CN116651720B - Preparation method of high-orientation horizontally-arranged boron nitride film - Google Patents
Preparation method of high-orientation horizontally-arranged boron nitride film Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
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- 238000007731 hot pressing Methods 0.000 claims abstract description 34
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- 229920001721 polyimide Polymers 0.000 claims description 5
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- 229940117955 isoamyl acetate Drugs 0.000 claims description 4
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- 238000005245 sintering Methods 0.000 description 2
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
- B05D1/38—Successively applying liquids or other fluent materials, e.g. without intermediate treatment with intermediate treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/007—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2601/00—Inorganic fillers
- B05D2601/20—Inorganic fillers used for non-pigmentation effect
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Abstract
The application discloses a preparation method of a high-orientation horizontally arranged boron nitride film, which comprises the following steps: using boron nitride powder as a raw material to prepare a slurry; coating the prepared slurry on a release film to obtain a film; compressing the film; repeating the coating and compressing steps for a plurality of times to obtain a pretreated film; and carrying out hot pressing treatment on the pretreated film to obtain the high-orientation horizontally arranged boron nitride film. According to the application, boron nitride powder with a certain diameter is selected to be matched with the coating thickness, and the matching proportion is as follows: boron nitride sheet diameter = 2-4:1, enabling more boron nitride powder in slurry to be horizontally arranged before solidification and molding, and obtaining a boron nitride film with high-orientation horizontal arrangement through multiple coating compression and hot pressing treatment, thereby improving the plane heat conduction performance and dielectric property of the boron nitride film; solves the problems of large energy consumption, difficult mass production and low horizontal directional arrangement degree of the boron nitride sheet layer formed by one-step coating compression molding in the traditional mode.
Description
Technical Field
The application relates to the field of heat conducting materials, in particular to a preparation method of a high-orientation horizontally arranged boron nitride film.
Background
The 5G-age equipment is miniaturized, intensified and light, and meanwhile, the superior performance is pursued, and the ultrahigh frequency signal adopted by the 5G technology has larger dielectric loss in the original material transmission, so that the radiating material of the mobile phone is also required to be more rigorous. In the field of intelligent terminals, this requirement is reflected in the need to simultaneously maintain excellent heat dissipation properties (high thermal conductivity) and to have excellent electrical properties (low dielectric, insulating). The hexagonal boron nitride film has a graphite-like layered structure, has good lubricity, electrical insulation heat conductivity and chemical corrosion resistance, has a theoretical heat conductivity of about 300W/m.K, but the heat conductivity of the hexagonal boron nitride film which is not oriented in practical application cannot be influenced by forming an effective heat conducting network, so that the development of a high-orientation horizontally arranged boron nitride film has a wide market prospect, the peeling is generally carried out by adopting a high-speed mechanical peeling or ultrasonic dispersion technology in the preparation process of the boron nitride film in the past, and then the film is coated and compressed for one time, so that the horizontally oriented arrangement degree of the boron nitride powder before solidification molding is not considered; in the preparation process in the prior art, high-speed mechanical stripping or ultrasonic dispersion stripping is generally used for modification, and then one-time coating, compression and film forming are carried out; the orderly arranged boron nitride heat dissipation films are manufactured by adopting a sintering mode; there are the following disadvantages: the high-speed mechanical stripping and high-temperature sintering modes have high energy consumption, the ultrasonic dispersion efficiency is low, the large-scale production is difficult to form, the horizontal directional arrangement degree of the boron nitride sheet layer formed by one-time coating compression molding is low, and the heat conductivity in the horizontal direction is limited.
In summary, through mass search by the applicant, at least the problem that the production process used in the prior art is difficult to produce in a large scale, the horizontal alignment degree of the boron nitride sheet layer formed by one-time coating compression molding is low, and the thermal conductivity in the horizontal direction is limited, so that development or improvement of a preparation method of the high-alignment horizontal alignment boron nitride film is needed.
