CN117757270A - Heat conduction gasket without volatile condensate and preparation method thereof - Google Patents
Heat conduction gasket without volatile condensate and preparation method thereof Download PDFInfo
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- CN117757270A CN117757270A CN202311803435.5A CN202311803435A CN117757270A CN 117757270 A CN117757270 A CN 117757270A CN 202311803435 A CN202311803435 A CN 202311803435A CN 117757270 A CN117757270 A CN 117757270A
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- 238000002360 preparation method Methods 0.000 title abstract description 16
- -1 polysiloxane Polymers 0.000 claims abstract description 63
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 56
- 239000007822 coupling agent Substances 0.000 claims abstract description 25
- 150000002978 peroxides Chemical class 0.000 claims abstract description 16
- 239000000945 filler Substances 0.000 claims abstract description 8
- 239000010409 thin film Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 238000003490 calendering Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 6
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- 239000011231 conductive filler Substances 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 abstract description 7
- 238000001704 evaporation Methods 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 6
- 239000010703 silicon Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000004132 cross linking Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 25
- 238000012360 testing method Methods 0.000 description 12
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 229910052731 fluorine Inorganic materials 0.000 description 10
- 239000011737 fluorine Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000011521 glass Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 3
- NABBBKKGVCQSKA-UHFFFAOYSA-N C1(CCCCC1)O.C(CCC)C#C Chemical compound C1(CCCCC1)O.C(CCC)C#C NABBBKKGVCQSKA-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- DDCDEKHXBABHHI-UHFFFAOYSA-N acetylene cyclohexanol Chemical compound C1(CCCCC1)O.C#C DDCDEKHXBABHHI-UHFFFAOYSA-N 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a heat-conducting gasket without volatile condensate and a preparation method thereof, and relates to the technical field of heat-conducting gaskets. The invention provides a heat conduction gasket without volatile condensate, which comprises the following components in percentage by weight: polysiloxane: 5-10%; and (3) a heat conducting filler: 80-90%; peroxide: 0.5-5%; coupling agent: 0.1-2.0%; wherein the D3-D20 content of the polysiloxane is less than 20ppm. According to the heat conduction gasket without volatile condensate, the polysiloxane is subjected to thin film evaporation in advance, and the low-volatile organic silicon polysiloxane is obtained. And then the alkenyl bond and peroxide are used for crosslinking reaction, so that the completeness of the reaction can be well ensured, and the heat-conducting gasket without volatile condensate is prepared. Meanwhile, the preparation method of the heat conduction gasket without volatile condensate is simple, is convenient for large-scale production and has low preparation cost.
Description
Technical Field
The invention relates to the technical field of heat-conducting gaskets, in particular to a heat-conducting gasket without volatile condensate and a preparation method thereof.
Background
The heat conducting gasket is a heat conducting and insulating composite material and is widely applied to various electronic products, and contacts between heating components and radiating components in electrical equipment. Its heat dissipation, flexibility, elasticity, etc. features enable it to cover uneven surfaces. Heat is conducted from the heating element to the heat dissipation element, so that the efficiency and the service life of the heating electronic component can be improved
The heat-conducting gaskets are widely used in the industries of security protection, automobiles, communication, electronics, energy storage and the like. After long-term use, the organic silicon heat-conducting gasket can separate out uncrosslinked low-molecular siloxane under continuous high temperature and compression conditions. The precipitated siloxane may volatilize onto the associated components, forming condensate; especially in security protection and optical module field, can directly cause sight interference to certain optical module field and security protection field's product.
In order to solve the problem in the current industry, 1, the silicon-free heat conduction gasket is used for replacing the organic silicon heat conduction gasket, but the silicon-free heat conduction gasket is poor in mechanical property and product reliability performance and high in cost. 2. After the heat-conducting gasket is formed, heating and vacuumizing are carried out for 24 hours at 150 ℃ and minus 0.1Mpa, but the production process is complex, the production efficiency is extremely low, the cost is extremely high, and the mass production cannot be realized.
Therefore, it is necessary to develop a heat conduction gasket without volatile condensate, so that the problem of sight interference caused by volatile condensate when an organosilicon heat conduction product is used in the fields of security protection, optical modules and the like can be well solved.
Disclosure of Invention
The invention aims to solve the technical problem that after the conventional heat conduction gasket is used for a long time, the sight line interference of products caused by organic condensate exists in the field of security protection and optical modules.
