CN117799185A - Boron nitride heat-conducting gasket and preparation method and application thereof - Google Patents
Boron nitride heat-conducting gasket and preparation method and application thereof Download PDFInfo
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- CN117799185A CN117799185A CN202311739577.XA CN202311739577A CN117799185A CN 117799185 A CN117799185 A CN 117799185A CN 202311739577 A CN202311739577 A CN 202311739577A CN 117799185 A CN117799185 A CN 117799185A
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- boron nitride
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- silica gel
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 123
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 77
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000741 silica gel Substances 0.000 claims abstract description 32
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 32
- 238000005520 cutting process Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 10
- 230000017525 heat dissipation Effects 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000945 filler Substances 0.000 claims description 12
- 239000000499 gel Substances 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 12
- -1 methyl vinyl trifluoropropyl Chemical group 0.000 description 11
- 239000004205 dimethyl polysiloxane Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 10
- 239000002002 slurry Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002131 composite material Substances 0.000 description 7
- 229920002379 silicone rubber Polymers 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229920002545 silicone oil Polymers 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000003698 laser cutting Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000000805 composite resin Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 239000002383 tung oil Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
- B29C69/001—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore a shaping technique combined with cutting, e.g. in parts or slices combined with rearranging and joining the cut parts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/283—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polysiloxanes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
- B32B3/266—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by an apertured layer, the apertures going through the whole thickness of the layer, e.g. expanded metal, perforated layer, slit layer regular cells B32B3/12
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/206—Insulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/302—Conductive
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/72—Density
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/04—Insulators
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Abstract
The invention discloses a boron nitride heat conduction gasket and a preparation method and application thereof, wherein the preparation method comprises the following steps: stirring and mixing organic silica gel and boron nitride powder, then carrying out cold pressing, and curing after the pressing is finished to obtain a boron nitride precursor tablet; slit cutting is carried out on the boron nitride precursor sheets to obtain slits, organic silica gel is coated on the surfaces of the boron nitride precursor sheets with the slits, then stacking is carried out, the alignment of the slits on each boron nitride precursor sheet is ensured in the stacking process, and the organic silica gel is filled in the slits to obtain a heat-conducting gasket precursor; and (3) solidifying the heat-conducting gasket precursor, and then cutting the heat-conducting gasket precursor into plates with different thicknesses along the vertical direction of the surface of the boron nitride precursor plate according to the requirements to obtain the boron nitride heat-conducting gasket. The preparation method is simple and environment-friendly, and the prepared boron nitride heat-conducting gasket has certain orientation, insulativity, good heat-conducting property and mechanical property, is low in density and has wide application prospect in the field of heat dissipation of electronic devices.
Description
Technical Field
The invention belongs to the field of heat-conducting silica gel gaskets, and particularly relates to a boron nitride heat-conducting gasket and a preparation method and application thereof.
Background
The increasing demand for high performance electronic devices has led to an increase in processor power density, resulting in extremely high heat generation, requiring efficient heat dissipation to ensure proper operation of the device. The conventional heat dissipation method can not meet the heat dissipation requirement of the high-power device. Therefore, it becomes critical to explore thermal interface materials with high thermal conductivity.
The ideal thermal interface material requires good mechanical properties to match its inherent surface roughness and maintain good heater-to-heat sink contact during thermal cycling while having excellent heat transfer properties. Polymeric materials are widely used in thermal interface materials for their excellent mechanical properties and processability.
However, the low thermal conductivity of polymeric materials limits their application, and polymeric materials typically have their thermal conductivity enhanced by the addition of highly thermally conductive materials such as metals, ceramics, and carbon-based fillers. The metal filler has high heat conductivity coefficient, but weak corrosion resistance and high density. However, the graphene, carbon fiber and other materials are conductive materials, and the graphene heat conduction gasket prepared by CN115092920a and the carbon fiber heat conduction gasket prepared by CN116769195A may cause conditions of electric leakage and the like in the electronic component to cause short circuit of the device.
