CN106634863A - Graphene based silica gel heat-conductive gasket and preparation method thereof - Google Patents
Graphene based silica gel heat-conductive gasket and preparation method thereof Download PDFInfo
- Publication number
- CN106634863A CN106634863A CN201611257806.4A CN201611257806A CN106634863A CN 106634863 A CN106634863 A CN 106634863A CN 201611257806 A CN201611257806 A CN 201611257806A CN 106634863 A CN106634863 A CN 106634863A
- Authority
- CN
- China
- Prior art keywords
- graphene
- silica gel
- aluminium
- based silica
- gel heat
- 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.)
- Pending
Links
Classifications
-
- 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
Abstract
The invention discloses a graphene based silica gel heat-conductive gasket and a preparation method thereof. The graphene based silica gel heat-conductive gasket is composed of the following components in parts by mass: 100 parts of modified graphene, 10 to 20 parts of vinyl silicone oil, 1 to 3 parts of hydrogen containing silicone oil, 0.1 to 0.3 part of a catalyst, 1 to 3 parts of a silane coupling agent, 0.02 to 0.05 part of an inhibitor and 300 to 800 parts of spherical aluminum oxide. The graphene based silica gel heat-conductive gasket prepared by using the method provided by the invention has excellent heat conductivity and stability, can reach heat conductivity of 6 W/m.k, does not occur oil penetration, is changed by no more than 5% in hardness and heat conductivity after ageing of 1000 hours at 150 DEG C, and can be applied to interface heat dissipation in the fields like LED illumination.
Description
[technical field]
The present invention relates to heat-conducting interface material, more particularly to a kind of graphene-based silica gel heat-conducting pad and preparation method thereof.
[background technology]
The advantages of LED is with energy-saving and environmental protection, life-span length, small volume, be widely used in illuminating, show, various indicator lamps and
The fields such as backlight.In particular with the fast development of field of LED illumination, its great power LED cooling is always individual urgently to be resolved hurrily
Difficulties.Because the fine or not extreme influence of the conducting-heat elements heat dispersion of LED the service life and energy-saving effect of LED,
The technological improvement of high-power LED illumination at present is primarily directed to heat dissipation problem.Graphene has super-high heat-conductive performance, its heat conduction system
Number is up to 5300W/mK, far above existing conductive filler material (such as Ag, Cu, Al2O3、BN、Si3N4Deng), therefore its work
For the filler of heat-conducting interface material, thermal conduction characteristic will be greatly improved, have the potentiality that grow a lot in LED Mirae Corp..But by
In the surface inertness of Graphene, there is stronger Van der Waals force between lamella and lamella, be susceptible to reunite, cause effective ratio table
Area is reduced, and the formation of good heat conductive path can be had influence on because of reunion in filling intrinsic silicon, therefore, how by Graphene with
Other heat filling particles realize compounding well, are sufficient filling with space, play the outstanding thermal conduction characteristic of Graphene, the property prepared
The excellent heat conductive silica gel pad of energy becomes the emphasis of research.
[content of the invention]
The technical problem to be solved in the present invention is to provide a kind of Graphene with other heat filling particle compoundings, heat conductivility
Good graphene-based silica gel heat-conducting pad and preparation method thereof.
The technical problem to be solved in the present invention is to provide the preparation method of the graphene-based silica gel heat-conducting pad of upper art.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is, a kind of graphene-based silica gel heat-conducting pad,
It is composed of the following components by mass parts：
Above-described graphene-based silica gel heat-conducting pad, described vinyl silicone oil contents of ethylene is 0.04%～
0.2%, viscosity 500cps～5000cps；The active hydrogen content of described containing hydrogen silicone oil is 0.16%～0.8%；Described urges
Agent is platinum catalyst；Described silane coupler is gamma-aminopropyl-triethoxy-silane, γ-(2,3- the third oxygen of epoxy) third
Base trimethoxy silane and/or γ-methacryloxypropyl trimethoxy silane；Described inhibitor is acetenyl hexamethylene
Alcohol；The particle diameter of described ball-aluminium oxide is 0.5 μm～70 μm；Described modified graphene is the reduction of aluminum oxide assembling modification
Graphene.
Above-described graphene-based silica gel heat-conducting pad, the preparation process of the modified graphene is comprised the following steps：
301st, in mass ratio 100：2.5:10～100:5:75, by the addition of graphene oxide, surface modifier and aluminium ion
Agent is scattered in the aqueous hydrogen peroxide solution that mass percent concentration is 20%～40%, temperature control at 150 DEG C～350 DEG C, plus
Heat treatment 1～2 hour；Solution is 1.5～3 with the volume ratio of solution；
302nd, it is cooled to after room temperature, addition excessive ammonia is alkali lye, at 50 DEG C～100 DEG C, heated sealed processes 30 points
Clock～2 hour；
303rd, environmental protection of the sediment that the Graphene for obtaining step 302 and aluminium hydroxide mix in inert gas
Under, calcination is decomposed 30 minutes～2 hours, obtains alumina modified Graphene.
