CN114958004B - Organic silicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, and preparation process and application thereof - Google Patents
Organic silicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, and preparation process and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 230000015556 catabolic process Effects 0.000 title claims abstract description 41
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 105
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 101
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 83
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229920001971 elastomer Polymers 0.000 claims abstract description 26
- 239000000806 elastomer Substances 0.000 claims abstract description 26
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 19
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 18
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 17
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 17
- 230000002378 acidificating effect Effects 0.000 claims abstract description 15
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 34
- 235000019441 ethanol Nutrition 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 16
- 239000000413 hydrolysate Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000009849 vacuum degassing Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 238000006459 hydrosilylation reaction Methods 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 description 33
- 238000006460 hydrolysis reaction Methods 0.000 description 33
- 239000000945 filler Substances 0.000 description 28
- 230000004048 modification Effects 0.000 description 23
- 238000012986 modification Methods 0.000 description 23
- 239000011159 matrix material Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000007822 coupling agent Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 102220064253 rs779277447 Human genes 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- MDLRQEHNDJOFQN-UHFFFAOYSA-N methoxy(dimethyl)silicon Chemical group CO[Si](C)C MDLRQEHNDJOFQN-UHFFFAOYSA-N 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 239000012258 stirred mixture Substances 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000007872 degassing Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000000051 modifying effect Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 239000004643 cyanate ester Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Polymers C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920003192 poly(bis maleimide) Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
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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
- C08K3/34—Silicon-containing compounds
-
- 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
- C08K3/28—Nitrogen-containing compounds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides an organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, which comprises the following preparation raw materials in percentage by mass: vinyl-terminated polydimethylsiloxane: 35-40%; crosslinking agent: 35-40%; modified micron silicon carbide: 18-22%; modified nano aluminum nitride: 0.1 to 5 percent; the modified micron silicon carbide is prepared by hydrolyzing micron silicon carbide and a silane coupling agent KH570 in an acidic alcohol water solution; the modified nano aluminum nitride is prepared by hydrolyzing nano aluminum nitride and a silane coupling agent KH570 in an acidic alcohol water solution. The modified nano aluminum nitride is added into the organic silicon elastomer/micron silicon carbide composite material, so that the nonlinear conductivity characteristic and the breakdown characteristic of the composite material can be improved. The invention also provides a preparation method and application of the organic silicon elastomer composite material with high nonlinear conductivity and breakdown characteristics.
Description
Technical Field
The invention belongs to the technical field of electronic packaging materials, and particularly relates to an organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, and a preparation process and application thereof.
Background
The active metal brazing process in high temperature and high pressure silicon carbide module packages is prone to producing metal bumps at the bottom of the module metallization layer, i.e., three bond points of the aluminum nitride ceramic substrate, the copper metallization layer and the packaging material. The high field strength created by such metal bump triple junction at high voltage is prone to produce partial discharge in the module, resulting in insulation degradation and even module failure. The nonlinear conductive material can uniformly generate high field intensity at three bonding points, so that partial discharge in a module packaging structure is inhibited, and the safety and reliability of the silicon carbide module in long-term operation under high-temperature and high-pressure environments are improved.
The silicone elastomer (silicone elastomer, SE) can operate for long periods at 250 ℃ because it has a high dissociation energy and a low energy barrier to rotation of siloxane bonds. In addition, silicone elastomers have lower storage modulus and hardness compared to other high temperature materials (e.g., polyimide, bismaleimide, and cyanate esters). This can effectively limit mechanical stresses in the package structure caused by Coefficient of Thermal Expansion (CTE) mismatch. Furthermore, silicone elastomers have excellent viscosity during potting (i.e., filling) and do not undergo volume shrinkage during curing. Therefore, silicone elastomers are a promising encapsulating material for high temperature applications.
In various studies, semiconducting fillers, such as silicon carbide (SiC), were added to silicone elastomer matrices to achieve nonlinear conductivity properties. However, it was found that as the semiconductive filler content increased, the breakdown strength rapidly decreased, although the nonlinear conductivity characteristic increased. This can lead to significant partial discharge and even device breakdown. On the other hand, when the semiconductive filler content is reduced, the nonlinear conductivity is impaired although the breakdown strength is increased, so that it is difficult to effectively reduce the local high electric field. Therefore, it is necessary to improve both the nonlinear conductivity and the breakdown strength.
Disclosure of Invention
The invention aims to provide an organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, a preparation process and application thereof.
The invention provides an organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, which comprises the following preparation raw materials in percentage by mass:
Vinyl-terminated polydimethylsiloxane: 35-40%; crosslinking agent: 35-40%; modified micron silicon carbide: 18-22%; modified nano aluminum nitride: 0.1 to 5 percent;
The modified micron silicon carbide is prepared by hydrolyzing micron silicon carbide and a silane coupling agent KH570 in an acidic alcohol water solution;
The modified nano aluminum nitride is prepared by hydrolyzing nano aluminum nitride and a silane coupling agent KH570 in an acidic alcohol water solution.
