CN112980215A - High-thermal-conductivity boron nitride powder filler and preparation method thereof - Google Patents
High-thermal-conductivity boron nitride powder filler and preparation method thereof Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
The invention discloses a high heat conduction boron nitride powder filler and a preparation method thereof, wherein the formula comprises the following components: the adhesive comprises sodium hydroxide, boron nitride, an epoxy silane coupling agent, absolute ethyl alcohol and deionized water, wherein the mass percentage of each component is as follows: 15-25 parts of sodium hydroxide, 40-60 parts of boron nitride, 20-30 parts of epoxy silane coupling agent, 10-20 parts of absolute ethyl alcohol and 5-10 parts of deionized water; the invention is safe and reliable, the microsphere boron nitride easily forms a heat conduction network, the particle size of the boron nitride is optimized, the heat conduction effect of the filler is improved, the wet modification process conditions of the epoxy silane coupling agent on the boron nitride powder are optimized, the boron nitride powder has good compatibility with organic matters, and the viscosity, the oiliness, the water content and the like meet the technical index requirements.
Description
Technical Field
The invention relates to the technical field of high-thermal-conductivity boron nitride powder fillers, in particular to a high-thermal-conductivity boron nitride powder filler and a preparation method thereof.
Background
The inorganic heat-conducting particles mainly comprise nitrides, carbides, oxides and the like, at present, the high heat-conducting insulating filler developed by industrial and scientific research units is mainly characterized in that the inorganic filler, the selection of the particle size and the shape of the inorganic filler and the modification of the filler body have great significance for preparing special high heat-conducting insulating materials, boron nitride is composed of nitrogen and boron atoms, because the boron nitride has the same structure as graphite and is of a laminated structure and is called white graphite, compared with other inorganic heat-conducting fillers, BN is a high-temperature insulating material with the most excellent ceramic performance, has high resistivity, high breakdown field strength, strong heat-conducting capability, the lowest dielectric loss and the lowest dielectric constant, is the optimal filling particle for developing composite materials with low dielectric loss, low dielectric constant and high heat-conducting property, and because boron nitride powder belongs to the hydrophobic and oleophobic property, has poor compatibility with an organic matrix and is not uniformly dispersed in the resin matrix, the agglomeration probability is high, and the heat conduction performance of the resin composite material is influenced; aiming at the defects, it is necessary to design a high-thermal-conductivity boron nitride powder filler and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity boron nitride powder filler and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a high-thermal-conductivity boron nitride powder filler comprises the following components in percentage by weight: the adhesive comprises sodium hydroxide, boron nitride, an epoxy silane coupling agent, absolute ethyl alcohol and deionized water, wherein the mass percentage of each component is as follows: 15-25 parts of sodium hydroxide, 40-60 parts of boron nitride, 20-30 parts of epoxy silane coupling agent, 10-20 parts of absolute ethyl alcohol and 5-10 parts of deionized water.
A preparation method of a high-thermal-conductivity boron nitride powder filler comprises the following steps of firstly, selecting materials; step two, boron nitride treatment; step three, ultrasonic dispersion; step four, preheating and sintering; step five, cooling and storing;
in the first step, the contents of the components are as follows: selecting 15-25 parts of sodium hydroxide, 40-60 parts of boron nitride, 20-30 parts of epoxy silane coupling agent, 10-20 parts of absolute ethyl alcohol and 5-10 parts of deionized water, and weighing;
in the second step, the boron nitride treatment comprises the following steps:
1) manually selecting a proper boron nitride powder raw material, filtering the boron nitride powder raw material, and pouring the boron nitride powder raw material into a reaction kettle;
2) adding absolute ethyl alcohol into the reaction kettle, uniformly stirring, adding sodium hydroxide again, mixing and stirring for 10-20 min;
3) pouring out the mixture, and filtering the mixture through a filter screen to obtain boron nitride powder;
in the third step, the ultrasonic dispersion comprises the following steps:
1) manually pouring boron nitride powder into an ultrasonic machine, adding deionized water, stirring for 10-20min, then adding an epoxy silane coupling agent while stirring, and carrying out wet modification treatment on the boron nitride powder until the solution becomes turbid;
2) starting an ultrasonic machine, ultrasonically stripping the mixed solution, then pouring the mixed solution into a centrifugal machine, and centrifugally dispersing;
in the fourth step, the preheating sintering comprises the following steps:
1) manually pouring out the mixture obtained in the step three 2), pouring the mixture into a tubular furnace, uniformly stirring, adding absolute ethyl alcohol again, mixing, stirring and standing;
2) raising the tubular temperature to 800 ℃ for preheating and sintering for 20-40min, then raising the temperature to 1200 ℃ for continuous sintering for 6-8h, taking out and standing to obtain the high-thermal-conductivity boron nitride powder filler;
and in the fifth step, standing and cooling the high-thermal-conductivity boron nitride powder filler obtained in the fourth step 2) to room temperature, automatically sealing and packaging the high-thermal-conductivity boron nitride powder filler by a sealing machine, and then packing and storing the sealed high-thermal-conductivity boron nitride powder filler in boxes integrally.