Compared with the above filler, boron nitride is an insulating material and has higher thermal conductivity, so boron nitride becomes an ideal filler for preparing a thermally conductive and insulating composite material. The publication No. CN 106273925A discloses a novel high-heat-conductivity insulating gasket which adopts a multi-layer composite structure and comprises a first modified silicon rubber layer, an intermediate layer and a second modified silicon rubber layer; the middle layer is prepared by pressing and forming a resin-based composite material, and the resin-based composite material comprises the following components in parts by weight: 10-20 parts of boron nitride powder, 1-4 parts of boron nitride nano-sheets, 2-8 parts of adhesive and 50-85 parts of polystyrene resin; the first modified silicon rubber layer and the second modified silicon rubber layer are the same in material and are prepared by curing the following materials in parts by weight: 20-40 parts of methyl vinyl silicone rubber, 8-15 parts of methyl vinyl trifluoropropyl silicone rubber, 1-3 parts of spherical nanometer aluminum nitride, 0.8-1.2 parts of flaky nanometer aluminum nitride, 5-8 parts of tung oil, 1-2 parts of cross-linking agent and 0.5-0.8 part of vulcanizing agent.
However, although boron nitride can be used as a filler for preparing a heat conductive and insulating composite material, boron nitride as a two-dimensional material has a thermal conductivity of 300W m in the in-plane direction -1 K -1 While the thermal conductivity in the out-of-plane direction is only 30W m -1 K -1 . Boron nitride heat conducting pad on the marketMost of the flakes are blended, do not orient boron nitride efficiently, and do not have good mechanical properties.
Therefore, in view of the above prior art, there is a need to prepare a highly thermally conductive insulating gasket with a certain orientation and having good mechanical properties for use in electronic devices.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a boron nitride heat conduction gasket, which is characterized in that organic silica gel and boron nitride powder are mixed, cut and processed after being oriented by cold pressing and shearing force, and then stacked and filled with the organic silica gel to prepare a high heat conduction insulating material.
A preparation method of a boron nitride heat-conducting gasket comprises the following steps:
(1) Stirring and mixing organic silica gel and boron nitride powder, then carrying out cold pressing, and curing after the pressing is finished to obtain a boron nitride precursor tablet;
(2) Slit cutting is carried out on the boron nitride precursor sheets obtained in the step (1) to obtain slits, organic silica gel is coated on the surfaces of the boron nitride precursor sheets, a plurality of boron nitride precursor sheets with the surfaces coated with the organic silica gel are stacked, the slits on the boron nitride precursor sheets are ensured to be aligned in the stacking process, and the organic silica gel is filled in the slits to obtain a heat-conducting gasket precursor;
(3) And (3) solidifying the heat-conducting gasket precursor obtained in the step (2), and then cutting the heat-conducting gasket precursor into pieces with different thicknesses along the vertical direction of the surface of the boron nitride precursor piece according to the requirement to obtain the boron nitride heat-conducting gasket.
According to the invention, the organic silica gel matrix is utilized, and anisotropic orientation of the boron nitride sheet is realized through cold pressing and shearing force, so that oriented high heat conduction is realized. The method combines two strategies for preparing the heat-conducting composite material: (1) The anisotropic high heat conduction filler is directionally arranged to obtain high heat conduction in a specific direction; (2) And constructing a sandwich structure by using a silica gel matrix as a connecting medium between the hexagonal boron nitride sheets. The heat-conducting composite material prepared by the method can realize good heat-conducting performance and mechanical performance under the condition of low density.
Preferably, the organic silica gel is polydimethylsiloxane added with a curing agent and a catalyst.
Preferably, the curing agent is hydrogen-containing silicone oil.
Preferably, the catalyst is a platinum (0) -1, 3-diethylene-1, 3-tetramethyl disiloxane platinum catalyst.
