CN102241965A - Heat-conductive silicone grease paste and its preparation method - Google Patents
Heat-conductive silicone grease paste and its preparation method Download PDFInfo
- Publication number
- CN102241965A CN102241965A CN2011101214771A CN201110121477A CN102241965A CN 102241965 A CN102241965 A CN 102241965A CN 2011101214771 A CN2011101214771 A CN 2011101214771A CN 201110121477 A CN201110121477 A CN 201110121477A CN 102241965 A CN102241965 A CN 102241965A
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- CN
- China
- Prior art keywords
- heat
- silicone grease
- filler
- preparation
- paste
- 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.)
- Granted
Links
- 239000004519 grease Substances 0.000 title claims abstract description 21
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 13
- 239000010949 copper Substances 0.000 claims abstract description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011787 zinc oxide Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 4
- 239000000945 filler Substances 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 239000006071 cream Substances 0.000 claims description 9
- 239000006210 lotion Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 229910017083 AlN Inorganic materials 0.000 claims description 6
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004898 kneading Methods 0.000 claims description 2
- 230000005855 radiation Effects 0.000 abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 230000032683 aging Effects 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000009413 insulation Methods 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000796 flavoring agent Substances 0.000 abstract 1
- 235000019634 flavors Nutrition 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 230000035939 shock Effects 0.000 abstract 1
- 230000001404 mediated effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000004577 thatch Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a heat-conductive silicone grease paste and its preparation method, and the method is characterized in that a powder filling material is mixed with aluminum nitride, zinc oxide, nanometer copper and organic silicone grease according to a certain ratio to prepare the paste. According to the invention, the nanometer level alumina coated copper powder is taken as the filling material, the prepared heat conductive silicone grease has the characteristics of no drying, no hardness and no melting under the condition of high temperature for long time, and has no flavor and no odor, no corrosion effect to metals such as iron, copper and aluminum. The invention has advantages of excellent electrical performance, insulation, moisture resistance, shock resistance, radiation resistance and aging resistance, and the heat conduction speed of the electron and electric appliance to a heat radiator can be accelerated, so that the heat radiation efficiency can be improved.
Description
Technical field
The present invention relates to a kind of heat-conducting silicone grease lotion and preparation method thereof.
Background technology
Whole world illumination association is illustrated in the foreseeable future, and large-power light-emitting diodes (Powerlight-emittingdiodes) will play crucial effects in the general lighting field.Since nineteen ninety-four, great power LED obtains fast development, has replaced conventional light source at numerous areas (as street lamp, automobile tail light, LCD backlight etc.).In recent years, the development of LED technology is maked rapid progress especially, and extra large thatch (Haitz) law that is similar to Moore's Law is obeyed in the lifting of its light efficiency and the decline of device cost, and promptly the LED price was reduced to originally 1/10 in per 10 years, and performance then improves 20 times.
The LED technology develops to high-power, high brightness, high-level efficiency, low-cost direction in the world.The optical characteristics of power LED and electrology characteristic depend on junction temperature strongly.Along with the increase of LED power, too high junction temperature can influence life-span and the reliability of LED, and it is increasingly serious that heat dissipation problem becomes.
The heat radiation of LED is more and more paid attention to by people now, and this is that the bad junction temperature of dispelling the heat is just high because the light decay of LED or its life-span are directly relevant with its junction temperature, and the life-span is weak point just, can prolong 2 times according to 10 ℃ of life-spans of the every reduction of A Leiniusi rule temperature.Compare with other lamp source, can produce serious heat dissipation problem, this mainly is because not by dispelling the heat.Generally speaking, the power consumption that is used for LED has 75%~85% finally to be converted to heat energy, and too much heat can reduce the light output of LED and produce colour cast, quickens LED and wears out.If with junction temperature is that 25 luminous when spending are 100%, junction temperature rises to 60 when spending so, and its luminous quantity just has only 90%; Junction temperature is 100 just to drop to 80% when spending; 140 degree just have only 70%.As seen improve heat radiation, the control junction temperature is crucial thing.The heating of LED can make that also its spectrum moves in addition; Colour temperature raises; Forward current increases (during the constant voltage power supply); Reversible circulation also increases; Variety of problems such as thermal stresses increases, thus, the heat radiation of LED is an of paramount importance problem in the design of LED light fixture.The characteristics of led chip are at the high heat of minimum volume generation.And the thermal capacity of LED itself is very little, thus must conduct these heats with the fastest speed, otherwise will produce very high junction temperature.After the led chip encapsulation, the thermal resistance from the chip to the pin is exactly a most important thermal resistance when using, and in general, the size of the face that the connects area of chip is the key of heat radiation, for different rated output, requires to have the face that the connects area of corresponding size.
