CN110042284A - A kind of preparation method of high-strength aluminum alloy - Google Patents

A kind of preparation method of high-strength aluminum alloy Download PDF

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Publication number
CN110042284A
CN110042284A CN201910379805.4A CN201910379805A CN110042284A CN 110042284 A CN110042284 A CN 110042284A CN 201910379805 A CN201910379805 A CN 201910379805A CN 110042284 A CN110042284 A CN 110042284A
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China
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aluminum alloy
graphene
strength aluminum
alloy
deionized water
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CN201910379805.4A
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Inventor
郭新立
殷亮亮
陈忠涛
张伟杰
刘园园
郑艳梅
唐璇
王艺璇
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Southeast University
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Southeast University
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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
    • C22C21/00Alloys based on aluminium
    • C22C21/06Alloys based on aluminium with magnesium as the next major constituent

Abstract

The present invention relates to a kind of preparation methods of high-strength aluminum alloy.Be used as aluminium alloy nanometer reinforcing phase using the graphene of environmentally protective shearing method preparation, can refining aluminum alloy crystal grain, while reinforced aluminium alloy, cost is relatively low, it is easy to accomplish produces in batches.Mainly comprise the following steps that: 1: according to the ratio by natural graphite, polyvinylpyrrolidone, sodium taurocholate ultrasonic disperse is in deionized water;2: mixed solvent in step 1 being placed in mixture of ice and water, while starting cutter, revolving speed is 5000-15000r min‑1, shear time 1-3h;3: the mixed solution sheared in step 2 being stood into 20-30h, so that bulky grain settles, obtains layering solution;4: by step 3 at the middle and upper levels liquid with 3000-6000r min‑1Rate centrifugal treating 20-60min, remove all unpeeled graphite flakes.Above-mentioned clear liquid is freeze-dried again after filtering, obtains powdery graphite alkene;5: by discharge plasma sintering furnace that the graphene of different ratio and (Al-1Mg) is powder sintered at high-strength alloy.

