CN110684511B - Preparation method of heat-conducting interface material - Google Patents
Preparation method of heat-conducting interface material Download PDFInfo
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- CN110684511B CN110684511B CN201910836757.7A CN201910836757A CN110684511B CN 110684511 B CN110684511 B CN 110684511B CN 201910836757 A CN201910836757 A CN 201910836757A CN 110684511 B CN110684511 B CN 110684511B
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Abstract
The invention belongs to the technical field of heat conduction materials, and particularly relates to a preparation method of a heat conduction interface material. The invention discloses a preparation method of a heat-conducting interface material, which comprises the following steps: s1, mixing raw materials; s2, directional orientation; s3, putting the container in the step S2 after pressing a heavy object on the container together into a vacuum drying box, vacuumizing the vacuum drying box to be less than or equal to-0.09 MPa, and vacuumizing the vacuum drying box after 5-10 minutes; removing the heavy object, placing the container in a vacuum drying oven, vacuumizing to-0.09 MPa or less, vacuumizing after 5-10 minutes, and compacting the material in a vibration compactor; and S4, curing to obtain the material.
Description
Technical Field
The invention belongs to the technical field of heat conduction materials, and particularly relates to a preparation method of a heat conduction interface material.
Background
The continuous development of material science enables the application proportion of the heat conduction materials in national defense industry and civil materials to be increased year by year, the heat conduction materials with the characteristics of light weight, good mechanical property, strong electrical insulation, low price and the like become the trend of future development, and the heat conduction materials have wide application prospects in the rapid development of the electronic industry today. Electronic industry products such as LEDs, microelectronic packaging materials and semiconductor devices are continuously developing toward miniaturization, lightness, thinness and intellectualization, and thus people have made higher demands on the thermal conductivity of the materials.
The heat conducting materials used in electronic devices, such as high heat dissipation materials and electronic packaging materials, often need to have excellent electrical insulation and high breakdown voltage to meet the use requirements. With the continuous reduction of the volume and the continuous improvement of the performance of miniaturized electronic equipment such as notebook computers, mobile communication and the like, the heat productivity of products is also remarkably increased. The continuous rise of the operating temperature deteriorates the stability and reliability of the electronic device and shortens the life span of the product. In order to ensure that electronic equipment operates efficiently and stably, the problem to be solved urgently is to prepare a material with high thermal conductivity and proper hardness to quickly and effectively guide out heat generated inside the equipment.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a method for preparing a thermal interface material, comprising the following steps: s1, mixing raw materials; s2, directional orientation; s3, putting the container in the step S2 after pressing a heavy object on the container together into a vacuum drying box, vacuumizing the vacuum drying box to be less than or equal to-0.09 MPa, and vacuumizing the vacuum drying box after 5-10 minutes; removing the heavy object, placing the container in a vacuum drying oven, vacuumizing to-0.09 MPa or less, vacuumizing after 5-10 minutes, and compacting the material in a vibration compactor; and S4, curing to obtain the material.
As a preferred technical solution, in the step S3, the weight applies a force of 400-700kgf to the container.
As a preferred technical solution, in the step S3, the weight applies a force of 600kgf to the container.
As a preferred technical solution, the step of mixing the S1 raw material comprises the following steps: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 5-20 min; adding silica gel, and stirring for 5-20min under planetary vacuum; adding carbon fiber, and stirring for 1-10min under planetary vacuum.
As a preferable technical scheme, the vacuum degree is less than-0.01 MPa.
As a preferable technical scheme, the vacuum degree is-0.05 MPa.
As a preferred technical solution, the S2 orientation step includes the following steps: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, compacting the mixed material in a vibration compactor after the mixed material is stacked to a certain height, and repeating stacking and compacting for 1-5 times;
as a preferable technical scheme, the caliber of the needle nozzle is 0.5-3 mm.
As a preferable technical scheme, the caliber of the needle nozzle is 1 mm.
The second aspect of the invention provides a heat-conducting interface material prepared by the preparation method.
Has the advantages that: the heat-conducting interface material prepared by the preparation method disclosed by the invention has excellent heat-conducting property and appropriate hardness, and can be well applied to heat dissipation in the field of electronic products.
