Bonding agent for bonding aluminum nitride ceramics and bonding method

Abstract

The invention discloses a bonding agent for bonding aluminum nitride ceramics and a bonding method, and belongs to the technical field of electrostatic chucks, and the bonding agent comprises the following components in parts by weight: 1.5-5.5 wt% of B2O3, 40-55 wt% of CaO, 40-55 wt% of AI2O3, an organic solvent, a dispersant and a binder. The bonding method comprises the steps that a first aluminum nitride sintered body and a second aluminum nitride sintered body which are bonded are prepared, the bonding face of the first aluminum nitride sintered body and the bonding face of the second aluminum nitride sintered body need to be machined firstly, alcohol serves as a cleaning agent, and ultrasonic cleaning is conducted for 30 min or above; the preparation method comprises the following steps: respectively weighing B2O3, CaO and AI2O3 according to a ratio, putting the weighed B2O3, CaO and AI2O3 together with an organic solvent, a dispersant and a binder into a ball milling tank, and carrying out ball milling for 4-6 hours to form a binding agent; the bonding agent is uniformly coated on the bonding surface of the first aluminum nitride sintered body and the second aluminum nitride sintered body, the thickness of the bonding agent is 90-110 [mu] m, bonding is carried out, the load of 10 kg / cm < 2 > is applied, nitrogen is filled at the temperature of 1200 DEG C for atmosphere protection, the bonding temperature is 1400-1800 DEG C, and the bonding time is 20-50 min.

Description

Technical Field

[0001] The present invention relates to the technical field of electrostatic chucks, and in particular to a bonding agent and a bonding method for bonding aluminum nitride ceramics. Background Art

[0002] There are generally two methods for joining aluminum nitride sintered bodies: solid phase joining and solid-liquid joining. Solid phase joining is a method of adding a bonding agent between aluminum nitride sintered bodies and joining them in a solid phase without melting the bonding agent. In order to obtain a good bonding state, a certain pressure needs to be applied and the bonding temperature is generally 1850°C or higher. However, due to the high temperature bonding, there is a risk of deformation of the product, and even deterioration of its electrical properties, especially resistivity, which has a very adverse effect on the product.

[0003] Solid-liquid bonding is a method of melting part of the bonding agent at a certain high temperature and performing bonding in a state of mixed solid and liquid phases. This bonding agent is generally a material containing 25-45wt% CaO, 5-30wt% Y2O3 and the remainder Al2O3. The bonding temperature is generally between 1650 and 1800°C, but there is still a risk of deformation at this bonding temperature. Summary of the invention

[0004] The technical problem to be solved by the present invention is to provide a bonding agent and a bonding method for bonding aluminum nitride ceramics, so as to solve the problem raised in the background technology and reduce the bonding temperature.

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

[0006] On one hand, the present invention discloses a bonding agent for bonding aluminum nitride ceramics, wherein the bonding agent comprises, by weight: 1.5-5.5wt% B2O3, 40-55wt% CaO, 40-55wt% AI2O3, and an organic solvent, a dispersant and a binder.

[0007] Preferably, the binder comprises, calculated by weight: 2-5wt% B2O3, 43-54wt% CaO, and 41-52wt% AI2O3.

[0008] Preferably, the organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate.

[0009] Preferably, the dispersant is lecithin.

[0010] Preferably, the binder is ethyl cellulose or acrylic resin.

[0011] Another aspect of the present invention discloses a bonding method for bonding an aluminum nitride ceramic bonding agent, the bonding method comprising:

[0012] Prepare in advance the first aluminum nitride sintered body and the second aluminum nitride sintered body to be joined. The joining surfaces of the first aluminum nitride sintered body and the second aluminum nitride sintered body need to be processed first. After the joining surfaces are processed to be qualified, use alcohol as a cleaning agent and put them into ultrasonic cleaning for more than 30 minutes;

[0013] B2O3, CaO, and AI2O3 are weighed in proportion, and put into a ball mill together with an organic solvent, a dispersant, and a binder for 4 to 6 hours to form a bonding agent;

[0014] The ball-milled bonding agent is evenly coated on the bonding surface of the first aluminum nitride sintered body and the second aluminum nitride sintered body with a thickness of 90 to 110 μm, and then placed in a furnace for bonding. 2 The load is removed, and nitrogen is filled into the atmosphere for protection at 1200℃. The joining temperature is 1400~1800℃, and the joining time is 20~50min.

[0015] After joining, the samples were taken out and each sample was tested for helium leak using a helium leak detector.

[0016] Preferably, the bonding surfaces of the first aluminum nitride sintered body and the second aluminum nitride sintered body require: a flatness of less than or equal to 5 μm, and a roughness of 0.3 to 1 μm.

