CN108941547A - A kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites - Google Patents
A kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 131
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 130
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 119
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 238000005253 cladding Methods 0.000 title claims abstract description 35
- 239000011159 matrix material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000004411 aluminium Substances 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 239000008187 granular material Substances 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 31
- 230000008569 process Effects 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 18
- 229910001431 copper ion Inorganic materials 0.000 abstract description 14
- 238000010406 interfacial reaction Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 30
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 18
- 229910052802 copper Inorganic materials 0.000 description 18
- 239000010949 copper Substances 0.000 description 18
- 235000019441 ethanol Nutrition 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 230000002708 enhancing effect Effects 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- 238000007542 hardness measurement Methods 0.000 description 5
- 238000004663 powder metallurgy Methods 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 230000002787 reinforcement Effects 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000006213 oxygenation reaction Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
-
- 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
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to a kind of preparation methods of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites, specifically includes the following steps: (1) ethanol solution is added in aluminium powder, add graphene oxide solution, copper-bath is added after stirring, stirring, stand to supernatant clarify, be filtered, washed, dry after obtain Copper-cladding Aluminum Bar graphene/aluminum composite granule；(2) hot pressed sintering is carried out to obtained Copper-cladding Aluminum Bar graphene/aluminum composite granule.Compared with prior art, the present invention is coated on the interfacial reaction that aluminium powder surface effectively avoids the reunion of graphene and graphene and aluminium occur by copper ion, the Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites prepared through the invention, microhardness improve 110% or more.
Description
Technical field
The present invention relates to a kind of preparation methods of composite material, multiple more particularly, to a kind of Copper-cladding Aluminum Bar graphene enhancing aluminium base
The preparation method of condensation material.
Background technique
Since density is small, performance stabilization has extensively aluminum matrix composite in aerospace and high-end automobile manufacturing field
Application.Compared to traditional reinforcement (ceramic particle, carbon fiber, carbon nanotube etc.), graphene low, mechanical property with density
Advantages, the graphenes such as high, good heat conductivity and thermal expansion coefficient are low are regarded as a kind of very promising from birth
Reinforcement.High performance graphene reinforced aluminum matrix composites are developed in success, and composite property not only can be improved, while
Composite density can be reduced.
In terms of the preparation method of graphene reinforced aluminum matrix composites, mainly there is powder metallurgy process, casting method, stirs
Mix the methods of friction processing.In the above-mentioned methods due to spies such as powder metallurgy process technical maturity, even tissue and near-net-shapes
Point is concerned in the preparation of graphene reinforced aluminum matrix composites.Currently, powder metallurgy, which becomes, prepares graphene enhancing
The important method of aluminum matrix composite.
It finds by prior art documents, Jingyue Wang et al. (Reinforcement with
graphene nanosheets in aluminum matrix composites,Scripta Materialia,2012,66,
It 594-597) has studied and aluminium powder surface is modified by the way that PVA solvent is added, improve the uniformly dispersed problem of graphene.
S.F.Bartolucci et al. (Graphene-aluminum nanocomposites, Materials Science and
Engineering A, 2011,528,7933-7937) it has studied powder metallurgy process and prepares graphene reinforced aluminum matrix composites
In the process, it results in since interfacial reaction has occurred in graphene and aluminium and has generated largely Al in the composite4C3Carbonization
Object reduces the mechanical property of composite material.Therefore, graphene reinforced metal-matrix composite mistake is prepared in powder metallurgy process
Cheng Zhong, graphene reinforcement uniformly dispersed and avoids graphene and aluminium that interfacial reaction occurs becoming preparation high-performance stone
The critical issue of black alkene reinforced aluminum matrix composites.
Chinese patent CN201710342605.2 discloses a kind of modified graphene reinforced aluminum matrix composites and its preparation
Cation surface activating is added after being uniformly dispersed specifically includes the following steps: graphene is added to absolute ethanol by (1) in method
Agent ultrasound, is made modified graphene after drying；(2) fine aluminium is melted, modified graphene is added when melting half, kept the temperature；(3) add
Add to keep the temperature after copper, carbon, iron, silicon carbide and lanthana and stir evenly, refines, stands, skimming operation obtains aluminium alloy melt；(4) to aluminium
Alloy melt carry out gravitational casting, obtain aluminium alloy castings, casting is once dissolved, cool down and ageing treatment after be made change
Property graphene reinforced aluminum matrix composites.The preparation method process is complicated, and interfacial reaction can occur for graphene and aluminium in the process, lead
Causing the mechanical property of composite material reduces.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of Copper-cladding Aluminum Bar graphenes
Reinforced aluminum matrix composites.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites, specifically includes the following steps:
(1) ethanol solution is added in aluminium powder, adds sonicated graphene oxide solution, sulphur is added after stirring
Sour copper solution, stirring, stand to supernatant clarify, be filtered, washed, dry after obtain Copper-cladding Aluminum Bar graphene/aluminum composite granule；
(2) hot pressed sintering is carried out to obtained Copper-cladding Aluminum Bar graphene/aluminum composite granule.
