CN107343374A - Radiator that a kind of graphene heat conducting coating is modified and preparation method thereof - Google Patents
Radiator that a kind of graphene heat conducting coating is modified and preparation method thereof Download PDFInfo
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- CN107343374A CN107343374A CN201610281272.2A CN201610281272A CN107343374A CN 107343374 A CN107343374 A CN 107343374A CN 201610281272 A CN201610281272 A CN 201610281272A CN 107343374 A CN107343374 A CN 107343374A
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Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
- H05K7/20409—Outer radiating structures on heat dissipating housings, e.g. fins integrated with the housing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
- B05D7/146—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies to metallic pipes or tubes
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/08—Constructions of heat-exchange apparatus characterised by the selection of particular materials of metal
- F28F21/081—Heat exchange elements made from metals or metal alloys
- F28F21/084—Heat exchange elements made from metals or metal alloys from aluminium or aluminium alloys
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- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Radiator being modified the invention provides a kind of graphene heat conducting coating and preparation method thereof.The radiator that the graphene heat conducting coating is modified is the heat radiating material for having graphene heat-conducting layer by outer surface, multiple fins with the root or whole outer surfaces being in contact with heat radiating material with graphene heat-conducting layer form, and the graphene heat-conducting layer is that the composite nano materials being made up of graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed.The radiator that the graphene heat conducting coating is modified be by the dispersion liquid of composite nano materials for forming graphene oxide quantum dot and the exfoliated graphene of liquid phase to impregnate, scratch, spin coating, spraying, in a manner of salivation or electrophoretic deposition etc., be prepared on the root or whole outer surfaces of outer surface and the fin being in contact with heat radiating material coated in heat radiating material.The radiator that graphene heat conducting coating provided by the invention is modified has the advantages that raw material sources are abundant and inexpensive, production efficiency is high, preparation process is simple, good heat dissipation effect.
Description
Technical field
The invention belongs to the field of engineering technology that radiates, radiator and its system that specially a kind of graphene heat conducting coating is modified
Preparation Method.
Background technology
The electronic products such as computer chip, high-power electronic device and photoelectric device, air-conditioning, TV, refrigerator, LED
Illumination etc. the modern transportation equipment such as family expenses and industrial electric apparatus, automobile, aircraft, steamer, high ferro, with they to
Lightweight, miniaturization, high power direction are developed, and heat caused by its unit area is more and more high, and heat control system is carried
Higher requirement is gone out.At present, the radiator such as traditional bundled tube, plate-fin undergoes multiple optimization design and long-term hair
After exhibition, the improvement of performance has run into bottleneck.Therefore, how quickly, safety the heat taken away on heater members into
In order to restrict an important topic of many industrial circle development.
Usual radiator is by the tubular type of collection heat or board-like substrate and various structures, large area radiating fin thereon
(alternatively referred to as fin) composition, heat during work on heater members imported into radiator substrate by heat exchange pattern,
It imported into fin based on heat exchange pattern again, and then by thermal convection current and heat radiation mode by the heat derives on fin
To surrounding medium, such a lasting process can reach the purpose of radiating, then can by caused heat and
When shift with avoid the device of thermal runaway or instrument just be referred to as radiator.
It is related to two heat transfer processes in above-mentioned radiating principle, that is, the equipment that generates heat is in contact leading of being formed with heat radiating material
Hot interface and its heat transfer process, and heat radiating material are in contact the thermally-conductive interface to be formed and its heat transfer with fin
Process, therefore, good radiator inevitable requirement have the material of as high as possible thermally-conductive interface and high thermal conductivity coefficient.Mesh
Before, radiator is mainly using thermal conductivity factor higher aluminium or copper metal material.However, the new material emerged in recent years
Graphene, its thermal conductivity factor are up to 5300W/mK, are 13 times of 25 times of aluminium and copper respectively, if answered
For being used as Heat Conduction Material in radiator, it is expected to that above-mentioned heat transfer process can be significantly improved.
Because graphene is a kind of flexible, light material in itself, it is impossible to used directly as radiating element, but can be with
Traditional aluminium or copper radiator part are used in combination, particularly this compound it is contemplated that between heat radiating material and fin
Thermal conduction rate have and be obviously improved.Therefore, it is necessary to develop a kind of dissipating for the graphene heat conducting coating modification of new construction
Hot device；Meanwhile a kind of new preparation method of development can be in graphite ene coatings without using adhesive, additionally it is possible to prevent
Two-dimensional graphene material forms front and rear stack in coating and is changed into the low three-dimensional graphite material of thermal conductivity factor, and then passes through this
The radiator of graphene heat conducting coating modification is prepared in one method.
In summary, development is a kind of with raw material sources are abundant and inexpensive, production efficiency is high, preparation process is simple and scattered
Radiator that the good graphene heat conducting coating of thermal effect is modified and preparation method thereof, it is still anxious in radiating field of engineering technology
The key issue that need to be solved.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide the radiator that a kind of graphene heat conducting coating is modified
And preparation method thereof.The radiator that the graphene heat conducting coating is modified has raw material sources abundant and inexpensive, production efficiency
High, preparation process is simple and the advantages that good heat dissipation effect.
To reach above-mentioned purpose, present invention firstly provides a kind of graphene heat conducting coating be modified radiator, its be by
Outer surface has the heat radiating material of graphene heat-conducting layer, and the root being in contact with heat radiating material or whole outer surfaces have
Multiple fins composition of graphene heat-conducting layer, wherein the graphene heat-conducting layer is by graphene oxide quantum dot and liquid phase
What the composite nano materials that exfoliated graphene is formed were formed.