Detailed Description
For purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
In order to solve the above problems, the present invention provides a method for preparing a thermal interface material, comprising the following steps:
s1, mixing raw materials;
s2, directional orientation;
s3, putting the container in the step S2 after pressing a heavy object on the container together into a vacuum drying box, vacuumizing the vacuum drying box to be less than or equal to-0.09 MPa, and vacuumizing the vacuum drying box after 5-10 minutes; removing the heavy object, placing the container in a vacuum drying oven, vacuumizing to-0.09 MPa or less, vacuumizing after 5-10 minutes, and compacting the material in a vibration compactor;
and S4, curing to obtain the material.
As a preferred embodiment, the preparation method of the thermal interface material comprises the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 5-20 min; adding silica gel, and stirring for 5-20min under planetary vacuum; adding carbon fiber, and stirring for 1-10min in planetary vacuum pumping;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, compacting the mixed material in a vibration compactor after the mixed material is stacked to a certain height, and repeating stacking and compacting for 1-5 times;
s3, putting the container in the step S2 after pressing a heavy object on the container together into a vacuum drying box, vacuumizing the vacuum drying box to be less than or equal to-0.09 MPa, and vacuumizing the vacuum drying box after 5-10 minutes; removing the heavy object, placing the container in a vacuum drying oven, vacuumizing to-0.09 MPa or less, vacuumizing after 5-10 minutes, and compacting the material in a vibration compactor;
s4, curing: and (5) placing the sample obtained in the step S3 in an oven at the temperature of 100 ℃ and 150 ℃ for 30-90min to obtain the sample.
Step S1
As a preferred embodiment, the step S1 is: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 15 min; adding silica gel, and stirring for 15min in planetary vacuum pumping; adding carbon fiber, and stirring for 5min in planetary vacuum pumping;
as a preferred embodiment, the vacuum is less than-0.01 MPa.
As a preferred embodiment, the degree of vacuum is-0.05 MPa.
As an embodiment, the weight parts of the preparation raw materials are as follows: 15-20 parts of silica gel, 30-35 parts of metal powder, 8-13 parts of metal oxide, 12-20 parts of carbon fiber and 1-5 parts of silane coupling agent;
preferably, the preparation raw materials comprise the following components in parts by weight: 18.8 parts of silica gel, 33.5 parts of metal powder, 10.6 parts of metal oxide, 16.5 parts of carbon fiber and 3.5 parts of silane coupling agent.
As an embodiment, the silica gel includes at least one of a hydroxyl-modified polydimethylsiloxane-type silica gel, a carboxyl-modified polydimethylsiloxane-type silica gel, and a silicon-hydrogen bond-containing polydimethylsiloxane-type silica gel.
As a preferred embodiment, the silica gel has a viscosity of 500-1000 mPas.
The viscosity test of the silica gel is in accordance with the standard ISO3219, and the temperature is 25 ℃.
In the present application, the silica gel is of the type Waker-9212A/B, purchased in Wake, Germany.
In one embodiment, the metal powder includes at least one of copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder, and tin powder.
In one embodiment, the metal powder is aluminum powder.
In a preferred embodiment, the metal powder is a spherical powder.
The shape and particle size of the metal particles affect the distribution of the metal particles in the polymer and the way of stacking among the particles, thereby affecting the ability of constructing heat conduction channels in the polymer and affecting the heat conduction and other properties of the polymer.
As a preferred embodiment, the average particle size of the metal powder is 1 to 70 μm; preferably, the average particle size of the metal powder is 5-40 microns;
as a preferred embodiment, the metal powder consists of metal powder with an average particle size of 1-10 microns and metal powder with an average particle size of 30-50 microns;
preferably, the weight ratio of the metal powder of 1-10 microns to the metal powder of 30-50 microns is (0.8-1.2): 1.
further preferably, the weight ratio of the 10 micron metal powder to the 40 micron metal powder is (0.8-1.2): 1.
more preferably, the weight ratio of the 10 micron metal powder to the 40 micron metal powder is 1: 1.
the metal oxide has lower heat conductivity than metal powder, but has good electrical insulation, good wear resistance and high hardness.
In one embodiment, the metal oxide has the formula MxOyWherein M is selected from one of Zn, Cu, Al, Ag, Ni, Fe and Mg, x is 1-2, and y is 1-3.
As a preferred embodiment, the metal oxide has the formula MxOyWherein M is Zn, x is 1, and y is 1.
In a preferred embodiment, the metal oxide is a spherical powder.
Preferably, the average particle size of the metal oxide is 400-800 nm.
More preferably, the average particle size of the metal oxide is 600 nm.
In a preferred embodiment, the carbon fibers have an average length of 50 to 200 μm.
Preferably, the carbon fibers have an average length of 150 microns.
