CN108950281A - A kind of polyethylene glycol repairs the preparation method of graphene reinforced aluminum matrix composites - Google Patents

A kind of polyethylene glycol repairs the preparation method of graphene reinforced aluminum matrix composites Download PDF

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CN108950281A
CN108950281A CN201810961859.7A CN201810961859A CN108950281A CN 108950281 A CN108950281 A CN 108950281A CN 201810961859 A CN201810961859 A CN 201810961859A CN 108950281 A CN108950281 A CN 108950281A
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graphene
polyethylene glycol
alloy
mass fraction
aluminum
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CN108950281B (en
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鞠渤宇
武高辉
杨文澍
姜龙涛
张强
陈国钦
康鹏超
修子扬
乔菁
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Harbin Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • C22C1/0416Aluminium-based alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-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
    • C22C32/0084Non-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

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  • Powder Metallurgy (AREA)
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Abstract

A kind of polyethylene glycol repairs the preparation method of graphene reinforced aluminum matrix composites, is related to a kind of preparation method of graphene reinforced aluminum matrix composites.Purpose is to solve the problems, such as that grinding aid generates residual in alloy matrix aluminum, and realize graphene selfreparing.Preparation: weighing graphene, polyethylene glycol and aluminum metal powder, be fitted into ball milling in ball grinder, is cold-pressed, and the preparation of composite material is carried out after cold pressing.The thermal decomposition of grinding aid polyethylene glycol generates activity C atom, being adsorbed on graphene fault location promotes graphene-structured integrality significantly, and form good interface connection, material overall performance is set to have a distinct increment, and it is in blocks that polyethylene glycol is conducive to aluminum metal powder, it solves the problems, such as single layer or the big cold welding between reduction aluminum metal powder of few dispersion difficulty of the layer graphene in aluminum matrix composite, easily removes, the excellent combination property of few layer of graphene reinforced aluminum matrix composites of preparation.The present invention is suitable for preparing graphene reinforced aluminum matrix composites.

Description

A kind of polyethylene glycol repairs the preparation method of graphene reinforced aluminum matrix composites
Technical field:
The present invention relates to a kind of preparation methods of graphene reinforced aluminum matrix composites.
Background technique:
Graphene has tensile strength, the elasticity modulus of 1TPa and the thermal conductivity of 5000W/ (mK) of up to 125GPa, Undoubtedly a kind of comprehensive performance is superior, near ideal reinforcement.Graphene can be divided into single-layer graphene, bilayer according to the number of plies Graphene, few layer graphene (3~10 layers) and multi-layer graphene (number of plies is greater than 10 layers, and overall thickness is less than 10nm).It uses at present Graphene is the most active come the research for improving the performance of resin and ceramics, and graphene is utilized to enhance Metal Substrate, especially enhances The research of aluminum matrix composite is relatively fewer.The process of preparation is mainly solid phase method and liquid phase method, and solid phase method includes various Powder metallurgy process, agitating friction weldering and newest discharge plasma sintering (SPS) method etc., liquid phase method includes pressure infiltration method Deng.
Graphene reinforced aluminum matrix composites have wide practical use, and calculate its theory using shear lag model and stretch Intensity is up to 1.5GPa, but finds its high-performance only in addition minute quantity graphene (0.5~1wt.% of <) in practical study When have part embodiment, its actual strength declines rapidly during the addition of high-content graphene, and much deviation theory calculates strong Degree.This is because aluminium powder pattern common in research is ball-type at present, ball-type aluminium powder specific surface area itself is lower, adsorption stone Black alkene content is few, is difficult to prepare the graphene reinforced aluminum matrix composites of high-volume fractional, and flake aluminum has higher reason By bulk density, it is more advantageous to reduction porosity, promotes the comprehensive performance of material;High-content graphene itself is easily reunited, Hole is agglomerated into composite material, reduces the intensity of matrix instead;Single-layer graphene involves great expense, it is difficult to make on a large scale With graphene used in research is mostly few layer graphene microchip of the number of plies at 10~50 layers, Van der Waals between graphene layer at present Power is weaker than Covalent bonding together, if interlayer slip occurs in fracture, graphene is difficult to play humidification, and therefore, it is desirable to pass through The mode of ball milling realizes the opening of graphene;Ball milling is conducive to the dispersion and opening of graphene, but common grinding aid, such as silane Coupling agent, ionic surfactant, stearic acid etc., grinding aid decompose difficult or decompose the impurity such as generation Si, Na, can remain in It in alloy matrix aluminum, can all change al alloy component, reduce properties of product, following process use is had an impact.
