CN111944498A - Heat-conducting gel with ultralow oil extraction amount and high flow rate performance and preparation method thereof - Google Patents
Heat-conducting gel with ultralow oil extraction amount and high flow rate performance and preparation method thereof Download PDFInfo
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- CN111944498A CN111944498A CN202010846190.4A CN202010846190A CN111944498A CN 111944498 A CN111944498 A CN 111944498A CN 202010846190 A CN202010846190 A CN 202010846190A CN 111944498 A CN111944498 A CN 111944498A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a heat-conducting gel with ultralow oil extraction amount and high flow rate performance and a preparation method thereof, wherein the heat-conducting gel comprises the following components in parts by weight: 60-98 parts of powder; 1-50 parts of silicone oil; 0.05-5 parts of a curing agent; 0.1-5 parts of a treating agent; 0.01-1 part of catalyst; 0.01-1 part of color paste; the powder consists of three spherical aluminas with different grain diameters, and the weight percentages of the three spherical aluminas are as follows: spherical alumina with a particle size of 30-50 μm: 40% -90%; spherical alumina with a particle size of 10-30 μm: 5% -30%; spherical alumina with a particle size of 0.1-10 μm: 5 to 30 percent. The oil separating amount of the heat-conducting gel is less than or equal to 12mm (55 ℃/168h), the flow rate is more than or equal to 6.5g/min (1.55mm @90psi), and the performances of ultralow oil separating amount and high flow rate are realized.
Description
Technical Field
The invention relates to the technical field of heat-conducting interface materials for the intelligent communication industry, in particular to a heat-conducting gel with ultralow oil yield and high flow rate performance and a preparation method thereof.
Background
With the rapid development of the smart phone industry and the coming of the 5G smart phone era, the power consumption of chipsets such as mobile phone CPUs (central processing units) and GPUs (graphic processing units) is higher and higher, and the generated heat is higher and higher. If the heat generated by the chipset cannot be dissipated in time, the hot spot temperature is too high, and the function and the service life of the mobile phone mainboard chip are reduced. Therefore, heat dissipation of the smart phone chip set becomes one of the important hot spots of particular concern for mobile phone manufacturers.
For the heat dissipation problem of CPU and GPU chips and other heat sources, the most common method is to dissipate heat by using artificial graphite sheets, copper foils or heat pipes. However, a certain gap inevitably exists between a heat source such as a CPU & GPU and a metal shield, and the existence of the gap increases contact thermal resistance, which seriously affects rapid heat transfer of a chip, causes a local over-high temperature of the chip, and causes trouble to heat dissipation of the chip.
The heat-conducting interface material is widely applied because the interface thermal resistance between the heat source and the radiating fin can be effectively reduced. The heat conducting gel is one of the most commonly used heat conducting media, and is a material used for filling a gap between a heat source and a heat radiating fin, so that heat emitted by the heat source is quickly conducted to the heat radiating fin, the temperature of a chip heat source is kept at a level capable of stably working, the service life of components such as chips is prolonged, and the heat sources such as the chips are prevented from being damaged due to poor heat radiation.
The heat conducting gel is prepared by mixing and dispersing silicone oil and a filler through a special process. However, the thermal conductivity of the thermal conductive gel for smart phones on the market is generally 3-3.5 w/m.K. Due to the limitation of the formula process, the oil separation rate of the heat-conducting gel is generally large. If the oil evolution rate of the thermal conductive gel is reduced, the flow rate is also reduced. In general, oil separation and flow rate are a pair of contradictions. The heat conducting gel on the market generally has the oil separating amount of 14-24mm (55 ℃/168h) and the flow rate of 2-6g/min (1.55mm @90 psi).
Chinese patent document CN111171575A discloses a heat-conducting gel with high heat conductivity and low oil yielding and a preparation process thereof. The paint comprises the following components in percentage by mass: 65-95 parts of powder; 5-30 parts of silicone oil; 0.01-10 parts of raw rubber; 0.1 to 5 portions of curing agent; 0.1-3 parts of a coupling agent; 0.5-1 part of catalyst; the powder comprises the components of a mixture of aluminum oxide and zinc oxide powder; the powder comprises the following components in percentage by mass: alumina: 60% -95%; zinc oxide: 5 to 40 percent. Wherein, in the powder, the grain diameter of the aluminum oxide is 10-80 microns, and the grain diameter of the zinc oxide is 1-10 microns. The heat conductivity coefficient of the heat conducting gel with high heat conductivity and low oil yielding performance can reach 3.5 w/m.K, the oil yield (oil yielding capacity) is less than 20mm (55 ℃/168h), and the minimum compression thickness can reach 0.08 mm.
