CN114921098A - Heat-conducting room temperature vulcanized silicone rubber and preparation method and application thereof - Google Patents
Heat-conducting room temperature vulcanized silicone rubber and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a heat-conducting room temperature vulcanized silicone rubber and a preparation method and application thereof, wherein the heat-conducting room temperature vulcanized silicone rubber comprises the following raw materials in percentage by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane; 20-40 parts of dealcoholization type cross-linking agent; 1-3 parts of a silane coupling agent; 5-40 parts of composite heat-conducting filler A; 5-40 parts of composite heat-conducting filler B; 1-3 parts of a catalyst. The heat-conducting room temperature vulcanized silicone rubber has the advantages of excellent mechanical property, good insulating property, high heat conductivity coefficient and the like, can be cured and molded without high temperature and high pressure, has low preparation cost and simple and environment-friendly process, and can provide a new idea for the field of heat dissipation of microelectronic equipment.
Description
Technical Field
The invention belongs to the technical field of silicon rubber materials, and particularly relates to heat-conducting room temperature vulcanized silicon rubber as well as a preparation method and application thereof.
Background
With the light weight and integration of electronic equipment, the heat dissipation problem of electronic devices becomes a key factor affecting the service life. Silicone rubber materials are widely used as heat dissipation materials for electronic devices because of their excellent insulation properties, high and low temperature resistance, chemical resistance, and flexibility. The heat conductivity coefficient of the silicone rubber is low, and the application of heat dissipation of electronic devices cannot be met, so that the heat conductivity coefficient needs to be improved on the premise of keeping the insulating performance. The related technology discloses a preparation method of flaky hexagonal boron nitride modified silicone rubber, which obviously improves the thermal conductivity coefficient, but has the defect of high filler content, and not only damages the mechanical property but also improves the cost. In the related art, the graphene modified silicone rubber is used for preparing the composite silicone rubber with excellent heat conductivity, but the high conductivity of the graphene obviously reduces the insulating property of the silicone rubber.
Disclosure of Invention
The present invention has been made to solve at least one of the above-mentioned problems occurring in the prior art. Therefore, the invention provides a heat-conducting room temperature vulcanized silicone rubber which is a room temperature vulcanized silicone rubber material with good mechanical property, insulation and high heat conductivity coefficient.
The second aspect of the invention provides a preparation method of the heat-conducting room temperature vulcanized silicone rubber.
The third aspect of the invention provides application of the heat-conducting room temperature vulcanized silicone rubber.
According to the first aspect of the invention, the heat-conducting room temperature vulcanized silicone rubber is provided, and comprises the following raw materials in percentage by mass:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane; 20-40 parts of dealcoholization type cross-linking agent; 1-3 parts of a silane coupling agent; 5-40 parts of composite heat-conducting filler A; 5-40 parts of composite heat-conducting filler B; 1-3 parts of a catalyst;
the composite heat-conducting filler A is a ceramic filler with silver nano particles loaded on the surface; the composite heat-conducting filler B is a heat-conducting insulating filler with silica nanoparticles loaded on the surface.
According to the invention, the alpha, omega-dihydroxy polydimethylsiloxane and the dealcoholization type cross-linking agent are subjected to condensation reaction under the action of the catalyst to provide mechanical properties for the silicone rubber, the ceramic filler is high in heat conductivity coefficient and insulating, and silver nanoparticles are loaded on the surface of the ceramic filler, so that on one hand, the heat conductivity coefficient of the silicone rubber can be improved, and simultaneously, the good insulating property is kept, on the other hand, the specific surface area of the ceramic filler can be further increased by the silver nanoparticles, so that a heat conduction path is more easily formed among the fillers, and the heat conductivity coefficient is further enhanced. Furthermore, the heat-conducting insulating filler with the surface loaded with the silicon dioxide nano particles is added, so that the wettability and the heat-conducting insulating property between the silicon dioxide nano particles and the silicon rubber are better, the interface compatibility between the heat-conducting insulating filler and the silicon rubber is improved, and the heat-conducting insulating property of the matrix is obviously enhanced; the silica nano particles also increase the specific surface area of the fillers, so that the fillers are easily connected to form a heat conduction path, and the transmission of phonons is facilitated.
In some embodiments of the invention, the α, ω -dihydroxy polydimethylsiloxane has a viscosity of 2000mPa · s to 5000mPa · s.
In some preferred embodiments of the present invention, the dealcoholization type crosslinking agent includes at least one of methyltrimethoxysilane and ethyl orthosilicate.
In some more preferred embodiments of the present invention, the silane coupling agent comprises at least one selected from KH550, KH 560.