Summary of the invention:
The present invention is difficult in order to which the grinding aid used in solving the dispersion and opening procedure of graphene decomposes or in aluminium alloy Residual is led to the problem of in matrix, proposes that a kind of polyethylene glycol repairs the preparation method of graphene reinforced aluminum matrix composites.
The preparation method that polyethylene glycol of the present invention repairs graphene reinforced aluminum matrix composites sequentially includes the following steps:
One, weighing
Make by the aluminum metal powder that mass fraction weighs 0.5%~4% graphene, 2%~50% polyethylene glycol and surplus For raw material;The graphene is few layer graphene, and average piece diameter is 200nm~15 μm, and average thickness is 1~30nm;The aluminium The average grain diameter of metal powder is 1~30 μm;
The aluminum metal powder is aluminium alloy;The aluminium alloy is Al-Si alloy, Al-Si-Cu alloy, Al-Cu-Mg conjunction One of gold, Al-Zn-Cu alloy, Al-Zn-Mg-Cu alloy, Al-Si-Cu-Mg alloy or in which several combinations;
The mass fraction of Si is 2%~25% in the Al-Si alloy;The mass fraction of Si is in Al-Si-Cu alloy The mass fraction of 0.5%~25%, Cu are 0.5%~53%;In Al-Cu-Mg alloy the mass fraction of Cu be 0.5%~ The mass fraction of 53%, Mg are 0.5%~38%;The mass fraction of Zn is the matter of 0.5%~55%, Cu in Al-Zn-Cu alloy Measuring score is 0.5%~53%;The mass fraction of Zn is that the mass fraction of 0.5%~55%, Mg is in Al-Zn-Mg-Cu alloy The mass fraction of 0.5%~38%, Cu are 0.5%~53%;In Al-Si-Cu-Mg alloy the mass fraction of Si be 0.5%~ The mass fraction that the mass fraction of 25%, Cu are 0.5%~53%, Mg is 0.5%~38%;
Two, graphene dispersion and prefabricated formation of lots
The weighed graphene of step 1, polyethylene glycol and aluminum metal powder are fitted into ball grinder, with 100~250rpm's The mixed powder that 0.5~7h of revolving speed ball milling is obtained, the mixed-powder obtained after ball milling is fitted into and is cold-pressed to obtain in cold stamping die Polyethylene glycol-graphene/aluminum precast body;
The specific steps being cold-pressed are as follows: be forced into 4 to mixed-powder in the case where pressing speed is 0.1~30mm/min ~8MPa and 5~20min of pressure maintaining;Ratio of grinding media to material in the ball grinder is (5~20): 1;
Three, prefabricated section is kept the temperature
Polyethylene glycol-graphene/aluminum precast body that step 2 obtains is put into vacuum drying oven, is heated to 350~380 DEG C simultaneously 2~2.5h is kept the temperature, then is warming up to 450~490 DEG C of 1~1.2h of heat preservation, polyethylene glycol is obtained and repairs graphene/aluminum precast body;
At 350~380 DEG C, polyethylene glycol is cracked, and the polyethylene glycol after cracking generates largely free oxygen functional group, is had Extremely strong reactivity diffuses to graphene surface at high temperature and carries out absorption combination, is formed in graphene fault location unique Bridging oxygen connection, so that the damaged degree sharp fall of graphene, also can prevent graphene from further being destroyed;450~490 Remaining polyethylene glycol decomposes completely under the conditions of DEG C, diffuses to precast body surface and is removed, and noresidue polyethylene glycol has been made and has repaired Multiple graphene/aluminum precast body;
Four, the polyethylene glycol reparation graphene/aluminum precast body obtained step 3 passes through pressure infiltration method, pressure-free impregnation Method, powder metallurgic method or discharge plasma sintering method are prepared into polyethylene glycol and repair graphene reinforced aluminum matrix composites, i.e., complete At.
