CN107343374B - Graphene heat-conducting coating modified radiator and preparation method thereof - Google Patents
Graphene heat-conducting coating modified radiator and preparation method thereof Download PDFInfo
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- CN107343374B CN107343374B CN201610281272.2A CN201610281272A CN107343374B CN 107343374 B CN107343374 B CN 107343374B CN 201610281272 A CN201610281272 A CN 201610281272A CN 107343374 B CN107343374 B CN 107343374B
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- 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
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- 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
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- 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
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- 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
Abstract
The invention provides a graphene heat conduction coating modified radiator and a preparation method thereof. The graphene heat conduction coating modified radiator is composed of a heat dissipation substrate with a graphene heat conduction layer on the outer surface, and a plurality of fins with graphene heat conduction layers on the root or the whole outer surface, which is in contact with the heat dissipation substrate, wherein the graphene heat conduction layer is formed by a composite nano material formed by graphene oxide quantum dots and liquid phase exfoliated graphene. The graphene heat conduction coating modified radiator is prepared by coating a dispersion liquid of a composite nano material formed by graphene oxide quantum dots and liquid-phase exfoliated graphene on the outer surface of a heat dissipation substrate and the roots or all outer surfaces of fins in contact with the heat dissipation substrate in the modes of dipping, blade coating, spin coating, spray coating, salivation, electrophoretic deposition and the like. The graphene heat-conducting coating modified radiator provided by the invention has the advantages of abundant and cheap raw material sources, high production efficiency, simple preparation process, good heat-radiating effect and the like.
Description
Technical Field
The invention belongs to the technical field of heat dissipation engineering, and particularly relates to a graphene heat conduction coating modified heat radiator and a preparation method thereof.
Background
Along with the development of light weight, miniaturization and high power of electronic products such as computer chips, high-power electronic equipment, photoelectric devices and the like, household and industrial electric appliances such as air conditioners, televisions, refrigerators, LED lighting and the like, and modern traffic equipment such as automobiles, airplanes, ships, high-speed rails and the like, the heat generated in unit area is higher and higher, and higher requirements are put forward for a thermal control system. At present, after the traditional tube bundle type radiator, plate fin type radiator and the like are subjected to multiple times of optimized design and long-term development, the improvement of performance has met a bottleneck. Therefore, how to rapidly and safely take away the heat from the heat generating device becomes an important issue restricting the development of many industrial fields.
Generally, a heat sink is composed of a tubular or plate-type base for collecting heat and a large-area heat dissipation fin (also called fin) with various structures on the base, when the heat sink works, heat on a heating device is guided into the base of the heat sink in a heat conduction mode, then the heat is guided into the fin in the heat conduction mode, and then the heat on the fin is guided out to a surrounding medium in a heat convection and heat radiation mode, so that the purpose of heat dissipation can be achieved in a continuous process, and a device or an instrument which can timely transfer the generated heat to avoid thermal runaway is called as the heat sink.
The heat dissipation principle includes two heat conduction processes, namely a heat conduction interface formed by the contact of the heating device and the heat dissipation substrate and a heat transfer process thereof, and a heat conduction interface formed by the contact of the heat dissipation substrate and the fins and a heat transfer process thereof, so that a good heat sink necessarily requires a material having a heat conduction interface as high as possible and a high heat conductivity coefficient. At present, the radiator mainly adopts aluminum or copper metal materials with higher heat conductivity coefficient. However, the thermal conductivity of the new material graphene emerging in recent years is as high as 5300W/m · K, which is 25 times that of aluminum and 13 times that of copper, respectively, and if the new material graphene is applied to a heat sink as a heat conductive material, the heat conduction process is expected to be remarkably improved.
Since graphene is a flexible and lightweight material, graphene cannot be directly used as a heat dissipation device, but can be used in combination with a conventional aluminum or copper heat dissipation device, and particularly, the heat conduction rate between a heat dissipation substrate and fins can be remarkably improved due to the combination. Therefore, a heat radiator modified by the graphene heat conducting coating with a new structure needs to be developed; meanwhile, a new preparation method is developed, an adhesive is not used in the graphene coating, two-dimensional graphene materials can be prevented from being stacked before and after the coating is formed and being converted into a three-dimensional graphite material with a low heat conductivity coefficient, and the graphene heat conduction coating modified radiator is prepared through the method.
In conclusion, the development of the graphene heat-conducting coating modified radiator and the preparation method thereof, which have the advantages of abundant and cheap raw material sources, high production efficiency, simple preparation process and good heat dissipation effect, is still a key problem to be solved urgently in the technical field of heat dissipation engineering.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a graphene thermal conductive coating modified radiator and a preparation method thereof. The graphene heat-conducting coating modified radiator has the advantages of rich and cheap raw material sources, high production efficiency, simple preparation process, good heat dissipation effect and the like.
In order to achieve the above object, the present invention provides a graphene thermal conductive coating modified heat sink, which comprises a heat dissipation substrate having a graphene thermal conductive layer on an outer surface thereof, and a plurality of fins having a graphene thermal conductive layer on a root portion or all outer surfaces thereof contacting the heat dissipation substrate, wherein the graphene thermal conductive layer is formed of a composite nanomaterial composed of graphene oxide quantum dots and liquid-phase exfoliated graphene.
In the above-mentioned heat sink modified by the graphene thermal conductive coating, preferably, the thickness of the graphene thermal conductive layer is 0.1-10 μm, and the in-plane thermal conductivity is 600-3000W/m · K.
In the above graphene thermal conductive coating modified heat sink, preferably, in the composite nanomaterial composed of the graphene oxide quantum dots and the liquid phase exfoliated graphene, the mass ratio of the graphene oxide quantum dots to the liquid phase exfoliated graphene is 0.0001-0.1: 1.
