CN115625938A - Boron nitride heat conduction gasket with high orientation degree and high out-of-plane heat conductivity, and preparation method and application thereof - Google Patents
Boron nitride heat conduction gasket with high orientation degree and high out-of-plane heat conductivity, and preparation method and application thereof Download PDFInfo
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
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- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/545—Polyvinyl alcohol
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- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
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Abstract
The invention discloses a boron nitride heat conduction gasket with high orientation degree and high out-of-plane heat conductivity, and a preparation method and application thereof. In the work, a large-area foldable boron azide nanosheet (boron nitride) based film is prepared by an electrostatic spinning method. And stacking the multiple layers of films, carrying out hot pressing, and cutting to obtain the boron nitride heat-conducting gasket. Since boron nitride has good micro-orientation and dense packing, the direction of cutting is perpendicular to the orientation of the film, and the resulting gasket has excellent out-of-plane thermal conductivity and good electrical insulation. The thermal conductivity is 18W/(m.K) to 21W/(m.K); volume resistivity of 2.0X 10 9 Ω·cm～4.0×10 9 Ω·cm。
Description
Technical Field
The invention belongs to the technical field of heat-conducting gaskets, and relates to a boron nitride heat-conducting gasket with high orientation degree and high out-of-plane heat conductivity, and a preparation method and application thereof.
Background
With the development of high-performance computing, artificial intelligence, and other GPU computing and cloud computing, microprocessors are developing towards higher power densities, larger chips, and higher frequencies. Thermal management of microprocessors is one of the biggest bottlenecks in improving performance and integration density. For example, current data centers consume more than 200 trillion watt-hours of electricity per year, with over 50% of the total electricity being used to remove excess heat rather than for data storage or computation. In both small mobile electronic devices and large communication terminals, waste heat from the heat source (chip) is dissipated into the heat sink through a series of thermal resistances of the multiple device layers and their interfaces. Therefore, if the waste heat cannot be removed in time, the performance, reliability and service life of the electronic product are seriously affected.
Thermal Interface Materials (TIMs) are used between the die and the heat spreader, and between the heat spreader and the heat spreader, to improve heat dissipation efficiency, topography, and distribution by enhancing thermal coupling and minimizing thermal resistance between non-uniform components. Simply and roughly distributing the boron nitride filler in the polymer system will undoubtedly increase the phonon scattering and increase the interface thermal resistance.
In the traditional thought, researchers only simply physically mix the filler and the polymer matrix, and cannot regulate and control the orientation and arrangement of the filler, so that high thermal conductivity is difficult to realize. In order to enhance the heat-conducting property of the gasket, researches focus on selecting new high-heat-conducting fillers or constructing a three-dimensional network and a vertical orientation structure to improve the heat-conducting efficiency. Cui et al prepared epoxy-based TIMs with a thermal conductivity of 21 W.m by arranging cubic boron arsenide along the growth direction of ice crystals using an ice template method -1 ·K -1 Unfortunately, the preparation of the ice template method is complicated and difficult to implement.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide a boron nitride thermal conductive gasket with high degree of orientation and high out-of-plane thermal conductivity, and a preparation method and an application thereof. In the work, the large-area foldable boron nitride nanosheet-based film is prepared by an electrostatic spinning method. And stacking the multiple layers of films, carrying out hot pressing, and cutting to obtain the boron nitride heat-conducting gasket. Since boron nitride has good micro-orientation and dense packing, the direction of cutting is perpendicular to the orientation of the film, and the resulting gasket has excellent out-of-plane thermal conductivity and good electrical insulation.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a boron nitride heat conduction gasket with high orientation degree and high out-of-plane thermal conductivity, the heat conduction gasket is a three-dimensional structure formed by stacking a plurality of boron nitride film structures, and two adjacent boron nitride film structures are connected with each other through polyvinyl alcohol; the boron nitride film structure comprises a boron nitride sheet and nano silver particles uniformly distributed on the boron nitride sheet.