According to the technical scheme, the contents of the components are respectively as follows: 20 parts of sodium hydroxide, 50 parts of boron nitride, 25 parts of epoxy silane coupling agent, 15 parts of absolute ethyl alcohol and 10 parts of deionized water.
According to the technical scheme, the reaction kettle in the step two 1) needs to be rinsed with clear water before being used.
According to the technical scheme, the power of the ultrasonic machine in the step three 1) is 500W.
According to the technical scheme, the mixture in the step four 1) needs to be filtered before being poured into the tube furnace.
According to the technical scheme, in the fifth step, disinfection treatment is required before boxing.
Compared with the prior art, the invention has the following beneficial effects: the invention is safe and reliable, the microsphere boron nitride is easy to form a heat conduction network, the particle size of the boron nitride is optimized, the heat conduction effect of the filler is improved, the wet modification process conditions of the epoxy silane coupling agent on the boron nitride powder are optimized, the boron nitride powder has good compatibility with organic matters, and the viscosity, the oiliness, the water content and the like meet the technical index requirements.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: a high heat conduction boron nitride powder filler and a preparation method thereof are disclosed:
example 1:
a high-thermal-conductivity boron nitride powder filler comprises the following components in percentage by weight: the adhesive comprises sodium hydroxide, boron nitride, an epoxy silane coupling agent, absolute ethyl alcohol and deionized water, wherein the mass percentage of each component is as follows: 25 parts of sodium hydroxide, 40 parts of boron nitride, 25 parts of an epoxy silane coupling agent, 15 parts of absolute ethyl alcohol and 10 parts of deionized water.
A preparation method of a high-thermal-conductivity boron nitride powder filler comprises the following steps of firstly, selecting materials; step two, boron nitride treatment; step three, ultrasonic dispersion; step four, preheating and sintering; step five, cooling and storing;
in the first step, the contents of the components are as follows: selecting 25 parts of sodium hydroxide, 40 parts of boron nitride, 25 parts of epoxy silane coupling agent, 15 parts of absolute ethyl alcohol and 10 parts of deionized water, and weighing;
in the second step, the boron nitride treatment comprises the following steps:
1) manually selecting a proper boron nitride powder raw material, filtering the boron nitride powder raw material, and then pouring the boron nitride powder raw material into a reaction kettle, wherein the reaction kettle needs to be rinsed by clear water before use;
2) adding absolute ethyl alcohol into the reaction kettle, uniformly stirring, adding sodium hydroxide again, mixing and stirring for 10-20 min;
3) pouring out the mixture, and filtering the mixture through a filter screen to obtain boron nitride powder;
in the third step, the ultrasonic dispersion comprises the following steps:
1) manually pouring boron nitride powder into an ultrasonic machine, wherein the ultrasonic machine power is 500W, adding deionized water, stirring for 10-20min, then adding an epoxy silane coupling agent while stirring, and carrying out wet modification treatment on the boron nitride powder until the solution becomes turbid;
2) starting an ultrasonic machine, ultrasonically stripping the mixed solution, then pouring the mixed solution into a centrifugal machine, and centrifugally dispersing;
in the fourth step, the preheating sintering comprises the following steps:
1) manually pouring out the mixture obtained in the step three 2), pouring the mixture into a tubular furnace, filtering the mixture before pouring the mixture into the tubular furnace, adding absolute ethyl alcohol after uniformly stirring, mixing, stirring and standing;
2) raising the tubular temperature to 800 ℃ for preheating and sintering for 20-40min, then raising the temperature to 1200 ℃ for continuous sintering for 6-8h, taking out and standing to obtain the high-thermal-conductivity boron nitride powder filler;
and in the fifth step, standing and cooling the high-thermal-conductivity boron nitride powder filler obtained in the fourth step 2) to room temperature, automatically sealing and packaging the high-thermal-conductivity boron nitride powder filler by a sealing machine, and then packing and storing the sealed high-thermal-conductivity boron nitride powder filler in boxes integrally, wherein the high-thermal-conductivity boron nitride powder filler needs to be sterilized before being packed in the boxes.