Preferably, the mass ratio of the curing agent, the catalyst and the polydimethylsiloxane in the organic silica gel is 0.02-0.03:0.01:1.
Preferably, the boron nitride powder is hexagonal boron nitride, the side length is 30-50 mu m, and the thickness is 0.5-2 mu m. The hexagonal boron nitride feedstock of the present invention is commercially available.
According to the invention, hexagonal boron nitride with the side length of 30-50 mu m and the thickness of 0.5-2 mu m is selected as a raw material, and if the particle size is too small, the contact area between the heat conducting fillers can be increased, so that the heat transfer efficiency is affected. If the particle size is too large, connection of the heat conducting filler is loosened, and then a heat transfer passage is blocked, so that the heat conducting performance is reduced.
Preferably, the mass ratio of the organic silica gel to the boron nitride powder is 2.8-3:7-7.2. If the proportion of the organic silica gel is too high, the curing time is increased, the heat conductivity coefficient is reduced, and if the proportion of the boron nitride is too high, the hardness of a sample is increased, and the mechanical property is reduced.
Preferably, in the step (1), the mixing time of the organic silica gel and the boron nitride powder is 7-10min, and the stirring speed is 3000-3500rpm.
Preferably, in step (2), the boron nitride precursor sheet is cut to a suitable size and placed on a laser cutting stage, and a slit is cut in the boron nitride precursor sheet using a laser.
Preferably, in the step (2), the number of the slits on the boron nitride precursor sheet is a plurality of slits which are uniformly distributed in parallel.
Preferably, in the step (2), the size of the slit on the boron nitride precursor sheet is 0.3mm×10mm, and the slit pitch is 0.25-0.3mm. The proper gap distance has the heat conduction and mechanical properties of the sample. Too large a gap can reduce thermal conductivity and too small a gap can reduce mechanical properties.
Preferably, the pressure of the cold pressing is 50-80 tons and the pressing time is 120-150 seconds. Too much pressure and too long time can affect the rebound resilience of the sample mechanics, and too little pressure and too short time can lead to untight bonding between precursors and lead to sample cracking.
Preferably, in step (2), the thickness of the silicone gel between adjacent boron nitride precursor sheets is controlled to be 45-55 μm. According to the invention, the adjacent boron nitride precursor sheets are tightly adhered together by spraying the organic silica gel between the adjacent boron nitride precursor sheets. The invention controls the thickness of the organic silica gel to enable the precursors to be tightly adhered, thereby increasing the mechanical property of the sample.
Preferably, in the steps (1) and (3), the curing temperature is 80-85 ℃ and the curing time is 30-45min.
In step (3), the heat conductive gasket precursor can be cut into sheets of different thicknesses, such as 0.2mm, 0.5mm and 1mm, as required along the vertical direction of the surface of the boron nitride precursor sheet.
The invention also provides the boron nitride heat-conducting gasket prepared by the preparation method. The boron nitride heat-conducting gasket has certain orientation, insulativity, good heat-conducting property and mechanical property.
Preferably, the density of the boron nitride heat conduction gasket is 1.4-1.7g cm -3 . The density of the boron nitride insulating gasket is lower than 2.0g cm -3 Far lower than the commonly used heat sink materials.
Preferably, the thermal conductivity of the boron nitride thermal conductive gasket along the orientation direction of the boron nitride filler is 5.5-6.5W m -1 K -1 。
The invention also provides application of the boron nitride heat conduction gasket in the field of heat dissipation of electronic devices. The boron nitride heat-conducting gasket has good heat-conducting property and mechanical property, and has wide application prospect in the field of heat dissipation of electronic devices.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the boron nitride heat-conducting gasket is simple and environment-friendly, and the high-molecular matrix organic silica gel is filled between the boron nitride fillers, and the fillers with certain orientation are connected together to form a heat-conducting network.
