CN110937902A - Preparation method of aluminum nitride ceramic substrate - Google Patents
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Abstract
The invention relates to the field of ceramics, in particular to a preparation method of an aluminum nitride ceramic substrate, which comprises the steps of carrying out hydrophobic modification, pulping, tape casting, curing, stamping, drying and sintering on aluminum nitride powder, solving the problems of easy hydrolysis and great reduction of heat conductivity caused by increase of oxygen content by carrying out surface modification on the aluminum nitride powder, preparing water-based slurry with high solid content, low viscosity and good fluidity by introducing a small amount of auxiliary agent, solving the defects of a substrate blank in molding and drying, and realizing high yield and uniform structure of the substrate.
Description
Technical Field
The invention relates to the field of ceramics, in particular to a preparation method of an aluminum nitride ceramic substrate.
Background
With the development of high power and very large scale integrated circuits, heat dissipation between the integrated circuit and the substrate is also becoming more important, and therefore, the substrate must have high thermal conductivity and electrical resistivity.
Aluminum nitride AlN is the only stable compound of Al and N, and is the largest semiconductor in the III-V group in energy gap values. The aluminum nitride ceramic has a series of excellent performances of high thermal conductivity, relatively low dielectric constant and dielectric loss, thermal expansion coefficient matched with chip materials such as silicon, gallium arsenide and the like, good interface compatibility, no toxicity, insulation and the like, and becomes a high-performance ceramic substrate material necessary for electronic packaging heat dissipation materials and assembling large-scale integrated circuits.
Currently, the main method for producing AlN ceramic substrates is tape casting, and most of them are organic solvent tape casting. The organic solvent tape casting adopts organic solvents (benzene, toluene, xylene, butanone and the like) with certain toxicity, is flammable and has serious pollution to the environment, and is harmful to the health of a human body. A large amount of organic matters exist in the formed blank, and the blank is easy to crack and deform in the later glue discharging process; in the drying process, the ceramic powder is settled, the density gradient is formed on the upper surface and the lower surface of the blank, cracks are easily generated on the upper surface, and the glossiness is poor. From the view point of operation cost and sustainable development, the water-based casting system is better, but the easy hydrolysis of the aluminum nitride powder seriously hinders the development of the water-based casting process of the aluminum nitride ceramics.
Disclosure of Invention
Based on the technical background, the invention provides a preparation method of an aluminum nitride ceramic substrate, which solves the problems of easy hydrolysis and great reduction of heat conductivity caused by increase of oxygen content by carrying out surface modification on aluminum nitride powder, and solves the defects of a substrate biscuit in molding and drying by introducing a small amount of auxiliary agent to prepare water-based slurry with high solid content, low viscosity and good fluidity, thereby realizing high yield and uniform structure of the substrate.
The invention is realized by the following technical scheme:
a preparation method of an aluminum nitride ceramic substrate comprises the following steps:
s1: carrying out hydrophobic modification on the aluminum nitride powder to obtain modified aluminum nitride powder;
s2: pulping modified aluminum nitride powder by using water as a solvent to obtain molding slurry;
s3: carrying out tape casting, curing, stamping and drying on the molding slurry to obtain a blank sheet;
s4: performing plastic removal and sintering on the blank sheet to obtain a finished product of the aluminum nitride ceramic substrate;
the hydrophobic modification method of S1 comprises the steps of soaking aluminum nitride powder in a hydrophobic liquid for 8-60 hours, wherein the hydrophobic liquid is a mixed liquid of alcohol, n-hexane and hexamethyl-silazane, and the alcohol is one of absolute ethyl alcohol, isopropanol or n-butanol (the weight ratio of the alcohol to the aluminum nitride powder to the n-hexane to the hexamethyl-silazane is 10: 1: 2-3.5: 0.06-0.13, and the hydrophobic liquid is subjected to hydrophobic treatment); or placing the aluminum nitride powder body in an air atmosphere or an oxygen atmosphere for heat treatment at the temperature of 650-750 ℃ for 20-60 min;
wherein, an additive is also added in the S2 pulping process, the additive comprises a sintering aid, a cross-linking agent, an adhesive and a plasticizer, the adhesive or the plasticizer is polyvinyl alcohol, and the addition amount of the adhesive or the plasticizer is 0.05-0.3% of the mass of the aluminum nitride powder;
wherein, the plastic removal and sintering in S4 are completed in one step, the plastic removal temperature is 600-800 ℃, the heat preservation time is 4-6h, the sintering final sintering temperature is 1720-1800 ℃, and the heat preservation time is 0.5-3 h.
