CN113773649A - High-reliability low-viscosity high-heat-conductivity heat-conducting gel and preparation method and application thereof - Google Patents
High-reliability low-viscosity high-heat-conductivity heat-conducting gel and preparation method and application thereof Download PDFInfo
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- CN113773649A CN113773649A CN202111127321.4A CN202111127321A CN113773649A CN 113773649 A CN113773649 A CN 113773649A CN 202111127321 A CN202111127321 A CN 202111127321A CN 113773649 A CN113773649 A CN 113773649A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000001879 gelation Methods 0.000 title description 2
- 229920002545 silicone oil Polymers 0.000 claims abstract description 28
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 25
- 239000000945 filler Substances 0.000 claims abstract description 18
- -1 polydimethylsiloxane trimethoxy silane Polymers 0.000 claims abstract description 18
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 17
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000003607 modifier Substances 0.000 claims abstract description 10
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 238000002715 modification method Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- KSLSOBUAIFEGLT-UHFFFAOYSA-N 2-phenylbut-3-yn-2-ol Chemical compound C#CC(O)(C)C1=CC=CC=C1 KSLSOBUAIFEGLT-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000000499 gel Substances 0.000 description 41
- 239000000203 mixture Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 1
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 229920006247 high-performance elastomer Polymers 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
Abstract
A high-reliability low-viscosity high-heat-conductivity heat-conducting gel, a preparation method and application thereof belong to the technical field of thermal interface materials. The heat-conducting gel is prepared by adopting a polydimethylsiloxane trimethoxy silane coupling agent as a modifier through an in-situ modification method. The raw materials of the heat-conducting gel comprise: 100-150 parts of vinyl silicone oil, 100-150 parts of hydrogen-containing silicone oil, 1-2 parts of polydimethylsiloxane trimethoxy silane coupling agent, 0.1-0.3 part of inhibitor, 1000-1100 parts of filler and 0.05-0.15 part of catalyst. According to the invention, the novel silane coupling agent with large molecular weight is added to prepare the heat-conducting gel, so that volatilization caused by working at high temperature can be effectively reduced, and the more stable heat-conducting gel with high reliability, low viscosity and high heat conductivity is prepared.
Description
Technical Field
The invention belongs to the technical field of thermal interface materials, and particularly relates to a high-reliability low-viscosity high-thermal conductivity heat-conducting gel, and a preparation method and application thereof.
Background
Thermal Interface Materials (TIMs) are widely used in electronic packages to enhance thermal conduction between a heat source and a heat sink interface. Thermal conductive gels are one of the more popular thermal interface materials because of their superior thermal conductivity and reliability. The heat-conducting gel can be placed at high temperature or can be subjected to condensation reaction with water molecules in the air to be crosslinked and cured, so that the high-performance elastomer is obtained. The heat conducting gel has flowability similar to that of heat conducting silicone grease, and can be compressed to 0.1mm under external force, so that the heat conducting gel has relatively low adhesive layer thickness and interface heat resistance, and can fill the gap between the chip and the heat sink effectively. Meanwhile, the heat-conducting gel works at high temperature, so that not only is excellent heat-conducting capacity required, but also certain stability and reliability need to be maintained under long-time high-temperature work, and the micromolecule reagent in the formula is easy to volatilize at high temperature for a long time to cause the failure of the heat-conducting gel, so an effective promotion scheme needs to be provided.
The prior art scheme is as follows: the existing preparation method of the heat-conducting gel is to add a coupling agent containing alkyl chains with 1-20 carbons to prepare single-component or double-component gel. The coupling agent containing alkyl chain with 1-20 carbons has small molecular weight and low boiling point, is easy to volatilize under long-time high-temperature work to cause internal structure defects and failures of the heat-conducting gel, and is not beneficial to normal work of electronic components.
The invention aims to prepare a low-viscosity high-heat-conductivity gel with excellent reliability by using a macromolecular silane coupling agent with large molecular weight as a modifier of a heat-conductivity filler.
Disclosure of Invention
In view of the problems in the prior art, the present invention is to design and provide a thermally conductive gel with high reliability, low viscosity and high thermal conductivity, and a preparation method and an application thereof. The invention uses a high-speed mixer to prepare the novel silane coupling agent modified heat-conducting gel by an in-situ modification method.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-reliability low-viscosity high-heat-conductivity heat-conducting gel is characterized in that the heat-conducting gel is prepared by adopting a polydimethylsiloxane trimethoxy silane coupling agent as a modifier through an in-situ modification method.