Preferably, in step (1), the graphene oxide solution is prepared by Hummers method.
Preferably, in step (1), the specific steps of the Hummers method are as follows: by high purity graphite and NaNO3It is added to
H2SO4In solution, uniform stirring is gradually added into KMnO4, after uniform stirring 1h, 200ml water is added, in 100 DEG C of stirring 1h, then
H is added2O2And HCl solution, it is centrifugated various sizes of graphene oxide.
Preferably, the mass ratio of the aluminium powder, graphene and the copper sulphate that are added in step (1) is 100:(0.3-1.0): (5-
15)。
It is furthermore preferred that the mass ratio of the aluminium powder being added in step (1), graphene oxide and copper sulphate is 100:0.3:10.
Preferably, in step (1): the ratio of water and alcohol is 1:7-1:8 in the ethanol solution.
It is furthermore preferred that in step (1): the ratio of water and alcohol is 1:7 in the ethanol solution.
Preferably, in step (1): the ratio of the aluminium powder of addition and ethanol solution is 10g:80mL.
Preferably, hot pressed sintering described in step (2) is carried out in two steps, and the first step is cold pressing treatment, and second step is hot pressing
Sintering.
It is furthermore preferred that the process conditions of the cold pressing treatment are as follows: load 6t, temperature are room temperature.
It is furthermore preferred that the process conditions of the hot pressed sintering are as follows: load 5-10t, temperature be 580 DEG C, processing the time be
3-4h。
It is furthermore preferred that the temperature-rise period of the hot pressed sintering are as follows: 1h is warming up to 580 DEG C, in 580 DEG C of heat preservation 3h.
In step (2): copper ion is coated on aluminium powder surface, and partial reduction occurs for simultaneous oxidation graphene, and is adsorbed on
Aluminium powder surface is finally cleaned and dried and forms graphene/copper/aluminium multilayer coating structure powder.
Before solution is added in copper sulphate, there is no anti-for the graphene oxide in aluminium powder and suspension with hydrophobic surface
It answers.After copper-bath is added, copper ion on the one hand can with the function oxygen groups of graphene oxide (including epoxy group, carbonyl and
Carboxyl) chemistry or electrostatical binding occurs, another aspect aluminium powder occurs displacement with copper ion and reacts, to help graphene oxide sheet
The surface for being attached to aluminium powder is inhaled, in this chemical reaction process, metal has promoted graphene oxide generation as reducing agent
Reduction reaction.Graphene/copper/aluminium multilayer coating structure powder has been prepared by wet process.On the other hand, the addition of copper ion
So that forming aluminium copper in sintering process further increases performance.Graphene oxide improves aluminum matrix composite as reinforcement
Performance, copper-bath provide copper ion.The hydrolysis of ethanol solution inhibition aluminium powder.
Copper sulphate is first added in the solution of aluminium powder and alcohol, afterwards plus graphene oxide solution, after repeatedly testing, hair
Now last alcohol washes process can all take copper ion out of.And the effect of Copper-cladding Aluminum Bar is not achieved.According to first oxygenation graphite
Alkene, after vulcanization acid copper solution, obtained 1%Cu2+, 3%Cu2+, 5%Cu2+Graphene/aluminum composite material hardness number, hardness
Value is respectively 33,50,71,68.In 3%Cu2+When, the hardness of composite material reaches maximum value.In addition, if the ratio mistake of water
It is more, then particle aluminium powder, which will occur seriously to hydrolyze, becomes aluminium hydroxide.If copper sulphate, which is added, excessively will appear saturation, extra
Copper ion can not adsorb completely.
