CN107142398B - A kind of Al4C3Modification on Al based composites and preparation method thereof - Google Patents
A kind of Al4C3Modification on Al based composites and preparation method thereof Download PDFInfo
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- CN107142398B CN107142398B CN201710251379.7A CN201710251379A CN107142398B CN 107142398 B CN107142398 B CN 107142398B CN 201710251379 A CN201710251379 A CN 201710251379A CN 107142398 B CN107142398 B CN 107142398B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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
Abstract
The invention discloses a kind of Al4C3Modification on Al based composites and preparation method thereof, are prepared by the following method: (1) preparing graphene oxide；(2) pure aluminium powder is then frozen in lower temperature and is kept for a period of time；(3) after mixing aluminium powder and a certain amount of graphene, ball milling is carried out to above-mentioned mixed freezing aluminium powder using high energy ball mill；(4) while carrying out ball milling after aluminium powder and the mixing of a certain amount of graphene, micro Al is added by amount4C3Powder further strengthens graphene coated aluminium powder interface cohesion；(5) graphene coated aluminium mixed-powder obtained is formed, carries out pressure maintaining under pressure and under this pressing pressure；(6) blank after cold moudling is put into the heating equipment with inert gas shielding and is sintered, finally prepare the graphene coated aluminum matrix composite of excellent combination property, convenient for its electronics industry popularization and application.
Description
Technical field
The present invention relates to a kind of Al4C3Modification on Al based composites and preparation method thereof, belong to metal material field.
Background technique
Composite material generally can be divided into three classes: polymer matrix composite (PMCs), metal-base composites (MMCs), pottery
Porcelain based composites (CMCs).Metal-base composites matrix is mainly aluminium, nickel, magnesium, titanium etc..Aluminium has on production composite material
Many features, such as light weight, density is small, plasticity is good, and aluminum-base composite technology is easily mastered, easy to process etc..In addition, aluminium base is multiple
Condensation material specific strength and specific stiffness are high, and high-temperature behavior is good, and more resistant to fatigue and wear-resisting, damping capacity is good, and thermal expansion coefficient is low.With it
His composite material is the same, it can combine specific mechanics and physical property, to meet the needs of product.Therefore, aluminum-base composite material
Material has become one of most common, most important material in metal-base composites.With the hair of automobile and aerospace field
Exhibition, especially to the specific strength of metal-base composites in space space, the adverse circumstances such as ionising radiation, specific modulus is anti-corrosion
Property, the performance requirements such as conductive and heat-conductive are higher, and traditional ceramic fibre and reinforced particulate are no longer satisfied to material property
It is required that.
Carbon nanotube has the excellent properties such as excellent mechanics, optics, electricity, high temperature resistant, corrosion-resistant, light weight, this makes
Obtaining it can be used as a kind of ideal reinforcing agent.The theory and experimental study of carbon nanotube mechanical property show carbon nanotube
Good toughness, stable structure, with minimum scale and excellent mechanical property, be ideal 1-dimention nano enhancing, toughening material.
Due to excellent mechanics and physical property, carbon nanotube is considered as one of aluminum matrix composite reinforcement of most prospect.Example
Such as it is situated between in the patent of invention of Publication No. CN103602843A, CN1546695A, CN1730688A, CN101613079A
Continued the technology of preparing of carbon nanotube enhanced aluminium-based composite material, but recent researches are found, using carbon nanotube as enhancing
Body is added in aluminum substrate and is not obvious to the reinforcing effect of aluminum matrix composite.Main problem is since carbon nanotube enhances aluminium
There are the agglomerations of carbon nanotube for based composites.
Graphene is a member belonged in numerous carbon materials, compared to other carbon materials, such as carbon nanotube, fowler
Alkene, graphite etc. have excellent physical property and mechanical property, this is related with its unique two-dimension plane structure.Graphene is
The two-dimentional monoatomic layer structure being made of sp2 hydbridized carbon atoms with six side nest lattice structure of bee.Each carbon atom with it is surrounding
Three carbon atom bondings, C-C bond distance are 1.42A.In graphene and graphite, since C-C bond angle is all 120 °, at this time
Be there is no tension, with C-C bond angle due to less than 120 ° there are compared with the fullerene of tension or carbon nanotube, graphite
The reactivity of C atom in alkene will be lower than the C atom in fullerene or carbon nanotube.