In the radiator that above-mentioned graphene heat conducting coating is modified, it is preferable that the thickness of the graphene heat-conducting layer is
0.1-10 μm, thermal conductivity factor is 600-3000W/mK in its face.
In the radiator that above-mentioned graphene heat conducting coating is modified, it is preferable that the graphene oxide quantum dot with
In the composite nano materials that the exfoliated graphene of liquid phase is formed, graphene oxide quantum dot and the exfoliated graphene of liquid phase
Mass ratio is 0.0001-0.1:1.
In the radiator that above-mentioned graphene heat conducting coating is modified, it is preferable that the heat radiating material can be solid
Tabular or bar-shaped metal materials or hollow tabular or tubular metal material containing inner chamber, and in institute
Liquid phase heat-absorbing medium or hot phase-change material can be contained by stating in inner chamber, wherein, the preferred aluminium of the metal material and/or copper,
The preferred water of liquid phase heat-absorbing medium, the hot preferred paraffin of phase-change material.
In the radiator that above-mentioned graphene heat conducting coating is modified, it is preferable that the fin can be by metal material
The tablet of manufactured any geometry, the spacing of fin being in contact with heat radiating material are not less than 1mm, wherein,
The preferred aluminium of the metal material and/or copper.
In the radiator that above-mentioned graphene heat conducting coating is modified, it is preferable that the graphene oxide quantum dot and liquid
The composite nano materials that mutually exfoliated graphene is formed be prepared by the following method to obtain (but be not limited to following preparation
Method)：In the solution containing graphene oxide quantum dot, artificial and/or native graphite powder is added, is well mixed
Afterwards, under the Aided Machine effect of high shear force, graphene oxide quantum dot of the absorption on graphite in solution is utilized
The cyclic process peel off, adsorbed, peel off again again, the artificial and/or native graphite powder dissociation and cutting are defined
The composite nano materials that the exfoliated graphene of liquid phase of two dimension is formed with graphene oxide quantum dot, and be scattered in described molten
In liquid.Wherein, there is provided the method for the Aided Machine of high shear force effect include ball milling, grinding, high-speed stirred and
One or more of combinations in shearing, ultrasound etc..The stripping of graphene oxide quantum dot of the absorption on graphite,
The time (time handled under the Aided Machine effect of the high shear force) for the cyclic process adsorb again, peeled off again
For less than 10 hours.Solvent in the solution containing graphene oxide quantum dot can be water or organic solvent,
Such as ethylene glycol, diethylene glycol (DEG), propane diols, N-2- methyl pyrrolidones, N,N-dimethylformamide and dimethyl sulfoxide (DMSO)
One or more of combinations in.It is particularly preferably, further comprising the steps of：The composite nano materials will be contained
Solution separated and/or cleaned, it is removing surplus, the graphene oxide quantum dot of free state and remnants not complete
The graphite composite powder of fully stripped and other impurities etc., graphene oxide quantum dot and the exfoliated stone of liquid phase after being purified
The solution for the composite nano materials that black alkene is formed.Wherein, it is described separation and/or cleaning method can include filtering,
One or more of combinations in centrifugation, dialysis, distillation, extraction and chemical precipitation etc..
In the preparation method of above-mentioned composite nano materials, it is preferable that described graphene oxide quantum dot is to pass through
What following steps were prepared：Contain the carbon system three-dimensional block materials of graphite laminate structure as anode using one, will described in
An end face (working face as anode) for carbon system three-dimensional block materials containing graphite laminate structure and an electrolyte
Liquid level of solution is parallel to be in contact, and is then interrupted using electrochemical oxidation or continuously the graphite flake layer of the end is cut
Cut and dissociate, obtain graphene oxide quantum dot, and be dissolved in the electrolyte solution, obtain graphene oxide amount
Son point solution.
According to the embodiment of the present invention, more specifically, above-mentioned graphene oxide quantum dot is by following step
Suddenly it is prepared：Using the carbon system three-dimensional block materials for containing graphite laminate structure as anode, by inertia electricity
Pole is connected as negative electrode, the respectively positive pole with dc source, negative pole；The inert electrode is dipped in (full leaching or leaching
Enter a part) in the electrolyte solution, and by the one of the carbon system three-dimensional block materials containing graphite laminate structure
Individual end face (working face as anode) is parallel with the electrolyte solution liquid level to be in contact；Then it is initially powered up, leads to
Cross and control the end face of the carbon system three-dimensional block materials to be interrupted with the electrolyte solution liquid level or continuously contact, utilize
Electrochemical oxidation is interrupted or continuously the graphite flake layer of the end is cut and dissociated, and obtains graphene oxide quantum
Point, and being dissolved in the electrolyte solution, obtains the graphene oxide quantum dot solution, the oxidation in the solution
The concentration of graphene quantum dot is generally below 10mg/mL.
In the preparation method of above-mentioned graphene oxide quantum dot, it is preferable that the carbon system three-dimensional block material end face
Operation interval be located at below electrolyte solution liquid level to top -5mm to 5mm (negative value represented below liquid level,
On the occasion of expression in ullage) in the range of.Allow end face to enter the error of solution before energization for relative liquid surface to be no more than
5mm, there is liquid level under surface tension and the mechanism of anodic oxidation generation bubble after energization and climb, cause to hold
Face can also be operated in the range of the top 5mm of the electrolyte solution liquid level before being powered.