The present invention have it is following the utility model has the advantages that
1, the grinding aid polyethylene glycol modest viscosity that the present invention selects, anti-oxidant, volatility is small, corrosion-free to metal, Decomposed in heat treatment process and generate a large amount of free oxygen functional group, oxygen functional group in conjunction with the carbon atom of defect graphene, Bridging oxygen key is formed, different defect carbon is carried out by reparation connection, the breakage for reducing graphene of high degree by bridging oxygen key Degree improves the ability that graphene accepts load, also prevents the further damage of graphene.And polyethylene glycol pyrolytic Product is pollution-free, easily removes under vacuum or atmosphere, and grinding aid residual is avoided to cause elasticity modulus, bending strength, surrender Intensity and tensile strength reduce, and the remaining polyethylene glycol of no grinding aid can be made and repair graphene reinforced aluminum matrix composites.
2, the present invention is using few layer of graphene, aluminum metal and polyethylene glycol as raw material, polyethylene glycol as ball milling grinding aid, Make aluminum metal particle deformation using grinding, shearing and the percussion that abrasive media generates in cylinder rotation in mechanical milling process For sheet;Wherein, coated with polyethylene glycol changes the shock row of ball-milling medium Yu aluminum metal powder behind aluminum metal powder surface To make the shearing force in hitting act more easily on aluminum metal powder surface, so that it is in blocks and advantageous to be conducive to aluminum metal powder It is detached from flake aluminum from ball-milling medium surface, facilitates subsequent operation.
3, the present invention is uniform using the flake aluminum piece diameter prepared after graphene, polyethylene glycol and aluminum metal powder ball milling, Radius-thickness ratio is big, and diameter is 20~50 μm, and with a thickness of 0.5~1 μm, radius-thickness ratio is big, effectively realizes graphene in flake aluminum Surface uniform adsorption advantageously reduces the reunion of graphene in the composite, solves single layer or few layer graphene in aluminium base The big problem of dispersion difficulty in composite material, and coated with polyethylene glycol is on flake aluminum surface prevents to generate after ball milling new Interface directly contacts, and advantageously reduces the cold welding between aluminum metal powder;Graphene reinforced aluminum matrix composites prepared by the present invention In the content of few layer of graphene reach as high as 4wt.%, much higher than at present using few layer of graphene as the content of direct raw material (being less than 1wt.%);
5, polyethylene glycol generates activity C atom after pyrolysis, possesses high go back after being adsorbed on graphene fault location Former activity, so that graphene oxidation defect is significantly repaired, makes the integrality of layer structure get a promotion, complete stratiform Graphene-structured is more advantageous to uniform distractive load, transmits stress, therefore reduce stress raisers, is conducive to composite wood Material bears bigger external force, and then improves the comprehensive performance of composite material;
6, for the present invention using polyethylene glycol as grinding aid, polyethylene glycol is water-soluble good and volatile, easily thermally decomposes, can It is removed by a variety of methods such as vacuum filtration, filters pressing, heat treatment, vacuum drying, to flake aluminum pattern without broken in removal process It is bad, the ingredient and subsequent applications of aluminium alloy are not influenced;
7, the excellent combination property of graphene reinforced aluminum matrix composites prepared by the present invention, elasticity modulus are more than 82GPa, Bending strength is greater than 700MPa, and yield strength is more than 450MPa, and tensile strength is more than 550MPa, and elongation percentage is more than 9%.