(2) The boron nitride heat-conducting gasket has certain orientation, insulativity, good heat-conducting property and mechanical property, and the density of the boron nitride heat-conducting gasket is lower than 2.0g cm -3 Far lower than the common heat dissipation materials, and has wide application prospect in the field of heat dissipation of electronic devices.
Drawings
FIG. 1 is a schematic view of a boron nitride precursor wafer prepared in example 1;
FIG. 2 is a schematic diagram of a thermally conductive gasket precursor prepared in example 1;
FIG. 3 is a schematic view of a boron nitride thermal pad prepared in example 1;
fig. 4 is a pressure strain graph of the cyclic test of the boron nitride thermal pad prepared in example 1.
Detailed Description
The present application is described in detail below with reference to examples.
Unless otherwise indicated, all starting materials in the examples of the present application were purchased commercially.
The method for testing the heat conductivity coefficient comprises the following steps: testing was performed using a laser thermal conductivity meter in accordance with the standard ASTM E1461-2013 standard.
Example 1
Raw materials: 20g of boron nitride sheet, 20g of polydimethylsiloxane, 0.5g of curing agent (hydrogen-containing silicone oil) and 0.2g of catalyst (platinum (0) -1, 3-diethylene-1, 3-tetramethyl disiloxane platinum catalyst).
Firstly, placing 20g of polydimethylsiloxane into a mixing cup, mixing 20g of boron nitride in a mixer for 5min at a rotating speed of 2750rpm to obtain a slurry mixture, finally adding 0.5g of curing agent and 0.2 of catalyst, and mixing for 5min continuously according to the parameters. The pressure of the cold press was set to 50 tons, and the slurry mixture was taken out and put under the cold press for 135 seconds and taken out. The above operations were repeated to obtain a number of boron nitride precursor sheets, as shown in fig. 1. And (3) putting the boron nitride precursor sheet into an oven, and setting the temperature at 80 ℃ for curing for 40min. Cutting the cured boron nitride precursor sheet into a proper size, placing the proper size on a laser cutting platform, and cutting slits with the size of 0.3mm multiplied by 10mm at intervals of 0.3mm by utilizing laser to obtain the boron nitride precursor sheet with the slits. And transferring and orderly stacking a second layer of boron nitride precursor sheet with slits on the first layer of boron nitride precursor sheet with slits, wherein the slits on the boron nitride precursor sheets are aligned in the stacking process, and the average thickness of the organic silica gel between the two layers is controlled to be 50 mu m. During the coating process, the slit (0.3 mm. Times.10 mm) was filled with silicone gel. The slit boron nitride precursor sheets were repeatedly stacked until the thickness reached about 10mm (about 40 boron nitride precursor sheets), to obtain a thermally conductive gasket precursor, as shown in fig. 2. And (3) putting the heat-conducting gasket precursor into an oven at 80 ℃ for 40min to completely solidify the silica gel. After curing, cutting is performed along the direction perpendicular to the plane of the boron nitride precursor sheet, and the boron nitride heat-conducting gasket is obtained, as shown in fig. 3.
The sample obtained in this example has a thermal conductivity of 6.486W m -1 K -1 Density of 1.36g/cm 3 。
To simulate the working environment of example 1 under long-term pressure, we conducted cyclic tests under an environment of 0.2 MPa. We observe a hysteresis cycle due to the mechanical energy dissipation caused by the first compression process. However, after the second cycle, the loading curve of the cycle was better matched with the loading curve of the second cycle, indicating that example 1 had better cycle stability at this stage. Exhibits good mechanical properties.
Comparative example 1
Raw materials: 20g of boron nitride sheet, 20g of polydimethylsiloxane, 0.5g of curing agent (hydrogen-containing silicone oil) and 0.2g of catalyst (platinum (0) -1, 3-diethylene-1, 3-tetramethyl disiloxane platinum catalyst).