Above-described graphene-based silica gel heat-conducting pad, described graphene oxide is the oxidation prepared with Hummer methods
Graphene；Described surface modifier be polyvinylpyrrolidone, dodecyl sodium sulfate, hexadecyltrimethylammonium chloride and
At least one in titanate coupling agent；Described aluminium ion additive is aluminum sulfate saturated aqueous solution, aluminium hydrogen sulfate saturation water
At least one in solution, aluminium chloride saturated aqueous solution and aluminum nitrate saturated aqueous solution；Excessive ammonia is mass percent concentration
20%～30% ammoniacal liquor；The temperature that calcination is decomposed is 1080 DEG C to 1120 DEG C.
A kind of its preparation method of above-mentioned graphene-based silica gel heat-conducting pad, comprises the following steps：
501st, by above-mentioned weight portion, vinyl silicone oil, containing hydrogen silicone oil, catalyst, silane coupler and inhibitor are stirred
Mix uniform；
502nd, after adding the ball-aluminium oxide that 300～800 mass parts are dried to stir, the modified stone of 100 mass parts is added
Black alkene continues to stir；
503rd, the mixed material for obtaining step 502 is kneaded 5～10 times, is then vacuumized and is sloughed bubble, obtains paste material；
504th, by the paste material for obtaining calendering, solidification, graphene-based silica gel heat-conducting pad is obtained.
Above-described graphene-based silica gel heat-conducting pad and preparation method thereof, in step 504, by paste material two is placed on
Layer PET mould release membrances in the middle of, pressure be 5～10MPa, temperature be 180 DEG C under conditions of calendering formation, solidify 0.5 hour.
Graphene-based silica gel heat-conducting pad prepared by the present invention has excellent heat conductivility and stability, thermal conductivity factor energy
6W/mK is reached, permeability is occurred without, aging 1000 hours at 150 DEG C, its hardness, thermal conductivity factor change≤5% can be applied
Radiate in the interface in the fields such as LED illumination.
[specific embodiment]
The preparation method of the graphene-based high thermal conductivity silica gel heat-conducting pad of the present invention, comprises the following steps：
1) modified graphene is prepared：Thermal reduction and modified integration are sealed using in graphene oxide, oxygenerating is derived from
Aluminium assembling modification Graphene.Specifically with Hummer methods prepare graphene oxide as presoma, addition polyvinylpyrrolidone,
One or more works in the surfactants such as dodecyl sodium sulfate, hexadecyltrimethylammonium chloride and titanate coupling agent
For surface modifier, aluminum sulfate saturated aqueous solution, aluminium hydrogen sulfate saturated aqueous solution, aluminium chloride saturated aqueous solution and aluminum nitrate saturation
One or more in the aqueous solution are used as aluminium ion additive, wherein graphene oxide：Surface modifier：Aluminium ion additive
Mass ratio is 100：2.5:10～100:5:75 and can produce the mass percent of the hydrogen peroxide of gas as solvent to be heated
Concentration is 20%～40%, and the excessive ammonia that mass percent concentration is 20%～30% is placed in high pressure anti-as alkali lye
In answering kettle, temperature control heats 1 hour～2 hours at 150 DEG C～350 DEG C, and hydrogen peroxide is acted on by thermogenetic gas
Under, thermal reduction processes the reduced graphene for obtaining less than 10 layers, while thermal reduction is processed, by the use of ammoniacal liquor as reaction base
Liquid, under conditions of aluminium ion is present, is processed 30 minutes～2 hours, by chemical reaction in 50 DEG C～100 DEG C sealed reactors
Al3++3NH3.H2O=Al (OH)3+3NH4 +, the aluminum hydroxide precipitation of synthesis, its carry out with Graphene self assembly obtain Graphene/
Aluminium hydroxide compound.Finally the mixture is carried out to be placed in high temperature furnace, in the guarantor of the inert gases such as nitrogen, helium or argon gas
Under shield, at 1 100 DEG C ± 20 DEG C, 30 minutes～2 hours are decomposed in calcination to temperature control, according to Al (OH)3=Al2O3+H2O
Decomposition reaction, cooling is derived from the modified Graphene of oxygenerating aluminium；
2) preparation of heat conductive silica gel pad：By 10～20 parts of vinyl silicone oils, 1～3 part of containing hydrogen silicone oil, 0.1～0.3 part of day
This SHIN-ETSU HANTOTAI platinum catalyst, 1～3 part of silane coupler, 0.02～0.05 part of ethynylcyclohexanol inhibitor, by above weight group
Divide to weigh and be added in plastic stir jar, be placed in homogenizer, be 50r/min～100r/min stirrings 0.2 in rotating speed
After hour, take out and add 300～800 parts of dry ball-aluminium oxides, be that 50r/min～2000r/min stirrings 0.2 are little in rotating speed
When～0.5 hour, 100 parts of modified graphenes of uniform rear addition to be mixed, rotating speed is that 50r/min～2000r/min stirrings 0.2 are little
When～1 hour；Subsequently the mixed material is kneaded 5～10 times by double roller machine of beginning to pratise, is then vacuumized and is sloughed bubble, obtain cream
Shape material；By paste material in the middle of two-layer PET mould release membrance, the calendering formation under the effect of uniform temperature certain pressure is made described
The silica gel heat-conducting pad of different-thickness.
