CN108085524B - A kind of preparation method of graphene reinforced aluminum matrix composites - Google Patents
A kind of preparation method of graphene reinforced aluminum matrix composites Download PDFInfo
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- CN108085524B CN108085524B CN201611039871.XA CN201611039871A CN108085524B CN 108085524 B CN108085524 B CN 108085524B CN 201611039871 A CN201611039871 A CN 201611039871A CN 108085524 B CN108085524 B CN 108085524B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
Abstract
The present invention proposes a kind of preparation method of graphene reinforced aluminum matrix composites, by two step ball-milling methods prepare graphene/aluminum mixed powder, cold moudling graphene/aluminum composite material material base, hot extrusion molding and etc. graphene/aluminum composite material is prepared.The present invention uses special technology mode, realizes graphene and is uniformly dispersed in aluminium base, reduces generation brittlement phase Al4C3, finally obtained the graphene/aluminum composite material of high-compactness, high volume parts.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene reinforced aluminum matrix composites, belong to metal-base composites technology
Field.
Background technique
Graphene is considered as metal-based compound as a kind of flexible two-dimensional material with desirable physical and mechanical property
The ideal reinforcement of material.Its thermal conductivity is up to about 5000W/mK, and elasticity modulus is about 1100GPa, and tensile strength is up to about
125GPa.For traditional reinforcement such as SiCp, SiCw and carbon fiber and carbon nanotube, graphene is as Metal Substrate
The reinforcement of composite material will improve the physical and mechanical properties of material to a greater extent.It is relatively early with starting and significant to obtain
Graphene/the polymer and graphene/ceramic composite of progress are compared, graphene reinforced metal-matrix composite
Relevant report is less.Currently, graphene reinforced metal-matrix composite focuses primarily upon in the metal materials such as aluminium, copper, magnesium, to
Obtain lightweight, it is high-strength, with good conductive, thermally conductive, antiwear characteristic composite material.However, being limited to graphene itself
Physical characteristic, there are a series of technical problems for the preparation of graphene reinforced metal-matrix composite.On the one hand, single layer or few layer
Graphene is inclined to very strong reunion, is not easy to prepare the composite material of high-volume fractional, and it is not easy during the preparation process
In being uniformly dispersed in aluminum substrate；On the other hand, conventional preparation techniques often make material undergo pyroprocess, and C/Al is easily sent out at interface
Raw reaction generates brittlement phase Al4C3Phase can significantly affect the comprehensive mechanical property of composite material.
Patent " a method of prepare graphene reinforced aluminum matrix composites " (application number 201510547587.2) record
The method for preparing graphene reinforced aluminum matrix composites, it is first modified to graphene and aluminium powder surface respectively, make graphene surface
It is negatively charged, aluminium powder surface is positively charged；Then by graphene and the aluminium powder system by way of electrostatic self-assembled in the solution
Standby mixed-powder；The densification of composite material is realized finally by hot pressed sintering." graphene enhances magnesium, aluminum-base composite material to patent
Material and preparation method thereof " (application number: 201610166347.2), proposition is stirred in ethanol solution by means of ultrasonic disperse and machinery
It mixes realization graphene/metallic particles and is mixed with mixed powder；Composite material is realized by hot pressed sintering and hot extrusion technique
Densification.Patent " a method of pass through graphene enhance metal material " (application number: 201410136468.3) and patent
" a kind of armour plate and preparation method thereof with reinforced phase gradient layer " (application number: 201510250004.X) is then by molten in alcohol
Ball milling is carried out to powder in liquid and prepares composite granule, is solubilization liquid since graphene is easy to reunite, in conventional means first by its point
It dissipates, mixes it with other powders by electrostatic interaction；The densification process of composite material passes through vacuum canning, heat etc.
Static pressure and hot extrusion technique are realized.
Above-mentioned several preparation methods are the mainstream preparation method of current graphene reinforced aluminum matrix composites, but there are still one
A little problems.Firstly, the densification of composite material is realized in first two preparation method by hot pressed sintering, in hot pressed sintering process
Middle C/Al interfacial reaction is inevitable；The mixed of graphene and metallic particles is realized in the solution secondly, being all made of in the above method
It closes, complex process, it is difficult to obtain the powder for the high-volume fractional graphene content being evenly distributed, and firm graphite cannot be obtained
Alkene/aluminium powder combines；Finally, latter two method, which is all made of vacuum canning, hot isostatic pressing and hot extrusion technique, realizes composite material
Densification, the technical process are cumbersome and expensive；In addition, hot isostatic pressing and extrusion temperature have been up to 480~500 DEG C, prolong significantly
The residence time of material at high temperature has been grown, C and Al reaction has been improved and generates brittlement phase Al4C3A possibility that, it is unfavorable for material power
Learn the raising of performance.
