CN108396166A - A kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy - Google Patents

A kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy Download PDF

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Publication number
CN108396166A
CN108396166A CN201810310755.XA CN201810310755A CN108396166A CN 108396166 A CN108396166 A CN 108396166A CN 201810310755 A CN201810310755 A CN 201810310755A CN 108396166 A CN108396166 A CN 108396166A
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powder
dimensional
preparation
high purity
aluminum
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CN108396166B (en
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刘马宝
马栓
石蓝
李昂
周仕琪
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Xian Jiaotong 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
    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16Metallic particles coated with a non-metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

Abstract

The present invention provides a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy, aluminum-based powder and high purity graphite ball are added three-dimensional vibrating batch mixer and carry out the mixed powder of three-dimensional vibrating by (1) simultaneously;(2) three-dimensional vibrating is mixed to the powder after powder and carries out plasma discharging activation and densification sintering;The preparation of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy is completed by above step;The method of the present invention is easy to operate, mixing powder using three-dimensional vibrating makes to generate friction and shearing force between aluminum-based powder and high purity graphite ball, the single layer stripped down or few layer graphene is set to be evenly coated on aluminum-based powder while carrying out mechanical stripping to high purity graphite ball, in-situ preparation of the realization graphene on matrix powder surface, discharge plasma sintering is recycled to carry out activation and densification sintering, the aluminium alloy bulk inner prepared has continuous three-dimensional grapheme network structure, and it is firmly combined between graphene and aluminum-based powder matrix, its mechanical strength and abrasion-resistant polishing machine is set to be significantly improved.