In some more preferred embodiments of the present invention, the catalyst comprises at least one selected from the group consisting of dibutyltin dilaurate, stannous isooctanoate.
In some more preferred embodiments of the present invention, in the composite heat conductive filler a, the mass ratio of the ceramic filler to the silver nanoparticles is 1: (0.2-0.5).
In some more preferred embodiments of the present invention, the ceramic filler comprises at least one selected from the group consisting of silicon carbide whiskers, hexagonal boron nitride, aluminum nitride.
In some more preferred embodiments of the present invention, in the composite heat conductive filler B, the mass ratio of the heat conductive insulating filler to the silica nanoparticles is 1: (0.5-1).
In some more preferred embodiments of the present invention, the thermally conductive and insulating filler includes at least one selected from graphene oxide and boron nitride.
According to a second aspect of the present invention, a method for preparing the heat-conducting room temperature vulcanized silicone rubber is provided, which comprises the following steps: uniformly mixing alpha, omega-dihydroxy polydimethylsiloxane, dealcoholization type cross-linking agent, silane coupling agent, composite heat-conducting filler A and composite heat-conducting filler B, adding catalyst, and curing to obtain the heat-conducting room-temperature vulcanized silicone rubber.
In some embodiments of the present invention, the preparation method of the composite heat conductive filler a comprises: dispersing a ceramic filler in N, N-dimethylformamide, adding a silver nitrate solution after ultrasonic treatment, stirring, standing, and filtering to obtain the composite heat-conducting filler A. In the composite heat-conducting filler A, N, N-dimethylformamide serves as both a solvent and a reducing agent, the special surface energy of the N, N-dimethylformamide can overcome weak van der Waals force among ceramic fillers in an ultrasonic-solvothermal process, so that the ceramic fillers are stripped and uniformly dispersed in the N, N-dimethylformamide, and silver nanoparticles are attached to the surfaces of the ceramic fillers through the weak reduction effect of the N, N-dimethylformamide to obtain the composite heat-conducting filler A.
In some more preferred embodiments of the present invention, the time of the sonication is between 24h and 48 h.
In some more preferred embodiments of the invention, the stirring is performed at 60 ℃ to 80 ℃ for 60min to 80 min.
In some more preferred embodiments of the present invention, the standing time is 24 to 48 hours.
In some more preferred embodiments of the present invention, the preparation method of the composite heat conductive filler a further comprises subjecting the product obtained by filtration to a purification treatment, wherein the purification treatment comprises the steps of washing and drying, wherein the washing is performed by using ethanol and acetone respectively; the drying is carried out at 60-80 ℃.
In some more preferred embodiments of the present invention, the method for preparing the composite thermally conductive filler B comprises: and dispersing the heat-conducting insulating filler in a solvent, adjusting the pH to 10-12 after ultrasonic treatment, performing ultrasonic treatment, adding a silicon source, and filtering to obtain the composite heat-conducting filler B.
In some more preferred embodiments of the present invention, the preparation method of the composite heat conductive filler B comprises: dispersing the heat-conducting insulating filler in a solvent, carrying out ultrasonic treatment for 120-240 min, adjusting the pH value to 10-12, carrying out ultrasonic treatment for 1-2 h, adding a silicon source, and filtering to obtain the composite heat-conducting filler B.
In some more preferred embodiments of the present invention, the silicon source comprises at least one of methyltrimethoxysilane, ethyl orthosilicate.
In some more preferred embodiments of the present invention, the preparation method of the composite heat conductive filler B further comprises a step of drying the filtered product under vacuum conditions at 60 ℃ to 80 ℃.
In some more preferred embodiments of the present invention, the curing is performed at 20 ℃ to 30 ℃ for 180min to 240 min.
In some more preferred embodiments of the present invention, the curing is performed in an environment having a humidity of 50% to 60%.
According to a third aspect of the invention, the application of the heat-conducting room temperature vulcanized silicone rubber in preparing heat-conducting silicone rubber sheets or microelectronic devices is provided.
The beneficial effects of the invention are as follows:
1. the heat-conducting room temperature vulcanized silicone rubber has the advantages of excellent mechanical property, good insulating property, high heat conductivity coefficient and the like, can be cured and molded without high temperature and high pressure, has low preparation cost and simple and environment-friendly process, and can provide a new idea for the field of heat dissipation of microelectronic equipment.
2. In the heat-conducting room temperature vulcanized silicone rubber, alpha, omega-dihydroxy polydimethylsiloxane and dealcoholization type cross-linking agent are subjected to condensation reaction under the action of a catalyst, so that mechanical properties are provided for the silicone rubber.
