CN113831140A - Si3N4Preparation method of heat-conducting ceramic material - Google Patents
Si3N4Preparation method of heat-conducting ceramic material Download PDFInfo
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Abstract
The invention discloses Si3N4The preparation method of the heat-conducting ceramic material comprises the following steps: modifying, preparing gel state suspension, forming, dehydrating and degreasing, and sintering. According to the invention, a high-uniformity and trace-amount graphene distribution structure is formed in a gel-state liquid, so that high-uniformity distribution of graphene is realized, blank forming is realized simultaneously, in-situ distribution of active graphene in a silicon nitride matrix is finally achieved, oxygen removal at a crystal boundary is realized, a glass phase is reduced, an alpha → beta phase transformation rate is improved, and the problems of deformation and cracking of a blank, limited crystal lattice oxygen removal effect and the like caused by uneven distribution due to direct addition of carbon are reduced; effectively improves the heat-conducting property and the strength of the material.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to Si3N4A preparation method of a heat-conducting ceramic material.
Background
The silicon nitride has the characteristics of high hardness, high strength, small thermal expansion coefficient and the like, is chemically inert to metal at high temperature and has high fracture toughness, and becomes an attractive substrate material for the 5G communication field. The heat-conducting property and dielectric loss characteristic of silicon nitride are mainly determined by compactness, glass phase content, beta phase proportion, grain size and the like.
The Chinese patent with application number of 2020101077487 discloses high-thermal-conductivity Si3N4Ceramics and process for their preparation, using Si3N4Powder and sintering aid Mg2Preparation of Si from Si and C3N4A ceramic. The technical scheme improves Si3N4The ceramic material has mechanical property and thermal conductivity, but the carbon is easily distributed unevenly when being directly added, and the excessive addition can reduce the compactness and increase the loss value. Therefore, how to regulate the content and the uniform distribution of the trace carbon is one of the key points for realizing the high-frequency, low-loss, high-heat conduction and the commercialization of the silicon nitride.
Disclosure of Invention
The invention aims to provide Si aiming at the defects in the prior art3N4The preparation method of the heat-conducting ceramic material enables the graphene to be uniformly distributed through gel forming, simultaneously realizes blank forming, and enhances Si3N4Uniformity of mixing of the powder with the graphene.
Another object of the present invention is to provide Si obtained by the above-mentioned production method3N4A thermally conductive ceramic material.
The purpose of the invention is realized by the following technical scheme:
si3N4The preparation method of the heat-conducting ceramic material comprises the following steps:
s1, modification: mixing Si3N4Pickling the powder in an acid solution to obtain modified Si3N4Powder;
s2, preparing gel state liquid: will modify Si3N4Aging the powder, adding nano graphene, a sintering aid and an alkaline solution, uniformly mixing, and then aging and neutralizingAnd then fully mixing with a monomer, a cross-linking agent, a dispersing agent and a catalyst to obtain Si3N4A gel state suspension formed by the sintering aid and the nano graphene;
s3, forming: filling the gel state liquid into a die cavity, and adding an initiator to form a blank body;
s4, dehydration and degreasing treatment: dehydrating the blank, and then heating and degreasing to uniformly distribute the nano graphene in the blank;
s5, sintering: carrying out hot-pressing sintering on the green body treated in the step S4 to obtain Si3N4A thermally conductive ceramic material.
Further, in step S2, the amount of the nano graphite phase is Si3N40.1-0.3 wt% of the powder, the nano graphene is of a single-layer structure, the graphene content is more than 50%, and the flake diameter is more than 10 μm.
Further, the alkaline solution in step S2 includes one or more of NaOH, KOH, and ammonia.
Further, the total mass of the gel raw material in step S2 is Si3N42-6% of the powder by mass, the monomer is one or more of acrylic acid, dimethylacrylamide, dimethylaminobutylacrylate, methacrylate and hydroxyethyl acrylate, and the crosslinking agent is at least one of N, N-methylene acrylamide and isocyanic acid radical.
Further, in step S2, the dispersant is at least one of ammonium polyacrylate and polyethylene glycol, and the catalyst is one or more of tetramethylethylenediamine, lewis acid, polyacrylamide, and the like.
Further, the initiator in step S3 is a persulfate-based initiator or a redox initiator.
