CN111154262A - Heat-conducting paste containing aluminum oxide and/or boron nitride and preparation method thereof - Google Patents
Heat-conducting paste containing aluminum oxide and/or boron nitride and preparation method thereof Download PDFInfo
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- CN111154262A CN111154262A CN201911327301.4A CN201911327301A CN111154262A CN 111154262 A CN111154262 A CN 111154262A CN 201911327301 A CN201911327301 A CN 201911327301A CN 111154262 A CN111154262 A CN 111154262A
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 55
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000945 filler Substances 0.000 claims abstract description 26
- 239000002199 base oil Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229920002545 silicone oil Polymers 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- -1 methyl hydrogen Chemical compound 0.000 claims description 14
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000003814 drug Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 4
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 229940079593 drug Drugs 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 239000003674 animal food additive Substances 0.000 claims description 2
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 238000010292 electrical insulation Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/32—Thermal decomposition of sulfates including complex sulfates, e.g. alums
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a heat conducting paste which is mainly prepared from the following components in percentage by mass: 35-80% of base oil and 20-65% of filler. The heat conductive paste of the present invention can provide stable electrical insulation performance and thermal oxidation stability,the heat conductivity is good, and the heat conductivity coefficient can reach 0.26-2.92 W.m‑1·K‑1In particular, when boron nitride or a composition of boron nitride and alumina (having a synergistic effect) is selected as the filler, a sufficient amount of heat conduction channels can be formed in the heat conductive paste, and the heat conductivity can be as high as 2.83-2.92 W.m‑1·K‑1And a good technical effect is obtained.
Description
Technical Field
The invention belongs to the field of electrical materials, and particularly relates to a heat-conducting paste containing aluminum oxide and/or boron nitride and a preparation method thereof.
Background
The high-voltage direct-current transmission technology is usually applied to long-distance electric energy transmission through overhead lines and submarine cables, and has the advantages of strong transmission capacity, small loss, low manufacturing cost and the like compared with the traditional alternating-current transmission technology. In the power transmission process, three-phase alternating current can be converted into direct current at a converter station and output, and a high-voltage thyristor converter valve is a key device in the converter station.
According to the relevant data, the working efficiency of the electronic circuit is reduced along with the increase of the working temperature when the reference temperature is more than 100 ℃. When the electronic device works at 70-80 ℃, the reliability of the working device is reduced by about 5% when the working temperature is increased by 1 ℃. In order to ensure the normal operation of the converter valve, heat generated in the process of alternating current and direct current conversion needs to be timely transmitted to the environment. Air is a poor conductor of heat transfer (thermal conductivity about 0.02 W.m)-1·K-1) The existence of the air layer can lead the heat generated by the electronic element during working not to be conducted out quickly in time, thus leading to the generation of heat accumulation, and the working temperature of the electronic element can be increased continuously, thereby greatly influencing the working stability and the service life of the electronic element. Therefore, a thermal interface material with good thermal conductivity needs to be filled in a gap between a thyristor of a converter valve and a water-cooled radiator, the key point for improving the heat dissipation efficiency is to reduce the thermal contact resistance between a heat source and a heat dissipation device, and in order to achieve the purpose, a material with good thermal conductivity needs to be introduced to fill an air gap between a solid and a solid contact surface so as to achieve the purpose of exhaustingAir is discharged and the thermal resistance is reduced.
At present, the heat conductivity coefficient of the polymer (such as epoxy resin, silicon oil and the like) used as the matrix of the thermal interface material is low, and the heat transfer speed is slow, so that the requirement of actual work and production cannot be met. To address this problem, researchers have begun to look for thermal interface materials with high thermal conductivity.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide the heat-conducting paste containing the alumina and/or the boron nitride and the preparation method thereof, which have good electrical insulation performance, thermal oxidation stability and heat-conducting performance, improve the heat-conducting efficiency and are mainly used for high-voltage direct-current power transmission.
The technical scheme provided by the invention is as follows:
a heat conducting paste is mainly prepared from the following components in percentage by mass: 35-80% of base oil and 20-65% of filler.