In order to solve the technical problems, the aim of the invention is realized by the following technical scheme: providing a thermally conductive gasket free of volatile condensate: utilizing olefinic bonds in low-volatility organosilicon polysiloxane (D3-D20 < 20 ppm) to carry out free radical reaction with peroxide; and adding a heat conducting filler to prepare the heat conducting gasket without volatile condensate. The heat-conducting gasket without volatile condensate prepared by the invention can not generate organic condensate after long-time application in the fields of security protection, optical modules and the like, and can not cause sight interference to products.
Specifically, the invention discloses a heat conduction gasket without volatile condensate, which comprises the following components in percentage by weight:
polysiloxane: 5-18%;
and (3) a heat conducting filler: 80-90%;
peroxide: 0.5-5%;
coupling agent: 0.1-2.0%;
wherein the D3-D20 content of the polysiloxane is less than 20ppm.
Preferably, the polysiloxane is a low-volatility silicone polysiloxane that evaporates through a thin film.
Preferably, the polysiloxane is an organosilicon polysiloxane with vinyl groups, and the viscosity of the polysiloxane is 100-10000cs.
Preferably, the heat conductive filler is at least one selected from boron nitride, aluminum oxide and aluminum hydroxide.
Preferably, the peroxide is benzoyl peroxide.
Preferably, the coupling agent is at least one selected from silane coupling agents, complex coupling agents and titanate coupling agents.
The invention also discloses a preparation method of the heat conduction gasket without volatile condensate, which comprises the following steps:
stirring and mixing the polysiloxane, the peroxide and the coupling agent according to the weight percentage to obtain a first mixture;
adding the heat conducting filler into the first mixture, and uniformly stirring to obtain a second mixture;
and (3) carrying out calendaring molding on the second mixture to obtain the heat-conducting gasket without volatile condensate.
Preferably, the polysiloxane is prepared by removing volatile matters in raw materials by a thin film evaporator before the raw materials are used, so that polysiloxane with D3-D20 content less than 20ppm is obtained.
The beneficial effects are that:
according to the heat-conducting gasket without volatile condensate, the polysiloxane used as the raw material is subjected to film evaporation in advance to obtain the low-volatile organic silicon polysiloxane, wherein the content of D3-D20 is less than 20ppm. The invention utilizes the alkenyl bond in polysiloxane and peroxide to carry out crosslinking reaction, and can well ensure the completeness of the reaction. The incompleteness of the addition reaction between the alkenyl bond in the organosilicon polysiloxane and the hydrogen-containing silicon oil in the case of an acetylene cyclohexanol inhibitor and a Karstedt catalyst is avoided.
The heat-conducting gasket without the volatile condensate has the excellent performance of the heat-conducting gasket without the volatile condensate, and meanwhile, the preparation method of the heat-conducting gasket without the volatile condensate is simple, convenient for mass production and low in preparation cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of a volatile condensate test performed on a heat conductive gasket without volatile condensate prepared in example 1 of the present invention;
FIG. 2 is a schematic illustration of a volatile condensate test performed on a non-volatile condensate heat conductive gasket made in accordance with comparative example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in the present specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
The invention provides a heat conduction gasket without volatile condensate, which comprises the following components in percentage by weight:
polysiloxane: 5-10%;
and (3) a heat conducting filler: 80-90%;
peroxide: 0.5-5%;
coupling agent: 0.1-2.0%;
wherein the D3-D20 content of the polysiloxane is less than 20ppm. The D3-D20 content of the polysiloxane without film evaporation is 1500-2000 ppm.
Wherein, the polysiloxane is preferably organosilicon polysiloxane with vinyl groups, and the viscosity of the polysiloxane is 100-10000cs; more preferably, the viscosity is 1000-10000cs.
The polysiloxane is low-volatility organic silicon polysiloxane with evaporated film.
The heat conductive filler of the present invention is preferably at least one selected from boron nitride, aluminum oxide, and aluminum hydroxide. Preferably, the boron nitride has a structure of flake or granule and a particle size of 3-200 microns; the aluminum nitride has a structure of angular shape or spherical shape and a grain diameter of 2-120 micrometers; the structure of the aluminum oxide and the aluminum hydroxide is spherical, spheroid or angular, and the grain diameter is 0.5-120 microns.
More preferably, the thermally conductive filler is spherical alumina having a particle size of 0.5 to 90 μm.
The peroxide of the present invention is preferably benzoyl peroxide.
The coupling agent of the present invention is preferably at least one of a silane coupling agent, a complex coupling agent, and a titanate coupling agent.
More preferably, the coupling agent is a silane-based coupling agent, such as KH560.