In the preparation method of above-mentioned graphene oxide quantum dot, the selected carbon system three containing graphite laminate structure
It is the works containing graphite flake layer for having regular shape to tie up block materials.Preferably, it is described to contain graphite laminate knot
The carbon system three-dimensional block materials of structure include graphite flake, paper, plate, silk, pipe, rod made of native graphite or electrographite,
Carbon fibre tow and works --- the one or more in felt, cloth, paper, rope, plate, pipe etc. formed with its braiding
Combination.
In the preparation method of above-mentioned graphene oxide quantum dot, it is preferable that parallel with the electrolyte solution liquid level
The end face being in contact is and the carbon system three-dimensional block materials containing graphite laminate structure (as working face)
Macro surface of one of microcosmic graphite flake layer two-dimensional orientation angle at 60-90 °.
In the preparation method of above-mentioned graphene oxide quantum dot, it is preferable that the electrolyte solution is with ion
The solution of conductive capability, and the electrical conductivity of the electrolyte solution is more than 10mS/cm.
In the preparation method of above-mentioned graphene oxide quantum dot, it is preferable that the electrification of the electrochemical oxidation process
Learn the operating voltage 5-80V that control parameter is dc source.
In the preparation method of above-mentioned graphene oxide quantum dot, the inert electrode is rotten with potential resistance to electrolyte contamination solution
The conductive electrode of erosion；Preferably, the inert electrode is stainless steel, titanium, platinum, nickel-base alloy, copper, lead, graphite
With one or more of combinations in titanium supported oxide electrode etc..
According to the embodiment of the present invention, it is preferable that the preparation method of above-mentioned graphene oxide quantum dot is also wrapped
Include following steps：The graphene oxide quantum dot solution is separated using physically and/or chemically method, to go
Except the electrolyte in the graphene oxide quantum dot solution and impurity etc., the graphene oxide quantum dot after being purified
Solution.It is highly preferred that the physically and/or chemically method for removing electrolyte and impurity etc. include filtering, centrifugation,
One or more of combinations in dialysis, distillation, extraction and chemical precipitation etc..Graphene oxide amount after the purification
The polar organic solvent for the graphene oxide quantum dot that son point solution can be the aqueous solution or be formed after being dehydrated
Solution, polar organic solvent therein can be ethylene glycol, diethylene glycol (DEG), ethylenediamine, N-2- methyl pyrrolidones, N, N-
One or more of combinations in dimethylformamide and dimethyl sulfoxide (DMSO) etc..
In the radiator that above-mentioned graphene heat conducting coating is modified, it is preferable that the graphene oxide quantum dot with
In the composite nano materials that the exfoliated graphene of liquid phase is formed, the thickness of the graphene oxide quantum dot for 2nm with
Under, two-dimensional slice footpath size is 1-25nm, carbon and oxygen and/or the atomic ratio 1 of nitrogen:1-5:1 (i.e. carbon number：Oxygen and/
Or nitrogen-atoms numbers).
In the radiator that above-mentioned graphene heat conducting coating is modified, it is preferable that the graphene oxide quantum dot with
In the composite nano materials that the exfoliated graphene of liquid phase is formed, the thickness of the exfoliated graphene of liquid phase is
0.7-10nm, two-dimensional slice footpath size are 0.1-50 μm, and phosphorus content is more than 93wt%.
On the other hand, a kind of preparation method for the radiator being modified present invention also offers graphene heat conducting coating, it is wrapped
Include following steps：
The composite nano materials that graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed are taken shape in into heat radiating material
Outer surface, formed graphene heat-conducting layer；
The composite nano materials that graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed are taken shape in into multiple fins
Root or whole outer surfaces, formed graphene heat-conducting layer；
Then by root of all fins with graphene heat-conducting layer along fin according to certain geometric layout and spacing
One or several ends of the heat radiating material with graphene heat-conducting layer are close-coupled at by mechanical bond or metallurgical binding
On face, the radiator that described graphene heat conducting coating is modified is obtained；
Or the preparation method comprises the following steps：
Root of multiple fins along fin is passed through into mechanical bond or metallurgical binding according to certain geometric layout and spacing
It is close-coupled on one or several end faces of heat radiating material；
Then the composite nano materials that graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed are taken shape in into radiating
The outer surface of base material, and the root for all fins being in contact with heat radiating material or whole outer surfaces (the step of shaping
Can carry out in step and step by step), graphene heat-conducting layer is formed, obtains the radiating that described graphene heat conducting coating is modified
Device.
In above-mentioned preparation method, it is preferable that the graphene heat-conducting layer through the following steps that formed：One is contained
There is the dispersion liquid of the composite nano materials of graphene oxide quantum dot graphene composition exfoliated with liquid phase, by impregnating,
One or more of modes in blade coating, spin coating, spraying, salivation and electrophoretic deposition etc., coated in heat radiating material outer surface
With on the root of fin or whole outer surfaces that are in contact with heat radiating material, after drying, described graphene heat conduction is formed
Layer.
In above-mentioned preparation method, it is preferable that contain graphene oxide quantum dot and the exfoliated graphite of liquid phase described
In the dispersion liquid for the composite nano materials that alkene is formed, the thickness of the graphene oxide quantum dot is below 2nm, two
Dimension piece footpath size is 1-25nm, carbon and oxygen and/or the atomic ratio 1 of nitrogen:1-5:1 (i.e. carbon number：Oxygen and/or nitrogen-atoms
Number)；The thickness of the exfoliated graphene of liquid phase is 0.7-10nm, and two-dimensional slice footpath size is 0.1-50 μm, phosphorus content
For more than 93wt%.