Description

A kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy
Technical field
The invention belongs to graphene reinforced aluminum matrix composites preparing technical fields, and in particular to a kind of three-dimensional grapheme net The preparation method of network structure high-strength abrasion-proof aluminum alloy.
Background technology
Because having many advantages, such as that density is low, specific strength is high, corrosion resisting property is good, ductility is excellent and processing performance is good, aluminium and its Alloy material is applied in large quantities in fields such as aerospace, automobile ship and machine-building, is most widely used one in industry Class non-ferrous metal structural material.But with the rapid development of modern industrial technology, common aluminum alloy has been unable to meet each field pair The requirement of material property.Therefore, people begin one's study the preparation and application of aluminum matrix composite, pass through the addition in aluminum substrate The reinforced phases such as grain, fiber improve the performance of material.
Graphene is due to its excellent mechanical property and physical property, once it is found that becoming the heat of every field research Door material, there is huge application potential in various fields.Especially graphene has excellent mechanical property, is to improve again The ideal reinforced phase of condensation material intensity.Simultaneously as graphene is the substantially single of the most common kollag-graphite of structure Member possesses friction coefficient more lower than graphite, shows good lubricity, so can also be used for wear-resisting detraction material and lubrication The preparation of agent.Therefore, graphene is added in fine aluminium or alloy matrix aluminum, prepares mechanical strength and wear resistance Excellent graphene reinforced aluminum matrix composites have been subjected to the concern of more and more researchers.
However, since strong π-π active forces and hydrophobic forces makes it easily reunite to graphene between layers, and And because density contrast between alloy matrix aluminum and graphene away from larger, is the preparation of graphene and its in alloy matrix aluminum It is evenly dispersed to bring very big difficulty.Simultaneously as the wetability between graphene and alloy matrix aluminum is poor, lead to the two circle The active force that face combines is also weaker.Therefore, preparation of industrialization and its business of the aluminum matrix composite that graphene is modified are realized Using still facing huge challenge.
Discharge plasma sintering has many advantages, such as that sintering temperature is low, heating rate is fast, material density is high, can inhibit crystal grain It grows up, refiner material crystal grain, and the plasma generated in sintering process has catharsis to particle surface, interface can be improved Bond strength, and then improve the performance of material.Therefore, the aluminium base that graphene modification is prepared using discharge plasma sintering technique is multiple Condensation material can further increase the performance of material.
Invention content
To solve the problems, such as that above-mentioned graphene reinforced aluminum matrix composites preparing technical field exists, the purpose of the present invention exists In providing a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy, by aluminum-based powder and high purity graphite ball one It rises and three-dimensional vibrating batch mixer is added, mixing powder by three-dimensional vibrating makes to generate frictional force and shearing between aluminum-based powder and high purity graphite ball Power makes the single layer stripped down or few layer graphene be evenly coated at aluminium base powder while carrying out mechanical stripping to high purity graphite ball On end, the powder after powder is then mixed to three-dimensional vibrating and carries out discharge plasma activation and densification sintering, completes three-dimensional graphite The preparation of alkene network structure high-strength abrasion-proof aluminum alloy;Graphene is crossed-over to be formed continuously inside the aluminum alloy materials of preparation Three-dimensional net structure so that its mechanical strength increases substantially;Using preparation method provided by the invention, simply and effectively solve At present prepared by graphene, the interface between evenly dispersed and graphene and matrix of the graphene in aluminum-based powder matrix has Effect combine three aspect existing for significant problem, for graphene reinforced aluminum matrix composites extensive use provide it is simple and effective Method.
In order to achieve the above object, the present invention adopts the following technical scheme that:
A kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy, is as follows:
Step 1:
It is mixed in powder machine 1. weighing the aluminum-based powder that quality is m and three-dimensional vibrating being added with high purity graphite ball, utilizes three-dimensional vibrating Mixed powder machine carries out three-dimensional vibrating to the mixture of aluminum-based powder and high purity graphite ball and mixes powder, and mixing powder by three-dimensional vibrating makes aluminium base powder Frictional force and shearing force are generated between end and high purity graphite ball, make to strip down while carrying out mechanical stripping to high purity graphite ball Single layer or few layer graphene are evenly coated on aluminum-based powder;The ratio between aluminum-based powder and the initial incremental amount of high purity graphite ball are 0.1:1~10:1, vibration frequency is 5~20Hz, and it is 0.5h~50h to mix the powder time;
2. after mixed powder, high purity graphite ball is taken out, weighs the quality of high purity graphite ball, it is mixed by adjusting three-dimensional vibrating The vibration frequency of powder and mixed powder time control high purity graphite addition m0, wherein m and m0Quantitative relationship according to required cladding The requirement of graphene number of plies carries out quantitative calculating using specific surface area;
Step 2:
Three-dimensional vibrating is mixed to the powder after powder to be added in mold, is placed in activated sintering stove and is activated and be densified burning Knot, sintering temperature are 490~560 DEG C, and heating rate is 20~100 DEG C/min, and sintering pressure is 25~40MPa, soaking time For 5~30min, sintering terminates to obtain three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy;The three-dimensional grapheme net of preparation Network structure high-strength abrasion-proof aluminum alloy material internal graphene is crossed-over to form continuous three-dimensional net structure so that its machinery Intensity increases substantially.
Preferably, the aluminum-based powder is the Al alloy powder of aluminium powder or each serial trade mark.
Preferably, the high purity graphite addition design:M0=2Smn/S0, m0- high purity graphite addition g;S-aluminium base Specific Surface Area Measurement m2/g;M-aluminum-based powder addition g;N-graphene coated the number of plies;S0- single-layer graphene specific surface area m2/g。
Preferably, three-dimensional vibrating mixes powder and carries out in an atmosphere or carry out in vacuum or carried out under protective atmosphere.
Preferably, activation and densification sintering are carried out to powder using discharge plasma activated sintering method.
Preferably, plasma discharging activated sintering and densification sintering are carried out in vacuum environment or under protective atmosphere.
Three-dimensional vibrating does not add any auxiliary agent during mixing powder, to keep the activity of the graphene generated, and avoids removing Single-layer graphene or few pollution between layer graphene and coated powder interface.
Compared to the prior art, the present invention has the following advantages:
(1) present invention is made to generate between aluminum-based powder and high purity graphite ball and be rubbed using the three-dimensional vibrating blending processes of powders of no auxiliary agent Wiping and shearing force make the single layer stripped down or few layer graphene uniformly coat while carrying out mechanical stripping to high purity graphite ball On aluminum-based powder, realize that graphene in the in-situ preparation on aluminum-based powder surface, keeps the activity of the graphene generated, and avoid Single layer or few pollution between layer graphene and aluminum-based powder interface.Solves the preparation, in the base of current high activity graphene The problem of evenly dispersed difficulty.
(2) powder after powder is mixed to three-dimensional vibrating using discharge plasma sintering method and carries out activation and densification sintering, Since sintering temperature is low, sintering time is short, and the plasma generated in sintering process can play the role of purifying particle surface, So that the three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy crystal grain prepared is tiny, consistency is high and between graphene and matrix It is firmly combined with, solves the problems, such as that the interface binding power between current graphene and matrix is poor.
Specific implementation mode
Preparation method of the present invention is described further with reference to specific embodiment, but the protection of the present invention Range is not limited to this.
Embodiment 1
1) 2024 Al alloy powder 25g are weighed respectively and high purity graphite ball 20g is spare;
2) 1) that the Al alloy powder weighed up in and high purity graphite ball are placed in RM-05 type Rocking Mill three-dimensional vibratings is mixed Three-dimensional vibrating is carried out in material machine and mixes powder, and vibration frequency 30Hz, it is 60min to mix the powder time;
3) after three-dimensional vibrating mixes powder, high purity graphite ball is taken out and is weighed, quality 19.93g is added to aluminium alloy High purity graphite in powder is 0.07g.
4) three-dimensional vibrating is mixed to the taking-up of the powder after powder, is placed in SL-SPS-325S discharge plasma sintering stoves and carries out very Sky sintering, vacuum degree 3.8Pa, sintering pressure 25MPa, sintering temperature are 495 DEG C, and heating rate is 50 DEG C/min, heat preservation Time is 5min, after heat preservation, is furnace-cooled to room temperature;
5) block that will be cooled to room temperature takes out to get to three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy.
Embodiment 2
1) 6061 Al alloy powder 25g are weighed respectively and high purity graphite ball 200g is spare;
2) 1) 6061 Al alloy powders in and high purity graphite ball are placed in RM-05 type Rocking Mill three-dimensional vibrating batch mixings Three-dimensional vibrating is carried out in machine and mixes powder, and vibration frequency 5Hz, it is 90min to mix the powder time;
3) after three-dimensional vibrating mixes powder, high purity graphite ball is taken out and is weighed, quality 219.88g is added to aluminium conjunction High purity graphite in bronze end is 0.12g.
4) three-dimensional vibrating is mixed to the taking-up of the powder after powder, is placed in SL-SPS-325S discharge plasma sintering stoves and carries out very Sky sintering, vacuum degree 4.5Pa, sintering pressure 40MPa, sintering temperature be 550 DEG C, before heating rate 4min be 100 DEG C/ Min, rear 3min are 50 DEG C/min, and soaking time 3min after heat preservation, is furnace-cooled to room temperature;
5) block that will be cooled to room temperature takes out to get to three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy.