Example 2:
a high-thermal-conductivity boron nitride powder filler comprises the following components in percentage by weight: the adhesive comprises sodium hydroxide, boron nitride, an epoxy silane coupling agent, absolute ethyl alcohol and deionized water, wherein the mass percentage of each component is as follows: 20 parts of sodium hydroxide, 50 parts of boron nitride, 25 parts of epoxy silane coupling agent, 15 parts of absolute ethyl alcohol and 10 parts of deionized water.
A preparation method of a high-thermal-conductivity boron nitride powder filler comprises the following steps of firstly, selecting materials; step two, boron nitride treatment; step three, ultrasonic dispersion; step four, preheating and sintering; step five, cooling and storing;
in the first step, the contents of the components are as follows: selecting 20 parts of sodium hydroxide, 50 parts of boron nitride, 25 parts of epoxy silane coupling agent, 15 parts of absolute ethyl alcohol and 10 parts of deionized water, and weighing;
in the second step, the boron nitride treatment comprises the following steps:
1) manually selecting a proper boron nitride powder raw material, filtering the boron nitride powder raw material, and then pouring the boron nitride powder raw material into a reaction kettle, wherein the reaction kettle needs to be rinsed by clear water before use;
2) adding absolute ethyl alcohol into the reaction kettle, uniformly stirring, adding sodium hydroxide again, mixing and stirring for 10-20 min;
3) pouring out the mixture, and filtering the mixture through a filter screen to obtain boron nitride powder;
in the third step, the ultrasonic dispersion comprises the following steps:
1) manually pouring boron nitride powder into an ultrasonic machine, wherein the ultrasonic machine power is 500W, adding deionized water, stirring for 10-20min, then adding an epoxy silane coupling agent while stirring, and carrying out wet modification treatment on the boron nitride powder until the solution becomes turbid;
2) starting an ultrasonic machine, ultrasonically stripping the mixed solution, then pouring the mixed solution into a centrifugal machine, and centrifugally dispersing;
in the fourth step, the preheating sintering comprises the following steps:
1) manually pouring out the mixture obtained in the step three 2), pouring the mixture into a tubular furnace, filtering the mixture before pouring the mixture into the tubular furnace, adding absolute ethyl alcohol after uniformly stirring, mixing, stirring and standing;
2) raising the tubular temperature to 800 ℃ for preheating and sintering for 20-40min, then raising the temperature to 1200 ℃ for continuous sintering for 6-8h, taking out and standing to obtain the high-thermal-conductivity boron nitride powder filler;
and in the fifth step, standing and cooling the high-thermal-conductivity boron nitride powder filler obtained in the fourth step 2) to room temperature, automatically sealing and packaging the high-thermal-conductivity boron nitride powder filler by a sealing machine, and then packing and storing the sealed high-thermal-conductivity boron nitride powder filler in boxes integrally, wherein the high-thermal-conductivity boron nitride powder filler needs to be sterilized before being packed in the boxes.
