CN109020556B - Preparation method of boron nitride insulating heat dissipation film based on mixed sintering - Google Patents
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Abstract
The invention discloses a preparation method of a boron nitride insulating heat dissipation film based on mixed sintering, which comprises the steps of mixing and sintering two-dimensional boron nitride and cubic boron nitride to obtain the boron nitride insulating heat dissipation film which is more closely and orderly arranged and connected in a space mode, specifically, uniformly mixing two-dimensional boron nitride micro-tablets and cubic boron nitride micro-powder, directly assembling the mixture on a flexible substrate, obtaining the heat dissipation film through flat hydraulic pressure or double-roller hot pressing, and then sintering the heat dissipation film at a high temperature to form new chemical bonds between transverse two-dimensional layered boron nitride and between longitudinal two-dimensional layered boron nitride and cubic boron nitride to obtain the boron nitride heat dissipation film. Compared with the commercial metal radiating fin, the graphite radiating film and the graphene radiating film at present, the radiating film has better application prospect.
Description
Technical Field
The invention relates to a preparation method of a boron nitride insulating heat dissipation film based on mixed sintering, and belongs to the technical field of heat dissipation material preparation.
Background
Electronic equipment is becoming more and more essential in people's lives, and as electronic equipment continues to integrate more powerful functions into smaller components, increases in temperature can result in slower operating speeds of the equipment, failures during device operation, potential safety hazards, size space limitations, and many other performance issues. Temperature control has become one of the key challenges in design, namely how to effectively remove more heat generated by devices within a larger unit area with more efficient use of space and smaller operating spaces. Heat dissipation film products have been developed to address the ever-increasing heat dissipation needs of electronic products. At present, products in the industry mainly comprise natural graphite, artificial graphite and graphite thin heat dissipation films. The heat dissipation effect of natural graphite is the worst of the three materials due to the structural factors of natural graphite itself. The artificial graphite can be made very thin, has very good heat dissipation effect, and is mainly reflected in that the heat dissipation speed is high, but one big problem of the artificial graphite is that the price is relatively expensive. The graphene heat dissipation film becomes a product competing with artificial graphite along with the development of a graphene technology, and the heat conduction performance of the graphene heat dissipation film can far exceed that of the artificial graphite, so that the graphene heat dissipation film becomes a mainstream of a new generation of heat dissipation products.
In addition, the graphite film or the graphene film has a problem that they are conductive materials and have a risk of short circuit when applied to electronic products. Therefore, the finished product is required to be coated with glue and coated with film, the processing process is inconvenient, and the edges of graphite are easy to fall off during the die cutting process, so that the edge covering treatment is required, and the process cost is high and troublesome. In addition, the heat-conducting properties of the polymer materials used for the film-covered edge-covering and the like are poor, and the heat-radiating effect of the final heat-radiating film is influenced by the polymer materials. Based on the technical background, the invention provides a preparation method of a boron nitride insulating heat dissipation film, wherein boron nitride has excellent heat conduction capability, and the heat dissipation film prepared by the preparation method can be applied to electronic products to avoid short circuit risks.
Disclosure of Invention
The invention aims to provide a preparation method of a boron nitride insulating and heat dissipating film based on mixed sintering, aiming at the defects of the prior art.
A preparation method of a boron nitride insulating heat dissipation film based on hybrid sintering comprises the following steps:
(1) uniformly mixing and dispersing the two-dimensional boron nitride micro-slabs and the cubic boron nitride micro-powder in a solution to obtain a boron nitride dispersion liquid, so that the two-dimensional boron nitride micro-slabs and the cubic boron nitride particles are uniformly and alternately distributed in the solution;
(2) depositing a boron nitride solution layer on the flexible substrate and drying to obtain a boron nitride film layer, wherein the boron nitride solution can be deposited on the flexible substrate through spraying, casting, dipping and other processes; the two-dimensional boron nitride micro-slabs and the cubic boron nitride particles in the boron nitride film are uniformly mixed and distributed, and the cubic boron nitride particles are distributed between the two-dimensional boron nitride micro-slabs to form a layered structure;
(3) then, the two-dimensional boron nitride micro-sheets and cubic boron nitride particles are arranged more closely and orderly by a sample obtained by flat hydraulic pressure or double-roller hot-pressing calendering;
(4) and stripping the processed boron nitride heat dissipation film from the flexible substrate, and sintering to form chemical bonds between the transverse two-dimensional layered boron nitride and between the longitudinal two-dimensional layered boron nitride and the cubic boron nitride, thereby obtaining the boron nitride insulating heat dissipation film with a compact and ordered connection space structure.
