CN107141815A - A kind of low modulus heat conduction organosilicon material of high temperature resistant and preparation method thereof - Google Patents
A kind of low modulus heat conduction organosilicon material of high temperature resistant and preparation method thereof Download PDFInfo
- Publication number
- CN107141815A CN107141815A CN201710489798.4A CN201710489798A CN107141815A CN 107141815 A CN107141815 A CN 107141815A CN 201710489798 A CN201710489798 A CN 201710489798A CN 107141815 A CN107141815 A CN 107141815A
- Authority
- CN
- China
- Prior art keywords
- low modulus
- high temperature
- temperature resistant
- silicone oil
- heat conduction
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- 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
-
- 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
-
- 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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
-
- 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
-
- 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 present invention provides a kind of low modulus heat conduction organosilicon material of high temperature resistant, including following preparing raw material:Silicone oil, conduction powder filler, low modulus auxiliary agent, high temperature resistant auxiliary agent, crosslinking agent and platinum catalyst;The mass ratio of the silicone oil and the conduction powder filler is 90 110:900 1100, the mass ratio of the conduction powder filler and the low modulus auxiliary agent is 100:0.5 2, the silicone oil, the high temperature resistant auxiliary agent, the crosslinking agent, the mass ratio of the platinum catalyst are followed successively by 100:0.1‑1:5‑15:0.1‑0.2.The invention belongs to organosilicon technical field, the radiating long-time stability of the heat conduction organosilicon material that the present invention is provided under the high temperature conditions are good, low modulus, gap easy to attach, thermal resistance is low, oil-tight, non-volatile, dispensing construction can be automated, is that more preferable interface Heat Conduction Material is provided between electronic apparatus heating element and radiating element or equipment.
Description
Technical field
The invention belongs to organosilicon technical field, more particularly to a kind of low modulus heat conduction organosilicon material of high temperature resistant and its system
Preparation Method.
Background technology
Growing with electronic enterprises, electronic product is to highly integrated, and high-power and small-sized miniaturization is constantly more
It is new to regenerate to meet the demand of emerging market.However, highly integrated, high-power and small-sized miniaturization can make electronic component unit plane
The heat produced in product drastically increases, if conducted not in time, and the performance of electric equipment products and life-span all will be by
To serious influence.
Therefore, in the design and fabrication of electric equipment products, for the heat that produces the heating elements such as chip and
When shed, it will usually install radiator additional to accelerate radiating, but often there is gap between radiator and heating element, gap is empty
Gas has very big thermal resistance, and the effect for having a strong impact on radiator is played, and conventional technical method is to use interface heat conduction material at present
Material filling gap, the thermal resistance between reduction heating element and radiator in time dissipates heat, so as to ensure equipment
Stabilization normally run.
Traditional interface Heat Conduction Material has two kinds of heat-conducting silicone grease and heat-conducting pad.Heat-conducting silicone grease is typically to use low viscosity silicon
A kind of never curing materials that oil is mixed with conduction powder filler, it is easy to a variety of modes of operation, being capable of the fast fast-growing of equipment
Production, can scrape very thin, so as to reduce thermal resistance and cost-effective, but not chemically reacted between silicone oil and conduction powder filler
Crosslinking so that silicone grease after being used for a long time and being used for a long time especially under high temperature, silicone oil can slowly separate out, cause silicone grease to become dry and cracked
And air inlet, heat transfer resistance is considerably increased, radiation stability is poor, have a strong impact on the use longevity of electric equipment products equipment
Life.Chinese patent application CN 105400202 discloses a kind of boron nitride/graphene composite heat-conducting silicone grease, each component and mass parts
Array turns into:10~30 parts of methyl phenyl silicone oil, modified boron nitride/graphene 60~90 parts of heat filling of compounding is silane coupled
Agent is the 3%~8% of heat filling, and crosslinking agent is the 0.1%~1% of methyl phenyl silicone oil, 0.1~1 part of structural improvement auxiliary agent,
0.1~1 part of antioxidant;Although having the advantages that high thermal conductivity coefficient, the problem of there is permeability can cause radiating after long-term use
Effect is substantially reduced.
The appearance of heat-conducting pad preferably resolves the dry and cracked efflorescence drawback after heat-conducting silicone grease is heated for a long time, but heat-conducting pad
Thickness is big compared with silicone grease, and thermal resistance is larger, while heat-conducting pad cannot be used for the quick production and construction of equipment, can increase construction cost.