Further, the persulfate initiator includes potassium persulfate, sodium persulfate, or ammonium persulfate.
Further, the redox initiator includes t-butyl hydroperoxide, sodium metabisulfite or sucrose.
Further, in the step S4, the dehydration treatment temperature is 60-90 ℃, and the time is 36-60 h; the heating and degreasing process comprises the steps of heating the blank from 100 ℃ to 1000 ℃, wherein the heating rate is 5 ℃/min, and the blank is respectively subjected to heat preservation for 1-2 times at the temperature of 200-.
Further, in the step S5, the hot-pressing sintering temperature is 4650-1900 ℃, and the pressure is 10-15 MPa.
Si obtained by the preparation method3N4A thermally conductive ceramic material.
Compared with the prior art, the invention has the following beneficial effects:
the invention effectively reduces Si through modification treatment3N4Oxides influencing the heat-conducting property of the material in the powder improve the surface energy and sintering activity of the powder, and can reduce the material cost; with simultaneous increase of Si3N4Uniformity of mixing of the powder with the graphene.
According to the invention, a high-uniformity and trace-amount graphene distribution structure is formed in a gel-state liquid, so that high-uniformity distribution of graphene is realized, blank forming is realized simultaneously, in-situ distribution of active graphene in a silicon nitride matrix is finally achieved, oxygen removal at a crystal boundary is realized, a glass phase is reduced, an alpha → beta phase transformation rate is improved, and the problems of deformation and cracking of a blank, limited crystal lattice oxygen removal effect and the like caused by uneven distribution due to direct addition of carbon are reduced; the heat conductivity and the strength of the material are effectively improved, and the heat conductivity coefficient reaches 120-150 W.m-1·K-1And the bending strength is over 800 MPa.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described in more detail with reference to the following examples, but the scope of the present invention is not limited to the following specific examples.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
This example provides Si3N4The preparation method of the heat-conducting ceramic material specifically comprises the following steps:
s1, modification: mixing Si3N4Pickling the powder in an acid solution to obtain modified Si3N4Powder, acidic solution is 3% HNO3Mixing with HCl with the concentration of 3% according to the ratio of 1: 1;
s2, preparing gel state liquid: will modify Si3N4Aging the powder, adding 0.2 wt% of nano graphene, 8 wt% of sintering aid (3 wt% of Y2O3 and 5 wt% of MgO) and alkaline solution, mixing uniformly, aging, neutralizing, and adding Si3N4The mixture of the powder and the nano-graphene is heated to 50 ℃ and fully mixed with 2 wt% of monomer acrylic acid, 0.5 wt% of cross-linking agent N, N-methylene acrylamide, 0.2 wt% of dispersing agent PEG400 and 0.2 wt% of catalyst tetramethyl ethylene diamine in a stirring and heating device, and the total mass of the gel raw material is Si3N42.9 wt% of the powder mass; to obtain Si3N4And nano-graphene;
s3, forming: filling the gel-state liquid into a die cavity, and adding 0.3 wt% of initiator potassium persulfate to form a blank;
s4, dehydration and degreasing treatment: dehydrating the blank, baking in an oven at 60 ℃ for 24h, baking at 70 ℃ for 12h, and baking at 80 ℃ for 12h to remove the compound water; then heating and degreasing, wherein the heating rate is 5 ℃/min, and degreasing is carried out after heat preservation is carried out for 2 hours at 350 ℃ and 700 ℃ respectively, so that the nano graphene is uniformly distributed in the blank;
s5, sintering: hot-pressing sintering the green body treated in the step S4 for 2h at 1850 ℃ under the pressure of 10MPa to obtain Si3N4A thermally conductive ceramic material.
The graphene used in the embodiment of the application is of a single-layer structure, the content of the graphene is more than 50%, and the diameter of each sheet is more than 10 micrometers.
