CN111892842A - Heat conduction mud and preparation method thereof - Google Patents
Heat conduction mud and preparation method thereof Download PDFInfo
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- CN111892842A CN111892842A CN202010765672.7A CN202010765672A CN111892842A CN 111892842 A CN111892842 A CN 111892842A CN 202010765672 A CN202010765672 A CN 202010765672A CN 111892842 A CN111892842 A CN 111892842A
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- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 51
- 238000003756 stirring Methods 0.000 claims abstract description 48
- 229920002545 silicone oil Polymers 0.000 claims abstract description 40
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 20
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000013538 functional additive Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000012258 stirred mixture Substances 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 33
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 22
- 239000002270 dispersing agent Substances 0.000 claims description 20
- 239000004014 plasticizer Substances 0.000 claims description 20
- 239000002562 thickening agent Substances 0.000 claims description 20
- 239000002113 nanodiamond Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- 230000001476 alcoholic effect Effects 0.000 claims description 16
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 16
- 239000007822 coupling agent Substances 0.000 claims description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 238000009775 high-speed stirring Methods 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 6
- 229920013822 aminosilicone Polymers 0.000 claims description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 239000012756 surface treatment agent Substances 0.000 claims description 4
- 239000011231 conductive filler Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000017525 heat dissipation Effects 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000007776 silk screen coating Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Abstract
The invention relates to the technical field of heat conduction materials, in particular to heat conduction mud, which is prepared from the following raw materials in parts by weight: 5-10 parts of terminal hydrogen-containing silicone oil, 0.5-2 parts of surface treating agent, 1-3 parts of functional additive, 70-80 parts of heat-conducting filler and 10-20 parts of matrix. The preparation method of the heat-conducting mud comprises the following steps: (1) modifying the heat-conducting filler; (2) adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture; (3) and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and 50 ℃ for vacuum heating for defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud. By adopting proper components and proportion, the prepared heat-conducting mud has the advantages of higher heat conductivity coefficient, lower thermal impedance, excellent high-temperature resistance and long service life.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to heat conduction mud and a preparation method thereof.
Background
As electronic devices continue to integrate more powerful functions into smaller components, temperature control has become one of the key elements in design, namely how to effectively remove more heat generated by a larger unit of power with a shrinking architecture and a smaller and smaller operating space. Every 10 ℃ reduction has important significance on the normal use and the service life of sensitive components.
If the heat conduction problem of the electronic components is not solved well, the service life of the equipment is directly influenced, the processing speed of signals is reduced, the power dissipation of the equipment is increased, and the like. In general, in order to solve the heat dissipation problem of heat-generating electronic components, heat sinks are disposed above the electronic components in the industry to dissipate heat of the components. However, the contact surface between the electronic component and the heat sink cannot be made to have an ideal flat surface, which is limited to the current industrial production technology. When the two contact each other, air exists in the interface gap between the two, which increases the interface thermal resistance and seriously affects the overall heat dissipation effect. Many heat dissipation technologies and related heat dissipation materials have been developed, and among them, heat conductive paste is one.
The current heat conduction mud is a jelly which is prepared by taking silicon resin as a base material, adding a heat conduction filler and a bonding material according to a certain proportion and processing by a special process. The heat conducting mud has good plasticity, can be kneaded into a certain shape as required, and is filled between an electronic element to be cooled and a radiator/shell and the like, so that the electronic element is in close contact with the radiator/shell, the thermal resistance is reduced, the temperature of an electronic element is quickly and effectively reduced, the service life of the electronic element is prolonged, and the reliability of the electronic element is improved.
However, with the rapid development of the overall miniaturization and high power of electronic products, the temperature of the heating component is continuously raised, and the existing heat conducting mud cannot meet the requirements, so that the research and development of the heat conducting mud with high heat conductivity, stable heat transfer performance, lower thermal impedance and better high temperature resistance become the direction and the focus of the research in the industry.
Based on the above, the invention provides heat conduction mud and a preparation method thereof, which are used for solving the problems in the prior art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provide the heat conduction mud with excellent heat conduction performance, low thermal impedance, high temperature resistance and long service life, and can meet the heat dissipation requirements of electronic heating components.