Summary of the invention
It is an object of the invention to overcome the shortage of prior art, provides a kind of graphene and be uniformly dispersed, subtract in aluminium base
Brittlement phase Al is generated less4C3Graphene reinforced aluminum matrix composites preparation method.
Technical solution of the invention: a kind of preparation method of graphene reinforced aluminum matrix composites passes through following step
It is rapid to realize:
The first step prepares graphene/aluminum mixed powder,
Graphene powder and aluminium powder ball milling mixing is uniform, and ball-milling technology is divided into two steps, first mixes 10 at 120~180rpm
~12h, then 10~12h is mixed at 200~300rpm；
The present invention is used in the incipient stage using first slow rear two fast step ball-milling methods and is mixed powder (120~180rpm) at a slow speed,
While guaranteeing graphene-structured integrality, makes its uniform adhesion to aluminium powder surface, effectively prevent the reunion of graphene；Then
Powder (200~300rpm) is mixed using high speed again, deforms flake aluminum further, graphene sheet layer is made to be embedded in aluminium powder surface, from
And it realizes firm graphene/aluminum powder and combines.
The present invention gives the selection process of two step ball-milling methods, realize the dry state mixing of graphene, obtain high volume point
Number mixed powder, two step ball millings change in above-mentioned requirements technique, do not have to performances such as the consistency of graphene/aluminum composite material
It significantly affects, can be neglected in engineering.
The present invention realizes the integrality and uniformly that dry state mixes the graphene of powder by preferred two steps ball-milling method technique
Property, and firm graphene/aluminum powder combination.
The aluminium powder that the present invention uses can be able to be object for pure aluminium powder or 1XXX system~8XXX line aluminium alloy powder, graphene
Logos or the graphene film or graphene oxide sheet of chemical method preparation；Aluminium powder and graphene are commercial products, art technology
Personnel choose suitable raw material according to practical.
Further, every 1~1.5h of ball milling stops 15~30min in two step ball millings.
Further, volume fraction of the Graphene powder in graphene/aluminum mixed powder can reach 5vol.% in this step,
And in the prior art, volume fraction of the Graphene powder in graphene/aluminum mixed powder is generally 2~3vol.%.
The first step is mixed the graphene/aluminum mixed powder of powder preparation, through cold moudling system by second step by two step ball-milling methods
Standby graphene/aluminum composite material material base；
The present invention prepares graphene/aluminum composite material material base using cold moudling, avoids material base C/Al circle at high temperature
Face, which reacts, generates brittlement phase Al4C3Phase.
Graphene and aluminium in material base are combined using vacuum canning, hot isostatic pressing in the prior art, realizes that graphene/aluminum is multiple
The densification of condensation material, then graphene being uniformly distributed in aluminium in graphene/aluminum composite material is realized by hot extrusion.This hair
Bright middle first cold moudling blank, by the subsequent adjustment to hot extrusion technique, realize graphene/aluminum composite material densification and
Graphene being uniformly distributed in aluminium.
Further, 150~300MPa of pressure of graphene/aluminum mixed powder cold moudling, the dwell time is in 10~20min
Between.This step only requires the green body for being pressed into graphene/aluminum mixed powder and being easy to subsequent step, surface flawless,
Cold pressing forming process can be arranged according to needs of production in those skilled in the art.
Third step, the graphene/aluminum composite material material base that second step obtains carry out hot extrusion and obtain graphene enhancing aluminium base
Composite material, the hot extrusion technique are as follows: 420~460 DEG C of temperature, extruding rate≤6mm/s, extrusion ratio is 10:1~40:
1。
The present invention is by setting special hot extrusion technique (temperature is low, extrusion speed is slow, preferred extrusion ratio), preferably
Temperature makes alumina particles have higher intensity, bigger in the shearing force in hot extrusion process between particle, more conducively graphene
Graphene that is shear-deformable and then obtaining more evenly is distributed；Under the conditions of preferred extrusion speed and extrusion ratio, guarantee material in height
There is the longer residence time under warm high shear deformation, realizes the densification of material.
Hot extrusion technique of the present invention gives preferred range, and those skilled in the art are compound according to required graphene/aluminum
The volume fraction of graphene determines concrete technology in preferred range in material.