Compared with prior art, the invention proposes a kind of preparation sides of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites
Method can prepare graphene/copper/aluminium multilayer coating structure powder, effectively avoid the dispersion unevenness and aluminium of graphene
Interfacial reaction between graphene helps to improve the mechanical property of graphene reinforced aluminum matrix composites.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of raw material graphene oxide sheet in embodiment 1；
Fig. 2 is the stereoscan photograph of the aluminium powder prepared in embodiment 1；
Fig. 3 is graphene/copper in embodiment 1/aluminium composite granule stereoscan photograph；
Fig. 4 is the compound fission EDS elemental analysis result of graphene/copper/aluminium in embodiment 1；
Fig. 5 is 1 fine aluminium of embodiment and Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites Vickers hardness result.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
(1) preparation of graphene oxide
The preparation method of graphene oxide: by 5g high purity graphite, 2.5g NaNO3It is added to H2SO4In solution, uniformly stir
It mixes, is then gradually added into KMnO4, uniform stirring 1 hour, 200ml water is added, is stirred 1 hour at 100 DEG C, H is added2O2And
HCl solution.It is then centrifugated various sizes of graphene oxide, obtains the almost the same graphene oxide solution of size.System
The stereoscan photograph of standby obtained graphene oxide sheet is as shown in Figure 1.
(2) graphene/copper/aluminium multilayer coating structure powder preparation
0.03g graphene oxide is dissolved in 10mL water, graphene oxide solution is made, is added to after sonicated
In the mixed solution of 10g aluminium powder and 80ml ethyl alcohol, in solution the volume ratio of water and ethyl alcohol be 1:7, with glass bar stirring 3~
5min is then added copper-bath and stirs, and the mass ratio of copper sulphate and aluminium powder is 1:10, stands to supernatant and clarifies, cleaning
It is dry.In this process, copper ion is coated on the surface of aluminium powder, and the reduction of part has occurred in simultaneous oxidation graphene, is formed
Redox graphene.The stereoscan photograph of raw material aluminium powder is as shown in Fig. 2, composite granule microscopic appearance is shown in Fig. 3, EDS member
Plain distribution results are as shown in Figure 4.Graphene coated can be obviously observed in the SEM image of Fig. 3 on aluminium powder surface, the EDS of Fig. 4 divides
Copper and carbon are contained in analysis display aluminium powder surface, and further demonstrating copper ion can be used as conjugative bridge promotion aluminium powder and graphene oxide
Absorption.
(3) hot pressed sintering of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites and composite material micro-hardness testing
Graphene/the copper prepared/aluminium multilayer coating structure powder is put into hot pressed sintering mold, is first 6t in load
Lower room temperature cold pressing, then uses hot pressed sintering, and sets hot pressed sintering parameter: loaded load is 5~10t, and argon gas is protected, the
One 580 DEG C of stage heating 1h, 580 DEG C of heat preservation 3h of second stage obtain the graphene enhancing alumina-base material of Copper-cladding Aluminum Bar.
To whether there is or not the graphene reinforced aluminum matrix composites of Copper-cladding Aluminum Bar to carry out micro-hardness testing, load 100N keeps carrying
Lotus time 10s.Every kind of material prepares 3 groups of samples, respectively tests 16 points, takes its average value, test results are shown in figure 5.
Test result shows that the graphene/copper/aluminium multilayer coating structure powder prepared by this method can be made into performance
Excellent Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites.Micro-hardness testing is the results show that Copper-cladding Aluminum Bar graphene enhances aluminium base
Composite material is compared with the material of no addition copper ion, and hardness is increased to 71 from 33, and Copper-cladding Aluminum Bar graphene enhances aluminum-base composite
Material (0.3wt% graphene content, 3wt% copper content) less adds the graphene reinforced aluminum matrix composites of copper ion
(0.3wt% graphene content) improves 110%.This method can be used for preparing high-performance copper doped graphene enhancing aluminum-base composite
Material.
Embodiment 2
(1) preparation of graphene oxide
The preparation method of graphene oxide: by 5g high purity graphite, 2.5g NaNO3It is added to H2SO4In solution, uniformly stir
It mixes, is then gradually added into KMnO4, uniform stirring 1 hour, 200ml water is added, is stirred 1 hour at 100 DEG C, H is added2O2And
HCl solution.It is then centrifugated various sizes of graphene oxide, obtains the almost the same graphene oxide solution of size.System
The stereoscan photograph of standby obtained graphene oxide sheet is as shown in Figure 1.
(2) graphene/copper/aluminium multilayer coating structure powder preparation
0.08g graphene oxide is dissolved in 10mL water, graphene oxide solution is made, is added to after sonicated
In the mixed solution of 10g aluminium powder and 80ml ethyl alcohol, in solution the volume ratio of water and ethyl alcohol be 1:8, with glass bar stirring 3~
5min is then added copper-bath and stirs, and the mass ratio of copper sulphate and aluminium powder is 0.5:10, stands to supernatant and clarifies, clearly
Wash drying.In this process, copper ion is coated on the surface of aluminium powder, and the reduction of part, shape has occurred in simultaneous oxidation graphene
At redox graphene.