Preferably, the crosslinking agent is dimethyl-methyl hydrogen siloxane.
Preferably, the average diameter of the micrometer silicon carbide is 5-20 mu m, and the density is 3.0-3.5 g/cm 3; the average diameter of the nano aluminum nitride is 80-200 nm, and the density is 3.2-3.8 g/cm 3.
The present invention provides a process for preparing a silicone elastomer composite having both high nonlinear electrical conductivity and breakdown characteristics as described above, comprising the steps of:
a) Mixing water, a silane coupling agent KH570 and absolute ethyl alcohol to obtain an ethanol solution of the silane coupling agent, and then adjusting the pH value of the ethanol solution of the silane coupling agent to 2.9-3.1, and hydrolyzing for 1.8-2.2 hours at room temperature to obtain a hydrolysate;
B) Dispersing micrometer silicon carbide or nanometer aluminum nitride in absolute ethyl alcohol to obtain a dispersion liquid, mixing the hydrolysate with the dispersion liquid, and stirring to obtain a stirring liquid;
c) Centrifuging the stirring liquid, washing and drying the centrifuged solid to obtain modified micrometer silicon carbide or modified nanometer aluminum nitride;
D) Mixing modified micrometer silicon carbide and modified nanometer aluminum nitride with vinyl end-capped polydimethylsiloxane, performing ultrasonic treatment, then mixing with a cross-linking agent, and stirring to obtain a mixture;
E) And (3) carrying out vacuum degassing and curing on the mixture to obtain the organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics.
Preferably, in the step a), the mass ratio of the absolute ethyl alcohol, the silane coupling agent KH570 and the water is (5 to 10): (1-3): 1.
Preferably, in the step B), the mass ratio of the micro silicon carbide or nano aluminum nitride to the absolute ethyl alcohol is (0.9-1.1): 1.
Preferably, the mass ratio of the micro silicon carbide or nano aluminum nitride to the silane coupling agent KH570 is (24-26): 1.
Preferably, the stirring temperature in the step B) is 50-80 ℃, the stirring time is 3-5 hours, and the stirring rotating speed is 300-600 r/min.
Preferably, the curing in the step E) is specifically:
The mixture after vacuum degassing is pre-cured for 0.5 to 2 hours at 78 to 82 ℃ and then cured for 3.9 to 4.1 hours at 198 to 202 ℃.
The present invention provides for the use of a silicone elastomer composite having both high nonlinear conductivity and breakdown characteristics as described above in power electronics high power device packages.
The invention provides an organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, which comprises the following preparation raw materials in percentage by mass: vinyl-terminated polydimethylsiloxane: 35-40%; crosslinking agent: 35-40%; modified micron silicon carbide: 18-22%; modified nano aluminum nitride: 0.1 to 5 percent; the modified micron silicon carbide is prepared by hydrolyzing micron silicon carbide and a silane coupling agent KH570 in an acidic alcohol water solution; the modified nano aluminum nitride is prepared by hydrolyzing nano aluminum nitride and a silane coupling agent KH570 in an acidic alcohol water solution. The method for modifying the micro-silicon carbide and the nano-aluminum nitride by using the silane coupling agent modified KH570 can ensure that the surface-modified micro-silicon carbide and nano-aluminum nitride are uniformly distributed in the organosilicon elastomer, obvious agglomeration and deposition phenomena are avoided, and the compatibility between the micro-nano filler modified KH570 and the organosilicon elastomer matrix is better. According to the invention, nano aluminum nitride is added into the organic silicon elastomer/micron silicon carbide composite material, so that the nonlinear conductivity and the breakdown characteristic of the composite material can be improved, and the optimal effect of improving the nonlinear conductivity and the breakdown characteristic can be achieved by doping a proper amount of nano aluminum nitride.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a reaction mechanism for preparing a silicone elastomer composite of the present invention having both high nonlinear electrical conductivity and breakdown characteristics;
FIG. 2 is a graph showing the average modification rates of modified micron silicon carbide at different pH values in the present invention;
FIG. 3 is a graph showing the average modification rates of modified micron silicon carbide at different hydrolysis temperatures in the present invention;
FIG. 4 is a graph showing the average modification rates of modified micron silicon carbide at different hydrolysis times in the present invention;
FIG. 5 shows the dispersion of KH570 modified micro-SiC filler (20 wt%) of comparative example 1 of the present invention on the cross section of a silicone elastomer composite;
FIG. 6 shows the dispersion of KH560 modified micro-SiC filler (20 wt%) of comparative example 2 of the present invention on the cross section of a silicone elastomer composite;
FIG. 7 is a graph showing nonlinear conductivity characteristics of silicone elastomer composite samples of examples 1-3 according to the present invention;
Fig. 8 is a graph showing dc breakdown field strength of the silicone elastomer composite samples of examples 1 to 3 according to the present invention.