The present invention compared with prior art the utility model has the advantages that
(1) present invention uses special technology mode (two step ball millings+cold pressing+special hot extrusion), realizes graphene and exists
It is uniformly dispersed in aluminium base, reduces generation brittlement phase Al4C3, it is multiple to have finally obtained high-compactness, the graphene/aluminum of high volume parts
Condensation material；
(2) present invention uses special ball milling mixing technique, in the case where avoiding graphene from reuniting, is prepared for high volume
Score graphene/aluminum mixed powder；
(3) present invention is limited by cold moudling and hot extrusion technique, and graphene/aluminum composite material is made to have high-compactness
While, effectively avoid the interfacial reaction of graphene and aluminum substrate generation；
(4) the special hot extrusion technique of the present invention is realizing the densification of graphene/aluminum composite material simultaneously, is making graphene
It is uniformly distributed in alloy matrix aluminum, solves C/Al interfacial reaction, the distribution of graphene, densifying materials and powder injection molding etc.
Problem；
(5) it present invention can be suitably applied to all kinds of using graphene as graphene/metal matrix composite materials of reinforced phase.
Detailed description of the invention
Fig. 1 is that graphene volume fraction is respectively 1vol.% (Fig. 1 a) and 5vol.% (Fig. 1 b) in the embodiment of the present invention
FLG/Al composite material powder SEM pattern；
Fig. 2 is that graphene volume fraction is respectively 1vol.% (Fig. 1 a) and 5vol.% (Fig. 1 b) in the embodiment of the present invention
The XRD result of FLG/Al composite material powder；
Fig. 3 is that graphene volume fraction is respectively 1vol.%FLG/6061Al composite material powder in the embodiment of the present invention
SEM pattern (partial enlarged view that Fig. 1 b is Fig. 1 a)；
Fig. 4 is that graphene volume fraction is respectively 1vol.%FLG/6061Al composite material powder in the embodiment of the present invention
XRD result；
Fig. 5 is that graphene volume fraction is respectively 0vol.% (fine aluminium), 1vol.% and 5vol.% in the embodiment of the present invention
The FLG/Al composite material consistency situation of change under different conditions during the preparation process；
Fig. 6 is that graphene volume fraction is respectively 1vol.%, 2vol.% and 5vol.%FLG/ in the embodiment of the present invention
The 6061Al composite material consistency situation of change under different conditions during the preparation process；
Fig. 7 is that powder is cold-pressed schematic diagram in the embodiment of the present invention；
Fig. 8 is flow chart of the present invention.
Specific embodiment
Below with reference to specific example and attached drawing, the present invention is described in detail.
Embodiment 1
The FLG/Al composite material that graphene volume parts are 1vol.% is prepared, specific steps are as shown in Figure 8:
1, graphene/aluminum mixed powder
It is that 1vol.% weighs aluminium powder and graphene powder according to graphene volume parts, is put into stainless steel jar mill；It presses
1~1.5g stearic acid is added according to every 100g mixed powder；According to ratio of grinding media to material 5:1~10:1, according to the gross mass scale of mixed powder
Abrading-ball is taken, is put into ball grinder；Guarantee between fill factor 0.5~0.7.Ball grinder completes dress in the glove box of argon atmosphere
Powder.The aluminium powder used in this step can be pure aluminium powder or 1XXX system~8XXX line aluminium alloy powder；The graphene used can be with
For graphene film or graphene oxide sheet prepared by physical method or chemical method, thickness can be between 1~20nm, and piece diameter is 10
Between~200 μm.The abrading-ball that ball milling uses can be stainless steel, tool steel, chromium steel, quenched and tempered steel, bearing steel, hard alloy steel
Matter or ceramic material.
Using planetary ball mill, with 10~12h of revolving speed 120~150rpm ball milling, every 1~1.5h of ball milling stops 15~
30min；With 10~12h of revolving speed 200~240RPM ball milling, every 1~1.5h of ball milling stops 15~30min.After the completion of ball milling, having
Powder is taken in the glove box of argon atmosphere.
2, cold moudling
Composite granule is put into mold shown in Fig. 7, push-down head is put into, applies pressure, prepares composite material material base.
In cold pressure procedure, guarantee pressure 250Mpa suffered by powder, the dwell time is in 20min, the composite material material base flawless of preparation.It is cold
Compression mould size is determined according to practical powder quality and use demand.
3, hot extrusion
Extrusion equipment prepares:
Graphite is uniformly mixed with lubricating oil, sleeve interior surface is being squeezed using the method for injection or coating and is squeezing prod cast
Inner surface uniform fold graphite lubricating oil (GLO).Material base is put into and is squeezed in sleeve, graphite pads are placed above.
Blank is preheated in resistance furnace together with extrusion die, preheating temperature is 420~440 DEG C, and the rate of heat addition is 5~10
DEG C/min, soaking time 1~3 hour.
Preheated blank is squeezed, extrusion ratio is between 30:1, extruding rate 5mm/s.