In the above graphene thermal conductive coating modified heat sink, preferably, the heat dissipation substrate may be a solid flat or bar-shaped metal material, or a hollow flat or tube-shaped metal material having an inner cavity, and the inner cavity may contain a liquid-phase heat absorption medium or a thermal phase change material, wherein the metal material is preferably aluminum and/or copper, the liquid-phase heat absorption medium is preferably water, and the thermal phase change material is preferably paraffin.
In the above-mentioned graphene thermal conductive coating modified heat sink, preferably, the fins may be sheets of any geometric shape made of a metal material, and the fin pitch in contact with the heat dissipation substrate is not less than 1mm, wherein the metal material is preferably aluminum and/or copper.
In the above graphene thermal conductive coating modified heat spreader, preferably, the composite nanomaterial composed of graphene oxide quantum dots and liquid-phase exfoliated graphene is prepared by the following method (but not limited to the following preparation method): adding artificial and/or natural graphite powder into a solution containing graphene oxide quantum dots, uniformly mixing, utilizing the cyclic processes of stripping, re-adsorbing and re-stripping of the graphene oxide quantum dots adsorbed on graphite in the solution under the auxiliary mechanical action of high shear force, dissociating and cutting the artificial and/or natural graphite powder into a quasi-two-dimensional composite nanomaterial consisting of liquid phase stripping type graphene and graphene oxide quantum dots, and dispersing the composite nanomaterial in the solution. Wherein, the method for providing the auxiliary mechanical action of the high shearing force comprises one or more of ball milling, grinding, high-speed stirring and shearing, ultrasound and the like. The time of the cyclic process of stripping, re-adsorption and re-stripping of the graphene oxide quantum dots adsorbed on the graphite (namely, the time of treatment under the auxiliary mechanical action of the high shear force) is less than 10 hours. The solvent in the solution containing the graphene oxide quantum dots can be water or an organic solvent, such as one or a combination of several of ethylene glycol, diethylene glycol, propylene glycol, N-2-methylpyrrolidone, N-dimethylformamide, dimethyl sulfoxide and the like. Particularly preferably, the method further comprises the following steps: and (3) separating and/or cleaning the solution containing the composite nano material, and removing the excessive and free graphene oxide quantum dots, the residual incompletely-stripped graphite powder, other impurities and the like to obtain the solution of the composite nano material consisting of the purified graphene oxide quantum dots and the liquid-phase stripped graphene. Wherein, the separation and/or cleaning method can comprise one or more of filtration, centrifugation, dialysis, distillation, extraction, chemical precipitation and the like.
In the preparation method of the composite nanomaterial, preferably, the graphene oxide quantum dot is prepared by the following steps: taking a carbon-based three-dimensional block material containing a graphite laminated structure as an anode, enabling one end face (serving as a working face of the anode) of the carbon-based three-dimensional block material containing the graphite laminated structure to be in parallel contact with the liquid level of an electrolyte solution, then intermittently or continuously cutting and dissociating a graphite sheet layer at the end face by electrochemical oxidation to obtain graphene oxide quantum dots, and dissolving the graphene oxide quantum dots in the electrolyte solution to obtain a graphene oxide quantum dot solution.
According to a specific embodiment of the present invention, more specifically, the graphene oxide quantum dot is prepared by the following steps: taking the carbon series three-dimensional block material containing the graphite laminated structure as an anode, taking an inert electrode as a cathode, and respectively connecting the inert electrode with the anode and the cathode of a direct current power supply; immersing (fully immersing or partially immersing) the inert electrode in the electrolyte solution, and enabling one end face (serving as a working face of an anode) of the graphite-layered-structure-containing carbon-based three-dimensional bulk material to be in parallel contact with the liquid level of the electrolyte solution; and then starting to electrify, controlling the end face of the carbon-based three-dimensional block material to be in intermittent or continuous contact with the liquid level of the electrolyte solution, utilizing electrochemical oxidation to intermittently or continuously cut and dissociate the graphite sheet layer at the end face to obtain graphene oxide quantum dots, and dissolving the graphene oxide quantum dots in the electrolyte solution to obtain the graphene oxide quantum dot solution, wherein the concentration of the graphene oxide quantum dots in the solution is generally less than 10 mg/mL.
In the above method for preparing graphene oxide quantum dots, preferably, the working space of the end face of the carbon-based three-dimensional bulk material is in a range of-5 mm to 5mm (negative values indicate below the liquid surface, and positive values indicate above the liquid surface) from below to above the liquid surface of the electrolyte solution. The error of allowing the end face to enter the solution before electrifying is not more than 5mm relative to the liquid level, and the liquid level rises under the mechanical action of surface tension and bubbles generated by anodic oxidation after electrifying, so that the end face can work in the range of 5mm above the liquid level of the electrolyte solution before electrifying.
In the preparation method of the graphene oxide quantum dot, the selected carbon-based three-dimensional block material containing the graphite lamellar structure is a structure with regular shapes and containing graphite sheets. Preferably, the carbon series three-dimensional block material containing the graphite laminated structure comprises one or a combination of more of graphite flakes, paper, plates, wires, tubes and rods made of natural graphite or artificial graphite, carbon fiber tows and structures woven by the carbon fiber tows, such as felts, cloth, paper, ropes, plates and tubes.
In the above method for preparing graphene oxide quantum dots, preferably, the end face (serving as a working face) in parallel contact with the liquid surface of the electrolyte solution is a macroscopic surface having an angle of 60 to 90 ° with one of two-dimensional orientations of microscopic graphite sheets of the carbon-based three-dimensional bulk material having a graphite layer structure.