In the application, metal powder, metal oxide, carbon fiber and the like have higher heat conductivity coefficient, but because of lack of active groups, the surface energy is lower, and the compatibility with silica gel is poorer, and the performances such as heat conductivity, hardness and the like of the heat conduction material can be influenced. According to the method, the silane coupling agent is added to carry out surface treatment on the metal powder, the metal oxide and the carbon material, so that the compatibility among the metal powder, the metal oxide and the carbon material is improved, and the interface adhesive force is improved.
In a preferred embodiment, the silane coupling agent is at least one selected from the group consisting of 1-vinyl-1, 1,3,3, 3-pentamethyldisiloxane, 1,3, 5-trivinyl-1, 1,3,5, 5-pentamethyltrisiloxane, vinyltris (dimethylsiloxy) silane, 1, 3-divinyltetraethoxydisiloxane, methacryloxypentamethyldisiloxane, vinyltris (trimethylsiloxy) silane, and vinyltrimethoxysilane.
In the present application, the silane coupling agent is of type KH 171.
In one embodiment, the ceramic material is selected from one or more of silicon carbide, aluminum nitride, silicon nitride, aluminum silicate, and zirconium oxide.
In a preferred embodiment, the ceramic material is aluminum nitride.
The aluminum nitride is a covalent bond compound, has a hexagonal wurtzite structure, is white or grey white, and has an Al atom and an adjacent N atom which are diverged (AIN)4) A tetrahedron. AIN has the theoretical density of 3.269, the Mohs hardness of 7-8, the decomposition at 2200-. In addition, the aluminum nitride has the characteristic of being not corroded by aluminum and other molten metals and gallium arsenide, and also has excellent electrical insulation and dielectric properties.
In a preferred embodiment, the aluminum nitride is a spherical powder.
As a preferred embodiment, the aluminum nitride has an average particle size of 0.5 to 5 μm;
in a preferred embodiment, the aluminum nitride has an average particle size of 1 μm.
The planetary stirrer is a novel high-efficiency dead-point-free mixing stirring device, and has a unique and novel stirring form, two or 3 multilayer blade stirrers and 1-2 automatic scrapers are arranged in a kettle, and the stirrers revolve around the axis of the kettle body and rotate around the axis at high speed at different rotating speeds, so that materials do complex motion in the kettle body, and the efficiency of the materials subjected to strong shearing and twisting is usually multiple times that of a common stirrer.
Step S2
As a preferred embodiment, the S2 orientation step includes the following steps: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, compacting the mixed material in a vibration compactor after the mixed material is stacked to a certain height, and repeating stacking and compacting for 3 times;
in a preferred embodiment, the needle mouth has a caliber of 0.5-3 mm.
In a preferred embodiment, the needle mouth has a diameter of 1 mm.
As a preferred embodiment, said certain height is referred to as 1/3-1/4 of the height of the container.
Specifically, the operation of repeating the stacking tapping for 3 times is as follows: the mixed material obtained in step S1 was put into an injection extruder, discharged through a needle nozzle, arranged in a bar form in a container, stacked to a height of 1/3, tapped by a vibration compactor, stacked to a height of 2/3, tapped by the vibration compactor, stacked to a height corresponding to the height of the container, and tapped by the vibration compactor.
This application utilizes the needle mouth to carry out the tap after spitting out the misce bene, can obtain the carbon fiber heat conduction material that has certain orientation.
Step S3
As a preferred embodiment, the container in step S2 is put into a vacuum drying oven together after being pressed with a weight, and is vacuumized to-0.09 MPa, and after 8 minutes, the container is vacuumized; after removing the heavy object, the container is placed in a vacuum drying oven to be vacuumized to-0.09 MPa, after 8 minutes, the container is vacuumized, and the material is compacted in a vibration compactor.
In a preferred embodiment, in step S3, the weight applies a force of 400-700kgf to the container.
In a preferred embodiment, in step S3, the weight applies a force of 600kgf to the container.
Step S4
As a preferred embodiment, the sample obtained in step S3 is placed in an oven at 120 ℃ for 60min to obtain the product.
According to the preparation method, the silane coupling agent is used for treating the metal powder, the metal oxide and the ceramic material, and then the metal powder, the metal oxide and the ceramic material are mixed with the silica gel and the carbon fiber, so that the compatibility among the metal powder, the metal oxide and the ceramic material is improved; and simultaneously, performing vacuum drying on the weight on the container in the step S2 through a directional orientation process to obtain a carbon fiber directional orientation heat conduction material, and the fillers with different particle sizes and the carbon fibers are distributed in the silica gel to form a heat conduction chain, wherein a plurality of parallel circuits are equivalently formed in a heat conduction material system, and heat flow passes through the plurality of parallel circuits, so that the heat conduction performance is improved.