The high-reliability low-viscosity high-heat-conductivity heat-conducting gel is characterized in that the heat-conducting gel comprises the following raw materials: 100-150 parts of vinyl silicone oil, 100-150 parts of hydrogen-containing silicone oil, 1-2 parts of polydimethylsiloxane trimethoxy silane coupling agent, 0.1-0.3 part of inhibitor, 1000-1100 parts of filler and 0.05-0.15 part of catalyst.
The high-reliability low-viscosity high-heat-conductivity heat-conducting gel is characterized in that the ratio of vinyl to hydrogen in the vinyl silicone oil is 1: 1-1.5.
The high-reliability low-viscosity high-thermal conductivity thermal conductive gel is characterized in that the inhibitor comprises 2-phenyl-3-butyn-2-ol, and the filler comprises aluminum powder.
A preparation method of a high-reliability low-viscosity high-thermal conductivity thermal conductive gel is characterized by comprising the following steps:
(1) weighing vinyl silicone oil, hydrogen-containing silicone oil, polydimethylsiloxane trimethoxy silane coupling agent and inhibitor, adding into a mixing tank, and uniformly stirring in a high-speed mixer to obtain a silicone oil matrix;
(2) adding a filler into the silicone oil matrix obtained in the step (1), and stirring uniformly in a high-speed mixer for the second time in a vacuum state; maintaining a vacuum state to remove bubbles generated in the heat conductive gel during the stirring process;
(3) and taking out the mixture, placing the mixture in an ice water environment, cooling the mixture to room temperature, adding a catalyst, uniformly stirring the mixture in a high-speed mixer for three times to obtain the heat-conducting gel, and placing the mixture in the ice water environment to reduce the temperature in the mixing tank, which is increased due to material stirring friction, so as to prevent direct curing due to overhigh crosslinking reaction speed after the catalyst is added.
The preparation method is characterized in that 100 parts of vinyl silicone oil, 150 parts of hydrogen-containing silicone oil, 1-2 parts of polydimethylsiloxane trimethoxy silane coupling agent and 0.1-0.3 part of 2-phenyl-3-butyne-2-ol are weighed in the step (1), and stirring conditions are as follows: the stirring speed is 1500-.
The preparation method is characterized in that the adding part ratio of the filler in the step (2) to the vinyl silicone oil in the step (1) is 10:1, and the filler comprises aluminum powder.
The preparation method is characterized in that the secondary stirring condition in the step (2) is as follows: the stirring speed is 1500-.
The preparation method is characterized in that the temperature reduction time in the step (3) is 10-20min, and the conditions of stirring for three times are as follows: the stirring speed is 500-800r/min, and the stirring time is 2-3 min.
The heat-conducting gel is applied to a thermal interface material with high stability, low viscosity and high heat conductivity.
The invention has the following beneficial effects:
compared with the method for preparing the heat-conducting gel by using the short-chain alkyl silane coupling agent, the method for preparing the heat-conducting gel by adding the novel silane coupling agent with the large molecular weight can effectively reduce volatilization caused by working at high temperature, and can prepare the more stable heat-conducting gel with high reliability, low viscosity and high heat conductivity.
Drawings
FIG. 1 is a flow chart of a high-speed mixer for preparing heat-conducting gel;
FIG. 2 shows the structural formula of the polydimethylsiloxane trimethoxy silane coupling agent.
Detailed Description
The invention will be further illustrated by the following figures and examples.
Basic experimental procedures:
(1) preparing heat-conducting gel with different silane coupling agents as modifiers in a high-speed mixer by an in-situ modification method. The flow chart is shown in fig. 1.
(2) The viscosities of the thermally conductive gels were characterized and compared separately using an antopa rheometer.
(3) And respectively measuring the heat conductivity coefficients of the cured heat-conducting gel by using a Ling heat conductivity test analyzer and comparing the measured heat conductivity coefficients.
(4) And (3) baking the heat-conducting gel prepared by modifying the cured different silane coupling agents in an oven at 125 ℃ for 48 hours, measuring the volatilization rate of the heat-conducting gel, and comparing the volatilization rate.
