CN112724677A - Dopamine modified boron nitride heat-conducting silicone grease and preparation method thereof - Google Patents
Dopamine modified boron nitride heat-conducting silicone grease and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
Abstract
The invention relates to the technical field of heat-conducting silicone grease, and discloses dopamine modified boron nitride heat-conducting silicone grease and a preparation method thereof, wherein the dopamine modified boron nitride heat-conducting silicone grease comprises the following steps: step 1: modifying the surface of Boron Nitride (BN) by utilizing dopamine at room temperature to prepare the dopamine modified boron nitride (BN-PDA) filler. Step 2: and mixing the dopamine modified boron nitride (BN-PDA) and other fillers with silicone oil to prepare the heat-conducting silicone grease. The invention adopts dopamine to modify the surface of the boron nitride, has simple preparation method and environmental protection, and improves the heat-conducting property and the oil seepage condition of the heat-conducting silicone grease prepared by modifying the boron nitride with the dopamine.
Description
Technical Field
The invention relates to the technical field of heat-conducting silicone grease, in particular to dopamine modified nitrided heat-conducting silicone grease and a preparation method thereof.
Background
As electronic components have advanced toward high integration and miniaturization, the shrinking of feature sizes in electronic devices inevitably leads to an increase in power density. The high-density integrated chip has wide application prospect in high and new technical fields of intelligent electronic equipment, household appliances, automobile industry, aerospace and the like. When two solid materials are connected with each other, a plurality of gaps exist on the microstructure of the contact surface, the ideal state of complete tight combination cannot be achieved, in the micropores of the gaps, the micropores can be filled with poor transmission medium air, and the existence of an air layer is not beneficial to heat dissipation, so that the stability and the service life of an electronic component are influenced. Thermal interface materials with good thermal conductivity are developed to fill air gaps between solid contact surfaces, so that the purpose of reducing thermal resistance is achieved, and long-term reliable operation of electronic components is met, and the thermal interface materials become an important development direction of heat conduction materials.
The heat conducting grease does not need to be cured, has certain fluidity, can effectively fill a gap between contact surfaces of solids, increases the contact area of the two solids, and is very thin when a certain external force is applied, thereby being beneficial to reducing the interface thermal resistance and improving the heat transfer performance. Compared with other types of thermal interface materials, the thermal grease is low in price and is therefore popular.
Boron nitride, called "white graphite", has high thermal conductivity and has been widely used in the field of electronic packaging and insulating materials in recent years. But due to the low solubility, few functional groups and chemical inertness of boron nitride, the boron nitride is difficult to be well combined with most polymer-based materials, so that the boron nitride has poor compatibility, and the thermal conductivity and long-term stability of the composite material are limited.
Therefore, the development of an environmentally friendly route for treating and functionalizing boron nitride and improving the compatibility of boron nitride with polymer-based materials to improve the thermal conductivity and oil bleeding of thermally conductive silicone grease is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides dopamine modified boron nitride heat-conducting silicone grease and a preparation method thereof. The invention adopts dopamine to modify the surface of the boron nitride, the preparation method is simple and environment-friendly, and the heat-conducting performance and the oil seepage condition of the heat-conducting silicone grease prepared by modifying the boron nitride are obviously improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the dopamine modified boron nitride heat-conducting silicone grease is prepared by the following steps:
(1) preparing dopamine modified BN, BN-PDA: preparing dopamine hydrochloride aqueous solution, adding trihydroxymethyl aminomethane powder, adjusting the pH value of the solution to be alkaline, then adding boron nitride powder, performing ultrasonic treatment and stirring, performing suction filtration and deionized water washing for a plurality of times, and finally performing freeze drying to obtain BN-PDA powder;
(2) preparing BN-PDA heat-conducting silicone grease: weighing BN-PDA powder to be mixed with silicone oil, placing the mixture into a ball milling tank, taking out a sample after ball milling, and performing vacuum defoaming to obtain the BN-PDA heat-conducting silicone grease.
Preferably, the dopamine hydrochloride aqueous solution in the step (1) has the weight concentration of 0.5-10% and the pH value of 8-10.
Preferably, the particle size of the boron nitride powder in step (1) is 0.1 to 100 μm.
Preferably, the ultrasonic treatment time in the step (1) is 30-120min, the stirring temperature is 15-35 ℃, the stirring time is 24-48h, and the freeze-drying time is 24-48 h.
Preferably, in the step (2), the BN-PDA powder is mixed with silicone oil, and a heat-conducting filler is further added, wherein the heat-conducting filler comprises one or a mixture of more than two of aluminum oxide, aluminum nitride, zinc oxide, aluminum powder, copper powder, silver powder, graphene, carbon nano tubes, diamond, silicon carbide and silicon nitride.
