CN109627776A - Solidfied material made of heat-conductive silicone composition and its solidification - Google Patents
Solidfied material made of heat-conductive silicone composition and its solidification Download PDFInfo
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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
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of heat-conductive silicone composition and its solidify manufactured solidfied material, heat-conductive silicone composition includes the component of following mass fraction: 80-120 parts of the high molecular weight silicone containing vinyl；5-20 parts of low molecular weight polysiloxane containing vinyl；5-10 parts of micromolecular hydroxyl silicone oil；It is heat filling 500-1000 parts modified；20-45 parts of reinforced filling of nanometer；1-10 parts of heat-resisting additive；And 0.05-15 parts of curing agent.Heat-conductive silicone composition of the invention, thermal coefficient is improved by the addition of modified heat filling, and nanometer reinforced filling is added to improve the physical property of its solidfied material.The thermal coefficient that the heat-conductive silicone composition solidifies solidfied material obtained is greater than 2W/ (mK), and its tensile strength is greater than 2MPa, and elongation at break is greater than 100%, good physical properties.
Description
Technical field
The present invention relates to solid made of a kind of thermally conductive composition more particularly to a kind of heat-conductive silicone composition and its solidification
Compound.
Background technique
With the continuous development of electronic technology, the size of component is smaller and smaller, and integrated level is also higher and higher.Component
A large amount of heat can be generated in operation, and the accumulation of these heats brings the service life and reliability of component fatal
It influences, in order to disperse the heat generated in operation quickly, there is inevitable requirement the Heat Conduction Material of more high thermal conductivity coefficient to go to conduct
These heats.
Existing general Heat Conduction Material mainly by it is softer it is gelatinous in the form of occur, tensile strength does not surpass generally
1MPa is crossed, but under some Special use environment, component had not only required Heat Conduction Material higher thermal coefficient, but also required tool
Have good physical property, to play a dual role of heat dissipation and physical protection, such as material have preferable tensile strength and compared with
Major rupture elongation.
Patent CN103436019A discloses a kind of method for obtaining high thermal conductivity coefficient thermally conductive composition, by spherical oxygen
Change aluminium to be sieved, then grind to organosilicon and filler mixture and then obtain a kind of high thermal conductivity composition, but the patent
There are not the physical characteristic and its improved method for referring to material.Patent CN103214853A discloses a kind of leading for high thermal conductivity coefficient
The method of hot composition is mentioned and aspherical and spheroidal particle is carried out mixing as heat filling come before improving the composition solidification
Mobility, also without concern solidfied material physical property.
Summary of the invention
The technical problem to be solved in the present invention is that providing the physical property of a kind of raising thermal coefficient and its solidfied material
Heat-conductive silicone composition and the heat-conductive silicone composition solidify manufactured solidfied material.
The technical solution adopted by the present invention to solve the technical problems is: a kind of heat-conductive silicone composition is provided, including
The component of following mass fraction:
Preferably, the high molecular weight silicone containing vinyl is in a molecule with two or more
The long-chain polysiloxanes of vinyl groups, there are two methyl groups for tool on each silicon atom.
Preferably, the high molecular weight silicone containing vinyl selects linear polydimethyl siloxane, average mark
Son amount range is 200,000-100 ten thousand.
Preferably, the low molecular weight polysiloxane containing vinyl is in a molecule with two or more
The short chain polysiloxane of vinyl groups, there are two methyl groups for tool on each silicon atom.
Preferably, the low molecular weight polysiloxane containing vinyl selects linear polydimethyl siloxane, average mark
Son amount range is 500-200000.
Preferably, the micromolecular hydroxyl silicone oil is the linear polysiloxane of both ends hydroxyl, average molecular weight range
For 200-2000.
Preferably, the modified heat filling includes modified aluminum oxide, modified oxidized magnesium, modified boron nitride, modification
One of aluminium nitride and modified aluminium hydroxide are a variety of.
Preferably, the partial size of the modified heat filling is 0.1 μm -40 μm.
Preferably, the nanometer reinforced filling includes that BET method specific surface area is greater than 50m2The fumed silica of/g, precipitating
One of method silica and Nano-sized Alumina Powder are a variety of.
