CN116444838B - Voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation diaphragm and preparation method thereof - Google Patents
Voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation diaphragm and preparation method thereof Download PDFInfo
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- 230000017525 heat dissipation Effects 0.000 title claims abstract description 38
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 28
- 239000010703 silicon Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 40
- 239000012528 membrane Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000003085 diluting agent Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000003607 modifier Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims description 64
- 238000000576 coating method Methods 0.000 claims description 34
- 239000011248 coating agent Substances 0.000 claims description 32
- 229920001721 polyimide Polymers 0.000 claims description 28
- 239000004642 Polyimide Substances 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- 238000007405 data analysis Methods 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 239000011265 semifinished product Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000004513 sizing Methods 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- -1 methyl vinyl siloxane Chemical class 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004945 silicone rubber Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- 150000001343 alkyl silanes Chemical class 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims 6
- 239000000758 substrate Substances 0.000 abstract description 5
- 238000009413 insulation Methods 0.000 abstract description 4
- 239000002210 silicon-based material Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 12
- 230000015556 catabolic process Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000000265 homogenisation Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/60—Additives non-macromolecular
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- 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
- C09K5/14—Solid materials, e.g. powdery or granular
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- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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Abstract
The invention discloses a voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane and a preparation method thereof, wherein the organic silicon heat dissipation membrane comprises a base material and a mixed material coated on the base material; wherein the base material is a composite PI film; the mixed material comprises the following components in parts by weight: 150-200 parts of heat conducting powder, 50-100 parts of silicon rubber, 500-700 parts of diluent, 0.1-1 part of modifier, 5-10 parts of curing agent, 0.01-0.2 part of retarder and 0.1-2 parts of catalyst. The heat conductivity and the insulation pressure resistance of the organic silicon radiating fin are improved by adopting the reinforced substrate composite PI film, the heat conductivity coefficient of the prepared organic silicon radiating film is more than 3W/m x k, and the problem that the heat conductivity coefficient of the organic silicon material reinforced by the PI film in the prior art is not high is solved.
Description
Technical Field
The invention relates to the technical field of heat dissipation and insulation, in particular to a voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane and a preparation method thereof.
Background
The organic silicon heat conduction material is a heat conduction material prepared from silica gel and a heat conduction filler, has excellent heat conduction, heat stability and insulation and pressure resistance characteristics, and realizes efficient heat dissipation of heating components. However, in practical application, when the thickness of the organic silicon heat conducting sheet is less than 0.2mm, the organic silicon heat conducting sheet has the problems of easy tearing, easy penetration, low heat conduction, no voltage resistance and the like. The industry has generally adopted the addition of reinforcing substrates and the use of coating processes to form the films. The reinforced substrate is generally PI film or glass fiber, but the heat conductivity coefficient reinforced by PI film is basically not high, and is difficult to reach or exceed 3W/m k, and the breakdown voltage is difficult to reach or exceed 5kv when reinforced by glass fiber. In addition, most of the diluent solvents used in the coating process are low-boiling organic solvents, and the diluent solvents are quick to volatilize at room temperature, have large smell and are high in safety risk.
Disclosure of Invention
Based on the problems existing in the background technology, the invention provides a voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane and a preparation method thereof, and the organic silicon heat dissipation membrane has the characteristics of high breakdown voltage and high thermal conductivity coefficient.
The invention is implemented by the following technical scheme:
the voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane comprises a base material and a mixed material coated on the base material;
wherein the base material is a composite PI film;
the mixed material comprises the following components in parts by weight: 150-200 parts of heat conducting powder, 50-100 parts of silicon rubber, 500-700 parts of diluent, 0.2-1 part of modifier, 5-10 parts of curing agent, 0.01-0.2 part of retarder and 0.1-2 parts of catalyst.
Further, the composite PI film is a heat-conducting polyimide film prepared by adding heat-conducting powder, the thickness of the composite PI film is 0.025-0.05mm, and the heat conductivity coefficient is 0.6-0.7W/. Times.k.
