CN106700660A - Graphene-coated oxide heat conduction filler and preparation method thereof - Google Patents
Graphene-coated oxide heat conduction filler and preparation method thereof Download PDFInfo
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- CN106700660A CN106700660A CN201710011059.4A CN201710011059A CN106700660A CN 106700660 A CN106700660 A CN 106700660A CN 201710011059 A CN201710011059 A CN 201710011059A CN 106700660 A CN106700660 A CN 106700660A
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 75
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000945 filler Substances 0.000 title abstract description 14
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 3
- 238000011049 filling Methods 0.000 claims description 41
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 19
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 18
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 18
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229920002125 Sokalan® Polymers 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- 239000004584 polyacrylic acid Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- -1 polypropylene Polymers 0.000 claims description 5
- 150000005837 radical ions Chemical class 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 239000012459 cleaning agent Substances 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 239000012798 spherical particle Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 150000002927 oxygen compounds Chemical class 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000002131 composite material Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000013019 agitation Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012946 outsourcing Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a graphene-coated oxide heat conduction filler and a preparation method thereof. The graphene-coated oxide heat conduction filler is prepared by compounding oxide, graphene and polyacrylate. The preparation method of the graphene-coated oxide heat conduction filler comprises the following steps of dissolving the polyacrylate into a solvent at room temperature, and forming a polyacrylate solution; adding the oxide into the polyacrylate solution at room temperature to form a first mixture; uniformly dispersing the graphene into the first mixture to form a second mixture; separating solid matter from the second mixture, and performing post-treatment, so as to obtain the graphene-coated oxide heat conduction filler. The graphene-coated oxide heat conduction filler has the advantages that the heat conduction coefficient is high, and the like; the graphene-coated oxide heat conduction filler is suitable for multiple types of macromolecular polymers; the preparation technology is simple, the operability is strong, the sources of raw materials are wide, the environment-friendly effect is realized, and the cost is low.
Description
Technical field
The present invention be more particularly directed to a kind of graphene coated oxide heat filling and preparation method thereof, belong to thermal interfacial material
Technical field.
Background technology
With the lifting of electronic product performance, high-power electrical, the extensive use of electronic product, under being assembled to high integration
Heat management propose requirement higher.At present, the production most simple and effective method of Heat Conduction Material is with the inorganization of high heat conduction
Compound or metal packing are filled to body, so as to improve the heat conductivility of material.
In all kinds of heat fillings, although nitride, carbide etc. are with thermal conductivity factor higher, there is price and hold high
It is expensive, the shortcomings of property is unstable, and the viscosity of system can be caused to increase in a large amount of filling process, so that limit product should
Use field.And aluminum oxide (Al2O3), magnesia (MgO), the inorganic oxide filler such as zinc oxide (ZnO) is due to cheap, system
It is standby to be simply widely used in all kinds of heat conduction products, but the thermal conductivity factor of inorganic oxide itself is not high, to make matrix
Obtaining thermal conductivity higher often needs to increase the loading of oxide filler, and this will cause the rigidity reinforced of composite, hardness
The drawbacks such as increase.
Research shows that low dimensional structures material shows excellent performance in terms of heat transfer.And Graphene be carbon atom with
SP2The bi-dimensional cellular shape lattice structure that key close-packed arrays are formed, with larger specific surface area, excellent stability, high
Heat conductivity value.And the two-dimentional geometrical shape of Graphene can form stronger coupling with matrix material, be expected to be applied to and lead
Hot filler it is modified.Accordingly, existing some researchers attempt being modified Graphene to inorganic heat filling, but its is past
The past chemical surface modification for needing to carry out Graphene and inorganic heat filling complexity, complex operation, high cost, it is difficult to scale
Change and implement.
The content of the invention
It is a primary object of the present invention to provide a kind of graphene coated oxide heat filling and preparation method thereof, with gram
Take the deficiencies in the prior art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
A kind of graphene coated oxide heat filling is the embodiment of the invention provides, it includes：85wt%~95wt%
Oxide, 5wt%~15wt% Graphenes, remainder includes polyacrylate；And polyacrylic acid in the heat filling
Content≤the 1wt% of salt.
A kind of graphene coated oxide heat filling is the embodiment of the invention provides, it is mainly by oxide, Graphene
It is compounded to form with polyacrylate；Also, in the graphene coated oxide heat filling, at least part of Graphene passes through
Reacted with absorption polyacrylic acid radical ion on oxides and combined with oxide, the polyacrylic acid radical ion derives from institute
State polyacrylate.