In above-mentioned preparation method, it is preferable that described to contain graphene oxide quantum dot and the exfoliated graphene of liquid phase
The dispersion liquid of the composite nano materials of composition, can be aqueous dispersions or polar organic solvent dispersion liquid, its
In polar organic solvent can include ethylene glycol, diethylene glycol (DEG), propane diols, N-2- methyl pyrrolidones, N, N- diformazans
One or more of combinations in base formamide and dimethyl sulfoxide (DMSO) etc., the concentration of composite nano materials can be with dispersion liquid
For 0.01-10mg/mL.
In above-mentioned preparation method, it is preferable that the mechanical bond or metallurgical binding of heat radiating material and fin are close-connected
Method, it can include in forging, extruding, die casting, pressing, gear shaping, screw closure, soldering and high temperature sintering etc.
One or more of combinations.
Point for the composite nano materials that graphene oxide quantum dot provided by the invention is formed with the exfoliated graphene of liquid phase
Dispersion liquid, there is the advantages of dispersion stabilization is good, the individual layer of graphene or few layer zero defect dispersed structure can be kept substantially,
Graphene heat-conducting layer is formed under non-adhesive using a variety of coated techniques beneficial on base material.It is prepared in the present invention
Graphene heat conducting coating be modified radiator in, piece interlayer of the graphene oxide quantum dot in the exfoliated graphene of liquid phase
It is compound with it, the structural intergrity of graphene layer can be not only kept, the interlayer for effectively suppressing graphene stacks, and oxygen
The functional group of graphite alkene quantum dot directly can interact with base material, be advantageous to graphene heat-conducting layer and combined with base material
The raising of power.The radiator that graphene heat conducting coating provided by the invention is modified has raw material sources abundant and inexpensive, raw
The advantages that producing simple efficiency high, preparation process and good heat dissipation effect.
Brief description of the drawings
Fig. 1 is the structure and heat for the radiator that the graphene heat conducting coating that the embodiment of the invention provides is modified
Conduction principle schematic diagram；
Fig. 2 is the structural representation of graphene heat-conducting layer provided by the invention；
Fig. 3 a and Fig. 3 b are respectively the AFM and its height for the graphene oxide quantum dot that embodiment 1 provides
Distribution map；
Fig. 4 a and Fig. 4 b are respectively the transmission electron microscope and its flake diameter distribution for the graphene oxide quantum dot that embodiment 1 provides
Figure；
Fig. 5 is the photoelectron spectroscopy figure for the graphene oxide quantum dot that embodiment 1 provides；
Fig. 6 is the composite Nano material that the graphene oxide quantum dot that embodiment 1 provides is formed with the exfoliated graphene of liquid phase
The atomic force microscopy diagram of material；
Fig. 7 a and Fig. 7 b are respectively the AFM and its height for the graphene oxide quantum dot that embodiment 7 provides
Distribution map；
Fig. 8 a and Fig. 8 b are respectively the transmission electron microscope and its flake diameter distribution for the graphene oxide quantum dot that embodiment 7 provides
Figure；
Fig. 9 is the photoelectron spectroscopy figure for the graphene oxide quantum dot that embodiment 7 provides.
Primary clustering symbol description：
Heat radiating material 1, fin 2, graphene heat-conducting layer 3, pyrotoxin 4, heat transfer 5, graphene oxide quantum dot
31st, the exfoliated graphene 32 of liquid phase.
Embodiment
In order to which technical characteristic, purpose and the beneficial effect of the present invention is more clearly understood, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Present invention firstly provides the composite nano materials that graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed
Dispersion liquid, it can be obtained by three kinds of approach.The first approach, the graphene oxide quantum that certain mass is matched
Point is uniform with the exfoliated graphene solid powder mechanical mixture of liquid phase, is added in water or polar organic solvent, it is ultrasonic or
Mechanical agitation uniformly obtains certain density dispersion liquid.Second of approach, in certain density graphene oxide quantum dot
Water or polar organic solvent solution in, add the exfoliated graphene powder of a certain amount of liquid phase or breast according to quality proportioning
Liquid, ultrasound or mechanical agitation uniformly obtain certain density dispersion liquid.The third approach, in graphene oxide quantum dot
Artificial and/or native graphite powder is added in solution, after being well mixed, (the example under the Aided Machine effect of high shear force
Such as, it is ultrasonic), using the stripping of graphene oxide quantum dot of the absorption on graphite in solution, adsorb and peel off again again
Cyclic process, by graphite composite powder dissociate and cut be defined two dimension with the exfoliated graphene of liquid phase and graphene oxide amount
The composite nano materials that son point is formed, then by the mixing containing above-mentioned composite nano materials and graphene oxide quantum dot etc.
Solution is separated and/or cleaned, and removes the incomplete of superfluous, free state graphene oxide quantum dot and remnants
The graphite composite powder of stripping and other impurities etc., what is finally obtained is that described graphene oxide quantum dot is shelled with liquid phase
The dispersion liquid for the composite nano materials that release graphene is formed.
