CN107955375A - Thermally conductive silicone rubber composite material and preparation method thereof - Google Patents
Thermally conductive silicone rubber composite material and preparation method thereof Download PDFInfo
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- CN107955375A CN107955375A CN201711258571.5A CN201711258571A CN107955375A CN 107955375 A CN107955375 A CN 107955375A CN 201711258571 A CN201711258571 A CN 201711258571A CN 107955375 A CN107955375 A CN 107955375A
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2201/011—Nanostructured additives
Abstract
The present invention provides a kind of preparation method of thermally conductive silicone rubber composite material, its step includes：Filler is uniformly mixed with liquid silastic, adds auxiliary agent, is ground, cures, the thermally conductive silicone rubber composite material is prepared, the filler is nano silver coated aluminum oxide.The present invention also provides a kind of thermally conductive silicone rubber composite material.The thermally conductive silicone rubber composite material of the offer of the present invention can greatly improve the thermal conductivity of material on the premise of identical cost, and reduce the hardness of material.The preparation method is added without harmful poisonous raw material, and simple process and low cost is good in economic efficiency.
Description
Technical field
The present invention relates to silastic material field, more particularly to a kind of thermally conductive silicone rubber composite material and preparation method thereof.
Background technology
In recent years, with hydrid integrated circuit (IC) and electronic building brick transistor, IC, memory component etc. are installed
Printed circuit board (PCB) density and integrated level raising, heat-conducting silicon rubber be used to making heat extremely efficient from these electronic building bricks
In the purpose dispersed.The heat conductivility of usual silicone rubber is poor, and thermal conductivity usually only has 0.1-0.2W/mK or so, and addition is led
Hot filler can improve the heat conductivility of silicon rubber.But as the increase of heat filling, the thermal conductivity of silastic material increase, but
Hardness is consequently increased at the same time, this is unfavorable for giving full play to silastic material connection heat source and heat sink heat transfer path.
The content of the invention
In view of this, it is necessary to provide it is a kind of with high-efficiency heat conduction ability, soft thermally conductive silicone rubber composite material and
Its preparation method.
One aspect of the present invention provides a kind of preparation method of thermally conductive silicone rubber composite material, its step includes：
Filler is uniformly mixed with liquid silastic, adds auxiliary agent, is ground, cures, the heat-conducting silicon rubber is prepared
Composite material, the filler are nano silver coated aluminum oxide.
Another aspect of the present invention provides thermally conductive silicone rubber composite material prepared by a kind of above method, including following parts by weight
Several following components：
3-5 parts of silicone rubber matrix；
20-30 parts of nano silver coated aluminum oxide.
The thermally conductive silicone rubber composite material of the offer of the present invention can greatly improve material on the premise of identical cost
Thermal conductivity, and reduce the hardness of material.The preparation method is added without harmful poisonous raw material, simple process and low cost,
It is good in economic efficiency.
Brief description of the drawings
Fig. 1 is the electron microscope of alumina particle section in comparative example 1 of the present invention.
Fig. 2 is the electron microscope of composite products section in comparative example 1 of the present invention.
Fig. 3 is the electron microscope of silver-plated alumina particle section in the embodiment of the present invention 1.
Fig. 4 is the electron microscope of composite products section in the embodiment of the present invention 1.
Main element symbol description
Nothing
Following embodiment will combine above-mentioned attached drawing and further illustrate the present invention.
Embodiment
The technical solution in the embodiment of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that
Described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, those of ordinary skill in the art's all other embodiments obtained without making creative work, belongs to
The scope of protection of the invention.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The normally understood implication of technical staff is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein " and/or " include one or more phases
The arbitrary and all combination of the Listed Items of pass.
In the case where there is no conflict, the feature in following embodiment and embodiment can be mutually combined.
The present invention provides a kind of preparation method of thermally conductive silicone rubber composite material.Although for the sake of clarity, this method quilt
Be portrayed as a series of numbered step, but number might not deciding step order.It should be appreciated that some steps can
To be skipped, implement at the same time, or need not be stringent implement according to putting in order.However, in general, shown in the method follows
The numerical order of step.
The preparation method of the thermally conductive silicone rubber composite material includes the following steps：
Filler, be uniformly mixed by S1 with liquid silastic, and the filler is nano silver coated aluminum oxide；
S2, add auxiliary agent；
S3, grinding, cure.