In the above method for preparing graphene oxide quantum dots, preferably, the electrolyte solution is a solution having ion conductivity, and the conductivity of the electrolyte solution is 10mS/cm or more.
In the above preparation method of the graphene oxide quantum dot, preferably, an electrochemical control parameter of the electrochemical oxidation process is a working voltage of a direct current power supply of 5 to 80V.
In the preparation method of the graphene oxide quantum dot, the inert electrode is a conductive electrode which is resistant to corrosion of an electrolyte solution; preferably, the inert electrode is one or a combination of several of stainless steel, titanium, platinum, nickel-based alloy, copper, lead, graphite, titanium-based oxide electrode and the like.
According to an embodiment of the present invention, preferably, the preparation method of the graphene oxide quantum dot further includes the following steps: and separating the graphene oxide quantum dot solution by adopting a physical and/or chemical method to remove electrolytes, impurities and the like in the graphene oxide quantum dot solution, so as to obtain the purified graphene oxide quantum dot solution. More preferably, the physical and/or chemical method for removing electrolytes, impurities and the like comprises one or a combination of several of filtration, centrifugation, dialysis, distillation, extraction, chemical precipitation and the like. The purified graphene oxide quantum dot solution can be an aqueous solution, and can also be a polar organic solvent solution of the graphene oxide quantum dot formed after dehydration, wherein the polar organic solvent can be one or a combination of more of ethylene glycol, diethylene glycol, ethylenediamine, N-2-methylpyrrolidone, N-dimethylformamide, dimethyl sulfoxide and the like.
In the above-described heat spreader modified with a graphene thermal conductive coating, in the composite nanomaterial composed of the graphene oxide quantum dots and the liquid-phase exfoliated graphene, the graphene oxide quantum dots have a thickness of 2nm or less, a two-dimensional sheet diameter size of 1 to 25nm, and an atomic ratio of carbon to oxygen and/or nitrogen of 1:1 to 5:1 (that is, the number of carbon atoms: the number of oxygen and/or nitrogen atoms).
In the above-mentioned heat sink modified by the graphene thermal conductive coating, preferably, in the composite nanomaterial composed of the graphene oxide quantum dots and the liquid phase exfoliated graphene, the thickness of the liquid phase exfoliated graphene is 0.7-10nm, the two-dimensional sheet diameter size is 0.1-50 μm, and the carbon content is 93wt% or more.
On the other hand, the invention also provides a preparation method of the graphene thermal conductive coating modified radiator, which comprises the following steps:
forming a composite nano material formed by graphene oxide quantum dots and liquid-phase exfoliated graphene on the outer surface of a heat dissipation substrate to form a graphene heat conduction layer;
forming a composite nano material consisting of graphene oxide quantum dots and liquid-phase exfoliated graphene on the roots or the whole outer surface of the plurality of fins to form a graphene heat conducting layer;
then, closely connecting all the fins with the graphene heat conduction layers on one or more end faces of the heat dissipation substrate with the graphene heat conduction layers along the roots of the fins according to certain geometric layout and certain intervals through mechanical bonding or metallurgical bonding to obtain the graphene heat conduction coating modified heat radiator;
alternatively, the preparation method comprises the following steps:
closely connecting a plurality of fins on one or more end surfaces of a heat dissipation substrate through mechanical bonding or metallurgical bonding according to certain geometric layout and spacing along the roots of the fins;
and then molding a composite nano material formed by the graphene oxide quantum dots and the liquid-phase exfoliated graphene on the outer surface of the heat dissipation substrate and the roots or all outer surfaces of all fins in contact with the heat dissipation substrate (the molding step can be carried out in one step or step by step), so as to form a graphene heat conduction layer, and obtain the heat radiator modified by the graphene heat conduction coating.
In the above preparation method, preferably, the graphene thermal conduction layer is formed by: and coating a dispersion liquid of a composite nano material containing graphene oxide quantum dots and liquid-phase exfoliated graphene on the outer surface of the heat dissipation substrate and the roots or all the outer surfaces of the fins in contact with the heat dissipation substrate in one or more modes of dipping, blade coating, spin coating, spray coating, salivation, electrophoretic deposition and the like, and drying to form the graphene heat conduction layer.
In the above preparation method, preferably, in the dispersion liquid of the composite nanomaterial comprising graphene oxide quantum dots and liquid phase exfoliated graphene, the graphene oxide quantum dots have a thickness of 2nm or less, a two-dimensional sheet diameter size of 1 to 25nm, and an atomic ratio of carbon to oxygen and/or nitrogen of 1:1 to 5:1 (i.e., the number of carbon atoms: the number of oxygen and/or nitrogen atoms); the thickness of the liquid phase exfoliated graphene is 0.7-10nm, the size of a two-dimensional sheet diameter is 0.1-50 mu m, and the carbon content is more than 93 wt%.
In the above preparation method, preferably, the dispersion liquid of the composite nanomaterial comprising graphene oxide quantum dots and liquid-phase exfoliated graphene may be an aqueous dispersion liquid or a polar organic solvent dispersion liquid, wherein the polar organic solvent may include one or a combination of ethylene glycol, diethylene glycol, propylene glycol, N-2-methylpyrrolidone, N-dimethylformamide, dimethyl sulfoxide and the like, and the concentration of the composite nanomaterial in the dispersion liquid may be 0.01-10 mg/mL.
In the above preparation method, preferably, the method for tightly connecting the heat dissipation substrate and the fin by mechanical bonding or metallurgical bonding may include one or a combination of forging, extruding, die casting, pressing, gear shaping, screwing, brazing, and high-temperature sintering.
