CN110343897A - A kind of preparation method and applications of crystalline flake graphite reinforced aluminum matrix composites - Google Patents
A kind of preparation method and applications of crystalline flake graphite reinforced aluminum matrix composites Download PDFInfo
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Abstract
The present invention relates to aluminum matrix composite technical field more particularly to a kind of preparation method and applications of crystalline flake graphite reinforced aluminum matrix composites.Include the following steps: that 1) crystalline flake graphite after cleaning is placed in mold and vibrate, align graphite, then aluminum material is placed on graphite, obtains the mold for being filled with graphite flake and aluminum material;2) mold for finally obtaining step 1) is placed in the device for being capable of providing Pressure Infiltration technology, then carries out heating and thermal insulation to mold under vacuum conditions;3) inert gas being injected in reaction environment to be pressurized, and continuing heat-insulation pressure keeping, molten aluminum immerses the gap in mold between crystalline flake graphite under the action of high pressure gas, i.e., is handled with infiltration;4) mold releasability is taken out after being cooled to room temperature, and both obtains crystalline flake graphite/aluminium composite material.The present invention prepares crystalline flake graphite reinforced aluminum matrix composites using gas pressure infiltration technology, while strict control interfacial reaction, obtains the composite material with high heat conductance.
Description
Technical field
The present invention relates to aluminum matrix composite technical field more particularly to a kind of crystalline flake graphite reinforced aluminum matrix composites
Preparation method and applications.
Background technique
It is only intended to increase understanding of the overall background of the invention for information disclosed in background of invention, without
It is existing well known to persons skilled in the art so to be considered as recognizing or imply that information composition has become in any form
Technology.
Electronics and information industry is the pillar industry of current world economy development, and development is swift and violent.It is small-sized with electronic device
Change and integrated process is constantly aggravated, increases the power of electronic device and unit area calorific value suddenly, lead to electronic device high temperature
The probability of failure improves, and the safety and efficient operation for making electronic device are by serious influence.So heat dissipation problem restricts electricity
The development of sub- device.In order to solve this problem, it is badly in need of the Electronic Packaging heat sink material of exploitation a new generation.First generation Electronic Packaging
The thermal conductivity 11-17W/mK of material Invar, Kovar, the thermal conductivity of the second generation electronic package material W-Cu, Cu-Mo and Al-Si
Less than 200W/mK, the thermal conductivity of third generation electronic package material SiCp/Al is less than 300W/mK, is not able to satisfy electronic device
Radiating requirements.Diamond/aluminum based composites thermal conductivity (350-670W/mK) is high, becomes high thermal conductivity, low bulk aluminium base heat management
Material.However, since diamond high rigidity, high price limit the extensive use of diamond/aluminum composite material.Graphite crystal
Thermal conductivity (~2000W/mK) along base plane is high, and alpha axial direction has nearly zero thermal expansion coefficient, and graphite flake and aluminium are prepared into
Graphite flake/aluminium composite material not only has high thermal conductivity, low expansion, also has excellent machinability, becomes new
Research hotspot.
In crystalline flake graphite reinforced aluminum matrix composites, interfacial reaction generates interfacial carbide between Al matrix and crystalline flake graphite
Object Al4C3, interface cohesion can be improved to obtain high thermal conductivity.The interface of interfacial reaction degree direct influence composite material
Structure and interface cohesion, good interface cohesion can reduce two-phase interface in composite material and be detached from introduced interface resistance,
Guarantee the effective transmitting of load between the two phases simultaneously.Therefore, Al and graphite flake interface cohesion are Al and graphite flake composite material
Field urgent problem to be solved.Currently, mainly using the preparation of the solid phase methods such as vacuum heating-press sintering and discharge plasma sintering
The aluminum matrix composite consistency of crystalline flake graphite enhancing is not high, and the excellent properties of crystalline flake graphite is made to fail to give full play to;Using crowded
Though the composite material of the liquid phase methods preparation such as pressure infiltration is fine and close high, thermal conductivity is not ideal enough.
Summary of the invention
In view of the above-mentioned problems, the present invention is intended to provide a kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites and its
Using.The present invention proposes to prepare crystalline flake graphite reinforced aluminum matrix composites using gas pressure infiltration technology, anti-at strict control interface
While answering, the composite material with higher heat-conductivity is obtained.
An object of the present disclosure: a kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites is provided.
Second purpose of the invention: the application of the preparation method of the crystalline flake graphite reinforced aluminum matrix composites is provided.