Further, the composite P I film was prepared by the following method:
a. preparing polyimide precursor slurry: adding the heat conducting powder into the polyimide acid solution, and uniformly stirring and mixing to obtain polyimide precursor slurry; wherein, the addition amount of the heat conducting powder accounts for 5-10% of the weight of the polyimide; the solid content of the polyimide acid solution is 40%;
b. dripping polyimide precursor slurry on a clean glass plate, spin-coating the glass plate into a film with a specified thickness by using a spin coater, placing the film into a high-temperature oven, setting the temperature rise program of the oven to 140 ℃/1h,160 ℃/1h,180 ℃/1h,200 ℃/1h,220-230 ℃/2h, carrying out thermal imidization treatment on polyimide acid, and removing the film from the glass plate after imidization is finished, thus obtaining the composite PI film.
Further, the heat conducting powder in the mixture and the composite PI film is flaky hexagonal boron nitride, the particle size is 5-10 mu m, and the thickness of a single sheet is less than 2 mu m.
Further, the silicone rubber is polydimethyl methyl vinyl siloxane, and the molecular weight of the silicone rubber is 30-70 ten thousand.
Further, the diluent is a dearomatization environment-friendly solvent oil D series, and the boiling point of the diluent is more than 100 ℃;
the modifier is one or a combination of a long-chain alkyl silane coupling agent and an epoxy silane coupling agent;
the curing agent is hydrogen-containing silicone oil;
the retarder is alkynol compound;
the catalyst is platinum Kadster catalyst.
Further, the preparation method of the voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane comprises the following preparation steps:
step one, slurry preparation: placing the heat conducting powder, the silicon rubber, the diluent, the modifier, the curing agent and the retarder into a ball milling tank for ball milling;
step two, homogenizing, dispersing and defoaming slurry: the slurry obtained in the first step is put into a homogenizer for homogenizing and dispersing, the slurry is detected by a homogenizing uniformity detecting system, the slurry is homogenized and uniform, a catalyst is added into the slurry, and stirring and defoaming are carried out on the slurry in a vacuum state;
step three, primary coating and drying: the composite PI film is placed on a coating machine in advance, the defoamed sizing agent is placed on the composite P I film for coating, and the coated composite PI film is placed into an oven for drying and curing to obtain a single-sided composite PI semi-finished product;
step four, secondary coating and drying: and (3) placing the single-sided composite PI semi-finished product obtained by one-step coating on a coating machine, coating the other uncoated surface of the composite PI film with defoamed slurry, and placing the coated surface in an oven for drying and curing to obtain the voltage-resistant high-thermal-conductivity organosilicon heat dissipation membrane.
Further, the ball milling rotating speed in the first step is 20-300r/min, and the ball milling time is 1-4h.
Further, the coating weight of the slurry after deaeration in the third step and the fourth step is 500-600g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The temperature of the oven is 120-150 ℃, and the curing time is 30-60min.
Further, the homogeneity uniformity detection system comprises:
the data acquisition module is used for acquiring an image of the slurry and comprises an industrial CCD camera, an industrial CCD system and an LED light source;
the data processing module is used for carrying out gray processing on the acquired slurry image;
the data analysis module is used for analyzing and processing the image information of the slurry, comparing the image information with a set threshold value and sending an instruction to control the running condition of the homogenizing equipment.
Further, the homogeneity uniformity detection system performs the following operations:
s1, a data acquisition module acquires images of slurry according to preset time by using an industrial CCD camera;
s2, denoising the acquired slurry image and carrying out gray value statistics by a data processing module to obtain a gray image I, and downsampling the obtained gray image I according to a sampling coefficient q, namely taking one pixel point every q pixel points in the transverse direction and the longitudinal direction on the image to simplify and form a gray image II;
s3, the data analysis module calculates an obtained gray level image two gray level average value w:
wherein a is i The gray value of the ith pixel in the second slurry gray image is L, and the number of the pixels contained in the second slurry gray image is L;
s4, the data analysis module calculates a gray value variance sigma of a slurry gray image II:
setting the optimal value obtained by the test as a threshold value, comparing the obtained gray value variance with the optimal value by the data analysis module, if the calculated value is larger than the threshold value, considering that the homogenization is uneven, continuing to work the homogenizing equipment, if the calculated value is smaller than the set threshold value, considering that the homogenization is even, meeting the requirement, and sending an instruction to the mixing homogenizing equipment by the data analysis module, and stopping working.
