CN110145728A - A kind of reinforcing heat radiation composite structure and preparation method thereof - Google Patents
A kind of reinforcing heat radiation composite structure and preparation method thereof Download PDFInfo
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- CN110145728A CN110145728A CN201910492168.1A CN201910492168A CN110145728A CN 110145728 A CN110145728 A CN 110145728A CN 201910492168 A CN201910492168 A CN 201910492168A CN 110145728 A CN110145728 A CN 110145728A
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- 230000005855 radiation Effects 0.000 title claims abstract description 32
- 230000003014 reinforcing effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 50
- 239000004642 Polyimide Substances 0.000 claims abstract description 25
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- 239000002184 metal Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims description 31
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- 239000004332 silver Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000004411 aluminium Substances 0.000 claims description 8
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- 238000000608 laser ablation Methods 0.000 claims description 7
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 7
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- 238000001338 self-assembly Methods 0.000 claims description 6
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- 238000003763 carbonization Methods 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims 2
- 150000003949 imides Chemical class 0.000 claims 2
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- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 4
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- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/02—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions
- B32B3/08—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions characterised by added members at particular parts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
- B32B3/266—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by an apertured layer, the apertures going through the whole thickness of the layer, e.g. expanded metal, perforated layer, slit layer regular cells B32B3/12
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V29/00—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems
- F21V29/50—Cooling arrangements
- F21V29/70—Cooling arrangements characterised by passive heat-dissipating elements, e.g. heat-sinks
- F21V29/83—Cooling arrangements characterised by passive heat-dissipating elements, e.g. heat-sinks the elements having apertures, ducts or channels, e.g. heat radiation holes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V29/00—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems
- F21V29/85—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems characterised by the material
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V29/00—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems
- F21V29/85—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems characterised by the material
- F21V29/89—Metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
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- B32B2255/205—Metallic coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/302—Conductive
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21Y—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES F21K, F21L, F21S and F21V, RELATING TO THE FORM OR THE KIND OF THE LIGHT SOURCES OR OF THE COLOUR OF THE LIGHT EMITTED
- F21Y2115/00—Light-generating elements of semiconductor light sources
- F21Y2115/10—Light-emitting diodes [LED]
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- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of reinforcing heat radiation composite structures and preparation method thereof, including graphene film (2) and it is deposited on the metal layer (3) of the graphene film (2) upper surface, the graphene film (2) and metal layer (3) are provided with array through-hole, and the metal layer (3) and array through-hole inner wall are attached with polyimides (4).On the one hand the present invention improves thermal conductivity compared with traditional metal material, facilitate the phenomenon that promoting conduction of the heat on entire radiating surface, improving temperature distributing disproportionation on radiating surface.The low sunlight absorptivity and high emissivity characteristic having simultaneously can be by the sun energy minimizations of absorption, and heat is made to be radiated space environment quickly, effectively improve whole radiating efficiency.
Description
Technical field
The invention belongs to cooling field, a kind of specifically reinforcing heat radiation composite structure and preparation method thereof.
Background technique
Electronic equipment develops to miniaturization and integrated direction so that device work heat flow density sharply increases, and takes effectively
Heat control system be to maintain the stable important channel of device operating temperature.In addition, as the mankind constantly deepen the exploration of space,
The task that satellite spacecraft is carried also becomes increasingly complex.The electronics thermal control technology operating temperature stable for maintenance spacecraft
Being one cannot be neglected technology.In the space of not medium, heat dissipation can only be carried out by heat transfer and heat radiation.It is suitable
Aerospace dissipating-heat environment is answered, the measure often taken is using thermal conductivity slightly higher metal material that the heat production of electronic device is quick
Export.It will be appreciated that the thermal conductivity of aluminium sheet or copper sheet is still lower (< 400W/mK), heat waste cannot be maximized
It loses.Meanwhile the characteristics such as aluminium sheet or the not pliable, high density of copper sheet also limit its extensive use.
