CN111073612A - Resin-free low-permeability oil heat conduction mud and preparation method thereof - Google Patents
Resin-free low-permeability oil heat conduction mud and preparation method thereof Download PDFInfo
- Publication number
- CN111073612A CN111073612A CN201911406108.XA CN201911406108A CN111073612A CN 111073612 A CN111073612 A CN 111073612A CN 201911406108 A CN201911406108 A CN 201911406108A CN 111073612 A CN111073612 A CN 111073612A
- Authority
- CN
- China
- Prior art keywords
- heat
- parts
- resin
- conducting filler
- filler
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses resin-free low-permeability oil heat conduction mud which comprises the following components in parts by weight: 11-30 parts of heat-conducting filler, 21-30 parts of heat-conducting filler, 31-30 parts of heat-conducting filler, 0.1-5 parts of coupling agent and 0.1-2 parts of antioxidant. The invention realizes low oil permeability by removing the silicone resin part in the conventional heat conduction, and improves the adhesive force between the filler and the filler by modifying the surface of the filler, so that the modified filler can be kneaded into a mass, thereby preparing the resin-free low oil permeability heat conduction mud which can be used for filling the gaps of radiators in the electronic industry, can be used for a long time at the temperature of minus 50-150 ℃, ensures low oil permeability, and improves the service life and stability of electronic elements.
Description
Technical Field
The invention relates to heat conduction mud, in particular to resin-free low-permeability oil heat conduction mud and a preparation method thereof.
Background
Along with the rapid development of economy in China, electronic components are increasingly miniaturized and highly integrated, and the heat productivity and the heat flux density of the electronic components are also increasingly high. The research shows that: firstly, the stability of the system is reduced by 10% when the using temperature of the chip rises by 2 ℃; and secondly, the failure of more than 50 percent of the electronic components is caused by overhigh temperature. For two decades, efforts have been made to solve the heat dissipation problem of electronic components, and much work has been done on heat sinks, electronic components, and heat conductive materials.
The heat conducting material is a material which is arranged between the electronic element and the radiator and has the functions of heat transfer and reducing contact thermal resistance, and consists of matrix resin and a heat conducting agent. The roughness of the surface of the common electronic element and the common heat sink on the market generally reaches more than 8 μm, if the electronic element and the heat sink are in direct contact, the effective contact area between the electronic element and the heat sink is only 10% of the area of the base of the heat sink (more air gaps exist), the contact thermal resistance is higher, the efficiency of the heat sink is finally low, and the stability of the electronic element is reduced. The gaps are filled with the heat conducting materials, so that the effective contact area between the electronic element and the radiator can be greatly increased, an effective heat conducting channel is established, the contact thermal resistance is reduced, and the effect of the radiator is fully exerted. Although the heat-conducting interface material exists in the form of an auxiliary material in an electronic product, the heat dissipation problem of the electronic component (product) is effectively solved, the reliability, the stability and the service life of the electronic component (product) are improved, and the heat-conducting interface material is an indispensable part in the electronic product.
Similar to heat conducting paste and heat conducting gasket, the heat conducting mud is also a heat conducting material widely accepted by the market, and has the characteristics of high automation degree (mechanical automation production, packaging and glue dispensing), good weather resistance, moderate thermal resistance and high heat conductivity, and has the defects of high oil permeability and relatively high filler cost.
A common composition of the heat transfer mud is a silicone resin with a low degree of crosslinking and a filler. The incompletely reacted silicone resin gradually bleeds out as the storage and use time is prolonged. The leaked silicone resin is diffused to the surface of the electronic element and continuously reacts with dust in the air, so that the electronic element is easy to be unstable, and phenomena such as breakdown, short circuit and the like occur. In order to ensure the fluidity (automatic production speed) of the heat-conducting mud, the filler of the heat-conducting mud is heat-conducting filler with high sphericity, so the cost is higher than that of the crushed filler.
Disclosure of Invention
The invention provides a resin-free low-oil-permeability heat-conducting mud and a preparation method thereof, aiming at the problem of high oil permeability of the existing heat-conducting mud.
The technical scheme for solving the technical problems is as follows: the resin-free low-permeability oil heat conduction mud is characterized by comprising the following components in parts by weight: 11-30 parts of heat-conducting filler, 21-30 parts of heat-conducting filler, 31-30 parts of heat-conducting filler, 0.1-5 parts of coupling agent and 0.1-2 parts of antioxidant.
