CN108410175A - A kind of preparation method of high heat conduction type thermal conductive silicon pad - Google Patents
A kind of preparation method of high heat conduction type thermal conductive silicon pad Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of high heat conduction type thermal conductive silicon pad, belong to Heat Conduction Material technical field.Score meter by weight weighs 10~20 parts of methyl vinyl silicone rubbers, 100~200 parts of modified micro-capsules successively, 50~70 parts of dimethicones, 10~30 parts of containing hydrogen silicone oils and 1~3 part of platinum catalyst, by methyl vinyl silicone rubber and dimethicone mixed grinding, obtain rubber silicone oil mixture, rubber silicone oil mixture is mixed with modified micro-capsule, and containing hydrogen silicone oil and platinum catalyst is added, is stirred, obtain base-material, after base-material is vacuumized, sulfidization molding is to get high heat conduction type thermal conductive silicon pad.High heat conduction type thermal conductive silicon pad prepared by technical solution of the present invention has the characteristics that excellent heat conductivility and insulation performance.
Description
Technical field
The invention discloses a kind of preparation methods of high heat conduction type thermal conductive silicon pad, belong to Heat Conduction Material technical field.
Background technology
In recent years, with scientific development, the fast development of microelectronic component, integration degree is higher and higher, component work
While making improved efficiency, heat also drastically accumulates, it is ensured that the reliability service of electric appliance, good heat dissipation is essential institute
This is solved the problems, such as so that there is an urgent need to high heat conduction proximate matter material.As the conventional thermal conductives material such as metal, inorganic material, though heat conductivility
It is good, but due to factors such as brittleness big, processing difficulties, conductions, limit its application field.And thermal-conductive polymer matrix composites because
Have many advantages, such as that light, corrosion-resistant, easy processing is considered as the ideal material that may replace conventional thermal conductive material for thermal control field
One of material.Heat conductive pad is high-performance gap filling Heat Conduction Material, is mainly used between electronic equipment and cooling fin or product casing
Transmit interface.With good sticky, flexible, good compression performance and with excellent pyroconductivity.It is set to use
Middle that the air between electronic original part and cooling fin can be made to be discharged completely, abundant to reach contact, heat dissipation effect obviously increases.
Heat conductive silica gel material is prepared at home mainly uses melt-blending process, since preparation method is relatively simple, so
Using universal, but in place of this method Shortcomings, such as in high filler loading capacity, poor processability, Article Stiffness Determination is bigger than normal, and filler divides
Dissipating property difference causes thermal conductivity not high.In addition to this, since thermal conductive silicon pad applies to be used as heat-transfer equipment in electronic equipment mostly, because
This, causes the appearance of equipment fault problem, thermal conductive silicon pad to also need to have good insulation performance to place electronic equipment short circuit,
Though but can be greatly improved with the addition heat conductivility of metal oxide, associated decreasing insulating influences its use
With development.
Therefore, how to improve traditional silicon pad heat conductivility and the bad disadvantage of insulation performance, to obtain more high combination property
Silicon pad, be its promote and application, meet industrial production demand urgent problem to be solved.
Invention content
The present invention solves the technical problem of：Heat conductivility and the bad disadvantage of insulation performance are padded for traditional silicon,
Provide a kind of preparation method of high heat conduction type thermal conductive silicon pad.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）By conduction oil and mixed glue solution in mass ratio 1：8~1：12 mixing, and the sodium sulphate of 3~5 times of heat conduction oil quality is added
Solution after being stirred, obtains micro-capsule blank, micro-capsule blank is cooled down, and the micro-capsule blank after cooling is pressed matter with formalin
Measure ratio 10：1~15：1 mixing, must pre-process micro-capsule blank, adjust the pH of pretreatment micro-capsule blank, and cure, and must pre-process micro-
Capsule, after pretreatment micro-capsule is filtered washing, freeze-drying obtains micro-capsule；
（2）By paraffin and pretreatment graphene oxide in mass ratio 5：1~5：2 mixing, and 0.2~0.6 times of Quality of Paraffin Waxes is added
Polyethylene wax, heating stirring mixing after, obtain mixing wax liquor；
（3）It will pretreatment zeolite and water in mass ratio 1：4~1：8 mixing, and 0.1~0.3 times of pretreatment zeolite quality is added
Aluminium chloride after being stirred, obtains zeolite mixture, adjusts zeolite mixture pH, and filtering obtains filter cake, and filtration cakes torrefaction is calcined,
Obtain modified zeolite；
（4）By micro-capsule with mix wax liquor in mass ratio 1：2~1：3 mixing, and the modified zeolite of 4~5 times of micro-capsule quality is added, in
After being stirred under nitrogen protection state, Freezing smashing, sieving obtains modified micro-capsule；
（5）Score meter by weight, weighs 10~20 parts of methyl vinyl silicone rubbers successively, 100~200 parts of modified micro-capsules, 50~
70 parts of dimethicones, 10~30 parts of containing hydrogen silicone oils and 1~3 part of platinum catalyst, by methyl vinyl silicone rubber and dimethyl
Silicone oil mixed grinding obtains rubber silicone oil mixture, and rubber silicone oil mixture mix with modified micro-capsule, and be added containing hydrogen silicone oil with
Platinum catalyst is stirred, and obtains base-material, and after base-material is vacuumized, sulfidization molding is to get high heat conduction type thermal conductive silicon pad.