Preferably, the heat-resistant agent is iron oxide or cerium oxide, and partial size is 0.05 μm -100 μm.
Preferably, the curing agent is the high molecular weight silicone containing vinyl containing 50% peroxide；The mistake
Oxide be benzoyl peroxide, 2,4- dichlorobenzoperoxide, benzoyl peroxide, peroxidating di tert butyl carbonate,
At least one of cumyl peroxide and 2,5- dimethyl -2,5- di-t-butyl hexane peroxide；Alternatively,
The curing agent is the composition of containing hydrogen silicone oil, delayed-action activator and platinum complex compound；The containing hydrogen silicone oil is single point
The hydrogen atom of at least two or more hydrogen bonds, the mass percentage of viscosity 10cs-500cs, hydrogen atom are in son amount
0.1%-1.6%；Containing hydrogen silicone oil additional amount is 0.1-10 parts；
The delayed-action activator is 3- methyl-1-- 3 alcohol of butine, 1- acetenyl-1- cyclohexanol, ethyl maleate, maleic acid allyl
One or more of mixture in ester；Delayed-action activator additional amount is 0.1-2 parts；
The platinum complex compound is Karstedt catalyst, and platinum content is 500-20000ppm；When Karstedt is urged
The platinum content of agent is 5000ppm, and additional amount is 0.1-5 parts.
The present invention also provides a kind of heat-conductive silicone compositions to solidify manufactured solidfied material.
Heat-conductive silicone composition of the invention, thermal coefficient is improved by the addition of modified heat filling, and nanometer is mended
Strong filler is added to improve the physical property of its solidfied material.The heat-conductive silicone composition solidifies the thermally conductive of solidfied material obtained
Coefficient is greater than 2W/ (mK), and its tensile strength is greater than 2MPa, and elongation at break is greater than 100%, good physical properties.
Specific embodiment
Heat-conductive silicone composition of the invention, the component including following mass fraction:
Wherein, the high molecular weight silicone containing vinyl is that have two or more vinyl in a molecule
The long-chain polysiloxanes of group, there are two methyl groups for tool on each silicon atom.High molecular weight silicone containing vinyl can
To contain longer side chain, it is also possible to straight chain.
Preferably, the high molecular weight silicone containing vinyl selects linear polydimethyl siloxane, average molecular weight
Range is 200,000-100 ten thousand；Average molecular weight further preferred 300,000-70 ten thousand.
Low molecular weight polysiloxane containing vinyl is that have two or more vinyl groups in a molecule
Short chain polysiloxane, there are two methyl groups for tool on each silicon atom.Low molecular weight polysiloxane containing vinyl can contain
There is longer side chain, is also possible to straight chain.
Preferably, the low molecular weight polysiloxane containing vinyl selects linear polydimethyl siloxane, average molecular weight
Range is 500-200000；The further preferred 2000-50000 of average molecular weight.
Linear polysiloxane of the micromolecular hydroxyl silicone oil for both ends hydroxyl, average molecular weight range 200-2000,
It is preferred that 300-1000.
Modified heat filling includes modified aluminum oxide, modified oxidized magnesium, modified boron nitride, modified aluminium nitride and changes
One of property aluminium hydroxide is a variety of.The addition of modified heat filling is to increase heat-conductive silicone composition loading to mention
High thermal conductivity coefficient, while reducing the thermal resistance between filler and siloxanes.
The shape of modified heat filling can be spherical shape, be also possible to aspherical.For spherical modification heat filling,
Partial size is 0.1 μm -40 μm, preferably 0.5 μm -30 μm.
Nanometer reinforced filling includes that BET method specific surface area is greater than 50m2The fumed silica of/g, precipitated silica
With one of Nano-sized Alumina Powder or a variety of.
Heat-resistant agent is iron oxide or cerium oxide, and partial size is 0.05 μm -100 μm, preferably 5 μm -40 μm.
Alternatively, curing agent can be the high molecular weight silicone containing vinyl containing 50% peroxide.Wherein,
Peroxide is benzoyl peroxide, 2,4- dichlorobenzoperoxide, benzoyl peroxide, the tertiary fourth of peroxidating two
At least one of ester, cumyl peroxide and 2,5- dimethyl -2,5- di-t-butyl hexane peroxide.