Detailed Description
The invention provides an organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, which comprises the following preparation raw materials in percentage by mass:
Vinyl-terminated polydimethylsiloxane: 35-40%; crosslinking agent: 35-40%; modified micron silicon carbide: 18-22%; modified nano aluminum nitride: 0.1 to 5 percent;
The modified micron silicon carbide is prepared by hydrolyzing micron silicon carbide and a silane coupling agent KH570 in an acidic alcohol water solution;
The modified nano aluminum nitride is prepared by hydrolyzing nano aluminum nitride and a silane coupling agent KH570 in an acidic alcohol water solution.
In the present invention, the mass fraction of the vinyl-terminated polydimethylsiloxane is preferably 35 to 40%, more preferably 36 to 39%, such as 35%,35.5%,36%,36.5%,37%,37.5%,38%,38.5%,39%,39.5%,40%, preferably a range having any of the above values as an upper limit or a lower limit.
The crosslinking agent is preferably dimethyl-methylhydrosiloxane, and the mass fraction of the crosslinking agent is preferably 35 to 40%, more preferably 36 to 39%, such as 35%,35.5%,36%,36.5%,37%,37.5%,38%,38.5%,39%,39.5%,40%, preferably a range value having any of the above values as an upper limit or a lower limit.
In the present invention, the mass ratio of the vinyl-terminated polydimethylsiloxane to the crosslinking agent is preferably 1: (0.9 to 1.1), more preferably 1:1.
In the invention, the modified micron silicon carbide is prepared by hydrolyzing micron silicon carbide and a silane coupling agent KH570 in an acidic alcohol water solution. The average diameter of the micrometer silicon carbide is 5-20 μm, more preferably 10-15 μm, and the density is 3.0-3.5 g/cm 3, more preferably 3.2-3.3 g/cm 3.
The modified nano aluminum nitride is prepared by hydrolyzing nano aluminum nitride and a silane coupling agent KH570 in an acidic alcohol water solution, wherein the average diameter of the nano aluminum nitride is preferably 80-200 nm, more preferably 100-150 nm, and the density is 3.2-3.8 g/cm 3, more preferably 3.4-3.5 g/cm 3.
The invention also provides a preparation process of the organic silicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, which comprises the following steps:
A) Mixing water, a silane coupling agent KH570 and absolute ethyl alcohol to obtain an ethanol solution, adjusting the pH value of the ethanol solution to 2.9-3.1, and hydrolyzing for 1.8-2.2 hours at room temperature to obtain a hydrolysate;
B) Dispersing micrometer silicon carbide or nanometer aluminum nitride in absolute ethyl alcohol to obtain a dispersion liquid, mixing the hydrolysate with the dispersion liquid, and stirring to obtain a stirring liquid;
c) Centrifuging the stirring liquid, washing and drying the centrifuged solid to obtain modified micrometer silicon carbide or modified nanometer aluminum nitride;
D) Mixing modified micrometer silicon carbide and modified nanometer aluminum nitride with vinyl end-capped polydimethylsiloxane, performing ultrasonic treatment, then mixing with a cross-linking agent, and stirring to obtain a mixture;
E) And (3) carrying out vacuum degassing and curing on the mixture to obtain the organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics.
The invention firstly modifies the micrometer silicon carbide and the nanometer aluminum nitride, and then dopes the modified micrometer silicon carbide and the modified nanometer aluminum nitride to the double-component organic silicon elastomer.
In the invention, water, a silane coupling agent KH570 and absolute ethyl alcohol are preferably mixed to obtain an ethanol solution of the silane coupling agent, then hydrochloric acid is used for adjusting the pH value of the ethanol solution of the silane coupling agent to 2.9-3.1, preferably 3.0, and hydrolysis is carried out for 1.8-2.2 hours at room temperature to obtain a hydrolysate. The step mainly comprises the step of hydrolyzing the silane coupling agent KH570 in the acidic environment of the hydrolysate to form silanol, wherein the reaction mechanism is shown as step ① in figure 1.
In the invention, the water is preferably deionized water, and the mass ratio of the absolute ethyl alcohol to the silane coupling agent KH570 to the water is preferably (5-10): (1-3): 1, more preferably (6 to 9): (1-2): 1, most preferably (7 to 8): (1-2): 1. wherein the mass fraction of the silane coupling agent KH570 in the hydrolysate is preferably 18-19 wt%.
In the present invention, the hydrolysis process directly affects the modifying effect of the filler, thereby indirectly affecting the properties of the silicone elastomer composite. If the PH value is too high, the hydrolysis rate of KH570 is too low, and KH570 cannot be fully hydrolyzed, so that the modification effect of the filler is reduced; if the PH is too low, the rate of hydrolysis of KH570 becomes too high, and the hydrolyzed PH570 tends to condense to form macromolecular floccules, which makes it impossible to effectively modify the filler, resulting in a decrease in the modification rate of the filler.