Further, the mass percentage of boron nitride is 70% to 85%, for example, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85% with respect to 100% of the total mass of the thermal conductive gasket; the density of the heat-conducting gasket is 2.0g/cm 3 ～2.4g/cm 3 The thickness is 1.2 mm-4.6 mm; wherein the diameter of the boron nitride sheet is 6-13 μm.
In a second aspect, the present invention provides a method for preparing a boron nitride thermal conductive gasket with high degree of orientation and high out-of-plane thermal conductivity, the method comprising the following steps: (1) preparation of boron nitride dispersion: placing boron nitride and polyvinylpyrrolidone (PVP) in a reactor, pouring N, N-Dimethylformamide (DMF) to obtain a boron nitride dispersion liquid, and carrying out ultrasonic treatment on the boron nitride dispersion liquid; (2) preparing boron nitride-Ag powder: adding deionized water into silver nitrate to obtain a silver nitrate aqueous solution; heating the boron nitride dispersion liquid in an oil bath, dripping the silver nitrate aqueous solution into the boron nitride dispersion liquid, and standing after complete dripping; pouring out, carrying out suction filtration, washing with deionized water and absolute ethyl alcohol, and drying to obtain boron nitride-Ag powder; (3) preparing a PVA aqueous solution; (4) Mixing the boron nitride-Ag powder with the PVA aqueous solution to obtain a boron nitride-Ag/PVA dispersion liquid; (5) Pumping the boron nitride-Ag/PVA dispersion liquid into a needle tube, and spinning to obtain a boron nitride-Ag/PVA film structure; (6) And stacking a plurality of film structures of the boron nitride-Ag/PVA, carrying out hot pressing to obtain a boron nitride-Ag/PVA bulk material, and cutting the boron nitride-Ag/PVA bulk material along a direction vertical to a film plane to obtain the boron nitride heat conduction gasket with high orientation degree and high out-of-plane heat conductivity.
Further, in the step (1), the mass ratio of the boron nitride to the polyvinylpyrrolidone to the DMF is 10: (3-7): (200-400); the ultrasonic treatment time is 15min to 30min, such as 15min, 18min, 20min, 22min, 25min, 28min, 30min and the like.
Further, in the step (2), the mass ratio of the boron nitride to the silver nitrate is 5: (2-4.5); the mass ratio of the silver nitrate to the deionized water is 1: (3-7); the temperature of the oil bath in the round bottom flask is 55-62 ℃, such as 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, 60 ℃, 61 ℃, 62 ℃ and the like; the stirring rate of the boron nitride-Ag/PVA dispersion is 250rpm to 400rpm, for example, 2500rpm, 330rpm, 340rpm, 360rpm, 380rpm, 400rpm, and the like.
Further, in the step (3), the mass ratio of PVA to water in the aqueous PVA solution is (3 to 9): 100.
further, in the step (4), the mass ratio of the boron nitride to the PVA is (0.35 to 6): 1.
further, the step (5) specifically includes the following steps: pumping the dispersion liquid of the boron nitride-Ag/PVA into a 20mL needle tube, and placing the needle tube into an electrostatic spinning machine; adjusting the movement distance of the electrostatic spinning nozzle to be 60 mm-100 mm, such as 60mm, 70mm, 80mm, 90mm, 100mm and the like; adjusting the rolling speed of the receiver roller to 1000 rpm-1500 rpm, such as 1000rpm, 1100rpm, 1200rpm, 1300rpm, 1400rpm, 1500rpm, etc.; adjusting and controlling the pump speed of the needle tube to ensure that the spraying speed of the mixed liquid is between 3mL/h and 6mL/h, such as 3mL/h, 4mL/h, 5mL/h, 6mL/h and the like; adjusting the positive and negative electrode voltages of the electrostatic spinning machine, wherein the positive electrode is 18 kv-22 kv, the negative electrode is-8 kv-12 kv, such as 18kv and-8 kv of the positive electrode, 20kv and-10 kv of the negative electrode, 22kv and-12 kv of the positive electrode, and the like; the spinning time is 4h-6h, such as 4h, 4.5h, 5h, 5.5h, 6h and the like.