Detailed description of the invention:
Fig. 1 is the metallographic characterization photo that the polyethylene glycol that embodiment 1 obtains repairs graphene reinforced aluminum matrix composites;
Specific embodiment:
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment Any reasonable combination.
Specific embodiment 1: present embodiment polyethylene glycol repairs the preparation method of graphene reinforced aluminum matrix composites It sequentially includes the following steps:
One, weighing
Make by the aluminum metal powder that mass fraction weighs 0.5%~4% graphene, 2%~50% polyethylene glycol and surplus For raw material;
Two, graphene dispersion and prefabricated formation of lots
The weighed graphene of step 1, polyethylene glycol and aluminum metal powder are fitted into ball grinder, with 100~250rpm's The mixed powder that 0.5~7h of revolving speed ball milling is obtained, the mixed-powder obtained after ball milling is fitted into and is cold-pressed to obtain in cold stamping die Polyethylene glycol-graphene/aluminum precast body;
Three, prefabricated section is kept the temperature
Polyethylene glycol-graphene/aluminum precast body that step 2 obtains is put into vacuum drying oven, is heated to 350~380 DEG C simultaneously 2~2.5h is kept the temperature, then is warming up to 450~490 DEG C of 1~1.2h of heat preservation, polyethylene glycol is obtained and repairs graphene/aluminum precast body;
Four, the polyethylene glycol reparation graphene/aluminum precast body obtained step 3 passes through pressure infiltration method, pressure-free impregnation Method, powder metallurgic method or discharge plasma sintering method are prepared into polyethylene glycol and repair graphene reinforced aluminum matrix composites, i.e., complete At.
Present embodiment have it is following the utility model has the advantages that
1, the grinding aid polyethylene glycol modest viscosity of present embodiment selection, anti-oxidant, volatility is small, to metal without corruption Erosion decomposes generate a large amount of free oxygen functional group during heat treatment, and the carbon atom of oxygen functional group and defect graphene occurs In conjunction with forming bridging oxygen key, different defect carbon carried out reparation connection by bridging oxygen key, high degree reduces graphene Damaged degree improves the ability that graphene accepts load, also prevents the further damage of graphene.And polyethylene glycol high temperature Decomposition product is pollution-free, easily removes under vacuum or atmosphere, avoid grinding aid residual cause elasticity modulus, bending strength, Yield strength and tensile strength reduce, and the remaining polyethylene glycol of no grinding aid can be made and repair graphene enhancing aluminum-base composite material Material.
2, using few layer of graphene, aluminum metal and polyethylene glycol as raw material, polyethylene glycol helps present embodiment as ball milling Grinding agent makes aluminum metal using grinding, shearing and the percussion that abrasive media generates in cylinder rotation in mechanical milling process Particle shape becomes sheet;Wherein, coated with polyethylene glycol changes ball-milling medium and aluminum metal powder behind aluminum metal powder surface Shock behavior makes the shearing force in hitting act more easily on aluminum metal powder surface, thus it is in blocks conducive to aluminum metal powder, and And be conducive to flake aluminum and be detached from from ball-milling medium surface, facilitate subsequent operation.