According to a particular embodiment of the invention, the nano silver coated aluminum oxide is made by following steps：
S11, sensitized treatment：Aluminium oxide will be added in the hydrochloric acid solution of stannous chloride, stirred, separation of solid and liquid, is sensitized
Aluminium oxide after processing；
S12, activation process：Aluminium oxide after the sensitized treatment is added in the hydrochloric acid solution of palladium bichloride, is stirred, Gu
Liquid separates, and obtains the aluminium oxide after activation process；
S13, silver-colored cladding process：Ammonium hydroxide is added dropwise in silver nitrate solution, silver ammino solution is made；By the wine of glucose
Aluminium oxide after stone acid mixed solution, activation process is added in the silver ammino solution, stirring, separation of solid and liquid, obtains described receive
The silver-colored coated aluminum oxide of rice.
According to a particular embodiment of the invention, in sensitized treatment, stannous oxide in the hydrochloric acid solution of the stannous chloride
Molar ratio with hydrochloric acid is 1:The solid-to-liquid ratio of 10-12, the aluminium oxide and the hydrochloric acid solution of the stannous chloride is 1:10-15.
In sensitized treatment step, stannous oxide forms one layer of liquid film with reduction in chlorination aluminium surface.In follow-up activation
In processing, the tin ion in this liquid film will be reacted with palladium ion, that is, follow-up reaction will be limited at aluminium oxide table
On face, rather than in solution.
According to a particular embodiment of the invention, in activation process, palladium bichloride and salt in the hydrochloric acid solution of the palladium bichloride
The molar ratio of acid is 3-5:100, the solid-to-liquid ratio of aluminium oxide and the hydrochloric acid solution of the palladium bichloride after the sensitized treatment is 1:
10-15.In the activation process step, tin ion reduces palladium ion, forms palladium particle, is deposited on oxidation aluminium surface and is formed
Even activation point, so that follow-up Argent grain can be uniformly wrapped in forming process in oxidation aluminium surface.
According to a particular embodiment of the invention, glucose and tartaric acid rub in the tartaric acid mixed solution of the glucose
Your ratio is 8-10:1, the silver ammino solution, the tartaric acid mixed solution of glucose and the ratio of the aluminium oxide after activation process are 5-
6:1。
According to a particular embodiment of the invention, the silver-colored cladding process further comprises, is received what is obtained after separation of solid and liquid
Processing is dried in the silver-colored coated aluminum oxide of rice, obtains nano silver coated aluminum oxide particle powder.Dry use is dried in vacuo,
Drying temperature is 60-80 DEG C, dry 8-10h.
According to a particular embodiment of the invention, the auxiliary agent includes but not limited to containing hydrogen silicone oil, platinum catalyst.It is described hydrogeneous
Silicone oil is used to linear silicon xanthan molecule being crosslinked adult form silicon rubber.The platinum catalyst is used to be catalyzed above-mentioned silica gel deformation reaction.
According to a particular embodiment of the invention, the containing hydrogen silicone oil addition is the 2% of silicon rubber quality, the platinum catalysis
Agent addition is less than the 0.1% of filler and silicon rubber total content.
According to a particular embodiment of the invention, it is described to be ground to mechanical lapping, include but not limited to ball milling, optics is ground
Mill, stuccoing grinding etc..
According to a particular embodiment of the invention, the curing refers in liquid silastic, adds certain proportion Silicon Containing Hydrogen
Oil, places 1h at 120 DEG C, and in the process, line style silicon rubber molecule forms build molecule, table by containing hydrogen silicone oil molecule cross-link
It is now that solid block material is changed into from viscous state substance.
The present invention also provides a kind of thermally conductive silicone rubber composite material prepared such as the above method, including following parts by weight
Following component：
3-5 parts of silicone rubber matrix：
20-30 parts of nano silver coated aluminum oxide.
According to a particular embodiment of the invention, the thermally conductive silicone rubber composite material includes the component of following parts by weight：
3.3 parts of silicone rubber matrix：
20 parts of nano silver coated aluminum oxide.
According to a particular embodiment of the invention, the thermal conductivity of the thermally conductive silicone rubber composite material is 1-2W/mK.It is preferred that
, the thermal conductivity of the thermally conductive silicone rubber composite material is 1.6W/mK.
Below by specific embodiment, the present invention is described further.