Disclosure of Invention
Based on the problems that the production process used in the prior art is difficult to realize large-scale production, the horizontal directional arrangement degree of the boron nitride sheet layer formed by one-time coating compression molding is low, and the heat conductivity in the horizontal direction is limited, the application provides a preparation method of a high-directional horizontal arrangement boron nitride film, which comprises the following specific technical scheme:
a preparation method of a high-orientation horizontally arranged boron nitride film comprises the following steps:
using boron nitride powder as a raw material to prepare a slurry;
coating the prepared slurry on a release film to obtain a film;
compressing the film;
repeating the coating and compressing steps for a plurality of times to obtain a pretreated film;
and carrying out hot pressing treatment on the pretreated film to obtain the high-orientation horizontally arranged boron nitride film.
Further, the preparation method comprises the following steps:
s1: uniformly mixing 100 parts by weight of boron nitride powder, 300-600 parts by weight of solvent and 10-50 parts by weight of polymer to obtain slurry;
s2, coating the obtained slurry on a release film by using a scraper to obtain a film;
s3, compressing the film;
s4, repeating the steps S2 and S3 for a plurality of times to obtain a pretreatment film;
and S5, carrying out hot pressing treatment on the pretreated film to obtain the high-orientation horizontally arranged boron nitride film.
Further, the boron nitride powder has a sheet diameter D50 of 50nm to 200 μm.
Further, the coating thickness of the coating is 5-1000 μm.
Further, the ratio of the thickness of the coating to the size of the sheet diameter of the boron nitride powder is 2-4:1.
further, the pressure of the compression treatment is 1-500 MPa, the temperature is 20-500 ℃, and the treatment time is 5 s-24 h.
Further, the pressure of the hot pressing treatment is 1-500 MPa, the temperature is 100-500 ℃, and the treatment time is 5 s-24 h.
Further, in the step S4, the steps S2 and S3 are repeated 2 to 50 times to obtain a pretreated film.
Further, the polymer is at least one selected from the group consisting of polyvinyl alcohol, urea formaldehyde resin, melamine formaldehyde resin, phenolic resin, epoxy resin, polyester resin, polyamide resin, polyvinyl chloride resin, polyurethane resin, polymethacrylate and polyimide resin.
Further, the solvent is at least one selected from deionized water, methanol, ethanol, propanol, butanol, ethyl acetate, isoamyl acetate, dimethylformamide, toluene, xylene and cyclohexane.
In the technical scheme, boron nitride powder with a certain diameter is selected to be matched with the coating thickness, and the matching proportion is the coating thickness: boron nitride sheet diameter = 2-4:1, enabling more boron nitride powder in slurry to be horizontally arranged before solidification and molding, and obtaining a boron nitride film with high-orientation horizontal arrangement through multiple coating compression and hot pressing treatment, thereby improving the plane heat conduction performance and dielectric property of the boron nitride film;
according to the scheme, the boron nitride powder with the size of one piece diameter is screened to be matched with the coating thickness, then simple mechanical mixing is carried out, multiple coating compression and hot pressing treatment can be carried out, the boron nitride film with high directional horizontal arrangement is obtained, the problems that the energy consumption is high, the large-scale production is difficult, the horizontal directional arrangement degree of the boron nitride sheet layers formed by one-time coating compression is low in the traditional mode are solved, the whole process does not need to carry out high-speed mechanical stripping on the boron nitride powder, the energy consumption is low, and the yield is large in scale. Meanwhile, the method has certain guiding significance on the coating film forming process of other two-dimensional materials.
Drawings
FIG. 1 is a scanning electron microscope image of a cross section of a highly oriented horizontally aligned boron nitride prepared in example 1 of the present application;
FIG. 2 is a scanning electron microscope image of a cross section of a boron nitride film prepared in example 2 of the present application;
FIG. 3 is a scanning electron microscope image of a cross section of a highly oriented horizontally aligned boron nitride film prepared in example 3 of the present application;
FIG. 4 is a scanning electron microscope image of a cross section of a highly oriented horizontally aligned boron nitride film prepared in example 5 of the present application;
FIG. 5 is a graph showing the effect of the high-orientation horizontally aligned boron nitride film prepared in example 1 and the boron nitride film prepared in example 2 in a simulation experiment environment;
FIG. 6 is a block diagram of a preparation process of the present application.