3, present embodiment is equal using the flake aluminum piece diameter prepared after graphene, polyethylene glycol and aluminum metal powder ball milling Even, radius-thickness ratio is big, and diameter is 20~50 μm, and with a thickness of 0.5~1 μm, radius-thickness ratio is big, effectively realizes graphene in flaky aluminum Powder surface uniform adsorption advantageously reduces the reunion of graphene in the composite, solves single layer or few layer graphene in aluminium The big problem of dispersion difficulty in based composites, and coated with polyethylene glycol is on flake aluminum surface prevents to generate after ball milling New interface directly contacts, and advantageously reduces the cold welding between aluminum metal powder;The graphene enhancing aluminium base of present embodiment preparation is multiple The content of few layer of graphene in condensation material reaches as high as 4wt.%, much higher than at present using few layer of graphene as direct raw material Content (is less than 1wt.%);
5, polyethylene glycol generates activity C atom after pyrolysis, possesses high go back after being adsorbed on graphene fault location Former activity, so that graphene oxidation defect is significantly repaired, makes the integrality of layer structure get a promotion, complete stratiform Graphene-structured is more advantageous to uniform distractive load, transmits stress, therefore reduce stress raisers, is conducive to composite wood Material bears bigger external force, and then improves the comprehensive performance of composite material;
6, present embodiment is using polyethylene glycol as grinding aid, and polyethylene glycol is water-soluble good and volatile, easily heat point Solution can be removed by a variety of methods such as vacuum filtration, filters pressing, heat treatment, vacuum drying, to flake aluminum pattern in removal process Without destruction, the ingredient and subsequent applications of aluminium alloy are not influenced;
7, the excellent combination property of the graphene reinforced aluminum matrix composites of present embodiment preparation, elasticity modulus are more than 82GPa, bending strength are greater than 700MPa, and yield strength is more than 450MPa, and tensile strength is more than 550MPa, and elongation percentage is more than 9%.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: graphene described in step 1 is Few layer graphene, average piece diameter are 200nm~15 μm, and average thickness is 1~30nm.Other steps and parameter and specific embodiment party Formula one is identical.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: aluminium gold described in step 1 The average grain diameter for belonging to powder is 1~30 μm.Other steps and parameter are the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: described in step 1 Aluminum metal powder is aluminium alloy.Other steps and parameter are identical as one of specific embodiment one to three.
Specific embodiment 5: present embodiment is unlike specific embodiment four: aluminium alloy described in step 1 is Al-Si alloy, Al-Si-Cu alloy, Al-Cu-Mg alloy, Al-Zn-Cu alloy, Al-Zn-Mg-Cu alloy, Al-Si-Cu-Mg One of alloy or in which several combinations.Other steps and parameter are identical as specific embodiment four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: the Al-Si is closed The mass fraction of Si is 2%~25% in gold;The mass fraction of Si is the quality of 0.5%~25%, Cu in Al-Si-Cu alloy Score is 0.5%~53%;The mass fraction that the mass fraction of Cu is 0.5%~53%, Mg in Al-Cu-Mg alloy is 0.5% ~38%;The mass fraction that the mass fraction of Zn is 0.5%~55%, Cu in Al-Zn-Cu alloy is 0.5%~53%;Al- The quality that the mass fraction that the mass fraction of Zn is 0.5%~55%, Mg in Zn-Mg-Cu alloy is 0.5%~38%, Cu point Number is 0.5%~53%;The mass fraction of Si is that the mass fraction of 0.5%~25%, Cu is in Al-Si-Cu-Mg alloy The mass fraction of 0.5%~53%, Mg are 0.5%~38%.Other steps and one of parameter and specific embodiment one to five It is identical.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: described in step 2 The specific steps being cold-pressed are as follows: be forced into 4~8MPa and pressure maintaining to mixed-powder in the case where pressing speed is 0.1~30mm/min 5~20min.Other steps and parameter are identical as one of specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: described in step 2 Ratio of grinding media to material in ball grinder is (5~20): 1.Other steps and parameter are identical as one of specific embodiment one to seven.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment 1:
The preparation method that the present embodiment polyethylene glycol repairs graphene reinforced aluminum matrix composites sequentially includes the following steps:
One, weighing