Preferably, in step 1) in, surface modifier is polyvinylpyrrolidone or titanate coupling agent；Aluminium ion adds
Plus agent preferably sulfuric acid aluminium saturated aqueous solution.
Preferably, in step 2) in, the vinyl silicone oil contents of ethylene of selection is 0.04%～0.2%, viscosity
500cps～5000cps；The active hydrogen content of hydrogen content of containing hydrogen silicone oil is 0.16%～0.8%；From silane coupler be
Gamma-aminopropyl-triethoxy-silane, γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane, γ-methacryloxypropyl
Trimethoxy silane；From ball-aluminium oxide be nippon particle diameter be 0.5 μm～40 μm；The temperature control of calendering formation
At 80 DEG C～250 DEG C, 0.2 hour～3 hours hardening time, pressure size is controlled in 5MPa～20MPa, made by heat conductive silica gel
The thickness of pad is 0.2mm～5mm.
With reference to embodiment, the invention will be further described, but following embodiments, only present pre-ferred embodiments
, therefore can not limit according to this present invention enforcement scope, i.e., according to the scope of the claims of the present invention and description made it is equivalent
Change and modification, all should still belong in the range of the present invention covers.
Embodiment 1:
1) modified graphene is prepared：Graphite oxide with the preparation of Hummer methods as presoma, make by PVP
For surface modifier, aluminum sulfate saturated aqueous solution as aluminium ion additive, in mass ratio by graphene oxide：Surface is modified
Agent：Aluminum sulfate saturated aqueous solution is with 20: 1:10 ratio, is scattered in the aqueous hydrogen peroxide solution that mass percent concentration is 40%
In, in being subsequently placed in autoclave, temperature control heats 1 hour～2 hours at 180 DEG C.The volume of hydrogen peroxide with it is front
Volume feed scope control is stated 1.5～3, cumulative volume is less than 1/2nd of reactor total measurement (volume).Hydrogen peroxide is heated product
Under raw gas effect, thermal reduction is processed and obtains reduced graphene of the number of plies less than 10 layers, and the cooling of question response kettle is reached after room temperature,
Continue add mass percent concentration be 30% excessive ammonia as alkali lye, temperature control is located in a kettle. in 50 DEG C of sealings
Reason 2 hours.The volume for adding alkali lye is 3/2 or so of aforementioned aluminum sulfate water saturation aqueous solution volume.In the bar that aluminium ion is present
Under part, by chemical reaction Al3++3NH3.H2O=Al (OH)3+3NH4 +, the aluminum hydroxide precipitation of synthesis, it is carried out with Graphene
Self assembly obtains Graphene/aluminium hydroxide compound.The mixture powder is obtained after Graphene/aluminium hydroxide composite filter,
Mixture powder is contained in quartz glass ware and is placed in high temperature furnace, in the guarantor of the protective gas such as nitrogen, helium or argon gas
Under shield, temperature control at 1 100 DEG C, according to Al (OH)3=Al2O3+ H2O decomposition reactions calcination 45 minutes, is derived from after cooling
The modified Graphene powder of oxygenerating aluminium；
2) preparation of heat conductive silica gel pad：By mass parts, by the vinyl silicone oil that 20 parts of viscosity are 2000cps, 1 part hydrogeneous
Measure the containing hydrogen silicone oil for 0.16%, 0.1 part of Japanese SHIN-ETSU HANTOTAI platinum catalyst, 1 part of gamma-aminopropyl-triethoxy-silane coupling agent,
0.02 part of ethynylcyclohexanol inhibitor, weighs and is added in plastic stir jar, is placed in homogenizer, is in rotating speed
After 100r/min is stirred 0.2 hour, the nippon ball of 70 μm of dry 500 part particle diameter and 300 parts of 35 μm of particle diameters is added
Shape aluminum oxide, is that 2000r/min is stirred 0.2 hour in rotating speed, 100 parts of homemade modified graphenes of uniform rear addition to be mixed,
Rotating speed is that 2000r/min is stirred 0.5 hour；Subsequently the mixed material is kneaded 10 times by twin-roll machine, then in vacuum drying oven
In vacuumize and slough bubble, obtain paste material；By paste material is in the stainless steel mould frame of 0.2mm thickness and is placed on two-layer
In the middle of PET mould release membrances, pressure be 10MPa, temperature be 180 DEG C under conditions of calendering formation, solidify 0.5 hour, make thickness
For the silica gel heat-conducting pad of 0.2mm.ASTM D5470 method of testings are adopted to obtain its thermal conductivity factor for 6W/mK.Compared to same
Under the conditions of etc. technique and proportion of filler, do not adding homemade modified graphene, the silicagel pad thermal conductivity factor prepared is only up to
Arrive 2.5W/mK or so.As can be seen here, the addition of homemade modified graphene can promote to form good heat conductive network path,
The conductive force that cooperates with of Graphene and other heat fillings is given full play to, the graphene-based silica gel heat-conducting pad of high heat conduction is obtained.It is real
Apply example 2:
1) modified graphene is prepared：Graphite oxide with the preparation of Hummer methods as presoma, make by PVP
For surface modifier, aluminum sulfate saturated aqueous solution as aluminium ion additive, in mass ratio by graphene oxide：Surface is modified
Agent：Aluminum sulfate saturated aqueous solution presses 20: 1:5 ratio, in being scattered in the aqueous hydrogen peroxide solution that mass percent concentration is 40%,
In being placed in autoclave, temperature control heats 2 hours at 180 DEG C, volume and the aforementioned base materials volume ratio model of hydrogen peroxide
System is contained 1.5～3, cumulative volume is less than 1/2nd of reactor total measurement (volume).Under hydrogen peroxide is by the effect of thermogenetic gas,
Thermal reduction is processed and obtains reduced graphene of the number of plies less than 10 layers.The cooling of question response kettle is reached after room temperature, continues to add mass ratio
By graphene oxide：Surface modifier：Aluminum sulfate presses 20: 1:5 ratio, is scattered in the excess that mass percent concentration is 25%
Ammoniacal liquor is heat-treated 2 hours as alkali lye, temperature control in 50 DEG C of sealed reactors.The volume for adding alkali lye is that aforementioned aluminum sulfate is satisfied
With 3/2 or so of aqueous solution volume.Under conditions of aluminium ion is present, by chemical reaction Al3++3NH3.H2O=Al (OH)3+
3NH4 +, the aluminum hydroxide precipitation of synthesis, it carries out self assembly and obtains Graphene/aluminium hydroxide compound with Graphene.Graphene/
Aluminium hydroxide composite filter obtains the mixture powder and is contained in quartz glass ware to be placed in high temperature furnace, in nitrogen, helium
Under the protection of the gas such as gas or argon gas, temperature control at 1 100 DEG C, according to Al (OH)3=Al2O3+ H2O decomposition reactions calcination 30
Minute, cooling is derived from the modified Graphene powder of oxygenerating aluminium；
2) preparation of heat conductive silica gel pad：By mass parts, just 20 parts viscosity are 2000cps vinyl silicone oils, and 1 part hydrogeneous
Measure the containing hydrogen silicone oil for 0.16%, 0.1 part of platinum catalyst, 1 part of gamma-aminopropyl-triethoxy-silane coupling agent and 0.02 part of second
Alkynyl cyclohexanol inhibitor, is added in plastic stir jar after weighing well, is placed in homogenizer, is 100r/min in rotating speed
After stirring 0.2 hour, 35 μm of dry 400 part particle diameter and 200 parts of 10 μm of particle diameter ball-aluminium oxides are added, be in rotating speed
2000r/min is stirred 0.2 hour, and 100 parts of homemade modified graphenes of uniform rear addition to be mixed, rotating speed is stirred for 2000r/min
Mix 0.5 hour；Subsequently the mixed material is kneaded 10 times by double roller machine of beginning to pratise, is then vacuumized in vacuum drying oven and is sloughed gas
Bubble, obtains paste material；By paste material is in the mould frame of 0.25mm thickness and is placed in the middle of two-layer PET mould release membrance, in pressure
It is calendering formation under conditions of 180 DEG C for 5MPa, temperature, after solidifying 0.5 hour, makes the silica gel heat conductive pad that thickness is 0.25mm
Piece.ASTM D5470 method of testings are adopted to measure its thermal conductivity factor for 5.8W/mK.Compared to equal technique and proportion of filler bar
Under part, when homemade modified graphene is not added, the silicagel pad thermal conductivity factor prepared is only 1.9W/mK or so.
Embodiment 3:
1) modified graphene is prepared：Graphite oxide with the preparation of Hummer methods as presoma, make by PVP
For surface modifier, aluminum sulfate saturated aqueous solution is used as aluminium ion additive, in mass ratio graphene oxide：Surface modifier：
Aluminum sulfate saturated aqueous solution=20: 1:5 ratio, in being scattered in the aqueous hydrogen peroxide solution that mass percent concentration is 40%, puts
In autoclave, temperature control heats 2 hours at 180 DEG C, volume and the aforementioned base materials volume range of hydrogen peroxide
1.5～3, cumulative volume is less than 1/2nd of reactor total measurement (volume) for control.It is hot under hydrogen peroxide is by the effect of thermogenetic gas
Reduction treatment obtains reduced graphene of the number of plies less than 10 layers.The cooling of question response kettle is reached after room temperature, continues to add quality percentage
Specific concentration be 25% excessive ammonia as alkali lye, temperature control heats 2 hours at 60 DEG C.Before the volume for adding alkali lye is
State 3/2 or so of aluminum sulfate saturated aqueous solution volume.Under conditions of aluminium ion is present, by chemical reaction Al3++3NH3.H2O
=Al (OH)3+3NH4 +, the aluminum hydroxide precipitation of synthesis, it carries out self assembly with Graphene and obtains Graphene/aluminium hydroxide being combined
Thing.It is filtrated to get the mixture powder and is contained in quartz glass ware and be placed in high temperature furnace, in nitrogen, helium or argon gas etc.