In the technical scheme, the two-dimensional boron nitride micro-tablet in the step (1) is obtained by liquid phase stripping hexagonal boron nitride or ball milling hexagonal boron nitride, and the diameter of the micro-tablet is 10 nanometers to 100 micrometers; the cubic boron nitride micro powder is obtained by grinding cubic boron nitride into powder, and the particle size is 10 nanometers to 100 micrometers.
The solution in the step (1) is one or more of water, alcohol, NMP, DMF, acetone and IPA.
The flexible substrate in the step (2) is a polymer film or a metal film; the boron nitride solution layer may have a thickness of 100 nanometers to 100 millimeters.
And (4) the hot pressing temperature of the pair roller in the step (3) is 0-1500 ℃.
And (4) the thickness of the two-dimensional boron nitride insulating heat dissipation film in the step (3) after being rolled is 5 nanometers to 5 millimeters.
And (4) after the boron nitride insulating heat dissipation film is peeled off from the flexible substrate, sintering at 900-3000 ℃, wherein the atmosphere environment is one or more of nitrogen, argon, helium, hydrogen, oxygen, methane and the like.
The boron nitride insulating heat dissipation film obtained by mixing and sintering the two-dimensional boron nitride and the cubic boron nitride provided by the invention is formed by uniformly mixing the two-dimensional boron nitride micro-slabs and the cubic boron nitride micro-powder and then directly assembling the two-dimensional boron nitride micro-slabs and the cubic boron nitride micro-powder on a flexible substrate, so that the two-dimensional boron nitride micro-slabs and the cubic boron nitride particles are arranged in a close and ordered manner. And then the heat dissipation films with different thicknesses can be obtained through roller hot pressing or flat hydraulic pressure, and then the heat dissipation films are sintered at high temperature, so that new chemical bonds are formed between the transverse two-dimensional boron nitride and between the longitudinal two-dimensional layered boron nitride and the cubic boron nitride, and the heat conduction is more rapid in the transverse direction and the longitudinal direction. Because for two-dimensional boron nitride micro-slabs, heat is mostly conducted in a two-dimensional plane, while the heat transfer of cubic boron nitride is isotropic. The heat will be conducted faster between the transverse sheets after the chemical bond is formed between the transverse layered boron nitride, and the heat will be better conducted between the longitudinal sheet boron nitride and the cubic boron nitride after the cubic boron nitride forms a new chemical bond with the layered boron nitride, which will greatly improve the heat transfer performance in the longitudinal direction. The obtained boron nitride heat dissipation film can be directly applied to heat dissipation of electronic products, and safety accidents caused by short circuit can not be caused.
Drawings
FIG. 1 is a schematic view of the microstructure of the boron nitride insulating heat sink film of the present invention.
Fig. 2 is a schematic diagram of the chemical bond formed between two-dimensional boron nitride and cubic boron nitride.
FIG. 3 is a graph showing the heat dissipation test effect of the boron nitride insulating heat dissipation film of example 1.
FIG. 4 is a graph showing the heat dissipation test effect of the boron nitride insulating heat dissipation film of example 2.
Detailed Description
Example 1
(1) Ball-milling hexagonal boron nitride powder in ball-milling equipment at the rotating speed of 200rpm for 24 hours to obtain two-dimensional boron nitride micro-tablets, wherein the tablet diameter is about 100 microns and the two-dimensional boron nitride micro-tablets can be horizontally and flatly distributed;
(2) mixing the obtained boron nitride micro-tablets with cubic boron nitride micro-powder with the particle size of 1 micron and uniformly dispersing the mixture in an NMP solution under the assistance of ultrasound to obtain a boron nitride NMP dispersion liquid, so that the two-dimensional boron nitride micro-tablets and the cubic boron nitride particles are uniformly and alternately distributed in the NMP solution;
(3) casting a boron nitride solution layer with the thickness of 10 millimeters on a copper foil substrate with the thickness of 25 micrometers, and drying to obtain a boron nitride film layer, so that a boron nitride film with a compact and ordered internal structure is obtained, and the two-dimensional boron nitride and the cubic boron nitride are in a uniformly spaced layered structure;
(4) rolling the film into a boron nitride insulating heat dissipation film with the thickness of 525 microns at room temperature by a pair of rollers directly so as to obtain more compact and ordered arrangement;
(5) and stripping the imprinted boron nitride film from the copper foil substrate to obtain a boron nitride insulating heat dissipation film with the thickness of 500 microns, and sintering and annealing at 1300 ℃ in an argon atmosphere environment to form new chemical bonds between the transverse two-dimensional layered boron nitride and between the longitudinal two-dimensional layered boron nitride and the cubic boron nitride, so that the compact and orderly connected spatial structure boron nitride insulating heat dissipation film is obtained.