Detailed Description
The present application will be described in further detail with reference to the following examples thereof in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The preparation method of the high-orientation horizontally arranged boron nitride film in the embodiment of the application comprises the following steps:
using boron nitride powder as a raw material to prepare a slurry;
coating the prepared slurry on a release film to obtain a film;
compressing the film;
repeating the coating and compressing steps for a plurality of times to obtain a pretreated film;
and carrying out hot pressing treatment on the pretreated film to obtain the high-orientation horizontally arranged boron nitride film.
In one embodiment, the method of preparation comprises the steps of:
s1: uniformly mixing 100 parts by weight of boron nitride powder, 300-600 parts by weight of solvent and 10-50 parts by weight of polymer to obtain slurry;
s2, coating the obtained slurry on a release film by using a scraper to obtain a film;
s3, compressing the film;
s4, repeating the steps S2 and S3 for a plurality of times to obtain a pretreatment film;
and S5, carrying out hot pressing treatment on the pretreated film to obtain the high-orientation horizontally arranged boron nitride film.
In one embodiment, the boron nitride powder has a sheet diameter D50 of 50nm to 200 μm.
In one embodiment, the boron nitride powder has a sheet diameter D50 of 100nm to 100 μm.
In one embodiment, the boron nitride powder has a sheet diameter D50 of 5 μm to 10 μm.
In one embodiment, the coating thickness of the coating is 5 μm to 1000 μm.
In one embodiment, the coating thickness of the coating is 10 μm to 500 μm.
In one embodiment, the coating thickness of the coating is 20 μm to 30 μm.
In one embodiment, the ratio of the thickness of the coating to the size of the sheet diameter of the boron nitride powder is 2-4:1.
in one embodiment, the pressure of the compression treatment is 1-500 MPa, the temperature is 20-500 ℃, and the treatment time is 5 s-24 h.
In one embodiment, the compression treatment pressure is 20-500 MPa, the temperature is 20-300 ℃, and the treatment time is 5 s-12 h.
In one embodiment, the compression treatment pressure is 15-30 MPa, the temperature is 20-40 ℃, and the treatment time is 10-15 min.
In one embodiment, the pressure of the hot pressing treatment is 1-500 MPa, the temperature is 100-500 ℃, and the treatment time is 5 s-24 h.
In one embodiment, the pressure of the hot pressing treatment is 20-60 MPa, the temperature is 100-300 ℃, and the treatment time is 5 s-12 h.
In one embodiment, the pressure of the hot pressing treatment is 20 MPa-30 MPa, the temperature is 100-150 ℃, and the treatment time is 30-35 min.
In one embodiment, in the step S4, the steps S2 and S3 are repeated 2 to 50 times to obtain the pretreated film.
In one embodiment, in the step S4, the steps S2 and S3 are repeated 2 to 10 times to obtain the pretreated film.
In one embodiment, in the step S4, the steps S2 and S3 are repeated 3 to 6 times to obtain the pretreated film.
In one embodiment, the polymer is selected from at least one of polyvinyl alcohol, urea formaldehyde resin, melamine formaldehyde resin, phenolic resin, epoxy resin, polyester resin, polyamide resin, polyvinyl chloride resin, polyurethane resin, polymethacrylate, polyimide resin.
In one embodiment, the solvent is selected from at least one of deionized water, methanol, ethanol, propanol, butanol, ethyl acetate, isoamyl acetate, dimethylformamide, toluene, xylene, and cyclohexane.
In one embodiment, the condition of uniform mixing in the step S1 is that the dispersion is carried out for 30min at a rotation speed of 1500rpm by using a mechanical dispersing machine.
In one embodiment, the release film is a double-sided release film.
Embodiments of the present application will be described in detail below with reference to specific examples.
Example 1:
the embodiment provides a preparation method of a high-orientation horizontally arranged boron nitride film, which comprises the following steps:
s1, mixing and stirring 1000g of boron nitride powder with the sheet diameter D50 of 10 mu m, 4000g of deionized water and 250g of urea-formaldehyde resin, wherein the rotating speed is 1500rpm, and the stirring time is 30min;
s2, coating the slurry on the double-sided release film by selecting the thickness of a scraper matched with the thickness of the scraper, wherein the coating thickness is 30 mu m, so as to obtain a film;
s3, carrying out compression treatment on the film, and carrying out hot pressing by using a flat plate at the temperature of 40 ℃ and the pressure of 30MPa for 10min;
s4, repeating the steps S2 and S3 three times;
and S5, finally, carrying out hot pressing treatment, namely carrying out hot pressing by using a flat plate, wherein the temperature is 100 ℃, the pressure is 30MPa, and the time is 30min, so as to obtain the high-orientation horizontally arranged boron nitride film with the thickness of 75 mu m.
