CN114684796B - Boron nitride nanosheet based on large length-diameter ratio, high-heat-conductivity insulating composite material and preparation method thereof - Google Patents
Boron nitride nanosheet based on large length-diameter ratio, high-heat-conductivity insulating composite material and preparation method thereof Download PDFInfo
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Abstract
The application discloses a boron nitride nano-sheet, wherein the transverse dimension of the boron nitride nano-sheet is between 1 and 15 mu m, the thickness is between 1 and 10nm, and the length-diameter ratio is between 600 and 2000. The preparation method of the boron nitride nano-sheet and the insulating composite material formed by the boron nitride nano-sheet and the polymer matrix.
Description
Technical Field
The application relates to the technical field of materials, in particular to a hexagonal boron nitride nanosheet and preparation of a high-heat-conductivity insulating composite material thereof.
Background
With the rapid development of miniaturization of electronic components, power systems, communication equipment and the like, the power density of the system is greatly increased, and the temperature of the working environment is rapidly increased. In order to ensure the long-time stable and reliable operation of the whole system, the continuous rise of the working temperature of the whole system must be prevented, so that the timely heat dissipation capability becomes a key factor for determining the performance, the reliability and the service life of the electronic equipment. It is well known that the heat dissipation capacity of electronic devices depends on the thermal management material used, not the device itself, which means that developing a high performance thermal management material is a problem to be solved. In particular, as the demand for multiple functions and multiple uses increases, in addition to the high heat conductive property, the insulating property, mechanical property, and the like of the thermal management material must be taken into consideration. The polymer material can basically meet the requirements except that the intrinsic heat conductivity is very low, so that the modification of the polymer material by adding the high heat conduction insulating filler becomes a feasible way for developing a new generation of high-performance heat management materials.
Hexagonal boron nitride nano-sheets are also called as 'white graphene', and are increasingly attracting attention because of the high heat conduction and insulation properties of the hexagonal boron nitride nano-sheets and the incomparable advantages of other heat conduction fillers. However, it is more difficult to delaminate than graphite due to the "lip-lip" effect between the bulk hexagonal boron nitride layers. The current mainstream methods for stripping hexagonal boron nitride include both chemical and physical methods. The chemical method is to use high activity chemical substances such as KMnO 4 -H 2 SO 4 -H 2 O 2 Or molten KOH-NaOH, etc., to functionalize or intercalate the bulk boron nitride, thereby achieving the effect of stripping the boron nitride. However, the chemical method has low stripping efficiency and yield because the chemical inertness of the boron nitride is very strong, and the length-diameter ratio of the stripped boron nitride nano-sheet is very small. The physical method mainly comprises two types of liquid-phase ultrasonic and ball milling, wherein the former uses cavitation effect, and the latter peels off the block hexagonal boron nitride through shearing force generated by severe collision between grinding balls, and compared with the chemical method, the physical method has the advantages of low cost, environmental friendliness, high yield and easiness for mass production. However, due to the violent and lengthy exfoliation process, secondary destruction of previously exfoliated boron nitride nanoplatelets is unavoidable, resulting in a dramatic decrease in lateral dimensions, and the resulting aspect ratio of the boron nitride nanoplatelets is often also unsatisfactory. A large number of related works show that the boron nitride nano-sheet with large length-diameter ratio has important significance for improving the composite heat conductivity, however, no method for obtaining the boron nitride nano-sheet with large length-diameter ratio on a large scale exists at present, and the method also becomes the current limit of the boron nitride-based heat conduction compositeThe important reason for the further improvement of the thermal conductivity of the composite material. Therefore, a new technology and method are needed to be developed to obtain the boron nitride nano-sheets with large length-diameter ratio in batches, so as to realize the breakthrough of the heat conductivity of the hexagonal boron nitride-based heat conduction composite material on the basis.
Disclosure of Invention
According to one aspect of the application, a boron nitride nano sheet is provided, wherein the transverse dimension of the boron nitride nano sheet is 1-15 mu m, the thickness is 1-10 nm, and the average length-diameter ratio is 600-2000.
Optionally, the aspect ratio is between 1000 and 2000.
Optionally, the aspect ratio is between 1100 and 2000. The aspect ratio is the ratio of the lateral dimension to the thickness of the boron nitride nanoplatelets.