Example 1:
(1) weighing 100 parts of vinyl silicone oil, 100-1: 1.5 parts of hydrogen-containing silicone oil and 1-2 parts of polydimethylsiloxane trimethoxy silane coupling agent as a modifier (the molecular weight of the polydimethylsiloxane trimethoxy silane coupling agent is 800, the content is 0.5wt percent), and 0.1-0.3 part of 2-phenyl-3-butyne-2-ol as an inhibitor in a mixing tank according to the preset ratio of vinyl to hydrogen groups of 1:1-1:1.5, and then stirring uniformly in a high-speed mixer at the speed of 1500-2000 r/min;
(2) adding 1000 parts of aluminum powder serving as a filler into the stirred silicone oil matrix, and stirring again in a high-speed mixer at a speed of 1500-2000r/min for 2-3min, wherein the vacuum state is kept during stirring to remove bubbles generated in the heat-conducting gel;
(3) taking out the mixing tank, placing the mixing tank in an ice water environment, and cooling for 10-20min, wherein the step is to reduce the temperature in the mixing tank, which is increased due to material stirring friction, so as to prevent direct curing due to excessively high crosslinking reaction speed after adding a catalyst;
(4) after the material mixing tank is cooled to room temperature, adding the catalyst and stirring for 2-3min in a high-speed mixer at the speed of 500-800r/min to obtain the heat-conducting gel prepared by taking the polydimethylsiloxane trimethoxy silane coupling agent as the modifier.
The structural formula of the polydimethylsiloxane trimethoxy silane coupling agent shown in figure 2 is obtained through tests.
Example 2:
compared with example 1, other experimental conditions and procedures were the same, and only the molecular weight of the polydimethylsiloxane trimethoxy silane coupling agent was changed to 2000, with a content of 0.5 wt%.
Example 3:
compared with example 1, other experimental conditions and procedures are the same, and only the molecular weight of the polydimethylsiloxane trimethoxy silane coupling agent is changed to 3500, and the content is 0.5 wt%.
Example 4:
compared to example 1, the other experimental conditions were the same as the procedure, except that the filler content was changed to 92 wt%.
Example 5:
compared to example 1, the other experimental conditions were the same as the procedure, except that the filler content was changed to 93 wt%.
Comparative example 1:
compared to example 1, the other experimental conditions were the same as the procedure, only changed to no modifier and a filler content of 90 wt.%.
Comparative example 2:
(1) weighing 100 parts of vinyl silicone oil, 100 parts of hydrogen-containing silicone oil, 1 part to 2 parts of dodecyl trimethoxy silane as a modifier and 0.1 part to 0.3 part of 2-phenyl-3-butyn-2-ol as an inhibitor in a mixing tank according to the preset ratio of 1:1 to 1:1.5 of vinyl to hydrogen, and then stirring uniformly in a high-speed mixer at the speed of 1500-2000 r/min;
(2) adding 1000 parts of aluminum powder serving as a filler into the stirred silicone oil matrix, and stirring again in a high-speed mixer at a speed of 1500-2000r/min for 2-3min, wherein the vacuum state is kept during stirring to remove bubbles generated in the heat-conducting gel;
(3) taking out the mixing tank, placing the mixing tank in an ice water environment, and cooling for 10-20min, wherein the step is to reduce the temperature in the mixing tank, which is increased due to material stirring friction, so as to prevent direct curing due to excessively high crosslinking reaction speed after adding a catalyst;
(4) after the material mixing tank is cooled to room temperature, adding the catalyst and stirring for 2-3min in a high-speed mixer at the speed of 500-800r/min to obtain the heat-conducting gel prepared by taking the dodecyl trimethoxy silane as the modifier.
As shown in the following table 1, both the dodecyl trimethoxy silane and the polydimethylsiloxane trimethoxy silane coupling agent can effectively carry out surface modification on the filler so as to reduce the viscosity of the heat-conducting gel, and on the basis that the effect of reducing the viscosity and improving the heat-conducting capacity of the heat-conducting gel is slightly superior to that of the former, the volatilization rate of the prepared heat-conducting gel at high temperature is greatly reduced, so that the stability of the heat-conducting gel is greatly improved, and the larger the molecular weight is, the smaller the volatilization rate is.
The invention is proved by experiments to be completely feasible.
TABLE 1 Performance data for comparative examples 1-2 and examples 1-5
Claims (10)
1. The high-reliability low-viscosity high-heat-conductivity heat-conducting gel is characterized in that the heat-conducting gel is prepared by adopting a polydimethylsiloxane trimethoxy silane coupling agent as a modifier through an in-situ modification method.