Further, the graphene coated oxide heat filling is (85~95) by mass ratio：(5~15)：(0~
1) oxide, Graphene and polyacrylate are compounded to form, and the consumption of the polyacrylate is not 0.
The embodiment of the present invention additionally provides a kind of preparation method of graphene coated oxide heat filling, and it includes：
A be dissolved in polyacrylate in solvent at room temperature by (), form polyacrylate solution；
B () to oxide is added in the polyacrylate solution, forms the first mixture at room temperature；
C be scattered in graphene uniform in first mixture by (), form the second mixture；
D () isolates the solid content in second mixture, the oxide heat conduction of post-treated acquisition graphene coated
Filler.
In some more preferred embodiment, polypropylene in polyacrylate dispersion liquid described in abovementioned steps (a)
The concentration of hydrochlorate is 0.3wt%~1.0wt%.
Further, the solvent preferably includes water.
In some more preferred embodiment, oxide and the mass ratio of Graphene that foregoing second mixture is included
It is 5：1~20：1.
In some more preferred embodiment, abovementioned steps (d) include：After second mixture is stood, remove
Remove supernatant, and filtration treatment carried out to remaining mixture, much filtrate is obtained with cleaning agent cleaning afterwards, then by much filtrate in
40 DEG C~80 DEG C vacuum drying, obtain the graphene coated oxide heat filling.
Preferably, the cleaning agent includes deionized water and/or ethanol etc., and not limited to this.
In some specific implementation cases of the invention, a kind of method for preparing graphene coated oxide heat filling can
To comprise the following steps：
A be dissolved in Sodium Polyacrylate in deionized water at room temperature by (), prepare Sodium Polyacrylate dispersion liquid；
B () to oxide is added in sodium polyacrylate solution, stirs at room temperature；
Graphene is added in c mixed system that () is obtained to step (b), and it is ultrasonically treated；
D () continues more than the mixed system 20min that whipping step (b) is obtained, stand, and is taken out after removing supernatant
Filter, and to be washed be placed in afterwards for several times with deionized water and ethanol and dry more than 4h in 60 DEG C of vacuum drying ovens, that is, obtain graphene coated
Oxide heat filling.
Further, in abovementioned steps (a), Sodium Polyacrylate can be dissolved in deionized water by high-speed stirred and be obtained
It is the sodium polyacrylate solution of 0.3wt%~1.0wt% to concentration.Preferably, the concentration of the sodium polyacrylate solution can be with
It is 0.7wt%.
The embodiment of the present invention additionally provides the graphene coated oxide heat filling prepared by foregoing any one method.
Further, foregoing oxide is preferably spherical in the present invention or spherical particle, and its particle diameter is less than 100 μm,
Especially preferably 0.1 μm~40 μm.
Further, oxide foregoing in the present invention includes any one in aluminum oxide, zinc oxide, magnesia or two
Plant the combination of the above, and not limited to this.
Further, polyacrylate foregoing in the present invention preferably includes Sodium Polyacrylate or polyacrylic acid potassium.Especially
For preferred, the weight average molecular weight of the Sodium Polyacrylate is 8 × 103~3 × 107。
Further, the piece footpath of Graphene foregoing in the present invention is 5 μm~30 μm, thickness≤10nm.
Further, Graphene foregoing in the present invention can be obtained by approach such as purchased in market, self-controls.
Polyacrylic acid radical ion is formed by making polyacrylate be ionized in solution in the present invention, and makes polypropylene acid group
Ion is specifically adsorbed on the surface of oxide, and interaction further occurs with Graphene is attached together, so as to be formed
Graphene coated oxide heat filling, is allowed to effectively be lifted in application the heat radiation elements of electronic product etc.
Heat dispersion, but also without detriment to the other performance of electronic product etc..
It is summarized, than prior art, graphene coated oxide heat filling of the invention has high thermal conductivity coefficient etc.
Advantage, is adapted as the heat filling application of electronic product etc., while its preparation process is simple, workable, raw material sources
Extensive and environment-friendly, low cost.
Brief description of the drawings
Fig. 1 a are the scanning electron microscope (SEM) photographs of alumina powder in embodiment 1.
Fig. 1 b are the scanning electron microscope (SEM) photographs of graphene coated aluminum oxide heat filling in embodiment 1.