The microstructure of the boron nitride insulating heat dissipation film prepared by the steps is shown in figure 1, firstly, two-dimensional layered boron nitride (a layer structure in the figure) can be staggered and superposed with boron nitride particles (a spherical structure in the figure), and the boron nitride particles can be filled on the boron nitride particles superposed layer by layer to form more compact and ordered arrangement. After the heat dissipation films with different thicknesses are obtained through hot pressing of rollers or hydraulic pressure, the heat dissipation films are sintered at high temperature, so that new chemical bonds are formed between the transverse two-dimensional layered boron nitride and between the longitudinal two-dimensional layered boron nitride and the cubic boron nitride, as shown in fig. 2, and the heat dissipation films are beneficial to faster heat conduction in the transverse direction and the longitudinal direction. For two-dimensional boron nitride micro-slabs, heat is mostly conducted in a two-dimensional plane, while the heat transfer of cubic boron nitride is isotropic. The heat will be conducted faster between the transverse sheets after the chemical bond is formed between the transverse layered boron nitride, and the heat will be better conducted between the longitudinal sheet boron nitride and the cubic boron nitride after the cubic boron nitride forms a new chemical bond with the layered boron nitride, which will greatly improve the heat transfer performance in the longitudinal direction. This also allows heat to be quickly conducted in all directions of the boron nitride insulating heat dissipation film, resulting in excellent heat dissipation performance. The boron nitride insulating heat dissipation film is applied to the surfaces of the double cameras of the OPPO mobile phone to test the heat dissipation effect of the OPPO mobile phone, the heat dissipation film and a traditional copper foil are subjected to a comparison experiment, the real-time temperatures of the left camera and the right camera are tested by an FLIR thermal imager, and the test result is shown in figure 3. In the temperature displayed by the FLIR thermal imager, the temperature can be reduced by more than 6 ℃ by the heat dissipation film, and compared with the traditional metal heat dissipation film, graphite heat dissipation film and the like, the heat dissipation film has better cooling effect, is insulating and non-conductive, and has application superiority.
Example 2
(1) Ball-milling hexagonal boron nitride powder for 12 hours in ball-milling equipment at the rotating speed of 400rpm to obtain two-dimensional boron nitride micro-tablets, wherein the tablet diameter is about 1 micron and can be horizontally and flatly distributed;
(2) mixing the obtained boron nitride micro-tablets with cubic boron nitride micro-powder with the particle size of 10 nanometers and uniformly dispersing the mixture in a DMF solution under the assistance of ultrasound to obtain boron nitride DMF dispersion liquid, so that the obtained two-dimensional boron nitride micro-tablets and cubic boron nitride particles are uniformly and alternately distributed in the DMF solution;
(3) spraying a boron nitride solution layer with the thickness of 10 microns on a copper foil substrate with the thickness of 25 microns, and drying to obtain a boron nitride film layer, so that a compact and ordered boron nitride film is obtained, and the boron nitride film layer is in a layered structure formed by two-dimensional boron nitride and cubic boron nitride in an interval arrangement;
(4) rolling the mixture at 500 ℃ to form a boron nitride insulating heat dissipation film with the thickness of 25.5 microns so as to obtain more compact and ordered arrangement;
(5) and stripping the stamped copper/boron nitride film, stripping boron nitride from the copper substrate to obtain a 500-nanometer-thick two-dimensional boron nitride insulating heat dissipation film, and sintering at 1500 ℃ in a nitrogen atmosphere environment to form new chemical bonds between the transverse two-dimensional layered boron nitride and between the longitudinal two-dimensional layered boron nitride and the cubic boron nitride, so as to obtain the compact and orderly-connected boron nitride insulating heat dissipation film.