Disclosure of Invention
In view of the above, the invention aims to provide a heat conducting gel with ultralow oil yield and high flow rate performance and a preparation method thereof, wherein the oil yield of the prepared heat conducting gel is less than or equal to 12mm (55 ℃/168h), and the flow rate is greater than or equal to 6.5g/min (1.55mm @90 psi).
The adopted technical scheme is as follows:
a heat conducting gel with ultralow oil extraction amount and high flow rate performance comprises the following components in parts by weight:
60-98 parts of powder;
1-50 parts of silicone oil;
0.05-5 parts of a curing agent;
0.1-5 parts of a treating agent;
0.01-1 part of catalyst;
0.01-1 part of color paste;
the powder consists of three spherical aluminas with different grain diameters, and the weight percentages of the three spherical aluminas are as follows:
spherical alumina with a particle size of 30-50 μm: 40% -90%;
spherical alumina with a particle size of 10-30 μm: 5% -30%;
spherical alumina with a particle size of 0.1-10 μm: 5 to 30 percent.
Further, the silicone oil is one or more of vinyl silicone oil, phenyl silicone oil, hydroxyl silicone oil, dimethyl silicone oil, amino silicone oil, methyl long-chain alkyl silicone oil and quaternary ammonium salt alkyl modified silicone oil.
Further, the curing agent is a mixture of terminal hydrogen-containing silicone oil and side cyanogen-containing silicone oil.
Further, the treating agent is a silane coupling agent, and the silane coupling agent is one or a mixture of more of aminopropyltrimethoxysilane, vinyl triethoxysilane, 3-aminopropyltriethoxysilane and vinyl trimethoxysilane. The silane coupling agent has the function of increasing the compatibility and the dispersibility of the powder and the silicone oil.
Further, the catalyst is chloroplatinic acid, and the platinum content is 100ppm-6000 ppm.
Further, the color paste is green color paste.
Further, the viscosity of the silicone oil is 100-3000 cps.
Further, one or more of an optional flame retardant and a thixotropic agent are also included.
The preparation method of the heat conducting gel with ultra-low oil extraction amount and high flow rate performance, which is disclosed by any one of the above schemes, comprises the following steps:
s1, pouring liquid silicone oil into a planetary power stirrer, and heating the planetary power stirrer to 130 ℃;
s2, adding spherical alumina powder with the grain diameter of 30-50 mu m, and stirring for 15 minutes;
s3, adding spherical alumina powder with the grain diameter of 10-30 mu m, and stirring for 15 minutes;
s4, adding spherical alumina powder with the grain diameter of 0.1-10 mu m, adding a treating agent, and integrally stirring for 30 minutes;
s5, adding a curing agent and a catalyst, and stirring for 15 minutes;
s6, adding color paste, and integrally stirring for 20 minutes;
s7, integrally vacuumizing the mixture obtained in the step S6 for 20 minutes, and cooling to normal temperature for later use;
and S8, packaging the final mixture obtained in the step S7 in a needle tube with a standard specification through glue filling equipment to obtain a heat-conducting gel product.
Further, in S6, adding color paste and other additives, and stirring for 20 minutes; the other additives are one or more of flame retardant and thixotropic agent.
Compared with the prior art, the heat-conducting gel has the following advantages:
the product disclosed by the invention has better heat dissipation effectThe thermal conductivity coefficient is more than or equal to 3.8W/(m.K), and the thermal resistance is less than or equal to 0.045 ℃ in2,/W @20psi, minimum compressed thickness 40 μm.
The oil yield of the product disclosed by the invention is lower than that of the heat-conducting gel in the current market, the sample is L80 xW 5mm xH 2mm, the oil evolution is less than or equal to 12mm (55 ℃/168H), and the flow rate is more than or equal to 6.5g/min (1.55mm @90 psi).
The heat-conducting gel is a thick non-flowing heat-conducting interface material. The minimum compression thickness of the product disclosed by the invention can reach 40 mu m, the heat conductivity coefficient is high, the thermal resistance is low, the oil output is low, and the reliability test environment can be met.
In addition, the product disclosed by the invention can realize full-automatic glue dispensing by utilizing equipment, accurately control the glue discharging amount, greatly save materials and reduce the labor cost, and can be applied to heat dissipation of the mainboard chip set of the smart phone.
