CN107189091A - The manufacture method of hexagonal boron nitride planes - Google Patents

The manufacture method of hexagonal boron nitride planes Download PDF

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Publication number
CN107189091A
CN107189091A CN201610146112.7A CN201610146112A CN107189091A CN 107189091 A CN107189091 A CN 107189091A CN 201610146112 A CN201610146112 A CN 201610146112A CN 107189091 A CN107189091 A CN 107189091A
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boron nitride
hexagonal boron
planes
manufacture method
nitride planes
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张静瑜
张国兴
陈家庆
赖中平
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BGT Materials Ltd
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BGT Materials Ltd
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Abstract

The present invention provides a kind of manufacture method of hexagonal boron nitride planes, including step：A) by dielectrical polymer dissolving in a solvent；B) hexagonal boron nitride powder is mixed, to form the hexagonal boron nitride coating sizing-agent well mixed；C) slurry is coated on multiple base materials, and be dried under Celsius 100 to 150 degree；D 1) for single hexagonal boron nitride planes, handled by rolling, dielectric polymer layer is peeled off on base material；D 2) for the hexagonal boron nitride planes on base material, hot pressing is carried out to the multiple base material and multiple hexagonal boron nitride planes under being spent Celsius 100 to 250, to form multi-layer substrate.Accordingly, hexagonal boron nitride planes can show 10 to 40 watts/ meter Du (w/m.k) thermal conductivity, and this is more notable than the heat management used at present.

