiments are made without departing from the principles and spirit of the present invention, and still fall within the protection scope of the present invention.

Claims

1. A hole-filling slurry for an aluminum nitride electrostatic chuck, characterized in that: The pore-filling slurry includes a powder and an organic phase, the powder includes a carbide and an inorganic substance, the carbide is WC or Mo2C or a mixture of the two, and the carbide includes powders within different particle size ranges in the following mass ratio: WC carbide powder or Mo2C carbide powder or a mixture of the two with a mass percentage of 1% to 15% and a particle size of 0.1 to 1 μm; WC carbide powder or Mo2C carbide powder or a mixture of the two with a mass percentage of 70% to 90%, and a particle size of 1 to 3 μm; WC carbide powder or Mo2C carbide powder or a mixture of the two with a mass percentage of 1% to 15% and a particle size of 3 to 5 μm; The inorganic substance is any one of Y2O3, MgO, and CaO, or a mixture of two or more thereof.

2. The hole-filling slurry for aluminum nitride electrostatic chuck according to claim 1, characterized in that: The organic phase comprises the following mass ratio: Binder: The binder is any one of ethyl cellulose, acrylic resin, PVB, or a mixture of any two or more thereof, accounting for 10% to 50% by weight; Solvent: The solvent is any one of terpineol, butyl carbitol, butyl carbitol acetate, dibutyl phthalate, and alcohol ester twelve, and the mass proportion thereof is 30% to 60%; Dispersant: The dispersant is lecithin or castor oil, and its mass proportion is 5% to 20%.

3. The hole-filling slurry for aluminum nitride electrostatic chuck according to claim 1, characterized in that: The mass proportions of the components in the pore-filling slurry are: 70 to 95 parts of carbide, 0.1 to 10 parts of inorganic matter, and 5 to 30 parts of organic phase.

4. A method for preparing a hole-filling slurry for an aluminum nitride electrostatic chuck according to any one of claims 1 to 3, characterized in that: The preparation method of the hole-filling slurry comprises: In a planetary ball mill, carbide, inorganic matter and organic phase are added according to the proportion, and ball milling is performed for more than 1 hour using a ball mill with a diameter of 3 to 5 mm at a rotation speed greater than or equal to 300 rpm to produce a slurry, which is then rolled 3 to 6 times using a three-roll rolling machine with a roller gap of 10 to 50 μm until the fineness reaches less than 5 μm, thereby producing the pore-filling slurry.