3. In the composite heat-conducting filler A in the heat-conducting room temperature vulcanized silicone rubber, N, N-dimethylformamide serves as a solvent and a reducing agent, the special surface energy of the N, N-dimethylformamide can overcome weak van der Waals force between ceramic fillers in an ultrasonic-solvent heating process, so that the ceramic fillers are peeled off and uniformly dispersed in the N, N-dimethylformamide, and the silver nanoparticles are attached to the surface of the ceramic fillers through the weak reduction effect of the N, N-dimethylformamide to obtain the composite heat-conducting filler A. The ceramic filler has high thermal conductivity and is insulating, so that the thermal conductivity of the silicon rubber can be improved, and the good insulating property is kept. The silver nano particles on the surface of the ceramic filler further increase the specific surface area of the filler, so that the fillers are easily connected to form a heat conduction path, and the heat conduction coefficient is further enhanced.
4. The composite heat-conducting filler B in the heat-conducting room-temperature vulcanized silicone rubber is a heat-conducting insulating filler with silica nanoparticles attached to the surface by a sol-gel method, the wettability and the heat-conducting insulating property of the silica nanoparticles and the silicone rubber are good, the interface compatibility of the heat-conducting insulating filler and the silicone rubber is improved, the heat-conducting insulating property of a matrix is further enhanced, and the specific surface area of the filler is further increased by the nano-silica particles, so that the fillers are easily connected to form a heat-conducting path, and the transmission of phonons is facilitated.
5. The content of the composite heat-conducting filler in the heat-conducting room temperature vulcanized silicone rubber is controlled in a lower range, so that the tensile property of the silicone rubber can be effectively improved without reducing the flexibility.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is an SEM image of a silicon carbide whisker of the invention.
Fig. 2 is an SEM image of graphene oxide according to the present invention.
Fig. 3 is an SEM image of composite thermally conductive filler a of the present invention.
Fig. 4 is an SEM image of composite heat conductive filler B of the present invention.
FIG. 5 is an SEM image of a thermally conductive silicone rubber of comparative example 1 of the present invention.
Fig. 6 is an SEM image of comparative example 2 heat conductive silicone rubber of the present invention.
FIG. 7 is an SEM image of a thermally conductive room temperature vulcanized silicone rubber of example 1 of the present invention.
FIG. 8 is an SEM image of a thermally conductive room temperature vulcanized silicone rubber of example 2 of the present invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
In the following examples or comparative examples, the preparation method of the composite heat conductive filler a is as follows:
s1: 1.0g of silicon carbide whiskers was dispersed in 300mL of N, N-dimethylformamide.
S2: the solution was sonicated in a sonic bath for 48h and centrifuged to collect the supernatant.
S3: 0.8g of solid silver nitrate was dissolved in 15mL of water to form an aqueous silver nitrate solution.
S4: dropping silver nitrate water solution into the supernatant, and stirring at 60 deg.C for 60 min.
S5: the mixture was then left at room temperature for 24 h.
S6: the mixture was filtered by vacuum and the product was collected, washed with ethanol and acetone, respectively.
S7: and finally, drying the product at 60 ℃ to obtain the composite heat-conducting filler A.
The preparation method of the composite heat-conducting filler B comprises the following steps:
s1: 1.0g of graphene oxide was dispersed in a mixture of 240mL of ethanol and 24mL of deionized water and sonicated for 120 min.
S2: to the solution was added 4mL of ammonium hydroxide to adjust the pH and sonicated for 1 h.
S3: 4mL of ethyl orthosilicate was added to the above solution, and the mixed solution was ultrasonically hydrolyzed for 180 min.
S4: the solution was kept at room temperature for 2 days.
S5: after standing for two days, the product was washed several times with ethanol and ionized water to remove free silica and collected by vacuum filtration.
S6: and drying the product at 60 ℃ to obtain the composite heat-conducting filler B.
Example 1
The embodiment prepares the heat-conducting room-temperature vulcanized silicone rubber, and the specific process comprises the following steps:
the method comprises the following steps of firstly, uniformly mixing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane (with the viscosity of 2000mPa & s), 20 parts of ethyl orthosilicate, 1 part of silane coupling agent KH550, 10 parts of composite heat-conducting filler A and 10 parts of composite heat-conducting filler B, removing bubbles, then adding 2 parts of catalyst dibutyltin dilaurate into the mixture, uniformly mixing, pouring the mixture into a mold after removing the bubbles, and curing for 240min at the temperature of 25 ℃ and the humidity of 50% to obtain the heat-conducting room-temperature silicon sulfide rubber.