Description

The manufacture method of hexagonal boron nitride planes
Technical field
The present invention relates to a kind of manufacture method of hexagonal boron nitride planes, 10 to 40 watts/ meter Du can be showed (w/m.k) thermal conductivity, this is more notable than the heat management used at present.
Background technology
The miniaturization of increase current densities and modern electronics efficiently except heat and can radiate, to conventional electronics Equipment and system are even more the key for making it reliably operate.Therefore, the industry be applicable to various heat managements should Novel heat-conducting material, and have in the urgent need to.If such material can have electrical insulating property, will more have Benefit, because they can be directly applied on electronic circuit.
Unfortunately, most of tool economic benefit and feasible insulating materials tool low heat conductivity, this serious limit Their application is made, it is impossible to be used as high-efficiency radiator.
It is known that substantial amounts of hexagonal boron nitride (hBN) has the heat of highest basal plane in other materials Conductance (is up to 400 watts/ meter Du) at room temperature, and almost matches with silver.In hexagonal boron nitride, Nearest interest is to study the graphene electrical insulating property for thermal management applications.Except excellent dielectricity Can, the hexagonal boron nitride crystal of several atomic layers shows a large amount of values, and it is expected that can exceed high heat conduction value. It is contemplated that by the rare combination of the electrical insulation characteristics of the hexagonal boron nitride with abnormal high-termal conductivity, for most Promising thermal management materials candidate material of future generation.However, the hexagonal boron crystal of multilayer is used In, it is necessary to make heat-conducting layer have pliability or shaped surfaces, and leading in practical application in the heat conduction of preferable side's property There is less thermojunction in road.These demands can be by obtaining multiple thin slices with hexagonal boron nitride crystal (preferably individual layer), and be implemented.Graphene platelet before has relatively high thermal conductivity (up to 100 watts/ meter Du), it was demonstrated that the graphene platelet has perfect coating characteristic.Unfortunately, such stone The potential thermal management applications quantity of black alkene thin slice is limited by their high conductivity.On the other hand, six side's nitrogen The expectable offer high-termal conductivity of boron thin slice and excellent electrical insulating property combination are provided, and turn into the allusion quotation of electronics industry Model.
The content of the invention
The main object of the present invention is to provide a kind of manufacture method of hexagonal boron nitride planes, can show 10 To 40 watts/ meter Du (w/m.k) thermal conductivity, this is more notable than the heat management used at present.
The secondary objective of the present invention is to provide a kind of manufacture method of hexagonal boron nitride planes, six side nitridation The thermal conductivity of boron thin slice can be lifted with cumulative mass density, to open fine setting hexagonal boron nitride planes The mode of hot property.
In order to obtain above-mentioned purpose, a kind of manufacture method of hexagonal boron nitride planes provided by the present invention, Including step：
A) by the dielectrical polymer dissolving of 10 to 80 percentage by weights in a solvent；
B) hexagonal boron nitride powder of 20 to 90 percentage by weights is mixed, to form the six side's nitrogen well mixed Change boron coating sizing-agent；
C) slurry is coated on multiple base materials, and be dried under Celsius 100 to 150 degree, After this process step, one layer of hexagonal boron nitride planes can be obtained；
D-1) for single hexagonal boron nitride diaphragm, handled by rolling, by dielectric polymer layer by water Peeled off on base material in batch；
D-2) for the hexagonal boron nitride diaphragm on multiple base materials, to described many under being spent Celsius 100 to 250 Individual base material and multiple hexagonal boron nitride planes carry out hot pressing, to form multi-layer substrate.
Embodiment for the present invention and its technical characterstic and effect, will hereafter coordinate schema explanation It is as follows.
Brief description of the drawings
Figure 1A is the optical image schematic diagram of hexagonal boron nitride planes, wherein, contrast it is vertical Change is derived from the engineer's scale of charging and 1 micron；
Figure 1B is the optical image sectional view of hexagonal boron nitride planes, wherein, engineer's scale is 1 micro- Rice；
Fig. 2 shows different densities of weight value ρ hexagonal boron nitride planes, under temperature funtion T Measured thermal conductivity κ；
Fig. 3 shows the thermal conductivity κ correspondence density functions of hexagonal boron nitride planes, Celsius 80 Measured at a temperature of degree, wherein, color GTG is by different indivedual of the upper left-to-right depth of figure Curve represents the analog result of the thermal contact conductance under different numerical value；
Fig. 4 is low-density sample A and high density sample B is used for the thin slice model signal of numerical simulation Figure, wherein, a single hexagonal boron nitride planes are 1 micron × 1 micron of a lateral dimension of tool, And thickness is 10 nanometers of solid block.
Embodiment
A kind of manufacture method of the hexagonal boron nitride planes of a preferred embodiment of the present invention, including Step：
A) by the dielectrical polymer dissolving of 10 to 80 percentage by weights in a solvent.Preferably It is that the dielectrical polymer is at least one of following polymers, including poly- terephthaldehyde Acetoacetic ester (PETP), polyphenylene sulfide (PPS), PEI (PEI), polyether-ether-ketone (PEEK), Polyether-ketone (PEK), polyimides (PI), polyvinylidene fluoride ethene (PVDF), phenolic aldehyde Resin or acrylic resin.
B) hexagonal boron nitride (hBN) powder of 20 to 90 percentage by weights is mixed, to be formed The hexagonal boron nitride coating sizing-agent well mixed.It is preferred that the hexagonal boron nitride powder Thickness be 1 to 500 nanometer, and its size be 0.1 to 100 micron.
C) slurry is coated on multiple base materials, and carried out under Celsius 100 to 150 degree Dry, after this process step, one layer of hexagonal boron nitride planes can be obtained.
D-1) for single hexagonal boron nitride planes, handled by rolling, dielectric is polymerize Nitride layer is peeled off on base material.
D-2) for the hexagonal boron nitride planes on multiple base materials, in the case where Celsius 100 to 250 spend Hot pressing is carried out to the multiple base material and multiple hexagonal boron nitride planes, to form multilayer base Material.
It is preferred that the multiple base material is conductive layer, such as calcium or aluminium foil.
It is preferred that the thickness of a conductive layer is between 10 microns to 100 microns.