Step（1）The conduction oil is biphenyl class conduction oil, any one in organosilicon conduction oil or benzene alkanes conduction oil
Kind.
Step（1）The mixed glue solution preparation method is by Arabic gum and gelatin in mass ratio 1：1~1：2 mixing, and
The water of 20~30 times of gelatin quality is added, is stirred, obtains mixed glue solution.
Step（2）The paraffin is the mineral wax mixture that carbon atom number is 24~32.
Step（2）The preparation method of the pretreatment graphene oxide is by graphene oxide and water in mass ratio 1：5~
1：8 mixing, obtain graphene oxide mixture, and graphene oxide mixture sonic oscillation filters, dry, must pre-process oxidation
Graphene.
Step（2）The molecular weight of the polyethylene wax is 1800~2500.
Step（3）The preparation method of the pretreatment zeolite is to crush zeolite, is sieved, and calcining obtains pretreatment zeolite.
Step（5）The dimethyl-silicon oil viscosity is 200~600cps.
Step（5）The hydrogen content of the containing hydrogen silicone oil is 10~30%.
The beneficial effects of the invention are as follows：
（1）The present invention contains heat conduction first when preparing high heat conduction type thermal conductive silicon pad using for micro-capsule and mixing wax liquor in micro-capsule
Oil can form one layer of heat conduction oil reservoir after being added in product in interiors of products, to make the heat-conducting effect of product improve, and
Since oil reservoir insulation performance is preferable, to make the insulation performance of product improve, secondly, mix wax liquor in containing light component paraffin with
And graphene oxide, graphene oxide can float up to product surface in product preparation process with light component paraffin, to make production
The heat conductivility on product surface improves, and since the presence of light component paraffin can be such that product still has after graphene oxide is added
Preferable insulation performance, to improve the insulation performance of product；
（2）Modified zeolite is added when preparing high heat conduction type thermal conductive silicon pad in the present invention, and hydrogen-oxygen has been adsorbed in one side modified zeolite
Change aluminium, and after calcined, aluminium hydroxide is changed into the calcining material containing Alpha-alumina and is adsorbed in zeolite, to make zeolite have
There is preferable thermal conductivity, and then after being added in product, the heat conductivility of product can be made to further increase, it is on the other hand, modified
Zeolite still contains a large amount of holes after calcining in zeolite, to which when preparing modified micro-capsule, modified zeolite can absorb part
The conduction oil contained in micro-capsule, and then the heat conductivility of zeolite further increases, the raising of zeolite surface lubricity can be uniformly distributed
In product system, and preferable thermal conducting path is formed in the product, the heat conductivility of product is made to further increase；
（3）The present invention uses polyethylene wax when preparing high heat conduction type thermal conductive silicon pad, and polyethylene wax can be in product preparation process
Melt, to play the role of good internal lubrication, to make heat filling inside system be uniformly distributed in product, and then makes
The heat conductivility of product improves, and after polyethylene wax cools and solidifies, can a certain amount of conduction oil be coated on polyethylene wax
In, to make polyethylene wax that there is certain conductive force, and then the thermal conductivity of product is made to further increase.
