CN116144179A - Functionalized modified heat-conducting silicone rubber material, preparation method and application - Google Patents
Functionalized modified heat-conducting silicone rubber material, preparation method and application Download PDFInfo
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Abstract
The invention discloses a functionalized modified heat-conducting silicone rubber material, a preparation method and application thereof, wherein the heat-conducting silicone rubber material comprises the following components in parts by weight: 80-100 parts of silicon rubber, 2.3-2.8 parts of silane coupling agent, 5-8 parts of carbon nano tube, 25-30 parts of metal oxide, 115-20 parts of self-made carbon fiber, 8-16 parts of metal organic porous material and 15-25 parts of fumed silica.
Description
Technical Field
The invention belongs to the technical field of rubber heat-conducting materials, and particularly relates to a functionalized modified heat-conducting silicon rubber material, a preparation method and application thereof.
Background
With the development of miniaturization, integration and densification of electronic component products, the working temperature of each component is greatly increased under the drive of high performance and high efficiency. Heat is gathered and is difficult to effectively diffuse out, so that the stability, reliability and durability of electronic components are seriously reduced, and the service life of electronic products is greatly reduced. Therefore, it is becoming more and more critical to increase the heat dissipation power of electronic products. In conventional electronic products, a heat sink is mounted together with electronic components, and heat is conducted out through the heat sink. Heat accumulation of electronic components is related not only to the heat generating component and the heat sink, but also to contact thermal resistance generated by incomplete contact between the interfaces of the heat generating component and the heat sink. When the requirement on heat dissipation power is not high, main factors such as contact thermal resistance and diffusion thermal resistance among components are not considered. However, while electronic product performance and power are continually increasing, there is an increasing demand for the level of thermal management technology. The very small gap between the heat generating component and the heat sink is about 99% occupied by air, which is detrimental to heat transfer.
The heat conducting material has the advantages of high heat conducting coefficient, good flexibility, low thermal expansion coefficient, good surface wettability and viscosity, easy installation, easy treatment, shock absorption damping and other comprehensive performances, so that when the electronic product requires low installation pressure, the heat interface material can well fill between the radiator and the heating component, reduce interface contact thermal resistance, form a tightly combined heat conducting passage and timely diffuse out the accumulated heat. At present, the thermal interface material is mainly made of polymer materials, but the crystallinity of the polymer is generally low, and the vibration of a molecular chain can produce scattering effect on phonons, so that the heat conduction performance of the high-molecular polymer materials is generally poor, and the requirement of high heat dissipation is difficult to meet.
Disclosure of Invention
The invention aims to provide a functionalized modified heat-conducting silicone rubber material which comprises the following components in parts by weight: 80-100 parts of silicon rubber, 2.3-2.8 parts of silane coupling agent, 5-8 parts of carbon nano tube, 25-30 parts of metal oxide, 15-20 parts of self-made carbon fiber, 8-16 parts of metal organic porous material and 15-25 parts of fumed silica.
The self-made carbon fiber is prepared by the following method:
(1) Dispersing cellulose in aqueous solution of urea and sodium hydroxide, then placing the aqueous solution at the temperature of between 5 ℃ below zero and 2 ℃ below zero for 1.5 to 3 hours, and stirring the aqueous solution again at room temperature for 3 to 8 times, wherein the mass ratio of the cellulose to the urea to the sodium hydroxide to the water is (1 to 1.2): (0.4-0.65): (0.42-0.55): (15-35).
(2) And (3) adding citric acid into the step (1), stirring, and then, placing the mixture at the temperature of minus 10 ℃ to minus 6 ℃ for freeze thawing for 3 to 7 hours to obtain a gel substance.
(3) Transferring the gel substance into an electrostatic spinning injection pump, spinning under the conditions of injection rate of 0.3-0.45 cm/h, injection distance of 8-12 cm and injection voltage of 9-12 kv, placing cellulose obtained on a receiving roller into a tubular furnace, and calcining at 750-900 ℃ for 1-2.5 h under nitrogen atmosphere to obtain the self-made carbon fiber.
Further, the silicone rubber is selected from any one of methyl vinyl silicone rubber, methyl vinyl phenyl silicone rubber and fluorosilicone rubber.