For achieving the above object, the invention discloses following technical proposals:
Firstly, the present invention discloses a kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites, include the following steps:
(1) crystalline flake graphite after cleaning is placed in mold and is vibrated, align graphite, aluminum material is then placed in stone
Mo Shang obtains the mold for being filled with graphite flake and aluminum material;
(2) mold that step (1) finally obtains is placed in the device for being capable of providing Pressure Infiltration technology, then in vacuum
Under the conditions of to mold carry out heating and thermal insulation;
(3) inert gas is injected in reaction environment to be pressurized, and continue heat-insulation pressure keeping, work of the molten aluminum in high pressure gas
With the gap in lower immersion mold between crystalline flake graphite, i.e., handled with infiltration;
(4) it is cooled to room temperature to reaction environment, takes out mold releasability, both obtain crystalline flake graphite/aluminium composite material.
As further technical solution, in step (1), the method for the cleaning crystalline flake graphite are as follows: put crystalline flake graphite
Enter dilute H2SO4Stirring and washing 8-15 minutes in solution, it then is washed to neutrality with distillation, micropore filters, and is with drying box drying
It can.
As further technical solution, in step (1), the size of the crystalline flake graphite is 32-80 mesh, for example, 32 mesh,
50 mesh, 80 mesh.
As further technical solution, in step (1), the mold is columnar structured.
As further technical solution, in step (2), the heating temperature of the mold is 750-850 DEG C, soaking time
10min-1h。
As further technical solution, in step (2), the vacuum degree of the vacuum condition is 0.08-0.13MPa.
As further technical solution, in step (3), the inert gas includes argon gas etc..
As further technical solution, in step (3), the heat-insulation pressure keeping are as follows: 750-850 DEG C of temperature, time 25-
35min。
As further technical solution, in step (3), the gas pressure is 1-3MPa, during preserving temperature and reducing temperature
It does not deflate unloading pressure.
The present invention prepares the interface crystalline flake graphite/Al formation mechenism to gas pressure infiltration technology and conducts in-depth research, hair
It is existing: interfacial reaction products Al4C3It is heterogeneous nucleation, when using gas pressure infiltration technology, interface A l4C3It is distributed in small and dispersed,
It can significantly improve crystalline flake graphite/Al composite material interface to combine, promote the thermal conductivity of composite material.
Finally, the present invention discloses the preparation method of the crystalline flake graphite reinforced aluminum matrix composites in Aeronautics and Astronautics, vapour
Application in the fields such as vehicle, electronics, sophisticated and futuristic weapons system.
Compared with prior art, the present invention achieve it is following the utility model has the advantages that
(1) present invention uses gas pressure infiltration technology, and high vacuum degree effectively can inhibit metallic aluminium to be oxidized, and applies high pressure
Gas push metallic aluminium flows to mold cavity various aspects, it is made to fill up the gap between graphite flake, so that graphite flake uniformly divides
In cloth aluminum substrate, it can effectively control crystalline flake graphite and the interface of aluminium base is combined closely, improve the consistency of composite material, and mention
High heat conductance.
(2) thermal conductivity of composite material prepared by the present invention is 275-462W/mK, density≤2.51g/cm3, crystalline flake graphite
Shared volume fraction be≤75.1%, meet Aeronautics and Astronautics, automobile, electronics and sophisticated and futuristic weapons system industry to high thermal conductivity
And the demand of lightweight hot encapsulation material.
Detailed description of the invention
The Figure of description for constituting a part of the invention is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.
Fig. 1 is the SEM figure of crystalline flake graphite reinforced aluminum matrix composites prepared by the embodiment of the present invention 1, wherein (a) is edge
The observation chart in parallel crystalline flake graphite direction;(b) for along the observation chart in vertical crystalline flake graphite direction.
Fig. 2 is the XRD diagram of crystalline flake graphite reinforced aluminum matrix composites prepared by the embodiment of the present invention 1.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the present invention.Unless another
It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.Such as, used herein, unless the context clearly indicates otherwise, otherwise singular shape
Formula is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As previously mentioned, at present mainly using the squama of the solid phase methods such as vacuum heating-press sintering and discharge plasma sintering preparation
The aluminum matrix composite consistency of piece graphite enhancing is not high, and the excellent properties of crystalline flake graphite is made to fail to give full play to;Using extruding
Though the composite material of the liquid phase methods such as infiltration preparation is fine and close high, thermal conductivity is not ideal enough.Therefore, the present invention proposes to use air pressure
Impregnation technology prepares crystalline flake graphite reinforced aluminum matrix composites;Now in conjunction with the drawings and specific embodiments to the present invention further into
Row explanation.