The composite nano materials that the graphene oxide quantum dot that above-mentioned approach is obtained is formed with the exfoliated graphene of liquid phase
Dispersion liquid, by impregnating, scratching, spin coating, spraying, one or more of modes in salivation and electrophoretic deposition etc.,
On outer surface and the root for the fin 2 being in contact with heat radiating material 1 or whole outer surfaces coated in heat radiating material 1,
And by controlling dispersion liquid concentration and coating amount, after drying, formed with it is certain thickness, with heat conduction in high face
The graphene heat-conducting layer being made up of graphene oxide quantum dot 31 and the exfoliated stacked in multi-layers of graphene 32 of liquid phase of coefficient
3, obtain the radiator of graphene heat conducting coating modification.When the radiator work that the graphene heat conducting coating is modified,
Caused heat first passes through the graphene heat-conducting layer 3 on the bottom surface of heat radiating material 1 on pyrotoxin 4, is passed along in-plane heat
5 are led, realizes and heat radiating material 1 is passed through by the rapid translating of heat point source to plane heat source, subsequent heat, it is vertically hot
Conduction 5 reaches the positions of heat radiating material 1 in fins 2 and the gap of fin 2, due to the surface of fin 2 and the gap of fin 2
The heat conduction velocity of graphene heat-conducting layer 3 on the surface of heat radiating material 1 is compared to fin 2 and the body of heat radiating material 1
Faster, it is achieved thereby that there is the radiator compared to no graphene heat-conducting layer 3 heat faster and being evenly distributed to pass
Ability is led, and then is advantageous to radiator subsequently in a manner of thermal convection current and heat radiation by heat derives to surrounding environment, thus
With more preferable heat dispersion.Fig. 1 is the structure and heat-conduction principle for the radiator that above-mentioned graphene heat conducting coating is modified
Schematic diagram；Fig. 2 is the structural representation of graphene heat-conducting layer provided by the invention.
Technical scheme is further described below by specific embodiment.
Embodiment 1
Graphene oxide quantum dot solution is prepared first.With T700 12K (12000 monofilament) polyacrylonitrile-radical
Carbon fibre tow is raw material, and the filament diameter of the carbon fiber is 7 μm, and it is made up of micro crystal graphite lamellar structure, crystallite
Three-dimensional dimension is oriented to 90% in 10-40nm, micro crystal graphite lamellar orientation compared to fiber axis.By above-mentioned 78 beam carbon
The tip surface of fibre bundle is had one's hair trimmed, and is vertically arranged in and is filled above the electrolytic cell that concentration is 0.5M sodium hydrate aqueous solutions,
It is connected as anode with the positive pole of dc source；It is again 100cm by an area2The stainless (steel) wires of SS 304 be dipped in entirely
In solution, it is connected as negative electrode with the negative pole of dc source；The neat point of carbon fibre tow is carefully adjusted before energization
End face and the parallel distance of liquid level of solution, are defined by just touching liquid level, it is allowed to tip surface enter solution error be
Relative liquid surface is no more than 3mm；Dc source is then turned on, controls constant voltage 32V, is started working, anode has
A large amount of bubble formations, visible solution climbs in the presence of surface tension and anodic oxidation generation bubble, now also adjustable
Section carbon fiber tip surface works in the range of ullage is no more than 5mm, the now work of opposite tip face area
Current density fluctuation range is 1-10A/cm2；It is less than 1A/cm with the trade current density of entering of electrolytic process2When it is (existing
As if tip surface widens with liquid level distance), can adjust the tip surface that furthers is carried out continuously electrolytic process with liquid level distance,
After tip surface and liquid level distance can also first be tuned up interrupting reaction, then the tip surface that furthers again exists with liquid level distance
- 3mm is to 5mm operated within range, so as to realize the intermitten service of electrolytic process；Along with the progress of electrolytic process,
Micro crystal graphite lamella on carbon fibre tow tip surface is electrochemically oxidized expansion dissociation and cutting, and constantly dissolving enters
In solution, solution colour is changed over time gradually by yellowish, bright orange, dark yellow, yellowish-brown to dark brown, corresponds to generation
Graphene oxide quantum dot concentration gradually increases, and finally obtaining concentration by 2000D film dialysis treatments is not higher than
10mg/mL graphene oxide quantum dot solution.Fig. 3 a and Fig. 3 b are respectively graphene oxide amount obtained above
The AFM and its height distribution map of son point, Fig. 4 a and Fig. 4 b are respectively graphene oxide amount obtained above
The transmission electron microscope and its flake diameter distribution figure of son point, Fig. 5 are the photoelectron spectroscopy of graphene oxide quantum dot obtained above
Figure, as we can see from the figure the thickness of the graphene oxide quantum dot be less than 2nm, particle size distribution range 3-15nm,
Carbon/(oxygen+nitrogen) atomic ratio is 3:2.
Then prepare what graphene oxide quantum dot was formed with the exfoliated graphene of liquid phase using the third above-mentioned approach
The dispersion liquid of composite nano materials, specifically includes following steps：It is the above-mentioned graphene oxide amounts of 2mg/mL in concentration
In son point solution (1L), 2g native graphite powders are added, being ultrasonically treated 2 hours, (wherein ultrasound works frequency is
20KHz, power 600W), graphite composite powder is dissociated and cut the be defined two-dimentional exfoliated graphene of liquid phase and oxidation
The compound nano material of graphene quantum dot；Finally, above-mentioned composite nano materials and graphene oxide quantum will be contained
The mixed solution of point etc. carries out being filtered by vacuum separation and cleaning, removes surplus, free state graphene oxide quantum dot
With remnants, the graphite composite powder that does not dissociate fully, by being redispersed in obtaining graphene oxide quantum dot and liquid in pure water
The aqueous dispersions of the composite nano materials of mutually exfoliated graphene.Fig. 6 is that the graphene oxide quantum dot is peeled off with liquid phase
The atomic force microscopy diagram for the composite nano materials that type graphene is formed, the wherein exfoliated graphene of liquid phase have 1-7nm
Thickness, 0.5-5 μm of two-dimensional slice footpath size, phosphorus content is more than 97wt%, graphene oxide in composite nano materials
The mass ratio of quantum dot and the exfoliated graphene of liquid phase is 0.001:1.