Further, the metal oxide is selected from zinc oxide and aluminum oxide with a mass ratio of 1 (0.9-1.2).
Further, the metal organic porous material is selected from metal organic framework materials; the metal organic framework material is selected from rod-shaped MOF-74 (Zn).
Further, the rod-shaped MOF-74 (Zn) is prepared by the following method:
s1: 2,5 dihydroxyterephthalic acid and zinc nitrate are mixed according to the mass ratio of 0.3-0.5: 1.74 to 2.88 in a volume ratio of 12 to 15:3:3, the mixed solution is obtained in the mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and deionized water, and the mixed solution is transferred to a reaction kettle to be heated for 24 hours.
S2: after the reaction is finished, centrifuging for 5-8 min at the rotating speed of 6000-8000 r/min, washing and drying by using ethanol to obtain the rod-shaped MOF-74 (Zn).
Another object of the present invention is to provide a method for preparing a functionalized modified heat conductive silicone rubber material, the method comprising the steps of:
1): weighing all materials for standby according to the formula, adding the silicon rubber into a double-roller open mill for uniform mixing, and then sequentially adding a silane coupling agent, a carbon nano tube, a metal oxide, self-made carbon fiber, a metal organic porous material and fumed silica for uniform mixing to obtain the heat-conducting silicon rubber prepolymer.
2): adding the heat-conducting silicone rubber prepolymer obtained in the step 1) into a flat vulcanizing machine, hot-pressing for 10-20 min at 165-170 ℃ and 10-15 MPa, then moving to 180-190 ℃ and heating for 5-10 min, vulcanizing for 0.6-1.2 h at 200-210 ℃ and vulcanizing for 0.5-1 h at 220-225 ℃ and cooling to obtain the silicone rubber heat-conducting material.
Further, the mass ratio of the citric acid in the step (2) to the solution obtained in the step (1) is (0.82-1.35): (3-6).
The invention further aims at providing a functionalized modified heat-conducting silicon rubber material which is applied to the technical field of electronic and aviation heat-conducting materials.
The invention also has the following beneficial effects:
1. according to the invention, the self-made carbon fiber is used as an additive, cellulose is dissolved by the self-made carbon fiber firstly, then the growth direction of cellulose crystals is ensured by adopting a freeze thawing mode, and then the carbonized carbon fiber obtained by electrostatic spinning can conduct heat better when the silicon rubber material is heated, so that the material has better comprehensive performance.
2. According to the invention, the metal organic porous material rod-shaped MOF-74 (Zn) is adopted, and the rod-shaped MOF-74 (Zn) has higher porosity and larger pore channels, so that metal heat conduction ions in the heat conduction silicone rubber material can enter the pore channels and are uniformly distributed in the heat conduction material, and heat conduction can be better carried out when the material is heated.
3. In the invention, the rod-shaped MOF-74 (Zn) has exposed metal sites, and can perform functional modification on the rubber material in the vulcanization process, thereby improving the mechanical properties, hardness and the like of the silicon rubber material.
Detailed Description
The following detailed description of the embodiments of the present invention is provided on the premise of the technical solution of the present invention, and the detailed implementation manner and specific operation process are provided, and it should be noted that, for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered as the protection scope of the present invention.
Example 1
The functional modified heat-conducting silicone rubber material comprises the following components in parts by weight: 80 parts of silicon rubber, 2.3 parts of silane coupling agent, 5 parts of carbon nano tube, 25 parts of metal oxide, 15 parts of self-made carbon fiber, 8 parts of metal organic porous material and 15 parts of fumed silica.
The self-made carbon fiber is prepared by the following method:
(1) Dispersing cellulose in aqueous solution of urea and sodium hydroxide, then placing the mixture at the temperature of-5 ℃ for 1.5 hours, and stirring the mixture again at the room temperature environment for 3 times, wherein the mass ratio of the cellulose to the urea to the sodium hydroxide to the water is 1:0.4:0.42:15.
(2) And (3) adding citric acid into the step (1), stirring, and standing at-10 ℃ for freezing and thawing for 3 hours to obtain a gel-like substance.