The graphene/aluminum mixed powder that the present embodiment obtains is as shown in Figure 1, by two step ball-milling methods, and graphene film is
It has fully embedded into inside aluminium powder, on its surface not it is observed that apparent graphene film；As shown in Fig. 2, existing in mixed powder
Graphene characteristic peak shows that graphene film is successfully mixed into aluminium powder.
Embodiment 2
The FLG/Al composite material for using above-mentioned technique to prepare graphene volume parts as 5vol.%, the present embodiment obtain
Graphene/aluminum mixed powder it is as shown in Figure 1, 2.
As Fig. 5 shows fine aluminium and graphene volume fraction is respectively 1vol.% (embodiment 1) and 5vol.% (embodiment
2) the FLG/Al composite material consistency situation of change under different conditions during the preparation process, as can be seen from the figure composite granule
The consistency of state is about 45%, its consistency can be of about 90 or more % after being cold-pressed, the densification of composite material after hot extrusion
Degree reaches 99% or more.
Embodiment 3,4,5
1, graphene/6061 aluminium mixed powders
It is respectively that 1vol.%, 2vol.%, 5vol.% weigh 6061 Al alloy powders and graphite according to graphene volume parts
Alkene powder, is put into stainless steel jar mill；Remaining ball milling is arranged with embodiment 1.
Using planetary ball mill, with 10~12h of revolving speed 120~180rpm ball milling, every 1~1.5h of ball milling stops 15~
30min；With 10~12h of revolving speed 240~300RPM ball milling, every 1~1.5h of ball milling stops 15~30min.After the completion of ball milling, having
Powder is taken in the glove box of argon atmosphere.
2, in pressure 250Mpa, dwell time in 20min, the FLG/6061Al composite material material of cold moudling flawless
Base.
3, hot extrusion
Preheating temperature is 440~460 DEG C, and the rate of heat addition is 5~10 DEG C/min, soaking time 1~3 hour.It will be preheated
Blank squeezed, extrusion ratio is respectively between 10:1,20:1 and 40:1, extruding rate be respectively 6mm/s, 5mm/s and
3mm/s.Remaining hot extrusion is arranged with embodiment 1.
The graphene that embodiment 3 obtains/6061Al mixed powder is as shown in figure 3,6061Al powder becomes under the shock of abrading-ball
For platelike disc, graphene film size becomes smaller, and is adhered to 6061Al powder surface；As shown in figure 4, being deposited in composite material powder
In graphene characteristic peak, show that graphene film has been added in composite granule.
It is respectively 1vol.%, 2vol.% and 5vol.%FLG/6061Al composite wood that Fig. 6, which show graphene volume fraction,
Expect that the consistency situation of change under different conditions during the preparation process, diagram show the consistency of composite granule state only about
50%, its consistency can be of about 80~90% after being cold-pressed, and the consistency of composite material reaches 99% or more after hot extrusion.
Unspecified part of the present invention is known to the skilled person technology.
Claims (3)
1. a kind of preparation method of graphene reinforced aluminum matrix composites, which is characterized in that realized by following steps:
The first step prepares graphene/aluminum mixed powder,
Graphene powder and aluminium powder ball milling mixing is uniform, and ball-milling technology is divided into two steps, first at 120~180rpm mixing 10~
12h, then 10~12h is mixed at 200~300rpm；
The application is using first slow rear two fast step ball-milling methods, in the incipient stage using powder i.e. 120~180rpm is mixed at a slow speed, then again
Powder i.e. 200~300rpm is mixed using high speed；
The first step is mixed the graphene/aluminum mixed powder of powder preparation by two step ball-milling methods, prepares stone through cold moudling by second step
Black alkene/aluminium composite material material base；
Third step, the graphene/aluminum composite material material base that second step obtains carry out hot extrusion and obtain graphene enhancing aluminum-base composite
Material, hot extrusion technique are as follows: 420~460 DEG C of temperature, extruding rate≤6mm/s, extrusion ratio is 10:1~40:1.
2. a kind of preparation method of graphene reinforced aluminum matrix composites according to claim 1, it is characterised in that: described
In the first step, every 1~1.5h of ball milling stops 15~30min in two step ball millings.
3. a kind of preparation method of graphene reinforced aluminum matrix composites according to claim 1, it is characterised in that: described
150~300MPa of pressure of graphene/aluminum mixed powder cold moudling in second step, the dwell time is between 10~20min.
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Cited By (1)
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| RU2781403C1 (en) * | 2021-12-02 | 2022-10-11 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский политехнический университет Петра Великого" (ФГАОУ ВО "СПбПУ") | Method for producing aluminum-graphene composite material with improved plasticity |
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| CN112846198B (en) * | 2021-01-05 | 2022-11-22 | 中冶赛迪工程技术股份有限公司 | Nanoparticle reinforced metal matrix composite material and preparation method thereof |
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