CN114672071A - Liquid metal composite material and preparation method and application thereof - Google Patents
Liquid metal composite material and preparation method and application thereof Download PDFInfo
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- CN114672071A CN114672071A CN202011564025.6A CN202011564025A CN114672071A CN 114672071 A CN114672071 A CN 114672071A CN 202011564025 A CN202011564025 A CN 202011564025A CN 114672071 A CN114672071 A CN 114672071A
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- 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
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The application discloses a liquid metal composite material and a preparation method and application thereof. The liquid metal composite material has a core-shell structure; the core comprises at least one liquid metal; the shell is a surface active substance. The liquid metal composite material has a uniformly coated nano-scale particle structure, can be used as an independent heat-conducting filler to be widely added into various polymer matrixes, and has high heat-conducting efficiency and good universality.
Description
Technical Field
The application relates to a liquid metal composite material and a preparation method and application thereof, belonging to the technical field of heat conduction materials.
Background
The thermal interface material connects the heat source and the heat sink in a manner of filling air gaps, ensures that heat generated by the electronic equipment during operation can be effectively transferred from the heat source to the heat sink to achieve a heat dissipation effect, and plays an important role in the electronic industry. Most of the active thermal interface materials are high-molecular matrix filled with high-thermal-conductivity filler particles, such as aluminum nitride, boron nitride, aluminum oxide, and the like.
In order to improve the thermal conductivity of the thermal interface material, a mode of increasing the addition of the heat-conducting filler is often adopted, however, the filler particles are rigid structures and have no deformation capability, and in order to ensure the compressibility of the thermal interface material, the content of the filler has a threshold value, so that the heat transfer performance of the thermal interface material cannot meet the heat dissipation requirement brought by the power density improved therewith.
The liquid metal is expected to be applied to the thermal interface material due to the high thermal conductivity, low thermal resistance, low viscosity, no toxicity and deformation capacity given by the liquid property, however, the liquid metal cannot be directly used as the thermal interface material due to the poor wettability of the surface tension and the metal interface, and the common component gallium in the liquid metal is easy to react with oxygen at normal temperature to form gallium oxide, which affects the service life of the liquid metal as the thermal interface material.
Liquid metal is currently used as a heat conducting material. Firstly, disperse it in the polymer matrix, however because liquid metal surface tension is big, easily take place the reunion, unable homodisperse has greatly reduced combined material's thermal conductivity and product stability in the polymer matrix. In addition, the interface wettability of the liquid metal and the polymer is poor, the capability of improving the heat conductivity of the matrix is influenced, another method is to add the solidified metal into the polymer matrix in a mixing mode, and the liquid metal composite material prepared by the method cannot realize high filler content addition due to the fact that the volume of the liquid metal is changed after phase change. In addition, due to the characteristic that liquid metal is easy to oxidize, the method of using liquid metal as the heat-conducting filler is mostly to compound the liquid metal with a polymer matrix in the preparation process, and the liquid metal cannot be directly used as the heat-conducting filler, so that the application range of the liquid metal as the heat-conducting filler is greatly limited.
Disclosure of Invention
According to one aspect of the application, the liquid metal composite material is provided, has a uniformly coated nano-scale particle structure, can be widely added into various polymer matrixes as an independent heat-conducting filler, and is high in heat-conducting efficiency and good in universality.
A liquid metal composite having a core-shell structure;
the core comprises at least one liquid metal;
the shell is a surface active substance.
Optionally, the liquid metal is from a metal and/or metal alloy;
the melting point of the metal or the metal alloy is 0-60 ℃;
optionally, the metal alloy includes at least one of a gallium indium alloy and a gallium indium tin alloy.
Optionally, the liquid metal comprises at least one of gallium, indium, tin.
Optionally, the surface active substance comprises at least one of organic matters with the hydrophilic-lipophilic balance value of 3-16; preferably, the surface active substance comprises at least one of dopamine, polyvinylpyrrolidone and sodium alginate.
Optionally, the mass ratio of the core to the shell of the liquid metal composite material is 100: 0.1 to 10.
Optionally, the particle size of the liquid metal composite material is 10 nm-20 μm;
The thickness of the shell is 1 nm-50 nm.
Optionally, the upper limit of the particle size of the liquid metal composite is 50nm, 100nm, 200nm, 250nm, 500nm, 1 μm, 5 μm, 20 μm; the lower limit is 1nm, 50nm, 100nm, 200nm, 250nm, 500nm, 1 μm, 5 μm.
Optionally, the shell has an upper thickness limit of 5nm, 10nm, 15nm, 20nm, 25nm, 30nm, 40nm, 50 nm; the lower limit is 1nm, 5nm, 10nm, 15nm, 20nm, 25nm, 30nm, 40 nm.
