NL2030496B1 - High-performance silicon-based thermally conductive gel and preparation method thereof - Google Patents

High-performance silicon-based thermally conductive gel and preparation method thereof Download PDF

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NL2030496B1
NL2030496B1 NL2030496A NL2030496A NL2030496B1 NL 2030496 B1 NL2030496 B1 NL 2030496B1 NL 2030496 A NL2030496 A NL 2030496A NL 2030496 A NL2030496 A NL 2030496A NL 2030496 B1 NL2030496 B1 NL 2030496B1
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thermally conductive
powder
silicon
gel
particle size
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NL2030496A
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NL2030496A (en
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Yang Fuhe
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Jiangsu Crystal River Electronic Tech Co Ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
    • 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
    • C08K2201/001—Conductive additives
    • 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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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present disclosure discloses a high-performance silicon-based thermally conductive gel and a preparation method thereof. The silicon-based thermally conductive gel 5 comprises an organic silicone gel, hydrogen-containing silicone oil, hydroxy silicone oil and thermally conductive powder. The thermally conductive powder is made by mixing different types of powders according to large, medium and small particle sizes. The product has excellent thixotropic properties, high thermal conductivity and good adhesion performance, can replace thermally conductive silicon gaskets, and can be lO operated by a dispenser in applications, which greatly improves production efficiency. During the production process, the macromolecular structures in the thermally conductive gel are connected into a network, which effectively prevents the exudation of low-molecular silicone oil, meanwhile, the high-performance silicon-based thermally conductive gel has high temperature resistance. The preparation method 15 provided herein is simple and feasible, the operation is simple, safe and reliable in application.