According to another aspect of the application, a method for preparing hexagonal boron nitride nano-sheets with large length-diameter ratio based on high-pressure micro-jet technology is provided: the high pressure generated by the high pressure micro-jet equipment is used for forcing the bulk hexagonal boron nitride dispersion liquid to pass through a narrow pore canal, and the peeling of the bulk hexagonal boron nitride is caused by the transverse shearing force generated by the flow velocity difference of different areas.
The preparation method of the boron nitride nanosheets is characterized by comprising the following steps:
and stripping the dispersion liquid containing the block hexagonal boron nitride by adopting a high-pressure micro-jet technology to obtain the boron nitride nanosheets.
Optionally, the pressure of the high-pressure micro-jet is regulated to obtain boron nitride nano-sheets with different length-diameter ratios.
Alternatively, high pressure microfluidic devices are used to generate high pressure and force the flow of liquid through a narrow orifice, thereby creating lateral shear forces that cause exfoliation of the bulk hexagonal boron nitride.
Optionally, the peeling pressure of the boron nitride nano sheet is between 50 and 125MPa, and the cycle passes are between 10 and 100 times.
Optionally, the peeling pressure of the boron nitride nano sheet is between 70 and 80MPa, and the cycle passes are between 45 and 55 times.
Optionally, the peeling pressure of the boron nitride nano-sheet is any value of 50 MPa, 75MPa, 100MPa and 125MPa and a range value between any two pressure values.
Optionally, the dispersion containing bulk hexagonal boron nitride comprises bulk boron nitride and a dispersant;
the dispersing agent is a mixed solvent of water and an organic solvent; the organic solvent is at least one selected from methanol, ethanol, propanol, isopropanol, dimethylformamide and methyl pyrrolidone.
Optionally, the concentration of the bulk hexagonal boron nitride in the dispersion liquid containing the bulk hexagonal boron nitride is 1-3 mg mL -1 Between them.
Optionally, the mass ratio of organic solvent/water in the dispersant is between 0 and 3.
Optionally, the dispersant organic solvent/water mass ratio is between 0.5 and 1.5, optimally the dispersant organic solvent/water mass ratio is 1.
Optionally, the concentration of the dispersion;
preferably, the concentration of the dispersion liquid is 1.5-2.5 mg mL -1 Between them.
Optionally, the lateral dimension of the block hexagonal boron nitride is 2-30 mu m.
Optionally, the method at least comprises the steps of: and uniformly dispersing the bulk boron nitride powder in the solution, generating high pressure by using high-pressure micro-jet equipment, forcing the bulk hexagonal boron nitride dispersion liquid to pass through a narrow pore canal, and collecting after a plurality of times of circulation, thus obtaining the boron nitride nano-sheet with the ultra-high length-diameter ratio.
Specifically, in one example, the preparation method includes the steps of:
a) The bulk hexagonal boron nitride powder was dispersed in an ethanol/water mixed solution (mass ratio 1: 1) Ultrasonic treatment in water bath for 30 min to obtain a concentration of 2 mg mL -1 Hexagonal boron nitride dispersion of (2);
b) Pouring the hexagonal boron nitride dispersion liquid into high-pressure micro-jet equipment for treatment, setting the equipment pressure to 75MPa, and continuously circulating for 50 times to finish stripping of the hexagonal boron nitride block;
c) And standing the treated dispersion liquid for 7 days, collecting upper-layer liquid, and carrying out suction filtration to obtain the hexagonal boron nitride nano-sheet with large length-diameter ratio.
According to yet another aspect of the present application, there is provided a boron nitride nanoplatelet/polymeric thermally conductive and insulating composite. The boron nitride nano sheet/polymer heat-conducting insulating composite material comprises the boron nitride nano sheet, the boron nitride nano sheet prepared by the method and a flexible polymer matrix.
Optionally, the composite material has an in-plane thermal conductivity of 10 to 70W m -1 K -1 The content of the boron nitride nano-sheet is between 20 and 85 and wt percent.
Optionally, the thickness of the composite material is 10-150 mu m, and the density is 1.0-3.0 g/cm 3 。
Optionally, the thickness of the composite material is 20-30 mu m, and the density is 1.5-2.0 g/cm 3 。
Optionally, the flexible polymer matrix comprises polyvinyl alcohol, polyvinylidene fluoride, polyurethane and nanocellulose.