The particle size of the heat-conducting filler 1, the particle size of the heat-conducting filler 2 and the particle size of the heat-conducting filler 3 are 0.01-1000um, and the heat-conducting fillers are respectively selected from one or more of active crystal whisker silicon, magnesium oxide, titanium dioxide, aluminum oxide, aluminum hydroxide, zinc oxide, carbon black, diamond, copper powder, aluminum powder, gold powder or silver powder; the coupling agent is one or more of trimethyl aluminate, triisopropyl aluminate, tribenzyl chlorate, gamma- (methacryloyloxy) propyl trimethoxy silane, KH550, KH570, stearic acid, monthly silicic acid or adipic acid; the antioxidant is one or more of 2, 8-di-tert-butyl-4-methylphenol, butyl hydroxy anisol, propyl gallate, dibutyl hydroxy toluene, tert-butyl hydroquinone, dilauryl thiodipropionate and sodium sulfite.
The invention also relates to a preparation method of the resin-free low-permeability oil heat conduction mud, which comprises the following steps: weighing the raw materials according to the weight parts, sequentially adding the heat-conducting filler 1, the heat-conducting filler 2, the heat-conducting filler 3 and the coupling agent into a stirring kettle, heating and stirring for 160min at the rotating speed of 55-65rpm and the temperature of 80 ℃, then adding the antioxidant, and stirring for 30min at the rotating speed of 35-40rpm and the temperature of 150 ℃; scraping the wall, stirring for 120min, vacuumizing to remove bubbles, cooling the material to room temperature, vacuumizing, and stirring for 30min to obtain the product.
The invention has the beneficial effects that: the invention realizes low oil permeability by removing the silicone resin part in the conventional heat conduction, and improves the adhesive force between the filler and the filler by modifying the surface of the filler, so that the modified filler can be kneaded into a mass, thereby preparing the resin-free low oil permeability heat conduction mud which can be used for filling the gaps of radiators in the electronic industry, can be used for a long time at the temperature of minus 50-150 ℃, ensures low oil permeability, and improves the service life and stability of electronic elements.
Detailed Description
The present invention is described below with reference to examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
A preparation method of resin-free low-permeability oil heat conduction mud comprises the following steps: adding 25g of aluminum oxide, 10g of aluminum hydroxide, 30g of magnesium oxide and 5g of stearic acid into a stirring kettle, heating and stirring for 160 minutes at the rotation speed of 64rpm and the temperature of 80 ℃; then adding 1g of sodium sulfite, stirring for 30 minutes at the rotating speed of 36rpm and the temperature of 150 ℃; scraping wall, stirring for 120min, vacuumizing to remove bubbles, cooling to room temperature, stirring, vacuumizing, and continuously stirring for 30 min.
Example 2
A preparation method of resin-free low-permeability oil heat conduction mud comprises the following steps: taking 10g of aluminum powder, 15g of copper powder, 1g of carbon black and KH5704g, adding into a stirring kettle, heating and stirring for 160 minutes at the rotating speed of 55rpm and the temperature of 80 ℃; then adding 0.5g of 2, 8-di-tert-butyl-4-methylphenol, stirring for 30 minutes at the rotating speed of 39rpm and the temperature of 150 ℃; scraping wall, stirring for 120min, vacuumizing to remove bubbles, cooling to room temperature, stirring, vacuumizing, and continuously stirring for 30 min.
Example 3
A preparation method of resin-free low-permeability oil heat conduction mud comprises the following steps: adding 20g of zinc oxide, 35g of alumina, 1g of carbon black and KH5704g into a stirring kettle, heating and stirring for 160 minutes at the rotating speed of 55rpm and the temperature of 80 ℃; then adding 0.5g of 2, 8-di-tert-butyl-4-methylphenol, stirring for 30 minutes at the rotating speed of 39rpm and the temperature of 150 ℃; scraping wall, stirring for 120min, vacuumizing to remove bubbles, cooling to room temperature, stirring, vacuumizing, and continuously stirring for 30 min.
The resin-free low-permeability oil heat-conducting mud obtained in examples 1 to 3 was subjected to heat aging: aging for 1000h at 150 ℃; aging at high and low temperatures: 30min-40 ℃, 30min 125 ℃, and 1000 cycles; and (3) humid heat aging: 85%, RH85 deg.C, 1000h, the results are shown in tables 1 and 2. The aging experiment result shows that the heat conduction mud without resin and with low oil permeability has low oil permeability after aging, has small thermal resistance change before and after aging, and can be used for a long time at the temperature of between 50 ℃ below zero and 150 ℃.
TABLE 1 aged oil bleeding value test results
TABLE 2 aged Heat conduction test results
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. The resin-free low-permeability oil heat conduction mud is characterized by comprising the following components in parts by weight: 11-30 parts of heat-conducting filler, 21-30 parts of heat-conducting filler, 31-30 parts of heat-conducting filler, 0.1-5 parts of coupling agent and 0.1-2 parts of antioxidant.