Example 2
This example provides Si3N4The preparation method of the heat-conducting ceramic material specifically comprises the following steps:
s1, modification: mixing Si3N4Pickling the powder in an acid solution to obtain modified Si3N4Powder, acid solution is HNO with the concentration of 2%3Mixing with HCl with concentration of 4% at a ratio of 1: 1;
s2, preparing gel state liquid: will modify Si3N4Aging the powder, adding nano graphene and 8 wt% of sintering aid (3 wt% of Y)2O3And 5 wt% MgO) and an alkaline solution, then aging, neutralizing, and adding Si3N4The mixture of the powder and 0.15 wt% of nano-graphene is fully mixed with 2.8 wt% of monomer methacrylate, 0.5 wt% of cross-linking agent N, N-methylene acrylamide, 0.5 wt% of dispersing agent PEG10000 and 0.3 wt% of catalyst tetramethyl ethylene diamine in a stirring and heating device by heating to 50 ℃, and the total mass of the gel raw material is Si3N41 wt% of the mass of the powder; to obtain Si3N4A gel state suspension formed by the sintering aid and the nano graphene;
s3, forming: filling the gel state liquid into a die cavity, and adding initiators of potassium persulfate and cane sugar to form a blank body;
s4, dehydration and degreasing treatment: dehydrating the blank, baking in an oven at 60 ℃ for 18h, baking at 70 ℃ for 8h, and baking at 85 ℃ for 8h to remove the compound water; then heating and degreasing, wherein the heating rate is 5 ℃/min, and degreasing is carried out after heat preservation is carried out for 2 hours at 350 ℃ and 700 ℃ respectively, so that the nano graphene is uniformly distributed in the blank;
s5, sintering: carrying out hot-pressing sintering on the green body treated in the step S4 for 3h at 1800 ℃ and under the pressure of 10MPa to obtain Si3N4A thermally conductive ceramic material.
Example 3
This example provides Si3N4The preparation method of the heat-conducting ceramic material specifically comprises the following steps:
s1, modification: mixing Si3N4Pickling the powder in an acid solution to obtainModified Si3N4Powder, acid solution of 4% HNO3Mixing with HCl with the concentration of 2% according to the ratio of 1: 1;
s2, preparing gel state liquid: will modify Si3N4Aging the powder, adding 0.3 wt% of nano graphene and 8 wt% of sintering aid (3 wt% of Y)2O3And 5 wt% MgO) and an alkaline solution, then aging, neutralizing, and adding Si3N4The mixture of the powder and the nano-graphene is fully mixed with 1.8 wt% of monomer hydroxyethyl acrylate, 0.4 wt% of cross-linking agent N, N-methylene acrylamide, 0.6 wt% of dispersant ammonium polyacrylate and 0.2 wt% of catalyst tetramethylethylenediamine in a stirring and heating device by heating to 50 ℃, wherein the total mass of the gel raw material is Si3N43 wt% of the mass of the powder; to obtain Si3N4A gel state suspension formed by the sintering aid and the nano graphene;
s3, forming: filling the gel-state liquid into a die cavity, and adding an initiator of 0.2 wt% of potassium persulfate and 0.1 wt% of sodium persulfate to form a blank;
s4, dehydration and degreasing treatment: dehydrating the blank, baking the blank in a baking oven at 68 ℃ for 32h, baking the blank at 75 ℃ for 12h, and baking the blank at 80 ℃ for 8h to remove the compound water; then heating and degreasing, wherein the heating rate is 5 ℃/min, and degreasing is carried out after heat preservation is carried out for 2 hours at 350 ℃ and 700 ℃ respectively, so that the nano graphene is uniformly distributed in the blank;
s5, sintering: carrying out hot-pressing sintering on the green body treated in the step S4, and carrying out hot-pressing sintering for 2h at 1750 ℃ under the pressure of 10MPa to obtain Si3N4A thermally conductive ceramic material.
Example 4
This example provides Si3N4The preparation method of the heat-conducting ceramic material specifically comprises the following steps:
s1, modification: mixing Si3N4Pickling the powder in an acid solution to obtain modified Si3N4Powder, acid solution of 3% H2SO4；
S2, preparing gel state liquid: will modify Si3N4Aging the powder, adding 0.12 wt% of nano graphene and 8 wt% of sintering aid (3 wt% of Y)2O3And 5 wt% MgO) and an alkaline solution, then aging, neutralizing, and adding Si3N4The mixture of the powder and the nano-graphene is fully mixed with 3.6 wt% of monomer methacrylate, 0.6 wt% of cross-linking agent isocyanic acid radical, 0.5 wt% of dispersant ammonium polyacrylate and 0.3 wt% of catalyst polyacrylamide in a stirring and heating device by heating to 50 ℃, and the total mass of the gel raw material is Si3N45 wt% of the mass of the powder; to obtain Si3N4A gel state suspension formed by the sintering aid and the nano graphene;
s3, forming: filling the gel-state liquid into a die cavity, and adding 0.3 wt% of initiator sodium peroxodisulfate to form a blank;
s4, dehydration and degreasing treatment: dehydrating the blank, baking in an oven at 60 ℃ for 24h, baking at 70 ℃ for 12h, and baking at 80 ℃ for 12h to remove the compound water; then heating and degreasing, wherein the heating rate is 5 ℃/min, and the nano graphene is uniformly distributed in the blank by respectively keeping the temperature at 400 ℃ and 650 ℃ for 2 hours for degreasing;
s5, sintering: hot-pressing sintering the green body treated in the step S4 for 2h at 1850 ℃ under the pressure of 10MPa to obtain Si3N4A thermally conductive ceramic material.