The invention also provides a preparation method of the heat conduction gasket without volatile condensate, which comprises the following steps:
mixing polysiloxane, peroxide and coupling agent in proportion to obtain a first mixture; specifically, the rotation speed is 25-65 rpm during stirring and mixing, and the stirring time is 15-25min.
Adding a heat conducting filler into the first mixture, and uniformly stirring to obtain a second mixture; specifically, the stirring conditions are: the rotating speed is 40-80 rpm, the vacuum degree is below-0.09, and the time is 30-60 minutes.
And (3) carrying out calendaring molding on the second mixture to obtain the heat-conducting gasket without volatile condensate.
Specifically, transferring the second mixture to a trough of a calender, after calendaring, setting the temperature of the conveying furnace to 120-150 ℃ and the conveying speed to 0.2-0.8m/min by a calendaring process to obtain a molded sheet, cutting off the rim charge contacting with air, and obtaining the cut sheet as the heat-conducting gasket without volatile condensate.
In other embodiments, the cutting molding can be performed by adopting a molding mode such as a wire cutting machine according to the requirements of customers, and the size required by the customers can be cut. The following are specific examples.
Example 1
The embodiment provides a heat conduction gasket without volatile condensate and a preparation method thereof, and the specific steps are as follows:
preparing raw materials (in weight percent): 8% methyl vinyl polysiloxane with a viscosity of 5000cs, 1.9% benzoyl peroxide, 0.1% KH560, 30% spherical 5 micron alumina, 60% spherical 45 micron alumina; wherein, the methyl vinyl polysiloxane is treated by a thin film evaporator in advance, and the content of D3-D20 is less than 20ppm.
And S1, placing polysiloxane, peroxide and coupling agent into a stirrer with the rotating speed of 25 revolutions per minute for stirring for 17 minutes, so that the components are uniformly mixed.
S2, turning on a stirrer, adding aluminum oxide into the stirrer at the rotating speed of 60 revolutions per minute and the vacuum degree of-0.09 Mpa, and stirring for 60 minutes to uniformly mix the components.
S3, assembling the fluorine release film at the film loading position of a knife coater, transferring the uniformly mixed material to a trough of a calender, tightly attaching the mixed material and the fluorine release film after calendering, and preparing the heat-conducting gasket sheet without volatile condensate by a calendering process, wherein the length of the conveying furnace is 12 meters and consists of 4 units, the temperature is 110 ℃, the temperature is 125 ℃, the conveying speed is 125 ℃ and the conveying speed is 0.4 m/min.
Example 2
The embodiment provides a heat conduction gasket without volatile condensate and a preparation method thereof, and the specific steps are as follows:
preparing raw materials (in weight percent): 5% ethyl vinyl polysiloxane with viscosity 10000cs, 5.0% benzoyl peroxide, 2.0% KH560, 44% aluminum nitride with angle of 80 microns, 44% spherical 5 microns alumina; wherein, the ethyl vinyl polysiloxane is treated by a thin film evaporator in advance, and the content of D3-D20 is less than 20ppm.
And S1, placing polysiloxane, peroxide and coupling agent into a stirrer with the rotating speed of 60 revolutions per minute for stirring for 15 minutes, so that the components are uniformly mixed.
S2, turning on a stirrer, adding aluminum nitride and aluminum oxide into the stirrer, and stirring the mixture for 40 minutes in the stirrer with the rotation speed of 80 revolutions per minute and the vacuum degree of-0.10 Mpa to uniformly mix the components.
S3, assembling the fluorine release film at the film loading position of a knife coater, transferring the uniformly mixed material to a trough of a calender, tightly attaching the mixed material and the fluorine release film after calendering, and preparing the heat-conducting gasket sheet without volatile condensate by a calendering process, wherein the length of the conveying furnace is 12 meters and consists of 4 units, the temperature is 110 ℃, the temperature is 125 ℃, the conveying speed is 125 ℃ and the conveying speed is 0.4 meter/min.
Example 3
The embodiment provides a heat conduction gasket without volatile condensate and a preparation method thereof, and the specific steps are as follows:
preparing raw materials (in weight percent): 10% ethyl vinyl polysiloxane with viscosity of 1000cs, 0.5% benzoyl peroxide, 0.5% titanate coupling agent GR-201, 9% granular 30 micron boron nitride, 40% spherical 50 micron aluminum nitride, 40% spheroidal 90 micron aluminum oxide; wherein, the ethyl vinyl polysiloxane is treated by a thin film evaporator in advance, and the content of D3-D20 is less than 20ppm.
And S1, placing polysiloxane, peroxide and a coupling agent into a stirrer with the rotating speed of 30 revolutions per minute for stirring for 20 minutes, and uniformly mixing the components.