According to the invention, through matching of different particle sizes of various powders, the thermal resistance of the heat-conducting gel is reduced, the precipitation of silicone oil is reduced, and the flow rate of the heat-conducting gel is increased.
According to the invention, spherical alumina with different particle sizes is used as a basic component of the powder additive, and finally a uniform dispersion system is formed in the silicone oil and other additives, so that the flow rate of the heat-conducting gel is greatly improved while the ultralow oil yield is achieved, the application of customers can be met, and the high-performance spherical alumina has a high practical value.
Detailed Description
The present invention is described in detail below with reference to specific examples, but the use and purpose of these exemplary embodiments are merely to exemplify the present invention, and do not set forth any limitation on the actual scope of the present invention in any form, and the scope of the present invention is not limited thereto.
Example 1
The heat conducting gel with ultralow oil extraction amount and high flow rate performance in the embodiment comprises the following components in parts by weight:
60 parts of powder;
1 part of silicone oil;
0.05 part of a curing agent;
0.1 part of a treating agent;
0.01 part of catalyst;
0.01 part of color paste;
wherein, the powder consists of three spherical alumina with different grain diameters, and the weight percentages are as follows:
spherical alumina with a particle size of 30-50 μm: 40 percent;
spherical alumina with a particle size of 10-30 μm: 30 percent;
spherical alumina with a particle size of 0.1-10 μm: 30 percent.
The silicone oil is a vinyl silicone oil. The viscosity of the silicone oil is 100-3000 cps. The curing agent is a mixture of terminal hydrogen-containing silicone oil and side cyanogen-containing silicone oil. The treating agent is aminopropyl trimethoxy silane. The catalyst is chloroplatinic acid, and the platinum content is 100ppm-6000 ppm. The color paste is green.
The preparation method comprises the following steps:
s1, pouring liquid silicone oil into a planetary power stirrer, and heating the planetary power stirrer to 130 ℃;
s2, adding spherical alumina powder with the grain diameter of 30-50 mu m, and stirring for 15 minutes;
s3, adding spherical alumina powder with the grain diameter of 10-30 mu m, and stirring for 15 minutes;
s4, adding spherical alumina powder with the grain diameter of 0.1-10 mu m, adding a treating agent, and integrally stirring for 30 minutes;
s5, adding a curing agent and a catalyst, and stirring for 15 minutes;
s6, adding color paste, and integrally stirring for 20 minutes;
s7, integrally vacuumizing the mixture obtained in the step S6 for 20 minutes, and cooling to normal temperature for later use;
and S8, packaging the final mixture obtained in the step S7 in a needle tube with a standard specification through glue filling equipment to obtain a heat-conducting gel product.
Example 2
The heat conducting gel with ultralow oil extraction amount and high flow rate performance in the embodiment comprises the following components in parts by weight:
75 parts of powder;
20 parts of silicone oil;
3 parts of a curing agent;
2 parts of a treating agent;
0.5 part of a catalyst;
0.1 part of color paste;
the powder consists of three spherical aluminas with different grain diameters, and the weight percentages of the three spherical aluminas are as follows:
spherical alumina with a particle size of 30-50 μm: 60 percent;
spherical alumina with a particle size of 10-30 μm: 20 percent;
spherical alumina with a particle size of 0.1-10 μm: 20 percent.
The silicone oil is phenyl silicone oil and hydroxyl silicone oil. The viscosity of the silicone oil is 100-3000 cps. The curing agent is a mixture of terminal hydrogen-containing silicone oil and side cyanogen-containing silicone oil. The treating agent is vinyl triethoxy siloxane catalyst which is chloroplatinic acid, and the platinum content is 100ppm-6000 ppm. The color paste is green.
The preparation method is as in example 1.
Example 3
The heat conducting gel with ultralow oil extraction amount and high flow rate performance in the embodiment comprises the following components in parts by weight:
98 parts of powder;
50 parts of silicone oil;
5 parts of a curing agent;
5 parts of a treating agent;
1 part of a catalyst;
1 part of color paste;
the powder consists of three spherical aluminas with different grain diameters, and the weight percentages of the three spherical aluminas are as follows:
spherical alumina with a particle size of 30-50 μm: 90 percent;
spherical alumina with a particle size of 10-30 μm: 5 percent;
spherical alumina with a particle size of 0.1-10 μm: 5 percent.
The silicone oil is dimethyl silicone oil and amino silicone oil. The viscosity of the silicone oil is 100-3000 cps. The curing agent is a mixture of terminal hydrogen-containing silicone oil and side cyanogen-containing silicone oil. The treating agent is 3-aminopropyl triethoxy silane and vinyl trimethoxy siloxane. The catalyst is chloroplatinic acid, and the platinum content is 100ppm-6000 ppm. The color paste is green.