Further, the step (6) specifically includes the following steps: tearing the boron nitride-Ag/PVA film structure from the receiver, cutting into 1cm 2 And stacked together, the stacking thickness is 1.5cm; placing the stacked boron nitride-Ag/PVA film structure into a hot press, and heating at 80-105 deg.C (for exampleHot pressing at 80 deg.C, 85 deg.C, 90 deg.C, 95 deg.C, 100 deg.C, 105 deg.C, etc.) and 10-20 MPa (e.g., 10MPa, 12MPa, 14MPa, 16MPa, 18MPa, 20MPa, etc.) to obtain boron nitride-Ag/PVA bulk structure; the boron nitride-Ag/PVA bulk structure is put into a cutting machine and cut along the direction perpendicular to the membrane structure, and the cutting thickness is 3 mm-5.6 mm, such as 3mm, 3.2mm, 3.6mm, 4mm, 4.2mm, 4.6mm, 4.8mm, 5mm, 5.2mm, 5.6mm and the like.
A third aspect of the present invention provides the use of a boron nitride thermal gasket having a high degree of orientation and a high out-of-plane thermal conductivity as described above in the field of heat dissipation.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a boron nitride heat conduction gasket with high orientation degree and high out-of-plane thermal conductivity, a preparation method and application thereof, wherein the heat conduction gasket is composed of a boron nitride sheet, ag filler and PVA, wherein nano silver particles of the filler are uniformly distributed on the boron nitride sheet, and the nano silver particles have a sintering effect after hot pressing, so that a new heat path is increased, and meanwhile, the binding force between boron nitrides is enhanced.
The boron nitride sheet-Ag filler was bonded by polyvinyl alcohol (PVA). Electrospinning at high electric field strengths first allowed the fillers to undergo initial in-plane alignment and fully cross-linked adjacent BNNS together by PVA. The subsequent hot pressing further improves the orientation degree and the filling density of the gasket, promotes PVA with viscosity to fill space gaps, and finally forms a compact structure. The prepared gasket not only has very high heat conductivity coefficient, but also has good electric insulation performance, and the heat conductivity coefficient is 18W/(m.K) -21W/(m.K); volume resistivity of 2.0X 10 9 Ω·cm～4.0×10 9 Ω·cm。
Drawings
One or more embodiments are illustrated by corresponding figures in the drawings, which are not to be construed as limiting the embodiments, unless expressly stated otherwise, and the drawings are not to scale.
Fig. 1 is a schematic structural view of a boron nitride thermal gasket obtained in example 1;
wherein, 1 is a heat-conducting gasket, 11 is a boron nitride film structure, 12 is polyvinyl alcohol, 111 is a boron nitride sheet, and 112 is nano silver particles.
Detailed Description
In order to solve the problems in the prior art, the invention provides a boron nitride heat conduction gasket with high orientation degree and high out-of-plane thermal conductivity, and a preparation method and application thereof.
The first aspect of the present invention provides a boron nitride thermal conduction pad 1 with high orientation degree and high out-of-plane thermal conductivity, as shown in fig. 1, the thermal conduction pad 1 is a three-dimensional structure formed by stacking a plurality of boron nitride film structures 11, and two adjacent boron nitride film structures 11 are connected to each other through the polyvinyl alcohol 12; the boron nitride film structure 11 includes a boron nitride sheet 111, and nano-silver particles 112 uniformly distributed on the boron nitride sheet 111.