Specific embodiment
In view of deficiency of the prior art, inventor is able to propose of the invention through studying for a long period of time and largely put into practice
Technical scheme.Further will be made to technical scheme, its implementation process and principle etc. with reference to some embodiments as follows
Illustrate.
The preparation method of the graphene coated aluminum oxide heat filling of embodiment 1 includes：
A the weight average molecular weight of 2.0g is at room temperature 8 × 10 by ()3Sodium Polyacrylate at a high speed be scattered in 2.8L deionized waters
In, obtain the Sodium Polyacrylate dispersion liquid that concentration is 1.0wt%；
B () is at room temperature to addition 200.0g alumina powders, the wherein grain of aluminum oxide in above-mentioned Sodium Polyacrylate dispersion liquid
Footpath scope is 0.2~50 μm.Then mechanical agitation 20min is carried out with the rotating speed of 7000r/min；
C () is 5 μm~30 μm to 40.0g pieces footpath is added in above-mentioned system, the outsourcing Graphene of thickness≤10nm, and ultrasound
30min；
D the above-mentioned system of () mechanical agitation is after 20 minutes, stand, and skims and carry out after supernatant suction filtration, and with deionized water with
After ethanol washing for several times, it is placed in 60 DEG C of vacuum drying ovens and dries more than 4 hours, that is, obtains the alumina powder of graphene coated,
The powder is graphene coated aluminum oxide heat filling.
Refering to the SEM figures for shown in Fig. 1 a being alumina powder before coated graphite alkene.It is graphene coated oxygen refering to Fig. 1 b
Change the SEM figures of aluminium heat filling.
The thermal conductivity factor of above-mentioned graphene coated aluminum oxide heat filling is tested according still further to ASTM D5470 standards,
Result shows that the thermal conductivity factor of the graphene coated aluminum oxide heat filling is 79.2W/mK, than uncoated aluminum oxide
The thermal conductivity factor of (28.3W/mK) increased 179.8%.And aforementioned polypropylene acid sodium, Graphene and alumina powder are taken according to 1：
20：100 mass ratio mixes in deionized water, then the thermal conductivity factor of the composite granule of vacuum dried formation is 30.9W/
mK。
The preparation method of the embodiment 2 graphene coated magnesia heat filling includes：
A 2.0g weight average molecular weight is at room temperature 3 × 10 by ()7Sodium Polyacrylate at a high speed be scattered in 2.8L deionized waters
In, obtain the polyacrylic acid potassium dispersion liquid of 0.3wt%；
B () is at room temperature to addition 200.0g magnesium oxide powders, the wherein grain of magnesia in above-mentioned polyacrylic acid potassium dispersion liquid
Footpath is 0.2~10 μm.Then mechanical agitation 20min is carried out with the rotating speed of 7000r/min；
C () is 5 μm~30 μm to 10.0g pieces footpath is added in above-mentioned system, the outsourcing Graphene of thickness≤10nm, and ultrasound
30min；
D the above-mentioned system of () mechanical agitation stands after 20 minutes.Skim and carry out after supernatant suction filtration, and with deionized water and
Ethanol washing is placed in 40 DEG C of vacuum drying ovens and dries 10 hours afterwards for several times, that is, obtain the magnesium oxide powder of graphene coated, described
Powder is graphene coated magnesia heat filling.
The thermal conductivity factor of above-mentioned graphene coated magnesia heat filling is tested according to ASTM D5470 standards, is tied
Fruit shows that the heat filling has Thermal conductivity.
The preparation method of the embodiment 3 graphene coated aluminum oxide/zinc oxide composite heat-conducting filler includes：
A 2.0g weight average molecular weight is at room temperature 4 × 10 by ()6Sodium Polyacrylate at a high speed be scattered in 2.8L deionized waters
In, obtain the Sodium Polyacrylate dispersion liquid of 0.7wt%；
B () is at room temperature to adding 200.0g composite granules (wherein aluminum oxide and oxidation in above-mentioned Sodium Polyacrylate dispersion liquid
The particle size range of zinc is respectively 0.2~50 μm and 0.2~10 μm, and both mass ratioes are 1:1), entered with the rotating speed of 7000r/min
Row mechanical agitation 20min；
C () is 5 μm~30 μm to 20.0g pieces footpath is added in above-mentioned system, the self-control Graphene of thickness≤10nm, and ultrasound
30min；
D the above-mentioned system of () mechanical agitation stands after 20 minutes.Skim and carry out after supernatant suction filtration, and with deionized water and
Ethanol washing is placed in 80 DEG C of vacuum drying ovens and dries more than 4 hours afterwards for several times, the composite granule for obtaining as graphene coated oxygen
Change aluminium/zinc oxide composite heat-conducting filler.