The invention has the beneficial effects that:
(1) The reinforced substrate composite PI film is adopted in the invention to improve the heat conductivity and the insulation pressure resistance of the organic silicon radiating fin. The composite PI film is a heat-conducting polyimide film prepared by adding heat-conducting powder, has high withstand voltage, the breakdown voltage is more than 4.5KV, the powder used for coating slurry is hexagonal flaky boron nitride powder with excellent withstand voltage and heat conduction, the particle size is 5-10 mu m, the thickness of a single sheet is less than 2 mu m, a multilayer powder stacking effect is formed after coating, the breakdown voltage can be effectively improved, and the breakdown voltage of a final finished product is more than 6KV. The invention can be widely applied to power conversion controller scenes such as IGBT modules and the like, and can effectively isolate high-voltage modules.
(2) The heat conductivity of the organosilicon heat dissipation membrane prepared by the invention is more than 3W/m x k, the problem that the heat conductivity of the organosilicon material enhanced by the PI membrane is not high in the prior art is solved, and the organosilicon heat dissipation membrane has high pressure resistance and excellent heat conduction characteristics.
(3) The diluent used in the preparation of the organic silicon is the dearomatization environment-friendly solvent oil D series with the boiling point higher than 100 ℃, and has the characteristics of low room temperature volatility, basically no smell, easy degradation, higher boiling point, high safety and the like.
Detailed Description
The technical scheme of the present invention will be further described in detail with reference to the following specific examples, but the scope of the present invention is not limited to the following examples.
Example 1
The heat conducting powder is flaky BN powder with the particle size of 10 mu m and the monolithic thickness of less than 2 mu m;
the silicon rubber is polydimethyl methyl vinyl siloxane, and the molecular weight of the silicon rubber is 50 ten thousand;
the diluent is dearomatized environment-friendly solvent oil, and the model is Exxsol D130;
the modifier is A-1873- (2, 3-epoxypropoxy) propyl trimethoxy silane;
the retarder is alkynyl cyclohexyl alcohol.
Preparation of a composite PI film:
a. preparing polyimide precursor slurry: adding the heat conducting powder into the polyimide acid solution, and uniformly stirring and mixing to obtain polyimide precursor slurry; wherein, the adding amount of the heat conducting powder accounts for 5 percent of the weight of the polyimide; the solid content of the polyimide acid solution is 40%;
b. dripping polyimide precursor slurry on a clean glass plate, spin-coating the glass plate into a film with a specified thickness by using a spin coater, placing the film into a high-temperature oven, setting the temperature rise program of the oven to 140 ℃/1h,160 ℃/1h,180 ℃/1h,200 ℃/1h,230 ℃/2h, carrying out thermal imidization treatment on polyimide acid, and removing the film from the glass plate after imidization is finished to obtain a composite PI film, wherein the thickness of the composite PI film is 0.038mm.
Preparation of a voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane:
step one, slurry preparation: placing 150g of heat conducting powder, 60g of silicon rubber, 600g of diluent, 0.2g of modifier, 8g of hydrogen-containing silicone oil and 0.1g of retarder into a ball milling tank for ball milling, wherein the ball milling speed is 200 r/min, and the ball milling time is 2h;
step two, homogenizing, dispersing and defoaming slurry: putting the slurry obtained in the first step into a homogenizer for homogenizing and dispersing, detecting by a homogenizing uniformity detecting system, homogenizing the slurry uniformly, adding 1g of platinum Kadset catalyst into the slurry, and stirring and defoaming the slurry in a vacuum state;
step three, primary coating and drying: the composite PI film is placed on a coating machine in advance, the defoamed sizing agent is placed on the composite PI film for coating, and the coating weight is 500g/m 2 After coating, placing the mixture into an oven at 150 ℃, and drying and curing the mixture for 60min to obtain a single-sided composite PI semi-finished product;
step four, secondary coating and drying: the single-sided composite PI semi-finished product obtained by one-step coating is placed on a coating machine, the other uncoated surface of the composite PI film is coated by defoamed sizing agent, and the coating weight is g/m 2 And (3) after coating, placing the film into an oven at 150 ℃, and drying and curing for 60min to obtain the voltage-resistant high-heat-conductivity-coefficient organic silicon heat dissipation film.
Example 2
Unlike example 1, the amount of the heat conductive powder used was 180g.
Example 3
Unlike example 1, the amount of the heat conductive powder used was 200g.