In a second aspect, the present invention provides a method for preparing a boron nitride thermal conductive gasket with high degree of orientation and high out-of-plane thermal conductivity, the method comprising the following steps: (1) preparation of boron nitride dispersion: placing boron nitride and polyvinylpyrrolidone (PVP) in a reactor, pouring N, N-Dimethylformamide (DMF) to obtain a boron nitride dispersion liquid, and placing the boron nitride dispersion liquid in an ultrasonic cleaning machine for ultrasonic treatment; (2) preparing boron nitride-Ag powder: adding deionized water into silver nitrate to obtain a silver nitrate aqueous solution; pouring the boron nitride dispersion liquid into a round-bottom flask, placing the round-bottom flask into an oil bath pan for oil bath heating, dripping the silver nitrate aqueous solution into the boron nitride dispersion liquid by using a constant-pressure funnel, and standing after complete dripping; pouring out, carrying out suction filtration, washing with deionized water and absolute ethyl alcohol, and drying in an oven to obtain boron nitride-Ag powder; (3) preparing a PVA aqueous solution; (4) Putting the boron nitride-Ag powder and the PVA aqueous solution into a mixer for mixing to obtain a boron nitride-Ag/PVA dispersion liquid; (5) Sucking the boron nitride-Ag/PVA dispersion liquid into a needle tube, and spinning by using an electrostatic spinning machine to obtain a boron nitride-Ag/PVA film structure; (6) Stacking a plurality of film structures of the boron nitride-Ag/PVA, putting the film structures into a hot press, carrying out hot pressing to obtain a boron nitride-Ag/PVA bulk material, and putting the boron nitride-Ag/PVA bulk material into a cutting machine to cut along a direction vertical to a film plane to obtain the boron nitride heat conduction gasket with high orientation degree and high out-of-plane heat conductivity.
A third aspect of the present invention provides the use of a boron nitride thermal gasket having a high degree of orientation and a high out-of-plane thermal conductivity as described above in the field of heat dissipation.
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The thermally conductive composites prepared in the examples and comparative examples were tested for thermal conductivity and volume resistivity, wherein the thermal conductivity was tested according to the standard test method for determining thermal diffusivity according to the american standard ASTM E1461 flash method; the volume resistivity was measured according to the test method for measuring the volume resistivity and surface resistivity of an organic substrate material by using the volume resistivity and surface resistivity of an IPC-TM-6502.5.17.1 insulating material.
Example 1
(1) Preparation of BNNS dispersion: 5g of BNNS was placed in a beaker, and PVP (3 g) was added in a BNNS: polyvinylpyrrolidone (PVP) mass ratio of 5.
(2) BNNS silver growing step: taking BNNS to silver nitrate in a mass ratio of 10:9 silver nitrate (4.5 g) in a test tube, 20mL of deionized water was added to prepare an aqueous silver nitrate solution. The BNNS dispersion prepared in step (1) was poured into a round bottom flask and the round bottom flask was placed in an oil bath, heated to 62 ℃ and stirred at 350 rpm. The aqueous silver nitrate solution was dropped into the BNNS dispersion using a constant pressure funnel at a rate of 7s to 10 s/drop, and reacted for 2 hours. After 2h, the silver nitrate aqueous solution was added to the dispersion, and the stirring speed was adjusted to 200rpm and stirred for 24h. And then, guiding out, carrying out suction filtration, washing for 3 times by using 300mL of deionized water, washing for 2 times by using 50mL of absolute ethyl alcohol, and then putting into an oven for drying to obtain BNNS-Ag powder.
(3) Preparing a PVA aqueous solution: PVA (12 g) with the molecular weight of 10000 is taken in a beaker, 250mL of water is added, the temperature is heated to 90 ℃, the stirring is carried out until the solution is evaporated to the total mass of 200g, and PVA aqueous solution with the PVA wt% =6% is obtained.
(4) And (3) mixing the BNNS-Ag powder (5 g) obtained in the step (3) and the PVA aqueous solution (14.7 g) obtained in the step (3) in a mixer to obtain a BNNS-Ag wt% =85% BNNS-Ag/PVA dispersion liquid.