Further, in the above-mentioned case,
in any of the above technical schemes, the composition is prepared from the following components in percentage by mass: 35-80% of base oil and 20-65% of filler; preferably, the feed additive is prepared from the following components in percentage by mass: 35-60% of base oil and 40-65% of filler; more preferably, the composition is prepared from the following components in percentage by mass: 40% of base oil and 60% of filler.
Further, in the above-mentioned case,
in any of the above technical solutions, the base oil is selected from silicone oil and/or modified silicone oil; preferably, the base oil is silicone oil, and the silicone oil is selected from methyl silicone oil, ethyl silicone oil, dimethyl silicone oil, phenyl silicone oil, methyl hydrogen-containing silicone oil, methyl phenyl silicone oil, methyl chlorphenyl silicone oil, methyl ethoxy silicone oil, methyl trifluoro propyl silicone oil, methyl vinyl silicone oil, methyl hydroxyl silicone oil, ethyl hydrogen-containing silicone oil, hydroxyl hydrogen-containing silicone oil and/or cyanogen-containing silicone oil.
Further, in the above-mentioned case,
in any of the above embodiments, the filler comprises at least boron nitride; preferably, the filler is boron nitride or a combination of boron nitride and alumina.
Further, in the above-mentioned case,
in any of the above technical solutions, the filler is a composition of boron nitride and alumina, and the mass ratio of boron nitride to alumina is 1: 0.8 to 1.2; preferably, the mass ratio of boron nitride to alumina is 1: 1.
further, in the above-mentioned case,
in any of the above technical solutions, the boron nitride is spherical boron nitride, and the particle size of the spherical boron nitride is 0.5 μm to 12 μm; preferably, the spherical boron nitride has a particle size of 1 μm to 5 μm.
Further, in the above-mentioned case,
in any one of the above technical schemes, the alumina is flake alumina, and the thickness of the flake alumina is 0.1 μm to 5 μm; preferably, the thickness of the tabular alumina is 0.2 to 0.5. mu.m.
The invention also provides a preparation method of the heat-conducting paste, which comprises the following steps: and (3) uniformly mixing the base oil and the filler according to the proportion to prepare the heat conducting paste.
Further, in the above-mentioned case,
in any of the above technical schemes, the base oil and the filler are ground to be uniform, and the heat is preserved for more than 1.5 hours at the temperature of 85-95 ℃.
Further, in the above-mentioned case,
in any of the above embodiments, the filler is selected from boron nitride and/or alumina;
wherein the content of the first and second substances,
the boron nitride is prepared by the following method:
(a1) according to the mass ratio of 1: 0.001-0.01: 15-30, respectively taking boron nitride, a surfactant and water, and uniformly mixing to prepare a solution X;
(a2) according to the mass ratio of 1: 80-150, respectively taking polyvinyl alcohol and water, and heating and dissolving to obtain a solution Y;
(a3) putting the solution X obtained in the step (a1) into a ball mill, ball-milling for at least 18h at the speed of 400 r/min-1000 r/min, adding the solution Y obtained in the step (a2), and continuing ball-milling for at least 18 h; the volume ratio of the solution X to the solution Y is 10: 1;
(a4) spray drying the solution obtained in the step (a3) to prepare boron nitride;
(a5) heating the boron nitride obtained in the step (a4) to 580-650 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for more than 0.8 h;
(a6) heating the boron nitride obtained in the step (a5) to 1000 ℃ at a heating rate of 10 ℃/min, then heating to 1500 ℃ at a heating rate of 5 ℃/min, finally heating to 1750-1850 ℃ at a heating rate of 2 ℃/min, and keeping the temperature for more than 1.5h to obtain the boron nitride;
and/or the presence of a gas in the gas,
the alumina is prepared by the following method:
(b1) according to the mol ratio of 1: 1: 1, respectively taking aluminum sulfate, sodium sulfate and potassium sulfate, adding water until the medicines are completely dissolved, and uniformly mixing to obtain a solution A;
(b2) according to the mass ratio of 1: 1, respectively taking sodium carbonate and trisodium phosphate, and adding water until the medicine is just completely dissolved to prepare a solution B;
(b3) heating the solution A obtained in the step (B1) to 45-60 ℃, and then adding the solution B obtained in the step (B2) to obtain alumina sol;
(b4) drying the alumina sol obtained in the step (b3) at the temperature of 140-160 ℃ to obtain gel;
(b5) and (b) crushing the gel obtained in the step (b4), and sintering at 1200-1600 ℃ for 3.5-8 h to obtain the gel.