Use the better heat abstractor of thermal conductivity, be decreased to the thermal resistance of environment, control LED internal temperature is unlikely high more too many than envrionment temperature, but this needs higher cost.In addition, the problem that is difficult to avoid is, after heat abstractor uses for some time, on the radiator element of lamp body shell, deposit dust, and aging the coming unstuck of medium layer that connects copper layer and aluminium base on the Al-alloy based copper clad plate will cause all thermal resistance to rise greatly, cause the integral heat sink degradation.
Summary of the invention
In order to reach less thermal resistance, improve the purpose of thermal conductivity, the invention provides a kind of heat-conducting silicone grease lotion and preparation method thereof.
The present invention adopts following technical scheme to achieve these goals:
The heat-conducting silicone grease lotion is characterized in that the weight ratio of its constitutive material is: powder filler 10-75%, aluminium nitride 5-45%, zinc oxide 0-10%, organic silicone grease 15-30%, nanometer copper 1-20%.
Described heat-conducting silicone grease lotion is characterized in that described powder filler is the alumina powder jointed filler of cupric 20%.
The preparation method of described heat-conducting silicone grease lotion is characterized in that may further comprise the steps:
(1) preparation powder filler: with AI (NO
3)
3.9HO with citric acid in molar ratio 1: the 1.2-1.5 proportioning is soluble in water, uses dense HNO
3Or dense NH
3H
2The O regulator solution is 3-4 to PH, colourless transparent solution, add nanometer copper by the weight ratio of raw material then and be uniformly dispersed, after filtration, evaporation, vacuum-drying, at 550-580 ℃ of roasting 10h, the alumina powder jointed filler of cupric 20%;
(2) will make powder filler, aluminium nitride, zinc oxide, organic silicone grease, nanometer copper by oneself by the weight ratio of raw material and add kneader and under the kneading state, mix, make the paste heat-conducting cream.
Beneficial effect of the present invention:
It is filler that the present invention adopts alumina in Nano level to coat copper powder, and the heat-conducting silicone grease of preparation has at long-time 280 ℃, in addition the high temperature more than 280 ℃ reveal put also do not do, not hard, insoluble, and tasteless, odorless does not all have corrosive nature to metals such as iron, copper, aluminium; Have excellent electric property, insulation, moistureproof, shockproof, radiation hardness is aging etc., and can accelerate electronics, the electrical equipment heat conduction velocity to heat abstractor, thereby the characteristics of raising radiating efficiency.
Embodiment
Preparation powder filler: with AI (NO
3)
3.9HO with citric acid in molar ratio 1: the 1.2-1.5 proportioning is soluble in water, uses dense HNO
3Or dense NH
3H
2The O regulator solution is 3-4 to PH, colourless transparent solution, add nanometer copper by the weight ratio of raw material then and be uniformly dispersed, after filtration, evaporation, vacuum-drying, at 550-580 ℃ of roasting 10h, the alumina powder jointed filler of cupric 20%, stand-by;
Embodiment 1
Earlier each component is mediated in kneader by following prescription (mass parts), on three-roll grinder, disperse then, mix and make the paste heat-conducting cream.
Powder filler 75%
Organic silicone grease 25%
Embodiment 2
Earlier each component is mediated in kneader by following prescription (mass parts), on three-roll grinder, disperse then, mix and make the paste heat-conducting cream.
Powder filler 52%
Aluminium nitride 25%
Organic silicone grease 23%
Embodiment 3
Earlier each component is mediated in kneader by following prescription (mass parts), on three-roll grinder, disperse then, mix and make the paste heat-conducting cream.
Embodiment 4
Earlier each component is mediated in kneader by following prescription (mass parts), on three-roll grinder, disperse then, mix and make the paste heat-conducting cream.
Embodiment 5
Earlier each component is mediated in kneader by following prescription (mass parts), on three-roll grinder, disperse then, mix and make the paste heat-conducting cream.
Embodiment 6
Earlier each component is mediated in kneader by following mass parts, on three-roll grinder, disperse then, mix and make the paste heat-conducting cream: powder filler 45%, aluminium nitride 25%, zinc oxide 5%, organic silicone grease 15%, nanometer copper 10%.