In the following example, damp furnace is soaked as offer Pressure Infiltration using the pressure that Hunan Dingli Technologies Co., Ltd. generates
The device of technology prepares crystalline flake graphite reinforced aluminum matrix composites.
Material phase analysis is carried out to composite material using X-ray diffractometer (XRD), diffraction conditions are Cu target K α line, scanning electricity
Pressure is 40kV, and electric current 40mA, scanning speed is 4 °/min, and 0.02 ° of step-length, sweep interval is 10-90 °.
The microscopic structure of composite material is observed using HitachiS-3400 type scanning electron microscope (SEM).
Using the thermal conductivity of the resistance to laser conductometer LFA457 measurement composite material speeded, along graphite flake direction and Vertical Square
Face measures respectively.
Using the quality of assay balance measurement sample.
Using the actual density of suspension method measurement composite material, principle is to utilize Archimedes's drainage.
Using the diameter and height of vernier caliper measurement sample, the volume for calculating sample three times is measured respectively, is then calculated
The theoretical density of sample.Consistency is percentage of the actual density divided by theoretical density.
Embodiment 1
A kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites, includes the following steps:
(1) crystalline flake graphite of 32 mesh is put into 10% H2SO4Stirring and washing 10 minutes in solution, then with distillation washing
To neutrality, micropore is filtered, is dried with drying box, spare.
(2) cleaned crystalline flake graphite is fitted into cylindrical graphite jig, graphite jig is then put into electricity
Then the mold for installing crystalline flake graphite is put into the glass sock that pressure soaks damp furnace by the vibration of magnetic vibration platform, vibration frequency 40-60HZ
In cylinder, and fine aluminium block is put on crystalline flake graphite in a mold, then the entire mold installed is put into the damp furnace induction of pressure leaching and is added
Hot-zone prepares heating.
(3) vacuum system is opened, soaking damp furnace to be pumped to vacuum degree to pressure is 0.1MPa;Then start recirculated water and air draft
Fan, restarts heating system, mold is heated to 850 DEG C, and keep the temperature 10min.
(4) pressure charging system that starting pressure soaks damp furnace pours high-purity (99.99%) argon gas into furnace, until furnace pressure is
1.0MPa stops inflation, closes pressure charging system;Then under the gas pressure of 1.0MPa, continue to keep the temperature 30min at 850 DEG C, it is complete
It heats at rear stopping, not being unloaded in temperature-fall period, until furnace temperature drops to room temperature and then unloads the air pressure in furnace again, close recirculated water
And exhaust fan.Mold releasability is taken out in blow-on, and acquisition diameter is 30mm, highly compound for graphite flake/aluminium of the cylindrical shape of 25mm
Material product.
Obtaining diameter along parallel crystalline flake graphite direction and vertical crystalline flake graphite direction on the product is 12.7mm, thick
Degree is the disk of 4mm, calorimetric conductance;As the result is shown: the thermal conductivity in the direction graphite flake/aluminium composite material X-Y is 462W/
Mk, the thermal conductivity of Z-direction are 63W/mk, density 2.50g/cm3。
Graphite flake/aluminium composite material the tissue topography obtained from above-mentioned two direction is observed, as a result such as Fig. 1 (a) and (b)
It is shown, it will thus be seen that white area is Al, and black region is graphite flake, it was demonstrated that graphite flake aligns, without apparent stomata
And crackle, consistency are up to 99.1%.
The XRD spectrum of graphite flake/aluminium composite material manufactured in the present embodiment is as shown in Fig. 2, as can be seen from the figure: in addition to
There is new phase Al in Al and graphite two-phase4C3, it was demonstrated that it is reacted at interface.
Embodiment 2
A kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites, includes the following steps:
(1) crystalline flake graphite of 50 mesh is put into 10% H2SO4Then stirring and washing 8 minutes in solution are washed to distillation
Neutrality, micropore is filtered, is dried with drying box, spare.
(2) with embodiment 1.
(3) vacuum system is opened, soaking damp furnace to be pumped to vacuum degree to pressure is 0.13MPa;Then start recirculated water and row
Fan restarts heating system, mold is heated to 850 DEG C, and keep the temperature 10min.
