CN113248931A - Heat-conducting gel with high heat conductivity and high extrusion rate and preparation method thereof - Google Patents
Heat-conducting gel with high heat conductivity and high extrusion rate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a heat-conducting gel with high heat conductivity and high extrusion rate, which comprises the following raw materials: vinyl silicone oil, heat-conducting powder filler, powder surface treating agent, cross-linking agent, inhibitor, high-temperature resistant pigment and catalyst; 100 parts of vinyl silicone oil and 2500-3500 parts of heat-conducting powder filler; the amount of the powder surface treating agent is 1-2 wt% based on the heat-conducting powder filler; a proper amount of high-temperature resistant pigment; based on the vinyl silicone oil, the dosage of the cross-linking agent is 5-10%, the dosage of the inhibitor is 0.03-0.05%, and the dosage of the catalyst is 0.2-0.25%. In addition, the invention also discloses a preparation method of the heat-conducting gel. The heat-conducting gel product has the advantages of high heat conductivity coefficient, good heat dissipation performance, no obvious settlement under the conditions of long-term placement and pressurization, small oil seepage, low oil yield, high extrusion rate under the condition that the dispensing pressure is less than or equal to 0.6Mpa, and is particularly suitable for rapid continuous dispensing production.
Description
Technical Field
The invention relates to the technical field of heat-conducting interface materials, in particular to a heat-conducting gel with high heat conduction and high extrusion rate and a preparation method thereof.
Background
With the rapid development of the production science and technology and the increasingly strict requirements on the product performance, the stability of the electronic product in terms of function use faces a severe market test, and how to solve the problem of heat dissipation of the equipment becomes the key of the overall miniaturization design of the electronic product. Because the air heat conductivity is poor, if the heat that equipment produced is not in time dispelled, then form local high temperature easily, and high temperature can cause electronic component to puncture and draw the arc etc. and then lead to damaging components and parts and subassembly to influence electronic product's reliability and normal work life cycle. Therefore, in the design and manufacture of electronic products, in order to dissipate heat generated by heat-generating components such as chips, interface heat conduction materials are generally used between the radiator and the heat-generating components so as to dissipate the heat in time, thereby ensuring the stable and normal operation of equipment. With the rapid development of the miniaturization and high power of the whole electronic product, the temperature of the heating component is continuously increased, and the research and development of the organic silicon heat conduction product with high heat conductivity, stable heat conduction performance, excellent high temperature resistance, no oil seepage, no volatilization and long service cycle has become the direction and the focus of the research in the industry.
In the operation process of the electronic equipment, the heat productivity is large, and in order to prolong the service life of components in the electronic equipment, a method of arranging a heat conduction material between the components and a radiator is generally adopted to conduct the heat to the outside of the electronic equipment. However, the conventional thermally conductive gel has several problems:
1. the heat conductivity coefficient is 2-4W/m.k, and the heat dissipation performance is not enough to meet the heat dissipation requirements of higher power and more complex environments;
2. the structure stability is insufficient, the sedimentation and the oil leakage are obvious under the pressurization or the long-term, and the non-reaction components in the system are easy to overflow;
3. the viscosity is high, the extrusion rate is low, the extrusion rate of a 30CC tube is less than 30g/min under the air pressure of 0.6MPa, and the rapid continuous dispensing production of the terminal is seriously influenced.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a heat-conducting gel with high heat conductivity and high extrusion rate, which has the advantages of high heat conductivity coefficient, good heat dissipation performance, no obvious sedimentation and oil leakage under the condition of long-time placement and pressurization, small oil yield, high extrusion rate under the condition that the dispensing pressure is less than or equal to 0.6Mpa, and is particularly suitable for rapid continuous dispensing production.
The invention also aims to provide a preparation method of the heat-conducting gel with high heat conductivity and high extrusion rate.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
the invention provides a heat-conducting gel with high heat conductivity and high extrusion rate, which comprises the following raw materials: vinyl silicone oil, heat-conducting powder filler, powder surface treating agent, cross-linking agent, inhibitor, high-temperature resistant pigment and catalyst; 100 parts of vinyl silicone oil and 2500-3500 parts of heat-conducting powder filler; the amount of the powder surface treating agent is 1-2 Wt% based on the heat-conducting powder filler; proper amount of high temperature resistant pigment; based on the vinyl silicone oil, the dosage of the cross-linking agent is 5-10%, the dosage of the inhibitor is 0.03-0.05%, and the dosage of the catalyst is 0.2-0.25%.