(3) And (3) transferring the gel substance into an electrostatic spinning injection pump, spinning under the conditions of an injection rate of 0.3cm/h, an injection distance of 8cm and an injection voltage of 9kv, placing the cellulose obtained on a receiving roller into a tube furnace, and calcining at 750 ℃ for 1h under a nitrogen atmosphere to obtain the self-made carbon fiber.
Wherein the silicone rubber is selected from methyl vinyl silicone rubber; the metal oxide is selected from zinc oxide and aluminum oxide in a mass ratio of 1:0.9; the mass ratio of the citric acid in the step (2) to the solution obtained in the step (1) is 0.82:3, a step of; the metal organic porous material is selected from metal organic framework materials; the metal organic framework material is selected from rod-shaped MOF-74 (Zn).
The rod-shaped MOF-74 (Zn) is prepared by adopting the following method:
s1: 2,5 dihydroxyterephthalic acid and zinc nitrate are mixed according to the mass ratio of 0.3:1.74 dissolved in a volume ratio of 12:3:3, the mixed solution is obtained in the mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and deionized water, and the mixed solution is transferred to a reaction kettle to be heated for 24 hours.
S2: after the reaction, centrifuging for 5min at the rotating speed of 6000r/min, washing and drying by using ethanol to obtain the rod-shaped MOF-74 (Zn).
The preparation method of the functionalized modified heat-conducting silicone rubber material comprises the following steps:
1): weighing all materials for standby according to the formula, adding the silicon rubber into a double-roller open mill for uniform mixing, and then sequentially adding a silane coupling agent, a carbon nano tube, a metal oxide, self-made carbon fiber, a metal organic porous material and fumed silica for uniform mixing to obtain the heat-conducting silicon rubber prepolymer.
2): and (2) adding the heat-conducting silicone rubber prepolymer obtained in the step (S1) into a flat vulcanizing machine, hot-pressing for 10min at 165 ℃ and 10MPa, then moving to 180 ℃ and heating for 5min, vulcanizing for 0.6h at 200 ℃ and vulcanizing for 0.5h at 220 ℃, and cooling to obtain the silicone rubber heat-conducting material.
Example 2
The functional modified heat-conducting silicone rubber material comprises the following components in parts by weight: 100 parts of silicon rubber, 2.8 parts of silane coupling agent, 8 parts of carbon nano tube, 30 parts of metal oxide, 20 parts of self-made carbon fiber, 16 parts of metal organic porous material and 25 parts of fumed silica.
The self-made carbon fiber is prepared by the following method:
(1) Dispersing cellulose in aqueous solution of urea and sodium hydroxide, then placing the mixture at the temperature of-2 ℃ for 3 hours, and stirring the mixture again at room temperature for 8 times, wherein the mass ratio of the cellulose to the urea to the sodium hydroxide to the water is 1.2:0.65:0.55:35.
(2) And (3) adding citric acid into the step (1), stirring, and standing at-6 ℃ for freeze thawing for 7 hours to obtain a gel-like substance.
(3) And (3) transferring the gel substance into an electrostatic spinning injection pump, spinning under the conditions of an injection rate of 0.45cm/h, an injection distance of 12cm and an injection voltage of 12kv, placing the cellulose obtained on a receiving roller into a tube furnace, and calcining at 900 ℃ for 2.5h under a nitrogen atmosphere to obtain the self-made carbon fiber.
Wherein the silicone rubber is selected from methyl silicone rubber; the metal oxide is selected from zinc oxide and aluminum oxide with a mass ratio of 1:1.2; the mass ratio of the citric acid in the step (2) to the solution obtained in the step (1) is 1.35:6, preparing a base material; the metal organic porous material is selected from metal organic framework materials; the metal organic framework material is selected from rod-shaped MOF-74 (Zn).
The rod-shaped MOF-74 (Zn) is prepared by adopting the following method:
s1: 2,5 dihydroxyterephthalic acid and zinc nitrate are mixed according to the mass ratio of 0.5:2.88 in a volume ratio of 15:3:3, the mixed solution is obtained in the mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and deionized water, and the mixed solution is transferred to a reaction kettle to be heated for 24 hours.