The thermal conductivity factor of above-mentioned graphene coated composite heat-conducting filler is tested according to ASTM D5470 standards, as a result
Show that the heat filling has Thermal conductivity.
It should be appreciated that above-described embodiment is only explanation technology design of the invention and feature, this is familiar with its object is to allow
The personage of item technology will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention.It is all
According to the equivalent change or modification that spirit of the invention is made, should all be included within the scope of the present invention.
Claims (10)
1. a kind of graphene coated oxide heat filling, it is characterised in that including：85wt%~95wt% oxides, 5wt%
~15wt% Graphenes, remainder includes polyacrylate；And the content of polyacrylate in the heat filling≤
1wt%.
2. graphene coated oxide heat filling according to claim 1, it is characterised in that：The oxide is spherical
Or spherical particle, its particle diameter is less than 100 μm, preferably 0.1 μm~40 μm；Preferably, the oxide includes aluminum oxide, oxygen
Any one in change zinc, magnesia or two or more combinations；And/or, the polyacrylate include Sodium Polyacrylate or
Polyacrylic acid potassium；Preferably, the weight average molecular weight of the Sodium Polyacrylate is 8 × 103~3 × 107；And/or, the Graphene
Piece footpath be 5 μm~30 μm, thickness≤10nm.
3. a kind of graphene coated oxide heat filling, it is characterised in that：The graphene coated oxide heat filling master
To be compounded to form by oxide, Graphene and polyacrylate；Also, in the graphene coated oxide heat filling,
At least part of Graphene is reacted by the polyacrylic acid radical ion with absorption on oxides and is combined with oxide, described poly- third
Olefin(e) acid radical ion derives from the polyacrylate.
4. graphene coated oxide heat filling according to claim 3, it is characterised in that：The graphene coated oxygen
Compound heat filling is (85~95) by mass ratio：(5~15)：The oxide of (0~1), Graphene and polyacrylate are compound
Formed, and the consumption of polyacrylate is not 0；Preferably, the oxide is spherical or spherical particle, and its particle diameter is less than
100 μm, especially preferably 0.1 μm~40 μm；Preferably, the oxide is including any in aluminum oxide, zinc oxide, magnesia
One or more combination；It is preferred that, the polyacrylate includes Sodium Polyacrylate or polyacrylic acid potassium；Preferably, institute
The weight average molecular weight for stating Sodium Polyacrylate is 8 × 103~3 × 107；Preferably, the piece footpath of the Graphene is 5 μm~30 μm, thick
Degree≤10nm.
5. a kind of preparation method of graphene coated oxide heat filling, it is characterised in that including：
A be dissolved in polyacrylate in solvent at room temperature by (), form polyacrylate solution；
B () to oxide is added in the polyacrylate solution, forms the first mixture at room temperature；
C be scattered in graphene uniform in first mixture by (), form the second mixture；
D () isolates the solid content in second mixture, the oxide heat filling of post-treated acquisition graphene coated.
6. preparation method according to claim 5, it is characterised in that：Polyacrylate solution cohesion described in step (a)
The concentration of acrylates is 0.3wt%~1.0wt%；Preferably, the polyacrylate includes Sodium Polyacrylate or polypropylene
Sour potassium；Preferably, the weight average molecular weight of the Sodium Polyacrylate is 8 × 103~3 × 107；Preferably, the solvent includes water.
7. preparation method according to claim 5, it is characterised in that：Oxide described in step (b) is spherical particle,
Its particle diameter is less than 100 μm, preferably 0.1 μm~40 μm；Preferably, the oxide is including in aluminum oxide, zinc oxide, magnesia
Any one or two or more combinations.
8. preparation method according to claim 5, it is characterised in that：The piece footpath of Graphene described in step (c) be 5 μm~
30 μm, thickness≤10nm；Preferably, the oxide that second mixture is included is 5 with the mass ratio of Graphene：1~20：1.
9. preparation method according to claim 5, it is characterised in that step (d) includes：Second mixture is stood
Afterwards, supernatant is removed, and filtration treatment is carried out to remaining mixture, much filtrate is obtained with cleaning agent cleaning afterwards, then will filter
Go out thing in 40 DEG C~80 DEG C vacuum drying, obtain the graphene coated oxide heat filling；Preferably, the cleaning agent bag
Include deionized water and/or ethanol.