In order to achieve the above object, the present invention provides the following technical solutions:
in a first aspect, the invention provides heat-conducting mud, which is prepared from the following raw materials in parts by weight:
in a further embodiment of the invention, the terminal hydrogen-containing silicone oil has a viscosity of 500-8000 Pa.s.
In a further embodiment of the invention, the surface treatment agent is a silane coupling agent or a titanate coupling agent.
In a further embodiment of the present invention, the functional additives include a plasticizer, a dispersant, a thickener and a leveling agent, and the functional additives respectively account for the following components in parts by weight: 3-5 parts of plasticizer, 2-4 parts of dispersant, 1-2 parts of thickener and 0.5-1 part of flatting agent.
In a further embodiment of the invention, the thermally conductive filler is composed of aluminum nitride, zinc oxide and nanodiamonds.
In a further embodiment of the invention the particle size of the aluminium nitride is 15-50 μm, the particle size of the aluminium oxide is 1-5 μm and the particle size of the nanodiamond is 20-100 nm.
In a further embodiment of the invention, the matrix is selected from one or more of dimethicone, amino silicone oil, phenyl silicone oil, hydroxyl silicone oil.
In a second aspect, the invention also provides a preparation method of the heat-conducting mud, which comprises the following steps:
s110: dissolving a silane coupling agent with ethanol to prepare a silane coupling agent alcoholic solution, stirring until the coupling agent is completely dissolved, adding a heat-conducting filler into the silane coupling agent alcoholic solution, stirring, and drying to obtain a modified heat-conducting filler;
s120: adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture;
s130: and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and at the temperature of 50 ℃ for vacuum heating and defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud.
In a further embodiment of the present invention, in the step S110, the stirring time is 40 to 60min, and the drying is performed in a drying oven at 200 ℃ for 1 h.
In a further embodiment of the present invention, in the step S120, the high speed stirring speed is 1200r/m, and the stirring time is 20-30 min.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts proper components and proportion to ensure that the prepared heat-conducting mud has higher heat conductivity coefficient, lower thermal impedance, excellent high-temperature resistance and long service life, in particular, the invention improves the compatibility between the heat-conducting filler and a matrix by modifying the heat-conducting filler, and can ensure that the heat-conducting filler is uniformly distributed in the matrix by adding functional additives, thereby improving the heat-conducting property of the heat-conducting mud and reducing the thermal impedance thereof, meanwhile, the added end hydrogen-containing silicone oil can carry out cross-linking reaction with the matrix to form a three-dimensional network structure, thus, the heat-conducting filler can be filled in the three-dimensional network structure, and the three-dimensional network structure is similar to the capsule wall of the heat-conducting mud, can tightly bind the heat-conducting filler together, improves the filling degree of the heat-conducting mud of the invention, thereby further improving the heat-conducting property of the heat-conducting mud, the thermal impedance is reduced, and the high-temperature resistance and the service life of the heat conducting mud are also obviously improved;
2. the heat-conducting filler is divided into three components with different particle diameters in a particle matching mode, namely, the aluminum nitride with the particle size of 15-50 mu m, the aluminum oxide with the particle size of 1-5 mu m and the nano diamond with the particle size of 20-100nm, so that the three particles can be mutually filled, and the heat-conducting mud has higher filling degree, thereby further improving the heat-conducting property of the invention and reducing the thermal impedance of the heat-conducting mud;
3. according to the invention, functional additives, namely the plasticizer, the dispersing agent, the thickening agent and the leveling agent are added into the heat conduction mud, wherein the plasticizer can improve the plasticity of the heat conduction mud, the dispersing agent can uniformly disperse the heat conduction filler in a matrix, so that the heat conduction mud keeps a stable and effective structure, the thickening agent can adjust the viscosity of the heat conduction mud, the coating performance of heat conduction is further improved, and the leveling agent can enable a silk-screen coating to be smoother, so that bubbles between a heat radiator and the coating are reduced, and the heat conduction efficiency is improved.
Detailed Description
The present invention is further described below in conjunction with specific examples to enable those skilled in the art to better understand the present invention and to practice it, but the examples are not intended to limit the present invention.