(5) And (4) pumping the dispersion liquid obtained in the step (3) by using a 20mL needle tube, and spinning by using an electrostatic spinning machine to obtain a BNNS-Ag/PVA film structure.
(7) And (3) putting the membrane structure obtained in the step (6) into a hot press, carrying out hot pressing for 1h at 105 ℃ under 20Mpa to obtain a block material, and then cutting the block material into a gasket with the thickness of 3mm in a cutting machine, wherein the product is named as BNNS-Ag (L)/PVA.
The heat conducting gasket prepared in the embodiment is subjected to heat conducting and volume resistivity performance index tests, the heat conducting coefficient is 21W/m.K, and the volume resistivity is 2.8 multiplied by 10 9 Ω·cm。
Example 2
The procedure was as in example 1 except that in step (2), the mass ratio of BNNS to silver nitrate was changed to 10: 10 instead of 10, and the product was named BNNS-Ag (S)/PVA.
The heat conducting gasket prepared in the embodiment is subjected to heat conducting and volume resistivity performance index tests, the heat conducting coefficient is 7W/m.K, and the volume resistivity is 6.2 multiplied by 10 9 Ω·cm。
Example 3
The same procedure as in example 1 was repeated except that in step (6), the hot pressing was carried out at 105 ℃ and 20MPa for 1 hour, instead of at 105 ℃ and 10MPa for 1 hour, and the product was named BNNS-Ag (L)/PVA-10.
The heat conducting gasket prepared in the embodiment is subjected to heat conducting and volume resistivity performance index tests, the heat conducting coefficient is 17W/m.K, and the volume resistivity is 3.6 multiplied by 10 9 Ω·cm。
Example 4
The same procedure as in example 1 was repeated except that in step (6), the hot pressing was carried out at 105 ℃ and 20MPa for 1 hour, instead of at 80 ℃ and 20MPa for 1 hour, and the product was named BNNS-Ag (L)/PVA-80.
The heat conducting gasket prepared by the embodiment is subjected to heat conducting and volume resistivity performance index tests, and the heat conducting coefficient is 15.6W/m.K, volume resistivity of 4.2X 10 9 Ω·cm。
Example 5
The same procedure as in example 1 was repeated except that the gasket cut to a thickness of 3mm in the cutter in step (6) was replaced with a gasket cut to a thickness of 5mm, and the product was named BNNS-Ag (L)/PVA-5.
The heat conducting gasket prepared in the embodiment is subjected to heat conducting and volume resistivity performance index tests, the heat conducting coefficient is 17.8W/m.K, and the volume resistivity is 4.4 multiplied by 10 9 Ω·cm。
Example 6
The same procedure as in example 1 was repeated except that the dispersion of BNNS-Ag/PVA having BNNS-Ag wt% =85% obtained in step (4) was replaced with a dispersion of BNNS-Ag/PVA having BNNS-Ag wt% =70% obtained by cutting, and the product was named BNNS-Ag (L)/PVA-70.
The heat conducting gasket prepared in the embodiment is subjected to heat conducting and volume resistivity performance index tests, the heat conducting coefficient is 14.2W/m.K, and the volume resistivity is 8.4 multiplied by 10 9 Ω·cm。
Example 7
The same procedure as in example 1 was repeated except that the dispersion of BNNS-Ag/PVA having BNNS-Ag wt% =85% obtained in step (4) was replaced with a dispersion of BNNS-Ag/PVA having BNNS-Ag wt% =50% cut, and the product was named BNNS-Ag (L)/PVA-50.
The heat conducting gasket prepared in the embodiment is subjected to heat conducting and volume resistivity performance index tests, the heat conducting coefficient is 9.8W/m.K, and the volume resistivity is 1.2 multiplied by 10 10 Ω·cm。
Comparative example 1
(1) Preparing a PVA aqueous solution: PVA (12 g) with the molecular weight of 10000 is taken in a beaker, 250mL of water is added, the temperature is heated to 90 ℃, the stirring is carried out until the solution is evaporated to the total mass of 200g, and PVA aqueous solution with the PVA wt% =6% is obtained.