S2: after the reaction, the mixture was centrifuged at 8000r/min for 8min, and washed with ethanol and dried to obtain rod-like MOF-74 (Zn).
The preparation method of the functionalized modified heat-conducting silicone rubber material comprises the following steps:
1): weighing all materials for standby according to the formula, adding the silicon rubber into a double-roller open mill for uniform mixing, and then sequentially adding a silane coupling agent, a carbon nano tube, a metal oxide, self-made carbon fiber, a metal organic porous material and fumed silica for uniform mixing to obtain the heat-conducting silicon rubber prepolymer.
2): and (2) adding the heat-conducting silicone rubber prepolymer obtained in the step (S1) into a flat vulcanizing machine, hot-pressing for 20min at 170 ℃ and 15MPa, then moving to 190 ℃ for heating for 10min, vulcanizing for 1.2h at 210 ℃ and vulcanizing for 1h at 225 ℃, and cooling to obtain the silicone rubber heat-conducting material.
Example 3
The functional modified heat-conducting silicone rubber material comprises the following components in parts by weight: 90 parts of silicon rubber, 2.5 parts of silane coupling agent, 6 parts of carbon nano tube, 27 parts of metal oxide, 16 parts of self-made carbon fiber, 10 parts of metal organic porous material and 20 parts of fumed silica.
The self-made carbon fiber is prepared by the following method:
(1) Dispersing cellulose in aqueous solution of urea and sodium hydroxide, then placing the mixture at the temperature of-4 ℃ for 2 hours, and stirring the mixture again at room temperature for 5 times, wherein the mass ratio of the cellulose to the urea to the sodium hydroxide to the water is 1.1:0.45:0.47:20.
(2) And (3) adding citric acid into the step (1), stirring, and standing at the temperature of-8 ℃ for freeze thawing for 5 hours to obtain a gel-like substance.
(3) Transferring the gel substance into an electrostatic spinning injection pump, spinning under the conditions of injection rate of 0.5cm/h, injection distance of 10cm and injection voltage of 10kv, placing cellulose obtained on a receiving roller into a tube furnace, and calcining at 800 ℃ for 1.5h under nitrogen atmosphere to obtain the self-made carbon fiber.
Wherein the silicone rubber is selected from methyl vinyl phenyl silicone rubber; the metal oxide is selected from zinc oxide and aluminum oxide in a mass ratio of 1:1; the mass ratio of the citric acid in the step (2) to the solution obtained in the step (1) is 0.96:4, a step of; the metal organic porous material is selected from metal organic framework materials; the metal organic framework material is selected from rod-shaped MOF-74 (Zn).
The rod-shaped MOF-74 (Zn) is prepared by adopting the following method:
s1: 2,5 dihydroxyterephthalic acid and zinc nitrate are mixed according to the mass ratio of 0.4:1.98 dissolved in a volume ratio of 13:3:3, the mixed solution is obtained in the mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and deionized water, and the mixed solution is transferred to a reaction kettle to be heated for 24 hours.
S2: after the reaction, the mixture was centrifuged at 7000r/min for 6min, and the mixture was washed with ethanol and dried to obtain rod-like MOF-74 (Zn).
The preparation method of the functionalized modified heat-conducting silicone rubber material comprises the following steps:
1): weighing all materials for standby according to the formula, adding the silicon rubber into a double-roller open mill for uniform mixing, and then sequentially adding a silane coupling agent, a carbon nano tube, a metal oxide, self-made carbon fiber, a metal organic porous material and fumed silica for uniform mixing to obtain the heat-conducting silicon rubber prepolymer.
2): and (2) adding the heat-conducting silicone rubber prepolymer obtained in the step (S1) into a flat vulcanizing machine, hot-pressing for 15min at 167 ℃ and 12MPa, then moving to 185 ℃ and heating for 7min, vulcanizing for 0.8h at 205 ℃ and vulcanizing for 0.7h at 222 ℃, and cooling to obtain the silicone rubber heat-conducting material.