Summary of the invention
The present invention provides a kind of reinforcing heat radiation composite structure and preparation method thereof, the structure and traditional metal material phase
Than on the one hand improving thermal conductivity, helping to promote conduction of the heat on entire radiating surface, improve Temperature Distribution on radiating surface
Uneven phenomenon.The low sunlight absorptivity and high emissivity characteristic having simultaneously can be by the sun energy minimizations of absorption, and make heat
Amount is radiated space environment quickly, effectively improves whole radiating efficiency.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of reinforcing heat radiation composite structure, including graphene film and the metal layer for being deposited on the graphene film upper surface,
The graphene film and metal layer are provided with array through-hole, and the metal layer and array through-hole inner wall are attached with polyimides.
Further, the metal layer is silver layer or aluminium layer.
Further, the silver layer or aluminium layer with a thickness of 200nm.
Further, the bore dia of the array through-hole be 100 μm~300 μm, Kong Zhongxin away from 0.4mm~0.8mm it
Between.
Further, the graphene film is replaced using highly oriented pyrolytic graphite.
A kind of preparation method according to reinforcing heat radiation composite structure described above, comprising the following steps:
Step 1: graphene oxide solution is prepared using liquid phase removing Hummers method, and in liquid-vapor interface self assembly shape
At graphene oxide membrane, then by being carbonized, being graphitized and prolong and suppress to obtain graphene film；
Step 2: will be existed again by direct current magnetron sputtering process after graphene film oxygen plasma treatment described in step 1
The metal layer is deposited thereon；
Step 3: it is formed on the film that step 2 is formed by graphene film and metal layer using the method for laser ablation
Array through-hole, metal covering is towards laser ablation direction；
Step 4: preparation polyimide acid (PAA)；
Step 5: the polyimide acid of step 4 preparation is coated in step 3 and is formed by the film with array through-hole
On；
Step 6: the film coated with polyimide acid prepared by step 5 is filtered, polyimide acid is enable
Penetrate into array through-hole side wall；
Step 7: the step 6 film obtained for being covered with polyimide acid is placed in atmosphere furnace, is made through ladder-elevating temperature
It obtains polyimide acid and completes imidization to obtain reinforcing heat radiation composite structure.
Further, the step 1 specifically includes: take 325 mesh of 3g natural flake graphite and 1.5g sodium nitrate with
The 120ml concentrated sulfuric acid is uniformly mixed in the water-bath of 0 DEG C of temperature, and 15g potassium permanganate is added in batches and obtains mixed liquor, by mixed liquor
Continue to stir 90min in 0 DEG C of temperature water bath, then be transferred to mixed liquor in 35 DEG C of water bath with thermostatic control, and stirred using machinery
It mixes device and is thoroughly mixed liquid, be slowly added 120ml deionized water in the backward mixed liquor of 4h and be diluted, and make mixed liquor
Temperature is no more than 100 DEG C, after addition, and obtained solution is continued to stir 15min in 95 DEG C of water-bath, obtains oxidation stone
Black solution obtains graphene oxide solution after 10wt% dilute hydrochloric acid twice and the washing of multiple deionized water, takes the concentration to be
The graphene oxide solution 50ml of 7mg/ml is slowly inverted in the Teflon mould that bottom surface is 5cm × 5cm, is being set as
It is dry in 35 DEG C of vacuum oven, it is self-assembly of graphene oxide membrane in liquid-gas interface, be carbonized using 1000 DEG C,
2800 DEG C of graphitizations and machinery, which prolong, to be pressed through journey the graphene film is made.
Further, the step 4 specifically includes: weighing 0.72 gram of 4,4'- diaminodiphenyl ether (ODA) and 1 gram respectively
Pyromellitic dianhydride (PMDA) is dissolved in 14 grams of n,N-dimethylacetamide (DMAc) solution according to sequencing and is mixed
Solution, and mixed solution is placed in 0 DEG C of water bath with thermostatic control and persistently stirs 1h, finally obtain polyimide acid (PAA).
Further, the step 7 specifically includes: the graphene film level that polyimide acid is covered in step 6 is set
In atmosphere furnace, the argon gas of 500ml/min is passed to as protection gas, is heated up with the heating rate of 0.5 DEG C/min, and respectively 80
DEG C, 110 DEG C, 140 DEG C, 170 DEG C, 200 DEG C and 220 DEG C of heat preservation 30min and complete imidizations in 250 DEG C of heat preservation 60min,
Finally obtain reinforcing heat radiation composite structure.