Further, the vinyl silicone oil is single-ended vinyl silicone oil, the viscosity is 50-1000 CP, and the structural formula is CH2＝CH-[Si(CH3)2-O]n-Si(CH3)3。
Preferably, the heat-conducting powder filler is one or a combination of more than two of alumina, zinc oxide, boron nitride, silicon nitride and aluminum nitride powder.
More preferably, the heat-conducting powder is composed of three different particle sizes, namely large particle size, medium particle size and small particle size, wherein the particle size of the large particle size is 50-80 um, the particle size of the medium particle size is 10-40 um, and the particle size of the small particle size is 0.2-10 um.
The purpose of extremely matching the particle sizes of the heat-conducting powder filler according to the large, medium and small particle sizes is to achieve the highest filling rate and further achieve the best heat conductivity; preferably, the particle shape of the heat conductive powder is spherical or ellipsoidal.
Preferably, the powder surface treatment agent is one or a combination of long-chain alkyl silane, titanate and stearate.
Preferably, the cross-linking agent is a mixture of terminal hydrogen-containing silicone oil and branched chain hydrogen-containing silicone oil.
More preferably, the cross-linking agent is hydrogen-containing silicone oil: branched hydrogen-containing silicone oil ═ 7: 3-5: 5, the compounded viscosity is 10-50 cp, wherein the structural formula of the hydrogen-terminated silicone oil is H-Si (CH)3)-2-O-[Si(CH3)2-O]n-Si(CH3)2-H, the structural formula of the branched chain hydrogen-containing silicone oil is C3H9-Si-O-[Si(CH3)(H)-O]n-Si-C3H9。
Preferably, the inhibitor is one or more of tetramethyltetravinylcyclotetrasiloxane, 1-ethynyl-1-cyclohexanol, 2-methyl-3-butyn-2-ol, 2-methyl-1-hexyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3, 7, 11-trimethyl-1-dodeca-yn-3-ol, diethyl allyl maleate, allyl glycidyl ether and diethylene glycol divinyl ether.
Preferably, the temperature-resistant pigment is cobalt blue, iron blue or titanium cyan pigment.
Preferably, the catalyst is a platinum catalyst.
The other purpose of the invention is realized by the following technical scheme:
the preparation method of the heat-conducting gel with high heat conductivity and high extrusion rate provided by the invention comprises the following steps: firstly, vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a catalyst and a powder surface treating agent are stirred and mixed uniformly in advance under the vacuum protection condition, then heat-conducting powder fillers are added into the mixture for treatment according to the small, medium and large particle sizes in multiple batches, high-temperature-resistant pigments are added into the mixture, finally, the temperature is controlled to be 60-80 ℃ under the vacuum protection condition, the reaction is carried out for 2.0-3.0 hours, and the mixture is cooled to room temperature, so that a heat-conducting gel finished product with high heat conductivity and high extrusion rate is obtained.
The technical scheme of the invention has the following beneficial effects:
(1) in the formula system, the single-ended vinyl silicone oil is adopted, so that not only can spatial net-shaped crosslinking be formed with the crosslinking agent, but also the heat-conducting powder filler is firmly wrapped in the crosslinking agent, thereby ensuring that the resin and the heat-conducting powder filler are not easy to delaminate, and preventing the heat-conducting powder filler from settling due to too high density; in the molecular structure of the single-end vinyl silicone oil, the compatibility of the single-end vinyl silicone oil with the heat-conducting filler is greatly improved due to the reduction of CH2 ═ CH-active polar groups, so that the viscosity of a finished product can be reduced, the filling ratio of the filler is increased, and the heat conductivity and the extrusion rate are improved; the viscosity of the finished product can be reduced by reducing or not adding plasticizers such as dimethyl silicon oil and the like, and the reaction components are not reduced, so that the product has the characteristics of less oil leakage and small oil yield.