Example 2
The embodiment provides a preparation method of a boron nitride heat dissipation film, which comprises the following steps:
s1, mixing and stirring 1000g of boron nitride powder with the sheet diameter D50 of 10 mu m, 4000g of deionized water and 250g of urea-formaldehyde resin, wherein the rotating speed is 1500rpm, and the stirring time is 30min;
s2, coating the slurry on the double-sided release film by selecting the thickness of a scraper matched with the thickness of the scraper, wherein the coating thickness is 120 mu m, so as to obtain a film;
s3, carrying out compression treatment on the film, and carrying out hot pressing by using a flat plate at the temperature of 40 ℃ and the pressure of 30MPa for 10min;
and S4, finally, carrying out hot pressing treatment, namely carrying out hot pressing by using a flat plate, wherein the temperature is 100 ℃, the pressure is 30MPa, and the time is 30min, so as to obtain the boron nitride film with the thickness of 75 mu m.
Example 3
The embodiment provides a preparation method of a high-orientation horizontally arranged boron nitride film, which comprises the following steps:
s1, mixing and stirring 1000g of boron nitride powder with the sheet diameter D50 of 10 mu m, 3000g of isoamyl acetate and 250g of polyimide resin, wherein the rotating speed is 1500rpm, and the stirring time is 30min;
s2, coating the slurry on the double-sided release film by selecting the thickness of a scraper matched with the thickness of the scraper, wherein the coating thickness is 30 mu m, so as to obtain a film;
s3, carrying out compression treatment on the film, and carrying out hot pressing by using a flat plate at the temperature of 40 ℃ and the pressure of 15MPa for 10min;
s4, repeating the steps S2 and S3 three times;
and S5, finally, carrying out hot pressing treatment, namely carrying out hot pressing by using a flat plate, wherein the temperature is 100 ℃, the pressure is 30MPa, and the time is 30min, so as to obtain the high-orientation horizontally arranged boron nitride film with the thickness of 75 mu m.
Example 4
The embodiment provides a preparation method of a high-orientation horizontally arranged boron nitride film, which comprises the following steps:
s1, mixing and stirring 1000g of boron nitride powder with the sheet diameter D50 of 20 mu m, 4000g of deionized water and 250g of urea-formaldehyde resin, wherein the rotating speed is 1500rpm, and the stirring time is 30min;
s2, coating the slurry on the double-sided release film by selecting the thickness of a scraper matched with the thickness of the scraper, wherein the coating thickness is 120 mu m, so as to obtain a film;
s3, carrying out compression treatment on the film, and carrying out hot pressing by using a flat plate at the temperature of 40 ℃ and the pressure of 30MPa for 10min;
and S4, finally, carrying out hot pressing treatment, namely carrying out hot pressing by using a flat plate, wherein the temperature is 100 ℃, the pressure is 30MPa, and the time is 30min, so as to obtain the high-orientation horizontally arranged boron nitride film with the thickness of 75 mu m.
Example 5
The embodiment provides a preparation method of a high-orientation horizontally arranged boron nitride film, which comprises the following steps:
s1, mixing and stirring 1000g of boron nitride powder with the sheet diameter D50 of 15 mu m, 3000g of absolute ethyl alcohol and 250g of polyimide resin, wherein the rotating speed is 1500rpm, and the stirring time is 30min;
s2, coating the slurry on the double-sided release film by selecting the thickness of a scraper matched with the thickness of the scraper, wherein the coating thickness is 120 mu m, so as to obtain a film;
s3, carrying out compression treatment on the film, and carrying out hot pressing by using a flat plate at the temperature of 40 ℃ and the pressure of 30MPa for 10min;
and S4, finally, carrying out hot pressing treatment, namely carrying out hot pressing by using a flat plate, wherein the temperature is 100 ℃, the pressure is 30MPa, and the time is 30min, so as to obtain the high-orientation horizontally arranged boron nitride film with the thickness of 75 mu m.
