CN105838077A - Surface treatment method of graphene used for producing heat conducting silicon sheets - Google Patents

Surface treatment method of graphene used for producing heat conducting silicon sheets Download PDF

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CN105838077A
CN105838077A CN201610209007.3A CN201610209007A CN105838077A CN 105838077 A CN105838077 A CN 105838077A CN 201610209007 A CN201610209007 A CN 201610209007A CN 105838077 A CN105838077 A CN 105838077A
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graphene
graphite alkene
silica gel
activated graphite
surface treatment
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刘诚
郎咸鑫
谭培于
王天勇
吴先信
柴建功
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SHENZHEN EVOPUTE INDUSTRY MATERIAL Co Ltd
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    • C08L83/00Compositions 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
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
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    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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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    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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Abstract

The invention discloses a surface treatment method of graphene used for producing heat conducting silicon sheets. The method comprises the following steps: 1, activating graphene: preparing an H2O2 and 98% concentrated H2SO4 mixed solution containing, by mass, 10-60% of H2O2 and 40-90% of concentrated H2SO4, adding 1-30 mass% of graphene, heating the obtained solution to 50-110DEG C, continuously stirring the solution for 10-80min, separating activated graphene, washing the separated activated graphene with water, and airing or drying the washed activated graphene to obtain active graphene; and 2, carrying out surface treatment on the active graphene: carrying out surface treatment on the active graphene prepared in step 1 through a silane coupling agent or a terminated 107 adhesive. The invention also discloses a graphene heat conduction silicon sheet made of graphene obtained through the graphene surface treatment method.

Description

A kind of surface treatment method of the Graphene for producing heat-conducting silica gel sheet
Technical field
The invention belongs to the preparation field of heat-conducting silica gel sheet, former specifically for preparing the Graphene of heat-conducting silica gel sheet Material and heat-conducting silica gel sheet itself.
Background technology
Along with various electronics, the multifunction of electric equipment products and miniaturization, the negative effect that heat dissipation problem brings The most serious.Due to internal temperature raising electronic component service life reduction, chip processing speed can be brought to slow down, The series of problems such as idle power increase, heat dissipation design has become the important composition portion of hyundai electronics electrical apparatus industry Point.Using fin to derive heat is one of the most frequently used heat dissipation design, but due to fin and thermal source it Between there is inevitable gap, significantly reduce radiating effect.
Thermal interfacial material (TIM), is also called Heat Conduction Material, be used for filling between thermal source with fin engage or The microvoid produced during contact and the hole of surface irregularity, improve between fin and thermal source greatly Real contact area, reduces system thermal resistance, improves the performance of device heat radiation.TIM include heat-conducting silicone grease, The variety classeses such as heat-conducting silica gel sheet, thermal conductive adhesive, phase-change material.
Heat-conducting silica gel sheet, is a kind of novel TIM occurred in recent years.Have due to self compared with tradition TIM Standby excellent elasticity, can be fitted in different materials surface in the case of applying pressure closely, thus greatly Amplitude reduction interface contact heat resistance.Simultaneously as heat-conducting silica gel sheet possesses elasticity, can be at a lot of electronics electricity Serve as cushion in device product, reduce electric equipment products internal structure caused by vibrations and collision and break Bad.Further, since heat-conducting silica gel sheet is originally as solid material, interiors of products uniform component is stable, thus keeps away Exempted to occur heat-conducting silicone grease layering, become dry, the phenomenon such as trickling, electric equipment products is greatly improved Stability and reliability.
Conventional heat-conducting silica gel sheet is many with metal-oxide, hydroxide, nitride as heat filling, including oxygen Change zinc, aluminium oxide, silicon dioxide, aluminium hydroxide, magnesium hydroxide, aluminium nitride etc., metal-oxide and hydrogen Oxide is cheap, but heat conductivity is relatively low, the most only 10~40W/m K, heat conduction prepared therefrom Silica gel piece heat conductivity generally only has 1~4W/m K;The heat conductivity of nitride is higher, reaches 200~400 W/m K, heat-conducting silica gel sheet heat conductivity prepared therefrom is generally up to 5~7W/m K, but this type of material Expensive, it is not suitable for producing in enormous quantities.Find new heat filling and become the primary of current TIM industry Problem.