Example 4
Unlike example 1, the amount of the heat conductive powder added was 8% by weight of the polyimide during the preparation of the composite PI film.
Example 5
Unlike example 1, the amount of the heat conductive powder added during the preparation of the composite PI film was 10% by weight of the polyimide.
Comparative example 1
Unlike example 1, the heat conductive powder was spherical alumina powder having a particle diameter of 5 μm in an amount of 360g.
Comparative example 2
Unlike example 1, the heat conductive powder was spherical alumina powder having a particle diameter of 5 μm in an amount of 450g.
Comparative example 3
Unlike example 1, the heat conductive powder was spherical alumina powder having a particle diameter of 5 μm in an amount of 600g.
Comparative example 4
Unlike example 1, the substrate was a PI film, i.e., the PI film did not contain a heat conductive powder.
Comparative example 5
Unlike example 1, the amount of the heat conductive powder added was 3% by weight of the polyimide during the preparation of the composite PI film.
Comparative example 6
Preparation of an organosilicon heat dissipation membrane:
step one, slurry preparation: placing 150g of heat conducting powder, 60g of silicon rubber, 600g of diluent, 0.2g of modifier, 8g of hydrogen-containing silicone oil and 0.1g of retarder into a ball milling tank for ball milling, wherein the ball milling speed is 200 r/min, and the ball milling time is 2h;
step two, homogenizing, dispersing and defoaming slurry: putting the slurry obtained in the first step into a homogenizer for homogenizing and dispersing, detecting by a homogenizing uniformity detecting system, homogenizing the slurry uniformly, adding 1g of platinum Kadset catalyst into the slurry, and stirring and defoaming the slurry in a vacuum state;
step three, coating and drying: the release film is placed on a coating machine in advance, the defoamed sizing agent is placed on the release film for coating, and the coating weight is 1250g/m 2 And (3) after coating, placing the film into an oven at 150 ℃, and drying and curing the film at 60min to obtain the organosilicon heat dissipation film.
Test examples
The finished products in examples 1 to 5 and comparative examples 1 to 6 were subjected to a voltage withstand test and a thermal conductivity test.
And (3) voltage resistance test: with reference to ASTM D149 standard execution, AC voltage mode, boost rate of 0.5kv/s, sample length and width of 100 x 100mm, each sample tested 5 sets of data, averaged
And (3) heat conduction coefficient test: with reference to ASTM D5470, the thermal conductivity is measured using a steady state heat flow method.
The test results are shown in table 1:
TABLE 1
As can be seen from the results in Table 1, the organosilicon heat dissipation films prepared in examples 1-5 have higher heat conductivity coefficients, which are all greater than 4.0W/mK, and breakdown voltages which are also greater than 6.5KV. The heat conducting powder added in the comparative examples 1-3 is spherical alumina powder with the particle size of 5 mu m, and the high-pressure resistance of the prepared organic silicon heat dissipation membrane is slightly lower than that of the organic silicon heat dissipation membrane prepared by the method, but the heat conducting coefficient of the prepared organic silicon heat dissipation membrane is obviously lower than that of the organic silicon heat dissipation membrane prepared by the method. In comparative example 4, P I film without heat conducting powder is used as a base material, and the high-pressure resistance and the heat conductivity coefficient of the prepared organic silicon heat radiating fin are obviously lower than those of the samples in examples 1-5. In comparative example 5, although the composite P I film was used, the amount of the heat conductive powder added was 3% by weight of the polyimide acid solution, and compared with comparative example 4, the high pressure resistance and the heat conductivity of the sample were significantly improved, but the various performance data were significantly lower than those of examples 1 to 5 due to the too low amount of the heat conductive powder added. In comparative example 6, the organosilicon heat dissipation membrane with the thickness of 0.18mm is directly prepared without using the reinforcing material, and the problems of easy tearing and easy puncture are found out that the organosilicon heat dissipation membrane has the heat conductivity coefficient of only 2.3W/m k, low heat conductivity, breakdown voltage of 1.6KV and no voltage resistance.
In one embodiment, a homogeneity uniformity detection system comprises:
the data acquisition module is used for acquiring an image of the slurry and comprises an industrial CCD camera, an industrial CCD system and an LED light source;
the data processing module is used for carrying out gray processing on the acquired slurry image;
the data analysis module is used for analyzing and processing the image information of the slurry, comparing the image information with a set threshold value and sending an instruction to control the running condition of the homogenizing equipment.