Example 6
The embodiment provides a preparation method of a high-orientation horizontally arranged boron nitride film, which comprises the following steps:
s1, mixing and stirring 800g of boron nitride powder with the sheet diameter D50 of 5 mu m, 3000g of N-methyl pyrrolidone and 250g of polyvinylidene fluoride, wherein the rotating speed is 1500rpm, and the stirring time is 30min;
s2, coating the slurry on the double-sided release film by selecting the thickness of a scraper matched with the thickness of the scraper, wherein the coating thickness is 20 mu m, so as to obtain a film;
s3, carrying out compression treatment on the film, and carrying out hot pressing by using a flat plate at the temperature of 80 ℃ and the pressure of 30MPa for 10min;
s4, repeating the steps S2 and S3 six times;
and S5, finally, carrying out hot pressing treatment, namely carrying out hot pressing by using a flat plate, wherein the temperature is 100 ℃, the pressure is 30MPa, and the time is 30min, so as to obtain the high-orientation horizontally arranged boron nitride film with the thickness of 75 mu m.
Example 7
And (3) detecting the performance of the heat dissipation film, namely respectively taking the boron nitride films prepared in examples 1-6, measuring the thermal diffusivity of the films by using a flash thermal diffusivity tester (LFA-467), measuring the specific heat capacity of the films by using a differential scanning calorimetry, measuring the density by using a drainage method, and measuring the dielectric constant and dielectric loss of the films at the 5G frequency by using a vector network analyzer, wherein the performance detection results of the boron nitride films are shown in the table 1.
Table 1:
as can be seen from the above table, the ratio of the coating thickness to the size of the boron nitride sheet in the embodiment of the present application is 3:1 the improvement of the thermal conductivity and the dielectric property ratio of the boron nitride film prepared by the method is very high, and the highest thermal conductivity is 46.67W.m -1 K -1 The dielectric constant @5GHz was 3.7758 and the dielectric loss @5GHz was 0.0028.
Example 8
Heat dissipation Capacity verification experiment
And determining the effect of the boron nitride film in the actual use environment by adopting a simulation experiment method for carrying out steady-state heat dissipation on a single heating source. And attaching the boron nitride film on a PCB heating plate for heating, observing the hot spot temperature on the surface of the film after reaching a steady state, and verifying the heat dissipation effect of the boron nitride film by observing the hot spot temperature change before and after film attachment. As a result of the simulation experiment, as shown in fig. five, a is a blank PCB heating plate, B is a high-orientation horizontally aligned boron nitride film provided in example 1 of the present application, and C is a boron nitride film provided in example 2 of the present application. It can be seen from the graph that the highest value of the surface hot spot temperature of B is the lowest, the next highest of C and the highest of A show that the high-orientation horizontally arranged boron nitride film prepared by the method of the embodiment 1 has the best heat dissipation effect.
During the experiment, it was found that the density of boron nitride was 2.2g/cm 3 The density of the polymer is generally in the range of 1.0 to 1.5 g/cm 3 And if the selected coating thickness is too thin, the surface of the casting film is defective, and a heat conduction channel in the film is blocked, so that the heat conductivity and dielectric property of the casting film are affected. Therefore, we propose to screen the size of the proper sheet diameter and the coating thickness to match, ensure that more vertical boron nitride powder is scraped to form more heat conduction channels in a horizontal orientation before the slurry is solidified and formed in the coating process, then compress the slurry to discharge air between the boron nitride sheets, so that the contact between the boron nitride sheets is more compact, and finally obtain the boron nitride film in a high-orientation horizontal arrangement through repeated coating and hot pressing. The heat conduction performance and the dielectric performance of the plane of the boron nitride film are improved; meanwhile, the energy consumption can be reduced, and the yield scale is large.
As can be seen from fig. 1 and 2, the product obtained by screening the matching of the size of the boron nitride sheet diameter and the coating thickness and carrying out multiple coating compression film forming has better horizontal directional arrangement, and meanwhile, the gaps between the boron nitride sheet layers are smaller, and the arrangement and stacking are more orderly, so that the thermal conductivity and the dielectric property of the product are improved.