Graphene, as a kind of brand-new Heat Conduction Material, has high heat conductivity (5000W/m K), Have the mechanical property of excellence simultaneously, be the desirable feedstock of a kind of heat-conductive composite material.But due to Graphene Specific surface area the hugest, oil factor is high, causes its addition in Polymer Systems to be difficult to more than 5% Above.It is contemplated that create a kind of novel surface processing method, improve Graphene in organosilicon systems Addition, thus reach to improve the purpose of material thermal conductivity.
To sum up, current Graphene field of polymer technology use be disadvantageous in that following some:
1. Graphene is directly added in the middle of macromolecular material, and owing to its specific surface area is big, oil factor is high, causes Graphene addition in Polymer Systems is substantially below 5%.Otherwise can have a strong impact on macromolecular material originally The mechanical performance of body.
2. the surface conditioning agent of routine is used, such as silane coupler, titanate coupling agent etc., due to Graphene There is not active group in surface, is difficult to accomplish that real surface processes.And the Graphene stability after processing is not Good, after process, effect duration is short, material various aspects of performance instability etc. after mixing with macromolecule.
Summary of the invention
The technical problem to be solved is for above-mentioned deficiency of the prior art, it is provided that Yi Zhongyong In the surface treatment method of the Graphene producing heat-conducting silica gel sheet, the Graphene after it processes can be further amounts of Be used for the production of heat-conducting silica gel sheet as heat filling, prepared heat-conducting silica gel sheet possesses high thermal conductivity coefficient.
In order to achieve the above object, food stage TPE material disclosed by the invention gives by the following technical solutions Realize:
The surface treatment method of a kind of Graphene for producing heat-conducting silica gel sheet, comprises the steps of:
(1) Graphene activation: first, configures H2O2With 98% dense H2SO4Mixed solution, wherein, H2O2 Mass ratio be 10%~60%, 98% dense H2SO4Mass ratio be 40%~90%;Secondly, to H2O2With 98% Dense H2SO4Mixed solution in add mass fraction be the Graphene of 1%~30%, be heated to 50~110 DEG C, and It is stirred continuously, continues 10~80min;After completing, the Graphene after activation is separated, washes, dries or dries After Gan, obtain Activated Graphite alkene;
(2) activation Graphene surface processes;The Activated Graphite alkene prepared in step (1) is passed through silane even Connection agent or end-blocking 107 carry out surface process.
The preferred embodiment of the present invention and further improvement are as follows:
One, the Activated Graphite alkene that step (1) prepares is entered by silane coupler in described step (2) Row surface processes and refers to: by 1~15g silane coupler, 10~50g ethanol, 50~the mixing of 500g water, delay Slow addition 100g Activated Graphite alkene, is sufficiently stirred for, is heated to 50~100 DEG C, backflow 30~120min.Complete Cheng Hou, the Graphene after processing separates, dries or dry stand-by;
Activated Graphite alkene step (1) prepared in described step (2) carries out surface by end-blocking 107 Process refers to: by 5~40g end-blockings 107,50~150g toluene, 50~150g hexamethylene, 50~150g Petroleum ether mixes, and is slowly added to 100g Activated Graphite alkene, is sufficiently stirred for, is heated to 40~120 DEG C, backflow 30~300min;After completing, the Graphene after processing separates, dries or dry stand-by.
Two, the molecular formula of described silane coupler is:
Wherein: R1For CH3And/or C2H5;R2For amine propyl group, epoxypropoxy, methacryloxypropyl One or more of base propyl group, vinyl, ureido-propyl and mercaptopropyi;
The molecular formula of described end-blocking 107 is:
Wherein: R1For CH3And/or C2H5;N value is 3~100.