Example 2
The embodiment prepares the heat-conducting room temperature vulcanized silicone rubber, and the specific process is as follows:
the heat-conducting room-temperature vulcanized silicone rubber is prepared by the following steps of uniformly mixing 100 parts by mass of alpha, omega-dihydroxy polydimethylsiloxane (with the viscosity of 2000 mPas), 30 parts by mass of ethyl orthosilicate, 1 part by mass of silane coupling agent KH550, 20 parts by mass of composite heat-conducting filler A and 20 parts by mass of composite heat-conducting filler B, removing bubbles, adding 2 parts by mass of catalyst dibutyltin dilaurate into the mixture, uniformly mixing, removing bubbles, pouring into a mold, and curing at 25 ℃ and the humidity of 50% for 240min to obtain the heat-conducting room-temperature vulcanized silicone rubber.
Comparative example 1
The comparative example prepares the heat-conducting silicon rubber, and the specific process comprises the following steps:
the preparation method comprises the following steps of firstly, uniformly mixing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane (with the viscosity of 2000mPa & s), 40 parts of ethyl orthosilicate, 1 part of silane coupling agent KH550 and 10 parts of composite heat-conducting filler A by mass, removing bubbles, then adding 2 parts of catalyst dibutyltin dilaurate into the mixture, uniformly mixing, pouring the mixture into a mold after removing the bubbles, and curing for 240min at the temperature of 25 ℃ and the humidity of 50% to obtain the heat-conducting silicone rubber.
Comparative example 2
The embodiment prepares the heat-conducting silicone rubber, and the specific process comprises the following steps:
the preparation method comprises the following steps of firstly, uniformly mixing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane (with the viscosity of 2000mPa & s), 40 parts of ethyl orthosilicate, 1 part of silane coupling agent KH550 and 10 parts of composite heat-conducting filler B by mass, removing bubbles, then adding 2 parts of catalyst dibutyltin dilaurate into the mixture, uniformly mixing, pouring the mixture into a mold after removing the bubbles, and curing for 240min at the temperature of 25 ℃ and the humidity of 50% to obtain the heat-conducting silicone rubber.
Test example 1
In this test example, SEM test was performed on the morphology of the material.
SEM images of the silicon carbide whisker, the graphene oxide, the composite heat-conducting filler A and the composite heat-conducting filler B are respectively shown in figures 1-4.
As can be seen from fig. 1 and 2: the surface of the unmodified silicon carbide whisker is smooth, the surface of the unmodified graphene oxide has no particles, and the unmodified graphene oxide has a small amount of broken sheet-shaped structures.
As can be seen from fig. 3 and 4: the surface of the silicon carbide whisker in the composite heat-conducting filler A becomes rough, namely silver nano particles are uniformly attached, and white particles are uniformly distributed on the surface of the laminated graphene oxide in the composite heat-conducting filler B, namely silicon dioxide nano particles are attached.
The SEM image of the heat conductive silicone rubber prepared in comparative example 1 is shown in fig. 5.
As can be seen from fig. 5: the composite heat-conducting filler A is uniformly dispersed in the silicon rubber, has no obvious separation phenomenon, and is beneficial to reducing the interface thermal resistance.
The SEM image of the thermally conductive silicone rubber obtained in comparative example 2 is shown in fig. 6.
As can be seen from fig. 6: the composite heat-conducting filler B is uniformly dispersed in the silicone rubber, and the silicone rubber has a lamellar structure due to the existence of the composite heat-conducting filler B, so that a heat-conducting network is constructed.
SEM images of the thermally conductive room temperature vulcanized silicone rubbers obtained in example 1 and example 2 are shown in fig. 7 and fig. 8, respectively.
As can be seen from fig. 7: the composite heat-conducting filler A and the composite heat-conducting filler B are uniformly dispersed in the silicone rubber, and the composite heat-conducting filler and the silicone rubber matrix have no obvious separation phenomenon and good compatibility.
As can be seen from fig. 8: the composite heat-conducting filler A and the composite heat-conducting filler B are uniformly dispersed in the silicone rubber, the filler content is obviously increased compared with that in the figure 7, and the lamellar filler and the whisker-shaped filler are mutually overlapped to form a heat-conducting channel.
Test example 2
The silicone rubbers obtained in examples and comparative examples were subjected to performance tests, and a general commercially available pure silicone rubber was used as a control.
Coefficient of thermal conductivity: the test is carried out according to GB/T10294-.
Volume resistivity: reference is made to the determination of the electrical conductivity and the dissipation performance resistivity of GB/T2439-2001 vulcanized rubber or thermoplastic rubber "
Shore A hardness: the test was carried out with reference to "GB/T531.1-2008 vulcanized rubber or thermoplastic rubber indentation hardness test method".