The dispersion liquid of the composite nanomaterial formed by the graphene oxide quantum dots and the liquid-phase exfoliated graphene has the advantage of good dispersion stability, can basically keep a single-layer or few-layer defect-free dispersion structure of the graphene, and is favorable for forming a graphene heat conduction layer on a base material by adopting various coating processes without an adhesive. In the radiator modified by the graphene heat-conducting coating prepared by the invention, the graphene oxide quantum dots are compounded between the sheets of the liquid-phase exfoliated graphene, so that the structural integrity of the graphene layer can be maintained, the interlayer stacking of the graphene can be effectively inhibited, the functional groups of the graphene oxide quantum dots can directly interact with the substrate, and the improvement of the binding force between the graphene heat-conducting layer and the substrate is facilitated. The graphene heat-conducting coating modified radiator provided by the invention has the advantages of abundant and cheap raw material sources, high production efficiency, simple preparation process, good heat-radiating effect and the like.
Drawings
Fig. 1 is a schematic diagram illustrating a structure and a heat conduction principle of a heat sink modified by a graphene thermal conductive coating according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a graphene thermal conduction layer provided in the present invention;
fig. 3a and 3b are an atomic force microscope and a height distribution diagram of the graphene oxide quantum dots provided in example 1, respectively;
fig. 4a and 4b are a transmission electron microscope and a sheet diameter distribution diagram of the graphene oxide quantum dot provided in example 1, respectively;
fig. 5 is a photoelectron energy spectrum of the graphene oxide quantum dot provided in example 1;
fig. 6 is an atomic force microscope image of a composite nanomaterial composed of graphene oxide quantum dots and liquid phase exfoliated graphene provided in example 1;
fig. 7a and 7b are an atomic force microscope and a height distribution diagram of the graphene oxide quantum dots provided in example 7, respectively;
fig. 8a and 8b are a transmission electron microscope and a sheet diameter distribution diagram of the graphene oxide quantum dots provided in example 7, respectively;
fig. 9 is a photoelectron spectrum of the graphene oxide quantum dot provided in example 7.
Description of the main component symbols:
the heat dissipation substrate comprises a heat dissipation substrate 1, fins 2, a graphene heat conduction layer 3, a heat source 4, a heat conduction layer 5, graphene oxide quantum dots 31 and liquid phase exfoliated graphene 32.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
The invention firstly provides a composite nano-material dispersion liquid formed by graphene oxide quantum dots and liquid-phase exfoliated graphene, which can be obtained through three ways. In the first approach, graphene oxide quantum dots and liquid-phase exfoliated graphene solid powder in a certain mass ratio are mechanically and uniformly mixed, added into water or a polar organic solvent, and ultrasonically or mechanically stirred uniformly to obtain a dispersion liquid with a certain concentration. In the second approach, a certain amount of liquid-phase exfoliated graphene powder or emulsion is added into water or polar organic solvent solution of graphene oxide quantum dots with a certain concentration according to a mass ratio, and the mixture is uniformly stirred by ultrasound or machinery to obtain dispersion liquid with a certain concentration. In the third approach, artificial and/or natural graphite powder is added into the graphene oxide quantum dot solution and is uniformly mixed, under the auxiliary mechanical action of high shear force (such as ultrasound), utilizing the cyclic processes of stripping, re-adsorption and re-stripping of graphene oxide quantum dots adsorbed on graphite in a solution to dissociate and cut graphite powder into a quasi-two-dimensional composite nano material formed by liquid-phase stripping type graphene and graphene oxide quantum dots, separating and/or cleaning a mixed solution containing the composite nano material and the graphene oxide quantum dots and the like to remove excessive and free graphene oxide quantum dots, residual incompletely stripped graphite powder and other impurities and the like, and finally obtaining the dispersion liquid of the composite nano material formed by the graphene oxide quantum dots and the liquid-phase stripping type graphene.
Coating the dispersion liquid of the composite nanomaterial formed by the graphene oxide quantum dots and the liquid-phase exfoliated graphene on the outer surface of the heat dissipation substrate 1 and the roots or all the outer surfaces of the fins 2 in contact with the heat dissipation substrate 1 in one or more modes of dipping, blade coating, spin coating, spray coating, salivation, electrophoretic deposition and the like, and forming the graphene heat conduction layer 3 which is formed by stacking the graphene oxide quantum dots 31 and the liquid-phase exfoliated graphene 32 layer by layer and has a certain thickness and a high in-plane heat conduction coefficient after controlling the concentration and coating amount of the dispersion liquid and drying to obtain the radiator modified by the graphene heat conduction coating. When this modified radiator of graphite alkene heat conduction coating during operation, the heat that produces on the source of generating heat 4 is earlier through the graphite alkene heat-conducting layer 3 on the 1 bottom surface of heat dissipation substrate, along plane direction heat-conduction 5, realize by the quick conversion of point heat source to a heat source, the heat permeates heat dissipation substrate 1 afterwards, along the heat conduction 5 position of heat dissipation substrate 1 in vertical direction heat-conduction 2 and fin 2 clearance, because the heat conduction speed of the graphite alkene heat-conducting layer 3 on the heat dissipation substrate 1 surface in fin 2 surface and fin 2 clearance is compared in fin 2 and heat dissipation substrate 1 body faster, thereby realized having compared in the radiator that does not have graphite alkene heat-conducting layer 3 and having faster and more evenly distributed's heat-conduction ability, and then be favorable to the follow-up heat conduction to the surrounding environment with thermal convection and thermal radiation mode with the radiator, therefore have better heat dispersion. Fig. 1 is a schematic diagram of the structure and heat conduction principle of the heat sink modified by the graphene heat-conducting coating; fig. 2 is a schematic structural diagram of a graphene thermal conduction layer provided in the present invention.