Further: comprise the steps of:
(1) Graphene activation: first, configures H2O2With 98% dense H2SO4Mixed solution, wherein, H2O2 Mass ratio be 35%, 98% dense H2SO4Mass ratio be 65%;Secondly, to H2O2With 98% dense H2SO4Mixed Closing addition mass fraction in solution is the Graphene of 15, is heated to 80 DEG C, and is stirred continuously, continues 50min; After completing, after the Graphene after activation is separated, washes, dries or dried, obtain Activated Graphite alkene;
(2) activation Graphene surface processes;The Activated Graphite alkene prepared in step (1) is passed through silane even Connection agent or end-blocking 107 carry out surface process.
In above-mentioned steps (2) by step (1) prepare Activated Graphite alkene carry out table by silane coupler Face processes and refers to: by 8g silane coupler, and 30g ethanol, 250g water mix, and is slowly added to 100g activity Graphene, is sufficiently stirred for, and is heated to 75 DEG C, and reflux 80min.After completing, the Graphene after processing divides From, dry or dry stand-by;
Activated Graphite alkene step (1) prepared in above-mentioned steps (2) carries out surface by end-blocking 107 Process refers to: 25g blocks 107, and 100g toluene, 100g hexamethylene, 100g petroleum ether mixes, slowly Adding 100g Activated Graphite alkene, be sufficiently stirred for, be heated to 80 DEG C, reflux 170min;After completing, at general Graphene after reason separates, dries or dry stand-by.
Further, also comprise the Graphene after step (2) being processed to be used for preparing Graphene heat conductive silica gel The step of sheet: this step is as follows:
Learn from else's experience by step (2) process after Graphene 10~100 parts, add ethenyl blocking poly dimethyl Siloxanes 30~200 parts, the methyl phenyl silicone oil 0 of ethenyl blocking~100 parts, containing hydrogen silicone oil 3~50 parts, Platinum catalyst 1~10 parts, inhibitor 0.1~0.5 part, 300~2000 mesh metal-oxide 50~500 parts put Enter mill or banbury is sufficiently mixed until uniformly;Then by mixture by hot pressing, scratch, roll, One or more mode molding of spraying, obtain Graphene heat-conducting silica gel sheet.
Further: described metal-oxide is aluminium oxide, zinc oxide or magnesium oxide.
The medicine have the advantages that
The present invention carries out surface active to Graphene at a certain temperature first by Strong oxdiative thing, makes Graphene Surface produces hydroxyl, carboxyl isoreactivity group.Then use silane coupler or end-blocking 107 etc. with silica The Organic substance of alkyl carries out surface process to Activated Graphite alkene, obtains stable surface reason Graphene.Then Graphene after processing prepares thermal conductive silicon with organic silicone oil, organic silicon rubber, containing hydrogen silicone oil with other adjuvants Film.
After graphenic surface is activated by the present invention, hydroxyl and carboxyl isoreactivity base can be produced on the surface of Graphene Group such that it is able to more preferable and silane coupler or end-blocking 107 reaction;
Method disclosed by the invention is in addition to can using traditional silane coupling agents, and the Graphene after activation is permissible Carrying out surface process with end-blocking 107, compared with silane coupler, the Graphene after end-blocking 107 process has The compatibility more preferable with silicone oil.
The present invention can be used alone Graphene, or uses with the collocation of conventional thermal conductive filler, can prepare High thermal conductive silicon film, is 3~40W/m K according to different formulations and its heat conductivity of technique.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not limit Qualitatively, it is impossible to limit protection scope of the present invention with following embodiment.
Embodiment 1:
The surface treatment method of a kind of Graphene for producing heat-conducting silica gel sheet, comprises the steps of:
(1) Graphene activation: first, configures H2O2With 98% dense H2SO4Mixed solution, wherein, H2O2 Mass ratio be 10%, 98% dense H2SO4Mass ratio be 40%;Secondly, to H2O2With 98% dense H2SO4Mixed Closing addition mass fraction in solution is the Graphene of 1%, is heated to 50 DEG C, and is stirred continuously, continues 10min; After completing, after the Graphene after activation is separated, washes, dries or dried, obtain Activated Graphite alkene;
(2) activation Graphene surface processes;The Activated Graphite alkene prepared in step (1) is passed through silane even Connection agent carries out surface process, and this process is: by 1g silane coupler, and 10g ethanol, 50g water mix, slow Slow addition 100g Activated Graphite alkene, is sufficiently stirred for, is heated to 50 DEG C, and reflux 30min.After completing, at general Graphene after reason separates, dries or dry stand-by;
Embodiment 2:
Embodiment 2 difference from Example 1 is:
The step (2) of embodiment 2 is that Activated Graphite alkene step (1) prepared is carried out by end-blocking 107 Surface processes, and this process is: by 5g end-blocking 107,50g toluene, 50g hexamethylene, 50g petroleum ether mixes, Being slowly added to 100g Activated Graphite alkene, be sufficiently stirred for, be heated to 40 DEG C, reflux 30min;After completing, will Graphene after process separates, dries or dry stand-by.