(2) The powder surface treating agent is adopted to carry out surface treatment on the heat-conducting powder filler, thereby eliminating hydroxyl or other active polar groups on the surface of the powder, reducing molecular acting force (such as hydrogen bonds and the like) among powder particles, greatly increasing the filling amount of the heat-conducting powder filler and effectively ensuring the high heat conductivity of the product. In addition, the heat-conducting filler is prepared by extremely mixing powder with different particle sizes, so that the heat conductivity coefficient is greatly improved, the stability of the material is greatly improved by adopting a step-by-step treatment mode, the overall viscosity of the material is reduced under the condition of high crosslinking density, and the aim of dispensing at high extrusion rate is fulfilled.
(3) Through the optimized design of the formula, the heat-conducting powder filler and the high-temperature-resistant pigment with high proportional dosage are adopted, so that the high-temperature-resistant performance of the product is improved, and the product can keep the stability for a long time under the high-temperature condition of 200 ℃.
(4) The heat-conducting gel product with high heat conductivity and high extrusion rate has the advantages of high heat conductivity coefficient, good heat dissipation performance, no obvious settlement under the conditions of long-term placement and pressurization, small oil leakage, low oil yield, high extrusion rate under the condition that the dispensing pressure is less than or equal to 0.6Mpa, and is particularly suitable for rapid continuous dispensing production; the preparation process is simple, can provide a better heat conduction solution for the assembly of electronic heating components (such as heat dissipation accessories and LED chip aluminum substrates) and the heat dissipation between the heating components and heat dissipation or other cooling equipment, and can be widely applied to the heat dissipation of the heating components such as high-power modules, integrated chips, power modules, automotive electronic products, controllers, communication equipment, computers and accessories thereof.
The present invention will be described in further detail with reference to examples
Detailed Description
The embodiment of the invention provides a heat-conducting gel with high heat conductivity and high extrusion rate, which comprises the following raw materials: vinyl silicone oil, heat-conducting powder filler, powder surface treating agent, cross-linking agent, inhibitor, platinum catalyst and high-temperature resistant pigment. Wherein the silicone oil is single-end vinyl silicone oil, and the viscosity is 50-1000 cp; the heat-conducting powder filler is one or a combination of aluminum oxide, zinc oxide, boron nitride, silicon carbide and aluminum nitride powder, the heat-conducting powder is composed of large, medium and small particles with different particle sizes, the particle size of the large particle size is 40-100 um, the particle size of the medium particle size is 10-40 um, and the particle size of the small particle size is 0.2-10 um; the powder surface treating agent is one or the combination of long-chain alkyl silane, titanate and hard fatty acid; the cross-linking agent is a mixture of terminal hydrogen-containing silicone oil and branched chain hydrogen-containing silicone oil according to a molar ratio of 7: 3-5: 5, and the compounded viscosity is 10-50 cp, wherein the structural formula of the terminal hydrogen-containing silicone oil is H-Si (CH3)2-O- [ Si (CH3)2-O ] n-Si (CH3)2-H, and the structural formula of the branched chain hydrogen-containing silicone oil is C3H9-Si-O- [ Si (CH3) (H) -O ] n-Si-C3H 9; the high temperature resistant pigment is cobalt blue, iron blue or titanium blue pigment; the platinum catalyst is a platinum catkin catalyst. The method comprises the following specific steps:
the first embodiment is as follows:
1. the embodiment of the invention relates to a heat-conducting gel with high heat conductivity and high extrusion rate, which comprises the following raw materials:
2. the preparation method of the heat-conducting gel with high heat conductivity and high extrusion rate includes the following steps: firstly, adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a catalyst and a surface treating agent into a planetary stirrer, stirring and mixing uniformly, adding a heat-conducting powder filler into the planetary stirrer in five batches according to small, medium and large particle sizes under the vacuum protection of-0.095 Mpa for treatment, adding a high-temperature resistant pigment, controlling the temperature to be 60-80 ℃ under the vacuum protection condition, reacting for 2.0-3.0 h, and cooling to room temperature to obtain a heat-conducting gel finished product with high heat conductivity and high extrusion rate.