With the miniaturization of electronic product complete machine and the fast development of high-power, heat generating component temperature is constantly raised, to boundary
Face Heat Conduction Material demand is further lifted, it is desirable to also harsher.There is provided a kind of both scattered with the stability and high efficiency under hot conditions
Hot property can realize that the interface Heat Conduction Material of automation rapid construction is significant again.
The content of the invention
To solve problems of the prior art (permeability, long-term radiation stability are not ideal enough), inventor passes through big
Amount experiment is screened and compounded to the component of organosilicon material, unexpected discovery:By a small amount of low modulus auxiliary agent of addition,
The surface polarity of conduction powder can be changed, contribute to the thermal conductive network chain of heat filling to be formed, the compatibility with silicone oil is improved, moreover it is possible to
Enough realize that the radiating long-time stability under the performance of soft and low modulus after heat conduction organosilicon material solidification, hot conditions are good,
Low modulus, gap easy to attach, thermal resistance is low, oil-tight, non-volatile, can automate dispensing construction, be electronic apparatus heating element
More preferable interface Heat Conduction Material is provided between radiating element or equipment.Based on above-mentioned discovery, so as to complete the present invention.
The purpose of the present invention will be further described in detail below reflect and description.
A kind of low modulus heat conduction organosilicon material of high temperature resistant, it is characterised in that:Including following preparing raw material:Silicone oil, heat conduction
Powder stuffing, low modulus auxiliary agent, high temperature resistant auxiliary agent, crosslinking agent and platinum catalyst;The silicone oil and the conduction powder filler
Mass ratio be 90-110:The mass ratio of 900-1100, the conduction powder filler and the low modulus auxiliary agent is 100:0.5-
2, the silicone oil, the high temperature resistant auxiliary agent, the crosslinking agent, the mass ratio of the platinum catalyst are followed successively by 100:0.1-1:5-
15:0.1-0.2.
The composition and amount ranges of above-mentioned preparing raw material, are that inventor is determined by lot of experiments.Using above-mentioned technology
Scheme, by a small amount of low modulus auxiliary agent of addition, can change the surface polarity of conduction powder, contribute to the heat conduction network chain of heat filling
Formed, improve the compatibility with silicone oil, additionally it is possible to realize the performance of soft and low modulus after heat conduction organosilicon material solidification, it is high
Radiating long-time stability under the conditions of temperature are good, and low modulus, gap easy to attach, thermal resistance is low, oil-tight, non-volatile, can automate a little
Glue is constructed, and is that more preferable interface Heat Conduction Material is provided between electronic apparatus heating element and radiating element or equipment.And it is existing
Technology then mainly realizes low modulus by adding crosslinking agent, but under the high temperature conditions, low modulus, which can not be stablized, to be kept.
In addition, the high temperature resistant auxiliary agent that is added of the present invention belongs to organic silicon metal complex compound, itself and basic silicon based polymers
Compatibility is good, in the organosilicon material system for being added to the present invention, significantly improves resistance to elevated temperatures, the low mould of high temperature resistant of preparation
Amount heat conduction organosilicon material can be used for a long time at 260 DEG C, and the problems such as Heat Conduction Material is not in cracking, efflorescence is effectively ensured
Long-term radiation stability under hot conditions.
Preferably, the mass ratio of the silicone oil and the conduction powder filler is 95-105:900-1050, the conductive powder
The mass ratio of body filler and the low modulus auxiliary agent is 100:0.7-1.5, the silicone oil, the high temperature resistant auxiliary agent, the crosslinking
Agent, the mass ratio of the platinum catalyst are followed successively by 100:0.2-0.8:8-14:0.12-0.18.