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
Firstly, preparing a graphene oxide quantum dot solution. T70012K (12000 monofilaments) polyacrylonitrile-based carbon fiber tows are used as raw materials, the monofilament diameter of the carbon fiber is 7 mu m, the carbon fiber is composed of a microcrystalline graphite sheet layer structure, the microcrystalline three-dimensional size is 10-40nm, and the orientation of the microcrystalline graphite sheet layer is 90% of that of the fiber axis. Shearing the tip end face of the 78 carbon fiber tows, vertically placing the sheared tip end face above an electrolytic cell filled with a 0.5M sodium hydroxide aqueous solution to be used as an anode and a direct currentThe positive pole of the power supply is connected; then, an area is 100cm2The SS 304 stainless steel net is fully immersed in the solution and is used as a cathode to be connected with the negative pole of a direct current power supply; carefully adjusting the parallel distance between the neat tip end surface of the carbon fiber tows and the liquid level of the solution before electrifying, and allowing the tip end surface to enter the solution with an error of no more than 3mm relative to the liquid level based on just contacting the liquid level; then a direct current power supply is turned on, a constant voltage of 32V is controlled, the anode starts to work, a large amount of bubbles are generated, the visible solution climbs under the action of surface tension and bubbles generated by anodic oxidation, the carbon fiber tip surface can be adjusted to work within a range not exceeding 5mm above the liquid level, and the fluctuation range of the working current density relative to the tip surface area is 1-10A/cm2(ii) a When the current density is lower than 1A/cm along with the electrolytic process2When the electrolysis process is carried out, the distance between the tip end surface and the liquid level can be adjusted to be close to the tip end surface, so that the electrolysis process is continuously carried out, or the distance between the tip end surface and the liquid level can be adjusted to be close to the tip end surface again, so that the reaction is interrupted, and the distance between the tip end surface and the liquid level is adjusted to be within a range of-3 mm to 5mm, so that the intermittent operation of the electrolysis process is realized; along with the electrolytic process, the microcrystalline graphite sheet layer on the tip end face of the carbon fiber tows is subjected to electrochemical oxidation, expansion, dissociation and cutting, is continuously dissolved and enters the solution, the color of the solution gradually changes from light yellow, bright yellow, dark yellow, yellowish brown to blackish brown along with the time, the concentration of the corresponding generated graphene oxide quantum dots is gradually increased, and finally the graphene oxide quantum dot solution with the concentration not higher than 10mg/mL is obtained through 2000D membrane dialysis treatment. Fig. 3a and 3b are an atomic force microscope and a height distribution diagram of the prepared graphene oxide quantum dot, respectively, fig. 4a and 4b are a transmission electron microscope and a sheet diameter distribution diagram of the prepared graphene oxide quantum dot, respectively, fig. 5 is a photoelectron energy spectrum diagram of the prepared graphene oxide quantum dot, and it can be seen from the diagram that the thickness of the graphene oxide quantum dot is less than 2nm, the particle size distribution range is 3-15nm, and the atomic ratio of carbon/(oxygen + nitrogen) is 3: 2.
Then, preparing a dispersion liquid of the composite nano material formed by the graphene oxide quantum dots and the liquid-phase exfoliated graphene by adopting the third way, and specifically comprising the following steps of: adding 2g of natural graphite powder into the graphene oxide quantum dot solution (1L) with the concentration of 2mg/mL, carrying out ultrasonic treatment for 2 hours (wherein the ultrasonic working frequency is 20KHz, and the power is 600W), and dissociating and cutting the graphite powder into a quasi-two-dimensional liquid phase exfoliated graphene and graphene oxide quantum dot composite nano material; and finally, carrying out vacuum filtration separation and cleaning on the mixed solution containing the composite nanomaterial and the graphene oxide quantum dots and the like, removing the excessive free graphene oxide quantum dots and the residual graphite powder which is not fully dissociated, and dispersing in pure water to obtain the aqueous dispersion of the composite nanomaterial of the graphene oxide quantum dots and the liquid-phase exfoliated graphene. FIG. 6 is an atomic force microscope image of a composite nanomaterial comprising the graphene oxide quantum dots and liquid phase exfoliated graphene, wherein the liquid phase exfoliated graphene has a thickness of 1-7nm, a two-dimensional sheet diameter size of 0.5-5 μm, a carbon content of 97 wt% or more, and a mass ratio of the graphene oxide quantum dots to the liquid phase exfoliated graphene in the composite nanomaterial is 0.001: 1.
Coating the dispersion (with the concentration of 1mg/mL) of the composite nanomaterial consisting of the graphene oxide quantum dots and the liquid-phase exfoliated graphene on the outer surface of the extruded and formed aluminum alloy radiator integrating the radiating base material and the fins in one step by a dipping method, and controlling the coating amount (1 mg/cm)2) And drying at 120 ℃ to obtain a graphene heat conduction layer, wherein the average thickness of the graphene heat conduction layer is 4 +/-1 mu m, and the in-plane heat conduction coefficient of the graphene heat conduction layer is 2100W/m.K, and finally the graphene heat conduction coating modified radiator is prepared.
A150W LED lamp is used as a heating source and is respectively arranged on the radiators before and after the graphene heat-conducting coating is modified, the surface temperature of the LED lamp is detected under the stable operation to compare the natural heat dissipation effect, and the result shows that the surface temperature of the LED lamp before the modification is 85 ℃ and the surface temperature of the LED lamp after the modification is 65 ℃.
