CN112625659A - High-thermal-conductivity heat-conducting silicone grease and preparation process thereof - Google Patents
High-thermal-conductivity heat-conducting silicone grease and preparation process thereof Download PDFInfo
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- CN112625659A CN112625659A CN202011533980.3A CN202011533980A CN112625659A CN 112625659 A CN112625659 A CN 112625659A CN 202011533980 A CN202011533980 A CN 202011533980A CN 112625659 A CN112625659 A CN 112625659A
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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
Abstract
The invention discloses a high-thermal-conductivity thermal-conductive silicone grease and a preparation method thereof, wherein the thermal-conductive silicone grease comprises the following components in parts by mass: 80-99 parts of powder; 1-20 parts of silicone oil; 0.01-5 parts of a coupling agent; the powder is a mixture of zinc oxide and metal aluminum powder which are directly mixed without forming an oxide film on the surface of the powder, and the powder comprises the following components in percentage by mass: metal aluminum powder: 80% -99%; zinc oxide: 1% -20%; the grain diameter of the metal aluminum powder is 1-30 microns, and the grain diameter of the zinc oxide is 0.1-5 microns. The heat-conducting silicone grease has the heat conductivity coefficient of 6.0-6.5W/m.K, is simpler in process and low in price, and can meet the market demand.
Description
Technical Field
The invention relates to the technical field of heat-conducting interface materials for high-power electronic and electrical equipment, in particular to high-heat-conducting silicone grease and a preparation process thereof.
Background
With the rapid development of the communication industry, the power consumption of the chip is higher and higher, and the heat flux density is higher and higher. If the heat of the chip cannot be quickly dissipated, the chip is over-heated, and the service life of the chip is affected.
For the heat dissipation problem of the communication product chip, a common heat dissipation design is to mount a spring screw radiator, a heat pipe or a VC radiator on a heat source. Between the chip and the heat sink, there is inevitably a certain gap, which leads to an increase in contact thermal resistance, and certainly seriously affects the rapid heat transfer of the chip.
The heat conducting interface material has the main function of reducing the contact thermal resistance between the heating chip and the radiator so as to achieve the purpose of fast heat dissipation. The heat-conducting silicone grease, as one of the heat-conducting interface materials, is often used in the situation where the gap is extremely thin, and is usually between 0.01 and 0.3 mm. Because of its high thermal conductivity, low thermal resistance, and low BLT, it is widely used.
The heat-conducting silicone grease is formed by mixing silicone oil, a filler and other additives, and is mainly divided into two categories: one type is the most common heat-conducting silicone grease of an alumina system, which generally comprises silicone oil, alumina, zinc oxide and additives, and the heat-conducting silicone grease is insulating heat-conducting silicone grease. The other is heat-conducting silicone grease of a metal aluminum powder system. The heat-conducting silicone grease generally comprises silicone oil, aluminum powder, zinc oxide and an additive. Compared with the heat-conducting silicone grease of an alumina system, the heat-conducting silicone grease of the metal aluminum powder is uninsulated, but the thermal property is far superior to that of the heat-conducting silicone grease of the alumina system, and the heat-conducting silicone grease is widely used in the communication and computer industries.
In the existing high-end heat-conducting silicone grease, the additive is generally aluminum nitride or metal aluminum powder. The heat conductivity coefficient of the metal aluminum powder can reach 200W/mK relative to the heat conductivity coefficient of the aluminum oxide powder of 36W/mK. 1-4W/m.K heat-conducting silicone grease of the existing alumina system on the market.
Chinese patent document CN111154271A discloses a heat-conducting silicone grease with high heat-conducting property and a preparation process thereof. The composition comprises the following components in parts by mass: 60-90 parts of powder; 10-40 parts of silicone oil; 1-5 parts of a coupling agent; the powder is a mixture of aluminum oxide, zinc oxide and graphite powder, wherein the powder comprises the following components in parts by weight: alumina: 20-35 parts of a solvent; zinc oxide: 10-15 parts; graphite powder: 60-70 parts. According to the invention, through matching various powders with different particle sizes, the thermal resistance of the heat-conducting silicone grease is further reduced, and the heat absorption of the heat-conducting silicone grease to a heat source is accelerated. The aluminum oxide and the zinc oxide are matched with the graphite powder to form the modified coated graphite powder. The modified coated graphite powder has a good bonding interface in the main component silicone oil of the heat-conducting silicone grease, and is beneficial to the dispersion of the modified coated graphite powder in the heat-conducting silicone grease, so that the thermal contact resistance between the interface of the modified coated graphite powder and the heat-conducting silicone grease is reduced, and the heat conductivity coefficient is improved. The heat conductivity coefficient of the heat-conducting silicone grease with high heat conductivity can be 4.5-5W/m.K. There is still room for further improvement.