Preferably, the low modulus auxiliary agent is selected from hydroxyvinyl silicone oil, alkoxy vinyl silicone oil or its composition, glues
Spend for 1-20cp.In organosilicon material technical field, hydroxyvinyl silicone oil and alkoxy vinyl silicone oil are often used as gluing
Connect auxiliary agent.Inventor is had found by creative work, by the organosilicon material system of the present invention, adding a small amount of hydroxyl second
Alkenyl silicone oil and/or alkoxy vinyl silicone oil are as low modulus auxiliary agent, and its viscosity is very low, contain or the hydroxyl that generates can be with
Heat filling powder surface hydroxyl reaction, changes powder surface polarity, improves and oil compatibility, it is ensured that can be dropped in batch mixing
Low material viscosity, improves the dispersion effect and filling rate of heat filling powder, contributes to the thermal conductive network chain of heat filling to be formed;Separately
One side hydroxyvinyl silicone oil and/or alkoxy vinyl silicone oil contain vinyl groups again, occur in silicone oil and crosslinking agent
During cross-linking reaction, energy subparticipation makes base polymer strand linearly lengthen into cross-linking reaction, then passes through branched hand over
Join to change network topology structure, reach crosslink density and the controllable purpose of distribution, help to realize heat conduction organosilicon material
The performance of soft and low modulus after solidification, at the same the low modulus base polymer network by hydroxyvinyl silicone oil and/or
Alkoxy vinyl silicone oil is connected chemically with heat filling powder, so that obtained heat conduction organosilicon material has simultaneously
Low modulus, heat conductivility be stable, it is oil-tight and non-volatile the advantages of.
It is highly preferred that the low modulus auxiliary agent by hydroxyvinyl silicone oil and alkoxy vinyl silicone oil with 4-10:1 matter
Amount is than composition, and viscosity is 1-16cp.Low modulus auxiliary agent is by hydroxyvinyl silicone oil and alkoxy vinyl silicone oil with 4-10:1
When mass ratio is constituted, 100% stress at definite elongation is lower, and low modulus is better.
Preferably, the high temperature resistant auxiliary agent is selected from organosilicon copper complex, organosilicon aluminium complex, organosilicon iron complex
With the one or more in organosilicon zirconium complex.
Preferably, the silicone oil is methyl vinyl silicon oil, phenyl-vinyl silicon oil or its composition, and viscosity is 250-
1000cp。
Preferably, the conduction powder filler be selected from aluminum oxide, zinc oxide, boron nitride, carborundum, aluminium nitride, graphene,
One or more in aluminium powder and carbon nanotube dust, its particle diameter is 0.1-100 μm.It is highly preferred that particle diameter is 0.5-20 μm, shape
Shape is ball-type.It is highly preferred that the conduction powder filler by aluminum oxide and boron nitride with 90:2 mass ratio composition, or by aoxidizing
Aluminium and zinc oxide are with 4:1 mass ratio composition, or by aluminum oxide and graphene with 90:2 mass ratio composition.
Preferably, the crosslinking agent by end containing hydrogen silicone oil and side containing hydrogen silicone oil with 1:1.5-2 mass ratio composition, the end
The hydrogen content of containing hydrogen silicone oil is 0.05-0.2wt%, and the hydrogen content of the side containing hydrogen silicone oil is 0.1-0.3wt%.
Preferably, the platinum catalyst is Karst platinum catalyst, and platinum content is 5000ppm.
Correspondingly, present invention also offers the preparation method of the low modulus heat conduction organosilicon material of high temperature resistant, including following step
Suddenly:
S1 puts into silicone oil in dispersion machine, and conduction powder filler and low modulus auxiliary agent are added in batches, is stirred;
Then S2 puts into high temperature resistant auxiliary agent, crosslinking agent in dispersion machine, stirs;
105-115 DEG C is warming up under the conditions of S3 vacuum protections, dispersed with stirring reaction 40-80min is vacuumized;
After S4 reactions terminate, treat that material is cooled to 68-72 DEG C, add platinum catalyst, vacuumize stirring reaction 25-
40min, is subsequently cooled to room temperature, that is, obtains the low modulus heat conduction organosilicon material of high temperature resistant.
Using above-mentioned technical proposal, by first adding conduction powder filler and low modulus auxiliary agent in batches into silicone oil, stir
High temperature resistant auxiliary agent and crosslinking agent are added after mixing uniformly, contributes to the formation of thermal conductive network chain and the product heat conduction organosilicon of heat filling
The holding of the premium properties such as material soft, low modulus, oil-tight.
