CN106700660B - Graphene coated oxide heat filling and preparation method thereof - Google Patents
Graphene coated oxide heat filling and preparation method thereof Download PDFInfo
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- CN106700660B CN106700660B CN201710011059.4A CN201710011059A CN106700660B CN 106700660 B CN106700660 B CN 106700660B CN 201710011059 A CN201710011059 A CN 201710011059A CN 106700660 B CN106700660 B CN 106700660B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 69
- 238000011049 filling Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 26
- 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 40
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 16
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 229920002125 Sokalan® Polymers 0.000 claims description 11
- 239000004584 polyacrylic acid Substances 0.000 claims description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 150000005837 radical ions Chemical class 0.000 claims description 5
- 239000012459 cleaning agent Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000012798 spherical particle Substances 0.000 claims description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 description 11
- 239000000843 powder Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 239000002131 composite material Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000000945 filler Substances 0.000 description 6
- 238000010907 mechanical stirring Methods 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- -1 polypropylene Polymers 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-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
- 238000012946 outsourcing Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 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
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 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
- 239000011231 conductive filler Substances 0.000 description 1
- 238000001035 drying 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
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 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
- 239000011159 matrix material Substances 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
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 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
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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 kind of graphene coated oxide heat fillings and preparation method thereof.The graphene coated oxide heat filling is mainly compounded to form by oxide, graphene and polyacrylate.The preparation method of the graphene coated oxide heat filling includes: that polyacrylate is dissolved in solvent at room temperature, forms polyacrylate solution；Oxide is added into the polyacrylate solution at room temperature, forms the first mixture；It disperses graphene uniform in first mixture, forms the second mixture；Isolate the solid content in second mixture, the post-treated oxide heat filling for obtaining graphene coated.Graphene coated oxide heat filling of the invention has many advantages, such as high thermal conductivity coefficient, is suitable for the heat filling of a variety of high molecular polymers, while its preparation process is simple, strong operability, raw material sources are extensive and environmental-friendly, at low cost.
Description
Technical field
The present invention is more particularly directed to a kind of graphene coated oxide heat fillings and preparation method thereof, belong to thermal interfacial material
Technical field.
Background technique
With the promotion of electronic product performance, high integration group is loaded in the extensive use of high-power electrical, electronic product
Heat management more stringent requirements are proposed.Currently, the production most simple and effective method of Heat Conduction Material is with the inorganization of high thermal conductivity
It closes object or metal packing is filled body, to improve the heating conduction of material.
In all kinds of heat fillings, although the thermal coefficient with higher such as nitride, carbide, it is high that there are prices
Expensive, the disadvantages of property is unstable, and the viscosity that will lead in a large amount of filling process system increases, to limit answering for product
Use field.And aluminium oxide (Al2O3), magnesia (MgO), the inorganic oxide fillers such as zinc oxide (ZnO) are due to cheap, system
It is standby to be simply widely used in all kinds of thermally conductive products, but the thermal coefficient of inorganic oxide itself is not high, to make matrix
The loading that higher thermal conductivity often needs to increase oxide filler is obtained, this will lead to the rigidity reinforced of composite material, 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 has biggish specific surface area, excellent stability, high
Heat conductivity value.And the two-dimentional geometrical shape of graphene can be formed with basis material it is stronger couple, be expected to be applied to and lead
The modification of hot filler.It attempts for graphene to be modified inorganic heat filling correspondingly, having some researchers, but its is past
It is complicated for operation, at high cost, it is difficult to scale toward the chemical surface modification for needing to carry out graphene and inorganic heat filling complexity
Change and implements.
Summary of the invention
The main purpose of the present invention is to provide a kind of graphene coated oxide heat filling and preparation method thereof, with gram
Take the deficiencies in the prior art.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides a kind of graphene coated oxide heat fillings comprising: 85wt%~95wt%
Oxide, 5wt%~15wt% graphene, rest part include polyacrylate；And polyacrylic acid in the heat filling
Content≤1wt% of salt.