Embodiment 1
(1) sensitized treatment process.13g micron order alumina powders are weighed, prepare the aqueous solution of stannous chloride and hydrochloric acid
200mL, wherein concentration are respectively stannous chloride 0.05mol/L, hydrochloric acid 0.6mol/L, pour into aluminium oxide 13g, stir 20min, mistake
Filter, and be washed with deionized one time.
(2) activated process.The aqueous solution 200mL of palladium bichloride and hydrochloric acid is prepared, wherein concentration is respectively palladium bichloride
0.003mol/L, hydrochloric acid 0.1mol/L, add the aluminium oxide after sensitized treatment, stir 20min, filtering, and be washed with deionized water
Wash one time.
(3) Argent grain process is grown.Dose volume fraction is 10% ammonia spirit 20mL, this is solution A；Prepare
The silver nitrate solution 100mL of 0.1mol/L, this is solution B；Agitating solution B, is gradually added dropwise to A in B, can produce brown and sink
Form sediment, be persistently added dropwise to untill brown precipitate just disappears, obtain solution C at this time；Glucose and tartaric acid solution 100mL are prepared,
Wherein concentration of glucose is 0.2mol/L, tartaric acid concentration 0.025mol/L, pours into solution C thereto and by activation process
Alumina powder afterwards, under lasting stirring, reaction carries out 5h, filtering, and is washed with deionized one time, 60 DEG C of vacuum dryings
8h, that is, obtain nano silver coated aluminum oxide particle powder.
(4) silicon rubber composite material process is prepared.20 parts of silver-plated alumina packings are mixed with 3.3 parts of liquid silastics,
2% containing hydrogen silicone oil and 0.05% platinum catalyst is added, with three-roll grinder batch mixing 20min, is transferred in molding die,
120 degree of lower curing 1h, are prepared into thermally conductive silicone rubber composite material.
The thermally conductive silicone rubber composite material prepared by the above method, wherein 4 parts of silicon rubber matrix, nano silver cladding oxygen
Change 25 parts of aluminium.The thermally conductive silicone rubber composite material thermal conductivity is 1.6W/mK after tested.
Embodiment 2
(1) sensitized treatment process.30g micron order alumina powders are weighed, prepare the aqueous solution of stannous chloride and hydrochloric acid
360mL, pours into aluminium oxide 36g, stirs 20min, filtering, and be washed with deionized one time.
(2) activated process.The aqueous solution 300mL of palladium bichloride and hydrochloric acid is prepared, wherein concentration is respectively palladium bichloride
0.004mol/L, hydrochloric acid 0.2mol/L, add the aluminium oxide after sensitized treatment, stir 20min, filtering, and be washed with deionized water
Wash one time.
(3) Argent grain process is grown.Dose volume fraction is 10% ammonia spirit 20mL, this is solution A；Prepare
The silver nitrate solution 100mL of 0.1mol/L, this is solution B；Agitating solution B, is gradually added dropwise to A in B, can produce brown and sink
Form sediment, be persistently added dropwise to untill brown precipitate just disappears, obtain solution C at this time；Glucose and tartaric acid solution 100mL are prepared,
Wherein concentration of glucose is 0.2mol/L, tartaric acid concentration 0.025mol/L, pours into solution C thereto and by activation process
Alumina powder afterwards, under lasting stirring, reaction carries out 5h, filtering, and is washed with deionized one time, 70 DEG C of vacuum dryings
10h, that is, obtain nano silver coated aluminum oxide particle powder.
(4) silicon rubber composite material process is prepared.30 parts of silver-plated alumina packings are mixed with 4 parts of liquid silastics, are added
Enter 3% containing hydrogen silicone oil and 0.1% platinum catalyst, with three-roll grinder batch mixing 20min, be transferred in molding die, 120
Degree is lower to cure 1h, is prepared into heat conductive silica gel gasket.
The thermally conductive silicone rubber composite material prepared by the above method, wherein 5 parts of silicon rubber matrix, nano silver cladding oxygen
Change 30 parts of aluminium.The thermally conductive silicone rubber composite material thermal conductivity is 2W/mK after tested.
Embodiment 3
(1) sensitized treatment process.30g micron order alumina powders are weighed, prepare the aqueous solution of stannous chloride and hydrochloric acid
330mL, pours into aluminium oxide 28g, stirs 20min, filtering, and be washed with deionized one time.