Compared with prior art, the present invention its remarkable advantage is:
(1) present invention is formed by the high thermal conductivity characteristic that " class sandwich " structure had both had carbon film material, herein in connection with
The flexible structure of high IR emissivity low sunlight absorptivity, while the presence of array hole plays inhibition layering in structure, by force
The effect for changing mechanical strength, under same radiating condition, highly heat-conductive material can accelerate high heat flux density and expand from hot spot to surrounding
It dissipates, higher Temperature Distribution on radiating surface is obtained, according to surface emissivity heat rejection and removal QrCalculation formula (1), high emissivity and
The biggish temperature difference can bring more heat dissipation total amounts, and array hole, which is formed by air duct, can produce heat transfer free convection effect,
With certain heat, which overcomes carbon material in the defect in space flight thermal control field, is suitable for system and electronic equipment temperature
The thermal control of degree and heat management；
Qr=ε σ (Td 4-Tspc 4) (1)
(2) silver layer of the present invention deposited by direct current magnetron sputtering process is specularly reflecting layer, and thickness is in 200nm
Left and right, the silver layer in the state can show stronger metallicity, have in solar spectrum wave band and infrared band higher
The radiation characteristic of overlayer polymer can be improved in reflectivity；
(3) array through-hole that laser ablation of the present invention is formed, enables precursor liquid to seep under the effect of the pressure
Enter array through-hole side wall, the composite construction that overlayer polymer extends in graphite linings, the structure can be formed after high-temperature process
The adhesive force between overlayer polymer and lower film can be effectively improved, the mechanical performance of laminated film entirety is promoted, is also heat
Air provides flow channel, brings certain Natural Heat Convection.
(4) manufacture craft of the present invention is simple, and polymer coating layer thickness is easily controllable, is easy to large-scale production, can large area
Preparation, and there is certain flexibility, suitable for many labyrinths, there is very big practical application value.
Detailed description of the invention
Fig. 1 is the preparation flow figure that the present invention strengthens heat radiation composite structure.
Fig. 2 is that the present invention strengthens the structural representation of heat radiation composite structure and strengthens radiating principle figure.
Specific embodiment
With reference to the accompanying drawings of the specification, the present invention is further illustrated.
In conjunction with Fig. 2, a kind of reinforcing heat radiation composite structure, including graphene film 2 and it is deposited on 2 upper surface of graphene film
Metal layer 3, the graphene film 2 and metal layer 3 be provided with array through-hole, and the metal layer 3 and array through-hole inner wall are attached
Have polyimides 4.
Further, the metal layer 3 is silver layer or aluminium layer.
Further, the silver layer or aluminium layer with a thickness of 200nm.
Further, the bore dia of the array through-hole be 100 μm~300 μm, Kong Zhongxin away from 0.4mm~0.8mm it
Between.
Further, the graphene film 3 is replaced using highly oriented pyrolytic graphite.
In conjunction with Fig. 1, a kind of preparation method according to reinforcing heat radiation composite structure described above, comprising the following steps:
Step 1: graphene oxide solution is prepared using liquid phase removing Hummers method, and in liquid-vapor interface self assembly shape
At graphene oxide membrane, then by being carbonized, being graphitized and prolong and suppress to obtain graphene film 2, the presence of the structure can accelerate heat transfer,
Effectively local temperature is avoided to increase；
Step 2: direct current magnetron sputtering process will be passed through again after the oxygen plasma treatment of graphene film 2 described in step 1
The specular layer of the metal layer 3 is deposited on it；
Step 3: using the method for laser ablation on the film that step 2 is formed by graphene film 2 and metal layer 3 shape
At array through-hole, metal covering is towards laser ablation direction；
Step 4: polymer precursor liquid polyimide acid (PAA) is prepared；
Step 5: the polyimide acid of step 4 preparation is coated in step 3 and is formed by the film with array through-hole
On；
Step 6: the film coated with polyimide acid prepared by step 5 is filtered, polyimide acid is enable
Array through-hole side wall is penetrated into, bond strength is on the one hand improved, on the other hand prevents array through-hole from being blocked by precursor liquid, in addition, battle array
Column through-hole provides good flow channel for air, facilitates the heat for further taking away headlamp generation；
Step 7: the step 6 film obtained for being covered with polyimide acid is placed in atmosphere furnace, is made through ladder-elevating temperature
It obtains polyimide acid and completes imidization to obtain reinforcing heat radiation composite structure.