Embodiment 3:
The surface treatment method of a kind of Graphene for producing heat-conducting silica gel sheet, comprises the steps of:
(1) Graphene activation: first, configures H2O2With 98% dense H2SO4Mixed solution, wherein, H2O2 Mass ratio be 35%, 98% dense H2SO4Mass ratio be 65%;Secondly, to H2O2With 98% dense H2SO4Mixed Closing addition mass fraction in solution is the Graphene of 15, is heated to 80 DEG C, and is stirred continuously, continues 50min; After completing, after the Graphene after activation is separated, washes, dries or dried, obtain Activated Graphite alkene;
(2) activation Graphene surface processes;The Activated Graphite alkene prepared in step (1) is passed through silane even Connection agent carries out surface process, and this process is: by 8g silane coupler, and 30g ethanol, 250g water mix, slow Slow addition 100g Activated Graphite alkene, is sufficiently stirred for, is heated to 75 DEG C, and reflux 80min.After completing, at general Graphene after reason separates, dries or dry stand-by;
Embodiment 4:
Embodiment 4 difference from Example 3 is:
The step (2) of embodiment 4 is that Activated Graphite alkene step (1) prepared is carried out by end-blocking 107 Surface processes, and this process is: by 25g end-blocking 107,100g toluene, 100g hexamethylene, 100g petroleum ether Mixing, is slowly added to 100g Activated Graphite alkene, is sufficiently stirred for, be heated to 80 DEG C, and reflux 170min;Complete Cheng Hou, the Graphene after processing separates, dries or dry stand-by.
Embodiment 5:
The surface treatment method of a kind of Graphene for producing heat-conducting silica gel sheet, comprises the steps of:
(1) Graphene activation: first, configures H2O2With 98% dense H2SO4Mixed solution, wherein, H2O2 Mass ratio be 60%, 98% dense H2SO4Mass ratio be 90%;Secondly, to H2O2With 98% dense H2SO4Mixed Closing addition mass fraction in solution is the Graphene of 30%, is heated to 110 DEG C, and is stirred continuously, continues 80min; After completing, after the Graphene after activation is separated, washes, dries or dried, obtain Activated Graphite alkene;
(2) activation Graphene surface processes;The Activated Graphite alkene prepared in step (1) is passed through silane even Connection agent carries out surface process, and this process is: by 15g silane coupler, and 50g ethanol, 500g water mix, Being slowly added to 100g Activated Graphite alkene, be sufficiently stirred for, be heated to 100 DEG C, reflux 120min.After completing, Graphene after processing separates, dries or dry stand-by;
Embodiment 6:
Embodiment 5 difference from Example 6 is:
The step (2) of embodiment 6 is that Activated Graphite alkene step (1) prepared is carried out by end-blocking 107 Surface processes, and this process is: by 40g end-blocking 107,150g toluene, 150g hexamethylene, 150g petroleum ether Mixing, is slowly added to 100g Activated Graphite alkene, is sufficiently stirred for, be heated to 120 DEG C, and reflux 300min;Complete Cheng Hou, the Graphene after processing separates, dries or dry stand-by.