Example 2
The main differences from example 1 are: coating a dispersion liquid of a composite nano material consisting of graphene oxide quantum dots and liquid-phase exfoliated graphene on the outer surface of a heat dissipation substrate and the outer surface of the fin root, which is in contact with the heat dissipation substrate, within the range of 1cm by adopting a spraying process, and drying at 120 ℃ to form a graphene heat conduction layer with the average thickness of 0.5 +/-0.1 mu m and the in-plane heat conduction coefficient of 1688W/m.K, so as to prepare the graphene heat conduction coating modified radiator.
Similarly, a 150W LED lamp is used as a heating source and is respectively arranged on the radiators before and after the graphene heat-conducting coating is modified, the surface temperature of the LED lamp in stable operation is detected to compare the natural heat dissipation effect, and the result shows that the surface temperature of the LED lamp before modification is 85 ℃ and the surface temperature of the LED lamp after modification is 78 ℃.
Example 3
The main differences from example 1 are: the heat dissipation substrate and the fins are processed and molded independently, dispersion liquid of a composite nano material formed by graphene oxide quantum dots and liquid-phase exfoliated graphene is coated by a spraying process, a graphene heat conduction layer with the average thickness of 0.5 +/-0.1 mu m and the in-plane heat conduction coefficient of 1688W/m.K is formed after drying at 120 ℃, and the heat dissipation substrate and the fins are connected into a whole by a gear shaping process to obtain the heat radiator modified by the graphene heat conduction coating.
Similarly, a 150W LED lamp is used as a heating source and is respectively arranged on the radiators before and after the graphene heat-conducting coating is modified, the surface temperature of the LED lamp in stable operation is detected to compare the natural heat dissipation effect, and the result shows that the surface temperature of the LED lamp before modification is 88 ℃ and the surface temperature of the LED lamp after modification is 72 ℃.
Example 4
The main differences from example 3 are: the heat dissipation substrate and the fins made of red copper are respectively and independently processed and formed, then dispersion liquid of a composite nano material formed by graphene oxide quantum dots and liquid-phase exfoliated graphene is coated by adopting a blade coating process, a graphene heat conduction layer with the average thickness of 1.0 +/-0.2 mu m and the in-plane heat conduction coefficient of 800W/m.K is formed after drying at 120 ℃, and then the heat dissipation substrate and the fins are connected and formed by adopting a brazing process, so that the heat radiator modified by the graphene heat conduction coating is prepared.
Similarly, a 150W LED lamp is used as a heating source and is respectively arranged on the radiators before and after the graphene heat-conducting coating is modified, the surface temperature of the LED lamp in stable operation is detected to compare the natural heat dissipation effect, and the result shows that the surface temperature of the LED lamp before modification is 80 ℃ and the surface temperature of the LED lamp after modification is 69 ℃.
Example 5
Preparing a dispersion liquid of the composite nanomaterial consisting of the graphene oxide quantum dots and the liquid-phase exfoliated graphene by adopting the second way: adding 10g of liquid phase exfoliated graphene powder (wherein the thickness of the graphene is 2-8nm, the two-dimensional sheet diameter size is 5-35 mu m, and the carbon content is more than 99 wt%) obtained by exfoliating artificial graphite powder with a dimethyl sulfoxide liquid phase into 1 liter of dimethyl sulfoxide solution containing 5mg/mL of graphene oxide quantum dots (the graphene oxide quantum dot aqueous solution obtained in example 1 is mixed with dimethyl sulfoxide with the same volume, heating the mixed solution by rotary evaporation at 189 ℃ to completely volatilize the water in the mixed solution, then carrying out ultrasonic treatment (the power is 600W and the frequency is 20KHz) for 30 minutes to obtain the graphene oxide quantum dots, wherein the thickness of the graphene oxide quantum dots is less than 1nm, the particle size distribution range is 3-10nm, and the atomic ratio of carbon to oxygen and nitrogen is 2:1), the ultrasonic treatment (the power is 300W and the frequency is 20KHz) is carried out for 10 minutes to be uniformly mixed, and filtering and cleaning the mixed solution to remove excessive free graphene oxide quantum dots, and finally dispersing the filtered matter by using dimethyl sulfoxide to obtain a dispersion liquid of a composite nano material formed by the graphene oxide quantum dots and the liquid-phase exfoliated graphene (the concentration of the composite nano material is 2mg/mL, wherein the mass ratio of the graphene oxide quantum dots to the liquid-phase exfoliated graphene is 0.01: 1).
Coating the dispersion obtained in the way on a copper pipe heat dissipation base material by a tape casting method and coating the dispersion on a flaky aluminum foil fin by a spin coating method respectively, and controlling the coating amount (0.25 mg/cm)2) And drying at 180 ℃ to obtain a graphene heat conduction layer, wherein the average thickness of the graphene heat conduction layer is 2 +/-0.1 mu m, the in-plane heat conduction coefficient is 1600W/m.K, and the copper pipe heat dissipation substrate and the flaky aluminum foil fin are connected and molded by adopting a screw locking process to finally obtain the graphene heat conduction coating modified radiator.
A1000W electronic chip is installed on the outer surface of a copper pipe heat dissipation base material to serve as a heating source, circulating cooling water is continuously introduced into the inner cavity of the copper pipe heat dissipation base material, the heat dissipater before and after modification of the graphene heat conduction coating is inspected, and the heat dissipation effect is compared by detecting the surface temperature of the electronic chip under stable operation, so that the result shows that the surface temperature of the electronic chip before modification is 65 ℃ and the surface temperature after modification is 55 ℃.
Example 6
The main differences from example 5 are: thermal phase change material paraffin is put into an inner cavity of a copper pipe heat dissipation substrate to serve as a heat absorption medium, the heat dissipater before and after modification of the graphene heat conduction coating is inspected, and the heat dissipation effect is compared by detecting the surface temperature of the electronic chip under stable operation, and the result shows that the surface temperature of the electronic chip before modification is 59 ℃ and the surface temperature after modification is 45 ℃.