Specific implementation mode
By graphene oxide and water in mass ratio 1：5~1：8 mixing, obtain graphene oxide mixture, by graphene oxide
Under conditions of frequency is 55~65kHz after 15~20min of sonic oscillation, filtering obtains filter cake, is in temperature by filter cake mixture
Under conditions of 70~80 DEG C after dry 20~40min, pretreatment graphene oxide is obtained；Zeolite is moved into pulverizer to crush, crosses 100
~180 mesh sieve, obtain refinement zeolite, will refinement zeolite move into calcining furnace, in temperature be 400~600 DEG C under conditions of calcining 15~
After 30min, pretreatment zeolite is obtained；By conduction oil and mixed glue solution in mass ratio 1：8~1：12 are mixed in beaker, and to beaker
The metabisulfite solution that the middle mass fraction that 3~5 times of heat conduction oil quality is added is 25~35% is 40~45 DEG C in temperature, and rotating speed is
Under conditions of 200~300r/min, after being stirred 20~50min, micro-capsule blank is obtained, micro-capsule blank is cooled to 15~20 DEG C
Afterwards, the formalin in mass ratio 10 for being 30~40% with mass fraction by the micro-capsule blank after cooling：1~15：1 mixing, Yu Wen
Degree is 15~22 DEG C, under conditions of rotating speed is 200~300r/min, after being stirred 20~30min, must pre-process micro-capsule base
Material, after the sodium hydroxide solution for being 5~8% with mass fraction adjusts the pH to 7.2~8.2 of pretreatment micro-capsule blank, and in temperature
After curing 30~40min under conditions of being 10~15 DEG C, pretreatment micro-capsule is obtained, pretreatment micro-capsule is filtered after washing 5~8 times,
Freeze-drying, obtains micro-capsule；By paraffin and pretreatment graphene oxide in mass ratio 5：1~5：2 mixing, and to paraffin and pre-process
In the mixture of graphene oxide be added 0.2~0.6 times of Quality of Paraffin Waxes polyethylene wax, in temperature be 100~120 DEG C, rotating speed
Under conditions of 200~300r/min, after being stirred 20~30min, mixing wax liquor is obtained；Pretreatment zeolite is pressed into quality with water
Than 1：4~1：8 mixing, and the chlorination for pre-processing 0.1~0.3 times of zeolite quality is added into the mixture of pretreatment zeolite and water
Aluminium is 40~65 DEG C in temperature, after rotating speed is stirred 30~40min under conditions of being 300~400r/min, obtains zeolite mixing
Object, after the sodium hydroxide solution for being 10~12% with mass fraction adjusts zeolite mixture pH to 5.0~7.0, filtering obtains filter residue,
Filter residue is moved into drying box, under conditions of being 80~90 DEG C in temperature after dry 20~30min, desciccate is obtained, is produced dry
Under conditions of object is 1000~1200 DEG C in temperature after 50~90min of calcining, modified zeolite is obtained；By micro-capsule with mix wax liquor by matter
Measure ratio 1：2~1：3 are mixed in flask, and the modified zeolite of 4~5 times of micro-capsule quality is added into flask, and to flask with 10
The rate of~15mL/min is passed through nitrogen, is 90~120 DEG C in temperature, under conditions of rotating speed is 230~330r/min, stirring is mixed
After closing 30~40min, micro-capsule zeolite mixture is obtained, by micro-capsule zeolite mixture Freezing smashing, 40~150 mesh sieve is crossed, obtains modification
Micro-capsule；Score meter by weight, weighs 10~20 parts of methyl vinyl silicone rubbers successively, 100~200 parts of modified micro-capsules, and 50~70
Part dimethicone, 10~30 parts of containing hydrogen silicone oils and 1~3 part of platinum catalyst, by methyl vinyl silicone rubber and dimethyl-silicon
Oil moves into grinder, after 20~30min of mixed grinding, obtains rubber silicone oil mixture, and rubber silicone oil mixture and modification is micro-
Capsule is mixed in blender, and containing hydrogen silicone oil and platinum catalyst are added into blender, is 50~70 DEG C in temperature, rotating speed is
After being stirred 50~80min under conditions of 230~300r/min, obtain base-material, after base-material is vacuumized, in temperature be 180~
Sulfidization molding is to get high heat conduction type thermal conductive silicon pad under conditions of 220 DEG C.The conduction oil is biphenyl class conduction oil, and organosilicon is led
Any one in deep fat or benzene alkanes conduction oil.The mixed glue solution preparation method be by Arabic gum and gelatin in mass ratio
1：1~1：2 mixing, and the water of 20~30 times of gelatin quality is added, it is stirred, obtains mixed glue solution.The paraffin is carbon atom
The mineral wax mixture that number is 24~32.The molecular weight of the polyethylene wax is 1800~2500.The dimethyl-silicon oil viscosity is
200~600cps.The hydrogen content of the containing hydrogen silicone oil is 10~30%.