In the technological process, firstly, boron nitride powder is screened, and then mixed with solvent and polymer according to a certain proportion. The sizing agent is coated on a double-sided release film by selecting the thickness of a scraper matched with the sizing agent, so as to obtain a film; and (3) compressing the film, discharging air between the boron nitride sheets, enabling the air between the boron nitride sheets to be in tight contact, obtaining a first layer of boron nitride film, then performing second coating and compressing treatment on the first layer of film, repeating the steps for a plurality of times, and finally performing hot pressing treatment on the obtained boron nitride film. The application can obtain the boron nitride film which is arranged horizontally in a high orientation through multiple coating and compression, thereby obviously improving the plane heat conduction performance and the dielectric property of the boron nitride film.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the application, which are described in detail and are not to be construed as limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of protection of the present application is to be determined by the appended claims.
Claims (3)
1. The preparation method of the high-orientation horizontally-arranged boron nitride film is characterized by comprising the following steps of:
s1: uniformly mixing 100 parts by weight of boron nitride powder, 300-600 parts by weight of solvent and 10-50 parts by weight of polymer to obtain slurry;
s2, coating the obtained slurry on a release film by using a scraper to obtain a film;
s3, compressing the film;
s4, repeating the steps S2 and S3 for 3-6 times to obtain a pretreatment film;
s5, carrying out hot pressing treatment on the pretreated film to obtain a high-orientation horizontally arranged boron nitride film;
wherein the sheet diameter D50 of the boron nitride powder is 5-10 mu m; the coating thickness of the coating is 20-30 mu m; the ratio of the thickness of the coating to the size of the sheet diameter of the boron nitride powder is 2-4:1, a step of; the pressure of the compression treatment is 15-30 MPa, the temperature is 20-40 ℃, and the treatment time is 10-15 min; the pressure of the hot pressing treatment is 20-30 MPa, the temperature is 100-150 ℃, and the treatment time is 30-35 min.
2. The method for producing a highly oriented horizontally aligned boron nitride film according to claim 1, wherein the polymer is at least one selected from the group consisting of polyvinyl alcohol, urea resin, melamine formaldehyde resin, phenol resin, epoxy resin, polyester resin, polyamide resin, polyvinyl chloride resin, polyurethane resin, polymethacrylate, polyimide resin.
3. The method for preparing a highly oriented horizontally aligned boron nitride film according to claim 2, wherein the solvent is at least one selected from the group consisting of deionized water, methanol, ethanol, propanol, butanol, ethyl acetate, isoamyl acetate, dimethylformamide, toluene, xylene, and cyclohexane.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106739397A (en) * | 2016-11-14 | 2017-05-31 | 青岛卓英社科技股份有限公司 | The preparation method of high-orientation absorbing material |
CN107189091A (en) * | 2016-03-15 | 2017-09-22 | Bgt材料有限公司 | The manufacture method of hexagonal boron nitride planes |
CN113179611A (en) * | 2021-03-15 | 2021-07-27 | 佛山市晟鹏科技有限公司 | Boron nitride heat dissipation film and preparation method and application thereof |
CN113524741A (en) * | 2021-07-29 | 2021-10-22 | 哈尔滨工业大学(威海) | Vertically-arranged boron nitride nanosheet high-molecular composite material heat-conducting sheet and preparation method thereof |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107189091A (en) * | 2016-03-15 | 2017-09-22 | Bgt材料有限公司 | The manufacture method of hexagonal boron nitride planes |
CN106739397A (en) * | 2016-11-14 | 2017-05-31 | 青岛卓英社科技股份有限公司 | The preparation method of high-orientation absorbing material |
CN113179611A (en) * | 2021-03-15 | 2021-07-27 | 佛山市晟鹏科技有限公司 | Boron nitride heat dissipation film and preparation method and application thereof |
WO2022193572A1 (en) * | 2021-03-15 | 2022-09-22 | 佛山市晟鹏科技有限公司 | Boron nitride heat dissipation film, preparation method therefor, and application thereof |
CN113524741A (en) * | 2021-07-29 | 2021-10-22 | 哈尔滨工业大学(威海) | Vertically-arranged boron nitride nanosheet high-molecular composite material heat-conducting sheet and preparation method thereof |
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