The second aspect of the invention provides a heat-conducting interface material prepared by the preparation method.
The interface material is used for heat dissipation of electronic products.
The electronic products include watches, smart phones, telephones, televisions, video disc players (VCD, SVCD, DVD), video recorders, camcorders, radios, radio cassettes, combination speakers, compact disc players (CD), computers, game machines, and the like.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
A preparation method of a heat-conducting interface material comprises the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 15 min; adding silica gel, and stirring for 15min in planetary vacuum pumping; adding carbon fiber, planetary vacuum-pumping and stirring for 5min, wherein the vacuum degree is-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 1 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively.
S3, putting the container in the step S2 together with a weight on the container, vacuumizing the container to-0.09 MPa, and vacuumizing the container after 8 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa, vacuumizing after 8 minutes, and compacting the material in a vibration compactor;
s4, curing: and (5) putting the sample obtained in the step S3 into an oven at 120 ℃ for 60min to obtain the product.
In the step S3, the weight applies a force of 600kgf to the container.
The weight parts of the preparation raw materials are as follows: 18.8 parts of silica gel, 33.5 parts of metal powder, 10.6 parts of metal oxide, 16.5 parts of carbon fiber and 3.5 parts of silane coupling agent.
Wherein the silica gel is of a Waker-9212A/B type and is purchased from Waker in Germany.
The metal powder consists of aluminum powder with the average particle size of 5 microns and aluminum powder with the average particle size of 40 microns; the weight ratio of the 10-micron aluminum powder to the 40-micron aluminum powder is 1: 1.
the molecular formula of the metal oxide is MxOyWherein M is Zn, x is 1, and y is 1; the average particle diameter of the metal oxide is 600 nm.
The carbon fibers had an average length of 150 microns.
The model of the silane coupling agent is KH 171.
The ceramic material is aluminum nitride, and the average grain diameter of the aluminum nitride is 1 micron.
Example 2
A preparation method of a heat-conducting interface material comprises the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 5 min; adding silica gel, and stirring for 5min under planetary vacuum; adding carbon fiber, stirring for 1min under planetary vacuum, and vacuum degree of-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 1 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively.
S3, putting the container in the step S2 together with a weight on the container, vacuumizing the container in a vacuum drying oven to-0.09 MPa, and vacuumizing the container after 10 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa, vacuumizing after 10 minutes, and compacting the material in a vibration compactor;
s4, curing: and (5) putting the sample obtained in the step S3 into an oven at 100 ℃ for 90min to obtain the product.
In the step S3, the weight applies a force of 400kgf to the container.
Wherein the preparation raw materials comprise the following components in parts by weight: 15 parts of silica gel, 30 parts of metal powder, 8 parts of metal oxide, 12 parts of carbon fiber and 1 part of silane coupling agent.
The specific components of the metal powder, the metal oxide, the ceramic material, the silica gel, the silane coupling agent, and the carbon material in step S1 are the same as those in example 1.
Example 3
A preparation method of a heat-conducting interface material comprises the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 20 min; adding silica gel, and stirring for 20min under planetary vacuum; adding carbon fiber, planetary vacuum-pumping and stirring for 10min, wherein the vacuum degree is-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 1 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively.
S3, putting the container in the step S2 together with a weight on the container, vacuumizing the container to-0.09 MPa, and vacuumizing the container after 5 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa after 5 minutes, and compacting the material in a vibration compactor;
s4, curing: and (5) putting the sample obtained in the step S3 into an oven at 150 ℃ for 30min to obtain the product.
In the step S3, the weight applies a force of 700kgf to the container.
Wherein the preparation raw materials comprise the following components in parts by weight: 20 parts of silica gel, 35 parts of metal powder, 13 parts of metal oxide, 20 parts of carbon fiber and 5 parts of silane coupling agent.
The specific components of the metal powder, the metal oxide, the ceramic material, the silica gel, the silane coupling agent, and the carbon material in step S1 are the same as those in example 1.
Example 4
A preparation method of a heat-conducting interface material comprises the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 15 min; adding silica gel, and stirring for 15min in planetary vacuum pumping; adding carbon fiber, planetary vacuum-pumping and stirring for 5min, wherein the vacuum degree is-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 1 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively.