Chinese patent document CN101294067A discloses a heat-conducting silicone grease composition, which comprises the following components in percentage by weight: 5-20% of organic silicone oil, 0.005-1% of silane coupling agent and the balance of heat-conducting powder, wherein the silane coupling agent is coated on the surface of the heat-conducting powder; wherein the heat conducting powder consists of powder with large, medium and small particle diameters according to the volume ratio of 10: 5-1: 5-0.1; the large particle size is 10.1 to 50 μm, the medium particle size is 1.1 to 10 μm, and the small particle size is 0.1 to 1 μm. The metal powder involved in the heat-conducting powder is subjected to heat treatment, and a layer of oxide film is formed on the surface of the metal powder. The metal powder is one or a mixture of two or more of aluminum, silver, copper or nickel, and the surface of the metal powder has an oxide film with a thickness of 10-200 nm. Although the thermal conductivity is 5.5-6.9W/m.K, the technical scheme needs a more complex oxidation process, so that the technical scheme has higher production cost and higher price and cannot meet the market demand.
Disclosure of Invention
In view of the above, the present invention is directed to a high thermal conductivity thermal grease and a preparation process thereof, wherein the thermal conductivity coefficient of the thermal grease is 6.0-6.5W/m · K, and the process is simpler and has a low price, thereby meeting market requirements.
The adopted technical scheme is as follows:
the invention relates to high-thermal-conductivity heat-conducting silicone grease which comprises the following components in parts by mass:
80-99 parts of powder;
1-20 parts of silicone oil;
0.01-5 parts of a coupling agent;
the powder is a mixture of zinc oxide and metal aluminum powder which are directly mixed without forming an oxide film on the surface of the powder, and the powder comprises the following components in percentage by mass:
metal aluminum powder: 80% -99%;
zinc oxide: 1% -20%;
the grain diameter of the metal aluminum powder is 1-30 microns, and the grain diameter of the zinc oxide is 0.1-5 microns.
Further, the particle size of the metal aluminum powder is 1-20 microns.
Further, the metal aluminum powder is composed of metal aluminum powder with different particle sizes.
Further, the metal aluminum powder: 90-99%; 1 to 10 percent of zinc oxide.
Further, the silicone oil is one or more of vinyl silicone oil, hydrogen-containing silicone oil, benzyl silicone oil, hydroxyl silicone oil, dimethyl silicone oil, methyl long-chain alkyl silicone oil or quaternary ammonium salt hydrocarbon modified silicone oil and the like.
Further, the coupling agent is octyl trimethoxy siloxane and phenyl siloxane.
Further, the viscosity of the silicone oil is 100-3000 cps.
Further, one or more of a stabilizer, a flame retardant, a colorant and a thixotropic agent are added into the heat-conducting silicone grease component.
The preparation method of the high-thermal-conductivity heat-conducting silicone grease comprises the following steps:
s1, pouring liquid silicone oil and a silane coupling agent into a planetary power mixer;
s2, sequentially adding metal aluminum powder mixtures with different particle sizes, and stirring for 15 minutes;
s3, adding zinc oxide powder and stirring for 15 minutes;
s4, finally, integrally stirring for 30 minutes;
s5, transferring the mixture obtained in the step S4 from the planetary power mixer to a three-roll grinder for grinding twice;
s6, transferring the mixture obtained by grinding in the step S5 from the three-roll grinder to a planetary power stirrer for stirring for 30 minutes;
s7, vacuumizing the whole mixture finally stirred in the step S6 for 30 minutes.
Further, in S2-S3, the corresponding stirring speed in the stirring process of the added metallic aluminum powder and zinc oxide powder is 20-40r/min, and the dispersion speed is 500-800 r/min;
in S4, the stirring speed corresponding to the stirring of the whole mixture for 30 minutes is 30-50r/min, and the dispersion speed is 600-1000 r/min;
in S6, the stirring speed corresponding to the whole mixture obtained by grinding is 30-50r/min, and the dispersion speed is 600-1000 r/min;
in S7, the degree of vacuum corresponding to the vacuumizer is-0.098 MPa.