The aluminum metal powder of 4% graphene, 50% polyethylene glycol and surplus is weighed as raw material by mass fraction;The stone Black alkene is few layer graphene, and average piece diameter is 200nm, average thickness 1nm;The average grain diameter of the aluminum metal powder is 1 μm;
The aluminum metal powder is aluminium alloy;The aluminium alloy is Al-Si alloy, the mass fraction of Si in Al-Si alloy It is 2%~25%;
Two, graphene dispersion and prefabricated formation of lots
The weighed graphene of step 1, polyethylene glycol and aluminum metal powder are fitted into ball grinder, with the revolving speed of 250rpm The mixed-powder obtained after ball milling is fitted into and is cold-pressed to obtain polyethylene glycol-in cold stamping die by the mixed powder that ball milling 0.5 obtains Graphene/aluminum precast body;
The specific steps being cold-pressed are as follows: be forced into 8MPa to mixed-powder in the case where pressing speed is 0.1mm/min And pressure maintaining 5min;Ratio of grinding media to material in the ball grinder is 5:1;
Three, prefabricated section is kept the temperature
Polyethylene glycol-graphene/aluminum precast body that step 2 obtains is put into vacuum drying oven, 360 DEG C is heated to and keeps the temperature 2h, then 470 DEG C of heat preservation 1h are warming up to, it obtains polyethylene glycol and repairs graphene/aluminum precast body;
At 350~380 DEG C, polyethylene glycol is cracked, and the polyethylene glycol after cracking generates largely free oxygen functional group, is had Extremely strong reactivity diffuses to graphene surface at high temperature and carries out absorption combination, is formed in graphene fault location unique Bridging oxygen connection, so that the damaged degree sharp fall of graphene, also can prevent graphene from further being destroyed;450~490 Remaining polyethylene glycol decomposes completely under the conditions of DEG C, diffuses to precast body surface and is removed, and noresidue polyethylene glycol has been made and has repaired Multiple graphene/aluminum precast body;
Four, the polyethylene glycol reparation graphene/aluminum precast body obtained step 3 passes through pressure infiltration method, pressure-free impregnation Method, powder metallurgic method or discharge plasma sintering method are prepared into polyethylene glycol and repair graphene reinforced aluminum matrix composites, i.e., complete At.
The pressure infiltration method specifically comprises the processes of: polyethylene glycol reparation graphene/aluminum precast body is put into vacuum pressure Infiltration furnace, fine aluminium block are put into the graphite jig of the furnace cavity bottom of vacuum gas pressure infiltration furnace, and polyethylene glycol repairs graphene/aluminum Precast body is placed in the furnace chamber top of vacuum gas pressure infiltration furnace, vacuum gas pressure infiltration furnace is closed and be evacuated to vacuum degree and be less than 10-4MPa, then heating, vacuum gas pressure infiltration furnace, is preheating to 400 for polyethylene glycol reparation graphene/aluminum precast body under vacuum ℃;Commercial-purity aluminium block is heated to 760 DEG C and keeps the temperature the aluminum metal that 0.5h melted;The polyethylene glycol of preheating is repaired into stone Black alkene/aluminium precast body stops heating after immersing the aluminum metal melted, is then passed through protective gas into vacuum gas pressure infiltration furnace, High-densit graphene reinforced aluminum matrix composites are obtained after the in-furnace temperature cooled to room temperature of vacuum gas pressure infiltration furnace Ingot casting;The protective gas is nitrogen;The pressure of the protective gas is 0.1MPa;
Fig. 1 is the metallographic characterization photo that the polyethylene glycol that embodiment 1 obtains repairs graphene reinforced aluminum matrix composites, from It can be seen that graphene microchip is evenly distributed in figure, without compared with macro aggregate, material entirety consistency is higher, and porosity is lower.This reality It is uniform using the flake aluminum piece diameter prepared after graphene, polyethylene glycol and aluminum metal powder ball milling to apply example, radius-thickness ratio is big, diameter It is 30~50 μm, with a thickness of 0.7~1 μm, radius-thickness ratio is big, effectively realize graphene in flake aluminum surface uniform adsorption, The reunion of graphene in the composite is advantageously reduced, solves point of single layer or few layer graphene in aluminum matrix composite The big problem of difficulty is dissipated, the content of few layer of graphene in composite material reaches as high as 4wt.%;Poly- second manufactured in the present embodiment Glycol repairs the excellent combination property of graphene reinforced aluminum matrix composites, elasticity modulus 82GPa, and bending strength is 800MPa, yield strength 550MPa, tensile strength 650MPa, elongation percentage 10%.