Description

HIGH-PERFORMANCE SILICON-BASED THERMALLY CONDUCTIVE GEL AND PREPARATION METHOD THEREOF
TECHNICAL FIELD [DI] The present disclosure relates to a silicone thermal interface material, and more particularly to a high-performance silicon-based thermally conductive gel and a preparation method thereof.
BACKGROUND ART
[02] In the electronic and electrical field, with the development of the integration technology and micro-encapsulation technology, electronic components and electronic equipment are developing towards miniaturization and microminiaturization, leading to more heat generated in a limited volume; at this time, high thermal conductivity insulation materials are required to quickly dissipate the generated heat. It is of great significance to the normal use and service life of sensitive components for every 10°C drop.
[03] At present, the silicon-based thermal pastes and thermally conductive silicon gaskets are mainly available in the markets. The silicon-based thermal pastes often precipitate out silicone oil during the storage and use, which will become dry and greatly reduce the thermal conductivity. The thermally conductive silicon gaskets need to be cut into corresponding shapes as required, and the gaskets need to be manually attached to corresponding positions, which will greatly reduce the production efficiency and use efficiency of the thermally conductive silicon gaskets.
SUMMARY
[04] The present disclosure is proposed to overcome the shortcomings of the prior art. The object of the present disclosure is to provide a high-performance silicon-based thermally conductive gel and a preparation method thereof.
[05] The present disclosure adopts the technical solution as follows: a high- performance silicon-based thermally conductive gel, comprising the following components in percentage by weight:
[06] 10% -15% of organic silicone gel;
[07] 3% -5% of hydrogen-containing silicone oil;
[08] 3% -5% of hydroxy silicone oil; and
[09] the balance of thermally conductive powder.
[10] The organic silicone gel is a silicone gel of polydiorganosiloxane containing vinyl groups, which includes two components A and B and is mixed in a ratio of 1:1.
[11] The hydrogen-containing silicone oil is linear methyl hydrogen silicone oil.
[12] The hydroxy silicone oil is a, -dihydroxy polydimethylsiloxane.
[13] The thermally conductive powder is one of or a mixture of two or more of aluminum oxide, zinc oxide, boron nitride, aluminum nitride, and aluminum powder.
[14] The thermally conductive powder is composed of powders with a large particle size, a medium particle size and a small particle size in a mass ratio of 5:3:1, wherein the particle size of large-size powder is 50-60 um, the particle size of medium-size powder is 20-30 um, and the particle size of small-size powder is 1-5 pm.
[15] According to performance requirements, the thermally conductive powder can further comprise a thickener, a surfactant, a flame retardant and a colorant.
[16] A method for preparing the high-performance silicon-based thermally conductive gel comprises the following steps:
[17] (1) drying thermally conductive powder
[18] baking the thermally conductive powder at 150°C for 20-40 hours, to remove water; 19] (11) grading thermally conductive powder of different particle sizes
[20] grading thermally conductive powder of different particle sizes, and pre- mixing thermally conductive powders with a large particle size, a medium particle size and a small particle size in a mass ratio of 5: 3 : 1;
[21] (1i1) mixing
[22] mixing the thermally conductive powder obtained in step ( 11 ) with organic silicone gel, hydrogen-containing silicone oil and hydroxy silicone oil in a double planetary mixer for 20 to 30 minutes;
[23] (tv) vulcanization
[24] performing full crosslinking of the mixture obtained in the step (iii) at 120°C for 24 hours, cooling, to obtain a high-performance silicon-based thermally conductive gel.
[25] Beneficial effects of the present disclosure
[26] The product of the present disclosure has a network structure connected by macromolecular structures, which effectively prevents the seepage of small molecular silicone oil, prevents the silicone oil from separating out and migrating into a device contactor, and avoids high contact resistance, arcing and mechanical wear.
[27] The product of the present disclosure has a plasticine-like appearance and can be kneaded into any shape at will, is suitable for operation and use with a dispenser.
Compared with thermally conductive pastes and thermally conductive silicon gaskets, a lot of manual operations are saved and the production efficiency is greatly improved.
[28] The present disclosure has better thixotropy and adhesion, does not flow like a thermally conductive paste during use, has better adhesion than a thermally conductive silicon gasket, and is easier to fill gaps, thereby improving thermal conductivity.
[29] The product of the present disclosure has low toxicity, is economical in use, and low in volatile weight loss, and does not require refrigeration, so the storage and operation procedures are simplified. The preparation method is simple, feasible, sate and reliable.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[30] The high-performance silicon-based thermally conductive gel and the preparation method thereof provided in the present disclosure will be described in detail below with reference to embodiments.
[31] A high-performance silicon-based thermally conductive gel, comprising the following components in percentage by weight:
[32] 10% -15% of organic silicone gel,
[33] 3% -5% of hydrogen-containing silicone oil;
[34] 3% -5% of hydroxy silicone oil; and
[35] the balance of thermally conductive powder.
[36] Wherein, the organic silicone gel is a silicone gel of polydiorganosiloxane containing vinyl groups, which includes two components A and B and is mixed in a ratio of 1:1.
[37] Wherein, the hydrogen-containing silicone oil is linear methyl hydrogen silicone oil.
[38] Wherein, the hydroxy silicone oil is 0,0 -dihydroxy polydimethylsiloxane.
[39] Wherein, the thermally conductive powder is one of or a mixture of two or more of aluminum oxide, zinc oxide, boron nitride, aluminum nitride, and aluminum powder.