The boron nitride insulating heat dissipation film prepared by the steps is applied to the surfaces of the double cameras of the OPPO mobile phone to test the heat dissipation effect, the boron nitride insulating heat dissipation film is compared with the traditional copper foil for experiment, the real-time temperature of the left camera and the right camera is tested by an FLIR thermal imager, and the test result is shown in FIG. 4. In the temperature displayed by the FLIR thermal imager, the temperature can be reduced by 4 to 5 ℃ in the same ratio by applying the heat dissipation film, and compared with the traditional metal heat dissipation film, graphite heat dissipation film and the like, the heat dissipation film has better cooling effect, and meanwhile, the heat dissipation film is insulating and non-conductive and has more superiority.
Example 3
(1) Ultrasonically dispersing hexagonal boron nitride powder in water in a 40KHz ultrasonic device for 24 hours to obtain an aqueous dispersion of two-dimensional boron nitride micro-tablets, wherein the tablet diameter is about 5 microns and the two-dimensional boron nitride micro-tablets can be transversely and flatly distributed;
(2) mixing the obtained boron nitride micro-tablets with cubic boron nitride micro-powder with the particle size of 50 nanometers and uniformly dispersing the mixture in an aqueous solution under the assistance of ultrasound to obtain a boron nitride aqueous dispersion liquid, so that the obtained two-dimensional boron nitride micro-tablets and cubic boron nitride particles are uniformly and alternately distributed in the aqueous solution;
(3) casting a boron nitride solution layer with the thickness of 200 microns on a PET substrate with the thickness of 20 microns, and drying to obtain a boron nitride film layer, so that a more compact and ordered boron nitride film is obtained, and the boron nitride film layer is in a layered structure formed by alternately arranging two-dimensional boron nitride and cubic boron nitride;
(4) rolling the film into a boron nitride insulating heat dissipation film with the thickness of 30 microns at 1500 ℃ by a roller directly so as to obtain more compact and ordered arrangement;
(5) stripping the imprinted boron nitride film from the PET substrate to obtain a 10-micron-thick two-dimensional boron nitride insulating heat dissipation film, and sintering the film in a mixed atmosphere environment of 1200 ℃ and hydrogen and argon, so that new chemical bonds are formed between transverse two-dimensional layered boron nitride and between longitudinal two-dimensional layered boron nitride and cubic boron nitride, and the compact and orderly-connected boron nitride insulating heat dissipation film is obtained.
Example 4
(1) Ultrasonically dispersing hexagonal boron nitride powder in water in a 40KHz ultrasonic device for 24 hours to obtain NMP dispersion liquid of two-dimensional boron nitride micro-tablets, wherein the tablet diameter is about 10 microns and the two-dimensional boron nitride micro-tablets can be horizontally and flatly distributed;
(2) mixing the obtained boron nitride micro-tablets with cubic boron nitride micro-powder with the particle size of 100 nanometers and uniformly dispersing the mixture in an NMP solution under the assistance of ultrasound to obtain a boron nitride NMP dispersion liquid, so that the obtained two-dimensional boron nitride micro-tablets and cubic boron nitride particles are uniformly and alternately distributed in the NMP solution;
(3) casting a boron nitride layer with the thickness of 300 microns on a copper foil substrate with the thickness of 20 microns, and drying to obtain a boron nitride film layer, so that a more compact and ordered boron nitride film is obtained, and the boron nitride film layer is in a layered structure formed by alternately arranging two-dimensional boron nitride and cubic boron nitride;
(4) feeding a boron nitride insulating heat dissipation film with the thickness of 35 microns on a flat hydraulic press to obtain more compact and ordered arrangement;
(5) and stripping the hydraulic boron nitride film from the copper foil substrate to obtain a two-dimensional boron nitride insulating heat dissipation film with the thickness of 15 microns, and sintering the two-dimensional boron nitride insulating heat dissipation film at 2400 ℃ in a helium atmosphere environment to form new chemical bonds between the transverse two-dimensional layered boron nitride and between the longitudinal two-dimensional layered boron nitride and the cubic boron nitride, so as to obtain the compact and orderly connected boron nitride insulating heat dissipation film.