Description

A kind of preparation method of high-strength aluminum alloy
Technical field
The invention belongs to metal material fields, are related to a kind of high-strength aluminum alloy method.
Background technique
Aluminium alloy is widely used in the industrial circles such as automobile, machinery, aerospace.Mixing reinforced phase is that one kind is able to ascend The effective ways of aluminium alloy comprehensive performance.By mixing reinforced phase, when stress, can hinder the dislocation motion in aluminium alloy, thus Reach enhancement purpose.Metal nano reinforced phase common at present is (for example, silicon carbide, carbon nanotube, boron nitride, aluminium oxide etc. are received Scale particles) in sinter treatment process, it is easy to appear the elements such as aluminium, the magnesium in crystal grain intensified element carbon and alloy and occurs Reaction forms multi-element compounds, to reduce intensified element effective content, and then occurs to strengthen decay.Therefore, aluminium alloy Nanometer reinforcing phase must have stable chemical property and efficiently strengthen efficiency, to obtain tiny, equal in alloy structure The isometric primary aluminium phase of even distribution.
Graphene is to pass through sp by single layer of carbon atom2The honeycomb two dimensional crystal material that hydridization is formed has high-intensitive, high The performances such as specific surface area, excellent thermally conductive and electric conductivity are a kind of potential aluminium alloy reinforcing materials.The study found that graphene Introducing can to aluminium alloy generate the invigoration effect of significant ground.However, currently used graphene is expensive, production process is easy Cause environmental pollution.The graphene that the present invention is prepared using shearing method can refine fine aluminium, together as novel aluminum alloy hardening agent When reinforced aluminium alloy, cost is relatively low, can be applied to the batch production of aluminium alloy.
Summary of the invention
Goal of the invention: the purpose of the present invention is to provide a kind of preparation methods of high-strength aluminum alloy, through the invention may be used To realize that complicated ingredient aluminium alloy is efficiently strengthened, the aluminium in common hardening agent and alloy is effectively solved, magnesium elements react Problem, meanwhile, reduce industrial production cost;In addition, hardening agent enhanced time prepared by the present invention is fast, the duration is long.
Technical solution: in order to reach foregoing invention purpose, a kind of preparation method for high-strength aluminum alloy that the present invention uses, Using natural graphite as raw material, polyvinylpyrrolidone, sodium taurocholate are added;It dispersing each component in deionized water, concentration is, Natural graphite 20-60mg mL-1, polyvinylpyrrolidone 2-8mg mL-1, sodium taurocholate 0.5-3mg mL-1, deionized water;Pass through Shearing method obtains graphene;
Step 1: by the natural graphite of said ratio, polyvinylpyrrolidone, sodium taurocholate is scattered in deionized water;
Step 2: mixed solvent in step 1 is placed in mixture of ice and water, is sheared, revolving speed 5000-15000r min-1, shear time 1-3h;
Step 3: the mixed solution sheared in step 2 being stood into 20-30h, so that bulky grain settles, it is molten to obtain layering Liquid;
Step 4: the layering solution that step 3 is obtained carries out centrifugal treating, and revolving speed is 3000-6000r min-1, it is centrifuged 20- 60min is to remove unpeeled graphite flake;It is freeze-dried again after above-mentioned clear liquid is filtered, obtains powdery graphite alkene;
Step 5: sintering furnace is passed through for graphene 0.1%-2wt% and the Al-1Mg powder of different ratio using sintering method Sinter high-strength aluminum alloy into.
It is described/sintering method be discharge plasma sintering.
It is described that reinforcing material of the graphene as aluminium alloy is obtained by shearing method.
The method being scattered in deionized water is ultrasonic wave added mechanical stirring.
The temperature of the sintering is 400-600 DEG C.
The utility model has the advantages that
(1) crystal grain that the novel aluminum alloy hardening agent that the present invention synthesizes is suitable for aluminium alloy is strengthened, and makes in its sintering structure Primary aluminium dendrite tiny equiax crystal is changed by original flourishing dendrite, and do not occur to strengthen decline and rotten degenerate Phenomena such as, to improve the comprehensive mechanical property of aluminium alloy.
(2) abundant raw material, cost is relatively low, and Preparation equipment is simple.
Detailed description of the invention
Fig. 1 (a) and (b) are that embodiment 1 is not added with and adds graphene commercial-purity aluminium microhardness impression comparison diagram respectively.
It is 0%, 0.1%, 0.2%, 0.5%, 1% and 2% graphene that Fig. 2 embodiment 2Al-1Mg, which mixes mass percent, Stress-strain curve diagram
Fig. 3 (a)-(f) is that embodiment 2Al-1Mg incorporation mass percent is 0%, 0.1%, 0.2%, 0.5% respectively, The alloy anode overlay film figure of 1% and 2% graphene.
It is 0%, 0.1%, 0.2% that Fig. 4 embodiment 3Mg-1Al, which mixes mass percent, the ess-strain of 0.4% graphene Curve graph.
Fig. 5 (a)-(d) is that the graphene that 2 mass fraction of embodiment is 0.5% is sintered in Al-1Mg alloy respectively Low power, high power TEM figure, diffraction spot point diagram and ultrahigh resolution TEM figure.
Fig. 6 (a)-(d) is that the graphene that 3 mass fraction of embodiment is 0.2% is sintered in Mg-1Al alloy respectively Low power, high power, super-high power TEM figure and diffraction spot point diagram.
Specific embodiment
The present invention is a kind of high-strength aluminum alloy method, and this method is broadly divided into two steps: the first step is to prepare shearing graphite Alkene adds a certain proportion of polyvinylpyrrolidone using natural graphite as raw material, and sodium taurocholate obtains graphene by shearing method. It disperses each component in deionized water, concentration is respectively natural graphite 20-60mg mL-1, polyvinylpyrrolidone 2-8mg mL-1, sodium taurocholate 0.5-3mg mL-1, deionized water 0.5-2L.By above-mentioned material ultrasonic disperse in deionized water.It will be above-mentioned mixed It closes solution to be placed in mixture of ice and water, be sheared, revolving speed is 5000-15000r min-1, shear time 1-3h.After shearing Mixed solution stands 20-30h, settles bulky grain, obtains layering solution.Centrifugal treating, revolving speed 2000- are carried out later 6000r min-1, 20-40min is centrifuged to remove unpeeled graphite flake;It is freezed again after finally above-mentioned clear liquid is filtered It is dry, obtain powdery graphite alkene.
Graphene uniform will be sheared ultrasonic disperse in ethanol, then, sequentially adds Al powder and 0.5-2% to second step Mg powder continues ultrasonic disperse and assists mechanical stir process 1-3h.Mixed solution is placed in baking oven at 40-70 DEG C dry 5- 9 hours to remove ethyl alcohol.Dry powder is finally packed into graphite jig, is placed in discharge plasma sintering furnace, in vacuum Under the conditions of be sintered, obtaining diameter and thickness is respectively 10-30mm and 5-20mm aluminum alloy sample.In order to consolidate Al-1Mg- XGNP composite material, the pressure and temperature used are respectively 40-60MPa and 400-600 DEG C, sintering time 20-60min.
Embodiment 1
Novel aluminum alloy crystal grain hardening agent is prepared according to above-mentioned steps, strengthening fine aluminium mass percent using this hardening agent is 0.1% and 0.5%.As shown in Figure 1, when being not added with hardening agent, commercial-purity aluminium smaller (metallography microscope of hardness under vickers hardness tester Impression is big under mirror);After adding hardening agent, so that the crystal grain of alloy is thinner, the effect of refined crystalline strengthening is produced, to show aluminium The hardness of alloy increases.
Embodiment 2
Novel aluminum alloy crystal grain hardening agent is prepared according to above-mentioned steps, strengthens Al-1Mg mass percent using this hardening agent It is 0.1%, 0.2%, 0.5%, 1% and 2%.As shown in Fig. 2, being the stress-strain diagram of each component part, can obviously send out Show graphene to the strengthening effect of Al-1Mg, this is because graphene in aluminium alloy, plays function served as bridge in stress, so that Tensile strength is higher.
Embodiment 3
Novel aluminum alloy crystal grain hardening agent is prepared according to above-mentioned steps, it is strong to prepare novel aluminum alloy crystal grain according to above-mentioned steps Agent, strengthening Mg-1Al mass percent using this hardening agent is 0.1%, 0.2% and 0.4%.As shown in Fig. 2, being each composition Partial stress-strain diagram, it is apparent that strengthening effect of the graphene to Mg-1Al, this is because the obstruction of graphene The movement of aluminium alloy Dislocations, macro manifestations go out intensity increase.
Fig. 1 is that commercial-purity aluminium strengthens front and back microhardness comparison in above-described embodiment 1.A is commercial-purity aluminium reinforcing in photo Preceding microhardness impression;B is microhardness impression after commercial-purity aluminium is strengthened, and the comparison of two figure impression sizes can intuitively find out shearing Reinforcing of the graphene to fine aluminium.
It is 0%, 0.1%, 0.2%, 0.5% that Fig. 2, which is that Al-1Mg mixes mass percent in above-described embodiment 2,1% He The stress-strain curve diagram of 2% graphene, it can be found that graphene is obvious to the invigoration effect effect of alloy Al-1Mg and mixes Amount is few, and when incorporation is 0.5%, effect is best.
Fig. 3 is aluminium alloy graphene-doped in above-described embodiment 2 and the anode overlay film figure for not mixing graphene, it can be seen that Graphene not only reinforced aluminium alloy, to aluminium alloy crystal grain there are also refining effect, the reason of this is also its reinforcing.
It is 0%, 0.1%, 0.2% that Fig. 4, which is that Mg-1Ag mixes mass percent in above-described embodiment 2,0.4% graphene Stress-strain curve diagram is mixing it can be found that graphene is obvious to the invigoration effect effect of alloy Mg-1Ag and incorporation is few When amount is 0.2%, effect is best.
Fig. 5 is mass fraction is 0.5% in above-described embodiment 2 the graphene sintered TEM figure in Al-1Mg alloy, It can be found that graphene drape, thickness plays good bridge in Al-1Mg alloy and make between 10-20 nanometers With.
Fig. 6 is mass fraction is 0.2% in above-described embodiment 3 the graphene sintered TEM figure in Mg-1Al alloy, It can be found that graphene is uniformly dispersed in Mg-1Al alloy, thickness is good with Mg-1Al alloy contact between 0.3-0.6 nanometers It is good, it is the main reason for improving intensity.