The test results are shown in table 1:
TABLE 1
As can be seen from Table 1: the heat conduction channel is formed between the composite heat conduction fillers, so that the heat conduction coefficient of the heat conduction room temperature vulcanized silicone rubber is obviously higher than that of pure silicone rubber, the heat conduction coefficient of the silicone rubber can be obviously improved by simultaneously adding the composite heat conduction filler A and the composite heat conduction filler B in the embodiments 1 and 2, the hardness is increased but the hardness is still at a lower level due to the addition of the fillers, the better flexibility of the silicone rubber is kept, and the volume resistivity is also obviously reduced due to the addition of the fillers, but the insulation performance is still met. Compared with the embodiment 1, the embodiment 2 has the advantages that the filler content is increased, so that a heat conduction path is easier to form, the phonon transfer efficiency is improved, and the heat conductivity coefficient is obviously improved.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the embodiments, and various changes can be made without departing from the gist of the present invention within the knowledge of those skilled in the art. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A heat-conducting room temperature vulcanized silicone rubber is characterized in that: the raw materials comprise the following components in percentage by mass:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane; 20-40 parts of dealcoholization type cross-linking agent; 1-3 parts of a silane coupling agent; 5-40 parts of composite heat-conducting filler A; 5-40 parts of composite heat-conducting filler B; 1-3 parts of a catalyst;
the composite heat-conducting filler A is a ceramic filler with silver nano particles loaded on the surface; the composite heat-conducting filler B is a heat-conducting insulating filler with silica nanoparticles loaded on the surface.
2. The thermally conductive room temperature vulcanizing silicone rubber of claim 1, wherein: in the composite heat-conducting filler A, the mass ratio of the ceramic filler to the silver nanoparticles is 1: (0.2-0.5).
3. The thermally conductive room temperature vulcanizing silicone rubber of claim 1, wherein: in the composite heat-conducting filler B, the mass ratio of the heat-conducting insulating filler to the silica nanoparticles is 1: (0.5 to 1).
4. The thermally conductive room temperature vulcanizing silicone rubber of claim 1, wherein: the viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is 2000 mPas-5000 mPas.
5. The thermally conductive room temperature vulcanizing silicone rubber of claim 1, wherein: the dealcoholization type cross-linking agent comprises at least one of methyltrimethoxysilane and ethyl orthosilicate.
6. The preparation method of the heat-conducting room temperature vulcanized silicone rubber as set forth in any one of claims 1 to 4, characterized in that: the method comprises the following steps: uniformly mixing alpha, omega-dihydroxy polydimethylsiloxane, dealcoholized cross-linking agent, silane coupling agent, composite heat-conducting filler A and composite heat-conducting filler B, adding a catalyst, and curing to obtain the heat-conducting room-temperature vulcanized silicone rubber.
7. The method of claim 5, wherein: the preparation method of the composite heat-conducting filler A comprises the following steps: dispersing a ceramic filler in N, N-dimethylformamide, adding a silver nitrate solution after ultrasonic treatment, stirring, standing, and filtering to obtain the composite heat-conducting filler A.
8. The production method according to claim 5, characterized in that: the preparation method of the composite heat-conducting filler B comprises the following steps: and dispersing the heat-conducting insulating filler in a solvent, adjusting the pH to 10-12 after ultrasonic treatment, performing ultrasonic treatment, adding a silicon source, and filtering to obtain the composite heat-conducting filler B.
9. The production method according to claim 5, characterized in that: the curing is carried out at 20-30 ℃ for 180-240 min.
10. An application of the heat-conducting room temperature vulcanized silicone rubber in the preparation of heat-conducting silicone rubber sheets or microelectronic devices.
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| CN109777113A (en) * | 2018-12-07 | 2019-05-21 | 华南理工大学 | A kind of insulating heat-conductive silicon rubber composite material and preparation method thereof |
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| CN113493676A (en) * | 2021-07-19 | 2021-10-12 | 深圳市新泰盈电子材料有限公司 | Condensed type two-component organic silicon pouring sealant and preparation method thereof |
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| US20080096030A1 (en) * | 2006-10-18 | 2008-04-24 | Shin -Etsu Chemical Co., Ltd. | Room temperature-curable, heat-conductive silicone rubber composition |
| CN106987123A (en) * | 2017-04-18 | 2017-07-28 | 上海大学 | Graphene/boron nitride loading nano silvery heat conduction speciality polymer material and preparation method |
| CN109777113A (en) * | 2018-12-07 | 2019-05-21 | 华南理工大学 | A kind of insulating heat-conductive silicon rubber composite material and preparation method thereof |
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