According to another aspect of the application, there is provided a method of making a liquid metal composite according to any one of the above, the method comprising:
and adding liquid metal into a solution containing a surfactant, performing ultrasonic treatment, and separating to obtain the liquid metal composite material.
Optionally, a solvent is included in the solution, the solvent comprising water;
the mass ratio of the surface active substance to the solvent is 10-50: 10000.
optionally, the mass ratio of the surface active substance to the solvent is 10-20: 10000.
optionally, the mass ratio of the surface active substance to the solvent is 30-50: 10000.
optionally, the mass ratio of the liquid metal to the surface active substance is 100: 10 to 50.
Optionally, the mass ratio of the liquid metal to the surface active substance is 100: 10 to 50.
Optionally, the mass ratio of the liquid metal to the surface active substance is 100: 10 to 15.
Optionally, the mass ratio of the liquid metal to the surface active substance is 100: 35-50.
Optionally, the power of the ultrasonic treatment is 10-1000W.
Optionally, the upper power limit of the sonication is 50W, 100W, 200W, 500W, 700W, 1000W; the lower limits are 10W, 50W, 100W, 200W, 500W, 700W.
Optionally, the time of the ultrasonic treatment is 10min to 2 h.
Optionally, the time of the ultrasonic treatment is 20-50 min.
Optionally, adding a stabilizer into the suspension obtained by ultrasonic treatment, and performing oscillation treatment and separation to obtain the liquid metal composite material.
Optionally, the stabilizer comprises at least one of an alkaline substance.
Optionally, the alkaline substance comprises tris base and/or NaOH.
Optionally, the mass ratio of the stabilizer to the surface active substance is 1-20: 10 to 50.
Optionally, the mass ratio of the stabilizer to the surface active substance is 1-10: 10 to 50.
Optionally, the conditions of the oscillation processing include: the rotation speed is 10-100 rpm, and the time is 0.5-6 h.
According to another aspect of the application, there is provided the use of a liquid metal composite according to any of the above or prepared according to the preparation method of any of the above as a heat conducting filler.
As an embodiment, the application provides a liquid metal heat-conducting filler and a preparation method thereof, the liquid metal heat-conducting filler has a uniformly coated nano-scale particle structure, can be widely added in various polymer matrixes as an independent heat-conducting filler, and has high heat-conducting efficiency and good universality.
A liquid metal heat-conducting filler is prepared from the following components in parts by weight:
100 parts of low-melting-point metal;
0.1-10 parts of surface active substances.
Optionally, the melting point of the low-melting-point metal is between 0 and 60 ℃, and the low-melting-point metal includes but is not limited to gallium, gallium-indium alloy, and alloys of gallium and other metals.
Optionally, the surface active substance is an organic substance with a hydrophilic-lipophilic Balance (Hydrophile-Lipophile Balance) value of 3-16, and is preferably dopamine, polyvinylpyrrolidone or sodium alginate.
Optionally, the particle size of the low melting point metal is 10nm to 20 μm.
Optionally, the surface active substance has a thickness of 1nm to 50nm
As another embodiment, the present application provides a method for preparing a liquid metal heat conductive filler, comprising the steps of:
(a) 10000 parts of deionized water by weight are added into 10-50 parts of surface active substances;
(b) adding 100 parts of liquid metal to the solution obtained in step (a);
(c) carrying out ultrasonic treatment on the liquid metal-containing solution obtained in the step (b) by using an ultrasonic machine;
(d) adding a stabilizer into the liquid metal particle suspension obtained in the step (c), and treating for 1-24 hours;
(e) and (d) centrifuging the liquid metal particle suspension obtained in the step (d), and cleaning with ethanol and deionized water to obtain the liquid metal heat-conducting filler.
Optionally, the power of the ultrasonic treatment in the step (c) is 10W-1000W.
Optionally, the stabilizer in step (d) is a substance for promoting the polymerization of the surface active substance, including but not limited to substances for adjusting the PH of the solution, such as tris base.
Optionally, the content of the stabilizer in the step (d) is 1-20 parts by weight.
Optionally, in the step (e), the centrifugal speed is 1000-5000 rpm, and the time is 5-60 min.
The beneficial effects that this application can produce include:
1) according to the liquid metal composite material provided by the application, after the liquid metal passes through the ultrasound and covers the organic matter layer, an organic matter-liquid metal core-shell structure is formed, and the liquid metal cannot be agglomerated through the interval action of the organic matter. The formed liquid metal particles coated with the organic matter can be independently used as a heat-conducting filler.