(3) hot pressed sintering of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites and composite material micro-hardness testing
Graphene/the copper prepared/aluminium multilayer coating structure powder is put into hot pressed sintering mold, is first 6t in load
Lower room temperature cold pressing, then uses hot pressed sintering, and sets hot pressed sintering parameter: loaded load is 5~10t, and argon gas is protected, the
One 580 DEG C of stage heating 1h, 580 DEG C of heat preservation 3h of second stage obtain the graphene enhancing alumina-base material of Copper-cladding Aluminum Bar.
Embodiment 3
(1) preparation of graphene oxide
The preparation method of graphene oxide: by 5g high purity graphite, 2.5g NaNO3It is added to H2SO4In solution, uniformly stir
It mixes, is then gradually added into KMnO4, uniform stirring 1 hour, 200ml water is added, is stirred 1 hour at 100 DEG C, H is added2O2And
HCl solution.It is then centrifugated various sizes of graphene oxide, obtains the almost the same graphene oxide solution of size.System
The stereoscan photograph of standby obtained graphene oxide sheet is as shown in Figure 1.
(2) graphene/copper/aluminium multilayer coating structure powder preparation
0.1g graphene oxide is dissolved in 10mL water, graphene oxide solution is made, is added to 10g after sonicated
In the mixed solution of aluminium powder and 80ml ethyl alcohol, the volume ratio of water and ethyl alcohol is 1:7 in solution, stirs 3~5min with glass bar, with
Copper-bath is added afterwards to stir, the mass ratio of copper sulphate and aluminium powder is 1.5:10, stands to supernatant and clarifies, and is cleaned and dried.
In this process, copper ion is coated on the surface of aluminium powder, and the reduction of part has occurred in simultaneous oxidation graphene, forms reduction
Graphene oxide.
(3) hot pressed sintering of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites and composite material micro-hardness testing
Graphene/the copper prepared/aluminium multilayer coating structure powder is put into hot pressed sintering mold, is first 6t in load
Lower room temperature cold pressing, then uses hot pressed sintering, and sets hot pressed sintering parameter: loaded load is 5~10t, and argon gas is protected, the
One 580 DEG C of stage heating 1h, 580 DEG C of heat preservation 3h of second stage obtain the graphene enhancing alumina-base material of Copper-cladding Aluminum Bar.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (9)
1. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites, which is characterized in that specifically includes the following steps:
(1) ethanol solution is added in aluminium powder, adds sonicated graphene oxide solution, copper sulphate is added after stirring
Solution, stirring, stand to supernatant clarify, be filtered, washed, dry after obtain Copper-cladding Aluminum Bar graphene/aluminum composite granule；
(2) hot pressed sintering is carried out to obtained Copper-cladding Aluminum Bar graphene/aluminum composite granule.
2. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites according to claim 1, feature exist
In in step (1), the graphene oxide solution is prepared by improving Hummers method.
3. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites according to claim 2, feature exist
In the specific steps for improving Hummers method are as follows: by high purity graphite and NaNO3It is added to H2SO4In solution, uniformly stir
It mixes, is gradually added into KMnO4, after uniform stirring 1h, 200ml water is added in 100 DEG C of stirring 1h, H is then added2O2And HCl is molten
Liquid is centrifugated various sizes of graphene oxide.
4. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites according to claim 1, feature exist
In the mass ratio of the aluminium powder, graphene and the copper sulphate that are added in step (1) is 100:(0.3-1.0): (5-15).
5. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites according to claim 1, feature exist
In in step (1): the volume ratio of water and alcohol is 1:7-1:8 in the ethanol solution.
6. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites according to claim 1, feature exist
In in step (1): the ratio of the aluminium powder of addition and ethanol solution is 10g:80mL.
7. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites according to claim 1, feature exist
In hot pressed sintering described in step (2) is carried out in two steps, and the first step is cold pressing treatment, and second step is hot pressed sintering.
8. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites according to claim 7, feature exist
In the process conditions of the cold pressing treatment are as follows: load 6t, temperature are room temperature.
9. a kind of preparation method of Copper-cladding Aluminum Bar graphene reinforced aluminum matrix composites according to claim 7, feature exist
In the process conditions of the hot pressed sintering are as follows: load 5-10t, temperature are 580 DEG C, and the processing time is 3-4h.
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Effective date of registration: 20240108 Address after: No. 143 Houtou, Xiban Village, Guanxun Town, Zhangpu County, Zhangzhou City, Fujian Province, 363200 Patentee after: Weng Senqi Address before: 200093 No. 516, military road, Shanghai, Yangpu District Patentee before: University of Shanghai for Science and Technology |