More than the prepared heat-conducting cream of each embodiment be the thermal conduction chemicals, can maximize the thermal conduction between semiconductor piece and the scatterer; Be exposed to for a long time under the hot environment and also can not harden; Environment-protecting asepsis; Have remarkable electrical insulation capability, but automated operation and silk screen printing.All can reach heat-conduction coefficient ThermalConductivity>4.5W/M.K thermal impedance Thermal Impedance<0.067 ℃-in2/W.
Claims (3)
1. a heat-conducting silicone grease lotion is characterized in that the weight ratio of its constitutive material is: powder filler 10-75%, aluminium nitride 5-45%, zinc oxide 0-10%, organic silicone grease 15-30%, nanometer copper 1-20%.
2. heat-conducting silicone grease lotion according to claim 1 is characterized in that described powder filler is the alumina powder jointed filler of cupric 20%.
3. the preparation method of heat-conducting silicone grease lotion according to claim 1 is characterized in that may further comprise the steps:
(1) preparation powder filler: with AI (NO
3)
3.9HO with citric acid in molar ratio 1: the 1.2-1.5 proportioning is soluble in water, uses dense HNO
3Or dense NH
3H
2The O regulator solution is 3-4 to PH, colourless transparent solution, add nanometer copper by the weight ratio of raw material then and be uniformly dispersed, after filtration, evaporation, vacuum-drying, at 550-580 ℃ of roasting 10h, the alumina powder jointed filler of cupric 20%;
(2) will make powder filler, aluminium nitride, zinc oxide, organic silicone grease, nanometer copper by oneself by the weight ratio of raw material and add kneader and under the kneading state, mix, make the paste heat-conducting cream.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 201110121477 CN102241965B (en) | 2011-05-12 | 2011-05-12 | Heat-conductive silicone grease paste and its preparation method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 201110121477 CN102241965B (en) | 2011-05-12 | 2011-05-12 | Heat-conductive silicone grease paste and its preparation method |
Publications (2)
Publication Number | Publication Date |
---|---|
CN102241965A true CN102241965A (en) | 2011-11-16 |
CN102241965B CN102241965B (en) | 2013-08-07 |
Family
ID=44960218
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN 201110121477 Expired - Fee Related CN102241965B (en) | 2011-05-12 | 2011-05-12 | Heat-conductive silicone grease paste and its preparation method |
Country Status (1)
Country | Link |
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CN (1) | CN102241965B (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103772993A (en) * | 2014-01-26 | 2014-05-07 | 一远电子科技有限公司 | High thermal conductivity nano-copper heat conducting silicon grease and preparation method thereof |
CN104974555A (en) * | 2015-06-27 | 2015-10-14 | 铜陵铜基粉体科技有限公司 | Spherical copper powder with corrosion resistance and excellent thermal stability, and preparation method thereof |
CN105524550A (en) * | 2016-01-22 | 2016-04-27 | 何挺 | Heat-conducting silicone grease and manufacturing method thereof |
CN109659281A (en) * | 2019-01-29 | 2019-04-19 | 中南大学 | A kind of high thermal conductivity electronic packaging composite material and preparation method thereof |
CN110358146A (en) * | 2018-04-10 | 2019-10-22 | 博世汽车部件(苏州)有限公司 | The copper nano-wire of alumina-coated, heat conductive silica gel and preparation method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101932684A (en) * | 2008-01-30 | 2010-12-29 | 道康宁东丽株式会社 | Thermally conductive silicone grease composition |
-
2011
- 2011-05-12 CN CN 201110121477 patent/CN102241965B/en not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101932684A (en) * | 2008-01-30 | 2010-12-29 | 道康宁东丽株式会社 | Thermally conductive silicone grease composition |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103772993A (en) * | 2014-01-26 | 2014-05-07 | 一远电子科技有限公司 | High thermal conductivity nano-copper heat conducting silicon grease and preparation method thereof |
CN104974555A (en) * | 2015-06-27 | 2015-10-14 | 铜陵铜基粉体科技有限公司 | Spherical copper powder with corrosion resistance and excellent thermal stability, and preparation method thereof |
CN105524550A (en) * | 2016-01-22 | 2016-04-27 | 何挺 | Heat-conducting silicone grease and manufacturing method thereof |
CN110358146A (en) * | 2018-04-10 | 2019-10-22 | 博世汽车部件(苏州)有限公司 | The copper nano-wire of alumina-coated, heat conductive silica gel and preparation method thereof |
CN109659281A (en) * | 2019-01-29 | 2019-04-19 | 中南大学 | A kind of high thermal conductivity electronic packaging composite material and preparation method thereof |
Also Published As
Publication number | Publication date |
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CN102241965B (en) | 2013-08-07 |
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Granted publication date: 20130807 Termination date: 20190512 |