If the hydrolysis temperature is too high, KH570 is easy to decompose or self-polymerize, so that the coupling effect is lost, and the filler cannot be effectively modified; if the hydrolysis temperature is too low, the hydrolysis rate of KH570 is too low and the modification efficiency is lower. If the hydrolysis time is too short, KH570 cannot be sufficiently hydrolyzed; if the hydrolysis time is too long, the KH570 hydrolysis product is obviously condensed, so that the modification effect of the KH570 hydrolysis product on the filler is reduced. In the present invention, the temperature of the hydrolysis is preferably 20 to 30 ℃, more preferably 25 to 28 ℃, and the time of the hydrolysis is preferably 1.8 to 2.2 hours, more preferably 1.9 to 2.1 hours, and most preferably 2 hours.
Therefore, the selection of appropriate pH, hydrolysis temperature and hydrolysis time is significant for successful modification of filler surfaces and even for determining composite properties.
The invention mixes the dried micrometer silicon carbide or the dried nanometer aluminum nitride with absolute ethyl alcohol to obtain dispersion liquid. In the invention, the preparation of the dispersion liquid and the hydrolysate of the silane coupling agent is not sequential, and the preparation sequence can be selected according to the requirement.
In the present invention, the drying temperature of the micro silicon carbide is preferably 115 to 125 ℃, such as 115 ℃,116 ℃,117 ℃,118 ℃,119 ℃,120 ℃,121 ℃,122 ℃,123 ℃,124 ℃,125 ℃, preferably a range value with any of the above values as an upper limit or a lower limit; the drying time of the micro silicon carbide is preferably 23.8 to 24.2 hours, such as 23.8 hours, 23.9 hours, 24 hours, 24.1 hours, 24.2 hours, and preferably a range value having any of the above values as an upper limit or a lower limit.
In the present invention, the drying temperature of the nano aluminum nitride is preferably 115 to 125 ℃, such as 115 ℃,116 ℃,117 ℃,118 ℃,119 ℃,120 ℃,121 ℃,122 ℃,123 ℃,124 ℃,125 ℃, preferably a range value with any of the above values as an upper limit or a lower limit; the drying time of the nano aluminum nitride is preferably 23.8 to 24.2 hours, for example, 23.8 hours, 23.9 hours, 24 hours, 24.1 hours, 24.2 hours, and preferably a range value having any of the above values as an upper limit or a lower limit.
In the present invention, the mass ratio of the dried micro silicon carbide or the dried nano aluminum nitride to the absolute ethanol is preferably (0.9 to 1.1): 1, more preferably 1:1.
And then pouring the hydrolysate of the silane coupling agent into the dispersion liquid, stirring in a constant-temperature water bath, and performing condensation reaction to obtain a stirring liquid. This step is the hydrolysis of the micro silicon carbide or micro aluminum nitride and the condensation reaction between the hydrolyzed silicon carbide and aluminum nitride and the hydrolyzed silane coupling agent KH570, as shown in steps ② and ③ in fig. 1.
In the invention, the mass ratio of the micro silicon carbide or nano aluminum nitride to the silane coupling agent KH570 is preferably (24-26): 1, more preferably 25:1. The stirring temperature is preferably 50 to 80 ℃, more preferably 60 to 70 ℃, such as 50 ℃,55 ℃,60 ℃,65 ℃,70 ℃,75 ℃,80 ℃, preferably a range value with any of the above values as an upper limit or a lower limit; the stirring time is preferably 3 to 5 hours, more preferably 3 to 4 hours, and the stirring rotation speed is preferably 300 to 600r/min, more preferably 400 to 500r/min.
And then placing the obtained stirring liquid into a centrifugal machine for centrifugal treatment, and washing by using absolute ethyl alcohol and deionized water in sequence.
In the present invention, the rotational speed of the centrifugal treatment is preferably 2000 to 3000r/min, more preferably 2200 to 2800r/min, and most preferably 2500 to 2600r/min.
And finally, placing the washed solution into a vacuum drying device for drying to obtain the modified micrometer silicon carbide or the modified nanometer aluminum nitride.
In the present invention, the drying temperature is preferably 128 to 132 ℃, such as 128 ℃,129 ℃,130 ℃,131 ℃,132 ℃, preferably a range value in which any of the above values is an upper limit or a lower limit; the drying time is preferably 1.8 to 2.2 hours, more preferably 1.9 to 2.1 hours, and most preferably 2 hours.
After the modified micro silicon carbide and the modified nano aluminum nitride are obtained, the modified micro silicon carbide and the modified nano aluminum nitride are doped in the double-component organic silicon elastomer, and the modified micro silicon carbide and the modified nano aluminum nitride undergo a hydrosilylation reaction with an organic silicon elastomer matrix, as shown in step ④ in fig. 1.