Claims (7)

1. a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy, it is characterised in that:Include the following steps:
Step 1:
It is mixed in powder machine 1. weighing the aluminum-based powder that quality is m and three-dimensional vibrating being added with high purity graphite ball, powder is mixed using three-dimensional vibrating Machine carries out three-dimensional vibrating to the mixture of aluminum-based powder and high purity graphite ball and mixes powder, by three-dimensional vibrating mix powder make aluminum-based powder with Frictional force and shearing force are generated between high purity graphite ball, make the single layer stripped down while carrying out mechanical stripping to high purity graphite ball Or few layer graphene is evenly coated on aluminum-based powder;The ratio between aluminum-based powder and the initial incremental amount of high purity graphite ball are 0.1:1 ~10:1, vibration frequency is 5~20Hz, and it is 0.5h~50h to mix the powder time;
2. after mixed powder, high purity graphite ball is taken out, the quality of high purity graphite ball is weighed, powder is mixed by adjusting three-dimensional vibrating Vibration frequency and mixed powder time control high purity graphite addition m0, wherein m and m0Quantitative relationship according to required coated graphite The requirement of the alkene number of plies carries out quantitative calculating using specific surface area;
Step 2:
Three-dimensional vibrating is mixed to the powder after powder to be added in mold, is placed in activated sintering stove and carries out activation and densification sintering, Sintering temperature is 490~560 DEG C, and heating rate is 20~100 DEG C/min, and sintering pressure is 25~40MPa, soaking time 5 ~30min, sintering terminate to obtain three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy;The three-dimensional grapheme network knot of preparation Structure high-strength abrasion-proof aluminum alloy material internal graphene is crossed-over to form continuous three-dimensional net structure so that its mechanical strength It increases substantially.
2. a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy according to claim 1, special Sign is:The aluminum-based powder is aluminium powder or Al alloy powder.
3. a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy according to claim 1, special Sign is:High purity graphite addition designs:m0=2Smn/S0, m0- high purity graphite addition g;S-aluminum-based powder specific surface area m2/g;M-aluminum-based powder addition g;N-graphene coated the number of plies;S0- single-layer graphene specific surface area m2/g。
4. a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy according to claim 1, special Sign is:Three-dimensional vibrating does not add any auxiliary agent during mixing powder, to keep the activity of the graphene of stripping, and avoids stripping Single layer or few pollution between layer graphene and Al alloy powder body interface.
5. a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy according to claim 1, special Sign is:Three-dimensional vibrating mixes powder and carries out or carried out under vacuum progress or protective atmosphere in an atmosphere.
6. a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy according to claim 1, special Sign is:Activation and densification sintering are carried out to powder using discharge plasma sintering method.
7. a kind of preparation method of three-dimensional grapheme network structure high-strength abrasion-proof aluminum alloy according to claim 6, special Sign is:Discharge plasma sintering carries out under vacuum environment or protective atmosphere.
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Cited By (4)