The schematic diagram and acceleration radiating of heretofore described reinforcing heat radiation composite structure are as shown in Figure 2.It will be above-mentioned
Composite construction when being pasted on hot spot heat source 1 by heat-conducting silicone grease, the high-termal conductivity of bottom graphene film 2 is by the high hot-fluid of hot spot
Quickly diffusion, upper layer polyimides emission coating 4 can increase the radiation heat transfer of heat dissipation plane in conjunction with specular layer 3, and array is logical
The presence in hole penetrates into overlayer polymer in graphite film, enhances the mechanical performance of composite construction, plays and inhibits layering
Effect, while good flow channel is improved for hot-air, certain Natural Heat Convection loss is generated, is integrally shown excellent
Heat dissipation characteristics.
Embodiment 1
A kind of preparation method according to reinforcing heat radiation composite structure described above the following steps are included:
1. preparing graphene oxide solution, concrete operations are as follows: take the day of 325 mesh of 3g using the Hummers method of liquid phase removing
Right crystalline flake graphite and 1.5g sodium nitrate are uniformly mixed in 0 DEG C of temperature water bath with the 120ml concentrated sulfuric acid, and 15g Gao Meng is added in batches
Sour potassium continues mixed liquor to stir 90min in 0 DEG C of temperature water bath.Then reaction solution is transferred in 35 DEG C of water bath with thermostatic control,
And reaction solution is sufficiently stirred using mechanical agitator.It is slowly added 120ml deionized water thereto after 4h to be diluted, and makes
The temperature of reaction solution is no more than 100 DEG C.After addition, obtained solution is continued to stir 15min in 95 DEG C of water-bath.Most
Graphite oxide solution can be obtained eventually.It is molten that graphene oxide is obtained after 10wt% dilute hydrochloric acid twice and deionized water washing for several times
Liquid.The graphene oxide solution 50ml that concentration is 7mg/ml is taken slowly to be inverted in the Teflon mould that bottom surface is 5cm × 5cm
In, it is dry in the vacuum oven for being set as 35 DEG C, graphene oxide membrane is self-assembly of in liquid-gas interface.Using
1000 DEG C of carbonizations, 2800 DEG C of graphitizations and mechanical prolong press through high thermal conductivity graphene film used in the obtained present invention of journey.
2. stoichiometrically weighing 0.72 gram of 4,4'- diaminodiphenyl ether (ODA) and 1 gram of pyromellitic dianhydride respectively
(PMDA), it is dissolved in 14 grams of n,N-dimethylacetamide (DMAc) solution according to sequencing, and mixed liquor is placed in 0 DEG C of perseverance
1h is persistently stirred in tepidarium, it is final to obtain precursor liquid PAA.
3. by high thermal conductivity graphene film oxygen plasma treatment 5min made from step 1, then the side for passing through magnetron sputtering
Method deposits the silver layer of about 200nm thickness on it.
4. the through-hole array for being about 150 μm by laser etching method formation diameter by the film in step 3, every square li
Rice grain pattern hole number is about 300, and Kong Zhongxin is away from 0.5mm or so.
5. by forerunner's drop-coated obtained in step 2 the obtained film of step 4 silver layer surface, using vacuum filtration
Method carries out the of short duration suction filtration process of 10s, and precursor liquid is made to penetrate into array hole inner wall under the effect of the pressure.
6. the graphene film for being covered with PAA in step 5 is horizontally placed in atmosphere furnace, the argon gas conduct of 500ml/min is passed to
Gas is protected, is heated up with the heating rate of 0.5 DEG C/min, and respectively at 80 DEG C, 110 DEG C, 140 DEG C, 170 DEG C, 200 DEG C, 220 DEG C are protected
Warm 30min and high-temperature process are completed in 250 DEG C of heat preservation 60min, finally obtains reinforcing heat radiation composite structure.