[40] The thermally conductive powder is composed of powders with a large particle size, a medium particle size and a small particle size in a mass ratio of 5:3:1, wherein the particle size of large-size powder 1s 50-60 um, the particle size of medium-size powder is 20-30 um, and the particle size of small-size powder is 1-5 um.
[41] The purpose of grading the thermally conductive powder according to the large, medium and small particle sizes is to achieve the highest filling rate, so as to achieve the best thermal conductivity coefficient. The particle shape of the thermally conductive powder is spherical or ellipsoidal.
[42] As adjustable components, some commonly used additives can also be added to the silicon-based thermally conductive gel of the present disclosure, which should not weaken the purpose of the present disclosure. The specific additives comprise a thickener, a surfactant, a flame retardant and a colorant.
[43] A method for preparing the silicon-based thermally conductive gel comprises the following steps:
[44] (1) drying thermally conductive powder
[45] baking the thermally conductive powder at 150°C for 20-40 hours, to remove water;
[46] (11) grading thermally conductive powder of different particle sizes
[47] grading thermally conductive powder of different particle sizes, and pre- mixing thermally conductive powders with a large particle size, a medium particle size and a small particle size in a mass ratio of 5:3 : 1;
[48] (1i1) mixing
[49] mixing the thermally conductive powder obtained in step ( 11 ) with organic silicone gel, hydrogen-containing silicone oil and hydroxy silicone oil in a double planetary mixer for 20 to 30 minutes;
[50] (iv) vulcanization
[51] performing full crosslinking of the mixture obtained in the step (iii) at 120°C for 24 hours, cooling, to obtain a high-performance silicon-based thermally conductive gel.
[52] Examples 1 to 3
[53] (1) Preparation of raw materials
[54] a. organic silicone gel (two components of A and B, mixed at a ratio of 1:1).
[55] b. methyl hydrogen silicone oil
[56] c. hydroxy silicone oil
[57] d. thermally conductive powder
[58] wherein: d1 aluminum powder (average particle size of 3um )
[59] d2 alumina powder (average particle size of 55um )
[60] d3 boron nitride powder (average particle size of 25um )
[61] After the above thermally conductive powders were dried, they were mixed according to the ratio shown in Table 1.
[62] (2) The above components were placed in a double planetary mixer according to a certain ratio ( specific components and ratios were shown in Table 1), and mixed, to obtain a silicon-based thermally conductive gel .
[63] The components of silicon-based thermally conductive gels in Examples 1 to 3 were shown in Table | below.
[64] Table 1 Component Ene bop 4 5 ;
[65] In order to verify the performance of the product of the present disclosure, the following tests were conducted.
[66] (1) Viscosity test
[67] The viscosity of the silicon-based thermally conductive gel prepared in Examples 1 to 3 was measured by a rotary viscometer (RVDVII, Brookfield) ata rotating speed of 10 RPM with a 07# rotor. The results were shown in Table 2, indicating that the viscosity was not large, which was conducive to the operation of the dispenser.
[68] (2) Thermal conductivity test
[69] The silicon-based thermally conductive gel prepared in Examples | to 3 was coated on the test table of the Hotdisk tester with a thickness controlled at 0.075 mm, then the thermal conductivity coefficient of the silicon-based thermally conductive gel was measured, results were shown in Table 2. The results indicated that the silicon-based thermally conductive gel had a high thermal conductivity coefficient and was suitable for occasions that require high heat dissipation.
[70] (3) Adhesion test 71] The silicon-based thermally conductive gel prepared in Examples 1 to 3 was dispensed with a 13# stainless steel needle onto an aluminum alloy substrate, to form a pile with a diameter of about 1 cm, then placed in a vibrating screen for vibrating for 1 hour. No gel fell, indicating that the silicon-based thermally conductive gel had strong adhesion.
[72] (4) Impact resistance test
[73] 1. Aging test 1: The silicon-based thermally conductive gel prepared in Examples | to 3 was baked at 150°C for 1000 hours.
[74] 2. Aging test 2: The silicon-based thermally conductive gel prepared in Examples 1 to 3 was tested under the condition of a temperature of 85°C and a RH of 85% for 1,000 hours.
[75] 3. Thermal shock test: the silicon-based thermally conductive gel prepared in Examples | to 3 was cycled for 600 times at a temperature of -55°C to 125°C.
[76] The silicon-based thermally conductive gels before and after the test were coated on the test table of a LW-9011R thermal resistance tester (manufactured by Taiwan LONG WIN), with the thickness controlled at 0. 1mm, and the thermal resistance was measured. Results were shown in Table 2. After the aging test, the thermal resistance was not reduced greatly, indicating that the product of the present disclosure had better thermal stability.
[77] The thermal shock test showed (Table 2) that the product of the present disclosure does not require refrigerated storage, which is convenient for storage and use.
[78] The test results of the silicon-based thermally conductive gel of the present disclosure were shown in Table 2 below.
[79] Table 2 Thermal 4.2 3.9 3.8 conductivity coefficient (W/mK) Thermal resistance | 0.019 0.021 0.025 en
Thermal resistance | 0.020 0.021 0.027 after aging test 1 (°Cein*/W) Thermal resistance | 0.021 0.022 0.029 after aging test 2 (°Cein’*/W) Thermal resistance | 0.025 0.027 0.028 after thermal shock test (°Cein®/W)
[80] The above descriptions are merely specific embodiments of the present disclosure, but the protection scope of the present disclosure is not limited hereto. All and any variations or substitutions that can be easily envisaged by those skilled in the art within the technical scope disclosed by the present disclosure shall be covered within the protection scope of the present disclosure. Therefore, the protection scope of the present disclosure should be subject to the protection scope as claimed by the appended claims.