The invention has the beneficial effects that: (1) the aluminum nitride powder is subjected to hydrophobic modification, so that the problem of reduced thermal conductivity caused by hydrolysis of the aluminum nitride powder in a water-based casting molding system is solved; (2) the defects of the substrate biscuit in the forming and drying process are overcome by introducing a small amount of multifunctional PVA auxiliary agent, and the high yield and the uniform structure of the substrate are realized.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
S1, weighing 3000g of absolute ethyl alcohol, 1050g of n-hexane and 39g of hexamethyldisilazane, and placing the mixture into a magnetic stirrer to stir for 30 min; then weighing 300g of aluminum nitride powder, putting the aluminum nitride powder into hydrophobic liquid, stirring for 24 hours, standing, and taking out the powder after the powder is separated from the liquid and drying;
s2, mixing the dried powder obtained in the step 1 with 60g of deionized water, taking water as a solvent, introducing a sintering aid, a monomer and a cross-linking agent, carrying out ball milling and mixing for 4 hours, adding 30g of a 3% polyvinyl alcohol aqueous solution, and continuing ball milling for 2 hours to obtain a molding slurry with good fluidity, high solid content and low viscosity after defoaming;
s3, placing the molding slurry in the step 2 in a casting machine for casting molding, curing, stamping and drying;
and S4, sintering the formed blank sheet in a nitrogen atmosphere protective furnace, preserving heat for 5 hours at the temperature of 620 ℃ for plastic removal, preserving heat for 1.5 hours at the final sintering temperature of 1750 ℃ to obtain the aluminum nitride ceramic substrate.
The aluminum nitride ceramic substrate prepared by the method has the density of 3.32g/cm3, the bending strength of 389MPa, the thermal expansion coefficient (RT-400 ℃) of 3.9 multiplied by 10 < -6 >/DEG C and the thermal conductivity of 180W/(m.K).
Example 2
S1, weighing 3000g of absolute ethyl alcohol, 700g of n-hexane and 18g of hexamethyldisilazane, and stirring in a magnetic stirrer for 30 min; then weighing 300g of aluminum nitride powder, putting the aluminum nitride powder into hydrophobic liquid, stirring for 60 hours, standing, and taking out the powder after the powder is separated from the liquid and drying;
s2, mixing the dried powder in the step 1 with 80g of deionized water, taking water as a solvent, introducing a sintering aid, a monomer and a cross-linking agent, carrying out ball milling and mixing for 4 hours, adding 5g of 3% polyvinyl alcohol aqueous solution, and continuing ball milling for 2 hours to obtain molding slurry with good fluidity, high solid content and low viscosity after defoaming;
s3, placing the molding slurry in the step 2 in a casting machine for casting molding, curing, stamping and drying;
and S4, placing the formed blank sheet into a nitrogen atmosphere protection furnace for sintering, preserving heat for 4 hours at 700 ℃ for plastic removal, preserving heat for 3 hours at 1720 ℃ for final sintering temperature, and obtaining the aluminum nitride ceramic substrate.
The aluminum nitride ceramic substrate prepared by the method has the density of 3.30g/cm3, the bending strength of 341MPa, the thermal expansion coefficient (RT-400 ℃) of 3.5 multiplied by 10 < -6 >/DEG C and the thermal conductivity of 172W/(m.K).