(4) pressure charging system that starting pressure soaks damp furnace pours high-purity (99.99%) argon gas into furnace, until furnace pressure is
2.0MPa stops inflation, closes pressure charging system;Then under the gas pressure of 2.0MPa, continue to keep the temperature 25min at 850 DEG C, it is complete
It heats at rear stopping, not being unloaded in temperature-fall period, until furnace temperature drops to room temperature and then unloads the air pressure in furnace again, close recirculated water
And exhaust fan.Mold releasability is taken out in blow-on, and acquisition diameter is 30mm, highly compound for graphite flake/aluminium of the cylindrical shape of 25mm
Material product.
Obtaining diameter along parallel crystalline flake graphite direction and vertical crystalline flake graphite direction on the product is 12.7mm, thick
Degree is the disk of 4mm, calorimetric conductance;As the result is shown: the thermal conductivity in the direction graphite flake/aluminium composite material X-Y is 405W/
Mk, the thermal conductivity of Z-direction are 52W/mk, density 2.37g/cm3。
Embodiment 3
A kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites, includes the following steps:
(1) crystalline flake graphite of 80 mesh is put into 10% H2SO4Stirring and washing 15 minutes in solution, then with distillation washing
To neutrality, micropore is filtered, is dried with drying box, spare.
(2) with embodiment 1.
(3) vacuum system is opened, soaking damp furnace to be pumped to vacuum degree to pressure is 0.08MPa;Then start recirculated water and row
Fan restarts heating system, mold is heated to 800 DEG C, and keep the temperature 60min.
(4) pressure charging system that starting pressure soaks damp furnace pours high-purity (99.99%) argon gas into furnace, until furnace pressure is
1.0MPa stops inflation, closes pressure charging system;Then under the gas pressure of 1.0MPa, continue to keep the temperature 30min at 800 DEG C, it is complete
It heats at rear stopping, not being unloaded in temperature-fall period, until furnace temperature drops to room temperature and then unloads the air pressure in furnace again, close recirculated water
And exhaust fan.Mold releasability is taken out in blow-on, and acquisition diameter is 30mm, highly compound for graphite flake/aluminium of the cylindrical shape of 25mm
Material product.
Obtaining diameter along parallel crystalline flake graphite direction and vertical crystalline flake graphite direction on the product is 12.7mm, thick
Degree is the disk of 4mm, calorimetric conductance;As the result is shown: the thermal conductivity in the direction graphite flake/aluminium composite material X-Y is 389W/
Mk, the thermal conductivity of Z-direction are 27W/mk, density 2.31g/cm3。
Embodiment 4
A kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites, includes the following steps:
(1) crystalline flake graphite of 32 mesh is put into 10% H2SO4Stirring and washing 10 minutes in solution, then with distillation washing
To neutrality, micropore is filtered, is dried with drying box, spare.
(2) with embodiment 1.
(3) vacuum system is opened, soaking damp furnace to be pumped to vacuum degree to pressure is 0.08MPa;Then start recirculated water and row
Fan restarts heating system, mold is heated to 750 DEG C, and keep the temperature 50min.
(4) pressure charging system that starting pressure soaks damp furnace pours high-purity (99.99%) argon gas into furnace, until furnace pressure is
3.0MPa stops inflation, closes pressure charging system;Then under the gas pressure of 3.0MPa, continue to keep the temperature 35min at 750 DEG C, it is complete
It heats at rear stopping, not being unloaded in temperature-fall period, until furnace temperature drops to room temperature and then unloads the air pressure in furnace again, close recirculated water
And exhaust fan.Mold releasability is taken out in blow-on, and acquisition diameter is 30mm, highly compound for graphite flake/aluminium of the cylindrical shape of 25mm
Material product.
Obtaining diameter along parallel crystalline flake graphite direction and vertical crystalline flake graphite direction on the product is 12.7mm, thick
Degree is the disk of 4mm, calorimetric conductance;As the result is shown: the thermal conductivity in the direction graphite flake/aluminium composite material X-Y is 401W/
Mk, the thermal conductivity of Z-direction are 54W/mk, density 2.42g/cm3。
Embodiment 5
A kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites, includes the following steps:
(1) crystalline flake graphite of 32 mesh is put into 10% H2SO4Stirring and washing 10 minutes in solution, then with distillation washing
To neutrality, micropore is filtered, is dried with drying box, spare.
(2) with embodiment 1.
(3) vacuum system is opened, soaking damp furnace to be pumped to vacuum degree to pressure is 0.08MPa;Then start recirculated water and row
Fan restarts heating system, mold is heated to 850 DEG C, and keep the temperature 30min.