Example 5
(1) Ultrasonically dispersing hexagonal boron nitride powder in water in a 40KHz ultrasonic device for 24 hours to obtain an alcohol dispersion liquid of two-dimensional boron nitride micro-tablets, wherein the tablet diameter is about 20 microns and the hexagonal boron nitride powder can be horizontally and flatly distributed;
(2) mixing the obtained boron nitride micro-tablets with cubic boron nitride micro-powder with the particle size of 200 nanometers and uniformly dispersing the mixture in alcohol under the assistance of ultrasound to obtain boron nitride alcohol dispersion liquid, so that the obtained two-dimensional boron nitride micro-tablets and cubic boron nitride particles are uniformly and alternately distributed in the alcohol solution;
(3) casting a boron nitride solution layer with the thickness of 2 millimeters on a PET substrate with the thickness of 20 micrometers, and drying to obtain a boron nitride film layer, so that a more compact and ordered boron nitride film is obtained, and the boron nitride film layer is in a layered structure formed by alternately arranging two-dimensional boron nitride and cubic boron nitride;
(4) hydraulically pressing the mixture into a boron nitride insulating heat dissipation film with the thickness of 120 microns on a roller hydraulic press so as to obtain more compact and ordered arrangement;
(5) and stripping the hydraulic boron nitride film from the PET substrate to obtain a two-dimensional boron nitride insulating heat dissipation film with the thickness of 100 microns, and sintering the two-dimensional boron nitride insulating heat dissipation film at 2000 ℃ in an argon atmosphere environment to form new chemical bonds between the transverse two-dimensional layered boron nitride and between the longitudinal two-dimensional layered boron nitride and the cubic boron nitride, so as to obtain the compact and orderly connected boron nitride insulating heat dissipation film.
Claims (6)
1. A preparation method of a boron nitride insulating heat dissipation film based on hybrid sintering is characterized by comprising the following steps:
(1) uniformly mixing and dispersing the two-dimensional boron nitride micro-slabs and the cubic boron nitride micro-powder in a solution to obtain a boron nitride dispersion liquid, so that the two-dimensional boron nitride micro-slabs and the cubic boron nitride particles are uniformly and alternately distributed in the solution;
(2) depositing a boron nitride solution layer on a flexible substrate and drying to obtain a boron nitride film layer, wherein two-dimensional boron nitride micro-sheets and cubic boron nitride particles in the boron nitride film are uniformly mixed and distributed;
(3) then, the two-dimensional boron nitride micro-sheets and cubic boron nitride particles are arranged more closely and orderly by a sample obtained by flat hydraulic pressure or double-roller hot-pressing calendering;
(4) and stripping the processed boron nitride heat dissipation film from the flexible substrate, and sintering at 900-3000 ℃ in one or more of nitrogen, helium, argon, hydrogen, oxygen and methane to form chemical bonds between the transverse two-dimensional layered boron nitride and between the longitudinal two-dimensional layered boron nitride and the cubic boron nitride, so as to obtain the boron nitride insulating heat dissipation film with a compact and orderly connected spatial structure.
2. The method for preparing the boron nitride insulating and heat dissipating film based on hybrid sintering as claimed in claim 1, wherein the two-dimensional boron nitride micro-slabs in step (1) are obtained by liquid phase stripping hexagonal boron nitride or ball milling hexagonal boron nitride micro-slabs, and the slab diameter is 10 nm to 100 μm; the cubic boron nitride micro powder is obtained by grinding cubic boron nitride into powder, and the particle size is 10 nanometers to 100 micrometers.
3. The method for preparing the boron nitride insulating heat dissipation film based on hybrid sintering as claimed in claim 1, wherein the solution in step (1) is one or more of water, alcohol, NMP, DMF, acetone, and IPA.
4. The method for preparing the boron nitride insulating and heat dissipating film based on hybrid sintering as claimed in claim 1, wherein the flexible substrate in step (2) is a polymer film or a metal film.
5. The method for preparing the boron nitride insulating and heat dissipating film based on hybrid sintering as claimed in claim 1, wherein the hot pressing temperature of the pair of rollers in the step (3) is 0 ℃ to 1500 ℃.
6. The method for preparing the boron nitride insulating and heat dissipating film based on hybrid sintering as claimed in claim 1, wherein the thickness of the boron nitride insulating and heat dissipating film obtained in step (3) after rolling is 5 nm to 5 mm.
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| EP3214059A1 (en) * | 2014-10-29 | 2017-09-06 | Tungaloy Corporation | Cubic boron nitride sintered body, and coated cubic boron nitride sintered body |
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