Under the protection of inert gas, temperature control at 1 100 DEG C, according to Al (OH)3=Al2O3+ H2O decomposition reactions calcination 30 minutes, it is cold
But it is derived from the modified Graphene powder of oxygenerating aluminium；
2) preparation of heat conductive silica gel pad：It is 3000cps vinyl silicone oils by 20 parts of viscosity by mass parts, 1 part of hydrogen content
For 0.8% containing hydrogen silicone oil, 0.1 part of Japanese SHIN-ETSU HANTOTAI platinum catalyst, 1 part of γ-methacryloxypropyl trimethoxy silicon
Alkane coupling agent, 0.02 part of ethynylcyclohexanol inhibitor, weighs and is added in plastic stir jar, is placed in homogenizer,
It is after 100r/min is stirred 0.2 hour, to further take out and add 500 parts of dry 70 μm of ball-aluminium oxides in rotating speed, is in rotating speed
2000r/min is stirred 0.2 hour, and 100 parts of homemade modified graphenes of uniform rear addition to be mixed, rotating speed is stirred for 2000r/min
Mix 0.5 hour；Subsequently the mixed material is kneaded 10 times by double roller machine of beginning to pratise, is then vacuumized in vacuum drying oven and is sloughed gas
Bubble, obtains paste material；It is big in pressure by paste material is in the mould frame of 0.2mm thickness and is placed in the middle of two-layer PET mould release membrance
Under conditions of little control 10MPa, 180 DEG C of calendering formations of temperature control after solidifying 0.5 hour, make the silica gel that thickness is 0.2mm
Heat-conducting pad.ASTM D5470 method of testings are adopted to obtain its thermal conductivity factor for 5W/mK.Compared to equal technique and filler ratio
Under the conditions of example, do not adding homemade modified graphene, the silicagel pad thermal conductivity factor prepared is only 1.2W/mK or so.
Using technical scheme：Have the advantages that：
(1) present invention seals thermal reduction and modified integration using graphene oxide, is derived from oxygenerating aluminium assembling modification
Graphene.
(2) the Graphene method of modifying takes full advantage of the labile hydrogen peroxide that is heated as solvent, adds polyethylene pyrrole
The surfactant such as pyrrolidone or titanate coupling agent, thermal reduction processing procedure is carried out to graphene oxide and obtains what surface was modified
Graphene.Using hydrogen peroxide by under the effect of thermogenetic gas, thermal reduction processes the reduced graphene for obtaining fewer layers, same with this
When, excessive ammonia is taken full advantage of as reaction alkali lye, under conditions of aluminium ion is present, by chemical reaction Al3++
3NH3.H2O=Al (OH)3+3NH4 +, the aluminum hydroxide precipitation of synthesis, it carries out self assembly and obtains Graphene/hydrogen-oxygen with Graphene
Change aluminium compound, high temperature sintering is finally carried out, according to Al (OH)3=Al2O3+ H2O decomposition reactions, cooling is made by oneself
Alumina modified Graphene.
(3) Van der Waals force between graphene sheet layer is overcome by being modified, it is to avoid cause it with heat conduction grain because of reuniting
Son uniformly mixes the problem being obstructed.By obtaining modified graphene heat filling is realized after interface modification with Graphene, more
It is dispersed in silicone oil matrix well, thermal conducting path is formed, so as to the Graphene heat conductive silica gel pad for preparing is with higher
Thermal conductivity factor.
(4) graphene-based silica gel heat-conducting pad prepared by the present invention has excellent heat conductivility and stability, heat conduction system
Number can reach 6W/mK, occur without permeability, and aging 1000 hours at 150 DEG C, its hardness, thermal conductivity factor change≤5% can
It is applied to the interface radiating in the fields such as LED illumination.
Claims (6)
1. a kind of graphene-based silica gel heat-conducting pad, it is characterised in that composed of the following components by mass parts：
2. graphene-based silica gel heat-conducting pad according to claim 1, it is characterised in that described vinyl silicone oil ethene
Base content is 0.04%～0.2%, viscosity 500cps～5000cps；The active hydrogen content of described containing hydrogen silicone oil is 0.16%
～0.8%；Described catalyst is platinum catalyst；Described silane coupler be gamma-aminopropyl-triethoxy-silane, γ-
(2,3- the third oxygen of epoxy) propyl trimethoxy silicane and/or γ-methacryloxypropyl trimethoxy silane；Described suppression
Preparation is ethynylcyclohexanol；The particle diameter of described ball-aluminium oxide is 0.5 μm～70 μm；Described modified graphene is oxidation
The reduced graphene of aluminium assembling modification.