Example 7
Firstly, preparing a graphene oxide quantum dot solution. Graphite paper with the thickness of 0.1mm is taken as a raw material and is vertically arranged above an electrolytic cell filled with a sodium sulfate aqueous solution with the concentration of 0.1M to be taken as an anode to be connected with the anode of a direct current power supply; then, an area is 100cm2The nickel sheet is fully immersed in the sodium sulfate aqueous solution and is used as a cathode to be connected with the negative electrode of a direct current power supply; carefully adjusting the parallel distance between one end face of the graphite paper and the liquid level of the solution before electrifying, and allowing the error of the end face entering the solution to be no more than 5mm relative to the liquid level on the basis of just contacting the liquid level; then a direct current power supply is turned on, constant voltage is controlled to be 40V, the operation is started, the anode generates a large amount of bubbles, the visible solution climbs under the action of surface tension and bubbles generated by anodic oxidation, the end face of the graphite paper can be adjusted to operate within the range of not more than 5mm above the liquid level, and the fluctuation range of the working current density of the area of the opposite end face is 1-300A/cm2And during the period, the distance between the end face of the graphite paper and the liquid level is adjusted to enable the electrolysis process to continuously or discontinuously run, and the graphite sheet layer on the end face of the graphite paper is subjected to electrochemical oxidation, expansion, dissociation and cutting and is continuously dissolved into the solution to obtain the electrolyte containing the graphene oxide quantum dots and the graphene oxide nanoplatelets. And respectively obtaining graphene oxide microchip slurry and mixed liquid containing graphene oxide quantum dots and sodium sulfate through multiple times of centrifugal separation and water washing. Then carrying out low-temperature treatment on the mixed solution of the graphene oxide quantum dots and the sodium sulfate, taking supernatant after most of sodium sulfate crystals are separated out, and dialyzingAnd finally, carrying out freeze drying at-80 ℃ for 48h to obtain the graphene oxide quantum dot powder. Fig. 7a and 7b are an atomic force microscope and a height distribution diagram of the prepared graphene oxide quantum dot, respectively, fig. 8a and 8b are a transmission electron microscope and a sheet diameter distribution diagram of the prepared graphene oxide quantum dot, respectively, fig. 9 is a photoelectron energy spectrum diagram of the prepared graphene oxide quantum dot, and it can be seen from the diagram that the thickness of the graphene oxide quantum dot is less than 2nm, the particle size distribution range is 3-7nm, and the carbon/oxygen atomic ratio is 4: 1.
The prepared graphene oxide quantum dots and graphene solid powder (LGNS produced by Qingdao Haimaicheng New Material Co., Ltd., thickness of graphene is 1-7nm, two-dimensional sheet diameter is 1-10 μm, and carbon content is more than 95 wt%) in a mass ratio of 0.01:1 are ball-milled and mixed uniformly, added into ethylene glycol, and processed for 1h at a rotation speed of 25m/s by a high-shear dispersion emulsifier to obtain a dispersion liquid of a composite nanomaterial formed by the graphene oxide quantum dots and graphene (wherein the concentration of the composite nanomaterial is 10 mg/mL).
Coating the dispersion of the composite nanomaterial consisting of the graphene oxide quantum dots and the liquid-phase exfoliated graphene on the outer surface of the extruded heat dissipation base material and fin integrated aluminum alloy radiator in one step by a dipping method, and controlling the coating amount (2 mg/cm)2) And drying at 120 ℃ to obtain a graphene heat conduction layer, wherein the average thickness of the graphene heat conduction layer is 8 +/-1 mu m, and the in-plane heat conduction coefficient of the graphene heat conduction layer is 1200W/m.K, and finally the graphene heat conduction coating modified radiator is prepared.
A150W LED lamp is used as a heating source and is respectively arranged on the radiators before and after the graphene heat-conducting coating is modified, the surface temperature of the LED lamp is detected under the stable operation to compare the natural heat dissipation effect, and the result shows that the surface temperature of the LED lamp before the modification is 85 ℃ and the surface temperature of the LED lamp after the modification is 72 ℃.
Claims (16)
1. A graphene heat conduction coating modified radiator is composed of a heat dissipation substrate with a graphene heat conduction layer on the outer surface, and a plurality of fins with graphene heat conduction layers on the root or the whole outer surface, which is in contact with the heat dissipation substrate, wherein the graphene heat conduction layer is formed by a composite nano material formed by graphene oxide quantum dots and liquid phase exfoliated graphene;
the composite nano material formed by the graphene oxide quantum dots and the liquid phase exfoliated graphene is prepared by the following steps: adding artificial and/or natural graphite powder into a solution containing graphene oxide quantum dots, uniformly mixing, dissociating and cutting the artificial and/or natural graphite powder into a quasi-two-dimensional composite nanomaterial consisting of liquid phase exfoliated graphene and graphene oxide quantum dots by utilizing the cyclic processes of stripping, re-adsorption and re-stripping of the graphene oxide quantum dots adsorbed on graphite in the solution under the auxiliary mechanical action of high shear force, and dispersing the composite nanomaterial in the solution;
and (2) separating and/or cleaning the solution containing the composite nano material, removing the excessive and free graphene oxide quantum dots, the residual incompletely-stripped graphite and other impurities, obtaining the composite nano material formed by the graphene oxide quantum dots and the graphene, and dispersing the composite nano material in the solution.