The heat-conducting paste provided by the invention not only can provide stable electrical insulation performance and thermal oxidation stability, but also has good heat-conducting performance, and the heat-conducting coefficient can reach 0.26-2.92 W.m-1·K-1In particular, when boron nitride or a composition of boron nitride and alumina (having a synergistic effect) is selected as the filler, a sufficient amount of heat conduction channels can be formed in the heat conductive paste, and the heat conductivity can be as high as 2.83-2.92 W.m-1·K-1And a good technical effect is obtained.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
Drawings
FIG. 1 is a scanning electron micrograph of the flaky alumina obtained in example 1 of the present invention;
FIG. 2 is a transmission electron micrograph of the flaky alumina obtained in example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of spherical boron nitride obtained in example 4 of the present invention;
FIG. 4 is a graph showing a distribution of the particle size of spherical boron nitride obtained in example 4 of the present invention.
Detailed Description
While the present invention will be described more fully hereinafter with reference to the accompanying specific embodiments, it is to be understood by those skilled in the art that the following descriptions are provided for purposes of illustration only and are not intended to limit the scope of the present invention.
In the present invention, those who do not specify specific conditions are performed according to conventional conditions or conditions recommended by the manufacturer, and those who do not specify the reagents or instruments used are conventional products commercially available.
Example 1
The heat conducting paste is prepared from the following components in percentage by mass: 80% of dimethyl silicone oil and 20% of flaky alumina;
the preparation method comprises the following steps:
(1) weighing 1 mol of aluminum sulfate, 1 mol of sodium sulfate and 1 mol of potassium sulfate respectively, and adding deionized water according to the solubility until the medicines are just completely dissolved to prepare a solution A;
(2) 60.589g of sodium carbonate and 0.783g of trisodium phosphate are weighed, and deionized water is added according to the solubility of sodium carbonate and trisodium phosphate until the medicaments are completely dissolved to prepare solution B;
(3) heating the solution A in a water bath to about 50 ℃, and slowly adding the solution B into the solution A to obtain hydrated alumina sol;
(4) drying the sol prepared in the step (3) in a drying oven at 150 ℃ to obtain gel;
(5) putting the gel prepared in the step (4) into a planetary ball mill for further crushing, then putting into a tubular furnace, and sintering for 5 hours at 1400 ℃ to prepare the flaky alumina filler, wherein the scanning electron microscope image and the transmission electron microscope image of the flaky alumina filler are respectively shown in the figures 1 and 2;
(6) mixing dimethyl silicone oil with flake aluminum oxide at a mass ratio of 80% to 20%, grinding to uniformity, placing into an oven, keeping the temperature at 90 deg.C for 2h, vacuumizing, testing the heat conductivity, and measuring the heat conductivity coefficient to be 0.26 W.m-1·K-1。
Example 2
The same parts of the thermal conductive paste of the invention as the embodiment 1 are not described again, but the mixture ratio is changed to be made of the following components by mass percent: 60% of dimethyl silicone oil and 40% of flaky alumina; the thermal conductivity was found to be 0.41 W.m-1·K-1。
Example 3
The same parts of the thermal conductive paste of the invention as the embodiment 1 are not described again, but the mixture ratio is changed to be made of the following components by mass percent: 40% of dimethyl silicone oil and 60% of flaky alumina; measured thermal conductivity coefficient of 0.66 W.m-1·K-1。
Example 4
The heat conducting paste is prepared from the following components in percentage by mass: 80% of dimethyl silicone oil and 20% of spherical boron nitride;
the preparation method comprises the following steps:
(1) weighing 3g of boron nitride powder, putting the boron nitride powder into a ball milling tank, adding 100mL of deionized water, and then adding 0.025g of SDBS (sodium dodecyl benzene sulfonate) to prepare a solution X;
(2) weighing 0.1g of PVA (polyvinyl alcohol) solid and 30mL of deionized water, putting the solid into a round-bottom flask, and stirring the solid and the deionized water in an oil bath kettle at the temperature of 80 ℃ until the solid and the deionized water are dissolved to prepare solution Y;
(3) putting the solution X in the step (1) into a ball milling tank, then putting the ball milling tank into a planetary ball mill, carrying out ball milling at the speed of 600r/min for 24 hours, then putting 5mL of solution Y, and continuing ball milling for 24 hours;
(4) spray drying the solution in the step (3) by using a spray dryer to prepare spherical boron nitride powder;
(5) placing the spherical boron nitride in the step (4) in a crucible, and preserving the heat for 1h in a muffle furnace at the temperature of 600 ℃, wherein the heating rate is 5 ℃/min;
(6) placing the spherical boron nitride in the step (5) in a porcelain boat, and preserving heat for 2h in a tubular furnace at 1800 ℃, wherein the heating rate is as follows: 10 ℃/min below 1000 ℃, 5 ℃/min at 1000-1500 ℃, 2 ℃/min at 1500-1800 ℃, and the scanning electron microscope picture and the particle size distribution picture are respectively shown in figure 3 and figure 4;
(7) mixing the dimethyl silicone oil with the spherical boron nitride in the step (6) according to the mass fraction of 80% and 20%, grinding the mixture to be uniform, putting the mixture into an oven, keeping the temperature for 2 hours at 90 ℃, testing the heat conductivity after vacuumizing, and measuring the heat conductivity coefficient to be 0.58 W.m-1·K-1。
Example 5
The same parts of the thermal conductive paste as embodiment 4 are not described again, but the thermal conductive paste is prepared from the following components in percentage by mass: 60% of dimethyl silicone oil and 40% of spherical boron nitride; the thermal conductivity coefficient is measured to be 1.78 W.m-1·K-1。
Example 6
The same parts of the thermal conductive paste as embodiment 4 are not described again, but the thermal conductive paste is prepared from the following components in percentage by mass: 40% of dimethyl silicone oil and 60% of spherical boron nitride; the thermal conductivity was found to be 2.83 W.m-1·K-1。
Example 7
The same parts of the heat-conducting paste disclosed by the invention as those in the embodiments 1 and 4 are not described again, but the heat-conducting paste is prepared from the following components in percentage by mass: 40% of dimethyl silicone oil, 30% of spherical boron nitride and 30% of flake aluminum oxide; measured thermal conductivity coefficient of 2.92 W.m-1·K-1。
The result shows that the heat-conducting paste provided by the invention takes the dimethyl silicone oil as the base oil, can provide stable electrical insulation performance and thermal oxidation stability, has good heat-conducting performance, and can reach the heat-conducting coefficient of 0.26-2.92 W.m-1·K-1In particular, boron nitride or a combination of boron nitride and alumina (having a synergistic effect) is selected as the filler, and sufficient thermal conductivity can be formed in the thermal pasteThe heat conductivity coefficient of the channel can reach 2.83-2.92 W.m-1·K-1And a good technical effect is obtained.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it is therefore intended that all such changes and/or modifications be considered within the scope of the appended claims.
Claims (10)
1. The heat conducting paste is characterized by being mainly prepared from the following components in percentage by mass: 35-80% of base oil and 20-65% of filler.
2. The heat conducting paste as claimed in claim 1, which is prepared from the following components in percentage by mass: 35-80% of base oil and 20-65% of filler; preferably, the feed additive is prepared from the following components in percentage by mass: 35-60% of base oil and 40-65% of filler; more preferably, the composition is prepared from the following components in percentage by mass: 40% of base oil and 60% of filler.