By graphene oxide and water in mass ratio 1：8 mixing, obtain graphene oxide mixture, by graphene oxide mixture
Under conditions of frequency is 65kHz after sonic oscillation 20min, filtering obtains filter cake, is done under conditions of being 80 DEG C in temperature by filter cake
After dry 40min, pretreatment graphene oxide is obtained；Zeolite is moved into pulverizer to crush, 180 mesh sieve is crossed, obtains refinement zeolite, will refine
Zeolite moves into calcining furnace, under conditions of being 600 DEG C in temperature after calcining 30min, obtains pretreatment zeolite；By conduction oil and epoxy glue
Liquid in mass ratio 1：12 are mixed in beaker, and the sodium sulphate that the mass fraction of 5 times of heat conduction oil quality is 35% is added into beaker
Solution is 45 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 50min, micro-capsule blank is obtained, by micro-capsule base
After material is cooled to 20 DEG C, the formalin in mass ratio 15 for being 40% with mass fraction by the micro-capsule blank after cooling：1 mixing, in
Temperature is 22 DEG C, under conditions of rotating speed is 300r/min, after being stirred 30min, must pre-process micro-capsule blank, use mass fraction
After pH to 8.2 for 8% sodium hydroxide solution adjusting pretreatment micro-capsule blank, and cure under conditions of being 15 DEG C in temperature
After 40min, pretreatment micro-capsule is obtained, pretreatment micro-capsule is filtered after washing 8 times, freeze-drying obtains micro-capsule；By paraffin and pretreatment
Graphene oxide in mass ratio 5：2 mixing, and Quality of Paraffin Waxes 0.6 is added with the mixture of pretreatment graphene oxide to paraffin
Polyethylene wax again is 120 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 30min, obtains mixing wax liquor；
It will pretreatment zeolite and water in mass ratio 1：8 mixing, and pretreatment zeolite matter is added into the mixture of pretreatment zeolite and water
The aluminium chloride of 0.3 times of amount is 65 DEG C in temperature, after rotating speed is stirred 40min under conditions of being 400r/min, obtains zeolite mixing
Object, after the sodium hydroxide solution for being 10% with mass fraction adjusts zeolite mixture pH to 5.0, filtering obtains filter residue, filter residue is moved
Enter drying box, under the conditions of at a temperature of 90 °C after dry 30min, obtain desciccate, by desciccate in temperature be 1200 DEG C
Under conditions of calcining 90min after, obtain modified zeolite；By micro-capsule with mix wax liquor in mass ratio 1：3 are mixed in flask, and to burning
The modified zeolite of 5 times of micro-capsule quality is added in bottle, then nitrogen is passed through with the rate of 15mL/min to flask, in temperature be 120 DEG C,
Under conditions of rotating speed is 330r/min, after being stirred 40min, micro-capsule zeolite mixture is obtained, micro-capsule zeolite mixture is freezed
It crushes, crosses 40 mesh sieve, obtain modified micro-capsule；Score meter by weight weighs 20 parts of methyl vinyl silicone rubbers, 200 parts of modifications successively
Micro-capsule, 70 parts of dimethicones, 30 parts of containing hydrogen silicone oils and 3 parts of platinum catalysts, by methyl vinyl silicone rubber and dimethyl-silicon
Oil moves into grinder, after mixed grinding 30min, obtains rubber silicone oil mixture, and rubber silicone oil mixture and modified micro-capsule are mixed
Together in blender, and containing hydrogen silicone oil and platinum catalyst are added into blender, in temperature be 70 DEG C, rotating speed 300r/min
Under conditions of be stirred 80min after, obtain base-material, after base-material is vacuumized, in temperature be 220 DEG C under conditions of sulfidization molding,
Up to high heat conduction type thermal conductive silicon pad.The conduction oil is biphenyl class conduction oil.The mixed glue solution preparation method is will be Arabic
Glue and gelatin in mass ratio 1：2 mixing, and the water of 30 times of gelatin quality is added, it is stirred, obtains mixed glue solution.The paraffin is
The mineral wax mixture that carbon atom number is 26~30.The molecular weight of the polyethylene wax is 2000~2400.The dimethicone
Viscosity is 300~500cps.The hydrogen content of the containing hydrogen silicone oil is 30%.
By graphene oxide and water in mass ratio 1：8 mixing, obtain graphene oxide mixture, by graphene oxide mixture
Under conditions of frequency is 65kHz after sonic oscillation 20min, filtering obtains filter cake, is done under conditions of being 80 DEG C in temperature by filter cake
After dry 40min, pretreatment graphene oxide is obtained；Zeolite is moved into pulverizer to crush, 180 mesh sieve is crossed, obtains refinement zeolite, will refine
Zeolite moves into calcining furnace, under conditions of being 600 DEG C in temperature after calcining 30min, obtains pretreatment zeolite；By paraffin and pretreatment oxygen
Graphite alkene in mass ratio 5：2 mixing, and 0.6 times of Quality of Paraffin Waxes is added with the mixture of pretreatment graphene oxide to paraffin
Polyethylene wax, in temperature be 120 DEG C, rotating speed be 300r/min under conditions of, after being stirred 30min, obtain mixing wax liquor；It will
Pre-process zeolite and water in mass ratio 1：8 mixing, and pretreatment zeolite quality is added into the mixture of pretreatment zeolite and water
0.3 times of aluminium chloride is 65 DEG C in temperature, after rotating speed is stirred 40min under conditions of being 400r/min, obtains zeolite mixing
Object, after the sodium hydroxide solution for being 10% with mass fraction adjusts zeolite mixture pH to 5.0, filtering obtains filter residue, filter residue is moved
Enter drying box, under the conditions of at a temperature of 90 °C after dry 30min, obtain desciccate, by desciccate in temperature be 1200 DEG C
Under conditions of calcining 90min after, obtain modified zeolite；Score meter by weight, weighs 20 parts of methyl vinyl silicone rubbers successively, 65 parts
Wax liquor, 100 parts of modified zeolites, 70 parts of dimethicones, 30 parts of containing hydrogen silicone oils and 3 parts of platinum catalysts are mixed, by ethylene methacrylic
Base silicon rubber is moved into dimethicone in grinder, after mixed grinding 30min, rubber silicone oil mixture is obtained, by rubber silicone oil
Mixture is added in blender, and containing hydrogen silicone oil and platinum catalyst are added into blender, is 70 DEG C in temperature, rotating speed is
After being stirred 80min under conditions of 300r/min, base-material is obtained, after base-material is vacuumized, sulphur under conditions of being 220 DEG C in temperature
Chemical conversion type is to get high heat conduction type thermal conductive silicon pad.The conduction oil is biphenyl class conduction oil.The mixed glue solution preparation method is will
Arabic gum and gelatin in mass ratio 1：2 mixing, and the water of 30 times of gelatin quality is added, it is stirred, obtains mixed glue solution.It is described
Paraffin is the mineral wax mixture that carbon atom number is 26~30.The molecular weight of the polyethylene wax is 2000~2400.The diformazan
Base silicon oil viscosity is 300~500cps.The hydrogen content of the containing hydrogen silicone oil is 30%.