Example 4
The functional modified heat-conducting silicone rubber material comprises the following components in parts by weight: 95 parts of silicon rubber, 2.7 parts of silane coupling agent, 7 parts of carbon nano tube, 28 parts of metal oxide, 18 parts of self-made carbon fiber, 15 parts of metal organic porous material and 24 parts of fumed silica.
The self-made carbon fiber is prepared by the following method:
(1) Dispersing cellulose in aqueous solution of urea and sodium hydroxide, then placing the mixture at the temperature of-3 ℃ for 2.5 hours, and stirring the mixture again at the room temperature environment for 7 times, wherein the mass ratio of the cellulose to the urea to the sodium hydroxide to the water is 1.15:0.6:0.53:30.
(2) And (3) adding citric acid into the step (1), stirring, and standing at the temperature of-7 ℃ for freeze thawing for 6 hours to obtain a gel-like substance.
(3) And (3) transferring the gel substance into an electrostatic spinning injection pump, spinning under the conditions of an injection rate of 0.4cm/h, an injection distance of 11cm and an injection voltage of 11kv, placing the cellulose obtained on a receiving roller into a tube furnace, and calcining at 850 ℃ for 2 hours in a nitrogen atmosphere to obtain the self-made carbon fiber.
Wherein the silicone rubber is selected from fluorosilicone rubber; the metal oxide is selected from zinc oxide and aluminum oxide with a mass ratio of 1:1.1; the mass ratio of the citric acid in the step (2) to the solution obtained in the step (1) is 1.31:5, a step of; the metal organic porous material is selected from metal organic framework materials; the metal organic framework material is selected from rod-shaped MOF-74 (Zn).
The rod-shaped MOF-74 (Zn) is prepared by adopting the following method:
s1: 2,5 dihydroxyterephthalic acid and zinc nitrate are mixed according to the mass ratio of 0.45:2.43 is dissolved in a volume ratio of 14:3:3, the mixed solution is obtained in the mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and deionized water, and the mixed solution is transferred to a reaction kettle to be heated for 24 hours.
S2: after the reaction, the mixture was centrifuged at 7500r/min for 7min, and then washed with ethanol and dried to obtain rod-like MOF-74 (Zn).
The preparation method of the functionalized modified heat-conducting silicone rubber material comprises the following steps:
1): weighing all materials for standby according to the formula, adding the silicon rubber into a double-roller open mill for uniform mixing, and then sequentially adding a silane coupling agent, a carbon nano tube, a metal oxide, self-made carbon fiber, a metal organic porous material and fumed silica for uniform mixing to obtain the heat-conducting silicon rubber prepolymer.
2): and (3) adding the heat-conducting silicone rubber prepolymer obtained in the step (S1) into a flat vulcanizing machine, hot-pressing for 18min at 168 ℃ and 13MPa, then moving to 188 ℃ and heating for 9min, vulcanizing for 1.1h at 207 ℃ and vulcanizing for 0.8h at 224 ℃, and cooling to obtain the silicone rubber heat-conducting material.
Performance test 1:
the tensile strength and elongation at break of the silicone rubber high thermal conductive materials prepared in examples 1 to 4 were tested according to ISO37-2017, the thermal conductivity was tested according to astm d5470 steady state hot plate method, and the test results are shown in table 1:
table 1. Results of performance test:
as can be seen from Table 1, the heat conductive silicone rubber materials prepared in examples 1 to 4 of the present invention have excellent mechanical properties and heat conductive properties.
Performance test 2:
the heat conducting materials of examples 1-4 were placed under the needle-in device of the hardness tester and tested with a shore oo hardness tester, the data were stabilized after the device had "beep" sound, the data were recorded (as an average of five different positions), the specific test results are shown in table 2,
table 2. Test results:
as can be seen from table 2, the thermally conductive silicone rubber material of the present invention has good hardness.