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CN109402601A (en) * 2018-11-09 2019-03-01 中国航空制造技术研究院 A kind of graphene microarray structure reinforced aluminum matrix composites preparation method
CN111485128A (en) * 2020-05-28 2020-08-04 山东海科创新研究院有限公司 Graphene aluminum alloy and preparation method thereof
CN111996407A (en) * 2020-08-25 2020-11-27 哈尔滨工业大学 Preparation method of graphene reinforced aluminum matrix composite material with dual-mode structure
CN112756603A (en) * 2020-12-29 2021-05-07 江苏烁源新材料科技有限公司 Aluminum-based alloy powder and preparation method and application thereof

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CN106082229A (en) * 2016-06-09 2016-11-09 大连海事大学 The composite of a kind of graphene coated nanometer silicon carbide and preparation method
CN106623890A (en) * 2016-09-14 2017-05-10 河南理工大学 Graphene/nanometer aluminum powder composite powder, graphene/aluminum base composite material containing composite powder and preparation method thereof
CN107442775A (en) * 2017-07-14 2017-12-08 成都新柯力化工科技有限公司 A kind of grapheme foam aluminum composite metal material and preparation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104711443A (en) * 2015-03-18 2015-06-17 上海和伍新材料科技有限公司 Graphene/copper composite and preparation method thereof
CN106082229A (en) * 2016-06-09 2016-11-09 大连海事大学 The composite of a kind of graphene coated nanometer silicon carbide and preparation method
CN106623890A (en) * 2016-09-14 2017-05-10 河南理工大学 Graphene/nanometer aluminum powder composite powder, graphene/aluminum base composite material containing composite powder and preparation method thereof
CN107442775A (en) * 2017-07-14 2017-12-08 成都新柯力化工科技有限公司 A kind of grapheme foam aluminum composite metal material and preparation method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109402601A (en) * 2018-11-09 2019-03-01 中国航空制造技术研究院 A kind of graphene microarray structure reinforced aluminum matrix composites preparation method
CN109402601B (en) * 2018-11-09 2021-06-08 中国航空制造技术研究院 Preparation method of graphene micro-lattice structure reinforced aluminum-based composite material
CN111485128A (en) * 2020-05-28 2020-08-04 山东海科创新研究院有限公司 Graphene aluminum alloy and preparation method thereof
CN111996407A (en) * 2020-08-25 2020-11-27 哈尔滨工业大学 Preparation method of graphene reinforced aluminum matrix composite material with dual-mode structure
CN111996407B (en) * 2020-08-25 2021-10-15 哈尔滨工业大学 Preparation method of graphene reinforced aluminum matrix composite material with dual-mode structure
CN112756603A (en) * 2020-12-29 2021-05-07 江苏烁源新材料科技有限公司 Aluminum-based alloy powder and preparation method and application thereof

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