(2) activated process.The aqueous solution 200mL of palladium bichloride and hydrochloric acid is prepared, wherein concentration is respectively palladium bichloride
0.003mol/L, hydrochloric acid 0.1mol/L, add the aluminium oxide after sensitized treatment, stir 20min, filtering, and be washed with deionized water
Wash one time.
(3) Argent grain process is grown.Dose volume fraction is 10% ammonia spirit 20mL, this is solution A；Prepare
The silver nitrate solution 100mL of 0.1mol/L, this is solution B；Agitating solution B, is gradually added dropwise to A in B, can produce brown and sink
Form sediment, be persistently added dropwise to untill brown precipitate just disappears, obtain solution C at this time；Glucose and tartaric acid solution 100mL are prepared,
Wherein concentration of glucose is 0.2mol/L, tartaric acid concentration 0.025mol/L, pours into solution C thereto and by activation process
Alumina powder afterwards, under lasting stirring, reaction carries out 5h, filtering, and is washed with deionized one time, 80 DEG C of vacuum dryings
9h, that is, obtain nano silver coated aluminum oxide particle powder.
(4) silicon rubber composite material process is prepared.20 parts of silver-plated alumina packings are mixed with 3 parts of liquid silastics, are added
Enter 2% containing hydrogen silicone oil and 0.05% platinum catalyst, with three-roll grinder batch mixing 20min, be transferred in molding die,
120 degree of lower curing 1h, are prepared into heat conductive silica gel gasket.
The thermally conductive silicone rubber composite material prepared by the above method, wherein 3 parts of silicon rubber matrix, nano silver cladding oxygen
Change 20 parts of aluminium.The thermally conductive silicone rubber composite material thermal conductivity is 1.8W/mK after tested.
Comparative example 1
20 parts of raw alumina fillers are mixed with 4 parts of liquid silastics, appropriate amount of addition agent are added, with three-roll grinder batch mixing
20 minutes, it is transferred in molding die, cures 1h under 120 degree, is prepared into heat conductive silica gel material.
Heat conductive silica gel material thermal conductivity is 1.3W/mK after tested.
The thermal conductivity of pure silicone rubber material is 0.12W/mK.
The product of the product of comparative example 1 and embodiment 1 is compared into discovery, the composite products thermal conductivity in embodiment 1
For 1.6W/mK, and the composite products thermal conductivity in comparative example 1 is 1.3W/mK.Secondly, the composite material production in embodiment 1
The hardness of thing is 60, and the hardness of the composite products in comparative example 1 is 65.The product hardness of embodiment 1 is than comparative example 1
Product is low, but thermal conductivity will height.So this technology can improve silicon rubber composite material in aluminium oxide electroplate
Thermal conductivity, while reduce material hardness.
Further, referring to Fig. 1-4, the electron microscope of 1 product of 1 product of comparative example and embodiment.
From Fig. 1-2 it can be seen that alumina raw material particle surface is largely smooth, fraction is slightly coarse, carries some lines
Road, this is conducive to silver in oxidation aluminium surface forming core and crystalline growth.From Fig. 3 and 4 as can be seen that nano-Ag particles are uniformly grown
In oxidation aluminium surface, and largely oxidation aluminium surface is covered with Argent grain, illustrates aluminium oxide whole table in the composite
The combination power of face and matrix is stronger, and then improves the thermal conductivity of composite material.And Argent grain soilless sticking phenomenon, Argent grain size
Differ, diameter is between 10~200nm.
In addition, the interfacial bonding property of aluminium oxide and silicone rubber matrix is poor it can be seen from Fig. 1-2, thus bring compared with
Big interface resistance.Silver-plated aluminium oxide is tightly wrapped up by silicone rubber matrix it can be seen from Fig. 3-4, no sharp interface, so boundary
Face thermal resistance is lowered.In addition, the Argent grain between alumina particle plays function served as bridge, connection has played adjacent oxidation
Aluminium, forms more heat conduction networks, so heat conductivity is enhanced.
In addition, those skilled in the art can also the claims in the present invention scope of disclosure and spirit in do other forms and
Various modifications, addition and replacement in details.Certainly, these various modifications, addition and replacements for being done according to present invention spirit
Deng change, should all be included within scope of the present invention.
Claims (10)
1. a kind of preparation method of thermally conductive silicone rubber composite material, its step include：
Filler is uniformly mixed with liquid silastic, adds auxiliary agent, is ground, cures, it is compound that the heat-conducting silicon rubber is prepared
Material, the filler are nano silver coated aluminum oxide.