Preferably, the silicone oil in step (2) is at least one of dimethyl silicone oil, epoxy silicone oil, vinyl silicone oil, benzyl silicone oil, hydroxyl silicone oil, methyl long-chain alkyl silicone oil, carboxyl silicone oil and amino silicone oil.
Preferably, the weight of the BN-PDA powder and the heat-conducting filler in the step (2) is 30-90% of the total weight of the heat-conducting grease.
Preferably, the ball milling time in the step (2) is 0.5-3h, and the rotating speed is 200-600 rpm.
Preferably, the vacuum centrifugal defoaming time in the step (2) is 5-10min, and the rotating speed is 400-1000 rpm.
Compared with the prior art, the invention has the beneficial effects that:
the invention aims at the defects that boron nitride has few functional groups and chemical inertness and is difficult to be well combined with most polymer-based materials, thereby limiting the thermal conductivity and long-term stability of the composite material. The dopamine is adopted to carry out surface modification on boron nitride, and then the dopamine is compounded with the silicone oil to prepare the heat-conducting silicone grease, so that the interface compatibility of the boron nitride filler and a silicone oil matrix can be improved, the dispersibility of the boron nitride filler in the silicone oil matrix is improved, and the interface thermal resistance is reduced, thereby improving the heat-conducting property of the heat-conducting silicone grease and improving the oil seepage condition of the heat-conducting silicone grease. Compared with the unmodified BN heat conduction grease, the BN-PDA heat conduction grease has the advantages that the heat conductivity can be improved by 4-13%, and the oil seepage condition is obviously improved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a graph showing a comparison of thermal conductivities of BN-PDA and BN heat conductive silicone grease provided in examples 1-3 and comparative examples 1-3 of the present application.
Fig. 2 is a photograph showing the oil bleeding of the thermally conductive silicone grease provided in example 1 of the present application and comparative example 1 after storage for 3 months at room temperature.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention.
Example 1
(1) Preparing dopamine modified BN, BN-PDA: adding 0.6g of dopamine hydrochloride into 300ml of deionized water solution, adding 0.36g of tris (hydroxymethyl) aminomethane powder, adjusting the pH =8.5, adding 15g of boron nitride powder (5 mu m), mechanically stirring and ultrasonically treating for 1h, magnetically stirring for 24h at normal temperature, performing suction filtration, washing with deionized water for 3 times, and finally freeze-drying for 12h to obtain BN-PDA powder.
(2) Preparing BN-PDA heat-conducting silicone grease: weighing 8g of BN-PDA powder and 12g of hydroxyl silicone oil, mixing, placing in a ball milling tank, carrying out ball milling at 400rpm for 1h, taking out a sample, and then carrying out vacuum defoamation at 500rpm for 5min to obtain the BN-PDA heat-conducting silicone grease.
In the BN-PDA heat-conducting silicone grease prepared in the embodiment, the mass of the BN-PDA is 40% of the total mass of the heat-conducting silicone grease.
Example 2
(1) Preparing dopamine modified BN, BN-PDA: adding 0.6g of dopamine hydrochloride into 300ml of deionized water solution, adding 0.36g of tris (hydroxymethyl) aminomethane powder, adjusting the pH =8.5, adding 15g of boron nitride powder (5 mu m), mechanically stirring and ultrasonically treating for 1h, magnetically stirring for 24h at normal temperature, performing suction filtration, washing with deionized water for 3 times, and finally freeze-drying for 12h to obtain BN-PDA powder.
(2) Preparing BN-PDA heat-conducting silicone grease: weighing 9g of BN-PDA powder and 11g of hydroxyl silicone oil, mixing, placing in a ball milling tank, carrying out ball milling at 400rpm for 1h, taking out a sample, and then carrying out vacuum defoamation at 500rpm for 5min to obtain the BN-PDA heat-conducting silicone grease.
In the BN-PDA heat-conducting silicone grease prepared in the embodiment, the mass of the BN-PDA is 45% of the total mass of the heat-conducting silicone grease.
Example 3
(1) Preparing dopamine modified BN, BN-PDA: adding 0.6g of dopamine hydrochloride into 300ml of deionized water solution, adding 0.36g of tris (hydroxymethyl) aminomethane powder, adjusting the pH =8.5, adding 15g of boron nitride powder (5 mu m), mechanically stirring and ultrasonically treating for 1h, magnetically stirring for 24h at normal temperature, performing suction filtration, washing with deionized water for 3 times, and finally freeze-drying for 12h to obtain BN-PDA powder.
(2) Preparing BN-PDA heat-conducting silicone grease: weighing 10g of BN-PDA powder and 10g of hydroxyl silicone oil, mixing, placing in a ball milling tank, ball milling at 400rpm for 1h, taking out a sample, and then carrying out vacuum defoamation at 500rpm for 5min to obtain the BN-PDA heat-conducting silicone grease.