2. The resin-free low-permeability oil heat-conducting mud as claimed in claim 1, wherein the particle size of the heat-conducting filler 1, the heat-conducting filler 2 and the heat-conducting filler 3 is 0.01-1000um, and the particle size is respectively selected from one or more of active whisker silicon, magnesium oxide, titanium dioxide, aluminum oxide, aluminum hydroxide, zinc oxide, carbon black, diamond, copper powder, aluminum powder, gold powder or silver powder.
3. The resin-free oil-permeable heat transfer mud according to claim 1, wherein the coupling agent is one or more of trimethyl aluminate, triisopropyl aluminate, tribenzyl chlorate, gamma- (methacryloyloxy) propyl trimethoxysilane, KH550, KH570, stearic acid, lauric acid, or adipic acid.
4. The resin-free low-permeability oil thermal mud according to claim 1, wherein the antioxidant is one or more of 2, 8-di-tert-butyl-4-methylphenol, butyl hydroxyanisole, propyl gallate, dibutyl hydroxytoluene, tert-butyl hydroquinone, dilauryl thiodipropionate, and sodium sulfite.
5. A method for preparing the resin-free low-permeability oil thermal mud according to any one of claims 1 to 4, characterized by comprising the steps of: weighing the raw materials according to the weight parts, sequentially adding the heat-conducting filler 1, the heat-conducting filler 2, the heat-conducting filler 3 and the coupling agent into a stirring kettle, heating and stirring for 160min at the rotating speed of 55-65rpm and the temperature of 80 ℃, then adding the antioxidant, and stirring for 30min at the rotating speed of 35-40rpm and the temperature of 150 ℃; scraping the wall, stirring for 120min, vacuumizing to remove bubbles, cooling the material to room temperature, vacuumizing, and stirring for 30min to obtain the product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911406108.XA CN111073612A (en) | 2019-12-31 | 2019-12-31 | Resin-free low-permeability oil heat conduction mud and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911406108.XA CN111073612A (en) | 2019-12-31 | 2019-12-31 | Resin-free low-permeability oil heat conduction mud and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111073612A true CN111073612A (en) | 2020-04-28 |
Family
ID=70320350
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911406108.XA Pending CN111073612A (en) | 2019-12-31 | 2019-12-31 | Resin-free low-permeability oil heat conduction mud and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111073612A (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1288921A (en) * | 2000-10-24 | 2001-03-28 | 华东理工大学 | Self-curing inorganic heat-conducting daub |
| AU2003219120A1 (en) * | 2002-04-27 | 2003-11-17 | Merck Patent Gmbh | Surface modification of phase change materials |
| CN101205459A (en) * | 2006-12-19 | 2008-06-25 | 成都市兴岷江电热电器有限责任公司 | Curing type heat-conducting daub |
| CN102533130A (en) * | 2010-12-07 | 2012-07-04 | 上海务宝机电科技有限公司 | Waterproof self-curing inorganic heat-conducting cement |
| CN106085252A (en) * | 2016-06-21 | 2016-11-09 | 北京派诺蒙能源科技有限公司 | A kind of heat-conducting daub and its preparation method and application |
| CN106753263A (en) * | 2016-12-27 | 2017-05-31 | 深圳德邦界面材料有限公司 | Heat conduction phase-change material and preparation method thereof |
| CN107474451A (en) * | 2017-09-22 | 2017-12-15 | 南京肯特复合材料股份有限公司 | Corrosion-resistant rotating shaft sealing ring PTFE resin composite and preparation method thereof |
| CN107987536A (en) * | 2018-01-04 | 2018-05-04 | 楼旭娟 | A kind of high heat conductive insulating silica gel piece and preparation method thereof |
| CN108003625A (en) * | 2017-12-21 | 2018-05-08 | 深圳市东成电子有限公司 | Low hypotonic oily heat-conducting silicone grease filler of volatilization and preparation method thereof |
| CN108624056A (en) * | 2018-05-09 | 2018-10-09 | 华东理工大学 | A kind of High thermal-conductive silicone grease boundary material and preparation method thereof |
| CN209325421U (en) * | 2018-12-25 | 2019-08-30 | 北京派诺蒙能源科技有限公司 | A kind of outer heating device of sulphur conveyance conduit |
-
2019
- 2019-12-31 CN CN201911406108.XA patent/CN111073612A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1288921A (en) * | 2000-10-24 | 2001-03-28 | 华东理工大学 | Self-curing inorganic heat-conducting daub |
| AU2003219120A1 (en) * | 2002-04-27 | 2003-11-17 | Merck Patent Gmbh | Surface modification of phase change materials |
| CN101205459A (en) * | 2006-12-19 | 2008-06-25 | 成都市兴岷江电热电器有限责任公司 | Curing type heat-conducting daub |