By graphene oxide and water in mass ratio 1：8 mixing, obtain graphene oxide mixture, by graphene oxide mixture
Under conditions of frequency is 65kHz after sonic oscillation 20min, filtering obtains filter cake, is done under conditions of being 80 DEG C in temperature by filter cake
After dry 40min, pretreatment graphene oxide is obtained；Zeolite is moved into pulverizer to crush, 180 mesh sieve is crossed, obtains refinement zeolite, will refine
Zeolite moves into calcining furnace, under conditions of being 600 DEG C in temperature after calcining 30min, obtains pretreatment zeolite；By conduction oil and epoxy glue
Liquid in mass ratio 1：12 are mixed in beaker, and the sodium sulphate that the mass fraction of 5 times of heat conduction oil quality is 35% is added into beaker
Solution is 45 DEG C in temperature, under conditions of rotating speed is 300r/min, after being stirred 50min, micro-capsule blank is obtained, by micro-capsule base
After material is cooled to 20 DEG C, the formalin in mass ratio 15 for being 40% with mass fraction by the micro-capsule blank after cooling：1 mixing, in
Temperature is 22 DEG C, under conditions of rotating speed is 300r/min, after being stirred 30min, must pre-process micro-capsule blank, use mass fraction
After pH to 8.2 for 8% sodium hydroxide solution adjusting pretreatment micro-capsule blank, and cure under conditions of being 15 DEG C in temperature
After 40min, pretreatment micro-capsule is obtained, pretreatment micro-capsule is filtered after washing 8 times, freeze-drying obtains micro-capsule；By paraffin and pretreatment
Graphene oxide in mass ratio 5：2 mixing are 120 DEG C in temperature, under conditions of rotating speed is 300r/min, are stirred 30min
Afterwards, mixing wax liquor is obtained；It will pretreatment zeolite and water in mass ratio 1：8 mixing, and add into the mixture of pretreatment zeolite and water
The aluminium chloride for entering to pre-process 0.3 times of zeolite quality is 65 DEG C in temperature, and rotating speed is stirred under conditions of being 400r/min
After 40min, zeolite mixture is obtained, the sodium hydroxide solution for being 10% with mass fraction adjusts mistake after zeolite mixture pH to 5.0
Filter, obtains filter residue, filter residue is moved into drying box, under the conditions of at a temperature of 90 °C after dry 30min, obtain desciccate, will dry
Under conditions of product is 1200 DEG C in temperature after calcining 90min, modified zeolite is obtained；By micro-capsule with mix wax liquor in mass ratio 1：3
It is mixed in flask, and the modified zeolite of 5 times of micro-capsule quality is added into flask, then be passed through to flask with the rate of 15mL/min
Nitrogen is 120 DEG C in temperature, under conditions of rotating speed is 330r/min, after being stirred 40min, obtains micro-capsule zeolite mixture, will
Micro-capsule zeolite mixture Freezing smashing crosses 40 mesh sieve, obtains modified micro-capsule；Score meter by weight weighs 20 parts of ethylene methacrylics successively
Base silicon rubber, 200 parts of modified micro-capsules, 70 parts of dimethicones, 30 parts of containing hydrogen silicone oils and 3 parts of platinum catalysts, by ethylene methacrylic
Base silicon rubber is moved into dimethicone in grinder, after mixed grinding 30min, rubber silicone oil mixture is obtained, by rubber silicone oil
Mixture is mixed in modified micro-capsule in blender, and containing hydrogen silicone oil and platinum catalyst are added into blender, is in temperature
70 DEG C, rotating speed be 300r/min under conditions of be stirred 80min after, obtain base-material, after base-material is vacuumized, in temperature be 220
Sulfidization molding is to get high heat conduction type thermal conductive silicon pad under conditions of DEG C.The conduction oil is biphenyl class conduction oil.The mixed glue solution
Preparation method is by Arabic gum and gelatin in mass ratio 1：2 mixing, and the water of 30 times of gelatin quality is added, it is stirred, obtains
Mixed glue solution.The paraffin is the mineral wax mixture that carbon atom number is 26~30.The dimethyl-silicon oil viscosity be 300~
500cps.The hydrogen content of the containing hydrogen silicone oil is 30%.