3. graphene-based silica gel heat-conducting pad according to claim 1, it is characterised in that the preparation of the modified graphene
Process is comprised the following steps：
301st, in mass ratio 100：2.5:10～100:5:75, by graphene oxide, surface modifier and aluminium ion additive point
Dissipate in the aqueous hydrogen peroxide solution that mass percent concentration is 20%～40%, temperature control at 150 DEG C～350 DEG C, at heating
Reason 1～2 hour；Solution is 1.5～3 with the volume ratio of solution；
302nd, it is cooled to after room temperature, addition excessive ammonia is alkali lye, at 50 DEG C～100 DEG C, heated sealed processes 30 minutes～2
Hour；
303rd, the Graphene for obtaining step 302 and the sediment of aluminium hydroxide mixing burn under the environmental protection of inert gas
Burn and decompose 30 minutes～2 hours, obtain alumina modified Graphene.
4. graphene-based silica gel heat-conducting pad according to claim 3, it is characterised in that described graphene oxide be with
Graphene oxide prepared by Hummer methods；Described surface modifier be polyvinylpyrrolidone, dodecyl sodium sulfate, 16
At least one in alkyl trimethyl ammonium chloride and titanate coupling agent；Described aluminium ion additive is that aluminum sulfate saturation is water-soluble
At least one in liquid, aluminium hydrogen sulfate saturated aqueous solution, aluminium chloride saturated aqueous solution and aluminum nitrate saturated aqueous solution；Excessive ammonia
For the ammoniacal liquor of mass percent concentration 20%～30%；The temperature that calcination is decomposed is 1080 DEG C to 1120 DEG C.
5. its preparation method of graphene-based silica gel heat-conducting pad described in a kind of claim 1, it is characterised in that including following step
Suddenly：
501st, the weight portion as described in claim 1, by vinyl silicone oil, containing hydrogen silicone oil, catalyst, silane coupler and suppression
Agent stirs；
502nd, after adding the ball-aluminium oxide that 300～800 mass parts are dried to stir, 100 mass parts modified graphenes are added
Continue to stir；
503rd, the mixed material for obtaining step 502 is kneaded 5～10 times, is then vacuumized and is sloughed bubble, obtains paste material；
504th, by the paste material for obtaining calendering, solidification, graphene-based silica gel heat-conducting pad is obtained.
6. graphene-based silica gel heat-conducting pad according to claim 5 and preparation method thereof, it is characterised in that in step
In 504, paste material is placed in the middle of two-layer PET mould release membrance, pressure be 5～10MPa, temperature be 180 DEG C under conditions of roll
Shaping, solidifies 0.5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611257806.4A CN106634863A (en) | 2016-12-30 | 2016-12-30 | Graphene based silica gel heat-conductive gasket and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611257806.4A CN106634863A (en) | 2016-12-30 | 2016-12-30 | Graphene based silica gel heat-conductive gasket and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106634863A true CN106634863A (en) | 2017-05-10 |
Family
ID=58837504
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611257806.4A Pending CN106634863A (en) | 2016-12-30 | 2016-12-30 | Graphene based silica gel heat-conductive gasket and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106634863A (en) |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286673A (en) * | 2017-07-26 | 2017-10-24 | 南通壹选工业设计有限公司 | A kind of device for transformer with high polymer compound buffer layer |
| CN107445144A (en) * | 2017-05-31 | 2017-12-08 | 柯良节 | The manufacture method of functionalised silica gel graphene |
| CN108034256A (en) * | 2017-12-01 | 2018-05-15 | 青岛德通纳米技术有限公司 | A kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery and preparation method thereof |
| CN108102144A (en) * | 2017-12-26 | 2018-06-01 | 中国科学院宁波材料技术与工程研究所 | A kind of graphene-based heat-conductive composite material and preparation method thereof |
| CN109096743A (en) * | 2018-08-11 | 2018-12-28 | 深圳市新纶科技股份有限公司 | A kind of graphene film aligned and preparation method thereof and composite radiating film |
| CN109294236A (en) * | 2018-08-21 | 2019-02-01 | 广州特种承压设备检测研究院 | A kind of preparation method of the graphene-based heat conductive silica gel of high dispersive |
| CN109535553A (en) * | 2018-11-09 | 2019-03-29 | 安徽江淮汽车集团股份有限公司 | A kind of flame-proof weather-resisting PP composite material and preparation method |
| CN109778590A (en) * | 2019-01-11 | 2019-05-21 | 浙江理工大学 | A kind of modified expanded graphite composite seal preparation method |