Example 3:
a high-thermal-conductivity boron nitride powder filler comprises the following components in percentage by weight: the adhesive comprises sodium hydroxide, boron nitride, an epoxy silane coupling agent, absolute ethyl alcohol and deionized water, wherein the mass percentage of each component is as follows: 15 parts of sodium hydroxide, 60 parts of boron nitride, 25 parts of epoxy silane coupling agent, 15 parts of absolute ethyl alcohol and 10 parts of deionized water.
A preparation method of a high-thermal-conductivity boron nitride powder filler comprises the following steps of firstly, selecting materials; step two, boron nitride treatment; step three, ultrasonic dispersion; step four, preheating and sintering; step five, cooling and storing;
in the first step, the contents of the components are as follows: selecting 15 parts of sodium hydroxide, 60 parts of boron nitride, 25 parts of epoxy silane coupling agent, 15 parts of absolute ethyl alcohol and 10 parts of deionized water, and weighing;
in the second step, the boron nitride treatment comprises the following steps:
1) manually selecting a proper boron nitride powder raw material, filtering the boron nitride powder raw material, and then pouring the boron nitride powder raw material into a reaction kettle, wherein the reaction kettle needs to be rinsed by clear water before use;
2) adding absolute ethyl alcohol into the reaction kettle, uniformly stirring, adding sodium hydroxide again, mixing and stirring for 10-20 min;
3) pouring out the mixture, and filtering the mixture through a filter screen to obtain boron nitride powder;
in the third step, the ultrasonic dispersion comprises the following steps:
1) manually pouring boron nitride powder into an ultrasonic machine, wherein the ultrasonic machine power is 500W, adding deionized water, stirring for 10-20min, then adding an epoxy silane coupling agent while stirring, and carrying out wet modification treatment on the boron nitride powder until the solution becomes turbid;
2) starting an ultrasonic machine, ultrasonically stripping the mixed solution, then pouring the mixed solution into a centrifugal machine, and centrifugally dispersing;
in the fourth step, the preheating sintering comprises the following steps:
1) manually pouring out the mixture obtained in the step three 2), pouring the mixture into a tubular furnace, filtering the mixture before pouring the mixture into the tubular furnace, adding absolute ethyl alcohol after uniformly stirring, mixing, stirring and standing;
2) raising the tubular temperature to 800 ℃ for preheating and sintering for 20-40min, then raising the temperature to 1200 ℃ for continuous sintering for 6-8h, taking out and standing to obtain the high-thermal-conductivity boron nitride powder filler;
and in the fifth step, standing and cooling the high-thermal-conductivity boron nitride powder filler obtained in the fourth step 2) to room temperature, automatically sealing and packaging the high-thermal-conductivity boron nitride powder filler by a sealing machine, and then packing and storing the sealed high-thermal-conductivity boron nitride powder filler in boxes integrally, wherein the high-thermal-conductivity boron nitride powder filler needs to be sterilized before being packed in the boxes.
The properties of the examples are compared in the following table:
based on the above, the invention has the advantages that the invention is safe and reliable, the microsphere boron nitride is easy to form a heat conduction network, the particle size of the boron nitride is optimized, the heat conduction effect of the filler is improved, the wet modification process conditions of the epoxy silane coupling agent on the boron nitride powder are optimized, the boron nitride powder has good compatibility with organic matters, and the viscosity, the oiliness, the water content and the like meet the technical index requirements.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The high-thermal-conductivity boron nitride powder filler is characterized in that: the formula comprises the following components: the adhesive comprises sodium hydroxide, boron nitride, an epoxy silane coupling agent, absolute ethyl alcohol and deionized water, wherein the mass percentage of each component is as follows: 15-25 parts of sodium hydroxide, 40-60 parts of boron nitride, 20-30 parts of epoxy silane coupling agent, 10-20 parts of absolute ethyl alcohol and 5-10 parts of deionized water.