Compared with prior art, beneficial effects of the present invention include:
(1) by the organosilicon material system of the present invention, adding a small amount of hydroxyvinyl silicone oil and/or alkoxy second
Alkenyl silicone oil is as low modulus auxiliary agent, and its viscosity is very low, and the hydroxyl for containing or generating can be with heat filling powder surface hydroxyl
Reaction, changes powder surface polarity, improves and oil compatibility, it is ensured that material viscosity can be reduced in batch mixing, improves heat conduction
The dispersion effect and filling rate of filler powder, contribute to the thermal conductive network chain of heat filling to be formed;Another aspect hydroxyvinyl silicon
Oil and/or alkoxy vinyl silicone oil contain vinyl groups again, when silicone oil and crosslinking agent crosslink reaction, can partly join
With into cross-linking reaction, making base polymer strand linearly lengthen, network topology knot is then changed by branched crosslinking
Structure, reaches crosslink density and the controllable purpose of distribution, helps to realize soft and low mould after heat conduction organosilicon material solidification
The performance of amount, at the same the low modulus base polymer network by hydroxyvinyl silicone oil and/or alkoxy vinyl silicone oil with
Heat filling powder is connected chemically, so that obtained heat conduction organosilicon material has low modulus, heat conductivility steady simultaneously
Fixed, oil-tight and non-volatile the advantages of.
(2) by the organosilicon material system of the present invention, adding a small amount of high temperature resistant auxiliary agent --- organic silicon metal network
Compound, it is good with basic silicon based polymers compatibility, significantly improves resistance to elevated temperatures, and the low modulus heat conduction of high temperature resistant of preparation has
Machine silicon materials can be used for a long time at 260 DEG C, and high temperature bar has been effectively ensured in the problems such as Heat Conduction Material is not in cracking, efflorescence
Long-term radiation stability under part.
(3) not only heat conductivility is reliable and stable under high temperature for the low modulus heat conduction organosilicon material of high temperature resistant that provides of the present invention,
And can be cut by arbitrary dimension, to adequately fill up the gap between electronic package surface and installed part surface, form high
The hot switching path of effect, moreover it is possible to damping vibration attenuation is played to electronic equipment and the convenient device that nondestructively carries out reprocesses the work such as recycling
With.The low modulus heat conduction organosilicon material of high temperature resistant that the present invention is provided can be realized to be replaced to existing heat-conducting pad and heat-conducting silicone grease
In generation, it can avoid causing the fluctuation, efflorescence, the risk of thermal conductive contact face reduction of thickness because of the change of humiture, realize certainly
Dynamic point glue pipelining, improves efficiency of construction, can be widely applied to integrated chip, power supply, electrokinetic cell, computer, communication
The radiating of the heating electronic package such as equipment and controller.
(4) preparation method for the low modulus heat conduction organosilicon material of high temperature resistant that the present invention is provided is simple, and obtained heat conduction has
Machine silicon materials steady quality, performance is good.
Embodiment
Below by specific embodiment, the present invention is described in further detail.
In the present invention, involved preparing raw material is conventional commercial product, or can pass through the normal of organosilicon technical field
Technological means is advised to obtain.For example:Hydroxyvinyl silicone oil is purchased from Zhejiang Runhe Organic Silicon New Material Co., Ltd.;Hold containing hydrogen silicone oil
Purchased from Jiangxi Hito Chemical Co., Ltd.;Side containing hydrogen silicone oil is purchased from Jiangxi Hito Chemical Co., Ltd..
The low modulus heat conduction organosilicon material of the high temperature resistant of embodiment one
The low modulus heat conduction organosilicon material of high temperature resistant, includes the preparing raw material of following mass fraction:
The viscosity of methyl vinyl silicon oil is 500cp;Aluminum oxide is spherical, and meso-position radius are 5 μm;Hydroxyvinyl silicone oil
Viscosity is 5cp;Crosslinking agent is made up of 4 parts of end containing hydrogen silicone oils and 6 parts of side containing hydrogen silicone oils;Platinum content is in the platinum catalyst of Karst
5000ppm。
The preparation method of the low modulus heat conduction organosilicon material of high temperature resistant, comprises the following steps:
S1 puts into silicone oil (methyl vinyl silicon oil) in dispersion machine, and conduction powder filler (oxygen is then added in batches
Change aluminium) and low modulus auxiliary agent (hydroxyvinyl silicone oil), it is uniformly mixed;
S2 puts into high temperature resistant auxiliary agent (organosilicon copper complex), crosslinking agent (end containing hydrogen silicone oil, side containing hydrogen silicone oil) point
Dissipate in machine, dispersed with stirring is uniform;
105 DEG C are warming up under the conditions of S3 vacuum protections, dispersed with stirring reaction 60min is vacuumized;
After S4 reactions terminate, treat that material is cooled to 70 DEG C, add platinum catalyst, vacuumize stirring reaction 30min, then
It is cooled to room temperature and obtains the low modulus heat conduction organosilicon finished material of high temperature resistant.