[0017] The above technical solution has the following beneficial effects:

[0018] By adopting the technical solution of the present application, the aluminum nitride bonding temperature is effectively reduced to below 1500°C, and the bonding effect is good, and the helium leakage is within 5×10 -9 mbar·L / s or less. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic structural diagram of an embodiment of the present invention. DETAILED DESCRIPTION

[0020] The specific embodiments of the present invention are further described below in conjunction with the accompanying drawings. 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 the various embodiments 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 bonding agent for bonding aluminum nitride ceramics, used in the field of electrostatic chucks, to bond aluminum nitride ceramic disks, the bonding agent comprises, by weight: 1.5-5.5wt% B2O3, 40-55wt% CaO, 40-55wt% AI2O3, the above materials are mixed with an organic solvent, a dispersant, and a binder to prepare the bonding agent, wherein the organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate, the dispersant is lecithin, and the binder is ethyl cellulose or acrylic resin;

[0023] Example 2

[0024] A bonding agent for bonding aluminum nitride ceramics is used in the field of electrostatic chucks to bond aluminum nitride ceramic disks. The bonding agent comprises, by weight, 1.5 wt% of B2O3, 40 wt% of CaO, and 40 wt% of AI2O3. The bonding agent is prepared by mixing the above materials with an organic solvent, a dispersant, and a binder. The organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate, the dispersant is lecithin, and the binder is ethyl cellulose or acrylic resin.

[0025] Example 3

[0026] A bonding agent for bonding aluminum nitride ceramics is used in the field of electrostatic chucks to bond aluminum nitride ceramic disks. The bonding agent includes, by weight, 5.5 wt% B2O3, 55 wt% CaO, and 55 wt% AI2O3. The bonding agent is prepared by mixing the above materials with an organic solvent, a dispersant, and a binder. The organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate, the dispersant is lecithin, and the binder is ethyl cellulose or acrylic resin.

[0027] Example 4

[0028] A bonding agent for bonding aluminum nitride ceramics. The bonding agent comprises, by weight, 2-5wt% B2O3, 43-54wt% CaO, and 41-52wt% AI2O3. The bonding agent is prepared by mixing the above materials with an organic solvent, a dispersant, and a binder. The organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate, the dispersant is lecithin, and the binder is ethyl cellulose or acrylic resin.

[0029] Example 5

[0030] refer to Figure 1 , a bonding method for bonding an aluminum nitride ceramic bonding agent, the bonding method comprising:

[0031] Prepare the first aluminum nitride sintered body 1 and the second aluminum nitride sintered body 2 to be joined in advance. The joining surfaces of the first aluminum nitride sintered body 1 and the second aluminum nitride sintered body 2 need to be processed first. After the joining surfaces are processed to be qualified, use alcohol as a cleaning agent and put them into ultrasonic cleaning for more than 30 minutes. The joining surfaces of the first aluminum nitride sintered body 1 and the second aluminum nitride sintered body 2 require: the flatness is less than or equal to 5μm, and the roughness is 0.3-1μm; the first aluminum nitride sintered body 1 can be a disc-shaped structure similar to an electrostatic chuck, and the second aluminum nitride sintered body 2 can be an axis structure;

[0032] B2O3, CaO, and AI2O3 are weighed in proportion, and put into a ball mill together with an organic solvent, a dispersant, and a binder for 4 to 6 hours to form a bonding agent;

[0033] The ball-milled bonding agent is evenly applied to the bonding surface of the first aluminum nitride sintered body 1 and the second aluminum nitride sintered body 2 to form a bonding layer 3 with a thickness of 90 to 110 μm. The bonding is carried out in a furnace and a 10 kg / cm 2 The load is removed, and nitrogen is filled into the atmosphere for protection at 1200℃. The joining temperature is 1400~1800℃, and the joining time is 20~50min.

[0034] After joining, the samples were taken out and each sample was tested for helium leak using a helium leak detector.

[0035] By adopting the technical solution of the present application, the bonding temperature of aluminum nitride ceramics is effectively reduced to below 1500°C, and the bonding effect is good, and the helium leakage is within 5×10 -9 mbar·L / s or less.

[0036] Example 6

[0037] A bonding agent for bonding aluminum nitride ceramics, the bonding agent includes, by weight, 2wt% B2O3, 53.9wt% CaO, and 44.1wt% AI2O3. The bonding agent is prepared by mixing the above materials with an organic solvent, a dispersant, and a binder. The organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate, the dispersant is lecithin, and the binder is ethyl cellulose or acrylic resin. Under the conditions of this embodiment, the bonding temperature requirement is 1400°C, and the helium leakage tested after bonding is within 5×10 -9 mbar·L / s or less.