2. The thermally conductive gel of claim 1, wherein the thermally conductive gel comprises the following raw materials: 100-150 parts of vinyl silicone oil, 100-150 parts of hydrogen-containing silicone oil, 1-2 parts of polydimethylsiloxane trimethoxy silane coupling agent, 0.1-0.3 part of inhibitor, 1000-1100 parts of filler and 0.05-0.15 part of catalyst.
3. The thermally conductive gel of claim 2, wherein the ratio of vinyl groups to hydrogen groups in the vinyl silicone oil is 1: 1-1.5.
4. The thermally conductive gel of claim 2, wherein said inhibitor comprises 2-phenyl-3-butyn-2-ol and said filler comprises aluminum powder.
5. A preparation method of a high-reliability low-viscosity high-thermal conductivity thermal conductive gel is characterized by comprising the following steps:
(1) weighing vinyl silicone oil, hydrogen-containing silicone oil, polydimethylsiloxane trimethoxy silane coupling agent and inhibitor, adding into a mixing tank, and uniformly stirring in a high-speed mixer to obtain a silicone oil matrix;
(2) adding a filler into the silicone oil matrix obtained in the step (1), and stirring uniformly in a high-speed mixer for the second time in a vacuum state;
(3) and taking out, placing in an ice water environment, cooling to room temperature, adding a catalyst, and uniformly stirring in a high-speed mixer for three times to obtain the heat-conducting gel.
6. The preparation method as claimed in claim 5, wherein the vinyl silicone oil 100 parts, the hydrogen-containing silicone oil 100 parts, the polydimethylsiloxane trimethoxy silane coupling agent 1-2 parts, and the 2-phenyl-3-butyn-2-ol 0.1-0.3 part are weighed in the step (1), and the stirring conditions are as follows: the stirring speed is 1500-.
7. The method according to claim 5, wherein the ratio of the filler in the step (2) to the vinyl silicone oil in the step (1) is 10:1, and the filler comprises aluminum powder.
8. The method according to claim 5, wherein the conditions of the second stirring in the step (2) are: the stirring speed is 1500-.
9. The preparation method according to claim 5, wherein the temperature reduction time in the step (3) is 10-20min, and the conditions of the three times of stirring are as follows: the stirring speed is 500-800r/min, and the stirring time is 2-3 min.
10. Use of the thermally conductive gel of claim 1 as a high stability, low viscosity, high thermal conductivity thermal interface material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114958002A (en) * | 2022-06-27 | 2022-08-30 | 韦尔通(厦门)科技股份有限公司 | Heat-conducting silica gel and preparation method thereof |
| CN115926474A (en) * | 2022-12-29 | 2023-04-07 | 深圳德邦界面材料有限公司 | Low-modulus high-elongation organic silicon heat-conducting gel |
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| JP2006188549A (en) * | 2004-12-28 | 2006-07-20 | Ge Toshiba Silicones Co Ltd | Addition reaction-curable type silicone gel composition, thermoconductive silicone composition and radiation sheet |
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| CN112705702A (en) * | 2020-12-07 | 2021-04-27 | 中国科学院深圳先进技术研究院 | Aluminum powder surface modification method |
| CN113174048A (en) * | 2021-04-25 | 2021-07-27 | 深圳先进电子材料国际创新研究院 | Macromolecular silane coupling agent and preparation method thereof |
| CN113429796A (en) * | 2021-07-27 | 2021-09-24 | 湖南创瑾技术研究院有限公司 | Single-component high-thermal-conductivity silicone gel and preparation method thereof |
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2021
- 2021-09-26 CN CN202111127321.4A patent/CN113773649A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006188549A (en) * | 2004-12-28 | 2006-07-20 | Ge Toshiba Silicones Co Ltd | Addition reaction-curable type silicone gel composition, thermoconductive silicone composition and radiation sheet |
| CN112500705A (en) * | 2020-11-16 | 2021-03-16 | 深圳德邦界面材料有限公司 | Low-viscosity low-modulus high-thermal-conductivity single-component gel and preparation method thereof |
| CN112705702A (en) * | 2020-12-07 | 2021-04-27 | 中国科学院深圳先进技术研究院 | Aluminum powder surface modification method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114958002A (en) * | 2022-06-27 | 2022-08-30 | 韦尔通(厦门)科技股份有限公司 | Heat-conducting silica gel and preparation method thereof |
| CN115926474A (en) * | 2022-12-29 | 2023-04-07 | 深圳德邦界面材料有限公司 | Low-modulus high-elongation organic silicon heat-conducting gel |
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Application publication date: 20211210 |