The homogeneity uniformity detection system performs the following operations:
s1, a data acquisition module acquires images of slurry according to preset time by using an industrial CCD camera;
s2, denoising the acquired slurry image and carrying out gray value statistics by a data processing module to obtain a gray image I, and downsampling the obtained gray image I according to a sampling coefficient q, namely taking one pixel point every q pixel points in the transverse direction and the longitudinal direction on the image to simplify and form a gray image II;
s3, the data analysis module calculates an obtained gray level image two gray level average value w:
wherein a is i The gray value of the ith pixel in the second slurry gray image is L, and the number of the pixels contained in the second slurry gray image is L;
s4, the data analysis module calculates a gray value variance sigma of a slurry gray image II:
setting the optimal value obtained by the test as a threshold value, comparing the obtained gray value variance with the optimal value by the data analysis module, if the calculated value is larger than the threshold value, considering that the homogenization is uneven, continuing to work the homogenizing equipment, if the calculated value is smaller than the set threshold value, considering that the homogenization is even, meeting the requirement, and sending an instruction to the homogenizing equipment by the data analysis module, and stopping working.
Based on the preparation method of the organic silicon heat dissipation membrane in the embodiment 1, the influence of the homogeneity uniformity detection system in the invention on the performance of the organic silicon heat dissipation membrane is tested and analyzed, and the detection result is shown in table 2.
TABLE 2
The invention has the beneficial effects that: according to the invention, the uniformity of the slurry is detected on line by the uniformity detecting system, the image of the slurry is acquired by the image acquisition module, the image is subjected to gray processing by the data processing module, the data analysis module is used for further analyzing and judging whether the slurry is uniform or not, if the slurry is uniform, the homogenizing equipment continues to work, and if the slurry is uniform, the data analysis module sends an instruction to the homogenizing equipment to stop working. Experiments show that the homogeneity uniformity detection system can intelligently control the homogeneity time, avoid too short homogeneity time and incapability of homogenizing the slurry, and reduce the performance of the obtained organosilicon heat dissipation membrane; meanwhile, the resource waste caused by overlong homogenizing time is avoided, and the production efficiency is improved.
Finally, it should be noted that: the above examples merely illustrate several embodiments of the present invention and are not intended to limit the invention, and any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art without departing from the spirit of the present invention are intended to be included in the scope of the present invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane is characterized by comprising a base material and a mixed material coated on the base material;
wherein the base material is a composite PI film;
the mixed material comprises the following components in parts by weight: 150-200 parts of heat conducting powder, 50-100 parts of silicon rubber, 500-700 parts of diluent, 0.1-1 part of modifier, 5-10 parts of curing agent, 0.01-0.2 part of retarder and 0.1-2 parts of catalyst;
the composite PI film is a heat-conducting polyimide film prepared by adding heat-conducting powder;
the addition amount of the heat conducting powder is 5-10% of the weight of the polyimide.
2. The voltage-resistant high thermal conductivity silicone heat dissipation membrane according to claim 1, wherein the composite PI has a thickness of 0.025-0.05mm and a thermal conductivity of 0.6-0.7W/k.
3. The voltage-resistant high thermal conductivity silicone heat dissipation membrane of claim 1, wherein the composite PI film is prepared by:
a. preparing polyimide precursor slurry: adding the heat conducting powder into the polyimide acid solution, and uniformly stirring and mixing to obtain polyimide precursor slurry; wherein the solid content of the polyimide acid solution is 40%;
b. dripping polyimide precursor slurry on a clean glass plate, spin-coating the glass plate into a film with a specified thickness by using a spin coater, placing the film into a high-temperature oven, setting the temperature rise program of the oven to 140 ℃/1h,160 ℃/1h,180 ℃/1h,200 ℃/1h,220-230 ℃/2h, carrying out thermal imidization treatment on polyimide acid, and removing the film from the glass plate after imidization is finished, thus obtaining the composite PI film.
4. The high thermal conductivity organosilicon heat dissipation membrane of claim 1, wherein the heat conductive powder in the mixture and the composite PI film is hexagonal boron nitride in the form of flakes, the particle size is 5-10 μm, and the monolithic thickness is less than 2 μm.