Example 3
S1, weighing 3000g of absolute ethyl alcohol, 600g of n-hexane and 25g of hexamethyldisilazane, and placing the mixture into a magnetic stirrer to stir for 30 min; then weighing 300g of aluminum nitride powder, putting the aluminum nitride powder into hydrophobic liquid, stirring for 24 hours, standing, and taking out the powder after the powder is separated from the liquid and drying;
s2, mixing the dried powder in the step 1 with 70g of deionized water, taking water as a solvent, introducing a sintering aid, a monomer and a cross-linking agent, carrying out ball milling and mixing for 4h, adding 15g of a 3% polyvinyl alcohol aqueous solution, continuing ball milling for 2h, and removing bubbles to obtain a molding slurry with good fluidity, high solid content and low viscosity;
s3, placing the molding slurry in the step 2 in a casting machine for casting molding, curing, stamping and drying;
and S4, placing the formed blank sheet into a nitrogen atmosphere protection furnace for sintering, preserving heat for 6 hours at the temperature of 600 ℃ for plastic removal, preserving heat for 0.5 hour at the final sintering temperature of 1800 ℃ to obtain the aluminum nitride ceramic substrate.
The aluminum nitride ceramic substrate prepared by the method has the density of 3.33g/cm3, the bending strength of 425MPa, the thermal expansion coefficient (RT-400 ℃) of 4.1 multiplied by 10 < -6 >/DEG C and the thermal conductivity of 190W/(m.K).
Example 4
S1, weighing 300g of aluminum nitride powder, and placing the aluminum nitride powder in an oxidizing atmosphere furnace for heat treatment at 650 ℃ for 60 min;
s2, mixing the powder subjected to heat treatment in the step 1 with 60g of deionized water, taking water as a solvent, introducing a sintering aid, a monomer and a cross-linking agent, ball-milling and mixing for 4 hours, adding 15g of a 3% polyvinyl alcohol aqueous solution, continuing ball-milling for 2 hours, and removing bubbles to obtain a molding slurry with good fluidity, high solid content and low viscosity;
s3, placing the molding slurry in the step 2 in a casting machine for casting molding, curing, stamping and drying;
and S4, sintering the formed blank sheet in a nitrogen atmosphere protective furnace, preserving heat for 4 hours at the temperature of 620 ℃ for plastic removal, preserving heat for 1.5 hours at the final sintering temperature of 1750 ℃ to obtain the aluminum nitride ceramic substrate.
The aluminum nitride ceramic substrate prepared by the method has the density of 3.32g/cm3, the bending strength of 383MPa, the thermal expansion coefficient (RT-400 ℃) of 3.9 multiplied by 10 < -6 >/DEG C and the thermal conductivity of 182W/(m.K).
Example 5
S1, weighing 300g of aluminum nitride powder, and placing the aluminum nitride powder in an oxidizing atmosphere furnace for heat treatment at 670 ℃ for 50 min;
s2, mixing the powder subjected to heat treatment in the step 1 with 80g of deionized water, taking water as a solvent, introducing a sintering aid, a monomer and a cross-linking agent, ball-milling and mixing for 4 hours, adding 5g of a 3% polyvinyl alcohol aqueous solution, continuing ball-milling for 2 hours, and removing bubbles to obtain a molding slurry with good fluidity, high solid content and low viscosity;
s3, placing the molding slurry in the step 2 in a casting machine for casting molding, curing, stamping and drying;
and S4, placing the formed blank sheet into a nitrogen atmosphere protection furnace for sintering, preserving heat for 4 hours at 700 ℃ for plastic removal, preserving heat for 3 hours at 1720 ℃ for final sintering temperature, and obtaining the aluminum nitride ceramic substrate.
The aluminum nitride ceramic substrate prepared by the method has the density of 3.31g/cm3, the bending strength of 337MPa, the thermal expansion coefficient (RT-400 ℃) of 3.7 multiplied by 10 < -6 >/DEG C and the thermal conductivity of 175W/(m.K).