Figure 1A and Figure 1B is referred to, the top of the film and section optical image map analysis are saturating The primarily transverse size for exposing hexagonal boron nitride film is about 10 nanometers, about 1 micron of tool it is flat Equal thickness.The optical image figure also shows how hexagonal boron nitride powder builds heat dissipation channel, To show its high-termal conductivity.Figure 1A is shown in the lateral contact between hexagonal boron nitride powder, And Figure 1B shows the sectional view of hexagonal boron nitride powder amorphous storehouse, this can ensure that heat can Radiated to all directions.
The pyroconductivity κ for the thin slice studied is calculated using following equation
κ=α ρ Cp, (1)
Here α is the thermal diffusion of inner face, and ρ refers to quality of materials density, and Cp is specific heat. These three parameters are to be individually acknowledged in an experiment.
Thermal diffusion α can be by can business system (the resistance to LFA 457 that speeds) as temperature T function Laser flash method be measured.In order to measure the thermal diffusivity of inner face, specific sample rack Have been used, it, which can be accommodated, is cut into the circular single hexagonal boron nitride film of 22 millimeters of diameter Sample.The diameter at the sample back side is about 5 millimeters, and by a laser beam with heating of glistening. Thermal diffusion under the function of time is the top perimeter along thin slice, by an infrared detector It is detected in 5 to 6 millimeters of center of a sample.In order to avoid unnecessary reflection, the sample This and sample holder have been sprayed-on graphite paint.During measuring, laser flash system Sample be with the nitrogen continuous wash of 30 ml/min flows.The specific heat Cp of the sample can make With sapphire as reference sample, entered with differential scanning calorimetry (DSC) (the resistance to F3 of DSC 404 that speed) Row is determined.The mass density ρ can be by weighting the known dimensions of the sample, with precise electronic Balance carry out amount scale.
In order to assess the effect of film composite, we measure four hexagonal boron nitride planes and existed Pyroconductivity κ under temperature funtion T, with different mass density ρ.As shown in Fig. 2 Mass density ρ is respectively 1.58,1.60,1.64,1.65 grams/cc of (g/cm3), Thermal conductivity is that " weakness " depends on temperature, and can be increased with the increase of density.The thermal conductivity The observed value of rate falls between 10 to 20 watts/ meter Du (w/m.k), this certainly industry Correlation.
In order to more preferably understand influence of the density of material in thermal conductivity, we have studied in matter The dependency degrees of κ at room temperature on metric density value ρ.The density of thin slice sample is with two kinds of differences Mode control：(i) (ρ change is only limited using the hexagonal boron nitride planes of different-thickness Change can be realized in this way), and (ii)：Change institute using extra rollers compress State hexagonal boron nitride planes.Both approaches have identical effect all in pyroconductivity. The amalgamation result of this research is shown in Fig. 3.Similar data display is in Fig. 2, the thermal conductivity Tend to as the density of hexagonal boron nitride planes increases and increases.
After systematic optical image test is carried out to the thin slice of different densities, our knot By being, variable density main reason is that existing between the hexagonal boron nitride planes of storehouse Pore size.Two thin slices with different densities are displayed in Fig. 4.Therefore, we Summarize by more spaces, the discontinuity in hot path can be caused, and reduce thermal conductivity Rate.
In order to confirm our suggestion, we set up the hot-fluid pattern of the thin slice in multiple tool spaces. We carry out numerical simulation using ABAQUS 2011, define meta analysis software kit.In order to explore Relation between effective and hexagonal boron nitride planes density, we pass through following equations Formula simulation control steady state thermal is passed：
Wherein, Q is heat flux, and(steady state heat transfer).The model system It is to be estimated using ABAQUS component types DC2D8, and as shown in figure 4, is micro- with 1 Rice × 1 micron lateral dimension and 10 nano thickness heat-conducting medium ordered stack solid block Band represent.In order to simulate hexagonal boron nitride planes, the pyroconductivity of the solid block is Select 390 watts/ meter Du (w/m.k) at room temperature.In order to change the effective density of emulation thin slice, We have adjusted the stack region between adjacent solid block, as shown in Fig. 4 samples A.B.In addition, In view of the imperfection thermo-contact between storehouse thin slice, limited thermal contact conductance has been introduced into Into the model.The final analog result passes through 105To 106Watt/meter2Spend (w/m2.k) Thermal contact conductance in scope is mutually matched to change experimental data.The six sides nitridation The gained effective thermal conductivity κ of boron thin sliceeffIt is to be calculated using Fourier's law：
Here q represents the total net hot-fluid in section by the thin slice, and L is the strip of foil The total length of band, and Δ T represents the temperature difference between the band hot junction and cold end.
The result of the numerical simulation is shown by the solid line in Fig. 3.Each curve is represented Has the thin slice efficient thermal conductivity of different thermal contact resistances between the thin slice of the storehouse.The emulation Only display is qualitative consistent with experimental data, because our model is simpler.One more accurate Simulation will have to consider the Size Distribution and contact conductance in packed density of thin slice according to Lai Xing.However, our initial pyroconductivities that are assumed to be are present inside the thin slice Space limitation, this is proved by this simple model.In addition, the contact heat Conductance rough estimate is 106Watt/meter2Spend (w/m2.k) sequence.There is contact conductane described The data not having in rate are still applicable to this system, but one is similar to the side's nitridation of graphene/six Boron interface discloses about 7106Watt/meter2Spend (w/m2.k), this amplitude order is higher than us Emulation estimate.Most probable explanation is that the surface of the hexagonal boron nitride planes is by solvent Residue pollutes, and which in turn reduces the thermal conductivity across thin slice to wafer interface.
Finally, we demonstrate hexagonal boron nitride ink can be used for manufacture have up to 20 watts/ The thin slice of meter Du (w/m.k) thermal conductivity.In the above-described embodiments, this is than at present in heat Material result used in management is more notable.We also confirm that effective thermal conductivity can be by changing Become thin slice packed density to adjust.We are also by improving thin slice to the quality of wafer interface To prove that one is used to increase the potential method of heat transfer.Reach electric insulation, hexagonal boron nitride Thin slice is possible to open a new approach, and can be used as advanced thermal management materials.
Although the present invention disclosed as above by the above embodiments, but itself and be not used to limit The fixed present invention, any those skilled in the art, without departing from the spirit and scope of the present invention, When can make a little change and retouching, thus the present invention scope of patent protection with claim Invention claim content is defined.