2) The liquid metal heat-conducting filler has a uniformly coated nano-scale particle structure, can be used as an independent heat-conducting filler and widely added into various polymer matrixes, and has high heat-conducting efficiency and good universality.
3) Compared with the traditional heat-conducting filler particles, the liquid metal composite particles formed by the liquid metal composite material provided by the application have low compression modulus, and the compressibility of the polymer matrix cannot be sharply reduced by adding a large amount of heat-conducting filler into the polymer matrix.
4) The application provides a liquid metal composite, the organic matter protective layer on liquid metal surface has isolated oxygen, makes it good as nanometer metal heat conduction filler stability, is convenient for transport and preserves.
5) The preparation method of the liquid metal composite material can control the particle size of the liquid metal to be 10nm or 20 microns through ultrasonic power, and can meet the requirements of various heat-conducting substrates.
6) The preparation method of the liquid metal composite material provided by the application has the advantages of simple preparation process of the heat-conducting filler, environmental friendliness, no toxic and harmful substances and easiness in large-scale preparation.
Drawings
Fig. 1 is a scanning electron microscope image of thermally conductive filler particles prepared in example 1 of the present application;
Fig. 2 is a transmission electron microscope image of a single thermally conductive filler particle prepared in example 1 of the present application.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
Example 1
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
(a) 1g of organic dopamine is added into 1 liter of deionized water to obtain a solution I;
(b) adding 10g of Ga with the melting point of 30 ℃ into the solution I to obtain a solution II;
(c) carrying out ultrasonic treatment on the solution II by using an ultrasonic machine to obtain a solution III, wherein the ultrasonic power is 500W, and the ultrasonic time is 30 min;
(d) adding 1g of Tris alkali (Tris-hydroxymethyl-aminomethane) into the solution III, and placing the solution III in a shaking table for treatment for 1h at the frequency of 20rpm to obtain a solution IV;
(e) and (3) centrifuging the solution IV, and cleaning with deionized water and ethanol in sequence to obtain the nano-composite material with the average particle size of 200nm, the thickness of an organic layer of 10nm and the mass ratio of the core shell of 100: 3, and (b) thermally conductive filler particles.
FIG. 1 is a scanning electron microscope image of the thermally conductive filler particles prepared in this example; the average particle size of the heat-conducting filler is 200 nm;
FIG. 2 is a transmission electron micrograph of a single particle of the thermally conductive filler prepared according to the present example; the heat-conducting filler particles are of a core-shell structure, and the organic matter layer is 10 nm.
Stability measurement of the thermally conductive filler particles obtained in this example:
when the liquid metal particles without the shell and the heat conductive filler particles prepared in this example were exposed to the air, an oxide layer was immediately formed on the surface of the liquid metal particles without the shell, and the heat conductive filler particles prepared in this example were exposed to the air for 60 days, and no oxide layer was formed on the surface. Therefore, the organic matter protective layer on the surface of the liquid metal of the heat-conducting filler particles prepared by the method isolates oxygen, and the stability is good.
The heat conductivity of the heat conductive filler particles obtained in this example was measured:
the thermal conductivity of the polymer thermal pad containing 90% by mass of the thermally conductive filler particles prepared in the embodiment is 15W/mK, and the compression modulus is 0.5 MPa.
Example 2
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
the procedure was as In example 1 except that In (b), a gallium-indium alloy having a melting point of 16 ℃, a Ga mass fraction of 75.5%, and an In mass fraction of 24.5% was added to the solution I.
The average particle size of the heat-conducting filler obtained in this example was 250nm, and the thickness of the organic layer was 10 nm.
Example 3
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
The procedure is as in example 1, except that in (b), a gallium indium tin alloy having a melting point of 3 ℃ is added to the solution I, wherein the mass ratio of gallium indium tin is 7: 1: 2.
the average particle size of the heat conductive filler provided in this embodiment is 250nm, and the thickness of the organic layer is 10 nm.
Example 4
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
the procedure was as in example 1 except that the amount of dopamine added in (a) was 5 g.
The average particle size of the heat conductive filler provided by this embodiment is 200nm, and the thickness of the organic layer is 30 nm.
Example 5
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
the procedure is as in example 1, except that (d) is carried out in a shaker for a treatment time of 6 hours.
The average particle size of the heat conductive filler provided by this embodiment is 200nm, and the thickness of the organic layer is 25 nm.
Example 6
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
the procedure was as in example 1, except that in (c) the ultrasonic power was 1000W.
The average particle size of the heat conductive filler provided by this embodiment is 50nm, and the thickness of the organic layer is 10 nm.
Example 7
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
the procedure was as in example 1, except that in (c) the ultrasonic power was 100W.