The low modulus heat conduction organosilicon material of the high temperature resistant of embodiment two
The low modulus heat conduction organosilicon material of high temperature resistant, includes the preparing raw material of following mass fraction:
The viscosity of methyl vinyl silicon oil is 500cp;Conduction powder filler is by 900 parts of aluminum oxide and 20 parts of boron nitride groups
Into aluminum oxide is spherical, and meso-position radius are 20 μm, and the meso-position radius of boron nitride are 2 μm;Low modulus auxiliary agent by hydroxyvinyl silicone oil and
Alkoxy vinyl silicone oil is with 6:1 mass ratio composition, viscosity is 15cp;Crosslinking agent is hydrogeneous by 4 parts of end containing hydrogen silicone oils and 6 parts of sides
Silicone oil is constituted;Platinum content is 5000ppm in the platinum catalyst of Karst.
The preparation method of the low modulus heat conduction organosilicon material of high temperature resistant is similar with embodiment one.
The low modulus heat conduction organosilicon material of the high temperature resistant of embodiment three
The low modulus heat conduction organosilicon material of high temperature resistant, includes the preparing raw material of following mass fraction:
The viscosity of phenyl-vinyl silicon oil is 1000cp;Conduction powder filler is by 800 parts of aluminum oxide and 200 parts of zinc oxide groups
Into aluminum oxide is spherical, and meso-position radius are 10 μm, and the meso-position radius of zinc oxide are 1.5 μm;The viscosity of alkoxy vinyl silicone oil is
10cp;Crosslinking agent is made up of 3 parts of end containing hydrogen silicone oils and 6 parts of side containing hydrogen silicone oils;Platinum content is in the platinum catalyst of Karst
5000ppm。
The preparation method of the low modulus heat conduction organosilicon material of high temperature resistant is similar with embodiment one.
The low modulus heat conduction organosilicon material of example IV high temperature resistant
The low modulus heat conduction organosilicon material of high temperature resistant, includes the preparing raw material of following mass fraction:
The viscosity of methyl vinyl silicon oil is 300cp;Conduction powder filler is by 900 parts of aluminum oxide and 20 parts of graphene groups
Into aluminum oxide is spherical, and meso-position radius are 10 μm;The viscosity of hydroxyvinyl silicone oil is 10cp;Crosslinking agent is by 5 parts of end containing hydrogen silicone oils
With 7.5 parts of side containing hydrogen silicone oil compositions;Platinum content is 5000ppm in the platinum catalyst of Karst.
The preparation method of the low modulus heat conduction organosilicon material of high temperature resistant is similar with embodiment one.
Comparative example 1
Heat conduction organosilicon material, includes the preparing raw material of following mass fraction:
The preparation method of heat conduction organosilicon material is similar with embodiment one.
The difference of comparative example 1 and embodiment two is:Do not include low modulus auxiliary agent.
Comparative example 2
The low modulus heat conduction organosilicon material of high temperature resistant, includes the preparing raw material of following mass fraction:
The preparation method of the low modulus heat conduction organosilicon material of high temperature resistant is similar with embodiment one.
The difference of comparative example 2 and embodiment two is:Do not include hydroxyvinyl silicone oil and alkoxy vinyl silicone oil, bag
Include hydroxy silicon oil.The viscosity of hydroxy silicon oil is 15cp.
Comparative example 3
The low modulus heat conduction organosilicon material of high temperature resistant, includes the preparing raw material of following mass fraction:
The preparation method of the low modulus heat conduction organosilicon material of high temperature resistant is similar with embodiment one.
The difference of comparative example 3 and embodiment two is:Do not include high temperature resistant auxiliary agent --- organosilicon iron complex.
Not be the same as Example, the performance detection of heat conduction organosilicon material made from comparative example
The performance test results such as institute of table 1 of heat conduction organosilicon finished material prepared by different embodiments of the invention, comparative example
Show.
Detection method:Density Detection is according to ASTM D792;Thermal conductivity factor is detected according to ASTMD5470-06;Hardness determination
According to ASTM D 2240-05;Fugitive constituent is detected under the conditions of 120 DEG C, 24h;Dielectric strength is detected according to GB/T1695-2005;
100% stress at definite elongation detected according to GB/T1683-81, and with the low modulus of this metrics evaluation.