S3, putting the container in the step S2 together with a weight on the container, vacuumizing the container to-0.09 MPa in a vacuum drying box, and vacuumizing the container after 12 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa, vacuumizing after 12 minutes, and compacting the material in a vibration compactor;
s4, curing: and (5) putting the sample obtained in the step S3 into an oven at 120 ℃ for 60min to obtain the product.
In the step S3, the weight applies a force of 200kgf to the container.
Wherein, the specific components and the parts by weight of the metal powder, the metal oxide, the ceramic material, the silica gel, the silane coupling agent and the carbon material in the step S1 are the same as those in the embodiment 1.
Example 5
A preparation method of a heat-conducting interface material comprises the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 15 min; adding silica gel, and stirring for 15min in planetary vacuum pumping; adding carbon fiber, planetary vacuum-pumping and stirring for 5min, wherein the vacuum degree is-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 1 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively.
S3, putting the container in the step S2 together with a weight on the container, vacuumizing the container to-0.09 MPa, and vacuumizing the container after 2 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa after 2 minutes, and compacting the material in a vibration compactor;
s4, curing: and (5) putting the sample obtained in the step S3 into an oven at 120 ℃ for 60min to obtain the product.
In the step S3, the weight applies a force of 1000kgf to the container.
Wherein, the specific components and the parts by weight of the metal powder, the metal oxide, the ceramic material, the silica gel, the silane coupling agent and the carbon material in the step S1 are the same as those in the embodiment 1.
Example 6
A method for preparing a thermal interface material, which comprises the following specific steps of example 1:
s3, placing the container in the step S2 in a vacuum drying oven, vacuumizing to-0.09 MPa, vacuumizing after 8 minutes, and compacting the material in a vibration compactor; putting the container on a weight, putting the container and the weight into a vacuum drying oven, vacuumizing the vacuum drying oven to-0.09 MPa, and vacuumizing the vacuum drying oven after 8 minutes;
in the step S3, the weight applies a force of 600kgf to the container.
Wherein, the specific components and the parts by weight of the metal powder, the metal oxide, the ceramic material, the silica gel, the silane coupling agent and the carbon material in the step S1 are the same as those in the embodiment 1.
Example 7
A preparation method of a heat-conducting interface material comprises the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 15 min; adding silica gel, and stirring for 15min in planetary vacuum pumping; adding carbon fiber, planetary vacuum-pumping and stirring for 5min, wherein the vacuum degree is-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 2.5 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively.
S3, putting the container in the step S2 together with a weight on the container, vacuumizing the container to-0.09 MPa, and vacuumizing the container after 8 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa, vacuumizing after 8 minutes, and compacting the material in a vibration compactor;
s4, curing: and (5) putting the sample obtained in the step S3 into an oven at 120 ℃ for 60min to obtain the product.
In the step S3, the weight applies a force of 600kgf to the container.
Wherein, the specific components and the parts by weight of the metal powder, the metal oxide, the ceramic material, the silica gel, the silane coupling agent and the carbon material in the step S1 are the same as those in the embodiment 1.
Performance testing
Coefficient of thermal conductivity: test methods refer to standard astm d5470, unit: W/(m.K).
Hardness: the heat conductive interface material was placed under the pin-in device of the hardness tester for testing with a Shore OO hardness tester, and the data was stabilized after the occurrence of a "tic" sound 3 seconds after the device (as an average of five different positions) in units of: shore OO. See table 1 for details.
TABLE 1
| Examples | Coefficient of thermal conductivity | Hardness of |
| Example 1 | 32 | 48 |
| Example 2 | 28 | 47 |
| Example 3 | 29 | 47 |
| Example 4 | 20 | 37 |
| Example 5 | 19 | 34 |
| Example 6 | 17 | 31 |
| Example 7 | 14 | 40 |
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (3)
1. A preparation method of a heat conduction interface material is characterized by comprising the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 15 min; adding silica gel, and stirring for 15min in planetary vacuum pumping; adding carbon fiber, planetary vacuum-pumping and stirring for 5min, wherein the vacuum degree is-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 1 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively;
s3, putting the containers in the step S2 after being weighted together into a vacuum drying oven, vacuumizing to-0.09 MPa, and vacuumizing after 8 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa, vacuumizing after 8 minutes, and compacting the material in a vibration compactor;
s4, curing: putting the sample obtained in the step S3 into an oven at 120 ℃ for 60min to obtain the product;
in the step S3, the weight applies force to the container at 600 kgf;
the weight parts of the preparation raw materials are as follows: 18.8 parts of silica gel, 33.5 parts of metal powder, 10.6 parts of metal oxide, 16.5 parts of carbon fiber and 3.5 parts of silane coupling agent;
wherein the silica gel is of a Waker-9212A/B type and is purchased from Wake of Germany;
the metal powder consists of aluminum powder with the average particle size of 5 microns and aluminum powder with the average particle size of 40 microns; the weight ratio of the 10-micron aluminum powder to the 40-micron aluminum powder is 1: 1;
the molecular formula of the metal oxide is MxOyWherein M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm;
the carbon fibers have an average length of 150 microns;
the model of the silane coupling agent is KH 171;
the ceramic material is aluminum nitride, and the average grain diameter of the aluminum nitride is 1 micron.