Preferably, the modified micron silicon carbide is firstly mixed with vinyl-terminated Polydimethylsiloxane (PDMS), and then mixed with the cross-linking agent after ultrasonic treatment, and the mixture is obtained by stirring.
In the present invention, the types and amounts of the raw materials are the same as those described above, and the present invention is not described herein.
In the present invention, the time of the ultrasonic treatment is preferably 29 to 31 minutes, more preferably 30 minutes; the stirring time is preferably 0.9 to 1.1 hours, more preferably 1 hour.
The resulting mixture is stirred and degassed in a vacuum oven and then poured into a mold for curing.
In the present invention, the time for the vacuum degassing is preferably 28 to 32 minutes, more preferably 29 to 31 minutes, and most preferably 30 minutes.
The curing is preferably performed at a low temperature and then at a high temperature; the temperature of the pre-curing is preferably 78-82 ℃, such as 78 ℃,79 ℃,80 ℃,81 ℃,82 ℃, preferably a range value with any of the above values as an upper or lower limit; the time for the pre-curing is preferably 0.5 to 2 hours, more preferably 1 to 1.5 hours; the curing temperature is preferably 198 to 202 ℃, such as 198 ℃,199 ℃,200 ℃,201 ℃,202 ℃, preferably a range value with any of the above values as an upper or lower limit; the curing time is preferably 3.9 to 4.1 hours, more preferably 4 hours.
And then placing the cured material in a vacuum oven for vacuum degassing for 0.9-1.1 hours, more preferably 1 hour, and removing residual impurities to obtain the organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics.
The invention also provides application of the organic silicon elastomer composite material with high nonlinear conductivity and breakdown characteristics in power electronic high-power device packaging.
The invention provides an organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, which comprises the following preparation raw materials in percentage by mass: vinyl-terminated polydimethylsiloxane: 35-40%; crosslinking agent: 35-40%; modified micron silicon carbide: 18-22%; modified nano aluminum nitride: 0.1 to 5 percent; the modified micron silicon carbide is prepared by hydrolyzing micron silicon carbide and a silane coupling agent KH570 in an acidic alcohol water solution; the modified nano aluminum nitride is prepared by hydrolyzing nano aluminum nitride and a silane coupling agent KH570 in an acidic alcohol water solution. The method for modifying the micro-silicon carbide and the nano-aluminum nitride by using the silane coupling agent modified KH570 can ensure that the surface-modified micro-silicon carbide and nano-aluminum nitride are uniformly distributed in the organosilicon elastomer, obvious agglomeration and deposition phenomena are avoided, and the compatibility between the micro-nano filler modified KH570 and the organosilicon elastomer matrix is better. According to the invention, nano aluminum nitride is added into the organic silicon elastomer/micron silicon carbide composite material, so that the nonlinear conductivity and the breakdown characteristic of the composite material can be improved, and the optimal effect of improving the nonlinear conductivity and the breakdown characteristic can be achieved by doping a proper amount of nano aluminum nitride.
In order to further illustrate the present invention, the following examples are provided to describe in detail a silicone elastomer composite having both high nonlinear conductivity and breakdown characteristics, its preparation process and application, but should not be construed as limiting the scope of the present invention.
Experimental materials: the A-component (vinyl terminated polydimethylsiloxane, PDMS) and the B-component (dimethyl-methylhydrosiloxane, crosslinker) of the two-component silicone elastomer are provided by Shenzhen Hasuncast, inc. Mixing ratio: part a/part B = 1/1 (by weight). The average diameter of the micrometer silicon carbide is 10 mu m, the density is 3.2g/cm 3, the average diameter of the nanometer aluminum nitride is 100nm, the density is 3.5g/cm 3, and the micrometer silicon carbide and the nanometer aluminum nitride are provided by Shanghai microphone Lin Shenghua Co., ltd.
Example 1
First, 50g of micrometer silicon carbide was placed in a vacuum oven at 120℃and dried continuously for 24 hours.
2G of deionized water, 4g of silane coupling agent KH570 and 16g of absolute ethyl alcohol are taken to prepare an ethanol solution of the coupling agent. The pH value of the ethanol solution of the coupling agent is adjusted to 3 by hydrochloric acid, and the coupling agent is hydrolyzed for 2 hours at room temperature to obtain hydrolysate.
50G of dried micrometer silicon carbide and 50g of absolute ethyl alcohol are dispersed in a beaker for 1h to prepare a dispersion liquid, the hydrolysate is poured into the dispersion liquid, and the mixture is stirred in a constant-temperature water bath for 4h at 60 ℃ and 500r/min to obtain a stirring liquid.
And (3) placing the stirring solution into a centrifugal machine for centrifugal treatment, wherein the centrifugal rotation speed is 2500r/min, and then repeatedly washing the stirring solution twice by respectively taking 100g of absolute ethyl alcohol and deionized water.