The heat conduction mud comprises the following components: the heat-conducting filler comprises hydrogen-containing silicone oil at the end, a surface treating agent, a functional assistant and a heat-conducting filler, wherein the viscosity of the hydrogen-containing silicone oil at the end is 500-8000Pa.s, the surface treating agent is a silane coupling agent or a titanate coupling agent, the functional assistant is a plasticizer, a dispersing agent, a thickening agent and a flatting agent, the plasticizer is methyl silicone oil, the dispersing agent is polyethylene wax, the thickening agent is polyvinyl alcohol, the flatting agent is an acrylic flatting agent, the heat-conducting filler comprises aluminum nitride, zinc oxide and nano diamond, and the matrix is one or more of dimethyl silicone oil, amino silicone oil, phenyl silicone oil and hydroxyl silicone oil.
The preparation process flow of the heat conduction mud comprises the following steps:
(1) dissolving a silane coupling agent with ethanol to prepare a silane coupling agent alcoholic solution, stirring until the coupling agent is completely dissolved, adding a heat-conducting filler into the silane coupling agent alcoholic solution, stirring, and drying to obtain a modified heat-conducting filler;
(2) adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture;
(3) and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and at the temperature of 50 ℃ for vacuum heating and defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud.
To further illustrate the technical solution of the present invention, the following examples are presented:
example 1
The heat conduction mud is prepared from the following raw materials in parts by weight:
wherein the viscosity of the terminal hydrogen-containing silicone oil is 500-8000 Pa.s.
Wherein the surface treating agent is a silane coupling agent.
The functional auxiliary agent comprises a plasticizer, a dispersing agent, a thickening agent and a flatting agent, and the functional auxiliary agent comprises the following components in parts by weight: 3 parts of plasticizer, 2 parts of dispersant, 1 part of thickener and 0.5 part of flatting agent.
Wherein the heat conducting filler is composed of aluminum nitride, zinc oxide and nano-diamond.
Wherein the particle size of the aluminum nitride is 15-50 μm, the particle size of the aluminum oxide is 1-5 μm, and the particle size of the nanodiamond is 20-100 nm.
Wherein the matrix is selected from dimethyl silicone oil and amino silicone oil.
In addition, the invention also provides a preparation method of the heat-conducting mud, which comprises the following steps:
s110: dissolving a silane coupling agent with ethanol to prepare a silane coupling agent alcoholic solution, stirring until the coupling agent is completely dissolved, adding a heat-conducting filler into the silane coupling agent alcoholic solution, stirring, and drying to obtain a modified heat-conducting filler;
s120: adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture;
s130: and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and at the temperature of 50 ℃ for vacuum heating and defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud.
In the step S110, the stirring time is 40min, and the drying is performed in a drying oven at 200 ℃ for 1 h.
In the step S120, the high-speed stirring speed is 1200r/m, and the stirring time is 20 min.
Example 2
The heat conduction mud is prepared from the following raw materials in parts by weight:
wherein the viscosity of the terminal hydrogen-containing silicone oil is 500-8000 Pa.s.
Wherein the surface treating agent is a titanate coupling agent.
The functional auxiliary agent comprises a plasticizer, a dispersing agent, a thickening agent and a flatting agent, and the functional auxiliary agent comprises the following components in parts by weight: 5 parts of plasticizer, 4 parts of dispersant, 2 parts of thickener and 1 part of flatting agent.
Wherein the heat conducting filler is composed of aluminum nitride, zinc oxide and nano-diamond.
Wherein the particle size of the aluminum nitride is 15-50 μm, the particle size of the aluminum oxide is 1-5 μm, and the particle size of the nanodiamond is 20-100 nm.
Wherein the matrix is selected from dimethyl silicone oil and phenyl silicone oil.
In addition, the invention also provides a preparation method of the heat-conducting mud, which comprises the following steps:
s110: dissolving a silane coupling agent with ethanol to prepare a silane coupling agent alcoholic solution, stirring until the coupling agent is completely dissolved, adding a heat-conducting filler into the silane coupling agent alcoholic solution, stirring, and drying to obtain a modified heat-conducting filler;
s120: adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture;
s130: and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and at the temperature of 50 ℃ for vacuum heating and defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud.
In the step S110, the stirring time is 60min, and the drying is performed in a drying oven at 200 ℃ for 1 h.
In the step S120, the high-speed stirring speed is 1200r/m, and the stirring time is 30 min.