| CN102533130A (en) * | 2010-12-07 | 2012-07-04 | 上海务宝机电科技有限公司 | Waterproof self-curing inorganic heat-conducting cement |
| CN106085252A (en) * | 2016-06-21 | 2016-11-09 | 北京派诺蒙能源科技有限公司 | A kind of heat-conducting daub and its preparation method and application |
| CN106753263A (en) * | 2016-12-27 | 2017-05-31 | 深圳德邦界面材料有限公司 | Heat conduction phase-change material and preparation method thereof |
| CN107474451A (en) * | 2017-09-22 | 2017-12-15 | 南京肯特复合材料股份有限公司 | Corrosion-resistant rotating shaft sealing ring PTFE resin composite and preparation method thereof |
| CN108003625A (en) * | 2017-12-21 | 2018-05-08 | 深圳市东成电子有限公司 | Low hypotonic oily heat-conducting silicone grease filler of volatilization and preparation method thereof |
| CN107987536A (en) * | 2018-01-04 | 2018-05-04 | 楼旭娟 | A kind of high heat conductive insulating silica gel piece and preparation method thereof |
| CN108624056A (en) * | 2018-05-09 | 2018-10-09 | 华东理工大学 | A kind of High thermal-conductive silicone grease boundary material and preparation method thereof |
| CN209325421U (en) * | 2018-12-25 | 2019-08-30 | 北京派诺蒙能源科技有限公司 | A kind of outer heating device of sulphur conveyance conduit |
Non-Patent Citations (3)
| Title |
|---|
| 于占江等: "《摩擦材料生产工艺》", 31 January 2018, 天津大学出版社 * |
| 周大纲: "《土工合成材料制造技术及性能》", 30 April 2019, 中国轻工业出版社 * |
| 邹海仲等: "复合粉体制备导热吸波材料及其表征", 《高分子材料科学与工程》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111286299B (en) | Bi-component condensed type encapsulating material convenient for construction and preparation method thereof | |
| CN110317581A (en) | A kind of pureed thermostable heat-conductive composite material and preparation method | |
| CN106634809B (en) | Anti-poisoning anti-settling high-bonding heat-conducting silica gel for packaging LED power supply | |
| CN114032063B (en) | High-heat-conductivity low-viscosity bi-component organic silicon pouring sealant and preparation method thereof | |
| CN112812570B (en) | Low-volatility double-crosslinking heat-conducting phase-change gel and preparation method thereof | |
| CN105419672A (en) | Preparation method of high-heat-dissipation electric-conductive glue used for high-power LED | |
| JP2013126925A (en) | Silica particle, method for producing the same, and paste for semiconductor packaging | |
| CN103409115A (en) | Enhanced heat conducting interface material and preparation method thereof | |
| CN112322042A (en) | High-thermal-conductivity single-component heat-conducting gel and preparation method thereof | |
| CN102675601A (en) | Low-warpage epoxy resin composite used for QFN (Quad Flat No Lead) | |
| CN102850724A (en) | Green and environment-friendly epoxy resin composition for high-power device packaging | |
| CN110724869A (en) | High-thermal-conductivity leakproof heat conduction material and preparation method and application thereof | |
| CN114574154A (en) | Low-viscosity two-component heat-conducting pouring sealant and preparation method thereof | |
| CN111073612A (en) | Resin-free low-permeability oil heat conduction mud and preparation method thereof | |
| CN113773649A (en) | High-reliability low-viscosity high-heat-conductivity heat-conducting gel and preparation method and application thereof | |
| CN104194716A (en) | Low-light-attenuation organic silicon crystal solidification adhesive for high-power COB (chip on board) packaging | |
| CN109880541A (en) | Can rapid curing and have high-adhesive-strength Heat Conduction Material | |
| CN115895269B (en) | Heat-conducting gel and preparation method and application thereof | |
| CN110364648B (en) | New energy lithium battery radiating gasket and preparation method thereof | |
| CN107828386A (en) | One kind has vulcanized by moisture shaping one pack system high heat conduction calking boundary material and preparation method thereof | |
| CN103146139A (en) | Epoxy resin composition for electronic parts encapsulation and electronic parts-equipped device using the same | |
| WO2019017053A1 (en) | Resin composition for sealing sheet, sealing sheet and semiconductor device | |
| CN114621726A (en) | Low-density ultrahigh-fluidity heat-conducting pouring sealant and preparation method thereof | |
| CN114921057B (en) | Epoxy plastic package material composition, preparation method and application | |
| CN102863744A (en) | High-power packaging epoxy resin composition with good forming performances |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200428 |
|
| RJ01 | Rejection of invention patent application after publication |