The embodiment of the invention provides a kind of graphene coated oxide heat fillings, mainly by oxide, graphene
It is compounded to form with polyacrylate；Also, in the graphene coated oxide heat filling, at least partly graphene passes through
It is reacted in conjunction with oxide with the polyacrylic acid radical ion of absorption on oxides, the polyacrylic acid radical ion derives from institute
State polyacrylate.
Further, the graphene coated oxide heat filling is (85~95): (5~15) by mass ratio: (0~
1) oxide, graphene and polyacrylate is compounded to form, and the dosage of the polyacrylate is not 0.
The embodiment of the invention also provides a kind of preparation methods of graphene coated oxide heat filling comprising:
(a) polyacrylate is dissolved in solvent at room temperature, forms polyacrylate solution；
(b) oxide is added into the polyacrylate solution at room temperature, forms the first mixture；
(c) it disperses graphene uniform in first mixture, forms the second mixture；
(d) solid content in second mixture is isolated, the post-treated oxide for obtaining graphene coated is thermally conductive
Filler.
In some more preferred embodiments, 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 embodiments, the mass ratio of oxide and graphene that aforementioned second mixture includes
For 5:1~20:1.
In some more preferred embodiments, abovementioned steps (d) include: after standing second mixture, to remove
Remove supernatant, and processing be filtered to remaining mixture, obtained much filtrate is cleaned with cleaning agent later, 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 ethyl alcohol etc., and without being limited thereto.
In some specific implementation cases of the invention, a kind of method preparing graphene coated oxide heat filling can
To include the following steps:
(a) Sodium Polyacrylate is dissolved in deionized water at room temperature, prepares Sodium Polyacrylate dispersion liquid；
(b) oxide is added into sodium polyacrylate solution at room temperature, stirs；
(c) graphene is added into the mixed system that step (b) is obtained, and is ultrasonically treated；
(d) continue the mixed system 20min or more that whipping step (b) is obtained, stand, remove supernatant and taken out later
Filter, and with deionized water and ethanol washing dry 4h or more is placed in 60 DEG C of vacuum drying ovens for several times to get graphene coated is arrived
Oxide heat filling.
Further, in abovementioned steps (a), Sodium Polyacrylate can be dissolved in deionized water by high-speed stirred and is obtained
The sodium polyacrylate solution for being 0.3wt%~1.0wt% to concentration.Preferably, the concentration of the sodium polyacrylate solution can be with
For 0.7wt%.
The embodiment of the invention also provides the graphene coated oxide heat fillings by aforementioned any method preparation.
Further, oxide above-mentioned is preferably spherical in the present invention or spherical particle, partial size less than 100 μm,
Especially preferably 0.1 μm~40 μm.
Further, in the present invention oxide above-mentioned include aluminium oxide, zinc oxide, in magnesia any one or two
Kind or more combination, and it is without being limited thereto.
Further, polyacrylate above-mentioned preferably includes Sodium Polyacrylate or polyacrylic acid potassium in the present invention.Especially
To be preferred, the weight average molecular weight of the Sodium Polyacrylate is 8 × 103~3 × 107。
Further, the piece diameter of graphene above-mentioned is 5 μm~30 μm in the present invention, thickness≤10nm.
Further, graphene above-mentioned can pass through the approach such as commercially available, self-control and obtain in the present invention.
Polyacrylic acid radical ion is formed by ionizing polyacrylate 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 and is attached together, to be formed
Graphene coated oxide heat filling is allowed to effectively promote the heat radiation elements of electronic product etc. in application
Heat dissipation performance, but also without detriment to the other performance of electronic product etc..
It is summarized, compared with the prior art, graphene coated oxide heat filling of the invention has high thermal conductivity coefficient etc.
Advantage is suitable for the heat filling application of electronic product etc., while its preparation process is simple, strong operability, raw material sources
It is extensive and environmental-friendly, at low cost.
Detailed description of the invention
Fig. 1 a is the scanning electron microscope (SEM) photograph of alumina powder in embodiment 1.