10. the graphene coated oxide heat filling that prepared by the method as any one of claim 5-9.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809468A (en) * | 2018-12-28 | 2019-05-28 | 南通奥新电子科技有限公司 | A kind of preparation method and applications of nano barium phthalate |
| CN113174147A (en) * | 2021-04-12 | 2021-07-27 | 华南理工大学 | Submicron spherical zinc oxide particle and preparation method thereof |
| CN113480875A (en) * | 2021-07-27 | 2021-10-08 | 雷索新材料(苏州)有限公司 | Aluminum oxide modified graphene, graphene heat dissipation coating and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006082962A1 (en) * | 2005-02-07 | 2006-08-10 | Shinano Kenshi Kabushiki Kaisha | Method for producing composite particles |
| CN102343239A (en) * | 2011-05-20 | 2012-02-08 | 四川大学 | Oxidized graphene or graphene/inorganic particle core/shell material and preparation method thereof |
| CN103205075A (en) * | 2012-01-17 | 2013-07-17 | 帛宏兴业股份有限公司 | Heat radiation material, heat radiation structure, and preparation method and application thereof |
| CN103706349A (en) * | 2014-01-21 | 2014-04-09 | 中国计量学院 | Nano ZnO microsphere/graphene photocatalyst and preparation method thereof |
| CN103725002A (en) * | 2013-12-27 | 2014-04-16 | 中国科学院深圳先进技术研究院 | Aluminum oxide composite material and preparation method thereof, and copper clad base plate |
| CN104007236A (en) * | 2014-05-26 | 2014-08-27 | 太原理工大学 | Preparation method and application of graphene/zinc oxide nano composite material |
| CN104724732A (en) * | 2015-02-26 | 2015-06-24 | 南昌大学 | Method for coating magnesia with graphene |
| JP2016108214A (en) * | 2014-11-28 | 2016-06-20 | 川研ファインケミカル株式会社 | Graphene-coated alumina, assembly of graphene-coated alumina, graphene-coated alumina-containing electronic material, and surface hydrophobic treatment method |
-
2017
- 2017-01-06 CN CN201710011059.4A patent/CN106700660B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006082962A1 (en) * | 2005-02-07 | 2006-08-10 | Shinano Kenshi Kabushiki Kaisha | Method for producing composite particles |
| CN102343239A (en) * | 2011-05-20 | 2012-02-08 | 四川大学 | Oxidized graphene or graphene/inorganic particle core/shell material and preparation method thereof |
| CN103205075A (en) * | 2012-01-17 | 2013-07-17 | 帛宏兴业股份有限公司 | Heat radiation material, heat radiation structure, and preparation method and application thereof |
| CN103725002A (en) * | 2013-12-27 | 2014-04-16 | 中国科学院深圳先进技术研究院 | Aluminum oxide composite material and preparation method thereof, and copper clad base plate |
| CN103706349A (en) * | 2014-01-21 | 2014-04-09 | 中国计量学院 | Nano ZnO microsphere/graphene photocatalyst and preparation method thereof |
| CN104007236A (en) * | 2014-05-26 | 2014-08-27 | 太原理工大学 | Preparation method and application of graphene/zinc oxide nano composite material |
| JP2016108214A (en) * | 2014-11-28 | 2016-06-20 | 川研ファインケミカル株式会社 | Graphene-coated alumina, assembly of graphene-coated alumina, graphene-coated alumina-containing electronic material, and surface hydrophobic treatment method |
| CN104724732A (en) * | 2015-02-26 | 2015-06-24 | 南昌大学 | Method for coating magnesia with graphene |
Non-Patent Citations (2)
| Title |
|---|
| MI ZHOU,等: "Heat transport enhancement of thermal energy storage material using graphene/ceramic composites", 《CARBON》 * |
| 杨晓喻: "氧化锌-石墨烯杂化材料的性能和机理研究", 《中国科学技术大学硕士学位论文》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809468A (en) * | 2018-12-28 | 2019-05-28 | 南通奥新电子科技有限公司 | A kind of preparation method and applications of nano barium phthalate |
| CN113174147A (en) * | 2021-04-12 | 2021-07-27 | 华南理工大学 | Submicron spherical zinc oxide particle and preparation method thereof |
| CN113480875A (en) * | 2021-07-27 | 2021-10-08 | 雷索新材料(苏州)有限公司 | Aluminum oxide modified graphene, graphene heat dissipation coating and preparation method thereof |
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