Example 3
The heat conduction mud is prepared from the following raw materials in parts by weight:
wherein the viscosity of the terminal hydrogen-containing silicone oil is 500-8000 Pa.s.
Wherein the surface treating agent is a silane coupling agent.
The functional auxiliary agent comprises a plasticizer, a dispersing agent, a thickening agent and a flatting agent, and the functional auxiliary agent comprises the following components in parts by weight: 4 parts of plasticizer, 3 parts of dispersant, 1.5 parts of thickener and 0.7 part of flatting agent.
Wherein the heat conducting filler is composed of aluminum nitride, zinc oxide and nano-diamond.
Wherein the particle size of the aluminum nitride is 15-50 μm, the particle size of the aluminum oxide is 1-5 μm, and the particle size of the nanodiamond is 20-100 nm.
Wherein the matrix is selected from dimethyl silicone oil and hydroxyl silicone oil.
In addition, the invention also provides a preparation method of the heat-conducting mud, which comprises the following steps:
s110: dissolving a silane coupling agent with ethanol to prepare a silane coupling agent alcoholic solution, stirring until the coupling agent is completely dissolved, adding a heat-conducting filler into the silane coupling agent alcoholic solution, stirring, and drying to obtain a modified heat-conducting filler;
s120: adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture;
s130: and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and at the temperature of 50 ℃ for vacuum heating and defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud.
In the step S110, the stirring time is 50min, and the drying is performed in a drying oven at 200 ℃ for 1 h.
In the step S120, the high-speed stirring speed is 1200r/m, and the stirring time is 25 min.
Example 4
The heat conduction mud is prepared from the following raw materials in parts by weight:
wherein the viscosity of the terminal hydrogen-containing silicone oil is 500-8000 Pa.s.
Wherein the surface treating agent is a titanate coupling agent.
The functional auxiliary agent comprises a plasticizer, a dispersing agent, a thickening agent and a flatting agent, and the functional auxiliary agent comprises the following components in parts by weight: 3.5 parts of plasticizer, 2.5 parts of dispersant, 1.3 parts of thickener and 0.6 part of flatting agent.
Wherein the heat conducting filler is composed of aluminum nitride, zinc oxide and nano-diamond.
Wherein the particle size of the aluminum nitride is 15-50 μm, the particle size of the aluminum oxide is 1-5 μm, and the particle size of the nanodiamond is 20-100 nm.
Wherein the matrix is selected from amino silicone oil and phenyl silicone oil.
In addition, the invention also provides a preparation method of the heat-conducting mud, which comprises the following steps:
s110: dissolving a silane coupling agent with ethanol to prepare a silane coupling agent alcoholic solution, stirring until the coupling agent is completely dissolved, adding a heat-conducting filler into the silane coupling agent alcoholic solution, stirring, and drying to obtain a modified heat-conducting filler;
s120: adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture;
s130: and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and at the temperature of 50 ℃ for vacuum heating and defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud.
In the step S110, the stirring time is 45min, and the drying is performed in a drying oven at 200 ℃ for 1 h.
In the step S120, the high-speed stirring speed is 1200r/m, and the stirring time is 23 min.
Example 5
The heat conduction mud is prepared from the following raw materials in parts by weight:
wherein the viscosity of the terminal hydrogen-containing silicone oil is 500-8000 Pa.s.
Wherein the surface treating agent is a silane coupling agent or a titanate coupling agent.
The functional auxiliary agent comprises a plasticizer, a dispersing agent, a thickening agent and a flatting agent, and the functional auxiliary agent comprises the following components in parts by weight: 4.5 parts of plasticizer, 3.5 parts of dispersant, 1.8 parts of thickener and 0.8 part of flatting agent.
Wherein the heat conducting filler is composed of aluminum nitride, zinc oxide and nano-diamond.
Wherein the particle size of the aluminum nitride is 15-50 μm, the particle size of the aluminum oxide is 1-5 μm, and the particle size of the nanodiamond is 20-100 nm.
Wherein the matrix is selected from phenyl silicone oil and hydroxyl silicone oil.
In addition, the invention also provides a preparation method of the heat-conducting mud, which comprises the following steps:
s110: dissolving a silane coupling agent with ethanol to prepare a silane coupling agent alcoholic solution, stirring until the coupling agent is completely dissolved, adding a heat-conducting filler into the silane coupling agent alcoholic solution, stirring, and drying to obtain a modified heat-conducting filler;
s120: adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture;
s130: and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and at the temperature of 50 ℃ for vacuum heating and defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud.