Finally, the washed solution is placed in a vacuum drying oven and dried for 2 hours at 130 ℃ to obtain the micron silicon carbide after surface modification.
Example 2
Firstly, 50g of nano aluminum nitride is placed in a vacuum drying oven at 120 ℃ and continuously dried for 24 hours.
2G of deionized water, 4g of silane coupling agent KH570 and 16g of absolute ethyl alcohol are taken to prepare an ethanol solution of the coupling agent. The pH value of the ethanol solution of the coupling agent is adjusted to 3 by hydrochloric acid, and the coupling agent is hydrolyzed for 2 hours at room temperature to obtain hydrolysate.
50G of dried nano aluminum nitride and 50g of absolute ethyl alcohol are dispersed in a beaker for 1h to prepare a dispersion liquid, the hydrolysate is poured into the dispersion liquid, and the mixture is stirred in a constant-temperature water bath for 4h at 60 ℃ and 500r/min to obtain a stirring liquid.
And (3) placing the stirring solution into a centrifugal machine for centrifugal treatment, wherein the centrifugal rotation speed is 2500r/min, and then repeatedly washing the stirring solution twice by respectively taking 100g of absolute ethyl alcohol and deionized water.
Finally, placing the washed solution in a vacuum drying oven, and drying for 2 hours at 130 ℃ to obtain the nano aluminum nitride with the surface modified.
Example 1 organosilicon elastomer/micro silicon carbide/nano aluminum nitride composite doped with 20wt% micro silicon carbide and 1wt% nano aluminum nitride (S20N 1)
(A) Mixing 20wt% of the modified micro silicon carbide of example 1, 1wt% of the modified nano aluminum nitride of example 2 with 39.5wt% of a component PDMS substrate, and performing ultrasonic treatment for 30min;
(b) Mixing the mixture after ultrasonic treatment with 39.5wt% of a component B dimethyl-methyl hydrogen siloxane cross-linking agent, and mechanically stirring for 1h;
(d) The stirred mixture was degassed in a vacuum oven for 30min, then poured into a mold, pre-cured at 80 ℃ for 1 hour, post-cured at 200 ℃ for 4 hours, then the sample was placed in the vacuum oven for degassing for 1 hour and residual impurities were removed to obtain a silicone elastomer/micro silicon carbide/nano aluminum nitride composite material doped with 20wt% micro silicon carbide and 1wt% nano aluminum nitride (S20N 1).
Example 2 organosilicon elastomer/micro silicon carbide/nano aluminum nitride composite doped with 20wt% micro silicon carbide and 3wt% nano aluminum nitride (S20N 3)
(A) Mixing 20wt% of the modified micro silicon carbide of example 1, 3wt% of the modified nano aluminum nitride of example 2 with 38.5wt% of a component PDMS substrate, and performing ultrasonic treatment for 30min;
(b) Mixing the mixture after ultrasonic treatment with 38.5wt% of a B component dimethyl-methyl hydrogen siloxane cross-linking agent, and mechanically stirring for 0.9-1.1 h;
(d) The stirred mixture was degassed in a vacuum oven for 30min, then poured into a mold, pre-cured at 80 ℃ for 1 hour, post-cured at 200 ℃ for 4 hours, then the sample was placed in the vacuum oven for degassing for 1 hour and residual impurities were removed to obtain a silicone elastomer/micro silicon carbide/nano aluminum nitride composite material doped with 20wt% micro silicon carbide and 3wt% nano aluminum nitride (S20N 3).
Average modification rate
The KH570 hydrolysis effect is indirectly reacted through the modification effect of the average modification rate on the micron SiC filler by directly reacting the KH570 after hydrolysis. The average modification ratio is defined as follows:
After the KH570 is successfully modified by hydrolysis, the surface of the filler is changed from polarity to non-polarity, the modified filler shows stronger hydrophobicity to water and can float on the water surface instead of sinking to the water bottom, so that the modification rate can be defined as follows: the larger the modification rate, the better the modification effect of the filler. The average modification ratio is the average value of the results obtained from 3 sets of repeated modification ratio test experiments under the same hydrolysis condition.
According to the preparation method in example 1, the hydrolysis temperature was kept at room temperature (25 ℃) for 2 hours, and the pH of the hydrolysate was adjusted to 2, 2.5, 3, 3.5 and 4 by hydrochloric acid, respectively, and the average modification ratio (micron SiC) at different pH values was as shown in FIG. 2.
The average modification ratio (micron SiC) at various hydrolysis temperatures, which were set at 15℃at 20℃at 25℃at 30℃at 35℃respectively, were as shown in FIG. 3, while maintaining the pH at 3 and the hydrolysis time at 2h according to the preparation method in example 1.
According to the preparation method in example 1, the pH was kept at 3, the hydrolysis temperature was room temperature (25 ℃ C.), and the hydrolysis times were set to 1.5h, 1.75h, 2h, 2.25h, and 2.5h, respectively, and the average modification ratios (micrometer SiC) at the different hydrolysis times were as shown in FIG. 4.