Curing agent may be the composition of containing hydrogen silicone oil, delayed-action activator and platinum complex compound.In the composition, containing hydrogen silicone oil
Additional amount is 0.1-10 parts (mass fraction), and delayed-action activator additional amount is 0.1-2 parts.
In the composition as curing agent, containing hydrogen silicone oil is hydrogen bond at least two or more in individual molecule amount
Hydrogen atom, viscosity 10cs-500cs, the mass percentage of hydrogen atom are 0.1%-1.6%.Delayed-action activator is 3- methyl-1-fourth
- 3 alcohol of alkynes, 1- acetenyl -1- cyclohexanol, ethyl maleate, mixture one or more of in the allyl propionate of Malaysia.Platinum complexing
Object is Karstedt catalyst (i.e. platinum catalyst), and the platinum content of the Karstedt catalyst is 500-20000ppm；When
When platinum content is 5000ppm in Karstedt catalyst, the additional amount of Karstedt catalyst is 0.1-5 parts.
The average molecular weight of component is weight average molecular weight in heat-conductive silicone composition of the invention, using toluene as solvent,
Using the result calculated after the test of high productivity computing method.Partial size refers to average grain diameter, the D50 measured using laser diffractometry
Partial size.
In addition, colorant, UV resistant agent can also be added as needed in heat-conductive silicone composition of the invention
Deng.
When heat-conductive silicone composition manufacture of the invention, biaxial extruder can be used, also can be used kneader or
Banbury (mixer), preferably kneader gradually feed kneading.
Heat-conductive silicone composition is pressed and molded on vulcanizing press and screw extrusion molding, curing time 180
Vulcanize 300 seconds at DEG C, solidfied material can be obtained.
Heat-conductive silicone composition of the invention solidifies manufactured solidfied material, and thermal coefficient is greater than 2W/ (mK), stretches strong
Degree is greater than 2MPa, and elongation at break is greater than 100%.As needed, solidfied material includes that various shape is such as round, rectangular or special-shaped
Radiating cap play the role of heat dissipation, insulation and protection for the electronic components such as light emitting diode.
Below by way of specific embodiment, the present invention is further described.
Embodiment 1
By the average molecular weight of 200g be 500,000 long-chain dimethyl silicone polymer, 20g average molecular weight be 5000
End-vinyl siloxane, the end hydroxyl silicone oil that the average molecular weight of 8g is 1000 are added in the kneader of 5L, and stirring at normal temperature 5 is divided
Clock, is then added portionwise the ball-aluminium oxide that the average grain diameter of 2000g is 30 μm respectively, and the BET method specific surface area of 80g is
200m2The fume colloidal silica of/g.High temperature, vacuum mix 4 hours after room temperature mixes 1 hour.Mixing finishes discharging, takes out 200g
The long-chain poly dimethyl that the average molecular weight of 1g dimethyl containing 50%2,5- -2,5- di-t-butyl hexane peroxide is 500,000 is added
Mixture of siloxanes is uniformly mixed on a mill, is vulcanized 300 seconds at 180 DEG C on vulcanizing press, and solidfied material is made.
Embodiment 2
By the average molecular weight of 200g be 800,000 long-chain dimethyl silicone polymer, 20g average molecular weight be 5000
End-vinyl siloxane, the end hydroxyl silicone oil that the average molecular weight of 8g is 1000 are added in the kneader of 5L, and stirring at normal temperature 5 is divided
Then the ball-aluminium oxide that the average grain diameter of 1900g is 20 μm, the spherical shape that 100g average grain diameter is 5 μm is added portionwise in clock respectively
Modified aluminium nitride, the BET method specific surface area of 80g are 300m2The fume colloidal silica of/g.High temperature, vacuum after room temperature mixes 1 hour
Mixing 4 hours.Mixing finishes discharging and takes out 200g, and 1g di-t-butyl hexane peroxide containing 50%2,5- dimethyl -2,5- is added
Average molecular weight be 500,000 long-chain polydimethylsiloxanemixture mixture, be uniformly mixed on a mill, in vulcanizing press
Vulcanize 300 seconds at upper 180 DEG C, solidfied material is made.