(2) Mixing BNNS powder (5 g) and the PVA aqueous solution (14.7 g) obtained in the step (1) in a mixer to obtain a BNNS-/PVA dispersion liquid with BNNS wt% = 85%.
(3) And (3) pumping the dispersion liquid obtained in the step (2) by using a 20mL needle tube, and spinning by using an electrostatic spinning machine to obtain a BNNS/PVA film structure.
(4) And (3) putting the membrane structure obtained in the step (3) into a hot press, carrying out hot pressing for 1h at 105 ℃ under 20Mpa to obtain a block material, and then cutting the block material into a gasket with the thickness of 3mm in a cutting machine, wherein the product is named as BNNS/PVA.
The heat conducting gasket prepared in the embodiment is subjected to heat conducting and volume resistivity performance index tests, the heat conducting coefficient is 3W/m.K, and the volume resistivity is 4.0 multiplied by 10 11 Ω·cm。
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples of implementations of the present application, and that various changes in form and details may be made therein without departing from the spirit and scope of the present application. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the scope or spirit of the present disclosure, and the scope of the present disclosure should be defined only by the appended claims.
Claims (10)
1. The boron nitride heat conduction gasket with high orientation degree and high out-of-plane thermal conductivity is characterized in that the heat conduction gasket is a three-dimensional structure formed by stacking a plurality of boron nitride film structures, and two adjacent boron nitride film structures are connected with each other through the polyvinyl alcohol;
the boron nitride film structure comprises a boron nitride sheet and nano silver particles uniformly distributed on the boron nitride sheet.
2. The boron nitride thermal pad according to claim 1, wherein the mass percentage of boron nitride is 70-85% based on 100% of the total mass of the thermal pad;
the density of the heat-conducting gasket is 2.0g/cm 3 ～2.4g/cm 3 The thickness is 1.2 mm-4.6 mm;
wherein the diameter of the boron nitride sheet is 6-13 μm.
3. The method of making a boron nitride thermal gasket of high degree of orientation and high out-of-plane thermal conductivity as claimed in claim 1 or 2, comprising the steps of:
(1) Preparing a boron nitride dispersion liquid: placing boron nitride and polyvinylpyrrolidone (PVP) in a reactor, pouring N, N-dimethylformamide to obtain a boron nitride dispersion liquid, and carrying out ultrasonic treatment on the boron nitride dispersion liquid;
(2) Preparing boron nitride-Ag powder: adding deionized water into silver nitrate to obtain a silver nitrate aqueous solution; heating the boron nitride dispersion liquid in an oil bath, dripping the silver nitrate aqueous solution into the boron nitride dispersion liquid, and standing after complete dripping; pouring out, performing suction filtration, cleaning with deionized water and absolute ethyl alcohol, and drying to obtain boron nitride-Ag powder;
(3) Preparing PVA water solution;
(4) Mixing the boron nitride-Ag powder with the PVA aqueous solution to obtain a boron nitride-Ag/PVA dispersion liquid;
(5) Pumping the boron nitride-Ag/PVA dispersion liquid into a needle tube, and spinning to obtain a boron nitride-Ag/PVA film structure;
(6) And stacking a plurality of the boron nitride-Ag/PVA film structures, then carrying out hot pressing to obtain a boron nitride-Ag/PVA bulk material, and cutting the boron nitride-Ag/PVA bulk material along a direction vertical to the film plane to obtain the boron nitride heat conduction gasket with high orientation degree and high out-of-plane thermal conductivity.
4. The method for preparing the boron nitride thermal conduction gasket with high orientation degree and high out-of-plane thermal conductivity according to claim 3, wherein in the step (1), the mass ratio of the boron nitride to the polyvinylpyrrolidone to the N, N-dimethylformamide is 10: (3-7): (200-400);
the ultrasonic treatment time is 15 min-30 min.