In the BN-PDA heat-conducting silicone grease prepared in the embodiment, the mass of the BN-PDA is 50% of the total mass of the heat-conducting silicone grease.
Example 4
(1) Preparing dopamine modified BN, BN-PDA: adding 0.6g of dopamine hydrochloride into 300ml of deionized water solution, adding 0.363g of tris (hydroxymethyl) aminomethane powder, adjusting the pH =8.5, adding 15g of boron nitride powder (5 mu m), mechanically stirring and ultrasonically treating for 1h, magnetically stirring for 24h at normal temperature, performing suction filtration, washing with deionized water for 3 times, and finally freeze-drying for 12h to obtain BN-PDA powder.
(2) Preparation of BN-PDA/Al heat-conducting silicone grease: weighing 5.6g of BN-PDA powder, 8.4g of 15umAl powder and 6g of hydroxyl silicone oil, mixing, placing in a ball milling tank, ball milling at 400rpm for 1h, taking out a sample, and then carrying out vacuum defoaming at 500rpm for 5min to obtain the BN-PDA/Al heat-conducting silicone grease.
The mass of BN-PDA and Al in the BN-PDA/Al heat-conducting silicone grease prepared in the embodiment is 70 percent of the total mass of the heat-conducting silicone grease.
Comparative example 1
(1) Preparation of BN heat-conducting silicone grease: weighing 8g of BN powder and 12g of hydroxyl silicone oil, mixing, placing in a ball milling tank, carrying out ball milling at 400rpm for 1h, taking out a sample, and carrying out vacuum defoaming at 500rpm for 5min to obtain the BN heat-conducting silicone grease.
In the BN heat-conductive silicone grease prepared in this example, the mass of BN was 40% of the total mass of the heat-conductive silicone grease.
Comparative example 2
(1) Preparation of BN heat-conducting silicone grease: weighing 9g of BN powder and 11g of hydroxyl silicone oil, mixing, placing in a ball milling tank, carrying out ball milling at 400rpm for 1h, taking out a sample, and carrying out vacuum defoaming at 500rpm for 5min to obtain the BN heat-conducting silicone grease.
In the BN heat-conductive silicone grease prepared in this example, the mass of BN was 45% of the total mass of the heat-conductive silicone grease.
Comparative example 3
(1) Preparation of BN heat-conducting silicone grease: weighing 10g of BN powder and 10g of hydroxyl silicone oil, mixing, placing in a ball milling tank, carrying out ball milling at 400rpm for 1h, taking out a sample, and then carrying out vacuum defoaming at 500rpm for 5min to obtain the BN heat-conducting silicone grease.
In the BN heat-conductive silicone grease prepared in this example, the mass of BN was 50% of the total mass of the heat-conductive silicone grease.
Comparative example 4
(1) Preparation of BN/Al heat-conducting silicone grease: weighing 5.6g of BN powder, 8.4g of 15 mu mAl powder and 6g of hydroxyl silicone oil, mixing, placing in a ball milling tank, ball milling at 400rpm for 1h, taking out a sample, and then carrying out vacuum defoaming at 500rpm for 5min to obtain the BN/Al heat-conducting silicone grease.
In the BN/Al heat-conducting silicone grease prepared in the embodiment, the mass of BN and Al is 70% of the total mass of the heat-conducting silicone grease.
TABLE 1 product Performance data for examples 1-4 and comparative examples 1-4
| Test items | Example 1 | Example 2 | Example 3 | Example 4 |
| Coefficient of thermal conductivity (w/m/k) | 1.024 | 1.220 | 1.445 | 2.295 |
| Test items | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Coefficient of thermal conductivity (w/m/k) | 1.158 | 1.368 | 1.513 | 2.476 |
As can be seen from the comparative example, as shown in fig. 1 and table 1, the heat conductive silicone oil prepared from BN modified by dopamine has higher heat conductivity than the BN heat conductive silicone oil. Meanwhile, the heat-conducting silicone grease prepared by compounding the BN-PDA and the Al has higher heat conductivity than the BN/Al heat-conducting silicone grease. The BN surface modification has better compatibility with the silicone oil, promotes the better combination of the BN and the silicone oil substrate, has lower interface thermal resistance and is beneficial to improving the heat-conducting property.
As shown in fig. 2, when BN-PDA heat conductive silicone grease and BN heat conductive silicone grease filled by 40% by mass were left on the printing paper after 3 months, it was clearly seen that oil exuded from the heat conductive silicone grease was adsorbed on the printing paper, and compared to the BN heat conductive silicone grease, the BN-PDA heat conductive silicone grease was significantly improved in oil exudation. Similarly, after the surface of BN is modified, the BN has better compatibility with silicone oil, promotes better combination of the BN and a silicone oil substrate, is favorable for improving the oil seepage condition of the BN heat-conducting silicone grease, and has long-term stability.