S2, turning on a stirrer, adding boron nitride, aluminum nitride and aluminum oxide into the stirrer, stirring for 70 minutes in the stirrer with the rotating speed of 40 revolutions per minute and the vacuum degree of-0.12 Mpa, and uniformly mixing the components.
S3, assembling the fluorine release film at the film loading position of a knife coater, transferring the uniformly mixed material to a trough of a calender, tightly attaching the mixed material and the fluorine release film after calendering, and preparing the heat-conducting gasket sheet without volatile condensate by a calendering process, wherein the length of the conveying furnace is 12 meters and consists of 4 units, the temperature is 100 ℃, 110 ℃, 125 ℃ and 125 ℃ in sequence, and the conveying speed is 0.4 meter/min.
Comparative example 1
The comparative example provides a heat conduction gasket and a preparation method thereof, and the specific steps are as follows:
preparing raw materials (in weight percent): 7% of methyl vinyl polysiloxane with a viscosity of 5000cs and without film evaporation treatment, 2.4% of methyl side hydrogen silicone oil with an active hydrogen content of 0.36%, 0.04% of hexyne cyclohexanol, 0.5% KH560, 0.06%2000ppm of Karstedt catalyst, 30% of spherical 5-micrometer alumina, 60% of spherical 45-micrometer alumina; the content of the methyl vinyl polysiloxane D3-D20 which is not subjected to film evaporation treatment is 1500-2000 ppm.
S1, placing polysiloxane, hydrogen-containing silicone oil, an inhibitor, a coupling agent and a platinum complex catalyst into a stirrer with the rotating speed of 25 revolutions per minute for stirring for 17 minutes, and uniformly mixing the component liquids.
S2, turning on a stirrer, adding aluminum oxide into the stirrer at the rotating speed of 60 revolutions per minute and the vacuum degree of-0.09 Mpa, and stirring for 60 minutes to uniformly mix the components.
S3, assembling the fluorine release film at the film loading position of a knife coater, transferring the uniformly mixed materials to a trough of a calender, tightly attaching the mixed materials and the fluorine release film after calendering, and preparing the heat-conducting gasket sheet by a calendering process, wherein the length of the conveying furnace is 12 meters and consists of 4 units, the temperature is 110 ℃, the temperature is 125 ℃, the conveying speed is 125 ℃ and the conveying speed is 0.4 meter/min.
Comparative example 2
The comparative example provides a heat conduction gasket and a preparation method thereof, and the specific steps are as follows:
preparing raw materials (in weight percent): 10% of methyl vinyl polysiloxane with a viscosity of 5000cs and without film evaporation treatment, 2.45% of methyl side hydrogen silicone oil with an active hydrogen content of 0.36%, 0.05% of hexyne cyclohexanol, 0.4% KH560, 0.1%2000ppm of Karstedt catalyst, 22% of spherical 5-micrometer alumina and 55% of spherical 45-micrometer alumina; the content of the methyl vinyl polysiloxane D3-D20 which is not subjected to film evaporation treatment is 1500-2000 ppm.
And S1, placing the organosilicon polysiloxane, the hydrogen-containing silicone oil, the inhibitor, the coupling agent and the platinum complex catalyst into a stirrer with the rotating speed of 25 revolutions per minute for stirring for 17 minutes, and uniformly mixing the components.
S2, turning on a stirrer, adding aluminum oxide into the stirrer at the rotating speed of 60 revolutions per minute and the vacuum degree of-0.09 Mpa, and stirring for 60 minutes to uniformly mix the components.
S3, assembling the fluorine release film at the film loading position of a knife coater, transferring the uniformly mixed materials to a trough of a calender, tightly attaching the mixed materials and the fluorine release film after calendering, and preparing the heat-conducting gasket sheet by a calendering process, wherein the length of the conveying furnace is 12 meters and consists of 4 units, the temperature is 110 ℃, the temperature is 125 ℃, the conveying speed is 125 ℃ and the conveying speed is 0.4 meter/min.
Performance detection
The heat conductive gasket sheets prepared in examples 1 to 3 and comparative examples 1 to 2 were cut to the same size for the following examination.
Hardness testing: test methods refer to standard ASTM D2240; test instrument: LXA- (OO) type.
And (3) heat conduction testing: test methods refer to standard ASTM D5470; test instrument: thermal tester LW9389.
