A high thermal conductivity aluminum nitride ceramic structural component and its preparation method

Abstract

This invention relates to the field of aluminum nitride ceramic technology, and proposes a high thermal conductivity aluminum nitride ceramic structural component and its preparation method. The aluminum nitride ceramic structural component comprises the following raw materials in parts by weight: 100 parts aluminum nitride, 5-10 parts sintering aid, 4-6 parts plasticizer, 5-10 parts binder, 1-1.5 parts dispersant, 2-2.5 parts aluminum dihydroxyaminoacetate, and 70-80 parts solvent. This technical solution solves the problems of low thermal conductivity and low flexural strength in related technologies for aluminum nitride ceramic structural components.

Description

Technical Field

[0001] This invention relates to the field of aluminum nitride ceramic technology, specifically to an aluminum nitride ceramic structural component with high thermal conductivity and its preparation method. Background Technology

[0002] Aluminum nitride ceramic structural components are ceramic structural components with aluminum nitride as the main crystalline phase, and they have important applications in the fields of electronics and information technology, mechanical engineering, chemical engineering, and optics. In the field of electronics and information technology, aluminum nitride ceramic structural components mainly include aluminum nitride ceramic substrates and aluminum nitride ceramic shells.

[0003] With the development of high-power and very large-scale integrated circuits, the importance of heat dissipation between integrated circuits and aluminum nitride ceramic substrates has become increasingly apparent. High thermal conductivity aluminum nitride ceramic substrates can dissipate heat, preventing equipment performance degradation and shortened lifespan due to overheating, thus extending equipment lifespan and improving operational stability. However, existing aluminum nitride ceramic substrates currently suffer from low thermal conductivity. Furthermore, in electronic packaging, aluminum nitride ceramics are often used as the casing for encapsulating electronic components. If the bending strength of the aluminum nitride ceramic casing is low, it is prone to bending deformation or even breakage under external forces, leading to chip damage and similarly reducing the lifespan of electronic devices.

[0004] Therefore, there is a need to provide an aluminum nitride ceramic structural component with high thermal conductivity and high flexural strength. Summary of the Invention

[0005] This invention proposes a high thermal conductivity aluminum nitride ceramic structural component and its preparation method, which solves the problems of low thermal conductivity and low bending strength of aluminum nitride ceramic structural components in related technologies.

[0006] The technical solution of the present invention is as follows:

[0007] This invention proposes a high thermal conductivity aluminum nitride ceramic structural component, comprising the following raw materials in parts by weight: 100 parts aluminum nitride, 5-10 parts sintering aid, 4-6 parts plasticizer, 5-10 parts binder, 1-1.5 parts dispersant, 2-2.5 parts aluminum dihydroxyaminoacetate, and 70-80 parts solvent.

[0008] As a further technical solution, the sintering aid includes one or two of yttrium trioxide and lanthanum oxide.

[0009] As a further technical solution, the sintering aid is composed of yttrium trioxide and lanthanum oxide.

[0010] As a further technical solution, the mass ratio of yttrium oxide to lanthanum oxide is 1:1.

[0011] As a further technical solution, the aluminum nitride is modified aluminum nitride, which is obtained by modifying aluminum nitride with a modifier, the modifier including a surfactant.

[0012] As a further technical solution, the surfactant is nonylphenol polyoxyethylene ether.

[0013] As a further technical solution, the modifier also includes p-acetaminophenylboronic acid.

[0014] As a further technical solution, the amount of the modifier added is 4% to 6% of the mass of aluminum nitride.

[0015] As a further technical solution, when the modifier is composed of a surfactant and p-acetaminophenylboronic acid, the mass ratio of the surfactant to the p-acetaminophenylboronic acid is 3:1~3.

[0016] In this invention, by using surfactants and acetaminophenboronic acid to modify aluminum nitride, the thermal conductivity and flexural strength of aluminum nitride ceramic components can be further improved.

[0017] As a further technical solution, the preparation method of the modified aluminum nitride includes the following steps: adding aluminum nitride to water and mixing evenly, adding a modifier for modification, and drying to obtain modified aluminum nitride.

[0018] As a further technical solution, the modification temperature is 70°C and the modification time is 3 hours.

[0019] As a further technical solution, the mass-to-volume ratio of aluminum nitride to water is 1g:10mL.

[0020] As a further technical solution, the plasticizer includes one or both of dibutyl phthalate and diethyl phthalate.

[0021] As a further technical solution, the dispersant includes one or more of sodium pyrophosphate, sodium hexametaphosphate, and triethyl phosphate.