In the step S110, the stirring time is 55min, and the drying is performed in a drying oven at 200 ℃ for 1 h.
In the step S120, the high-speed stirring speed is 1200r/m, and the stirring time is 28 min.
Comparative example 1
Essentially the same procedure as in the examples was followed except that the terminal hydrogen-containing silicone oil was absent.
Comparative example 2
The preparation method was substantially the same as in the examples, except that the surface treatment agent was absent.
Comparative example 3
Essentially the same procedure as in the examples, except that the functional aid was absent.
Examples of the experiments
Specific experimental tests were as follows:
1. and (3) viscosity testing:
the thermally conductive pastes obtained in examples 1 to 5 and comparative examples 1 to 3 were measured for viscosity with a rotational viscometer (RVDV II, Brookfield) at 8rpm using a # 07 spindle.
2. And (3) testing thermal conductivity:
the heat conductive pastes prepared in examples 1 to 5 and comparative examples 1 to 3 were screen-printed on the test table of a Hotdisk tester to a thickness of 0.075mm, and the thermal conductivity of the heat conductive paste was measured.
3. Impact resistance test:
a. aging test: the heat-conductive pastes obtained in examples 1 to 5 and comparative examples 1 to 3 were baked at 150 ℃ for 1000 hours.
b. Cold and hot shock test: the heat-conducting pastes obtained in examples 1 to 5 and comparative examples 1 to 3 were circulated 600 times at-55 ℃ to 125 ℃.
Before and after the test, the silicon-free heat conducting paste was applied to a test table of an LW-9011R thermal resistance meter (manufactured by Taiwan Riyo) by screen printing, the thickness was controlled to 0.1mm, and the thermal resistance value was measured. The results are shown in Table 1, and after aging test, the thermal performance of the product is not reduced greatly, which shows that the product of the invention has better thermal stability.
The cold and heat shock test (see table 1) shows that the present invention does not require refrigeration for storage and is convenient for storage and use.
Table 1 shows the results of the test
As can be seen from table 1, the thermal conductive paste prepared according to the present invention has a low viscosity, is advantageous for coating operation, has a high thermal conductivity, a low thermal resistance, and an excellent high temperature resistance, and as can be seen from comparative examples 1 to 3, the thermal conductivity of the thermal conductive paste according to the present invention can be improved, the thermal resistance thereof can be reduced, and the high temperature resistance thereof can be improved by adding the hydrogen-containing silicone oil, the surface treatment agent, and the functional auxiliary agent to the thermal conductive paste.
In summary, the main innovation points of the heat conduction mud of the invention are as follows:
(1) the invention adopts proper components and proportion to ensure that the prepared heat-conducting mud has higher heat conductivity coefficient, lower thermal impedance, excellent high-temperature resistance and long service life, in particular, the invention improves the compatibility between the heat-conducting filler and a matrix by modifying the heat-conducting filler, and can ensure that the heat-conducting filler is uniformly distributed in the matrix by adding functional additives, thereby improving the heat-conducting property of the heat-conducting mud and reducing the thermal impedance thereof, meanwhile, the added end hydrogen-containing silicone oil can carry out cross-linking reaction with the matrix to form a three-dimensional network structure, thus, the heat-conducting filler can be filled in the three-dimensional network structure, and the three-dimensional network structure is similar to the capsule wall of the heat-conducting mud, can tightly bind the heat-conducting filler together, improves the filling degree of the heat-conducting mud of the invention, thereby further improving the heat-conducting property of the heat-conducting mud, the thermal impedance is reduced, and the high-temperature resistance and the service life of the heat conducting mud are also obviously improved;
(2) the heat-conducting filler is divided into three components with different particle diameters in a particle matching mode, namely, the aluminum nitride with the particle size of 15-50 mu m, the aluminum oxide with the particle size of 1-5 mu m and the nano diamond with the particle size of 20-100nm, so that the three particles can be mutually filled, and the heat-conducting mud has higher filling degree, thereby further improving the heat-conducting property of the invention and reducing the thermal impedance of the heat-conducting mud;
(3) according to the invention, functional additives, namely the plasticizer, the dispersing agent, the thickening agent and the leveling agent are added into the heat conduction mud, wherein the plasticizer can improve the plasticity of the heat conduction mud, the dispersing agent can uniformly disperse the heat conduction filler in a matrix, so that the heat conduction mud keeps a stable and effective structure, the thickening agent can adjust the viscosity of the heat conduction mud, the coating performance of heat conduction is further improved, and the leveling agent can enable a silk-screen coating to be smoother, so that bubbles between a heat radiator and the coating are reduced, and the heat conduction efficiency is improved.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. The heat conduction mud is characterized by being prepared from the following raw materials in parts by weight:
5-10 parts of hydrogen-terminated silicone oil;
0.5-2 parts of a surface treating agent;
1-3 parts of a functional assistant;
70-80 parts of heat-conducting filler;
10-20 parts of a matrix.