5. The method for preparing a boron nitride thermal gasket with high degree of orientation and high out-of-plane thermal conductivity as claimed in claim 3, wherein in the step (2), the mass ratio of the boron nitride to the silver nitrate is 5: (2-4.5);
the mass ratio of the silver nitrate to the deionized water is 1: (3-7);
the temperature of the round bottom flask oil bath is 55-62 ℃;
the stirring speed of the boron nitride-Ag/PVA dispersion liquid is 250 rpm-400 rpm.
6. The method for preparing a boron nitride thermal pad with high degree of orientation and high out-of-plane thermal conductivity according to claim 3, wherein in the step (3), the mass ratio of PVA to water in the PVA aqueous solution is (3-9): 100.
7. the method for preparing a boron nitride thermal pad with high degree of orientation and high out-of-plane thermal conductivity according to claim 3, wherein in the step (4), the mass ratio of the boron nitride to the PVA is (0.35-6): 1.
8. the method for preparing the boron nitride thermal conduction gasket with high orientation degree and high out-of-plane thermal conductivity according to claim 3, wherein the step (5) specifically comprises the following steps:
sucking the dispersion liquid of the boron nitride-Ag/PVA into a 20mL needle tube, and placing the mixture in an electrostatic spinning machine;
adjusting the movement distance of the electrostatic spinning nozzle to be 60-100 mm;
adjusting the rolling speed of the receiver roller to 1000-1500 rpm;
adjusting the pump rate of the control needle tube to ensure that the ejection rate of the mixed liquid is between 3mL/h and 6mL/h;
adjusting the voltage of the anode and the cathode of the electrostatic spinning machine, wherein the anode is 18 kv-22 kv, and the cathode is-8 kv-12 kv;
the spinning time is 4-6 h.
9. The method for preparing the boron nitride thermal conduction gasket with high orientation degree and high out-of-plane thermal conductivity according to claim 3, wherein the step (6) specifically comprises the following steps:
the film of boron nitride-Ag/PVAThe structure is taken off from the receiver and cut into 1cm 2 And stacked together to a stack thickness of 1.5cm;
putting the stacked boron nitride-Ag/PVA film structure into a hot press, and hot-pressing at 80-105 ℃ and 10-20 Mpa to obtain a boron nitride-Ag/PVA blocky structure;
and putting the boron nitride-Ag/PVA blocky structure into a cutting machine, and cutting along the direction vertical to the film structure, wherein the cutting thickness is 3-5.6 mm.
10. Use of the boron nitride thermal gasket of high degree of orientation and high out-of-plane thermal conductivity as claimed in claim 1 or 2 in the field of heat dissipation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116715962A (en) * | 2023-08-10 | 2023-09-08 | 四川大学 | Functionalized boron nitride thermochromic silicon rubber composite heat dissipation gasket and preparation method thereof |
| CN117603506A (en) * | 2024-01-22 | 2024-02-27 | 汕头大学 | Boron nitride heat conduction material with three-dimensional network structure and preparation and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116715962A (en) * | 2023-08-10 | 2023-09-08 | 四川大学 | Functionalized boron nitride thermochromic silicon rubber composite heat dissipation gasket and preparation method thereof |
| CN116715962B (en) * | 2023-08-10 | 2023-10-10 | 四川大学 | Functionalized boron nitride thermochromic silicon rubber composite heat dissipation gasket and preparation method thereof |
| CN117603506A (en) * | 2024-01-22 | 2024-02-27 | 汕头大学 | Boron nitride heat conduction material with three-dimensional network structure and preparation and application thereof |
| CN117603506B (en) * | 2024-01-22 | 2024-04-23 | 汕头大学 | Boron nitride heat conduction material with three-dimensional network structure and preparation and application thereof |
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