[0022] As a further technical solution, the adhesive includes one or more of polyvinyl butyral, ethyl cellulose, and polyvinyl alcohol.

[0023] As a further technical solution, the solvent is ethanol.

[0024] This invention also proposes a method for preparing aluminum nitride ceramic structural components with high thermal conductivity, comprising the following steps:

[0025] S1. After mixing aluminum nitride, sintering aid, dispersant, aluminum dihydroxyaminoacetate and solvent evenly, the mixture is ball-milled for the first time to obtain a mixture;

[0026] S2. After adding plasticizer and binder to the mixture and mixing evenly, perform a second ball milling to obtain a cast slurry;

[0027] S3. Cast the casting slurry into a shape, dry it, and press it to obtain a blank;

[0028] S4. After removing the binder from the blank, sinter it to obtain an aluminum nitride ceramic structural component.

[0029] As a further technical solution, the rotation speed of the first ball mill and the second ball mill is 800 rpm, the time of the first ball mill is 3 hours, and the time of the second ball mill is 1 hour.

[0030] As a further technical solution, in step S4, the sintering is carried out by heating to 1600°C at a heating rate of 5~15°C / min, then heating to 1700~1900°C at a heating rate of 2~6°C / min, and then sintering for 2~3 hours.

[0031] As a further technical solution, in step S4, the sintering is carried out by heating to 1600°C at a heating rate of 10°C / min, then heating to 1700~1900°C at a heating rate of 5°C / min, and then sintering for 2~3 hours.

[0032] In this invention, by limiting the parameters during the sintering process and using sintering aids, the thermal conductivity and flexural strength of aluminum nitride ceramic components can be further improved.

[0033] The working principle and beneficial effects of this invention are as follows:

[0034] In this invention, the raw materials for aluminum nitride ceramic structural components include aluminum nitride, sintering aids, plasticizers, binders, dispersants, aluminum dihydroxyaminoacetate, etc. Among them, aluminum nitride has high thermal conductivity. The addition of plasticizers and binders can increase the flexibility and viscosity of the green body. The addition of sintering aids can improve the thermal conductivity and bending strength of aluminum nitride ceramics. The addition of aluminum dihydroxyaminoacetate can not only improve the thermal conductivity of aluminum nitride ceramic structural components, but also improve the bending strength of aluminum nitride ceramic structural components. Detailed Implementation

[0035] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0036] In the following examples and comparative examples: the particle size of aluminum nitride is 5 μm; the weight-average molecular weight of polyvinyl butyral is 30,000.

[0037] Example 1

[0038] A method for preparing a high thermal conductivity aluminum nitride ceramic structural component includes the following steps:

[0039] S1. Mix 100 parts aluminum nitride, 5 parts sintering aid, 4 parts dibutyl phthalate, 5 parts polyvinyl butyral, 1 part sodium hexametaphosphate, 2 parts aluminum dihydroxyaminoacetate, and 70 parts ethanol evenly, and then ball mill at 800 rpm for 4 hours to obtain a cast slurry; wherein the sintering aid is lanthanum oxide.

[0040] S2. Cast the slurry into a shape, dry it, and press it to obtain a blank;

[0041] S3. After removing the binder from the blank, heat it to 1600℃ at a heating rate of 5℃ / min under a nitrogen atmosphere, then heat it to 1700℃ at a heating rate of 2℃ / min, and sinter for 3 hours to obtain aluminum nitride ceramic structural parts.

[0042] Example 2

[0043] A method for preparing a high thermal conductivity aluminum nitride ceramic structural component includes the following steps:

[0044] S1. Mix 100 parts aluminum nitride, 10 parts sintering aid, 6 parts diethyl phthalate, 10 parts polyvinyl butyral, 1.5 parts triethyl phosphate, 2.5 parts aluminum dihydroxyaminoacetate, and 80 parts ethanol evenly, and then ball mill at 800 rpm for 4 hours to obtain a cast slurry; wherein the sintering aid is lanthanum oxide.

[0045] S2. Cast the slurry into a shape, dry it, and press it to obtain a blank;

[0046] S3. After removing the binder from the blank, heat it to 1600℃ at a heating rate of 15℃ / min under a nitrogen atmosphere, and then heat it to 1900℃ at a heating rate of 6℃ / min. After sintering for 2 hours, aluminum nitride ceramic structural parts are obtained.