2. The graphene thermal conductive coating modified heat sink according to claim 1, wherein the thickness of the graphene thermal conductive layer is 0.1-10 μm, and the in-plane thermal conductivity thereof is 600-3000W/m-K.
3. The graphene thermal conductive coating modified heat sink of claim 1, wherein the heat sink substrate is a solid flat or bar-shaped metal material, or a hollow flat or tube-shaped metal material containing an inner cavity.
4. The graphene thermal conductive coating modified heat spreader of claim 3, wherein the metallic material comprises aluminum and/or copper.
5. The graphene thermal conductive coating modified heat sink of claim 1, 3 or 4, wherein the fins are sheets of any geometric shape made of metal material, and the fin pitch in contact with the heat dissipation substrate is not less than 1 mm.
6. The graphene thermal conductive coating modified heat spreader of claim 5, wherein the metallic material comprises aluminum and/or copper.
7. The graphene thermal conductive coating modified heat sink of claim 3, 4 or 6, wherein a liquid phase heat absorbing medium or a thermal phase change material is contained in the inner cavity of the heat sink substrate.
8. The graphene thermal conductive coating modified heat sink of claim 5, wherein a liquid phase heat absorbing medium or a thermal phase change material is contained in the inner cavity of the heat dissipation substrate.
9. The graphene thermal conductive coating modified heat sink of claim 7, wherein the liquid phase heat absorbing medium is water and the thermal phase change material is paraffin.
10. The graphene thermal conductive coating modified heat sink of claim 8, wherein the liquid phase heat absorbing medium is water and the thermal phase change material is paraffin.
11. The graphene thermal conductive coating modified heat spreader of claim 1, wherein in the composite nanomaterial of graphene oxide quantum dots and liquid phase exfoliated graphene, the mass ratio of graphene oxide quantum dots to liquid phase exfoliated graphene is 0.0001-0.1: 1;
the thickness of the graphene oxide quantum dots is less than 2nm, the two-dimensional sheet diameter size is 1-25nm, and the atomic ratio of carbon to oxygen and/or nitrogen is 1:1-5: 1;
the thickness of the liquid phase exfoliated graphene is 0.7-10nm, the size of the two-dimensional sheet diameter is 0.1-50 mu m, and the carbon content is more than 93 wt%.
12. The graphene thermal conductive coating modified heat spreader of claim 1, wherein the high shear force assisted mechanical action is provided by one or a combination of ball milling, grinding, high speed stirring and shearing, ultrasound; the time of the cycle process of stripping, re-adsorbing and re-stripping of the graphene oxide quantum dots adsorbed on the graphite is less than 10 hours.
13. The graphene thermal conductive coating modified heat sink of claim 1 or 12, wherein the separation and/or cleaning method comprises one or a combination of filtration, centrifugation, dialysis, distillation, extraction and chemical precipitation.
14. A preparation method of a graphene heat conduction coating modified radiator comprises the following steps:
forming a composite nano material formed by graphene oxide quantum dots and liquid-phase exfoliated graphene on the outer surface of a heat dissipation substrate to form a graphene heat conduction layer;
forming a composite nano material consisting of graphene oxide quantum dots and liquid-phase exfoliated graphene on the roots or the whole outer surface of the plurality of fins to form a graphene heat conducting layer;
then, closely connecting all the fins with the graphene heat conduction layers on one or more end faces of the heat dissipation substrate with the graphene heat conduction layers along the roots of the fins according to certain geometric layout and certain intervals through mechanical bonding or metallurgical bonding to obtain the graphene heat conduction coating modified heat radiator;
alternatively, the preparation method comprises the following steps:
closely connecting a plurality of fins on one or more end surfaces of a heat dissipation substrate through mechanical bonding or metallurgical bonding according to certain geometric layout and spacing along the roots of the fins;
then, forming a composite nano material formed by the graphene oxide quantum dots and the liquid-phase exfoliated graphene on the outer surface of the heat dissipation substrate and the roots or all outer surfaces of all fins in contact with the heat dissipation substrate to form a graphene heat conduction layer, so as to obtain the heat radiator modified by the graphene heat conduction coating;
the composite nano material formed by the graphene oxide quantum dots and the liquid phase exfoliated graphene is prepared by the following steps: adding artificial and/or natural graphite powder into a solution containing graphene oxide quantum dots, uniformly mixing, dissociating and cutting the artificial and/or natural graphite powder into a quasi-two-dimensional composite nanomaterial consisting of liquid phase exfoliated graphene and graphene oxide quantum dots by utilizing the cyclic processes of stripping, re-adsorption and re-stripping of the graphene oxide quantum dots adsorbed on graphite in the solution under the auxiliary mechanical action of high shear force, and dispersing the composite nanomaterial in the solution;
and (2) separating and/or cleaning the solution containing the composite nano material, removing the excessive and free graphene oxide quantum dots, the residual incompletely-stripped graphite and other impurities, obtaining the composite nano material formed by the graphene oxide quantum dots and the graphene, and dispersing the composite nano material in the solution.
15. The method of manufacturing of claim 14, wherein the graphene thermal conductive layer is formed by: and coating a dispersion liquid of a composite nano material containing graphene oxide quantum dots and liquid-phase exfoliated graphene on the outer surface of the heat dissipation substrate and the roots or all the outer surfaces of the fins in contact with the heat dissipation substrate in one or more modes of dipping, blade coating, spin coating, spray coating, salivation and electrophoretic deposition, and drying to form the graphene heat conduction layer.
16. The method for manufacturing a heat sink as claimed in claim 14, wherein the method for mechanically or metallurgically bonding the heat sink base material and the fins tightly comprises one or more of forging, pressing, die casting, pressing, gear shaping, screwing, brazing and sintering at high temperature.
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