Embodiment 2
A kind of preparation method according to reinforcing heat radiation composite structure described above the following steps are included:
1. graphene film described in embodiment 1 is replaced generation with highly oriented pyrolytic graphite.
2. stoichiometrically weighing 0.72 gram of 4,4'- diaminodiphenyl ether (ODA) and 1 gram of pyromellitic dianhydride respectively
(PMDA), it is dissolved in 14 grams of n,N-dimethylacetamide (DMAc) solution according to sequencing, and mixed liquor is placed in 0 DEG C of perseverance
1h is persistently stirred in tepidarium.It is final to obtain precursor liquid PAA.
3. the oxygen plasma treatment 5min of high thermal conductivity graphite film described in step 1 is passed through the method for magnetron sputtering
The silver layer of about 200nm thickness is deposited on it.
4. the through-hole array for being about 150 μm by laser etching method formation diameter by the film in step 3, every square li
Rice grain pattern hole number is about 305, and Kong Zhongxin is away from 0.5mm or so.
5. by forerunner's drop-coated obtained in step 2 the obtained film of step 4 silver layer surface, using vacuum filtration
Method carries out the of short duration suction filtration process of 10s, and precursor liquid is made to penetrate into array hole inner wall under the effect of the pressure.
6. the graphene film for being covered with PAA in step 5 is horizontally placed in atmosphere furnace, the argon gas conduct of 500ml/min is passed to
Gas is protected, is heated up with the heating rate of 0.5 DEG C/min, and respectively at 80 DEG C, 110 DEG C, 140 DEG C, 170 DEG C, 200 DEG C, 220 DEG C are protected
Warm 30min and high-temperature process are completed in 250 DEG C of heat preservation 60min, finally obtains reinforcing heat radiation composite structure.Bottom graphite
The thermal conductivity of film reaches as high as 1600W/mK.Its sun wave band spectral absorption is 0.15, infrared emittance 0.86.
Embodiment 3
A kind of preparation method according to reinforcing heat radiation composite structure described above the following steps are included:
1. selecting highly oriented pyrolytic graphite film as substrate high thermal conductivity film by embodiment 2.
2. stoichiometrically weighing 0.72 gram of 4,4'- diaminodiphenyl ether (ODA) and 1 gram of pyromellitic dianhydride respectively
(PMDA), it is dissolved in 14 grams of n,N-dimethylacetamide (DMAc) solution according to sequencing, and mixed liquor is placed in 0 DEG C of perseverance
1h is persistently stirred in tepidarium.It is final to obtain precursor liquid PAA.
3. heavy by the high thermal conductivity graphite film oxygen plasma treatment 5min in step 1, then by the method for magnetron sputtering
The silver layer of product about 200nm thickness.
4. the through-hole array for being about 300 μm by laser etching method formation diameter by the film in step 3, every square li
Rice grain pattern hole number is about 305, and Kong Zhongxin is away from 0.6mm or so.
5. by forerunner's drop-coated obtained in step 2 the obtained film of step 4 silver layer surface, using vacuum filtration
Method carries out the of short duration suction filtration process of 5s, and precursor liquid is made to penetrate into array hole inner wall under the effect of the pressure.
6. the graphene film for being covered with PAA in step 5 is horizontally placed in atmosphere furnace, the argon gas conduct of 500ml/min is passed to
Gas is protected, is heated up with the heating rate of 0.5 DEG C/min, and respectively at 80 DEG C, 110 DEG C, 140 DEG C, 170 DEG C, 200 DEG C, 220 DEG C are protected
Warm 30min and high-temperature process are completed in 250 DEG C of heat preservation 60min, finally obtains reinforcing heat radiation composite structure.
Basic principles and main features and advantage of the invention have been shown and described above.The technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes and improvements
It all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent circle
It is fixed.
Claims (9)
1. a kind of reinforcing heat radiation composite structure, which is characterized in that including graphene film (2) and be deposited on the graphene film (2)
The metal layer (3) of upper surface, the graphene film (2) and metal layer (3) are provided with array through-hole, the metal layer (3) and battle array
Column through-hole wall face is attached with polyimides (4).
2. reinforcing heat radiation composite structure according to claim 1, which is characterized in that the metal layer (3) is silver layer or aluminium
Layer.