| CN110157196A (en) * | 2019-03-22 | 2019-08-23 | 中国科学院工程热物理研究所 | A kind of grapheme material oriented alignment and with silicagel pad composite forming method and product |
| CN111718694A (en) * | 2020-06-19 | 2020-09-29 | 宝依德精密模切(无锡)有限公司 | Heat conducting fin and preparation method thereof |
| CN111876875A (en) * | 2020-07-02 | 2020-11-03 | 安第斯智能科技(广东)有限公司 | Single-face corrugated board bonding paper-pressing high-temperature-resistant belt |
| CN112625658A (en) * | 2019-10-09 | 2021-04-09 | 广东乐普泰新材料科技有限公司 | Efficient heat-conducting gasket and preparation method thereof |
| CN112985624A (en) * | 2021-02-24 | 2021-06-18 | 上海军辉信息技术有限公司 | Building intelligent monitoring system for weak current engineering |
| CN114015117A (en) * | 2021-10-22 | 2022-02-08 | 世晨材料技术(上海)有限公司 | Heat-conducting filler and anti-aging organic silicon heat-conducting gel prepared from heat-conducting filler |
| CN114196211A (en) * | 2021-12-28 | 2022-03-18 | 佛山金戈新材料股份有限公司 | Preparation method of low-specific-gravity high-heat-conductivity gasket |
| CN114605967A (en) * | 2022-03-30 | 2022-06-10 | 安徽碳华新材料科技有限公司 | Preparation method of modified graphene with high thermal conductivity |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234828A (en) * | 2010-04-28 | 2011-11-09 | 中国科学院力学研究所 | In situ preparation method of self-lubricating ceramic coating on aluminium alloy surface |
| CN103436027A (en) * | 2013-09-09 | 2013-12-11 | 北京化工大学 | Heat-conducting electric insulation silicon rubber thermal interface material and preparation method thereof |
| CN103723704A (en) * | 2012-10-15 | 2014-04-16 | 海洋王照明科技股份有限公司 | Graphene/nano-alumina compound and preparation method thereof |
| CN105368051A (en) * | 2015-11-13 | 2016-03-02 | 深圳德邦界面材料有限公司 | High-heat conductivity heat-conduction silica gel pad and preparation method thereof |
| CN105400201A (en) * | 2015-12-14 | 2016-03-16 | 湖南工业大学 | Spherical alumina/graphene composite heat-conducting silicone grease and preparation method thereof |
| CN105964193A (en) * | 2016-04-25 | 2016-09-28 | 东南大学 | Method for preparing graphene oxide-alumina composite aerogel |
-
2016
- 2016-12-30 CN CN201611257806.4A patent/CN106634863A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234828A (en) * | 2010-04-28 | 2011-11-09 | 中国科学院力学研究所 | In situ preparation method of self-lubricating ceramic coating on aluminium alloy surface |
| CN103723704A (en) * | 2012-10-15 | 2014-04-16 | 海洋王照明科技股份有限公司 | Graphene/nano-alumina compound and preparation method thereof |
| CN103436027A (en) * | 2013-09-09 | 2013-12-11 | 北京化工大学 | Heat-conducting electric insulation silicon rubber thermal interface material and preparation method thereof |
| CN105368051A (en) * | 2015-11-13 | 2016-03-02 | 深圳德邦界面材料有限公司 | High-heat conductivity heat-conduction silica gel pad and preparation method thereof |
| CN105400201A (en) * | 2015-12-14 | 2016-03-16 | 湖南工业大学 | Spherical alumina/graphene composite heat-conducting silicone grease and preparation method thereof |
| CN105964193A (en) * | 2016-04-25 | 2016-09-28 | 东南大学 | Method for preparing graphene oxide-alumina composite aerogel |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445144A (en) * | 2017-05-31 | 2017-12-08 | 柯良节 | The manufacture method of functionalised silica gel graphene |
| CN107286673A (en) * | 2017-07-26 | 2017-10-24 | 南通壹选工业设计有限公司 | A kind of device for transformer with high polymer compound buffer layer |
| CN108034256A (en) * | 2017-12-01 | 2018-05-15 | 青岛德通纳米技术有限公司 | A kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery and preparation method thereof |
| CN108102144A (en) * | 2017-12-26 | 2018-06-01 | 中国科学院宁波材料技术与工程研究所 | A kind of graphene-based heat-conductive composite material and preparation method thereof |
| CN109096743B (en) * | 2018-08-11 | 2021-11-12 | 新纶新材料股份有限公司 | Graphene film in oriented arrangement, preparation method thereof and composite heat dissipation film |
| CN109096743A (en) * | 2018-08-11 | 2018-12-28 | 深圳市新纶科技股份有限公司 | A kind of graphene film aligned and preparation method thereof and composite radiating film |
| CN109294236A (en) * | 2018-08-21 | 2019-02-01 | 广州特种承压设备检测研究院 | A kind of preparation method of the graphene-based heat conductive silica gel of high dispersive |
| WO2020037902A1 (en) * | 2018-08-21 | 2020-02-27 | 广州特种承压设备检测研究院 | Preparation method of high-dispersion graphene-based heat conductive silica gel |
| CN109535553A (en) * | 2018-11-09 | 2019-03-29 | 安徽江淮汽车集团股份有限公司 | A kind of flame-proof weather-resisting PP composite material and preparation method |
| CN109778590A (en) * | 2019-01-11 | 2019-05-21 | 浙江理工大学 | A kind of modified expanded graphite composite seal preparation method |