Claims (9)
1. The dopamine modified boron nitride heat-conducting silicone grease is characterized by being prepared by the following steps:
(1) preparing dopamine modified BN, BN-PDA: preparing dopamine hydrochloride aqueous solution, adding trihydroxymethyl aminomethane powder, adjusting the pH value of the solution to be alkaline, then adding boron nitride powder, performing ultrasonic treatment and magnetic stirring, performing suction filtration and deionized water washing for several times, and finally performing freeze drying to obtain BN-PDA powder;
(2) preparing BN-PDA heat-conducting silicone grease: weighing BN-PDA powder and silicone oil, mixing, placing in a ball milling tank, taking out a sample after ball milling, and carrying out vacuum centrifugal defoaming to obtain the BN-PDA heat-conducting silicone grease.
2. The dopamine-modified boron nitride heat-conducting silicone grease as claimed in claim 1, wherein the dopamine hydrochloride aqueous solution in step (1) has a weight concentration of 0.5-10% and a pH of 8-10.
3. The dopamine-modified boron nitride heat-conducting silicone grease as claimed in claim 1, wherein the particle size of the boron nitride powder in step (1) is 0.1-100 μm.
4. The dopamine-modified boron nitride heat-conducting silicone grease as claimed in claim 1, wherein the ultrasonic treatment time in step (1) is 30-120min, the stirring temperature is 15-35 ℃, the stirring time is 24-48h, and the freeze-drying time is 24-48 h.
5. The dopamine-modified boron nitride heat-conducting silicone grease as claimed in claim 1, wherein in step (2), the BN-PDA powder and the silicone oil are mixed, and a heat-conducting filler is further added, wherein the heat-conducting filler is one or a mixture of more than two of aluminum oxide, aluminum nitride, zinc oxide, aluminum powder, copper powder, silver powder, graphene, carbon nanotubes, diamond, silicon carbide and silicon nitride.
6. The dopamine-modified boron nitride heat-conducting silicone grease according to claim 1, wherein the silicone oil in step (2) is at least one of dimethyl silicone oil, epoxy silicone oil, vinyl silicone oil, benzyl silicone oil, hydroxy silicone oil, methyl long-chain alkyl silicone oil, carboxyl silicone oil and amino silicone oil.
7. The dopamine-modified boron nitride heat-conducting silicone grease as claimed in claim 1, wherein the weight of the BN-PDA powder and the heat-conducting filler in the step (2) accounts for 30-90% of the total weight of the heat-conducting silicone grease.
8. The dopamine-modified boron nitride heat-conducting silicone grease as claimed in claim 1, wherein the ball milling time in step (2) is 0.5-3h, and the rotation speed is 200-600 rpm.
9. The dopamine-modified boron nitride heat-conducting silicone grease as claimed in claim 1, wherein the vacuum centrifugal defoaming time in step (2) is 5-10min, and the rotation speed is 400-1000 rpm.
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| CN113200527A (en) * | 2021-06-18 | 2021-08-03 | 苏州鸿凌达电子科技有限公司 | Modification treatment method of hexagonal boron nitride |
| CN113636529A (en) * | 2021-07-15 | 2021-11-12 | 西安理工大学 | Preparation method of boron nitride and aluminum oxide heat-conducting filler |
| CN113698736A (en) * | 2021-10-09 | 2021-11-26 | 深圳市鑫奕龙达电子有限公司 | Halogen-free flame-retardant heat-conducting wire insulating layer and preparation method thereof |
| CN114672285A (en) * | 2022-03-11 | 2022-06-28 | 北京建筑大学 | Copper oxide nanofluid and preparation method and application thereof |
| CN114989608A (en) * | 2022-07-01 | 2022-09-02 | 宁夏清研高分子新材料有限公司 | Heat-conducting polysulfone composite material and preparation method thereof |
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| CN114989608B (en) * | 2022-07-01 | 2024-01-30 | 宁夏清研高分子新材料有限公司 | Heat-conducting polysulfone composite material and preparation method thereof |
| CN116552072A (en) * | 2023-04-18 | 2023-08-08 | 江苏谷田新材料科技有限公司 | Aluminum-plastic composite film and processing technology thereof |
| CN116552072B (en) * | 2023-04-18 | 2023-12-15 | 江苏谷田新材料科技有限公司 | Aluminum-plastic composite film and processing technology thereof |
| CN116390469A (en) * | 2023-05-29 | 2023-07-04 | 南京邮电大学 | Heat conduction wave-absorbing material for C band of 5G network, preparation and application thereof |
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Application publication date: 20210430 |