The dispersion liquid for the composite nano materials that above-mentioned graphene oxide quantum dot graphene exfoliated with liquid phase is formed is (dense
Spend for 1mg/mL), heat radiating material and the fin integration by extrusion forming are coated in by the step of method one of dipping
Aluminium alloy heat radiator outer surface on, and by controlling coating amount (1mg/cm2), obtain graphene after 120 DEG C of dryings
Heat-conducting layer, the average thickness of the graphene heat-conducting layer is 4 ± 1 μm, and thermal conductivity factor is 2100W/mK in its face, most
The radiator that obtained graphene heat conducting coating is modified eventually.
Above-mentioned radiating after one 150W LED is attached separately into graphene heat conducting coating before modified as pyrotoxin
On device, natural cooling effect is contrasted by detecting the surface temperature under LED stable operation, the results showed that modified
Preceding LED surface temperature is 85 DEG C, and modified is 65 DEG C.
Embodiment 2
It is with the Main Differences of embodiment 1：Only by heat radiating material and the fin root 1cm being in contact with heat radiating material
In the range of outer surface, answering for graphene oxide quantum dot exfoliated with liquid phase graphene composition is coated using spraying coating process
The dispersion liquid of nano material is closed, 0.5 ± 0.1 μm of formation thickness average out to after 120 DEG C of drying, thermal conductivity factor is in face
1688W/mK graphene heat-conducting layer, the radiator that graphene heat conducting coating is modified is made.
Equally, it is upper after one 150W LED being attached separately into graphene heat conducting coating before modified as pyrotoxin
State on radiator, contrast natural cooling effect by detecting the surface temperature under LED stable operation, as a result table
The bright surface temperature of LED before modified is 85 DEG C, and modified is 78 DEG C.
Embodiment 3
It is with the Main Differences of embodiment 1：After heat radiating material and fin each separately machined shaping, then adopt respectively
The composite nano materials formed with spraying coating process coating graphene oxide quantum dot with the exfoliated graphene of liquid phase disperse
Liquid, 0.5 ± 0.1 μm of thickness average out to is formed after 120 DEG C of dryings, the graphene that thermal conductivity factor is 1688W/mK in face
Heat-conducting layer, then heat radiating material and fin are linked into an integrated entity using gear shaping technique, it is made what graphene heat conducting coating was modified
Radiator.
Equally, it is upper after one 150W LED being attached separately into graphene heat conducting coating before modified as pyrotoxin
State on radiator, contrast natural cooling effect by detecting the surface temperature under LED stable operation, as a result table
The bright surface temperature of LED before modified is 88 DEG C, and modified is 72 DEG C.
Embodiment 4
It is with the Main Differences of embodiment 3：Use the heat radiating material and fin of red copper material instead, each it is separately machined into
After type, then compound the receiving of doctor blade process coating graphene oxide quantum dot graphene composition exfoliated with liquid phase is respectively adopted
The dispersion liquid of rice material, 1.0 ± 0.2 μm of formation thickness average out to after 120 DEG C of drying, thermal conductivity factor is 800W/mK in face
Graphene heat-conducting layer, then heat radiating material is connected into shaping with fin using soldering processes, graphene heat conducting coating is made
Modified radiator.
Equally, it is upper after one 150W LED being attached separately into graphene heat conducting coating before modified as pyrotoxin
State on radiator, contrast natural cooling effect by detecting the surface temperature under LED stable operation, as a result table
The bright surface temperature of LED before modified is 80 DEG C, and modified is 69 DEG C.
Embodiment 5
The compound of graphene oxide quantum dot graphene composition exfoliated with liquid phase is made using second above-mentioned of approach
The dispersion liquid of nano material：(will in 1 liter of dimethyl sulphoxide solution of the graphene oxide quantum dot containing 5mg/mL
The graphene oxide quantum dot aqueous solution and isometric dimethyl sulfoxide (DMSO) obtained in embodiment 1 is miscible, passes through 189 DEG C
Revolving heats above-mentioned mixed solution so that moisture content therein volatilizees completely, then surplus solution is carried out into ultrasound (power is
600W, frequency 20KHz) 30 minutes and be made, wherein the thickness of graphene oxide quantum dot is less than 1nm, grain
Footpath distribution is 3-10nm, carbon/(oxygen+nitrogen) atomic ratio is 2:1), 10g is added to peel off by dimethyl sulfoxide (DMSO) liquid phase
The exfoliated graphene powder of liquid phase (the wherein thickness 2-8nm of graphene, the two-dimensional slice footpath chi that electrographite powder obtains
Very little 5-35 μm, phosphorus content is more than 99wt%), ultrasonic (power 300W, frequency 20KHz) is mixed for 10 minutes
Close uniformly, then mixed solution filtered and cleaned, remove surplus, free state graphene oxide quantum dot,
Dimethyl sulfoxide (DMSO) dispersing and filtering thing is finally used again, obtains what graphene oxide quantum dot was formed with the exfoliated graphene of liquid phase
(composite nano materials concentration is 2mg/mL, wherein graphene oxide quantum dot and liquid to the dispersion liquid of composite nano materials
The mass ratio of mutually exfoliated graphene is 0.01:1).