According to still another aspect of the present application, there is provided a method for preparing the above-mentioned boron nitride nanosheet/polymer heat conductive and insulating composite material, comprising the steps of:
and dispersing the boron nitride nano-sheets in a flexible polymer matrix to form a continuous heat conduction network, thereby obtaining the composite material.
Optionally, mixing the solution containing the boron nitride nano-sheets and the flexible polymer matrix, and forming a film to obtain the composite material.
Optionally, the film forming mode comprises suction filtration and casting.
In the present application, the flexible polymer matrix includes, but is not limited to, flexible polymer matrices such as polyvinyl alcohol (PVA), polyvinylidene fluoride (PVDF), polyurethane (PU), nanocellulose (CNF), and the like.
The application has the beneficial effects that:
the application is thatThe high-pressure micro-jet technology is adopted to strip the bulk boron nitride, so that the boron nitride nano-sheet with large length-diameter ratio is obtained, the method has large yield and high efficiency, is environment-friendly, and solves the problem of difficult strip preparation of the hexagonal boron nitride nano-sheet; on the basis, the application also provides a high heat conduction and insulation composite material based on the obtained boron nitride nano-sheet and a preparation method thereof, and the in-plane thermal conductivity of the composite material is 10-70W m -1 K -1 The content of the boron nitride nano-sheet is between 20 and 85 and wt percent, and the problem of low in-plane thermal conductivity of the boron nitride-based heat conduction composite material is solved.
Drawings
FIG. 1 is a schematic diagram of a bulk hexagonal boron nitride exfoliation process;
FIG. 2 is a Raman spectrum of a boron nitride nanosheet prepared at a pressure of 75 MPa;
FIG. 3 is a scanning electron microscope image of boron nitride nanoplatelets prepared at a pressure of 75 MPa;
FIG. 4 is a scanning probe microscope image of boron nitride nanoplatelets prepared at a pressure of 75 MPa;
fig. 5 is a cross-sectional scanning electron microscope image of a heat-conducting composite material with boron nitride nano-sheets prepared under a pressure of 75MPa as a heat-conducting filler.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples. Unless otherwise indicated, the starting materials employed in the examples were all from commercial purchases and were used as received without treatment; the instruments and equipment used in the examples all adopt manufacturer recommended parameters.
Raw materials and reagents used in the application:
block hexagonal boron nitride: dandong Nissan science and technology Co., ltd;
PVA: shanghai Ala Biochemical technology Co., ltd.
CNF: gui Linji macro technologies limited.
Instrument apparatus:
the peeling preparation of the boron nitride nanosheets adopts a high-pressure nano dispersing machine: shanghai Maich Industrial Equipment Co., ltd;
in-plane thermal conductivity of the samples was measured using LFA 467 laser flash apparatus (Netzsch, germany);
the morphology of the samples was determined using a field emission scanning electron microscope (Quanta FEG250, FEI, USA);
the thickness of the samples was measured using a scanning probe microscope (Dimension ICON, bruker, USA).
A high heat conduction insulating composite material based on hexagonal boron nitride nano-sheets with large length-diameter ratio and a preparation method thereof are provided, wherein the composite material is formed by compounding hexagonal boron nitride nano-sheets with large length-diameter ratio as heat conduction reinforcing filler with a flexible polymer matrix through the modes of suction filtration, tape casting and the like.
Optionally, the method at least comprises the steps of:
a) And uniformly dispersing the bulk boron nitride powder in the solution, generating high pressure by using high-pressure micro-jet equipment, forcing the bulk hexagonal boron nitride dispersion liquid to pass through a narrow pore canal, and collecting after a plurality of times of circulation, thus obtaining the boron nitride nano-sheet with the ultra-high length-diameter ratio.
Optionally, the lateral dimension of the hexagonal boron nitride block is 2-30 mu m;
alternatively, the dispersant includes, but is not limited to, a mixed solution of methanol, ethanol, propanol, isopropanol, dimethylformamide, methylpyrrolidone, and water;
optionally, the dispersant organic solvent/water mass ratio is between 0 and 3;
optionally, the concentration of the dispersion is 1-3 mg mL -1 Between them;
optionally, the peeling pressure of the boron nitride nano sheet is between 50 and 125MPa, and the cycle passes are between 10 and 100 times;
b) The boron nitride nano-sheet with large length-diameter ratio is uniformly mixed with a high polymer matrix by means of suction filtration, tape casting and the like, and a heat conduction path is formed in the boron nitride nano-sheet, so that the high heat conduction insulating composite material is prepared.