Example 6
S1, weighing 300g of aluminum nitride powder, and placing the aluminum nitride powder in an oxidizing atmosphere furnace for heat treatment at the treatment temperature of 750 ℃ for 20 min;
s2, mixing the powder subjected to heat treatment in the step 1 with 70g of deionized water, taking water as a solvent, introducing a sintering aid, a monomer and a cross-linking agent, ball-milling and mixing for 4 hours, adding 15g of a 3% polyvinyl alcohol aqueous solution, continuing ball-milling for 2 hours, and removing bubbles to obtain a molding slurry with good fluidity, high solid content and low viscosity;
s3, placing the molding slurry in the step 2 in a casting machine for casting molding, curing, stamping and drying;
and S4, placing the formed blank sheet into a nitrogen atmosphere protection furnace for sintering, preserving heat for 4 hours at the temperature of 600 ℃ for plastic removal, preserving heat for 0.5 hour at the final sintering temperature of 1800 ℃ to obtain the aluminum nitride ceramic substrate.
The aluminum nitride ceramic substrate prepared by the method has the density of 3.33g/cm3, the bending strength of 440MPa, the thermal expansion coefficient (RT-400 ℃) of 4.4 multiplied by 10 < -6 >/DEG C and the thermal conductivity of 194W/(m.K).
Claims (10)
1. A preparation method of an aluminum nitride ceramic substrate is characterized by comprising the following steps:
s1: carrying out hydrophobic modification on the aluminum nitride powder to obtain modified aluminum nitride powder;
s2: pulping modified aluminum nitride powder by using water as a solvent to obtain molding slurry;
s3: carrying out tape casting, curing, stamping and drying on the molding slurry to obtain a blank sheet;
s4: and performing plastic removal and sintering on the blank sheet to obtain a finished product of the aluminum nitride ceramic substrate.
2. The method of claim 1, wherein the hydrophobic modification step S1 is carried out by immersing the aluminum nitride powder in a hydrophobic liquid for 8-60 h.
3. The method of claim 2, wherein the hydrophobic liquid is a mixture of alcohols, n-hexane and hexamethyl-disilazane, wherein the alcohol: aluminum nitride powder: n-hexane: the mass ratio of the hexamethyl-disilazane is 10: 1: 2-3.5: 0.06-0.13.
4. The method of claim 2, wherein the hydrophobic liquid is a mixture of an alcohol, n-hexane, and hexamethyl-silazane, wherein the alcohol: aluminum nitride powder: n-hexane: the mass ratio of hexamethyl silazane is 10: 1: 2-3.5: 0.06-0.13.
5. The method of claim 3 or 4, wherein the alcohol is one of absolute ethanol, isopropanol or n-butanol.
6. The method of claim 1, wherein the hydrophobic modification step S1 is carried out by subjecting the aluminum nitride powder to heat treatment in an air atmosphere or an oxygen atmosphere.
7. The method as claimed in claim 6, wherein the heat treatment temperature is 650-750 ℃ and the treatment time is 20-60 min.
8. The method of claim 1, wherein additives including sintering aid, cross-linking agent, binder and plasticizer are added during the S2 pulping process.
9. The method of claim 8, wherein the binder or plasticizer is polyvinyl alcohol and the amount of the binder or plasticizer is 0.05-0.3% by mass of the aluminum nitride powder.
10. The method as claimed in claim 1, wherein the step of removing plastic and sintering is performed in S4 at one time, the temperature for removing plastic is 600-700 ℃ and the temperature for sintering is 4-6h, the temperature for final sintering is 1720-1800 ℃ and the temperature for sintering is 0.5-3 h.
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| CN111875386A (en) * | 2020-08-07 | 2020-11-03 | 福建臻璟新材料科技有限公司 | Aluminum nitride ceramic substrate and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111875386A (en) * | 2020-08-07 | 2020-11-03 | 福建臻璟新材料科技有限公司 | Aluminum nitride ceramic substrate and preparation method thereof |
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