Claims (8)

-9- Conclusies L Hoogwaardige, thermisch geleidende gel op basis van silicium, die de volgende componenten in gewichtspercentage omvat: 10% — 15% organische siliconegel; 3% — 5% waterstofhoudende siliconeolie; 3% — 5% hydroxysiliconeolie; en de balans van thermisch geleidende poeder.-9- Conclusions L High performance silicon based thermal conductive gel comprising the following components by weight: 10% — 15% organic silicone gel; 3% — 5% hydrogenated silicone oil; 3% — 5% hydroxysilicone oil; and the balance of thermally conductive powder. 2. Hoogwaardige, thermisch geleidende gel op basis van silicium volgens conclusie 1, waarbij de organische siliconegel een siliconegel van polydiorganosiloxaan is die vinylgroepen bevat, die twee componenten A en B omvat en gemengd is in een verhouding van 1:1.The high-performance silicon-based thermally conductive gel according to claim 1, wherein the organic silicone gel is a polydiorganosiloxane silicone gel containing vinyl groups, comprising two components A and B and mixed in a ratio of 1:1. 3. Hoogwaardige, thermisch geleidende gel op basis van silicium volgens conclusie 1, waarbij de waterstofhoudende siliconeolie lineaire methylwaterstofsiliciumolie is.The high-performance silicon-based thermally conductive gel according to claim 1, wherein the hydrogen-containing silicone oil is linear methyl hydrogen silicon oil. 4. Hoogwaardige, thermisch geleidende gel op basis van silicium volgens conclusie 1, waarbij de hydroxysiliconeolie een a, w-dihydroxypolydimethylsiloxaan is.The high performance silicon-based thermally conductive gel of claim 1, wherein the hydroxysilicone oil is an α,ω-dihydroxypolydimethylsiloxane. 5. Hoogwaardige, thermisch geleidende gel op basis van silicium volgens conclusie 1, waarbij de thermisch geleidende poeder één is van of een mengsel van twee of meer is van aluminiumoxide, zinkoxide, boornitride, aluminiumnitride en aluminiumpoeder.The high performance silicon-based thermally conductive gel according to claim 1, wherein the thermally conductive powder is one or a mixture of two or more of aluminum oxide, zinc oxide, boron nitride, aluminum nitride and aluminum powder. 6. Hoogwaardige, thermisch geleidende gel op basis van silicium volgens conclusie 5, waarbij de thermisch geleidende poeder samengesteld is uit poeder met een grote deeltjesgrootte, een middelgrote deeltjesgrootte en een kleine deeltjesgrootte in een massaverhouding van 5:3:1, waarbij de deeltjesgrootte van grotedeeltjespoeder 50 — 60 um is, de deeltjesgrootte van middelgrotedeeltjespoeder 20 — 30 um is en de deeltjesgrootte van kleinedeeltjespoeder 1 — 5 um is.The high performance silicon-based thermally conductive gel according to claim 5, wherein the thermally conductive powder is composed of powder having a large particle size, a medium particle size and a small particle size in a mass ratio of 5:3:1, the particle size of large particle powder is 50-60 um, the particle size of medium particle powder is 20-30 um, and the particle size of small particle powder is 1-5 um. 7. Hoogwaardige, thermisch geleidende gel op basis van silicium volgens conclusie 1, waarbij de thermisch geleidende poeder verder een verdikkingsmiddel, eenThe high performance silicon-based thermally conductive gel of claim 1, wherein the thermally conductive powder further contains a thickener, a -10- oppervlakteactieve stof, een vlamweringsmiddel en een kleurstof omvat.-10- surfactant, a flame retardant and a colorant. 8. Werkwijze voor het bereiden van de hoogwaardige, thermisch geleidende gel op basis van silicium volgens conclusie 1, die de volgende stappen omvat: (1) het drogen van thermisch geleidende poeder het bakken van de thermisch geleidende poeder bij 150°C gedurende 20 — 40 uur; (ii) het indelen van de thermisch geleidende poeder van verschillende deeltjesgroottes het indelen van de thermisch geleidende poeder van verschillende deeltjesgroottes, en het vooraf mengen van de thermisch geleidende poeders met een grote deeltjesgrootte, een middelgrote deeltjesgrootte en een kleine deeltjesgrootte in een massaverhouding van 5:3:1; (iii) mengen het mengen van de thermisch geleidende poeder die verkregen is in stap (11) met organische siliconegel, waterstofhoudende siliconeolie en hydroxysiliconeolie in een dubbele planeetmenger gedurende 20 — 30 minuten; (iv) vulkanisatie het uitvoeren van volledige dwarsverbinding van het mengsel dat verkregen is in stap (tij) bij 120°C gedurende 24 uur, het afkoelen, om een hoogwaardige, thermisch geleidende gel op basis van silicium te verkrijgen.The process for preparing the high performance silicon-based thermally conductive gel according to claim 1, comprising the steps of: (1) drying thermally conductive powder baking the thermally conductive powder at 150°C for 20- 40 hours; (ii) classifying the thermally conductive powder of different particle sizes classifying the thermally conductive powder of different particle sizes, and pre-mixing the thermally conductive powders having a large particle size, a medium particle size and a small particle size in a mass ratio of 5 :3:1; (iii) mixing mixing the thermally conductive powder obtained in step (11) with organic silicone gel, hydrogenated silicone oil and hydroxysilicone oil in a double planetary mixer for 20-30 minutes; (iv) vulcanization performing complete cross-linking of the mixture obtained in step (tide) at 120°C for 24 hours, cooling, to obtain a high-quality silicon-based thermally conductive gel.
NL2030496A 2022-01-11 2022-01-11 High-performance silicon-based thermally conductive gel and preparation method thereof NL2030496B1 (en)

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