(4) pressure charging system that starting pressure soaks damp furnace pours high-purity (99.99%) argon gas into furnace, until furnace pressure is
1.0MPa stops inflation, closes pressure charging system;Then under the gas pressure of 1.0MPa, continue to keep the temperature 25min at 850 DEG C, it is complete
It heats at rear stopping, not being unloaded in temperature-fall period, until furnace temperature drops to room temperature and then unloads the air pressure in furnace again, close recirculated water
And exhaust fan.Mold releasability is taken out in blow-on, and acquisition diameter is 30mm, highly compound for graphite flake/aluminium of the cylindrical shape of 25mm
Material product.
Obtaining diameter along parallel crystalline flake graphite direction and vertical crystalline flake graphite direction on the product is 12.7mm, thick
Degree is the disk of 4mm, calorimetric conductance;As the result is shown: the thermal conductivity in the direction graphite flake/aluminium composite material X-Y is 402W/
Mk, the thermal conductivity of Z-direction are 41W/mk, density 2.44g/cm3。
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of crystalline flake graphite reinforced aluminum matrix composites, which comprises the steps of:
(1) crystalline flake graphite after cleaning is placed in mold and is vibrated, align graphite, aluminum material is then placed in graphite
On, obtain the mold for being filled with graphite flake and aluminum material;
(2) mold that step (1) finally obtains is placed in the device for being capable of providing Pressure Infiltration technology, then in vacuum condition
Under to mold carry out heating and thermal insulation;
(3) inert gas being injected in reaction environment to be pressurized, and continuing heat-insulation pressure keeping, molten aluminum is under the action of high pressure gas
The gap in mold between crystalline flake graphite is immersed, i.e., is handled with infiltration;
(4) it is cooled to room temperature to reaction environment, takes out mold releasability, both obtain crystalline flake graphite/aluminium composite material.
2. the preparation method of crystalline flake graphite reinforced aluminum matrix composites as described in claim 1, which is characterized in that step (2)
In, the heating temperature of the mold is 750-850 DEG C, soaking time 10min-1h.
3. the preparation method of crystalline flake graphite reinforced aluminum matrix composites as described in claim 1, which is characterized in that step (2)
In, the vacuum degree of the vacuum condition is 0.08-0.13MPa.
4. the preparation method of crystalline flake graphite reinforced aluminum matrix composites as described in claim 1, which is characterized in that step (3)
In, the inert gas is argon gas.
5. the preparation method of crystalline flake graphite reinforced aluminum matrix composites as described in claim 1, which is characterized in that step (3)
In, the heat-insulation pressure keeping are as follows: 750-850 DEG C of temperature, time 25-35min.
6. the preparation method of crystalline flake graphite reinforced aluminum matrix composites as described in claim 1, which is characterized in that step (3)
In, the gas pressure is 1-3MPa, unloading pressure of not deflating during preserving temperature and reducing temperature.
7. the preparation method of crystalline flake graphite reinforced aluminum matrix composites as described in any one in claim 1-5, which is characterized in that
In step (1), the method for the cleaning crystalline flake graphite are as follows: crystalline flake graphite is put into dilute H2SO4Stirring and washing 8-15 points in solution
Clock, is then washed to neutrality with distillation, and micropore is filtered, dried with drying box.
8. the preparation method of crystalline flake graphite reinforced aluminum matrix composites as described in any one in claim 1-5, which is characterized in that
In step (1), the size of the crystalline flake graphite is 32-80 mesh.
9. the preparation method of crystalline flake graphite reinforced aluminum matrix composites as described in any one in claim 1-5, which is characterized in that
In step (1), the mold is columnar structured.
10. such as the preparation method of the described in any item crystalline flake graphite reinforced aluminum matrix composites of claim 1-9, feature exists
In application in Aeronautics and Astronautics, automobile, electronics, sophisticated and futuristic weapons system.
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CN111235420A (en) * | 2020-01-16 | 2020-06-05 | 西北工业大学 | Method for improving interlayer arrangement uniformity of flake graphite aluminum-based composite material by adding copper-plated aluminum sheet |
CN114619013A (en) * | 2022-02-28 | 2022-06-14 | 江南大学 | Method for preparing high-performance aluminum-based flake graphite composite material |
CN115354296A (en) * | 2022-08-24 | 2022-11-18 | 哈尔滨工业大学 | Method for improving thermal conductivity of graphite film aluminum composite material |
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