3. reinforcing heat radiation composite structure according to claim 2, which is characterized in that the silver layer or aluminium layer with a thickness of
200nm。
4. reinforcing heat radiation composite structure according to claim 1, which is characterized in that the bore dia of the array through-hole is
100 μm~300 μm, Kong Zhongxin is away between 0.4mm~0.8mm.
5. reinforcing heat radiation composite structure according to claim 1, which is characterized in that the graphene film (3) uses Gao Ding
It is replaced to pyrolytic graphite.
6. a kind of preparation method according to claim 1 for strengthening heat radiation composite structure, it is characterised in that including following step
It is rapid:
Step 1: graphene oxide solution is prepared using liquid phase removing Hummers method, and is self-assembly of oxygen in liquid-vapor interface
Graphite alkene film, then by being carbonized, being graphitized and prolong and suppress to obtain graphene film (2)；
Step 2: graphene film described in step 1 (2) is existed with direct current magnetron sputtering process is passed through after oxygen plasma treatment again
The metal layer (3) are deposited thereon；
Step 3: using the method for laser ablation on the film that step 2 is formed by graphene film (2) and metal layer (3) shape
At array through-hole, metal covering is towards laser ablation direction；
Step 4: preparation polyimide acid (PAA)；
Step 5: the polyimide acid of step 4 preparation is coated in step 3 and is formed by the film with array through-hole；
Step 6: the film coated with polyimide acid prepared by step 5 is filtered, polyimide acid is enable to penetrate into
Array through-hole side wall；
Step 7: the step 6 film obtained for being covered with polyimide acid is placed in atmosphere furnace, to gather through ladder-elevating temperature
Acid imide acid completes imidization to obtain reinforcing heat radiation composite structure.
7. according to the method described in claim 6, it is characterized in that, the step 1 specifically includes: taking the natural squama of 3g325 purpose
Piece graphite and 1.5g sodium nitrate are uniformly mixed in the water-bath of 0 DEG C of temperature with the 120ml concentrated sulfuric acid, and 15g permanganic acid is added in batches
Potassium obtains mixed liquor, and mixed liquor is continued to stir 90min in 0 DEG C of temperature water bath, mixed liquor is then transferred to 35 DEG C of perseverance
In tepidarium, and it is thoroughly mixed liquid using mechanical agitator, is slowly added 120ml deionized water in the backward mixed liquor of 4h
It is diluted, and the temperature of mixed liquor is made to be no more than 100 DEG C, after addition, the water-bath by obtained solution at 95 DEG C relays
Continuous stirring 15min, obtains graphite oxide solution, is aoxidized after 10wt% dilute hydrochloric acid twice and the washing of multiple deionized water
Graphene solution takes the graphene oxide solution 50ml that concentration is 7mg/ml to be slowly inverted in the polytetrafluoro that bottom surface is 5cm × 5cm
It is dry in the vacuum oven for being set as 35 DEG C in ethylene mold, it is self-assembly of graphene oxide membrane in liquid-gas interface,
Prolong using 1000 DEG C of carbonizations, 2800 DEG C of graphitizations and machinery and presses through journey the graphene film (2) are made.
8. the method according to the description of claim 7 is characterized in that the step 4 specifically includes: 0.72 gram 4 is weighed respectively,
4'- diaminodiphenyl ether (ODA) and 1 gram of pyromellitic dianhydride (PMDA), are dissolved in 14 grams of N, N- dimethyl according to sequencing
Mixed solution is obtained in acetamide (DMAc) solution, and mixed solution is placed in 0 DEG C of water bath with thermostatic control and persistently stirs 1h, is finally obtained
It obtains polyimide acid (PAA).
9. according to the method described in claim 8, it is characterized in that, the step 7 specifically includes: poly- by being covered in step 6
The graphene film of acid imide acid is horizontally placed in atmosphere furnace, passes to the argon gas of 500ml/min as protection gas, with 0.5 DEG C/min
Heating rate heating, and respectively in 80 DEG C, 110 DEG C, 140 DEG C, 170 DEG C, 200 DEG C and 220 DEG C heat preservation 30min and 250
DEG C heat preservation 60min complete imidization, finally obtain reinforcing heat radiation composite structure.
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