[0047] Example 3

[0048] A method for preparing a high thermal conductivity aluminum nitride ceramic structural component includes the following steps:

[0049] S1. Mix 100 parts aluminum nitride, 5 parts sintering aid, 1 part sodium hexametaphosphate, 2 parts aluminum dihydroxyaminoacetate, and 70 parts ethanol evenly, and then ball mill at 800 rpm for 3 hours to obtain a mixture; wherein the sintering aid is lanthanum oxide.

[0050] S2. Add 4 parts of dibutyl phthalate and 5 parts of polyvinyl butyral to the mixture, and ball mill at 800 rpm for 1 hour to obtain the cast slurry.

[0051] S3. Cast the slurry into a shape, dry it, and press it to obtain a blank;

[0052] S4. After removing the binder from the blank, heat it to 1600℃ at a heating rate of 5℃ / min under a nitrogen atmosphere, and then heat it to 1700℃ at a heating rate of 2℃ / min. After sintering for 3 hours, aluminum nitride ceramic structural parts are obtained.

[0053] Example 4

[0054] Compared with Example 3, the only difference in this example is that the aluminum nitride is modified aluminum nitride. The preparation method of the modified aluminum nitride in this example is as follows: aluminum nitride is added to water and mixed evenly, then nonylphenol polyoxyethylene ether is added, stirred at 70°C for 3 hours, and dried to obtain modified aluminum nitride; wherein the mass-volume ratio of aluminum nitride to water is 1g:10mL, and the amount of nonylphenol polyoxyethylene ether added is 6% of the mass of aluminum nitride.

[0055] Example 5

[0056] Compared with Example 4, the only difference in this example is that nonylphenol polyoxyethylene ether is replaced with an equal amount of acetaminophenboronic acid.

[0057] Example 6

[0058] Compared with Example 4, the only difference in this example is that nonylphenol polyoxyethylene ether is replaced with equal amounts of nonylphenol polyoxyethylene ether and para-acetaminophenylboronic acid in a mass ratio of 3:1.

[0059] Example 7

[0060] Compared with Example 6, the only difference in this example is that the mass ratio of nonylphenol polyoxyethylene ether to acetaminophenboronic acid is 3:2.

[0061] Example 8

[0062] Compared with Example 6, the only difference in this example is that the mass ratio of nonylphenol polyoxyethylene ether to acetaminophenboronic acid is 1:1.

[0063] Example 9

[0064] Compared with Example 7, the only difference in this example is that the combined mass of nonylphenol polyoxyethylene ether and acetaminophenylboronic acid added is 4% of the mass of aluminum nitride.

[0065] Example 10

[0066] Compared with Example 7, the only difference in this example is step S4. Step S4 in this example is: S4, after removing the binder from the blank, the temperature is raised to 1600°C at a heating rate of 15°C / min under a nitrogen atmosphere, and then raised to 1700°C at a heating rate of 2°C / min, and sintered for 3 hours to obtain aluminum nitride ceramic structural parts.

[0067] Example 11

[0068] Compared with Example 7, the only difference in this example is step S4. Step S4 in this example is: S4, after removing the binder from the blank, the temperature is raised to 1600°C at a heating rate of 10°C / min under a nitrogen atmosphere, and then raised to 1700°C at a heating rate of 2°C / min, and sintered for 3 hours to obtain aluminum nitride ceramic structural parts.

[0069] Example 12

[0070] Compared with Example 7, the only difference in this example is step S4. Step S4 in this example is: S4, after removing the binder from the blank, the temperature is raised to 1600°C at a heating rate of 10°C / min under a nitrogen atmosphere, and then raised to 1700°C at a heating rate of 8°C / min, and sintered for 3 hours to obtain aluminum nitride ceramic structural parts.

[0071] Example 13

[0072] Compared with Example 11, the only difference in this example is that the sintering aid is composed of yttrium trioxide and lanthanum oxide in a mass ratio of 1:1.

[0073] Comparative Example 1

[0074] Compared with Example 1, the only difference in this comparative example is that aluminum dihydroxyaminoacetate is not added.

[0075] The bending strength and thermal conductivity of the aluminum nitride ceramic structural components prepared in Examples 1-13 and Comparative Example 1 were measured respectively. The bending strength of the samples was determined by the three-point bending test according to GB / T 6569-2006 "Test Method for Bending Strength of Fine Ceramics"; the thermal conductivity of the samples was determined according to GB / T 32064-2015 "Test Method for Thermal Conductivity and Thermal Diffusion Coefficient of Building Materials by Transient Plane Heat Source". The test results are shown in Table 1.