The Graphene that above-described embodiment 1, embodiment 3 and embodiment 5 prepare possesses high stability, heat conductivity; Simultaneously embodiment 2, embodiment 3 and embodiment 5 correspondence compare embodiment 1, embodiment 3 and embodiment 5 The Graphene prepared possesses the more preferable compatibility, and stability is higher.On the whole, along with the increase of formula ratio, Stability and the compatibility of the Graphene after the process of surface are the highest, it is possible to realize in silica gel piece preparation process The purpose of middle increase addition.It is used alone Graphene, or uses with the collocation of conventional thermal conductive filler, can make For obtaining high thermal conductive silicon film, it is 3~40W/m K according to different formulations and its heat conductivity of technique.
Graphene after activation can carry out surface process with end-blocking 107, compared with silane coupler, and end-blocking Graphene after 107 process has the compatibility more preferable with silicone oil.
Prepare heat-conducting silica gel sheet for the surface treatment method using above-mentioned Graphene, We conducted following reality Execute example:
Embodiment 7:
Graphene heat-conducting silica gel sheet, comprises the following steps:
Learn from else's experience respectively the Graphene 10 after being processed by the surface treatment method of embodiment 1~6~100 parts, respectively Proceed as follows and prepare heat-conducting silica gel sheet:
Add the polydimethylsiloxane 30 parts of ethenyl blocking, the methyl phenyl silicone oil 1 part of ethenyl blocking, Containing hydrogen silicone oil 3 parts, platinum catalyst 1 part, inhibitor 0.1 part, 300 mesh metal-oxide 50 parts are put into Mill is sufficiently mixed until uniformly;Then by mixture by calendering formation, Graphene heat conductive silica gel is obtained Sheet.
Embodiment 8:
Graphene heat-conducting silica gel sheet, comprises the following steps:
Graphene 55 parts after learning from else's experience respectively by the surface treatment method process of embodiment 1~6, is carried out respectively Following operation prepares heat-conducting silica gel sheet:
Add the polydimethylsiloxane 115 parts of ethenyl blocking, the methyl phenyl silicone oil 55 of ethenyl blocking Part, containing hydrogen silicone oil 26 parts, platinum catalyst 6 parts, inhibitor 0.3 part, 1150 mesh metal-oxides 260 Part is put into mill and is sufficiently mixed until uniformly;Then by mixture by calendering formation, obtain Graphene and lead Hot silica gel piece.
Embodiment 9:
Graphene heat-conducting silica gel sheet, comprises the following steps:
Graphene 100 parts after learning from else's experience respectively by the surface treatment method process of embodiment 1~6, is carried out respectively Following operation prepares heat-conducting silica gel sheet:
Add the polydimethylsiloxane 200 parts of ethenyl blocking, the methyl phenyl silicone oil 100 of ethenyl blocking Part, containing hydrogen silicone oil 50 parts, platinum catalyst 10 parts, inhibitor 0.5 part, 2000 mesh metal-oxides 500 Part is put into mill and is sufficiently mixed until uniformly;Then by mixture by calendering formation, obtain Graphene and lead Hot silica gel piece.
The thickness of the heat-conducting silica gel sheet that above-described embodiment 7~8 prepares is 1~3mm;Heat conductivity 3~ 10W/m·K;It possesses low cost to compare conventional thermal conductive silica gel piece, and heat conductivity is high, is suitable to large-scale production.
Above the preferred embodiment for the present invention is explained in detail, but the invention is not restricted to above-mentioned embodiment party Formula, in the ken that those of ordinary skill in the art are possessed, it is also possible to without departing from present inventive concept On the premise of make a variety of changes, these changes relate to correlation technique well-known to those skilled in the art, this Both fall within the protection domain of patent of the present invention a bit.
Many other can be made without departing from the spirit and scope of the present invention to change and remodeling.Should be appreciated that this Invention is not limited to specific embodiment, and the scope of the present invention is defined by the following claims.

Claims (6)

1. the surface treatment method being used for producing the Graphene of heat-conducting silica gel sheet, it is characterised in that comprise Following steps:
(1) Graphene activation: first, configures H2O2With 98% dense H2SO4Mixed solution, wherein, H2O2 Mass ratio be 10%~60%, 98% dense H2SO4Mass ratio be 40%~90%;Secondly, to H2O2With 98% Dense H2SO4Mixed solution in add mass fraction be the Graphene of 1%~30%, be heated to 50~110 DEG C, and It is stirred continuously, continues 10~80min;After completing, the Graphene after activation is separated, washes, dries or dries After Gan, obtain Activated Graphite alkene;
(2) activation Graphene surface processes;The Activated Graphite alkene prepared in step (1) is passed through silane even Connection agent or end-blocking 107 carry out surface process.