The average particle size of the heat conductive filler provided in this example is 1 μm, and the thickness of the organic layer is 10 nm.
Example 8
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
the procedure was as in example 1 except that the organic material added to the deionized water in (a) was sodium alginate.
The average particle size of the heat conductive filler provided in this embodiment is 200nm, and the thickness of the organic layer is 15 nm.
Example 9
A preparation method of a liquid metal heat-conducting filler comprises the following steps:
the procedure is as in example 1 except that in (a) polyvinylpyrrolidone with an organic matter having a degree of polymerization of 450 is added to deionized water.
The average particle size of the heat conductive filler provided by this embodiment is 200nm, and the thickness of the organic layer is 15 nm. Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A liquid metal composite material is characterized in that the liquid metal composite material has a core-shell structure;
The core comprises at least one liquid metal;
the shell is a surface active substance.
2. A liquid metal composite according to claim 1, wherein the liquid metal is derived from a metal and/or metal alloy;
the melting point of the metal or the metal alloy is 0-60 ℃;
preferably, the metal alloy comprises at least one of gallium indium alloy and gallium indium tin alloy;
preferably, the liquid metal comprises at least one of gallium, indium, tin.
3. The liquid metal composite of claim 1, wherein the surface active substance comprises at least one of organic substances having a hydrophilic-lipophilic balance value of 3 to 16; preferably, the surface active substance comprises at least one of dopamine, polyvinylpyrrolidone and sodium alginate.
4. The liquid metal composite of claim 1, wherein the liquid metal composite has a core-shell mass ratio of 100: 0.1 to 10.
5. The liquid metal composite of claim 1, wherein the liquid metal composite has a particle size of 10nm to 20 μ ι η;
the thickness of the shell is 1 nm-50 nm.
6. A method of producing a liquid metal composite according to any one of claims 1 to 5, wherein the method comprises:
And adding liquid metal into a solution containing a surfactant, and carrying out ultrasonic treatment and separation to obtain the liquid metal composite material.
7. The method of claim 6, wherein the solution includes a solvent, the solvent including water;
the mass ratio of the surface active substance to the solvent is 10-50: 10000;
preferably, the mass ratio of the liquid metal to the surface active substance is 100: 10 to 50.
8. The preparation method according to claim 6, wherein the power of the ultrasonic treatment is 10-1000W;
preferably, the time of the ultrasonic treatment is 10min to 2 h.
9. The preparation method according to claim 6, wherein a stabilizer is added into the suspension obtained by ultrasonic treatment, and the suspension is subjected to oscillation treatment and separation to obtain the liquid metal composite material;
preferably, the stabilizer includes at least one of an alkaline substance;
preferably, the alkaline substance comprises tris base and/or NaOH;
preferably, the mass ratio of the stabilizer to the surface active substance is 1-20: 10 to 50;
preferably, the conditions of the oscillation treatment include: the rotation speed is 10-100 rpm, and the time is 0.5-6 h.
10. Use of a liquid metal composite according to any one of claims 1 to 5 or prepared by the method of any one of claims 6 to 9 as a thermally conductive filler.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115197677A (en) * | 2022-07-27 | 2022-10-18 | 空间液金技术研究(昆山)有限公司 | Thermal interface material with phase change function, preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135685A (en) * | 2017-06-15 | 2019-01-04 | 中国科学院理化技术研究所 | A kind of insulating heat-conductive nano material and its preparation and application based on liquid metal |
| CN110655827A (en) * | 2018-06-28 | 2020-01-07 | 中国科学院青岛生物能源与过程研究所 | Micron or nano-scale liquid metal water-based dispersion liquid and preparation method thereof |
| CN110729071A (en) * | 2019-12-19 | 2020-01-24 | 北京梦之墨科技有限公司 | Liquid metal conductive paste and electronic device |
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- 2020-12-25 CN CN202011564025.6A patent/CN114672071A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135685A (en) * | 2017-06-15 | 2019-01-04 | 中国科学院理化技术研究所 | A kind of insulating heat-conductive nano material and its preparation and application based on liquid metal |
| CN110655827A (en) * | 2018-06-28 | 2020-01-07 | 中国科学院青岛生物能源与过程研究所 | Micron or nano-scale liquid metal water-based dispersion liquid and preparation method thereof |
| CN110729071A (en) * | 2019-12-19 | 2020-01-24 | 北京梦之墨科技有限公司 | Liquid metal conductive paste and electronic device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115197677A (en) * | 2022-07-27 | 2022-10-18 | 空间液金技术研究(昆山)有限公司 | Thermal interface material with phase change function, preparation method and application thereof |
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