Fig. 1 b is the scanning electron microscope (SEM) photograph of graphene coated aluminium oxide heat filling in embodiment 1.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose of the invention
Technical solution.It as follows will be further to works such as technical solution of the present invention, its implementation process and principles in conjunction with several embodiments
It illustrates.
The preparation method of 1 graphene coated aluminium oxide heat filling of embodiment includes:
(a) at room temperature by the weight average molecular weight of 2.0g be 8 × 103Sodium Polyacrylate high speed dispersion in 2.8L deionized water
In, obtain the Sodium Polyacrylate dispersion liquid that concentration is 1.0wt%；
(b) 200.0g alumina powder is added into above-mentioned Sodium Polyacrylate dispersion liquid at room temperature, wherein the grain of aluminium oxide
Diameter range is 0.2~50 μm.Then mechanical stirring 20min is carried out with the revolving speed of 7000r/min；
(c) it is 5 μm~30 μm that 40.0g piece diameter is added into above-mentioned system, thickness≤10nm outsourcing graphene, and ultrasound
30min；
(d) the above-mentioned system of mechanical stirring after twenty minutes, stand, filtered after skimming supernatant, and with deionized water with
Ethanol washing for several times after, be placed in 60 DEG C of vacuum drying ovens dry 4 hours it is above to get to the alumina powder of graphene coated,
The powder is graphene coated aluminium oxide heat filling.
It is the SEM figure of the alumina powder before coated graphite alkene shown in a refering to fig. 1.B is graphene coated oxygen refering to fig. 1
Change the SEM figure of aluminium heat filling.
It is tested according still further to thermal coefficient of the ASTM D5470 standard to above-mentioned graphene coated aluminium oxide heat filling,
The result shows that the thermal coefficient of the graphene coated aluminium oxide heat filling is 79.2W/mK, than uncoated aluminium oxide
The thermal coefficient of (28.3W/mK) increases 179.8%.And take aforementioned polypropylene acid sodium, graphene and alumina powder according to 1:
The mass ratio of 20:100 mixes in deionized water, then vacuum dried formation composite granule thermal coefficient be 30.9W/
mK。
The preparation method of the graphene coated magnesia heat filling of embodiment 2 includes:
(a) at room temperature by 2.0g weight average molecular weight be 3 × 107Sodium Polyacrylate high speed dispersion in 2.8L deionized water
In, obtain the polyacrylic acid potassium dispersion liquid of 0.3wt%；
(b) 200.0g magnesium oxide powder is added into above-mentioned polyacrylic acid potassium dispersion liquid at room temperature, wherein the grain of magnesia
Diameter is 0.2~10 μm.Then mechanical stirring 20min is carried out with the revolving speed of 7000r/min；
(c) it is 5 μm~30 μm that 10.0g piece diameter is added into above-mentioned system, thickness≤10nm outsourcing graphene, and ultrasound
30min；
(d) the above-mentioned system of mechanical stirring after twenty minutes, is stood.Filtered after skimming supernatant, and with deionized water and
Ethanol washing is placed in 40 DEG C of vacuum drying ovens dry 10 hours for several times to get the magnesium oxide powder for arriving graphene coated, described
Powder is graphene coated magnesia heat filling.
It tests, ties according to thermal coefficient of the ASTM D5470 standard to above-mentioned graphene coated magnesia heat filling
Fruit shows that the heat filling has Thermal conductivity.