Claims (8)
1. The functional modified heat-conducting silicone rubber material is characterized by comprising the following components in parts by weight: 80-100 parts of silicon rubber, 2.3-2.8 parts of silane coupling agent, 5-8 parts of carbon nano tube, 25-30 parts of metal oxide, 115-20 parts of self-made carbon fiber, 8-16 parts of metal organic porous material and 15-25 parts of fumed silica;
the self-made carbon fiber is prepared by the following method:
(1) Dispersing cellulose in aqueous solution of urea and sodium hydroxide, then placing the aqueous solution at the temperature of between 5 ℃ below zero and 2 ℃ below zero for 1.5 to 3 hours, and stirring the aqueous solution again at room temperature for 3 to 8 times, wherein the mass ratio of the cellulose to the urea to the sodium hydroxide to the water is (1 to 1.2): (0.4-0.65): (0.42-0.55): (15-35);
(2) Adding citric acid into the step (1), stirring, and then, placing the mixture at the temperature of minus 10 ℃ to minus 6 ℃ for freeze thawing for 3 to 7 hours to obtain a gel substance;
(3) Transferring the gel substance into an electrostatic spinning injection pump, spinning under the conditions of injection rate of 0.3-0.45 cm/h, injection distance of 8-12 cm and injection voltage of 9-12 kv, placing cellulose obtained on a receiving roller into a tubular furnace, and calcining at 750-900 ℃ for 1-2.5 h under nitrogen atmosphere to obtain the self-made carbon fiber.
2. The functionally modified thermally conductive silicone rubber material of claim 1, wherein said silicone rubber is selected from any one of methyl vinyl silicone rubber, methyl vinyl phenyl silicone rubber and fluorosilicone rubber.
3. The functionally modified heat conductive silicone rubber material according to claim 1, wherein the metal oxide is selected from zinc oxide and aluminum oxide with a mass ratio of 1 (0.9-1.2).
4. The functionally modified heat conductive silicone rubber material according to claim 1, wherein the mass ratio of the citric acid in the step (2) to the solution obtained in the step (1) is (0.82-1.35): (3-6).
5. A functionalized modified thermally conductive silicone rubber material according to claim 1, wherein the metal organic porous material is selected from the group consisting of metal organic framework materials; the metal organic framework material is selected from rod-shaped MOF-74 (Zn).
6. The functionally modified thermally conductive silicone rubber material of claim 5, wherein the rod-like MOF-74 (Zn) is prepared by the following method:
s1: 2,5 dihydroxyterephthalic acid and zinc nitrate are mixed according to the mass ratio of 0.3-0.5: 1.74 to 2.88 in a volume ratio of 12 to 15:3:3, transferring the mixed solution into a reaction kettle to be heated for 24 hours;
s2: after the reaction is finished, centrifuging for 5-8 min at the rotating speed of 6000-8000 r/min, washing and drying by using ethanol to obtain the rod-shaped MOF-74 (Zn).
7. The method for preparing a functionalized modified heat conductive silicone rubber material according to any one of claims 1 to 6, wherein the preparation method comprises the following steps:
1): weighing materials for standby according to the formula, adding the silicon rubber to a double-roller open mill for uniform mixing, and then sequentially adding a silane coupling agent, a carbon nano tube, a metal oxide, self-made carbon fiber, a metal organic porous material and fumed silica for uniform mixing to obtain a heat-conducting silicon rubber prepolymer;
2): adding the heat-conducting silicone rubber prepolymer obtained in the step 1) into a flat vulcanizing machine, hot-pressing for 10-20 min at 165-170 ℃ and 10-15 MPa, then moving to 180-190 ℃ and heating for 5-10 min, vulcanizing for 0.6-1.2 h at 200-210 ℃ and vulcanizing for 0.5-1 h at 220-225 ℃ and cooling to obtain the silicone rubber heat-conducting material.
8. A functionalized modified heat conducting silicone rubber material according to any one of claims 1-6, which is applied to the technical field of electronic and aviation heat conducting materials.
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| CN111057379A (en) * | 2019-12-26 | 2020-04-24 | 华南理工大学 | High-thermal-conductivity insulating silicone rubber composite material containing carbon fibers and preparation method thereof |
| CN113097466A (en) * | 2021-04-02 | 2021-07-09 | 宁波润锦环保科技有限公司 | Lithium ion battery negative electrode material MoS2Preparation method of @ CFs |
| CN113101904A (en) * | 2021-04-28 | 2021-07-13 | 长春工业大学 | Preparation method of polymer composite metal organic framework material |
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