The performance test results of the not heat conduction organosilicon material made from be the same as Example of table 1
As known from Table 1, the heat conduction organosilicon material that the embodiment of the present invention one is provided to example IV has good heat conduction
Performance, have the advantages that low modulus, it is oil-tight, non-volatile, dispensing construction (paste) can be automated, and the heat ageing of performance is stable
Property is good.The resultant effect of wherein embodiment two is optimal, illustrates that hydroxyvinyl silicone oil and alkoxy vinyl silicone oil are used in conjunction with
Resultant effect for improving heat conduction organosilicon material, especially low modulus properties and low modulus heat aging property have important work
With.And the low modulus auxiliary agent that the present invention is provided is not used in comparative example 1 to comparative example 3,100% stress at definite elongation is larger, and hardness is higher,
Increasing by a relatively large margin occur in 100% stress at definite elongation and hardness especially after thermal ageing test, and low modulus properties substantially deteriorate.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (10)
1. a kind of low modulus heat conduction organosilicon material of high temperature resistant, it is characterised in that:Including following preparing raw material:Silicone oil, conductive powder
Body filler, low modulus auxiliary agent, high temperature resistant auxiliary agent, crosslinking agent and platinum catalyst;The silicone oil and the conduction powder filler
Mass ratio is 90-110:The mass ratio of 900-1100, the conduction powder filler and the low modulus auxiliary agent is 100:0.5-2,
The silicone oil, the high temperature resistant auxiliary agent, the crosslinking agent, the mass ratio of the platinum catalyst are followed successively by 100:0.1-1:5-
15:0.1-0.2.
2. the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1, it is characterised in that:The silicone oil with it is described
The mass ratio of conduction powder filler is 95-105:900-1050, the quality of the conduction powder filler and the low modulus auxiliary agent
Than for 100:0.7-1.5, the silicone oil, the high temperature resistant auxiliary agent, the crosslinking agent, the platinum catalyst mass ratio successively
For 100:0.2-0.8:8-14:0.12-0.18.
3. the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1 or 2, it is characterised in that:The low modulus
Auxiliary agent is selected from hydroxyvinyl silicone oil, alkoxy vinyl silicone oil or its composition, and viscosity is 1-20cp.
4. the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1 or 2, it is characterised in that:The low modulus
Auxiliary agent is by hydroxyvinyl silicone oil and alkoxy vinyl silicone oil with 4-10:1 mass ratio composition, viscosity is 1-16cp.
5. the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1 or 2, it is characterised in that:The high temperature resistant
The one kind of auxiliary agent in organosilicon copper complex, organosilicon aluminium complex, organosilicon iron complex and organosilicon zirconium complex
Or it is a variety of.
6. the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1 or 2, it is characterised in that:The silicone oil is
Methyl vinyl silicon oil, phenyl-vinyl silicon oil or its composition, viscosity are 250-1000cp.
7. the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1 or 2, it is characterised in that:The conductive powder
Body filler in aluminum oxide, zinc oxide, boron nitride, carborundum, aluminium nitride, graphene, aluminium powder and carbon nanotube dust one
Plant or a variety of, its particle diameter is 0.1-100 μm.
8. the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1 or 2, it is characterised in that:The crosslinking agent
By end containing hydrogen silicone oil and side containing hydrogen silicone oil with 1:1.5-2 mass ratio composition, the hydrogen content of the end containing hydrogen silicone oil is 0.05-
0.2wt%, the hydrogen content of the side containing hydrogen silicone oil is 0.1-0.3wt%.
9. the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1 or 2, it is characterised in that:The platinum is urged
Agent is Karst platinum catalyst, and platinum content is 5000ppm.