Zeolite is moved into pulverizer to crush, 180 mesh sieve is crossed, obtains refinement zeolite, refinement zeolite is moved into calcining furnace, in temperature
After calcining 30min under conditions of being 600 DEG C, pretreatment zeolite is obtained；By conduction oil and mixed glue solution in mass ratio 1：12 are mixed in
In beaker, and the metabisulfite solution that the mass fraction of 5 times of heat conduction oil quality is 35% is added into beaker, is 45 DEG C in temperature, turns
Under conditions of speed is 300r/min, after being stirred 50min, micro-capsule blank is obtained, after micro-capsule blank is cooled to 20 DEG C, will be cooled down
The formalin in mass ratio 15 that micro-capsule blank afterwards is 40% with mass fraction：1 mixing is 22 DEG C in temperature, and rotating speed is
Under conditions of 300r/min, after being stirred 30min, micro-capsule blank must be pre-processed, the sodium hydroxide for being 8% with mass fraction is molten
Liquid adjust pretreatment micro-capsule blank pH to 8.2 after, and in temperature be 15 DEG C under conditions of solidification 40min after, must pre-process micro-
Capsule filters pretreatment micro-capsule after washing 8 times, and freeze-drying obtains micro-capsule；It will pretreatment zeolite and water in mass ratio 1：8 mixing,
And the aluminium chloride of 0.3 times of zeolite quality of pretreatment is added into the mixture of pretreatment zeolite and water, in temperature be 65 DEG C, rotating speed
After being stirred 40min under conditions of 400r/min, zeolite mixture is obtained, the sodium hydroxide solution for being 10% with mass fraction
It is filtered after adjusting zeolite mixture pH to 5.0, obtains filter cake, filter cake is moved into drying box, it is dry under the conditions of at a temperature of 90 °C
After 30min, desciccate is obtained, under conditions of being 1200 DEG C in temperature by desciccate after calcining 90min, obtains modified zeolite；It will
Micro-capsule is added in flask, and the modified zeolite of 5 times of micro-capsule quality is added into flask, then logical with the rate of 15mL/min to flask
Enter nitrogen, be 120 DEG C in temperature, under conditions of rotating speed is 330r/min, after being stirred 40min, obtain micro-capsule zeolite mixture,
By micro-capsule zeolite mixture Freezing smashing, 40 mesh sieve is crossed, modified micro-capsule is obtained；Score meter by weight weighs 20 parts of methyl second successively
Alkenyl silicon rubber, 200 parts of modified micro-capsules, 70 parts of dimethicones, 30 parts of containing hydrogen silicone oils and 3 parts of platinum catalysts, by methyl second
Alkenyl silicon rubber is moved into dimethicone in grinder, after mixed grinding 30min, rubber silicone oil mixture is obtained, by rubber silicon
Oily mixture is mixed in modified micro-capsule in blender, and containing hydrogen silicone oil and platinum catalyst are added into blender, in temperature
It is 70 DEG C, after rotating speed is stirred 80min under conditions of being 300r/min, obtains base-material, after base-material is vacuumized, be in temperature
Sulfidization molding is to get high heat conduction type thermal conductive silicon pad under conditions of 220 DEG C.The conduction oil is biphenyl class conduction oil.The mixing
Glue preparation method is by Arabic gum and gelatin in mass ratio 1：2 mixing, and the water of 30 times of gelatin quality is added, stirring is mixed
It closes, obtains mixed glue solution.300~500cps of the dimethyl-silicon oil viscosity.The hydrogen content of the containing hydrogen silicone oil is 30%.