The dispersion liquid that above-mentioned approach is obtained, it is coated in respectively by the tape casting on copper pipe heat radiating material, and passes through rotation
Coating is coated on sheet aluminium foil fin, and by controlling coating amount (0.25mg/cm2), obtain stone after 180 DEG C of dryings
Black alkene heat-conducting layer, the average thickness of the graphene heat-conducting layer is 2 ± 0.1 μm, and thermal conductivity factor is 1600W/mK in its face,
Copper pipe heat radiating material is connected by shaping with sheet aluminium foil fin using screw closure technique again, finally obtained graphene heat conduction
Coating modified radiator.
One 1000W electronic chip is installed on copper pipe heat radiating material outer surface as pyrotoxin, in copper pipe radiating base
Recirculated cooling water is continuously passed through in material inner chamber, the above-mentioned radiator after investigating graphene heat conducting coating before modified, passes through inspection
The surface temperature surveyed under electronic chip stable operation contrasts radiating effect, the results showed that electronic chip surface temperature before modified
Spend for 65 DEG C, modified is 55 DEG C.
Embodiment 6
It is with the Main Differences of embodiment 5：Hot phase-change material paraffin is put into copper pipe heat radiating material inner chamber as suction
Thermal medium, the above-mentioned radiator after investigating graphene heat conducting coating before modified, by detecting under electronic chip stable operation
Surface temperature contrast radiating effect, the results showed that electronic chip surface temperature is 59 DEG C before modified, modified to be
45℃。
Embodiment 7
Graphene oxide quantum dot solution is prepared first.Using graphite paper thick 0.1mm as raw material, it is vertically arranged in
Fill above the electrolytic cell that concentration is 0.1M aqueous sodium persulfate solutions, be connected as anode with the positive pole of dc source；
It is again 100cm by an area2Nickel sheet be dipped in entirely in the aqueous sodium persulfate solution, as negative electrode and the negative pole of dc source
It is connected；An end face of graphite paper and the parallel distance of liquid level of solution are carefully adjusted before energization, just to touch
Liquid level is defined, it is allowed to which the error that the end face enters solution is no more than 5mm for relative liquid surface；Then turn on dc source,
Constant voltage 40V is controlled, is started working, anode there are a large amount of bubble formations, in surface tension and anodic oxidation generation gas
Visible solution climbs in the presence of bubble, now also can adjust the scope that graphite paper end face is no more than 5mm in ullage
Interior work, now the working current density fluctuation range of opposing end surface area is 1-300A/cm2, during which adjust graphite
Paper end face makes electrolytic process continuously or discontinuously run with liquid level distance, and the graphite flake layer on graphite paper end face is by electrochemistry oxygen
Change expansion dissociation and cutting, constantly dissolving is entered in solution, is obtained containing graphene oxide quantum dot and graphite oxide
The electrolyte of alkene microplate.By repeatedly centrifuging and washing, graphene oxide microplate slurry, Yi Jihan are respectively obtained
There is the mixed liquor of graphene oxide quantum dot and sodium sulphate.The mixed liquor of graphene oxide quantum dot and sodium sulphate is entered again
Row low-temperature treatment, after most of sodium sulfate crystal is separated out, supernatant is taken to obtain comprising only graphite oxide by dialysis
The aqueous solution of alkene quantum dot, finally -80 DEG C of freeze-drying 48h of process, obtain graphene oxide quantum dot powder.Figure
7a and Fig. 7 b are respectively the AFM and its height distribution map of graphene oxide quantum dot obtained above, figure
8a and Fig. 8 b are respectively the transmission electron microscope of graphene oxide quantum dot obtained above and its flake diameter distribution figure, Fig. 9 are
The photoelectron spectroscopy figure of graphene oxide quantum dot obtained above, the as we can see from the figure graphene oxide quantum dot
Thickness be less than 2nm, particle size distribution range 3-7nm, carbon/oxygen atom ratio are 4:1.
It is 0.01 by mass ratio:The 1 above-mentioned graphene oxide quantum dot being prepared and graphene solid powder (Qingdao
The LGNS of extra large sea alkene new material Co., Ltd production, the thickness 1-7nm of graphene, 1-10 μm of two-dimensional slice footpath size,
Phosphorus content is more than 95wt%) after ball milling mixing is uniform, it is added in ethylene glycol, by high-shearing dispersion emulsifying machine,
After handling 1h under rotating speed 25m/s, the composite nano materials that graphene oxide quantum dot is formed with graphene are obtained
Dispersion liquid (composite nano materials concentration therein is 10mg/mL).
The dispersion liquid for the composite nano materials that above-mentioned graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed, leads to
The step of method one for crossing dipping is coated in outside the aluminium alloy heat radiator by heat radiating material and the fin integration of extrusion forming
On surface, and by controlling coating amount (2mg/cm2), graphene heat-conducting layer is obtained after 120 DEG C of dryings, the graphene
The average thickness of heat-conducting layer is 8 ± 1 μm, and thermal conductivity factor is 1200W/mK in its face, finally obtained graphene heat conduction
Coating modified radiator.
Above-mentioned radiating after one 150W LED is attached separately into graphene heat conducting coating before modified as pyrotoxin
On device, natural cooling effect is contrasted by detecting the surface temperature under LED stable operation, the results showed that modified
Preceding LED surface temperature is 85 DEG C, and modified is 72 DEG C.
Claims (10)
1. the radiator that a kind of graphene heat conducting coating is modified, it is the radiating for having graphene heat-conducting layer by outer surface
Base material, and multiple fins that the root being in contact with heat radiating material or whole outer surfaces have graphene heat-conducting layer form,
Wherein described graphene heat-conducting layer is the composite Nano being made up of graphene oxide quantum dot and the exfoliated graphene of liquid phase
What material was formed.