A kind of surface treatment method of the Graphene for producing heat-conducting silica gel sheet, It is characterized in that, Activated Graphite alkene step (1) prepared in described step (2) is by silane coupled Agent carries out surface process and refers to: by 1~15g silane coupler, and 10~50g ethanol, 50~500g water mix, It is slowly added to 100g Activated Graphite alkene, is sufficiently stirred for, be heated to 50~100 DEG C, backflow 30~120min. After completing, the Graphene after processing separates, dries or dry stand-by;
Activated Graphite alkene step (1) prepared in described step (2) carries out surface by end-blocking 107 Process refers to: by 5~40g end-blockings 107,50~150g toluene, 50~150g hexamethylene, 50~150g Petroleum ether mixes, and is slowly added to 100g Activated Graphite alkene, is sufficiently stirred for, is heated to 40~120 DEG C, backflow 30~300min;After completing, the Graphene after processing separates, dries or dry stand-by.
A kind of surface treatment method of the Graphene for producing heat-conducting silica gel sheet, It is characterized in that, the molecular formula of described silane coupler is:
Wherein: R1For CH3And/or C2H5;R2For amine propyl group, epoxypropoxy, methacryloxypropyl One or more of base propyl group, vinyl, ureido-propyl and mercaptopropyi;
The molecular formula of described end-blocking 107 is:
Wherein: R1For CH3And/or C2H5;N value is 3~100.
A kind of surface treatment method of the Graphene for producing heat-conducting silica gel sheet, It is characterized in that, comprise the steps of:
(1) Graphene activation: first, configures H2O2With 98% dense H2SO4Mixed solution, wherein, H2O2 Mass ratio be 35%, 98% dense H2SO4Mass ratio be 65%;Secondly, to H2O2With 98% dense H2SO4Mixed Closing addition mass fraction in solution is the Graphene of 15, is heated to 80 DEG C, and is stirred continuously, continues 50min; After completing, after the Graphene after activation is separated, washes, dries or dried, obtain Activated Graphite alkene;
(2) activation Graphene surface processes;The Activated Graphite alkene prepared in step (1) is passed through silane even Connection agent or end-blocking 107 carry out surface process.
In above-mentioned steps (2) by step (1) prepare Activated Graphite alkene carry out table by silane coupler Face processes and refers to: by 8g silane coupler, and 30g ethanol, 250g water mix, and is slowly added to 100g activity Graphene, is sufficiently stirred for, and is heated to 75 DEG C, and reflux 80min.After completing, the Graphene after processing divides From, dry or dry stand-by;
Activated Graphite alkene step (1) prepared in above-mentioned steps (2) carries out surface by end-blocking 107 Process refers to: 25g blocks 107, and 100g toluene, 100g hexamethylene, 100g petroleum ether mixes, slowly Adding 100g Activated Graphite alkene, be sufficiently stirred for, be heated to 80 DEG C, reflux 170min;After completing, at general Graphene after reason separates, dries or dry stand-by.
5. the surface of a kind of Graphene for producing heat-conducting silica gel sheet as described in Claims 1 to 4 is arbitrary Reason method, it is characterised in that: also comprise the Graphene after step (2) being processed and be used for preparing Graphene heat conduction The step of silica gel piece: this step is as follows:
Learn from else's experience by step (2) process after Graphene 10~100 parts, add ethenyl blocking poly dimethyl Siloxanes 30~200 parts, the methyl phenyl silicone oil 0 of ethenyl blocking~100 parts, containing hydrogen silicone oil 3~50 parts, Platinum catalyst 1~10 parts, inhibitor 0.1~0.5 part, 300~2000 mesh metal-oxide 50~500 parts put Enter mill or banbury is sufficiently mixed until uniformly;Then by mixture by hot pressing, scratch, roll, One or more mode molding of spraying, obtain Graphene heat-conducting silica gel sheet.