2. A preparation method of a heat conduction interface material is characterized by comprising the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 5 min; adding silica gel, and stirring for 5min under planetary vacuum; adding carbon fiber, stirring for 1min under planetary vacuum, and vacuum degree of-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 1 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively;
s3, putting the containers in the step S2 after being weighted together into a vacuum drying oven, vacuumizing to-0.09 MPa, and vacuumizing after 10 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa, vacuumizing after 10 minutes, and compacting the material in a vibration compactor;
s4, curing: putting the sample obtained in the step S3 into an oven at 100 ℃ for 90min to obtain the product;
in the step S3, the weight applies force to the container at 400 kgf;
wherein the preparation raw materials comprise the following components in parts by weight: 15 parts of silica gel, 30 parts of metal powder, 8 parts of metal oxide, 12 parts of carbon fiber and 1 part of silane coupling agent;
wherein the silica gel is of a Waker-9212A/B type and is purchased from Wake of Germany;
the metal powder consists of aluminum powder with the average particle size of 5 microns and aluminum powder with the average particle size of 40 microns; the weight ratio of the 10-micron aluminum powder to the 40-micron aluminum powder is 1: 1;
the molecular formula of the metal oxide is MxOyWherein M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm;
the carbon fibers have an average length of 150 microns;
the model of the silane coupling agent is KH 171;
the ceramic material is aluminum nitride, and the average grain diameter of the aluminum nitride is 1 micron.
3. A preparation method of a heat conduction interface material is characterized by comprising the following steps:
s1, mixing raw materials: carrying out planetary vacuum pumping and stirring on a silane coupling agent, metal powder, metal oxide and a ceramic material for 20 min; adding silica gel, and stirring for 20min under planetary vacuum; adding carbon fiber, planetary vacuum-pumping and stirring for 10min, wherein the vacuum degree is-0.05 MPa;
s2, directional orientation: putting the mixed material obtained in the step S1 into an injection extruder, discharging the mixed material through a needle nozzle, arranging the mixed material in a container in a strip shape, stacking the mixed material to 1/3 height, compacting the material in a vibration compactor, and repeating stacking and compacting for 3 times, wherein the caliber of the needle nozzle is 1 mm;
the length, width and height of the container are 250mm, 150mm and 150mm respectively;
s3, putting the containers in the step S2 after being weighted together into a vacuum drying oven, vacuumizing to-0.09 MPa, and vacuumizing after 5 minutes; removing the heavy object, putting the container in a vacuum drying oven, vacuumizing to-0.09 MPa after 5 minutes, and compacting the material in a vibration compactor;
s4, curing: putting the sample obtained in the step S3 in an oven at 150 ℃ for 30min to obtain the product;
in step S3, the weight applies a force of 700kgf to the container;
wherein the preparation raw materials comprise the following components in parts by weight: 20 parts of silica gel, 35 parts of metal powder, 13 parts of metal oxide, 20 parts of carbon fiber and 5 parts of silane coupling agent;
wherein the silica gel is of a Waker-9212A/B type and is purchased from Wake of Germany;
the metal powder consists of aluminum powder with the average particle size of 5 microns and aluminum powder with the average particle size of 40 microns; the weight ratio of the 10-micron aluminum powder to the 40-micron aluminum powder is 1: 1;
the molecular formula of the metal oxide is MxOyWherein M is Zn, x is 1, and y is 1; the average particle diameter of the metal oxide is600nm；
The carbon fibers have an average length of 150 microns;
the model of the silane coupling agent is KH 171;
the ceramic material is aluminum nitride, and the average grain diameter of the aluminum nitride is 1 micron.
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