Embodiment 3
By the average molecular weight of 200g be 600,000 long-chain dimethyl silicone polymer, 20g average molecular weight be 5000
End-vinyl siloxane, the end hydroxyl silicone oil that the average molecular weight of 8g is 800 are added in the kneader of 5L, and stirring at normal temperature 5 is divided
Clock, the average grain diameter that 2100g is then added portionwise respectively is 15 μm of ball-aluminium oxide, and the average grain diameter of 100g is 1 μm and changes
Property spherical shape magnesia, the BET method specific surface area of 80g is 250m2The fume colloidal silica of/g.It is high temperature after room temperature mixes 1 hour, true
Sky mixing 4 hours.Mixing, which finishes to discharge, takes out 200g, addition 0.3g, the containing hydrogen silicone oil that hydrogen content 0.7%, viscosity are 30cs,
0.05g 1- acetenyl -1- cyclohexanol, is uniformly mixed on a mill；Add the Karstedt method catalyst of 5000ppm
0.1g, mill is uniform, vulcanizes 300 seconds at 180 DEG C on vulcanizing press later, and solidfied material is made.
Comparative example 1
By the average molecular weight of 200g be 100,000 long-chain dimethyl silicone polymer, 20g average molecular weight be 5000
End-vinyl siloxane, the end hydroxyl silicone oil that the average molecular weight of 8g is 800 are added in the kneader of 5L, and stirring at normal temperature 5 is divided
Clock, is then added portionwise the ball-aluminium oxide that the average grain diameter of 1200g is 30 μm respectively, and the BET method specific surface area of 80g is
200m2The fume colloidal silica of/g.High temperature after room temperature mixes 1 hour, vacuum mix 4 hours.Mixing finishes discharging and takes out 200g
The long-chain poly dimethyl that the average molecular weight of 1g dimethyl containing 50%2,5- -2,5- di-t-butyl hexane peroxide is 500,000 is added
Mixture of siloxanes is uniformly mixed on a mill, is vulcanized 300 seconds at 180 DEG C on vulcanizing press, and solidfied material is made.
Comparative example 2
By the average molecular weight of 200g be 100,000 long-chain dimethyl silicone polymer, 20g average molecular weight be 5000
End-vinyl siloxane, the end hydroxyl silicone oil that the average molecular weight of 8g is 800 are added in the kneader of 5L, and stirring at normal temperature 5 is divided
Then the aluminium oxide that the average grain diameter of 2000g is 20 μm is added portionwise in clock respectively, high temperature, vacuum mixing after room temperature mixes 1 hour
4 hours.Mixing finishes discharging and takes out being averaged for 200g addition 1g dimethyl containing 50%2,5- -2,5- di-t-butyl hexane peroxide
The long-chain polydimethylsiloxanemixture mixture that molecular weight is 500,000, is difficult in flakes, not mix in open mill.
The physical property of solidfied material made from above-described embodiment 1-3 and comparative example 1-2 is tested, as shown in table 1 below.
Table 1
Wherein, hardness is ASTM D2240 using the measurement examination of shore A type hardness tester, test method；Tensile strength and fracture are stretched
Long rate uses puller system, and test method is ASTM D412, and thermal coefficient is tested using Hotdisk conductometer, and test method is
ISO22007-2-2015。
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (10)
1. a kind of heat-conductive silicone composition, which is characterized in that the component including following mass fraction:
80-120 parts of high molecular weight silicone containing vinyl；
5-20 parts of low molecular weight polysiloxane containing vinyl；
5-10 parts of micromolecular hydroxyl silicone oil；
It is heat filling 500-1000 parts modified；
20-45 parts of reinforced filling of nanometer；
1-10 parts of heat-resisting additive；And
0.05-15 parts of curing agent.
2. heat-conductive silicone composition according to claim 1, which is characterized in that the high-molecular-weight poly containing vinyl
Siloxanes is the long-chain polysiloxanes in a molecule with two or more vinyl groups, is had on each silicon atom
There are two methyl groups.