The preparation method is as in example 1.
The heat-conducting gels obtained in examples 1 to 3 were subjected to performance tests, and the test results were as follows:
the heat conductivity coefficient is more than or equal to 3.8W/m.k, and the thermal resistance is less than or equal to 0.045 ℃ in2The value of/W @20psi, the sample size L80 xW 5mm xH 2mm, the oil evolution is less than or equal to 12mm (55 ℃/168H), and the flow rate is more than or equal to 6.5g/min (1.55mm @90 psi).
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (10)
1. The heat conducting gel with ultralow oil extraction amount and high flow rate performance is characterized by comprising the following components in parts by weight:
60-98 parts of powder;
1-50 parts of silicone oil;
0.05-5 parts of a curing agent;
0.1-5 parts of a treating agent;
0.01-1 part of catalyst;
0.01-1 part of color paste;
the powder consists of three spherical aluminas with different grain diameters, and the weight percentages of the three spherical aluminas are as follows:
spherical alumina with a particle size of 30-50 μm: 40% -90%;
spherical alumina with a particle size of 10-30 μm: 5% -30%;
spherical alumina with a particle size of 0.1-10 μm: 5 to 30 percent.
2. The ultra-low oil extraction and high flow rate performance heat conduction gel according to claim 1, wherein the silicone oil is one or more of vinyl silicone oil, phenyl silicone oil, hydroxyl silicone oil, dimethyl silicone oil, amino silicone oil, methyl long-chain alkyl silicone oil and quaternary ammonium salt hydrocarbon-based modified silicone oil.
3. The ultra-low oil extraction and high flow rate performance heat conducting gel according to claim 1, wherein the curing agent is a mixture of terminal hydrogen-containing silicone oil and side cyanogen-containing silicone oil.
4. The ultra-low oil extraction and high flow rate performance thermal conductive gel according to claim 1, wherein the treating agent is a silane coupling agent, and the silane coupling agent is one or more of aminopropyltrimethoxysilane, vinyltriethoxysilane, 3-aminopropyltriethoxysilane and vinyltrimethoxysilane.
5. The ultra-low oil extraction and high flow rate performance thermal conductive gel according to claim 1, wherein the catalyst is chloroplatinic acid, and the platinum content is 100ppm to 6000 ppm.
6. The ultra-low oil run-out and high flow rate performance thermal conductive gel according to claim 1, wherein the color paste is green color paste.
7. The ultra-low oil extraction and high flow rate performance thermal gel as claimed in claim 1, wherein the viscosity of the silicone oil is 100-3000 cps.
8. The ultra-low oil extraction and high flow rate performance thermal conductive gel of claim 1, further comprising one or more of an optional flame retardant and a thixotropic agent.
9. A method for preparing the heat conducting gel with ultra-low oil extraction and high flow rate performance according to any one of claims 1 to 7, which is characterized by comprising the following steps:
s1, pouring liquid silicone oil into a planetary power stirrer, and heating the planetary power stirrer to 130 ℃;
s2, adding spherical alumina powder with the grain diameter of 30-50 mu m, and stirring for 15 minutes;
s3, adding spherical alumina powder with the grain diameter of 10-30 mu m, and stirring for 15 minutes;
s4, adding spherical alumina powder with the grain diameter of 0.1-10 mu m, adding a treating agent, and integrally stirring for 30 minutes;
s5, adding a curing agent and a catalyst, and stirring for 15 minutes;
s6, adding color paste, and integrally stirring for 20 minutes;
s7, integrally vacuumizing the mixture obtained in the step S6 for 20 minutes, and cooling to normal temperature for later use;
and S8, packaging the final mixture obtained in the step S7 in a needle tube with a standard specification through glue filling equipment to obtain a heat-conducting gel product.
10. The method for preparing the heat-conducting gel with ultra-low oil extraction amount and high flow rate performance according to claim 9, wherein color paste and other additives are added in S6, and the whole is stirred for 20 minutes; the other additives are one or more of flame retardant and thixotropic agent.
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| CN114573988A (en) * | 2022-04-18 | 2022-06-03 | 闽都创新实验室 | Interface heat management material and preparation method thereof |
| CN115926473A (en) * | 2022-12-27 | 2023-04-07 | 福建臻璟新材料科技有限公司 | Low-oil-yield heat-conducting gel and preparation method thereof |
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Application publication date: 20201117 |