10. the preparation method of the low modulus heat conduction organosilicon material of high temperature resistant according to claim 1, it is characterised in that:Bag
Include following steps:
S1 puts into silicone oil in dispersion machine, and conduction powder filler and low modulus auxiliary agent are added in batches, is stirred;
Then S2 puts into high temperature resistant auxiliary agent, crosslinking agent in dispersion machine, stirs;
105-115 DEG C is warming up under the conditions of S3 vacuum protections, dispersed with stirring reaction 40-80min is vacuumized;
After S4 reactions terminate, treat that material is cooled to 68-72 DEG C, add platinum catalyst, vacuumize stirring reaction 25-40min, so
After be cooled to room temperature, that is, obtain the low modulus heat conduction organosilicon material of high temperature resistant.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710489798.4A CN107141815B (en) | 2017-06-24 | 2017-06-24 | High-temperature-resistant low-modulus heat-conducting organosilicon material and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710489798.4A CN107141815B (en) | 2017-06-24 | 2017-06-24 | High-temperature-resistant low-modulus heat-conducting organosilicon material and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN107141815A true CN107141815A (en) | 2017-09-08 |
CN107141815B CN107141815B (en) | 2020-03-24 |
Family
ID=59782158
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710489798.4A Active CN107141815B (en) | 2017-06-24 | 2017-06-24 | High-temperature-resistant low-modulus heat-conducting organosilicon material and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107141815B (en) |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109385094A (en) * | 2018-10-29 | 2019-02-26 | 镇江亿维硅材料科技有限公司 | A kind of silicon rubber conducting masterbatch and its preparation method and application |
CN109627776A (en) * | 2018-11-14 | 2019-04-16 | 深圳市飞荣达科技股份有限公司 | Solidfied material made of heat-conductive silicone composition and its solidification |
CN110643180A (en) * | 2019-09-19 | 2020-01-03 | 安徽若水化工有限公司 | Low-thermal-resistance organic heat-conducting silicon material with high-temperature durability and preparation method thereof |
CN110760186A (en) * | 2019-09-18 | 2020-02-07 | 安徽若水化工有限公司 | Regenerated silicon material and preparation method thereof |
CN110791104A (en) * | 2019-09-19 | 2020-02-14 | 安徽若水化工有限公司 | High-temperature-resistant low-modulus silicon material and preparation method thereof |
CN111534358A (en) * | 2020-05-09 | 2020-08-14 | 中山市特好德润滑科技有限公司 | Heat-conducting lubricating grease and preparation method and application thereof |
CN111909519A (en) * | 2020-07-27 | 2020-11-10 | 深圳市新亚新材料有限公司 | Flexible heat-conducting silicon rubber and preparation method and application thereof |
CN114106560A (en) * | 2021-12-15 | 2022-03-01 | 东莞市新懿电子材料技术有限公司 | Preparation method and product of heat-conducting silica gel |
CN116120890A (en) * | 2023-02-23 | 2023-05-16 | 东莞市富颖电子材料有限公司 | Heat-conducting adhesive tape and preparation method thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20060079634A1 (en) * | 2003-05-30 | 2006-04-13 | Shin-Etsu Chemical Co., Ltd. | RTV heat conductive silicone rubber compositions |
CN104497575A (en) * | 2014-12-22 | 2015-04-08 | 广州市白云化工实业有限公司 | High-thermal-conductivity organosilicone mud and preparation method thereof |
CN105503930A (en) * | 2015-12-30 | 2016-04-20 | 肇庆皓明有机硅材料有限公司 | Soluble organic metal complex and preparing method and application thereof |
-
2017
- 2017-06-24 CN CN201710489798.4A patent/CN107141815B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20060079634A1 (en) * | 2003-05-30 | 2006-04-13 | Shin-Etsu Chemical Co., Ltd. | RTV heat conductive silicone rubber compositions |
CN104497575A (en) * | 2014-12-22 | 2015-04-08 | 广州市白云化工实业有限公司 | High-thermal-conductivity organosilicone mud and preparation method thereof |
CN105503930A (en) * | 2015-12-30 | 2016-04-20 | 肇庆皓明有机硅材料有限公司 | Soluble organic metal complex and preparing method and application thereof |
Non-Patent Citations (1)
Title |
---|
陈春荣: "低模量有机硅密封材料的制备与性能研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅱ辑》 * |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109385094A (en) * | 2018-10-29 | 2019-02-26 | 镇江亿维硅材料科技有限公司 | A kind of silicon rubber conducting masterbatch and its preparation method and application |
CN109627776A (en) * | 2018-11-14 | 2019-04-16 | 深圳市飞荣达科技股份有限公司 | Solidfied material made of heat-conductive silicone composition and its solidification |
CN110760186A (en) * | 2019-09-18 | 2020-02-07 | 安徽若水化工有限公司 | Regenerated silicon material and preparation method thereof |