Example two:
1. the embodiment of the invention relates to a heat-conducting gel with high heat conductivity and high extrusion rate, which comprises the following raw materials:
2. the preparation method of the heat-conducting gel with high heat conductivity and high extrusion rate includes the following steps: firstly, adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a catalyst and a surface treating agent into a planetary stirrer, stirring and mixing uniformly, adding a heat-conducting powder filler into the planetary stirrer for treatment according to six batches of small, medium and large particle sizes under the vacuum protection of-0.095 Mpa, adding a high-temperature resistant pigment, controlling the temperature to be 60-80 ℃ under the vacuum protection condition, reacting for 2.0-3.0 h, and cooling to room temperature to obtain a heat-conducting gel finished product with high heat conductivity and high extrusion rate.
Example three:
1. the embodiment of the invention relates to a heat-conducting gel with high heat conductivity and high extrusion rate, which comprises the following raw materials:
2. the preparation method of the heat-conducting gel with high heat conductivity and high extrusion rate includes the following steps: firstly, adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a catalyst and a surface treating agent into a planetary stirrer, stirring and mixing uniformly, adding a heat-conducting powder filler into the planetary stirrer for treatment according to seven batches of small, medium and large particle sizes under the vacuum protection of-0.095 Mpa, adding a high-temperature resistant pigment, controlling the temperature to be 60-80 ℃ under the vacuum protection condition, reacting for 2.0-3.0 h, and cooling to room temperature to obtain a heat-conducting gel finished product with high heat conductivity and high extrusion rate.
Example four:
1. the embodiment of the invention relates to a heat-conducting gel with high heat conductivity and high extrusion rate, which comprises the following raw materials:
2. the preparation method of the heat-conducting gel with high heat conductivity and high extrusion rate includes the following steps: firstly, adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a catalyst and a surface treating agent into a planetary stirrer, stirring and mixing uniformly, adding a heat-conducting powder filler into the planetary stirrer for treatment according to seven batches of small, medium and large particle sizes under the vacuum protection of-0.095 Mpa, adding a high-temperature resistant pigment, controlling the temperature to be 60-80 ℃ under the vacuum protection condition, reacting for 2.0-3.0 h, and cooling to room temperature to obtain a heat-conducting gel finished product with high heat conductivity and high extrusion rate.
The physical and chemical performance indexes of the finished product of the heat-conducting gel with high heat conductivity and high extrusion rate prepared by the embodiments of the invention are shown in the following table 1.
TABLE 1 physicochemical Properties of high thermal conductivity high extrusion Rate thermally conductive gels prepared according to the examples of the present invention
The raw material composition and the preparation method process parameters of the heat-conducting gel with high heat conductivity and high extrusion rate are not limited to the above-listed examples, and the scope of the invention is not limited thereby, and all changes of equivalent structures or equivalent processes, or direct or indirect application to other related technical fields, which are made by the present specification, are included in the scope of the invention.
Claims (10)
1. A heat-conducting gel with high heat conductivity and high extrusion rate is characterized by comprising the following raw materials: vinyl silicone oil, heat-conducting powder filler, powder surface treating agent, cross-linking agent, inhibitor, high-temperature resistant pigment and catalyst; the weight portions are as follows: 100 parts of vinyl silicone oil and 2500-3500 parts of heat-conducting powder filler; the amount of the powder surface treating agent is 1-2 Wt% based on the heat-conducting powder filler; a proper amount of high-temperature-resistant color paste; based on the vinyl silicone oil, the dosage of the cross-linking agent is 5-10%, the dosage of the inhibitor is 0.03-0.05%, and the dosage of the catalyst is 0.2-0.25%; the vinyl silicone oil is single-ended vinyl silicone oil, the viscosity is 50-1000 CP, and the structural formula is CH2＝CH-[Si(CH3)2-O]n-Si(CH3)3。
2. The thermally conductive gel of claim 1, characterized in that: the heat-conducting powder filler is one or a composition of more than two of alumina, zinc oxide, boron nitride, silicon nitride and aluminum nitride powder.