2. A preparation method of a high-thermal-conductivity boron nitride powder filler comprises the following steps of firstly, selecting materials; step two, boron nitride treatment; step three, ultrasonic dispersion; step four, preheating and sintering; step five, cooling and storing; the method is characterized in that:
in the first step, the contents of the components are as follows: selecting 15-25 parts of sodium hydroxide, 40-60 parts of boron nitride, 20-30 parts of epoxy silane coupling agent, 10-20 parts of absolute ethyl alcohol and 5-10 parts of deionized water, and weighing;
in the second step, the boron nitride treatment comprises the following steps:
1) manually selecting a proper boron nitride powder raw material, filtering the boron nitride powder raw material, and pouring the boron nitride powder raw material into a reaction kettle;
2) adding absolute ethyl alcohol into the reaction kettle, uniformly stirring, adding sodium hydroxide again, mixing and stirring for 10-20 min;
3) pouring out the mixture, and filtering the mixture through a filter screen to obtain boron nitride powder;
in the third step, the ultrasonic dispersion comprises the following steps:
1) manually pouring boron nitride powder into an ultrasonic machine, adding deionized water, stirring for 10-20min, then adding an epoxy silane coupling agent while stirring, and carrying out wet modification treatment on the boron nitride powder until the solution becomes turbid;
2) starting an ultrasonic machine, ultrasonically stripping the mixed solution, then pouring the mixed solution into a centrifugal machine, and centrifugally dispersing;
in the fourth step, the preheating sintering comprises the following steps:
1) manually pouring out the mixture obtained in the step three 2), pouring the mixture into a tubular furnace, uniformly stirring, adding absolute ethyl alcohol again, mixing, stirring and standing;
2) raising the tubular temperature to 800 ℃ for preheating and sintering for 20-40min, then raising the temperature to 1200 ℃ for continuous sintering for 6-8h, taking out and standing to obtain the high-thermal-conductivity boron nitride powder filler;
and in the fifth step, standing and cooling the high-thermal-conductivity boron nitride powder filler obtained in the fourth step 2) to room temperature, automatically sealing and packaging the high-thermal-conductivity boron nitride powder filler by a sealing machine, and then packing and storing the sealed high-thermal-conductivity boron nitride powder filler in boxes integrally.
3. The boron nitride powder filler with high thermal conductivity according to claim 1, wherein: the contents of the components are respectively as follows: 20 parts of sodium hydroxide, 50 parts of boron nitride, 25 parts of epoxy silane coupling agent, 15 parts of absolute ethyl alcohol and 10 parts of deionized water.
4. The preparation method of the boron nitride powder filler with high thermal conductivity according to claim 2, characterized by comprising the following steps: and in the second step 1), the reaction kettle needs to be rinsed with clear water before being used.
5. The preparation method of the boron nitride powder filler with high thermal conductivity according to claim 2, characterized by comprising the following steps: the power of the ultrasonic wave in the step three 1) is 500W.
6. The preparation method of the boron nitride powder filler with high thermal conductivity according to claim 2, characterized by comprising the following steps: and in the step four 1), the mixture is required to be filtered before being poured into the tube furnace.
7. The preparation method of the boron nitride powder filler with high thermal conductivity according to claim 2, characterized by comprising the following steps: and in the fifth step, disinfection treatment is required before boxing.
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| CN113930087A (en) * | 2021-10-18 | 2022-01-14 | 湖南碳导新材料科技有限公司 | Surface modified boron nitride powder for heat-conducting filler and preparation method thereof |
| CN116891713A (en) * | 2023-07-13 | 2023-10-17 | 东莞市欣美电子材料有限公司 | Multicomponent pouring sealant and manufacturing process thereof |
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| CN116891713A (en) * | 2023-07-13 | 2023-10-17 | 东莞市欣美电子材料有限公司 | Multicomponent pouring sealant and manufacturing process thereof |
| CN116891713B (en) * | 2023-07-13 | 2024-01-26 | 东莞市欣美电子材料有限公司 | Multicomponent pouring sealant and manufacturing process thereof |
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