5. The high thermal conductivity silicone heat dissipation membrane of claim 1, wherein the silicone rubber is a polydimethyl methyl vinyl siloxane having a molecular weight of 30-70 ten thousand.
6. The high thermal conductivity silicone heat dissipation membrane with voltage resistance according to claim 1, wherein the diluent is dearomatized environment-friendly solvent oil D series with boiling point greater than 100 ℃;
the modifier is one or a combination of a long-chain alkyl silane coupling agent and an epoxy silane coupling agent;
the curing agent is hydrogen-containing silicone oil;
the retarder is alkynol compound;
the catalyst is platinum Kadster catalyst.
7. A method for preparing the voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane according to any one of claims 1 to 5, which is characterized by comprising the following preparation steps:
step one, slurry preparation: placing the heat conducting powder, the silicon rubber, the diluent, the modifier, the curing agent and the retarder into a ball milling tank for ball milling;
step two, homogenizing, dispersing and defoaming slurry: the slurry obtained in the first step is put into a homogenizer for homogenizing and dispersing, the slurry is detected by a homogenizing uniformity detecting system, the slurry is homogenized and uniform, a catalyst is added into the slurry, and stirring and defoaming are carried out on the slurry in a vacuum state;
step three, primary coating and drying: the composite PI film is placed on a coating machine in advance, the defoamed sizing agent is placed on the composite PI film for coating, and the composite PI film is placed into an oven for drying and curing after being coated, so that a single-sided composite PI semi-finished product is obtained;
step four, secondary coating and drying: and (3) placing the single-sided composite PI semi-finished product obtained by one-step coating on a coating machine, coating the other uncoated surface of the composite PI film with defoamed slurry, and placing the coated surface in an oven for drying and curing to obtain the voltage-resistant high-thermal-conductivity organosilicon heat dissipation membrane.
8. The method for preparing the voltage-resistant high-thermal-conductivity-coefficient organic silicon heat dissipation membrane according to claim 7, wherein the ball milling rotating speed is 20-300r/min and the ball milling time is 1-4h in the first step.
9. The method for preparing a high thermal conductivity silicone heat dissipation membrane according to claim 7, wherein the coating amount of the defoamed slurry in the third and fourth steps is 500-600g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The temperature of the oven is 120-150 ℃ and the curing time is 30-60min.
10. The method of manufacturing a voltage tolerant high thermal conductivity silicone heat sink membrane of claim 7, wherein the uniformity detection system comprises:
the data acquisition module is used for acquiring an image of the slurry and comprises an industrial CCD camera, an industrial CCD system and an LED light source;
the data processing module is used for carrying out gray processing on the acquired slurry image;
the data analysis module is used for analyzing and processing the image information of the slurry, comparing the image information with a set threshold value and sending an instruction to control the running condition of the homogenizing equipment.
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| WO2017201847A1 (en) * | 2016-05-23 | 2017-11-30 | 东莞珂洛赫慕电子材料科技有限公司 | Heat-insulating polyimide composite film used in electric heating film substrate |
| CN114316328A (en) * | 2022-01-19 | 2022-04-12 | 东莞市鸿亿导热材料有限公司 | High-thermal-conductivity insulating radiating fin for new energy battery and preparation method thereof |
| CN114605823A (en) * | 2020-12-08 | 2022-06-10 | 株洲时代华鑫新材料技术有限公司 | Insulating high-thermal-conductivity polyimide composite film, preparation method and application thereof |
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| US20060127686A1 (en) * | 2004-12-15 | 2006-06-15 | Meloni Paul A | Thermally conductive polyimide film composites having high thermal conductivity useful in an electronic device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017201847A1 (en) * | 2016-05-23 | 2017-11-30 | 东莞珂洛赫慕电子材料科技有限公司 | Heat-insulating polyimide composite film used in electric heating film substrate |
| CN106750454A (en) * | 2016-11-30 | 2017-05-31 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of insulation one-way heat conduction polyimide film high and preparation method thereof |
| CN114605823A (en) * | 2020-12-08 | 2022-06-10 | 株洲时代华鑫新材料技术有限公司 | Insulating high-thermal-conductivity polyimide composite film, preparation method and application thereof |
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