3. The thermally conductive gel of claim 2, characterized in that: the heat-conducting powder body is composed of large, medium and small particles with different particle sizes, wherein the particle size of the large particle size is 50-80 um, the particle size of the medium particle size is 10-40 um, and the particle size of the small particle size is 0.2-10 um.
4. The thermally conductive gel of claim 1, characterized in that: the powder surface treating agent is one or the combination of long-chain alkyl silane, titanate and stearate.
5. The thermally conductive gel of claim 1, characterized in that: the cross-linking agent is a mixture of terminal hydrogen-containing silicone oil and branched chain hydrogen-containing silicone oil.
6. The high thermal conductivity high extrusion rate thermally conductive gel of claim 5Glue, its characterized in that: the cross-linking agent is hydrogen-containing silicone oil according to the molar ratio: branched hydrogen-containing silicone oil ═ 7: 3-5: 5, the compounded viscosity is 10-50 cp, wherein the structural formula of the hydrogen-terminated silicone oil is H-Si (CH)3)2-O-[Si(CH3)2-O]n-Si(CH3)2-H, the structural formula of the branched chain hydrogen-containing silicone oil is C3H9-Si-O-[Si(CH3)(H)-O]n-Si-C3H9。
7. The thermally conductive gel with high thermal conductivity and high extrusion rate according to claim 1, wherein said inhibitor is one or more selected from the group consisting of tetramethyltetravinylcyclotetrasiloxane, 1-ethynyl-1-cyclohexanol, 2-methyl-3-butyn-2-ol, 2-methyl-1-hexyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3, 7, 11-trimethyl-1-dodecayn-3-ol, diethylallyl maleate, allyl glycidyl ether and diethylene glycol divinyl ether.
8. The thermally conductive gel with high thermal conductivity and high extrusion rate as claimed in claim 1, wherein said high temperature resistant pigment is cobalt blue, iron blue or titanium cyan pigment.
9. The thermally conductive gel of claim 1, characterized in that: the catalyst is a platinum catalyst.
10. A method for preparing a thermally conductive gel with high thermal conductivity and high extrusion rate according to any one of claims 1 to 9, comprising the steps of: firstly, vinyl silicone oil, a cross-linking agent, an inhibitor, a catalyst and a powder surface treating agent are stirred and mixed uniformly in advance, then heat-conducting powder fillers are added into the mixture in batches according to small, medium and large particle sizes for treatment, a high-temperature-resistant pigment is added into the mixture, finally, the temperature is controlled to be 60-80 ℃ under the vacuum protection condition, the reaction lasts for 2.0-3.0 hours, and the mixture is cooled to room temperature to obtain a heat-conducting gel finished product with high heat conductivity and high extrusion rate.
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| CN113736266A (en) * | 2021-09-27 | 2021-12-03 | 广州集泰化工股份有限公司 | Double-component heat-conducting gel and preparation method and application thereof |
| CN113817178A (en) * | 2021-10-18 | 2021-12-21 | 深圳市德镒盟电子有限公司 | Low-oil-permeability high-heat-conductivity heat-conducting gel and preparation method thereof |
| CN114045036A (en) * | 2021-11-30 | 2022-02-15 | 广州市白云化工实业有限公司 | Heat-conducting gel composition and preparation method thereof |
| CN114276789A (en) * | 2021-12-31 | 2022-04-05 | 北京中石伟业科技股份有限公司 | High-thixotropic silicon-based heat-conducting gel and preparation method thereof |
| CN115403933A (en) * | 2022-09-28 | 2022-11-29 | 苏州泰吉诺新材料科技有限公司 | High-extrusion low-oil-permeability single-component heat-conducting gel and preparation method thereof |
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| CN113817178A (en) * | 2021-10-18 | 2021-12-21 | 深圳市德镒盟电子有限公司 | Low-oil-permeability high-heat-conductivity heat-conducting gel and preparation method thereof |
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| CN115895277A (en) * | 2022-12-22 | 2023-04-04 | 广州市白云化工实业有限公司 | Pre-cured single-component heat-conducting gel and preparation method thereof |
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Application publication date: 20210813 |