Volatile condensate test: sample size:test instrument: a heating table and a fan; test conditions: the temperature is 130 ℃ and 24 hours. The testing steps are as follows: cutting the sample into->Placing on a heating table with +.>The hollow glass cylinder cup is sleeved outside the heat conducting gasket, and flat glass sheets are arranged on the glass cup in an empty mode; the fan is turned on, and the fan blows against the glass,the heating station was set to 130℃and after 24 hours the glass and glass sheet were observed for condensate.
The test results obtained are shown in the following table.
Table 1 test results table
| Examples | Hardness (Shore OO) | Coefficient of thermal conductivity (W/m.k) | With or without volatile condensate |
| Example 1 | 42 | 3.2 | None (see figure 1) |
| Example 2 | 45 | 2.89 | Without any means for |
| Example 3 | 40 | 2.45 | Without any means for |
| Comparative example 1 | 50 | 3.05 | There are (see FIG. 2) |
| Comparative example2 | 48 | 2.78 | Has the following components |
In general, in order to remove volatile organic compounds in the heat-conducting pad, the product needs to be baked for the second time, and the specific process is as follows:
step 1: tearing the release film on the rolled heat-conducting gasket, and placing a stripping cover with length, width and height of 350 mm-250 mm-50 mm on the heat-conducting gasket of the torn release film;
step 2: setting the temperature of the vacuum oven to 150 ℃, opening and vacuumizing to-0.1 Mpa, and placing the heat-conducting gasket into the vacuum oven;
step 3: after 24 hours, the heat conduction gasket is taken out of the vacuum oven, and the glass cover is taken out;
step 4: the heat conducting pad is cooled down rapidly by a fan, and then a protective film is attached to the surface of the heat conducting pad.
Through the secondary baking, volatile organic compounds in the gasket can be effectively removed, but the process is quite complex and time-consuming.
As can be seen from table 1 and fig. 1-2, the thermal conductive pad without volatile condensate prepared in examples 1-3 is comparable to comparative examples 1-2 in terms of hardness and thermal conductivity and energy absorption, but from the test results of volatile condensate, the thermal conductive pad without volatile condensate prepared in the invention has simple preparation process, no need of secondary baking, simplified process, improved production efficiency and reduced cost. And the heat conductive gaskets prepared in the formulas of comparative examples 1-2 have volatile condensate.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (9)
1. The heat-conducting gasket without volatile condensate is characterized by comprising the following components in percentage by weight:
polysiloxane: 5-10%;
and (3) a heat conducting filler: 80-90%;
peroxide: 0.5-5%;
coupling agent: 0.1-2.0%;
wherein the D3-D20 content of the polysiloxane is less than 20ppm.
2. The non-volatile condensate heat conductive gasket of claim 1 wherein said polysiloxane is a low volatile silicone polysiloxane with vinyl groups.
3. The thermally conductive condensate free gasket of claim 1 wherein said polysiloxane has a viscosity of 100-10000cs.
4. A thermally conductive gasket free of volatile condensate according to any one of claims 1 to 3, wherein the polysiloxane is a thin film evaporated low volatile silicone polysiloxane.
5. The non-volatile condensate heat conductive gasket of claim 1 wherein said heat conductive filler is selected from at least one of boron nitride, aluminum oxide, aluminum hydroxide.
6. The non-volatile condensate thermal pad of claim 1, wherein the peroxide is benzoyl peroxide.
7. The thermally conductive gasket of claim 1 wherein said coupling agent is selected from at least one of silane-based coupling agents, complex-based coupling agents, titanate-based coupling agents.
8. The method of preparing a thermally conductive gasket free of volatile condensate as claimed in any one of claims 1 to 7, comprising the steps of:
stirring and mixing the polysiloxane, the peroxide and the coupling agent according to the weight percentage to obtain a first mixture;
adding the heat conducting filler into the first mixture, and uniformly stirring to obtain a second mixture;
and (3) carrying out calendaring molding on the second mixture to obtain the heat-conducting gasket without volatile condensate.
9. The method for preparing a heat-conducting gasket without volatile condensate according to claim 8, wherein the polysiloxane raw material is subjected to a thin film evaporator before use, and the volatile matters in the raw material are removed, so that polysiloxane with D3-D20 content less than 20ppm is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311803435.5A CN117757270A (en) | 2023-12-26 | 2023-12-26 | Heat conduction gasket without volatile condensate and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311803435.5A CN117757270A (en) | 2023-12-26 | 2023-12-26 | Heat conduction gasket without volatile condensate and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN117757270A true CN117757270A (en) | 2024-03-26 |
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| CN202311803435.5A Pending CN117757270A (en) | 2023-12-26 | 2023-12-26 | Heat conduction gasket without volatile condensate and preparation method thereof |
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