The embodiment 3 graphene coated aluminium oxide/zinc oxide composite heat-conducting filler preparation method includes:
(a) at room temperature by 2.0g weight average molecular weight be 4 × 106Sodium Polyacrylate high speed dispersion in 2.8L deionized water
In, obtain the Sodium Polyacrylate dispersion liquid of 0.7wt%；
(b) 200.0g composite granule (wherein aluminium oxide and oxidation is added into above-mentioned Sodium Polyacrylate dispersion liquid at room temperature
The particle size range of zinc is respectively 0.2~50 μm and 0.2~10 μm, and the mass ratio of the two is 1:1), with the revolving speed of 7000r/min into
Row mechanical stirring 20min；
(c) it is 5 μm~30 μm that 20.0g piece diameter is added into above-mentioned system, thickness≤10nm self-control graphene, and ultrasound
30min；
(d) the above-mentioned system of mechanical stirring after twenty minutes, is stood.Filtered after skimming supernatant, and with deionized water and
Ethanol washing is placed in 80 DEG C of vacuum drying ovens drying 4 hours or more for several times, and obtained composite granule is graphene coated oxygen
Change aluminium/zinc oxide composite heat-conducting filler.
It is tested according to thermal coefficient of the ASTM D5470 standard to above-mentioned graphene coated composite heat-conducting filler, as a result
Show that the heat filling has Thermal conductivity.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this
The personage of item technology cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all
Equivalent change or modification made by Spirit Essence according to the present invention, should be covered by the protection scope of the present invention.
Claims (14)
1. a kind of graphene coated oxide heat filling, it is characterised in that: the graphene coated oxide heat filling master
To be (85~95) by mass ratio: (5~15): oxide, graphene and the polyacrylate of (0~1) are compounded to form, wherein gathering
The dosage of acrylates is not 0；Also, in the graphene coated oxide heat filling, at least partly graphene passes through
It is reacted in conjunction with oxide with the polyacrylic acid radical ion of absorption on oxides, the polyacrylic acid radical ion derives from institute
State polyacrylate, the oxide includes aluminium oxide, zinc oxide, any one or two or more combinations in magnesia,
The oxide is spherical or spherical particle, and partial size is less than 100 μm, and the piece diameter of the graphene is 5 μm~30 μm, thickness
≤10nm。
2. graphene coated oxide heat filling according to claim 1, it is characterised in that: the partial size of the oxide
It is 0.1 μm~40 μm.
3. graphene coated oxide heat filling according to claim 1, it is characterised in that: the polyacrylate packet
Include Sodium Polyacrylate or polyacrylic acid potassium.
4. graphene coated oxide heat filling according to claim 3, it is characterised in that: the Sodium Polyacrylate
Weight average molecular weight is 8 × 103~3 × 107。
5. the preparation method of graphene coated oxide heat filling as described in claim 1, characterized by comprising:
(a) polyacrylate is dissolved in solvent at room temperature, forms polyacrylate solution；
(b) oxide is added into the polyacrylate solution at room temperature, forms the first mixture；
(c) it disperses graphene uniform in first mixture, forms the second mixture；
(d) solid content in second mixture, the post-treated oxide heat filling for obtaining graphene coated are isolated.
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%.
7. preparation method according to claim 5 or 6, it is characterised in that: the polyacrylate includes Sodium Polyacrylate
Or polyacrylic acid potassium.
8. preparation method according to claim 5, it is characterised in that: the weight average molecular weight of the Sodium Polyacrylate be 8 ×
103~3 × 107。
9. preparation method according to claim 5, it is characterised in that: the solvent includes water.
10. preparation method according to claim 5, it is characterised in that: the partial size of the oxide is 0.1 μm~40 μm.
11. preparation method according to claim 5, it is characterised in that: the oxide and stone that second mixture includes
The mass ratio of black alkene is 5:1~20:1.
12. preparation method according to claim 5, which is characterized in that step (d) includes: that second mixture is quiet
It postpones, removes supernatant, and processing is filtered to remaining mixture, obtained much filtrate is cleaned with cleaning agent later, then will
Much filtrate is dried in vacuo in 40 DEG C~80 DEG C, obtains the graphene coated oxide heat filling.
13. preparation method according to claim 12, it is characterised in that: the cleaning agent includes deionized water and/or second
Alcohol.
14. the graphene coated oxide heat filling prepared by any one of claim 5-13 the method.
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| CN201710011059.4A CN106700660B (en) | 2017-01-06 | 2017-01-06 | Graphene coated oxide heat filling and preparation method thereof |
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