As can be seen from FIGS. 2 to 4, when the pH value is 3 and the hydrolysis temperature is 25 ℃ and the hydrolysis time is 2 hours, the modification effect of the hydrolyzed KH570 on the micron SiC filler is optimal, and the pH value is 3, the hydrolysis temperature is 25 ℃ and the hydrolysis time is 2 hours, which is the optimal condition for the hydrolysis of the KH 570.
Example 3 organosilicon elastomer/micro silicon carbide/nano aluminum nitride composite doped with 20wt% micro silicon carbide and 5wt% nano aluminum nitride (S20N 5)
(A) Mixing 20wt% of the modified micro silicon carbide of example 1, 5wt% of the modified nano aluminum nitride of example 2 with 37.5wt% of a component PDMS substrate, and performing ultrasonic treatment for 30min;
(b) Mixing the mixture after ultrasonic treatment with 37.5wt% of a component B dimethyl-methyl hydrogen siloxane cross-linking agent, and mechanically stirring for 1h;
(d) The stirred mixture was degassed in a vacuum oven for 30min, then poured into a mold, pre-cured at 80 ℃ for 1 hour, post-cured at 200 ℃ for 4 hours, then the sample was placed in the vacuum oven for degassing for 1h and residual impurities were removed to obtain a silicone elastomer/micro silicon carbide/nano aluminum nitride composite material doped with 20wt% micro silicon carbide and 5wt% nano aluminum nitride (S20N 5).
Comparative example 1 organosilicon elastomer/micrometer silicon carbide composite doped with 20wt% micrometer silicon carbide (S20)
(A) Mixing 20wt% of the modified micrometer silicon carbide of example 1 with 40wt% of a component PDMS substrate, and sonicating for 30min;
(b) Mixing the mixture after ultrasonic treatment with 40wt% of a component B dimethyl-methyl hydrogen siloxane cross-linking agent, and mechanically stirring for 1h;
(d) The stirred mixture was degassed in a vacuum oven for 30min, then poured into a mold, pre-cured at 80 ℃ for 1 hour, post-cured at 200 ℃ for 4 hours, then the sample was placed in the vacuum oven for 1 hour, and residual impurities were removed to obtain a 20wt% micrometer silicon carbide doped silicone elastomer/micrometer silicon carbide composite (S20).
Comparative example 2
A20 wt% micrometer silicon carbide doped silicone elastomer/micrometer silicon carbide composite was prepared as in comparative example 1, except that KH560 was used instead of KH570 for the modified micrometer silicon carbide used in comparative example 2.
The SEM images of the composite materials obtained in comparative examples 1 and 2 are shown in fig. 5 to 6, and fig. 5 is an SEM image of the composite material in comparative example 1, and fig. 6 is an SEM image of the composite material obtained in comparative example 2. As can be seen in FIG. 6, a large number of voids exist in the matrix, resulting from the filler falling off the matrix, and most of the filler floats on the surface of the silicone elastomer matrix, not being coated by the silicone elastomer, indicating poor compatibility of KH560 modified filler with the silicone elastomer. As can be seen from FIG. 5, the holes in the matrix are obviously less than those in FIG. 6, and most of the filler is coated by the silicon elastomer matrix, and the surface of the matrix presents an uneven appearance, which indicates that the interface compatibility between the micrometer SiC filler modified by KH570 and the silicon elastomer matrix is better. In addition, the filler dispersion in fig. 5 is more uniform than that of fig. 6. The invention provides a complete KH570 modified filler method, by which micro-nano fillers can be uniformly dispersed in an organosilicon elastomer matrix, and the interface compatibility of the micro-nano fillers and the organosilicon elastomer matrix is good.
The composite materials prepared in comparative example 1 and examples 1 to 3 were subjected to detection of nonlinear conductivity characteristics, the results of which are shown in FIG. 7,
The nonlinear conductivity coefficient (α) is calculated by equation (1) as shown in table 1.
Wherein E is a certain field intensity in the nonlinear conduction interval, sigma is the conductivity corresponding to the field intensity E in the nonlinear conduction interval, E b is the switching field intensity of the nonlinear conduction, and sigma b is the conductivity corresponding to E b.
TABLE 1 nonlinear conductivity coefficients
| S20 | S20N1 | S20N3 | S20N5 |
| 4.02 | 4.27 | 6.12 | 5.39 |
As can be seen from Table 1, the nonlinear conductivity coefficients of S20N1, S20N3 and S20N5 are all higher than that of S20, which indicates that the nonlinear conductivity characteristics of the nano aluminum nitride composite material can be improved by doping the nano aluminum nitride into the organic silicon elastomer/micrometer silicon carbide composite material, wherein the nonlinear conductivity coefficient of S20N3 is the largest, and the nonlinear conductivity characteristics of the organic silicon elastomer/micrometer silicon carbide composite material can be improved best when the doping mass fraction of the nano aluminum nitride is 3 wt%.