[0076] Table 1. Performance test results of aluminum nitride ceramic structural components in Examples 1-13 and Comparative Example 1

[0077]

[0078] Compared with Comparative Example 1, aluminum dihydroxyaminoacetate was added in Example 1. As a result, the thermal conductivity and flexural strength of the aluminum nitride ceramic structure in Example 1 were higher than those in Comparative Example 1, indicating that adding aluminum dihydroxyaminoacetate can improve the thermal conductivity and flexural strength of the aluminum nitride ceramic structure.

[0079] Compared with Example 1, the raw materials in Example 3 were ground twice. As a result, the thermal conductivity and bending strength of the aluminum nitride ceramic structural parts in Example 3 were higher than those in Example 1, indicating that grinding the raw materials twice can improve the thermal conductivity and bending strength of the aluminum nitride ceramic structural parts.

[0080] Compared with Example 3, Examples 4-8 used different modifiers to modify aluminum nitride. As a result, the thermal conductivity and flexural strength of the aluminum nitride ceramic structural parts in Examples 6-8 were higher than those in Examples 3-5. This indicates that modifying aluminum nitride with nonylphenol polyoxyethylene ether and acetaminophenboronic acid can further improve the thermal conductivity and flexural strength of aluminum nitride ceramic structural parts.

[0081] Compared with Example 6, Examples 7 and 8 changed the ratio of nonylphenol polyoxyethylene ether and p-acetaminophenylboronic acid. As a result, the thermal conductivity and flexural strength of the aluminum nitride ceramic component in Example 7 were higher than those in Examples 6 and 8, indicating that when the mass ratio of nonylphenol polyoxyethylene ether to p-acetaminophenylboronic acid is 3:2, the thermal conductivity and flexural strength of the aluminum nitride ceramic component can be further improved.

[0082] Compared with Example 7, Examples 10-12 changed the sintering conditions, and Example 13 changed the sintering aids. As a result, the thermal conductivity and flexural strength of the aluminum nitride ceramic component in Example 11 were higher than those in Examples 10 and 12. At the same time, the thermal conductivity and flexural strength of the aluminum nitride ceramic component in Example 13 were higher than those in Example 11. This shows that the limitation of the sintering aids and sintering conditions in this invention can further improve the thermal conductivity and flexural strength of the aluminum nitride ceramic component.

[0083] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A high thermal conductivity aluminum nitride ceramic structural component, characterized in that, The raw material comprises the following components by weight: 100 parts aluminum nitride, 5-10 parts sintering aid, 4-6 parts plasticizer, 5-10 parts binder, 1-1.5 parts dispersant, 2-2.5 parts aluminum dihydroxyaminoacetate, and 70-80 parts solvent. The aluminum nitride is modified aluminum nitride, which is obtained by modifying aluminum nitride with a modifier. The modifier is composed of nonylphenol polyoxyethylene ether and acetaminophenboronic acid in a mass ratio of 3:

2.

2. The high thermal conductivity aluminum nitride ceramic structural component according to claim 1, characterized in that, The sintering aid includes one or both of yttrium trioxide and lanthanum oxide.

3. The high thermal conductivity aluminum nitride ceramic structural component according to claim 1, characterized in that, The amount of the modifier added is 4% to 6% of the mass of aluminum nitride.

4. The high thermal conductivity aluminum nitride ceramic structural component according to claim 1, characterized in that, The plasticizer includes one or both of dibutyl phthalate and diethyl phthalate.

5. The high thermal conductivity aluminum nitride ceramic structural component according to claim 1, characterized in that, The dispersant includes one or more of sodium pyrophosphate, sodium hexametaphosphate, and triethyl phosphate.

6. A method for preparing a high thermal conductivity aluminum nitride ceramic structural component according to any one of claims 1 to 5, characterized in that, Includes the following steps: S1. After mixing aluminum nitride, sintering aid, dispersant, aluminum dihydroxyaminoacetate and solvent evenly, the mixture is ball-milled for the first time to obtain a mixture; S2. After adding plasticizer and binder to the mixture and mixing evenly, perform a second ball milling to obtain a cast slurry; S3. Cast the casting slurry into a shape, dry it, and press it to obtain a blank; S4. After removing the binder from the blank, sinter it to obtain an aluminum nitride ceramic structural component.

7. The method for preparing a high thermal conductivity aluminum nitride ceramic structural component according to claim 6, characterized in that, In step S4, the sintering is performed by heating the temperature to 1600°C at a heating rate of 5~15°C / min, then heating it to 1700~1900°C at a heating rate of 2~6°C / min, and then sintering for 2~3 hours.

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