2. The thermal conductive paste as claimed in claim 1, wherein the viscosity of the terminal hydrogen-containing silicone oil is 500-8000 Pa.s.
3. The thermal conductive paste of claim 1, wherein the surface treatment agent is a silane coupling agent or a titanate coupling agent.
4. The heat conduction mud as claimed in claim 1, wherein the functional additives comprise a plasticizer, a dispersant, a thickener and a leveling agent, and the functional additives comprise the following components in parts by weight: 3-5 parts of plasticizer, 2-4 parts of dispersant, 1-2 parts of thickener and 0.5-1 part of flatting agent.
5. The thermal conductive paste of claim 1, wherein the thermal conductive filler is composed of aluminum nitride, zinc oxide, and nanodiamond.
6. The thermal mud of claim 4, wherein the aluminum nitride has a particle size of 15-50 μm, the aluminum oxide has a particle size of 1-5 μm, and the nanodiamond has a particle size of 20-100 nm.
7. The heat conduction mud of claim 1, wherein the matrix is selected from one or more of dimethyl silicone oil, amino silicone oil, phenyl silicone oil and hydroxyl silicone oil.
8. The method for preparing the heat conducting mud according to any one of claims 1 to 7, characterized by comprising the following steps:
s110: dissolving a silane coupling agent with ethanol to prepare a silane coupling agent alcoholic solution, stirring until the coupling agent is completely dissolved, adding a heat-conducting filler into the silane coupling agent alcoholic solution, stirring, and drying to obtain a modified heat-conducting filler;
s120: adding the substrate and the terminal hydrogen-containing silicone oil into a container, uniformly stirring, adding the modified heat-conducting filler and the functional auxiliary agent, and stirring at a high speed to obtain a mixture;
s130: and (3) placing the uniformly stirred mixture in a vacuum condition of 0.08MPa and 50 ℃ for vacuum heating for defoaming for 1h, and then cooling to room temperature to obtain the heat-conducting mud.
9. The method for preparing the heat-conducting mud as claimed in claim 8, wherein in the step S110, the stirring time is 40-60min, and the drying is performed in a drying oven at 200 ℃ for 1 h.
10. The method for preparing the heat conducting mud as claimed in claim 8, wherein in the step S120, the high speed stirring speed is 1200r/m, and the stirring time is 20-30 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103923463A (en) * | 2005-12-27 | 2014-07-16 | 信越化学工业株式会社 | Heat Conductive Silicone Grease Compositions |
| CN104497575A (en) * | 2014-12-22 | 2015-04-08 | 广州市白云化工实业有限公司 | High-thermal-conductivity organosilicone mud and preparation method thereof |
| CN108603033A (en) * | 2016-03-18 | 2018-09-28 | 信越化学工业株式会社 | Heat conductivity silicon-ketone composition and semiconductor device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923463A (en) * | 2005-12-27 | 2014-07-16 | 信越化学工业株式会社 | Heat Conductive Silicone Grease Compositions |
| CN104497575A (en) * | 2014-12-22 | 2015-04-08 | 广州市白云化工实业有限公司 | High-thermal-conductivity organosilicone mud and preparation method thereof |
| CN108603033A (en) * | 2016-03-18 | 2018-09-28 | 信越化学工业株式会社 | Heat conductivity silicon-ketone composition and semiconductor device |
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Application publication date: 20201106 |