By graphene oxide and water in mass ratio 1：8 mixing, obtain graphene oxide mixture, by graphene oxide mixture
Under conditions of frequency is 65kHz after sonic oscillation 20min, filtering obtains filter cake, is done under conditions of being 80 DEG C in temperature by filter cake
After dry 40min, pretreatment graphene oxide is obtained；By conduction oil and mixed glue solution in mass ratio 1：12 are mixed in beaker, and to
The metabisulfite solution that the mass fraction of 5 times of heat conduction oil quality is 35% is added in beaker, in temperature be 45 DEG C, rotating speed 300r/
Under conditions of min, after being stirred 50min, micro-capsule blank is obtained, after micro-capsule blank is cooled to 20 DEG C, by the micro-capsule after cooling
The formalin in mass ratio 15 that blank is 40% with mass fraction：1 mixing is 22 DEG C in temperature, and rotating speed is the item of 300r/min
Under part, after being stirred 30min, micro-capsule blank must be pre-processed, the sodium hydroxide solution for being 8% with mass fraction adjusts pretreatment
After the pH to 8.2 of micro-capsule blank, and in temperature be 15 DEG C under conditions of solidification 40min after, obtain pretreatment micro-capsule, will pre-process micro-
After capsule suction filtration washing 8 times, freeze-drying obtains micro-capsule；By paraffin and pretreatment graphene oxide in mass ratio 5：2 mixing, and to
Paraffin and the polyethylene wax that 0.6 times of Quality of Paraffin Waxes is added in the mixture of pretreatment graphene oxide, are 120 DEG C in temperature, turn
Under conditions of speed is 300r/min, after being stirred 30min, mixing wax liquor is obtained；By micro-capsule with mix wax liquor in mass ratio 1：3 is mixed
Nitrogen is passed through with the rate of 15mL/min together in flask, then to flask, is 120 DEG C in temperature, rotating speed is the item of 330r/min
Under part, after being stirred 40min, microcapsule mixture is obtained, by microcapsule mixture Freezing smashing, 150 mesh sieve is crossed, obtains modified micro-capsule；
Score meter by weight weighs 20 parts of methyl vinyl silicone rubbers successively, and 200 parts of modified micro-capsules, 70 parts of dimethicones, 30 parts contain
Hydrogen silicone oil and 3 parts of platinum catalysts move into methyl vinyl silicone rubber and dimethicone in grinder, mixed grinding
After 30min, rubber silicone oil mixture is obtained, rubber silicone oil mixture and modified micro-capsule are mixed in blender, and to blender
Middle addition containing hydrogen silicone oil and platinum catalyst are 70 DEG C in temperature, and rotating speed is stirred 80min under conditions of being 300r/min
Afterwards, base-material is obtained, after base-material is vacuumized, sulfidization molding is to get high heat conduction type thermal conductive silicon pad under conditions of being 220 DEG C in temperature.
The conduction oil is biphenyl class conduction oil.The mixed glue solution preparation method is by Arabic gum and gelatin in mass ratio 1：2 is mixed
It closes, and the water of 30 times of gelatin quality is added, be stirred, obtain mixed glue solution.The paraffin is the stone that carbon atom number is 26~30
Wax mixture.The molecular weight of the polyethylene wax is 2000~2400.The dimethyl-silicon oil viscosity is 300~500cps.Institute
The hydrogen content for stating containing hydrogen silicone oil is 30%.
Comparative example：The thermal conductive silicon pad of Shenzhen Science and Technology Ltd. production.
The high heat conduction type thermal conductive silicon pad of 1 to 5 gained of example and comparative example product are subjected to performance detection, specific detection method
It is as follows：
Heat conductivility：Test specimen thermal conductivity is detected according to GB/T 11205；
Insulation performance：Test specimen volume resistivity is detected according to GB/T1410.
Specific testing result is as shown in table 1：
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Thermal conductivity/（W/（m·K）） | 3.12 | 1.64 | 2.73 | 2.34 | 1.95 | 0.87 |
| Volume resistivity/（103Ω·cm） | 3.13 | 1.37 | 2.84 | 2.36 | 1.86 | 0.05 |
By 1 testing result of table it is found that high heat conduction type thermal conductive silicon pad prepared by technical solution of the present invention has excellent heat conductivility
And the characteristics of insulation performance, it has broad prospects in the development that thermal conductive silicon pads industry.
Claims (9)
1. a kind of preparation method of high heat conduction type thermal conductive silicon pad, which is characterized in that specifically preparation method is：
（1）By conduction oil and mixed glue solution in mass ratio 1：8~1：12 mixing, and the sodium sulphate of 3~5 times of heat conduction oil quality is added
Solution after being stirred, obtains micro-capsule blank, micro-capsule blank is cooled down, and the micro-capsule blank after cooling is pressed matter with formalin
Measure ratio 10：1~15：1 mixing, must pre-process micro-capsule blank, adjust the pH of pretreatment micro-capsule blank, and cure, and must pre-process micro-
Capsule, after pretreatment micro-capsule is filtered washing, freeze-drying obtains micro-capsule；
（2）By paraffin and pretreatment graphene oxide in mass ratio 5：1~5：2 mixing, and 0.2~0.6 times of Quality of Paraffin Waxes is added
Polyethylene wax, heating stirring mixing after, obtain mixing wax liquor；
（3）It will pretreatment zeolite and water in mass ratio 1：4~1：8 mixing, and 0.1~0.3 times of pretreatment zeolite quality is added
Aluminium chloride after being stirred, obtains zeolite mixture, adjusts zeolite mixture pH, and filtering obtains filter cake, and filtration cakes torrefaction is calcined,
Obtain modified zeolite；
（4）By micro-capsule with mix wax liquor in mass ratio 1：2~1：3 mixing, and the modified zeolite of 4~5 times of micro-capsule quality is added, in
After being stirred under nitrogen protection state, Freezing smashing, sieving obtains modified micro-capsule；
（5）Score meter by weight, weighs 10~20 parts of methyl vinyl silicone rubbers successively, 100~200 parts of modified micro-capsules, 50~
70 parts of dimethicones, 10~30 parts of containing hydrogen silicone oils and 1~3 part of platinum catalyst, by methyl vinyl silicone rubber and dimethyl
Silicone oil mixed grinding obtains rubber silicone oil mixture, and rubber silicone oil mixture mix with modified micro-capsule, and be added containing hydrogen silicone oil with
Platinum catalyst is stirred, and obtains base-material, and after base-material is vacuumized, sulfidization molding is to get high heat conduction type thermal conductive silicon pad.