Claims (5)

1. a kind of preparation method of high-strength aluminum alloy, it is characterised in that: using natural graphite as raw material, add polyvinylpyrrolidine Ketone, sodium taurocholate;It disperses each component in deionized water, concentration is natural graphite 20-60mg mL-1, polyvinylpyrrolidine Ketone 2-8mg mL-1, sodium taurocholate 0.5-3mg mL-1, deionized water;Graphene is obtained by shearing method;
Step 1: by the natural graphite of said ratio, polyvinylpyrrolidone, sodium taurocholate is scattered in deionized water;
Step 2: mixed solvent in step 1 being placed in mixture of ice and water, is sheared, revolving speed is 5000-15000r min-1, Shear time 1-3h;
Step 3: the mixed solution sheared in step 2 being stood into 20-30h, so that bulky grain settles, obtains layering solution;
Step 4: the layering solution that step 2 is obtained carries out centrifugal treating, and revolving speed is 3000-6000r min-1, it is centrifuged 20- 60min is to remove unpeeled graphite flake;It is freeze-dried again after above-mentioned clear liquid is filtered, obtains powdery graphite alkene;
Step 5: by sintering furnace that the graphene 0.1%-2wt% and Al-1Mg of different ratio is powder sintered using sintering method At high-strength aluminum alloy.
2. a kind of high-strength aluminum alloy preparation method as described in claim 1, which is characterized in that the sintering method is to put Electro-plasma sintering.
3. a kind of high-strength aluminum alloy preparation method as described in claim 1, which is characterized in that described to be obtained by shearing method Graphene is as aluminium alloy reinforcing material.
4. a kind of high-strength aluminum alloy preparation method as described in claim 1, which is characterized in that described to be scattered in deionized water In method be ultrasonic wave added mechanical stirring.
5. a kind of high-strength aluminum alloy preparation method as described in claim 1, which is characterized in that the temperature of the sintering is 400-600℃。
CN201910379805.4A 2019-05-08 2019-05-08 A kind of preparation method of high-strength aluminum alloy Pending CN110042284A (en)

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CN114277273A (en) * 2021-12-20 2022-04-05 江苏拓创石墨烯科技有限公司 Preparation method of graphene/aluminum-magnesium alloy composite material

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Application publication date: 20190723