Optionally, the thickness of the composite material is 10-150 mu m, and the density is 1.0-3.0 g/cm 3 。
Optionally, the composite material has an in-plane thermal conductivity of 10 to 70W m -1 K -1 The content of the boron nitride nano-sheet is between 20 and 85 and wt percent.
Optionally, the polymer includes, but is not limited to, a flexible polymer matrix such as PVA, PVDF, PU, CNF.
Example 1:
0.5. 0.5 g block of hexagonal boron nitride powder was added to 500ml of ethanol/water mixed solution (ethanol/water mass ratio 1:1), followed by sonication in a water bath for 30 min. And pouring the obtained hexagonal boron nitride dispersion liquid into a feed inlet of a high-pressure nano-dispersion machine, regulating the pressure of equipment to 50 MPa, and continuously circulating for 50 times. Diluting the dispersion liquid obtained after high-pressure nano dispersion by 10 times, standing for 7 days, collecting upper liquid, and carrying out suction filtration to obtain the hexagonal boron nitride nano sheet, wherein the hexagonal boron nitride nano sheet is marked as sample No. 1.
Example 2:
the difference from example 1 is that: the pressure of the apparatus was adjusted to 75MPa and designated sample 2#.
Example 3
The difference from example 1 is that: the pressure of the apparatus was adjusted to 100MPa and designated sample 3#.
Example 4
The difference from example 1 is that: the pressure of the apparatus was adjusted to 125MPa and designated sample 4#.
Example 5
Adding the prepared boron nitride nano-sheet 30 mg into 30 mL deionized water under the equipment pressure of 50 MPa, performing water bath ultrasonic treatment for 15 min, adding 0.2 g PVA aqueous solution (the PVA content is 5 wt%), performing water bath ultrasonic treatment and stirring for 15 min to obtain a uniform mixed solution, and performing suction filtration to form a film to obtain the high-heat-conductivity insulating composite material, which is denoted as sample No. 5.
Example 6
The difference from example 5 is that: the boron nitride nanoplatelets used were replaced with boron nitride nanoplatelets prepared at a device pressure of 75MPa, designated sample 6#.
Example 7
The difference from example 5 is that: the boron nitride nanoplatelets used were replaced with boron nitride nanoplatelets prepared at an equipment pressure of 100MPa, designated sample # 7.
Example 8
The difference from example 5 is that: the boron nitride nanoplatelets used were replaced with boron nitride nanoplatelets prepared at a device pressure of 125MPa, designated sample # 8.
Example 9
The difference from example 5 is that: the PVA aqueous solution was replaced with CNF aqueous solution (CNF content 1 wt%), designated sample 9#.
Example 10 Raman Spectroscopy and morphology analysis of boron nitride nanoplatelets
Raman spectrum characterization is performed on the boron nitride nanoplatelets prepared by peeling examples 1 to 4 respectively, which are typically represented by example 2, as shown in fig. 2. The raman spectral characterization results show that the boron nitride nanoplatelets exhibit raman characteristics of typical boron nitride nanoplatelets.
Scanning electron microscope analysis was performed on the boron nitride nanoplatelets prepared by peeling examples 1 to 4# respectively, typically represented by example 2, as shown in fig. 3. The scanning electron microscope results show that the average transverse dimension of the boron nitride nano-sheet is about 4.7 mu m.
Scanning probe microscopic analysis was performed on the boron nitride nanoplatelets prepared by peeling examples 1 to 4, respectively, typically represented by example 2, as shown in fig. 4. Scanning probe microscopy results showed that the boron nitride nanoplatelets had a thickness of 3.0. 3.0 nm.
Scanning electron microscope analysis was performed on the thermally conductive and insulating composite materials obtained in examples 5 to 9, respectively, as typified by example 6, as shown in fig. 5. The scanning electron microscope results show that the boron nitride nanosheets show good horizontal arrangement in the high polymer substrate.