CN110643180A (en) * | 2019-09-19 | 2020-01-03 | 安徽若水化工有限公司 | Low-thermal-resistance organic heat-conducting silicon material with high-temperature durability and preparation method thereof |
CN110791104A (en) * | 2019-09-19 | 2020-02-14 | 安徽若水化工有限公司 | High-temperature-resistant low-modulus silicon material and preparation method thereof |
CN111534358A (en) * | 2020-05-09 | 2020-08-14 | 中山市特好德润滑科技有限公司 | Heat-conducting lubricating grease and preparation method and application thereof |
CN111534358B (en) * | 2020-05-09 | 2022-03-29 | 中山市特好德润滑科技有限公司 | Heat-conducting lubricating grease and preparation method and application thereof |
CN111909519A (en) * | 2020-07-27 | 2020-11-10 | 深圳市新亚新材料有限公司 | Flexible heat-conducting silicon rubber and preparation method and application thereof |
CN114106560A (en) * | 2021-12-15 | 2022-03-01 | 东莞市新懿电子材料技术有限公司 | Preparation method and product of heat-conducting silica gel |
CN116120890A (en) * | 2023-02-23 | 2023-05-16 | 东莞市富颖电子材料有限公司 | Heat-conducting adhesive tape and preparation method thereof |
CN116120890B (en) * | 2023-02-23 | 2023-08-18 | 东莞市富颖电子材料有限公司 | Heat-conducting adhesive tape and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN107141815B (en) | 2020-03-24 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107141815A (en) | A kind of low modulus heat conduction organosilicon material of high temperature resistant and preparation method thereof | |
CN109517390A (en) | A kind of high performance organo-silicon material and preparation method thereof | |
CN102337033B (en) | Additive high-thermal-conductivity organic silicon electronic pouring sealant and preparation method thereof | |
CN103059576A (en) | High-heat-conductivity flexible silica gel gasket and preparation method thereof | |
CN104974711B (en) | High-temperature resistance organic silicon adhesive | |
CN109438987A (en) | High thermal-conductive silicone grease and preparation method thereof | |
CN105754342A (en) | Low-viscosity heat conducting silicone grease and preparation method thereof | |
CN103030976A (en) | Single-component heat-curing liquid silicone rubber and preparation method thereof | |
CN112961657B (en) | Composite heat conduction material and preparation method thereof, heat conduction gel and preparation method thereof | |
CN109971415B (en) | High-thermal-conductivity organic silicon adhesive and preparation method thereof | |
JP5155033B2 (en) | Thermally conductive silicone composition | |
CN110330947A (en) | A kind of thermally conductive gel of carbon nanotubes and its preparation and application | |
CN102093838A (en) | High-temperature cured two-component pouring sealant and preparation method thereof | |
CN107177345A (en) | A kind of heat conduction Silica hydrogel and preparation method | |
CN114410113B (en) | Flowing type fine heat-conducting silicone grease and preparation method thereof | |
CN107739513A (en) | A kind of heat-conducting silicone grease and its processing method and application | |
CN109535722A (en) | A kind of high-temperature resistant silicone material and preparation method thereof | |
JP2020007569A (en) | Thermally conductive sheet | |
CN109111740A (en) | A kind of high thermal conductivity graphene thermal solidity insulator interface material and preparation method thereof | |
CN114015117A (en) | Heat-conducting filler and anti-aging organic silicon heat-conducting gel prepared from heat-conducting filler | |
CN114958002A (en) | Heat-conducting silica gel and preparation method thereof | |
CN111363368A (en) | Fluid-like high-thermal-conductivity organic silicon gel and preparation method and application thereof | |
CN111944498A (en) | Heat-conducting gel with ultralow oil extraction amount and high flow rate performance and preparation method thereof | |
CN108148558A (en) | A kind of thermally conductive gel of graphene-containing and its preparation method and application | |
CN107513368A (en) | High temperature resistant and low-expansion heat conduction casting glue and preparation method and application |
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 | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CP01 | Change in the name or title of a patent holder |
Address after: 526072 Lianhua Town Development Zone, Dinghu District, Guangdong City, Zhaoqing province (three sets of Liantang village, Deng Wutou) Patentee after: Guangdong Haoming silicone materials Co., Ltd Address before: 526072 Lianhua Town Development Zone, Dinghu District, Guangdong City, Zhaoqing province (three sets of Liantang village, Deng Wutou) Patentee before: ZHAOQING HOMEEN ORGANIC SILICON MATERIAL Co.,Ltd. |
|
CP01 | Change in the name or title of a patent holder |