Fig. 8 shows the dc breakdown field strengths of the S20, S20N1, S20N3 and S20N5 samples prepared by the above steps, and the breakdown field strengths obtained by the four case samples at the national standard of 63.2% breakdown probability are respectively: 10.66,12.53,15.67,14.20kV/mm.
As can be seen from fig. 8, the dc breakdown field strengths of S20N1, S20N3 and S20N5 are all higher than S20, which indicates that the breakdown characteristic can be improved by incorporating nano aluminum nitride into the organosilicon elastomer/micrometer silicon carbide composite material, wherein the maximum breakdown of S20N3 indicates that the effect of improving the breakdown characteristic of the organosilicon elastomer/micrometer silicon carbide composite material is best when the doping mass fraction of nano aluminum nitride is 3 wt%. As can be seen from fig. 7 and 8, when the nano aluminum nitride is doped into the organosilicon elastomer/micrometer silicon carbide composite material, the nonlinear conductivity and the breakdown characteristic of the composite material can be improved, and when the doping mass fraction of the nano aluminum nitride is 3wt%, the improvement effect on the nonlinear conductivity and the breakdown characteristic of the organosilicon elastomer/micrometer silicon carbide composite material is best.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. The application of the modified micro silicon carbide and the modified nano aluminum nitride in improving the nonlinear conductivity and breakdown characteristics of an organosilicon elastomer material at the same time comprises the following preparation raw materials in percentage by mass:
Vinyl-terminated polydimethylsiloxane: 35-40%; crosslinking agent: 35-40%; modified micron silicon carbide: 18-22%; modified nano aluminum nitride: 0.1 to 5 percent;
The modified micron silicon carbide is prepared by hydrolyzing micron silicon carbide and a silane coupling agent KH570 in an acidic alcohol water solution; the average diameter of the micrometer silicon carbide is 5-20 mu m, and the density is 3.0-3.5 g/cm 3;
the modified nano aluminum nitride is prepared by hydrolyzing nano aluminum nitride and a silane coupling agent KH570 in an acidic alcohol water solution; the average diameter of the nano aluminum nitride is 80-200 nm, and the density is 3.2-3.8 g/cm 3;
the organic silicon elastomer composite material is prepared by the following steps:
a) Mixing water, a silane coupling agent KH570 and absolute ethyl alcohol to obtain an ethanol solution of the silane coupling agent, and then adjusting the pH value of the ethanol solution of the silane coupling agent to 2.9-3.1, and hydrolyzing for 1.8-2.2 hours at room temperature to obtain a hydrolysate;
B) Dispersing micrometer silicon carbide or nanometer aluminum nitride in absolute ethyl alcohol to obtain a dispersion liquid, mixing the hydrolysate with the dispersion liquid, and stirring to obtain a stirring liquid;
c) Centrifuging the stirring liquid, washing and drying the centrifuged solid to obtain modified micrometer silicon carbide or modified nanometer aluminum nitride;
D) Mixing modified micrometer silicon carbide and modified nanometer aluminum nitride with vinyl end-capped polydimethylsiloxane, performing ultrasonic treatment, then mixing with a cross-linking agent, and stirring to obtain a mixture;
E) And (3) pre-curing the mixture for 0.5-2 hours at 78-82 ℃ after vacuum degassing, and then curing for 3.9-4.1 hours at 198-202 ℃ to generate hydrosilylation reaction, thus obtaining the organosilicon elastomer composite material with high nonlinear conductivity and breakdown characteristics.
2. The use according to claim 1, wherein the cross-linking agent is dimethyl-methylhydrosiloxane.
3. The use according to claim 1, characterized in that in step a), the mass ratio of absolute ethanol, silane coupling agent KH570 and water is (5-10): (1-3): 1.
4. The use according to claim 1, wherein in step B), the mass ratio of micro silicon carbide or nano aluminum nitride to absolute ethanol is (0.9-1.1): 1.
5. The use according to claim 1, characterized in that the mass ratio of micro silicon carbide or nano aluminum nitride to silane coupling agent KH570 is (24-26): 1.
6. The use according to claim 1, wherein the stirring in step B) is carried out at a temperature of 50 to 80 ℃, for a period of 3 to 5 hours, and at a rotational speed of 300 to 600r/min.
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| WO2015003508A1 (en) * | 2013-07-12 | 2015-01-15 | 中国科学院上海硅酸盐研究所 | Highly insulating silicon carbide/boron nitride ceramic material and preparation method therefor |
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| WO2015003508A1 (en) * | 2013-07-12 | 2015-01-15 | 中国科学院上海硅酸盐研究所 | Highly insulating silicon carbide/boron nitride ceramic material and preparation method therefor |
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