2. the radiator that graphene heat conducting coating according to claim 1 is modified, wherein, the graphene is led
The thickness of thermosphere is 0.1-10 μm, and thermal conductivity factor is 600-3000W/mK in its face.
3. the radiator that graphene heat conducting coating according to claim 1 is modified, wherein, in the oxidation stone
In the composite nano materials that black alkene quantum dot is formed with the exfoliated graphene of liquid phase, graphene oxide quantum dot is shelled with liquid phase
The mass ratio of release graphene is 0.0001-0.1:1；
The thickness of described graphene oxide quantum dot is below 2nm, and two-dimensional slice footpath size is 1-25nm, carbon and oxygen
And/or the atomic ratio 1 of nitrogen:1-5:1；
The thickness of the exfoliated graphene of described liquid phase is 0.7-10nm, and two-dimensional slice footpath size is 0.1-50 μm, carbon containing
Measure as more than 93wt%.
4. the radiator that graphene heat conducting coating according to claim 1 is modified, wherein, the heat radiating material
It is solid tabular or bar-shaped metal materials, or hollow tabular or tubular metal material containing inner chamber；It is preferred that
Ground, the metal material include aluminium and/or copper；
The fin is the tablet of geometry any made of metal material, the wing being in contact with heat radiating material
Piece spacing is not less than 1mm；Preferably, the metal material includes aluminium and/or copper.
5. the radiator that graphene heat conducting coating according to claim 4 is modified, wherein, in the radiating base
Contain liquid phase heat-absorbing medium or hot phase-change material in the inner chamber of material；Preferably, the liquid phase heat-absorbing medium is water, described
Hot phase-change material is paraffin.
6. the radiator that the graphene heat conducting coating according to claim 1 or 3 is modified, wherein, described oxygen
The composite nano materials that graphite alkene quantum dot graphene exfoliated with liquid phase is formed are through the following steps that be prepared
's：In the solution containing graphene oxide quantum dot, artificial and/or native graphite powder is added, after being well mixed,
Under the Aided Machine effect of high shear force, the stripping of graphene oxide quantum dot of the absorption on graphite in solution is utilized
From, the cyclic process adsorbing, peel off again again, the artificial and/or native graphite powder dissociation and cutting are defined two
The composite nano materials that the exfoliated graphene of liquid phase of dimension is formed with graphene oxide quantum dot, and it is scattered in the solution
In；
Preferably, there is provided the method for the Aided Machine of high shear force effect include ball milling, grinding, high-speed stirred and
One or more of combinations in shearing, ultrasound；The stripping of graphene oxide quantum dot of the absorption on graphite,
The time for the cyclic process adsorb again, peeled off again is less than 10 hours.
7. the radiator that graphene heat conducting coating according to claim 6 is modified, wherein, described oxidation stone
The preparation process for the composite nano materials that black alkene quantum dot graphene exfoliated with liquid phase is formed also includes：It will contain described
The solution of composite nano materials is separated and/or cleaned, and removes surplus, free state graphene oxide quantum dot
With the remnants graphite not being completely exfoliated and other impurities, the graphene oxide quantum dot after being purified is shelled with liquid phase
The solution for the composite nano materials that release graphene is formed；Wherein, it is described separation and/or cleaning method include filtering,
One or more of combinations in centrifugation, dialysis, distillation, extraction and chemical precipitation.
8. a kind of preparation method for the radiator that graphene heat conducting coating is modified, it comprises the following steps：
The composite nano materials that graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed are taken shape in into heat radiating material
Outer surface, formed graphene heat-conducting layer；
The composite nano materials that graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed are taken shape in into multiple fins
Root or whole outer surfaces, formed graphene heat-conducting layer；
Then by root of all fins with graphene heat-conducting layer along fin according to certain geometric layout and spacing
One or several ends of the heat radiating material with graphene heat-conducting layer are close-coupled at by mechanical bond or metallurgical binding
On face, the radiator that described graphene heat conducting coating is modified is obtained；
Or the preparation method comprises the following steps：
Root of multiple fins along fin is passed through into mechanical bond or metallurgical binding according to certain geometric layout and spacing
It is close-coupled on one or several end faces of heat radiating material；
Then the composite nano materials that graphene oxide quantum dot and the exfoliated graphene of liquid phase are formed are taken shape in into radiating
The outer surface of base material, and the root for all fins being in contact with heat radiating material or whole outer surfaces, form graphene and lead
Thermosphere, obtain the radiator that described graphene heat conducting coating is modified.
9. preparation method according to claim 8, wherein, the graphene heat-conducting layer through the following steps that
Formed：The composite nano materials that one is formed containing graphene oxide quantum dot and the exfoliated graphene of liquid phase disperse
Liquid, by impregnating, scratching, one or more of modes in spin coating, spraying, salivation and electrophoretic deposition, coated in scattered
On the root or whole outer surfaces of hot substrate outer surface and the fin being in contact with heat radiating material, after drying, described in formation
Graphene heat-conducting layer.
10. preparation method according to claim 8, wherein, the mechanical bond or metallurgy of heat radiating material and fin
Being tightly combined the method for connection includes forging, extruding, die casting, pressing, gear shaping, screw closure, soldering and high temperature burning
One or more of combinations in knot.
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| CN113363369B (en) * | 2021-05-31 | 2022-09-20 | 华中科技大学 | LED quantum dot radiating fin, LED and preparation method thereof |
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