Embodiment 2:
The preparation method that the present embodiment polyethylene glycol repairs graphene reinforced aluminum matrix composites sequentially includes the following steps:
One, weighing
The aluminum metal powder of 4% graphene, 2% polyethylene glycol and surplus is weighed as raw material by mass fraction;The stone Black alkene is few layer graphene, and average piece diameter is 15 μm, average thickness 30nm;The average grain diameter of the aluminum metal powder is 30 μ m;
The aluminum metal powder is aluminium alloy;The Al-Cu-Mg alloy, the mass fraction of Cu is in Al-Cu-Mg alloy The mass fraction of 0.5%~53%, Mg are 0.5%~38%;
Two, graphene dispersion and prefabricated formation of lots
The weighed graphene of step 1, polyethylene glycol and aluminum metal powder are fitted into ball grinder, with the revolving speed of 250rpm The mixed-powder obtained after ball milling is fitted into and is cold-pressed to obtain polyethylene glycol-in cold stamping die by the mixed powder that ball milling 0.5 obtains Graphene/aluminum precast body;
The specific steps being cold-pressed are as follows: be forced into 4MPa simultaneously to mixed-powder in the case where pressing speed is 30mm/min Pressure maintaining 10min;Ratio of grinding media to material in the ball grinder is 10:1;
Three, prefabricated section is kept the temperature
Polyethylene glycol-graphene/aluminum precast body that step 2 obtains is put into vacuum drying oven, 360 DEG C is heated to and keeps the temperature 2h, then 470 DEG C of heat preservation 1h are warming up to, it obtains polyethylene glycol and repairs graphene/aluminum precast body;
Four, the polyethylene glycol reparation graphene/aluminum precast body obtained step 3 passes through pressure infiltration method, pressure-free impregnation Method, powder metallurgic method or discharge plasma sintering method are prepared into polyethylene glycol and repair graphene reinforced aluminum matrix composites, i.e., complete At.
The pressure infiltration method specifically comprises the processes of: polyethylene glycol reparation graphene/aluminum precast body is put into vacuum pressure Infiltration furnace, fine aluminium block are put into the graphite jig of the furnace cavity bottom of vacuum gas pressure infiltration furnace, and polyethylene glycol repairs graphene/aluminum Precast body is placed in the furnace chamber top of vacuum gas pressure infiltration furnace, vacuum gas pressure infiltration furnace is closed and be evacuated to vacuum degree and be less than 10-4MPa, then heating, vacuum gas pressure infiltration furnace, is preheating to 400 for polyethylene glycol reparation graphene/aluminum precast body under vacuum ℃;Commercial-purity aluminium block is heated to 760 DEG C and keeps the temperature the aluminum metal that 0.5h melted;The polyethylene glycol of preheating is repaired into stone Black alkene/aluminium precast body stops heating after immersing the aluminum metal melted, is then passed through protective gas into vacuum gas pressure infiltration furnace, High-densit graphene reinforced aluminum matrix composites are obtained after the in-furnace temperature cooled to room temperature of vacuum gas pressure infiltration furnace Ingot casting;The protective gas is nitrogen;The pressure of the protective gas is 0.1MPa;
The present embodiment utilizes the flake aluminum piece diameter prepared after graphene, polyethylene glycol and aluminum metal powder ball milling uniform, Radius-thickness ratio is big, and diameter is 10~20 μm, and with a thickness of 0.5~0.8 μm, radius-thickness ratio is big, effectively realizes graphene in flaky aluminum Powder surface uniform adsorption advantageously reduces the reunion of graphene in the composite, solves single layer or few layer graphene in aluminium The content of the big problem of dispersion difficulty in based composites, few layer of graphene in composite material reaches as high as 4wt.%;This The excellent combination property of the polyethylene glycol reparation graphene reinforced aluminum matrix composites of embodiment preparation, elasticity modulus 92GPa, Bending strength is 710MPa, yield strength 460MPa, tensile strength 560MPa, elongation percentage 10%.