A kind of surface treatment method of the Graphene for producing heat-conducting silica gel sheet, It is characterized in that: described metal-oxide is aluminium oxide, zinc oxide or magnesium oxide.
CN201610209007.3A 2016-04-06 2016-04-06 Surface treatment method of graphene used for producing heat conducting silicon sheets Pending CN105838077A (en)

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CN106832961A (en) * 2017-02-28 2017-06-13 深圳市大族元亨光电股份有限公司 The preparation method of Graphene thermal conductive silicon rubber cushion
CN108165016A (en) * 2018-01-19 2018-06-15 林荣铨 A kind of preparation method of modified graphene heat-conducting silicone grease
CN108264771A (en) * 2018-01-19 2018-07-10 林荣铨 A kind of preparation method and applications of graphene heat-conducting silicone grease
CN112812714A (en) * 2021-02-06 2021-05-18 惠州东铭新能源研究院有限公司 Fireproof flame-retardant buffer aerogel product capable of absorbing stress and manufacturing method thereof
CN114316598A (en) * 2022-01-26 2022-04-12 广东信力科技股份有限公司 Preparation method of high-thermal-conductivity organic silicon rubber composite material

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1636938A (en) * 2004-11-26 2005-07-13 中国科学院长春应用化学研究所 Silicon carbide surface modifying method
CN103087404A (en) * 2011-10-31 2013-05-08 上海杰事杰新材料(集团)股份有限公司 Graphene filled polymer matrix composite material and its preparation method
CN103342896A (en) * 2013-06-26 2013-10-09 苏州天脉导热科技有限公司 High temperature resistant heat-conducting silica gel sheet and preparation method thereof
CN103937259A (en) * 2014-04-04 2014-07-23 东莞市柏力有机硅科技有限公司 Graphene oxide modified compound type heat conducting silicone rubber and preparation method thereof
CN104610780A (en) * 2015-01-12 2015-05-13 中国科学院宁波材料技术与工程研究所 Modification method for silicon carbide particles
CN105400202A (en) * 2015-12-14 2016-03-16 湖南工业大学 Boron nitride/graphene composite heat-conducting silicone grease and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1636938A (en) * 2004-11-26 2005-07-13 中国科学院长春应用化学研究所 Silicon carbide surface modifying method
CN103087404A (en) * 2011-10-31 2013-05-08 上海杰事杰新材料(集团)股份有限公司 Graphene filled polymer matrix composite material and its preparation method
CN103342896A (en) * 2013-06-26 2013-10-09 苏州天脉导热科技有限公司 High temperature resistant heat-conducting silica gel sheet and preparation method thereof
CN103937259A (en) * 2014-04-04 2014-07-23 东莞市柏力有机硅科技有限公司 Graphene oxide modified compound type heat conducting silicone rubber and preparation method thereof
CN104610780A (en) * 2015-01-12 2015-05-13 中国科学院宁波材料技术与工程研究所 Modification method for silicon carbide particles
CN105400202A (en) * 2015-12-14 2016-03-16 湖南工业大学 Boron nitride/graphene composite heat-conducting silicone grease and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106832961A (en) * 2017-02-28 2017-06-13 深圳市大族元亨光电股份有限公司 The preparation method of Graphene thermal conductive silicon rubber cushion
CN108165016A (en) * 2018-01-19 2018-06-15 林荣铨 A kind of preparation method of modified graphene heat-conducting silicone grease
CN108264771A (en) * 2018-01-19 2018-07-10 林荣铨 A kind of preparation method and applications of graphene heat-conducting silicone grease
CN112812714A (en) * 2021-02-06 2021-05-18 惠州东铭新能源研究院有限公司 Fireproof flame-retardant buffer aerogel product capable of absorbing stress and manufacturing method thereof
CN114316598A (en) * 2022-01-26 2022-04-12 广东信力科技股份有限公司 Preparation method of high-thermal-conductivity organic silicon rubber composite material

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Application publication date: 20160810