Si prepared in examples 1 to 43N4The heat-conducting ceramic material is subjected to performance test, and the result is as follows:
it should be understood that the above examples are only for clearly illustrating the technical solutions of the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. Si3N4The preparation method of the heat-conducting ceramic material is characterized by comprising the following steps:
s1, modification: mixing Si3N4Pickling the powder in an acid solution to obtain modified Si3N4Powder;
s2, preparing gel state liquid: will modify Si3N4Aging the powder, adding nano graphene, a sintering aid and an alkaline solution, uniformly mixing, aging, neutralizing, and fully mixing with a monomer, a cross-linking agent, a dispersing agent and a catalyst to obtain Si3N4A gel state suspension formed by the sintering aid and the nano graphene;
s3, forming: filling the gel state liquid into a die cavity, and adding an initiator to form a blank body;
s4, dehydration and degreasing treatment: dehydrating the blank, and then heating and degreasing to uniformly distribute the nano graphene in the blank;
s5, sintering: carrying out hot-pressing sintering on the green body treated in the step S4 to obtain Si3N4A thermally conductive ceramic material.
2. Si according to claim 13N4The preparation method of the heat-conducting ceramic material is characterized in that the acidic solution in the step S1 comprises HNO3、HCl、H2SO4And one or more of acetic acid, wherein the concentration of the solution is 2-5%.
3. Si according to claim 13N4The preparation method of the heat-conducting ceramic material is characterized in that the dosage of the nano graphene in the step S2 is Si3N40.1-0.3 wt% of the powder, the nano graphene is of a single-layer structure, the graphene content is more than 50%, and the flake diameter is more than 10 μm.
4. According to claim 1Si as described above3N4The preparation method of the heat-conducting ceramic material is characterized in that the alkaline solution in the step S2 comprises one or more of NaOH, KOH and ammonia water.
5. Si according to claim 13N4The preparation method of the heat-conducting ceramic material is characterized in that the total mass of the gel raw material in the step S2 is Si3N42-6% of the powder by mass, the monomer is one or more of acrylic acid, dimethylacrylamide, dimethylaminobutylacrylate, methacrylate and hydroxyethyl acrylate, and the crosslinking agent is at least one of N, N-methylene acrylamide and isocyanic acid radical.
6. Si according to claim 13N4The preparation method of the heat-conducting ceramic material is characterized in that in the step S2, the dispersant is at least one of ammonium polyacrylate and polyethylene glycol, and the catalyst is one or more of tetramethylethylenediamine, Lewis acid, polyacrylamide and the like.
7. Si according to claim 13N4The preparation method of the heat-conducting ceramic material is characterized in that the initiator in the step S3 is a persulfate initiator or a redox initiator.
8. Si according to claim 13N4The preparation method of the heat-conducting ceramic material is characterized in that the dehydration treatment temperature in the step S4 is 60-90 ℃, and the time is 36-60 h; the heating and degreasing process comprises the steps of heating the blank from 100 ℃ to 1000 ℃, wherein the heating rate is 5 ℃/min, and the blank is respectively subjected to heat preservation for 1-2 times at the temperature of 200-.
9. Si according to claim 13N4The preparation method of the heat-conducting ceramic material is characterized in that in the step S5, the hot-pressing sintering temperature is 1650-1900 ℃, and the pressure is 10-15 MPa.
10. Si obtained by the preparation method of any one of claims 1 to 93N4A thermally conductive ceramic material.
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