Claims (8)

1. the preparation method that a kind of polyethylene glycol repairs graphene reinforced aluminum matrix composites, it is characterised in that: this method press with Lower step carries out:
One, weighing
The aluminum metal powder of 0.5%~4% graphene, 2%~50% polyethylene glycol and surplus is weighed as former by mass fraction Material;
Two, graphene dispersion and prefabricated formation of lots
The weighed graphene of step 1, polyethylene glycol and aluminum metal powder are fitted into ball grinder, with the revolving speed of 100~250rpm The mixed-powder obtained after ball milling is fitted into cold stamping die and is cold-pressed to obtain poly- second by the mixed powder that 0.5~7h of ball milling is obtained Glycol-graphene/aluminum precast body;
Three, prefabricated section is kept the temperature
Polyethylene glycol-graphene/aluminum precast body that step 2 obtains is put into vacuum drying oven, 350~380 DEG C is heated to and keeps the temperature 2~2.5h, then 450~490 DEG C of 1~1.2h of heat preservation are warming up to, it obtains polyethylene glycol and repairs graphene/aluminum precast body;
Four, the polyethylene glycol reparation graphene/aluminum precast body obtained step 3 passes through pressure infiltration method, pressure-free impregnation method, powder Last metallurgy method or discharge plasma sintering method are prepared into polyethylene glycol and repair graphene reinforced aluminum matrix composites, that is, complete.
2. polyethylene glycol according to claim 1 repairs the preparation method of graphene reinforced aluminum matrix composites, feature Be: graphene described in step 1 is few layer graphene, and average piece diameter is 200nm~15 μm, and average thickness is 1~30nm.
3. polyethylene glycol according to claim 1 or 2 repairs the preparation method of graphene reinforced aluminum matrix composites, special Sign is: the average grain diameter of aluminum metal powder described in step 1 is 1~30 μm.
4. the method according to claim 3 for preparing graphene reinforced aluminum matrix composites with polyethylene glycol auxiliary, special Sign is: aluminum metal powder described in step 1 is aluminium alloy.
5. polyethylene glycol according to claim 4 repairs the preparation method of graphene reinforced aluminum matrix composites, feature Be: the aluminium alloy is Al-Si alloy, Al-Si-Cu alloy, Al-Cu-Mg alloy, Al-Zn-Cu alloy, Al-Zn-Mg-Cu One of alloy, Al-Si-Cu-Mg alloy or in which several combinations.
6. polyethylene glycol according to claim 5 repairs the preparation method of graphene reinforced aluminum matrix composites, feature Be: the mass fraction of Si is 2%~25% in the Al-Si alloy;The mass fraction of Si is 0.5% in Al-Si-Cu alloy The mass fraction of~25%, Cu are 0.5%~53%;The mass fraction of Cu is 0.5%~53%, Mg's in Al-Cu-Mg alloy Mass fraction is 0.5%~38%;The mass fraction of Zn is that the mass fraction of 0.5%~55%, Cu is in Al-Zn-Cu alloy 0.5%~53%;The mass fraction that the mass fraction of Zn is 0.5%~55%, Mg in Al-Zn-Mg-Cu alloy is 0.5%~ The mass fraction of 38%, Cu are 0.5%~53%;The mass fraction of Si is 0.5%~25%, Cu in Al-Si-Cu-Mg alloy Mass fraction be 0.5%~53%, Mg mass fraction be 0.5%~38%.
7. polyethylene glycol according to claim 6 repairs the preparation method of graphene reinforced aluminum matrix composites, feature It is: the specific steps being cold-pressed described in step 2 are as follows: pressurize in the case where pressing speed is 0.1~30mm/min to mixed-powder To 4~8MPa and 5~20min of pressure maintaining.
8. polyethylene glycol according to claim 6 repairs the preparation method of graphene reinforced aluminum matrix composites, feature Be: the ratio of grinding media to material in ball grinder described in step 2 is (5~20): 1.
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