2. a kind of preparation method of high heat conduction type thermal conductive silicon pad according to claim 1, it is characterised in that：Step（1）Institute
It is biphenyl class conduction oil to state conduction oil, any one in organosilicon conduction oil or benzene alkanes conduction oil.
3. a kind of preparation method of high heat conduction type thermal conductive silicon pad according to claim 1, it is characterised in that：Step（1）Institute
It is by Arabic gum and gelatin in mass ratio 1 to state mixed glue solution preparation method：1~1：2 mixing, and gelatin quality 20~30 is added
Water again, is stirred, obtains mixed glue solution.
4. a kind of preparation method of high heat conduction type thermal conductive silicon pad according to claim 1, it is characterised in that：Step（2）Institute
It is the mineral wax mixture that carbon atom number is 24~32 to state paraffin.
5. a kind of preparation method of high heat conduction type thermal conductive silicon pad according to claim 1, it is characterised in that：Step（2）Institute
The preparation method for stating pretreatment graphene oxide is by graphene oxide and water in mass ratio 1：5~1：8 mixing, obtain graphite oxide
Alkene mixture filters graphene oxide mixture sonic oscillation, dry, obtains pretreatment graphene oxide.
6. a kind of preparation method of high heat conduction type thermal conductive silicon pad according to claim 1, it is characterised in that：Step（2）Institute
The molecular weight for stating polyethylene wax is 1800~2500.
7. a kind of preparation method of high heat conduction type thermal conductive silicon pad according to claim 1, it is characterised in that：Step（3）Institute
The preparation method for stating pretreatment zeolite is to crush zeolite, is sieved, and calcining obtains pretreatment zeolite.
8. a kind of preparation method of high heat conduction type thermal conductive silicon pad according to claim 1, it is characterised in that：Step（5）Institute
It is 200~600cps to state dimethyl-silicon oil viscosity.
9. a kind of preparation method of high heat conduction type thermal conductive silicon pad according to claim 1, it is characterised in that：Step（5）Institute
The hydrogen content for stating containing hydrogen silicone oil is 10~30%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824949A (en) * | 2019-01-29 | 2019-05-31 | 常州市讯德电器有限公司 | A kind of preparation method of wear-resisting type railroad track composite rubber material |
| CN110540706A (en) * | 2019-09-05 | 2019-12-06 | 上海阿莱德实业股份有限公司 | Preparation method of heat-conducting interface material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831181A (en) * | 2010-05-21 | 2010-09-15 | 浙江三元电子科技有限公司 | Addition thermal conductive insulation silicon rubber composite material and preparation method thereof |
| CN103436019A (en) * | 2013-08-23 | 2013-12-11 | 深圳市鸿富诚屏蔽材料有限公司 | High-heat-conductivity electric-insulation heat-conducting silica gel gasket and preparation method thereof |
| CN103740108A (en) * | 2014-01-17 | 2014-04-23 | 华为技术有限公司 | High-thermal-conductivity elastic composite material and preparation method thereof |
| CN106279829A (en) * | 2016-08-20 | 2017-01-04 | 张伟 | A kind of Graphene composite rubber material of heat-conductivity conducting and preparation method thereof |
-
2018
- 2018-03-28 CN CN201810263901.8A patent/CN108410175A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831181A (en) * | 2010-05-21 | 2010-09-15 | 浙江三元电子科技有限公司 | Addition thermal conductive insulation silicon rubber composite material and preparation method thereof |
| CN103436019A (en) * | 2013-08-23 | 2013-12-11 | 深圳市鸿富诚屏蔽材料有限公司 | High-heat-conductivity electric-insulation heat-conducting silica gel gasket and preparation method thereof |
| CN103740108A (en) * | 2014-01-17 | 2014-04-23 | 华为技术有限公司 | High-thermal-conductivity elastic composite material and preparation method thereof |
| CN106279829A (en) * | 2016-08-20 | 2017-01-04 | 张伟 | A kind of Graphene composite rubber material of heat-conductivity conducting and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 周文英，等: "《聚合物基导热复合材料》", 30 June 2017, 国防工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824949A (en) * | 2019-01-29 | 2019-05-31 | 常州市讯德电器有限公司 | A kind of preparation method of wear-resisting type railroad track composite rubber material |
| CN110540706A (en) * | 2019-09-05 | 2019-12-06 | 上海阿莱德实业股份有限公司 | Preparation method of heat-conducting interface material |
| CN110540706B (en) * | 2019-09-05 | 2022-06-10 | 上海阿莱德实业股份有限公司 | Preparation method of heat-conducting interface material |
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