Compared with the prior art, the heat-conducting silicone grease has the following advantages:
the advantages are that: the heat conductivity coefficient of the metal aluminum powder as one additive is 200W/(M.K); the addition of the aluminum powder greatly improves the overall heat conductivity coefficient of the product.
The advantages are that: the aluminum powder is favorable for the dispersion of the aluminum powder in the heat-conducting silicone grease, and an effective heat-conducting network can be formed in the heat-conducting silicone grease, so that the contact thermal resistance between interfaces is reduced, and the aims of improving the heat-conducting property of the heat-conducting silicone grease and prolonging the service life of the heat-conducting silicone grease are fulfilled.
The advantages are that: the addition of the zinc oxide increases the specific surface area of the material, reduces the thermal resistance of the silicone grease body, remarkably improves the absorption rate of the initial temperature of the hot end, achieves the effect of rapid heat dissipation, and can improve the thixotropy of the heat-conducting silicone grease.
According to the invention, metal aluminum and zinc oxide are used as basic components of the powder additive, and finally a uniform dispersion system is formed in the silicone oil, so that the silicone oil has high thermal conductivity and good thixotropy, the heat dissipation efficiency of the heat-conducting silicone grease is greatly improved, and the silicone oil has a strong practical value.
The powder is a mixture of zinc oxide and metal aluminum powder which are directly mixed without forming an oxide film on the surface of the powder, wherein the metal aluminum powder accounts for 80-99 percent; zinc oxide: 1% -20%; the high-thermal-conductivity silicone grease prepared from the powder has the advantages that on one hand, the thermal conductivity coefficient of the silicone grease is 6.0-6.5W/m.K, on the other hand, the process is simpler, the price is low, and the market demand can be met.
According to the invention, through matching various different particle sizes of the metal aluminum powder, the thermal resistance of the heat-conducting silicone grease is further reduced, and the heat transfer of the heat-conducting silicone grease to a heat source is accelerated, so that the purpose of rapid heat dissipation is achieved.
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 invention relates to high-thermal-conductivity heat-conducting silicone grease which comprises the following components in parts by mass:
80 parts of powder; 5 parts of silicone oil; 1 part of a coupling agent;
the powder is a mixture of zinc oxide and metal aluminum powder which are directly mixed without forming an oxide film on the surface of the powder, and the powder comprises the following components in percentage by mass:
metal aluminum powder: 90 percent; zinc oxide: 10 percent;
the grain diameter of the metal aluminum powder is 1-20 microns, and the grain diameter of the zinc oxide is 0.1-5 microns. The metal aluminum powder is composed of metal aluminum powder with different particle sizes.
The silicone oil is a vinyl silicone oil. The viscosity of the silicone oil is 100-3000 cps.
The coupling agent is octyl trimethoxy siloxane and phenyl siloxane.
The preparation method of the high-thermal-conductivity heat-conducting silicone grease comprises the following steps:
s1, pouring liquid silicone oil and a silane coupling agent into a planetary power mixer;
s2, sequentially adding metal aluminum powder mixtures with different particle sizes, and stirring for 15 minutes; the stirring speed is 20-40r/min, and the dispersion speed is 500-800 r/min;
s3, adding zinc oxide powder and stirring for 15 minutes; the stirring speed is 20-40r/min, and the dispersion speed is 500-800 r/min;
s4, finally, integrally stirring for 30 minutes; the stirring speed is 30-50r/min, and the dispersion speed is 600-;
s5, transferring the mixture obtained in the step S4 from the planetary power mixer to a three-roll grinder for grinding twice;
s6, transferring the mixture obtained by grinding in the step S5 from the three-roll grinder to a planetary power stirrer for stirring for 30 minutes; the stirring speed is 30-50r/min, and the dispersion speed is 600-;
s7, integrally vacuumizing the mixture finally stirred in the step S6 for 30 minutes; the vacuum degree is-0.098 Mpa. And packaging the final mixture in a 200mL tank to obtain the heat-conducting silicone grease.
Example 2
Referring to example 1, unlike example 1, the highly thermally conductive silicone grease of the present example is composed of the following components in parts by mass: 90 parts of powder; 10 parts of silicone oil; 2 parts of a coupling agent; the mass ratio of each component in the powder is as follows: metal aluminum powder: 95 percent; zinc oxide: 5 percent.
Example 3
Referring to example 1, unlike example 1, the highly thermally conductive silicone grease of the present example is composed of the following components in parts by mass: 95 parts of powder; 15 parts of silicone oil; 3 parts of a coupling agent; the mass ratio of each component in the powder is as follows: metal aluminum powder: 96 percent; zinc oxide: 4 percent.