Example 11 thermal conductivity test of thermally conductive and insulating composite
In-plane thermal conductivity tests are respectively carried out on samples 5-9 # and the test results show that the samples 5-9 # have higher in-plane thermal conductivity and are 60-70W m -1 K -1 。
Sample No. 5 has an in-plane thermal conductivity of 60W m -1 K -1 ；
Sample 6# has an in-plane thermal conductivity of 68 Wm -1 K -1 ；
Sample 7# has an in-plane thermal conductivity of 61W m -1 K -1 ；
Sample 8# has an in-plane thermal conductivity of 62W m -1 K -1 ；
Sample 9# has an in-plane thermal conductivity of 70W m -1 K -1 。
While the application has been described in terms of preferred embodiments, it will be understood by those skilled in the art that various changes and modifications can be made without departing from the scope of the application, and it is intended that the application is not limited to the specific embodiments disclosed.
Claims (14)
1. The preparation method of the boron nitride nanosheets is characterized by comprising the following steps:
stripping the dispersion liquid containing the block hexagonal boron nitride by adopting a high-pressure micro-jet technology to obtain the boron nitride nanosheets;
the transverse dimension of the boron nitride nanosheets is 1-15 mu m, the thickness is 1-10 nm, and the average length-diameter ratio is 1100-2000;
regulating the pressure of the high-pressure microjet to obtain boron nitride nano-sheets with different length-diameter ratios;
generating high pressure by using a high pressure micro-jet device and forcing the liquid flow through a narrow pore canal, thereby generating a transverse shearing force to cause stripping of the bulk hexagonal boron nitride;
the peeling pressure of the boron nitride nano sheet is 50-125 MPa, and the cycle time is 10-100 times;
the dispersion liquid containing the bulk hexagonal boron nitride comprises the bulk boron nitride and a dispersing agent;
the dispersing agent is a mixed solvent of water and an organic solvent.
2. The method according to claim 1, wherein the peeling pressure of the boron nitride nanosheets is between 70 and 80mpa, and the cycle passes are between 45 and 55 times.
3. The method according to claim 1, wherein,
the organic solvent is at least one selected from methanol, ethanol, propanol, isopropanol, dimethylformamide and methyl pyrrolidone.
4. The method according to claim 3, wherein the concentration of the bulk hexagonal boron nitride in the bulk hexagonal boron nitride-containing dispersion is 1 to 3 mg/mL -1 Between them.
5. A method of preparation according to claim 3, wherein the mass ratio of organic solvent/water in the dispersant is between 0 and 3.
6. The method of claim 3, wherein the lateral dimension of the hexagonal boron nitride block is between 2 and 30 μm.
7. A boron nitride nanosheet, characterized in that it is prepared by the method of any one of claims 1-6,
the transverse dimension of the boron nitride nanosheets is 1-15 mu m, the thickness is 1-10 nm, and the average length-diameter ratio is 1100-2000.
8. The boron nitride nano sheet/polymer heat conduction and insulation composite material is characterized by comprising the boron nitride nano sheet and a flexible polymer matrix, wherein the boron nitride nano sheet/polymer heat conduction and insulation composite material is prepared by the method according to any one of claims 1-7.
9. The boron nitride nanoplatelet/polymer thermally conductive and electrically insulating composite of claim 8, wherein the composite has an in-plane thermal conductivity mediumAt 10-70 Wm -1 K -1 The content of the boron nitride nano-sheet is 20-85wt%.
10. The boron nitride nanosheet/polymer heat-conducting and insulating composite material according to claim 8, wherein the composite material has a thickness of 10-150 μm and a density of 1.0-3.0 g/cm 3 。
11. The boron nitride nanosheet/polymer heat-conducting and insulating composite material of claim 8, wherein the flexible polymer matrix comprises polyvinyl alcohol, polyvinylidene fluoride, polyurethane, nanocellulose.
12. A method for preparing the boron nitride nanosheet/polymer heat-conducting and insulating composite material according to any one of claims 8-11, which is characterized by comprising the following steps:
and dispersing the boron nitride nano-sheets in a flexible polymer matrix to form a continuous heat conduction network, thereby obtaining the composite material.
13. The method according to claim 12, wherein the composite material is obtained by mixing a solution containing boron nitride nanoplatelets and a flexible polymer matrix to form a film.
14. The method according to claim 13, wherein the film forming method comprises suction filtration and casting.
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