| CN110157196A (en) * | 2019-03-22 | 2019-08-23 | 中国科学院工程热物理研究所 | A kind of grapheme material oriented alignment and with silicagel pad composite forming method and product |
| CN110157196B (en) * | 2019-03-22 | 2021-09-07 | 中国科学院工程热物理研究所 | Graphene material directional arrangement and silica gel pad composite forming method and product |
| CN112625658A (en) * | 2019-10-09 | 2021-04-09 | 广东乐普泰新材料科技有限公司 | Efficient heat-conducting gasket and preparation method thereof |
| CN111718694A (en) * | 2020-06-19 | 2020-09-29 | 宝依德精密模切(无锡)有限公司 | Heat conducting fin and preparation method thereof |
| CN111876875A (en) * | 2020-07-02 | 2020-11-03 | 安第斯智能科技(广东)有限公司 | Single-face corrugated board bonding paper-pressing high-temperature-resistant belt |
| CN112985624A (en) * | 2021-02-24 | 2021-06-18 | 上海军辉信息技术有限公司 | Building intelligent monitoring system for weak current engineering |
| CN114015117A (en) * | 2021-10-22 | 2022-02-08 | 世晨材料技术(上海)有限公司 | Heat-conducting filler and anti-aging organic silicon heat-conducting gel prepared from heat-conducting filler |
| CN114015117B (en) * | 2021-10-22 | 2024-01-09 | 世晨材料技术(上海)有限公司 | Heat-conducting filler and ageing-resistant organic silicon heat-conducting gel prepared from heat-conducting filler |
| CN114196211A (en) * | 2021-12-28 | 2022-03-18 | 佛山金戈新材料股份有限公司 | Preparation method of low-specific-gravity high-heat-conductivity gasket |
| CN114605967A (en) * | 2022-03-30 | 2022-06-10 | 安徽碳华新材料科技有限公司 | Preparation method of modified graphene with high thermal conductivity |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106634863A (en) | Graphene based silica gel heat-conductive gasket and preparation method thereof | |
| CN107353017A (en) | A kind of graphene coated alumina ceramic powder and preparation method and application | |
| CN108383530B (en) | ZrB2Preparation process of-SiC ceramic composite powder by precursor conversion method | |
| CN109371308B (en) | The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end | |
| WO2017041454A1 (en) | High thermal conductivity composite interface material and preparation method therefor | |
| CN106747640B (en) | A kind of beta-silicon nitride nanowire enhancing porous silicon carbide silicon materials and preparation method thereof | |
| JP6676479B2 (en) | Hexagonal boron nitride powder and method for producing the same | |
| CN103981381A (en) | Method for preparing nano aluminum oxide dispersion enhanced copper-base composite material according to sol-gel method | |
| CN106810267A (en) | A kind of preparation method of high purity silicon nitride Si powder | |
| CN105253896A (en) | Preparation method for graphene-4A type molecular sieve composite material | |
| CN111484334B (en) | High alpha-phase silicon nitride powder and preparation method thereof | |
| CN105523528A (en) | Method for preparing boron nitride nanosheet by using eutectic salt to strip boron nitride powder at high temperature | |
| CN107488349A (en) | A kind of heat-conducting silicone grease being modified using graphene and aluminum oxide binary additive and preparation method thereof | |
| CN111793363B (en) | Annual ring-shaped graphene organic silicon resin bionic composite material and preparation method and application thereof | |
| CN106186773B (en) | A kind of air entrained concrete foaming agent and its application method | |
| CN110317977B (en) | Preparation method of graphene aerogel aluminum composite material | |
| CN106833545A (en) | A kind of high heat conduction Composition spacer material and preparation method | |
| CN109465464A (en) | A method of preparing alumina-based ceramic metal nano composite powder | |
| CN107128925A (en) | A kind of method that non-hydrolytic sol-gel combination carbothermic method prepares SiC powder | |
| CN113292857A (en) | Heat-conducting gel containing whiskers and preparation method thereof | |
| CN113401890A (en) | Preparation method of graphene quantum dot reinforced aluminum matrix composite | |
| CN104528724A (en) | Laminar nano-grade silicon carbide low-temperature preparation method | |
| CN109082109A (en) | A kind of polyamide and graphene high heat conducting nano composite material and preparation method thereof | |
| CN114230154B (en) | Quartz crucible with long service life and low deformation rate and preparation method thereof | |
| CN109338178A (en) | It is a kind of to use SrCO3Rotten hypereutectic al-si composite material and Modification Manners |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170510 |
|
| RJ01 | Rejection of invention patent application after publication |