2. preparation method as claimed in claim 1, it is characterised in that the nano silver coated aluminum oxide passes through following steps system
：
Sensitized treatment：Aluminium oxide will be added in the hydrochloric acid solution of stannous chloride, stirred, separation of solid and liquid, after obtaining sensitized treatment
Aluminium oxide；
Activation process：Aluminium oxide after the sensitized treatment is added in the hydrochloric acid solution of palladium bichloride, is stirred, separation of solid and liquid,
Obtain the aluminium oxide after activation process；
Silver-colored cladding process：Ammonium hydroxide is added dropwise in silver nitrate solution, silver ammino solution is made；The tartaric acid of glucose is mixed
Aluminium oxide after solution, activation process is added in the silver ammino solution, stirring, separation of solid and liquid, obtains the nano silver cladding
Aluminium oxide.
3. preparation method as claimed in claim 2, it is characterised in that in the hydrochloric acid solution of the stannous chloride stannous oxide with
The molar ratio of hydrochloric acid is 1:The solid-to-liquid ratio of 10-12, the aluminium oxide and the hydrochloric acid solution of the stannous chloride is 1:10-15.
4. preparation method as claimed in claim 2, it is characterised in that palladium bichloride and hydrochloric acid in the hydrochloric acid solution of the palladium bichloride
Molar ratio be 3-5:100, the solid-to-liquid ratio of aluminium oxide and the hydrochloric acid solution of the palladium bichloride after the sensitized treatment is 1:10-
15。
5. preparation method as claimed in claim 2, it is characterised in that glucose in the tartaric acid mixed solution of the glucose
Molar ratio with tartaric acid is 8-10:1, the silver ammino solution, tartaric acid mixed solution and the oxygen after activation process of glucose
The ratio for changing aluminium is 5-6:1.
6. preparation method as claimed in claim 2, it is characterised in that the silver cladding process further comprises, by solid-liquid point
Processing is dried in the nano silver coated aluminum oxide obtained from after, obtains nano silver coated aluminum oxide particle powder.
7. preparation method as claimed in claim 1, it is characterised in that the auxiliary agent is containing hydrogen silicone oil and platinum catalyst.
8. a kind of thermally conductive silicone rubber composite material that as claimed in claim 1 prepared by method, it is characterised in that including following weight
The following component of number：
3-5 parts of silicone rubber matrix；
20-30 parts of nano silver coated aluminum oxide.
9. thermally conductive silicone rubber composite material as claimed in claim 8, the thermally conductive silicone rubber composite material includes following parts by weight
Several components：
3.3 parts of silicone rubber matrix；
20 parts of nano silver coated aluminum oxide.
10. thermally conductive silicone rubber composite material as claimed in claim 8, the thermal conductivity of the thermally conductive silicone rubber composite material is 1-
2W/mK。
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| CN201711258571.5A CN107955375A (en) | 2017-12-01 | 2017-12-01 | Thermally conductive silicone rubber composite material and preparation method thereof |
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| CN201711258571.5A CN107955375A (en) | 2017-12-01 | 2017-12-01 | Thermally conductive silicone rubber composite material and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09111124A (en) * | 1995-10-17 | 1997-04-28 | Toray Dow Corning Silicone Co Ltd | Heat-conductive silicone rubber and its composition |
| CN101885918A (en) * | 2010-07-09 | 2010-11-17 | 东莞新东方化工有限公司 | Heat conducting silicon rubber |
| JP2012201106A (en) * | 2011-03-28 | 2012-10-22 | Denki Kagaku Kogyo Kk | Thermoconductive molding and use thereof |
-
2017
- 2017-12-01 CN CN201711258571.5A patent/CN107955375A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09111124A (en) * | 1995-10-17 | 1997-04-28 | Toray Dow Corning Silicone Co Ltd | Heat-conductive silicone rubber and its composition |
| CN101885918A (en) * | 2010-07-09 | 2010-11-17 | 东莞新东方化工有限公司 | Heat conducting silicon rubber |
| JP2012201106A (en) * | 2011-03-28 | 2012-10-22 | Denki Kagaku Kogyo Kk | Thermoconductive molding and use thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张元元等: "纳米银颗粒包覆氧化铝的制备及其硅胶复合材料热导率", 《当代化工》 * |
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Application publication date: 20180424 |