The heat-conductive silicone grease prepared in the embodiments 1-3 has a thermal conductivity of 6.0-6.5W/m.K or more and a thermal resistance of 0.05-0.07 ℃ cm2a/W @40psi, a BLT (thermal interface material thickness) of 0.02-0.04mm @40psi, and a breakdown strength of 700-.
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 high-thermal-conductivity heat-conducting silicone grease is characterized by comprising the following components in parts by mass:
80-99 parts of powder;
1-20 parts of silicone oil;
0.01-5 parts of a coupling agent;
the powder is a mixture of zinc oxide and metal aluminum powder which are directly mixed without forming an oxide film on the surface of the powder, and the powder comprises the following components in percentage by mass:
metal aluminum powder: 80% -99%;
zinc oxide: 1% -20%;
the grain diameter of the metal aluminum powder is 1-30 microns, and the grain diameter of the zinc oxide is 0.1-5 microns.
2. The high thermal conductive silicone grease as recited in claim 1, wherein the metal aluminum powder has a particle size of 1-20 μm.
3. The high thermal conductive silicone grease as recited in claim 1, wherein the metal aluminum powder is composed of metal aluminum powders of different particle sizes.
4. The high thermal conductivity thermal grease as claimed in claim 1, wherein the metal aluminum powder is composed of metal aluminum powders with different particle sizes: 90-99%; 1 to 10 percent of zinc oxide.
5. The silicone grease of claim 1, wherein the silicone oil is one or more of vinyl silicone oil, hydrogen-containing silicone oil, benzyl silicone oil, hydroxy silicone oil, dimethyl silicone oil, methyl long-chain alkyl silicone oil, or quaternary ammonium salt hydrocarbon-modified silicone oil.
6. The high thermal conductivity thermal grease according to claim 1, wherein the coupling agent is octyl trimethoxy siloxane and phenyl siloxane.
7. The silicone grease of claim 1, wherein the viscosity of the silicone oil is 100-3000 cps.
8. The high thermal conductive silicone grease as claimed in claim 1, wherein one or more of a stabilizer, a flame retardant, a colorant, and a thixotropic agent is further added to the thermal conductive silicone grease component.
9. A method for preparing the highly thermally conductive silicone grease of any one of claims 1-8, comprising the steps of:
s1, pouring liquid silicone oil and a silane coupling agent into a planetary power mixer;
s2, sequentially adding metal aluminum powder mixtures with different particle sizes, and stirring for 15 minutes;
s3, adding zinc oxide powder and stirring for 15 minutes;
s4, finally, integrally stirring for 30 minutes;
s5, transferring the mixture obtained in the step S4 from the planetary power mixer to a three-roll grinder for grinding twice;
s6, transferring the mixture obtained by grinding in the step S5 from the three-roll grinder to a planetary power stirrer for stirring for 30 minutes;
s7, vacuumizing the whole mixture finally stirred in the step S6 for 30 minutes.
10. The method for preparing a highly thermally conductive silicone grease as claimed in claim 9,
in S2-S3, the corresponding stirring speed in the stirring process of the added metal aluminum powder and zinc oxide powder is 20-40r/min, and the dispersion speed is 500-800 r/min;
in S4, the stirring speed corresponding to the stirring of the whole mixture for 30 minutes is 30-50r/min, and the dispersion speed is 600-1000 r/min;
in S6, the stirring speed corresponding to the whole mixture obtained by grinding is 30-50r/min, and the dispersion speed is 600-1000 r/min;
in S7, the degree of vacuum corresponding to the vacuumizer is-0.098 MPa.
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| CN202011533980.3A CN112625659A (en) | 2020-12-22 | 2020-12-22 | High-thermal-conductivity heat-conducting silicone grease and preparation process thereof |
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Cited By (3)
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| CN113105744A (en) * | 2021-04-14 | 2021-07-13 | 中兴通讯股份有限公司 | Heat-conducting silicone grease, preparation method thereof and chip assembly |
| CN113881406A (en) * | 2021-10-22 | 2022-01-04 | 梅剑雄 | High-thermal-conductivity heat-conducting silicone grease and preparation method thereof |
| CN114276790A (en) * | 2022-01-26 | 2022-04-05 | 江西宏柏新材料股份有限公司 | Preparation method of insulating high-thermal-conductivity silicone grease |
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