Firstly, placing 20g of polydimethylsiloxane into a mixing cup, mixing 20g of boron nitride in a mixer for 5min at a rotating speed of 2750rpm to obtain a slurry mixture, finally adding 0.5g of curing agent and 0.2 of catalyst, and mixing for 5min continuously according to the parameters. The pressure of the cold press is set to be 50 tons, the slurry mixture is directly put into a customized 20mm multiplied by 20mm mold, the composite material obtained through the pressing of the cold press is subjected to an oven at 80 ℃ for 40min, and the silica gel is completely solidified. After curing, the high thermal conductivity composite was obtained as a blended comparative sample by cutting in the vertical direction.
The thermal conductivity of the sample obtained in this comparative example was 5.235W m -1 K -1 Density of 1.33g/cm 3 。
Comparative example 2
Raw materials: 20g of boron nitride sheet, 20g of polydimethylsiloxane, 0.5g of curing agent (hydrogen-containing silicone oil) and 0.2g of catalyst (platinum (0) -1, 3-diethylene-1, 3-tetramethyl disiloxane platinum catalyst).
Firstly, placing 20g of polydimethylsiloxane into a mixing cup, mixing 20g of boron nitride in a mixer for 5min at a rotating speed of 2750rpm to obtain a slurry mixture, finally adding 0.5g of curing agent and 0.2 of catalyst, and mixing for 5min continuously according to the parameters. The pressure of the cold press is set to be 30 tons, a proper amount of the slurry mixture is taken out and put under the cold press, and the slurry mixture is taken out after being pressed. Repeating the above operation to obtain a plurality of boron nitride precursor sheets. And (3) putting the boron nitride precursor sheet into an oven, and setting the temperature at 80 ℃ for curing for 40min. And cutting the cured boron nitride precursor sheet into a proper size, placing the proper size on a laser cutting platform, and cutting slits with the size of 0.3mm multiplied by 10mm at certain intervals by using laser to obtain the boron nitride precursor sheet with the slits. And transferring and orderly stacking a second layer of boron nitride precursor sheet with slits on the first layer of boron nitride precursor sheet with slits, wherein the slits on the boron nitride precursor sheets are aligned in the stacking process, and the average thickness of the organic silica gel between the two layers is controlled to be 50 mu m. During the coating process, the slit (0.3 mm. Times.10 mm) was filled with silicone gel. And repeatedly stacking the boron nitride precursor sheets with the patterns until the thickness reaches about 10mm (about 30 boron nitride precursor sheets), thereby obtaining the heat-conducting gasket precursor. And (3) putting the heat-conducting gasket precursor into an oven at 80 ℃ for 40min to completely solidify the silica gel. And after curing, cutting along the direction perpendicular to the plane of the boron nitride precursor sheet to obtain the boron nitride heat-conducting gasket.
The thermal conductivity of the sample obtained in this comparative example was 4.826. 4.826W m -1 K -1 Density of 1.25g/cm 3 。
Comparative example 3
Raw materials: 20g of boron nitride sheet, 20g of polydimethylsiloxane, 0.5g of curing agent (hydrogen-containing silicone oil) and 0.2g of catalyst (platinum (0) -1, 3-diethylene-1, 3-tetramethyl disiloxane platinum catalyst).