[0038] Example 7

[0039] A bonding agent for bonding aluminum nitride ceramics, the bonding agent includes, by weight, 4.9wt% B2O3, 52.3wt% CaO, and 41.7wt% AI2O3. The bonding agent is prepared by mixing the above materials with an organic solvent, a dispersant, and a binder. The organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate, the dispersant is lecithin, and the binder is ethyl cellulose or acrylic resin. Under the conditions of this embodiment, the bonding temperature requirement is 1400°C, and the helium leakage tested after bonding is less than 1×10 -8 mbar·L / s or less.

[0040] Comparative Example 1

[0041] A bonding agent for bonding aluminum nitride ceramics, the bonding agent includes, by weight, 55wt% of CaO and 45wt% of AI2O3, the above materials are mixed with an organic solvent, a dispersant, and a binder to prepare the bonding agent, wherein the organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate, the dispersant is lecithin, and the binder is ethyl cellulose or acrylic resin. Under the conditions of this embodiment, the bonding temperature requirement is 1550°C, and the helium leakage tested after bonding is within 1×10 -8 mbar·L / s or less.

[0042] Comparative Example 2

[0043] A bonding agent for bonding aluminum nitride ceramics, the bonding agent includes, by weight, 43wt% of CaO, 52wt% of AI2O3, and 5wt% of Y2O3, the above materials are mixed with an organic solvent, a dispersant, and a binder to prepare the bonding agent, wherein the organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate, the dispersant is lecithin, and the binder is ethyl cellulose or acrylic resin. Under the conditions of this embodiment, the bonding temperature requirement is 1800°C, and the helium leakage tested after bonding is within 5×10 -9 mbar·L / s or less.

[0044] Table 1:

[0045]

[0046] As shown in Table 1, 2 wt% B2O3 was added to the bonding agent in Example 6, and 4.9 wt% B2O3 was added to the bonding agent in Example 7. The bonding temperature requirement of the bonding agents prepared in the two examples was 1400°C, which was lower than that of Comparative Examples 1 and 2 without adding B2O3.

[0047] The embodiments of the present invention are described in detail above with reference to the accompanying drawings, 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 scope of protection of the present invention.

Claims

1. A bonding agent for bonding aluminum nitride ceramics, characterized in that: The bonding agent comprises, by weight: 1.5-5.5wt% B2O3, 40-55wt% CaO, 40-55wt% AI2O3, an organic solvent, a dispersant and a binder.

2. A bonding agent and bonding method for bonding aluminum nitride ceramics according to claim 1, characterized in that: The bonding agent comprises, by weight: 2-5 wt% B2O3, 43-54 wt% CaO, and 41-52 wt% Al2O3.

3. The bonding agent for bonding aluminum nitride ceramics according to claim 1, characterized in that: The organic solvent is diethylene glycol monobutyl ether or diethylene glycol butyl ether acetate.

4. The bonding agent for bonding aluminum nitride ceramics according to claim 1, characterized in that: The dispersant is lecithin.

5. The bonding agent for bonding aluminum nitride ceramics according to claim 1, characterized in that: The binder is ethyl cellulose or acrylic resin.

6. A method for bonding a bonding agent for bonding aluminum nitride ceramics according to any one of claims 1 to 5, characterized in that: The joining method comprises: Prepare in advance the first aluminum nitride sintered body and the second aluminum nitride sintered body to be joined. The joining surfaces of the first aluminum nitride sintered body and the second aluminum nitride sintered body need to be processed first. After the joining surfaces are processed to be qualified, use alcohol as a cleaning agent and put them into ultrasonic cleaning for more than 30 minutes; B2O3, CaO, and AI2O3 are weighed in proportion, and put into a ball mill together with an organic solvent, a dispersant, and a binder for 4 to 6 hours to form a bonding agent; The ball-milled bonding agent is evenly coated on the bonding surface of the first aluminum nitride sintered body and the second aluminum nitride sintered body with a thickness of 90 to 110 μm, and then placed in a furnace for bonding. 2 The load is removed, and nitrogen is filled into the atmosphere for protection at 1200℃. The joining temperature is 1400~1800℃, and the joining time is 20~50min. After joining, the samples were taken out and each sample was tested for helium leak using a helium leak detector.

7. A bonding method for bonding an aluminum nitride ceramic bonding agent according to claim 6, characterized in that: The bonding surfaces of the first aluminum nitride sintered body and the second aluminum nitride sintered body require a flatness of less than or equal to 5 μm and a roughness of 0.3 to 1 μm.

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