3. heat-conductive silicone composition according to claim 2, which is characterized in that the high-molecular-weight poly containing vinyl
Siloxanes selects linear polydimethyl siloxane, and average molecular weight range is 200,000-100 ten thousand.
4. heat-conductive silicone composition according to claim 1, which is characterized in that the low molecular weight containing vinyl is poly-
Siloxanes is the short chain polysiloxane in a molecule with two or more vinyl groups, is had on each silicon atom
There are two methyl groups.
5. heat-conductive silicone composition according to claim 4, which is characterized in that the low molecular weight containing vinyl is poly-
Siloxanes selects linear polydimethyl siloxane, average molecular weight range 500-200000.
6. heat-conductive silicone composition according to claim 1, which is characterized in that the micromolecular hydroxyl silicone oil is both ends
The linear polysiloxane of hydroxyl, average molecular weight range 200-2000；
The modified heat filling includes modified aluminum oxide, modified oxidized magnesium, modified boron nitride, modified aluminium nitride and changes
One of property aluminium hydroxide is a variety of.
7. heat-conductive silicone composition according to claim 6, which is characterized in that the partial size of the modified heat filling is
0.1μm-40μm。
8. heat-conductive silicone composition according to claim 1, which is characterized in that the nanometer reinforced filling includes BET
Method specific surface area is greater than 50m2One of fumed silica, precipitated silica and Nano-sized Alumina Powder of/g are more
Kind；
The heat-resistant agent is iron oxide or cerium oxide, and partial size is 0.05 μm -100 μm.
9. heat-conductive silicone composition according to claim 1, which is characterized in that the curing agent is containing 50% peroxidating
The high molecular weight silicone containing vinyl of object；The peroxide is benzoyl peroxide, 2,4- dichloro benzoyl peroxide first
Acyl, benzoyl peroxide, peroxidating di tert butyl carbonate, cumyl peroxide and 2,5- dimethyl -2,5- di-t-butyl
At least one of butylperoxyhexane；Alternatively,
The curing agent is the composition of containing hydrogen silicone oil, delayed-action activator and platinum complex compound；The containing hydrogen silicone oil is individual molecule amount
On at least two or more hydrogen bond hydrogen atom, viscosity 10cs-500cs, the mass percentage of hydrogen atom is 0.1%-
1.6%；Containing hydrogen silicone oil additional amount is 0.1-10 parts；
The delayed-action activator is 3- methyl-1-- 3 alcohol of butine, 1- acetenyl-1- cyclohexanol, ethyl maleate, Malaysia allyl propionate
The mixture of middle one or more；Delayed-action activator additional amount is 0.1-2 parts；
The platinum complex compound is Karstedt catalyst, and platinum content is 500-20000ppm；When Karstedt catalyst
Platinum content be 5000ppm, additional amount be 0.1-5 parts.
10. a kind of described in any item thermally conductive compositions of claim 1-9 solidify manufactured solidfied material.
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| CN113913019A (en) * | 2021-12-06 | 2022-01-11 | 祥雅(嘉兴)科技有限公司 | High-heat-conductivity liquid silicone rubber for composite material mold |
| CN114729193A (en) * | 2019-11-14 | 2022-07-08 | 信越化学工业株式会社 | Thermally conductive silicone composition and thermally conductive silicone sheet |
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| CN110343389A (en) * | 2019-06-04 | 2019-10-18 | 深圳市飞荣达科技股份有限公司 | Anisotropy insulating heat-conductive composition and preparation method thereof |
| CN110938406A (en) * | 2019-11-04 | 2020-03-31 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Bi-component organic silicon pouring sealant and preparation method thereof |
| CN114729193A (en) * | 2019-11-14 | 2022-07-08 | 信越化学工业株式会社 | Thermally conductive silicone composition and thermally conductive silicone sheet |
| CN114729193B (en) * | 2019-11-14 | 2023-08-22 | 信越化学工业株式会社 | Thermally conductive silicone composition and thermally conductive silicone sheet |
| CN113913019A (en) * | 2021-12-06 | 2022-01-11 | 祥雅(嘉兴)科技有限公司 | High-heat-conductivity liquid silicone rubber for composite material mold |
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