Firstly, placing 20g of polydimethylsiloxane into a mixing cup, mixing 20g of boron nitride in a mixer for 5min at a rotating speed of 2750rpm to obtain a slurry mixture, finally adding 0.5g of curing agent and 0.2 of catalyst, and mixing for 5min continuously according to the parameters. The pressure of the cold press is set to be 10 tons, a proper amount of the slurry mixture is taken out and put under the cold press, and the slurry mixture is taken out after being pressed. Repeating the above operation to obtain a plurality of boron nitride precursor sheets. And (3) putting the boron nitride precursor sheet into an oven, and setting the temperature at 80 ℃ for curing for 40min. And cutting the cured boron nitride precursor sheet into a proper size, placing the proper size on a laser cutting platform, and cutting slits with the size of 0.3mm multiplied by 10mm at certain intervals by using laser to obtain the boron nitride precursor sheet with the slits. And transferring and orderly stacking a second layer of boron nitride precursor sheet with slits on the first layer of boron nitride precursor sheet with slits, wherein the slits on the boron nitride precursor sheets are aligned in the stacking process, and the average thickness of the organic silica gel between the two layers is controlled to be 50 mu m. In the coating process, the boron nitride precursor sheets with the slits are repeatedly stacked until the thickness reaches about 10mm, (about 25 boron nitride precursor sheets), and the heat-conducting gasket precursor is obtained. And (3) putting the heat-conducting gasket precursor into an oven at 80 ℃ for 40min to completely solidify the silica gel. And after curing, cutting along the direction perpendicular to the plane of the boron nitride precursor sheet to obtain the boron nitride heat-conducting gasket.
The thermal conductivity of the sample obtained in this comparative example was 4.325W m -1 K -1 Density of 1.22g/cm 3 。
The foregoing description is only a few examples of the present application and is not intended to limit the present application in any way, and although the present application is disclosed in the preferred examples, it is not intended to limit the present application, and any person skilled in the art may make some changes or modifications to the disclosed technology without departing from the scope of the technical solution of the present application, and the technical solution is equivalent to the equivalent embodiments.
Claims (10)
1. The preparation method of the boron nitride heat-conducting gasket is characterized by comprising the following steps of:
(1) Stirring and mixing organic silica gel and boron nitride powder, then carrying out cold pressing, and curing after the pressing is finished to obtain a boron nitride precursor tablet;
(2) Slit cutting is carried out on the boron nitride precursor sheets obtained in the step (1) to obtain slits, organic silica gel is coated on the surfaces of the boron nitride precursor sheets, a plurality of boron nitride precursor sheets with the surfaces coated with the organic silica gel are stacked, the slits on the boron nitride precursor sheets are ensured to be aligned in the stacking process, and the organic silica gel is filled in the slits to obtain a heat-conducting gasket precursor;
(3) And (3) solidifying the heat-conducting gasket precursor obtained in the step (2), and then cutting the heat-conducting gasket precursor into pieces with different thicknesses along the vertical direction of the surface of the boron nitride precursor piece according to the requirement to obtain the boron nitride heat-conducting gasket.
2. The preparation method of claim 1, wherein the boron nitride powder is hexagonal boron nitride, the side length is 30-50 μm, the thickness is 0.5-2 μm, and the mass ratio of the organic silica gel to the boron nitride powder is 2.8-3:7-7.2.
3. The method of claim 1, wherein the plurality of slits are arranged in parallel.
4. A method of preparing as claimed in claim 3 wherein the slits in the boron nitride precursor sheet are 0.3mm x 10mm in size and the slit spacing is 0.25-0.3mm.
5. The method according to claim 1, wherein the cold pressing pressure is 50-80 tons and the pressing time is 120-150 seconds.
6. The method according to claim 1, wherein in the steps (1) and (3), the curing temperature is 80 to 85 ℃ and the curing time is 30 to 45min.
7. The method of claim 1, wherein the thickness of the silicone gel between adjacent boron nitride precursor sheets is controlled to be 45-55 μm.
8. The boron nitride heat-conducting gasket prepared by the preparation method according to any one of claims 1 to 7.
9. The boron nitride thermal pad of claim 8, wherein the boron nitride thermal pad has a density of 1.4-1.7g cm -3 The method comprises the steps of carrying out a first treatment on the surface of the The heat conductivity coefficient along the orientation direction of the boron nitride filler is 5.5-6.5. 6.5W m -1 K -1 。
10. Use of a boron nitride thermally conductive gasket according to claim 8 or 9 in the field of heat dissipation of electronic devices.
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