3. The thermal conductive paste according to claim 1 or 2, wherein the base oil is selected from silicone oil and/or modified silicone oil; preferably, the base oil is silicone oil, and the silicone oil is selected from methyl silicone oil, ethyl silicone oil, dimethyl silicone oil, phenyl silicone oil, methyl hydrogen-containing silicone oil, methyl phenyl silicone oil, methyl chlorphenyl silicone oil, methyl ethoxy silicone oil, methyl trifluoro propyl silicone oil, methyl vinyl silicone oil, methyl hydroxyl silicone oil, ethyl hydrogen-containing silicone oil, hydroxyl hydrogen-containing silicone oil and/or cyanogen-containing silicone oil.
4. The thermal paste according to claim 1 or 2, wherein the filler contains at least boron nitride; preferably, the filler is boron nitride or a combination of boron nitride and alumina.
5. The paste as claimed in claim 4, wherein the filler is a composition of boron nitride and alumina, and the mass ratio of boron nitride to alumina is 1: 0.8 to 1.2; preferably, the mass ratio of boron nitride to alumina is 1: 1.
6. the paste as claimed in claim 4, wherein the boron nitride is spherical boron nitride having a particle size of 0.5 to 12 μm; preferably, the spherical boron nitride has a particle size of 1 μm to 5 μm.
7. The paste as claimed in claim 4, wherein the alumina is a plate-like alumina having a thickness of 0.1 to 5 μm; preferably, the thickness of the tabular alumina is 0.2 to 0.5. mu.m.
8. The method for preparing the thermal conductive paste according to any one of claims 1 to 7, comprising the steps of: and (3) uniformly mixing the base oil and the filler according to the proportion to prepare the heat conducting paste.
9. The method according to claim 8, wherein the base oil and the filler are ground to be uniform and the temperature is maintained at 85-95 ℃ for more than 1.5 h.
10. The method according to claim 8, wherein the filler is selected from boron nitride and/or alumina;
wherein the content of the first and second substances,
the boron nitride is prepared by the following method:
(a1) according to the mass ratio of 1: 0.001-0.01: 15-30, respectively taking boron nitride, a surfactant and water, and uniformly mixing to prepare a solution X;
(a2) according to the mass ratio of 1: 80-150, respectively taking polyvinyl alcohol and water, and heating and dissolving to obtain a solution Y;
(a3) putting the solution X obtained in the step (a1) into a ball mill, ball-milling for at least 18h at the speed of 400 r/min-1000 r/min, adding the solution Y obtained in the step (a2), and continuing ball-milling for at least 18 h; the volume ratio of the solution X to the solution Y is 10: 1;
(a4) spray drying the solution obtained in the step (a3) to prepare boron nitride;
(a5) heating the boron nitride obtained in the step (a4) to 580-650 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for more than 0.8 h;
(a6) heating the boron nitride obtained in the step (a5) to 1000 ℃ at a heating rate of 10 ℃/min, then heating to 1500 ℃ at a heating rate of 5 ℃/min, finally heating to 1750-1850 ℃ at a heating rate of 2 ℃/min, and keeping the temperature for more than 1.5h to obtain the boron nitride;
and/or the presence of a gas in the gas,
the alumina is prepared by the following method:
(b1) according to the mol ratio of 1: 1: 1, respectively taking aluminum sulfate, sodium sulfate and potassium sulfate, adding water until the medicines are just dissolved, and uniformly mixing to prepare a solution A;
(b2) according to the mass ratio of 80: 1, respectively dissolving sodium carbonate, trisodium phosphate and water to prepare a solution B;
(b3) heating the solution A obtained in the step (B1) to 45-60 ℃, and then adding the solution B obtained in the step (B2) to obtain alumina sol;
(b4) drying the alumina sol obtained in the step (b3) at the temperature of 140-160 ℃ to obtain gel;
(b5) and (b) crushing the gel obtained in the step (b4), and sintering at 1200-1600 ℃ for 3.5-8 h to obtain the gel.
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