Claims (5)

1. a kind of manufacture method of hexagonal boron nitride planes, it is characterised in that including step：
A. by the dielectrical polymer dissolving of 10 to 80 percentage by weights in a solvent；
B. the hexagonal boron nitride powder of 20 to 90 percentage by weights is mixed, to form the hexagonal boron nitride coating sizing-agent well mixed；
C. the slurry is coated on multiple base materials, and be dried under Celsius 100 to 150 degree, after this process step, one layer of hexagonal boron nitride planes can be obtained；
D-1. for single hexagonal boron nitride planes, handled by rolling, dielectric polymer layer is peeled off on base material；
D-2. for the hexagonal boron nitride planes on multiple base materials, hot pressing is carried out to the multiple base material and multiple hexagonal boron nitride planes under being spent Celsius 100 to 250, to form multi-layer substrate.
2. the manufacture method of hexagonal boron nitride planes according to claim 1, it is characterized in that, the dielectrical polymer is at least one of following polymers, including polyethylene terephthalate (PETP), polyphenylene sulfide (PPS), PEI (PEI), polyether-ether-ketone (PEEK), polyether-ketone (PEK), polyimides (PI), polyvinylidene fluoride ethene (PVDF), phenolic resin or acrylic resin.
3. the manufacture method of hexagonal boron nitride planes according to claim 1, it is characterised in that the thickness of the hexagonal boron nitride powder is 1 to 500 nanometer, and its size is 0.1 to 100 micron.
4. the manufacture method of hexagonal boron nitride planes according to claim 1, it is characterised in that the multiple base material is conductive layer, such as calcium or aluminium foil.
5. the manufacture method of hexagonal boron nitride planes according to claim 1, it is characterised in that the thickness of a conductive layer is between 10 microns to 100 microns.
CN201610146112.7A 2016-03-15 2016-03-15 The manufacture method of hexagonal boron nitride planes Pending CN107189091A (en)

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CN110845813A (en) * 2019-11-18 2020-02-28 苏州溪能环保科技有限公司 Preparation method of hexagonal boron nitride/polyvinylidene fluoride composite material with excellent dielectric property
CN116651720A (en) * 2023-05-25 2023-08-29 佛山(华南)新材料研究院 Preparation method of high-orientation horizontally-arranged boron nitride film

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US20120188730A1 (en) * 2009-10-22 2012-07-26 Denki Kagaku Kogyo Kabushiki Kaisha Insulating sheet, circuit board, and process for production of insulating sheet
CN104086929A (en) * 2008-10-21 2014-10-08 日立化成工业株式会社 Heat conducting sheet, manufacturing method thereof, and heat radiator that utilizes the same

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CN104086929A (en) * 2008-10-21 2014-10-08 日立化成工业株式会社 Heat conducting sheet, manufacturing method thereof, and heat radiator that utilizes the same
CN102421829A (en) * 2009-05-13 2012-04-18 纳幕尔杜邦公司 A film prepared from a casting composition comprising a polymer and surface modified hexagonal boron nitride particles
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CN110845813A (en) * 2019-11-18 2020-02-28 苏州溪能环保科技有限公司 Preparation method of hexagonal boron nitride/polyvinylidene fluoride composite material with excellent dielectric property
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