However, the two-dimensional structure of graphene makes graphene is opposite to be easier to control and be dispersed in aluminium compared with carbon nanotube
In matrix, therefore the reinforcing effect of graphene is given full play to, has prepared high performance graphene reinforced aluminum matrix composites
Cause the concern of more and more researchers.Through the literature search of existing technologies, Chinese patent CN105081310A is disclosed
A kind of method preparing graphene reinforced aluminum matrix composites: (1) graphene oxide is prepared；(2) surface of aluminium powder is modified；
(3) graphene oxide-aluminium composite powder is prepared；(4) preparation of graphene reinforced aluminum matrix composites；Graphene oxide-aluminium is multiple
It closes powder to be added in the mold that material is graphite, under conditions of argon gas is protected, pressure is 25MPa and temperature is 600 DEG C
It is sintered 1h-2h, cooled to room temperature obtains graphene reinforced aluminum matrix composites.105624446 A of Chinese patent CN is public
It has opened graphene enhancing magnesium, aluminum matrix composite and preparation method thereof: graphene is dissolved in ultrasonic disperse in ethanol in proper amount solution,
Metal powder is intermittently charged into solution immediately, while carrying out ultrasonic disperse and mechanical stirring, obtains the stone of favorable dispersibility
Black alkene/metallic particles mixed solution；Mixed solution is successively carried out to low temperature heating water bath goes solvent, vacuum drying at powder, inertia
Sustained manual is ground under atmosphere, obtains evenly dispersed graphene/metallic particles composite powder；By composite powder hot pressing it is blocking and
Hot extrusion finally obtains graphene/metal-base composites.It has also been found that, Chinese patent CN104264000A is disclosed in retrieval
A kind of high thermal conductivity aluminum matrix composite and its method for preparing powder metallurgy that graphene is modified: (1) by reinforcement particle strong acid
Solution impregnates, and is then cleaned with deionized water to neutral, drying, removes surface impurity, the reinforcement particle being activated；
(2) the reinforcement particle of activation processing is added in graphene dispersing solution, by mechanical stirring or ultrasonic disperse, in its table
Bread covers graphene nanometer sheet, prepares the modified reinforcement particle of graphene；(3) by the modified reinforcement particle of graphene with
The mixing of aluminum substrate powder prepares the modified high thermal conductivity aluminum matrix composite of graphene by green compact and sintering.
Although graphene reinforced aluminum matrix composites comprehensive comparison prepared by the prior art is excellent, graphene exists
Fail uniformly to be distributed among aluminium base, can not make to reach more effective interface cohesion between graphene and aluminum substrate.
Summary of the invention
The present invention is intended to provide a kind of Al4C3Modification on Al based composites are that a kind of chemical stability is good, interfacial bonding property
Can good graphene coated aluminium powder particle high-performance aluminum-base composite material, convenient for its electronics industry popularization and application.This
Invention additionally provides the preparation method of the composite material.
The present invention provides a kind of Al4C3Modification on Al based composites, comprise the following raw materials by weight percent:
Graphene: 0.20-0.60%, Al4C3: 0.06-0.30%, Al:99.1-99.74%.
It joined Al in the Al sill4C3, Al4C3Addition so that the interface cohesion of graphene and aluminium powder more steps up
It is close, make prepared composite material that there is superior comprehensive performance, for consistency up to 99.% or more, hardness number is 33HV or more.
The present invention provides a kind of Al4C3The preparation method of Modification on Al based composites, comprising the following steps:
(1) graphene oxide is prepared；
(2) then pure aluminium powder is freezed 2.0~5.0 hours in temperature -200~-50 DEG C；
(3) after aluminium powder and graphene oxide mixing will be freezed, high energy ball mill is utilized to carry out ball milling；In mechanical milling process,
Al is added by amount4C3Powder；
(4) graphene coated aluminium mixed-powder obtained is pressed, carries out pressure maintaining；
(5) blank after cold moudling is put into the heating equipment with inert gas shielding and is sintered.
In the above method, the process for preparing graphene oxide is as follows: first by 4.0g graphite, 6.0g K2S2O8With
6.0gP2O5It is scattered in the 30ml concentrated sulfuric acid, after oleic acid is bathed 6 hours, mixed liquor is cooled to room temperature, diluted with 2L deionized water,
Overnight, filtering, product spontaneously dry；The graphite that pretreatment obtains is added in 0 DEG C of 300ml of the concentrated sulfuric acid, 35g is added
KMnO4, ice bath, holding temperature is lower than 20 DEG C；After dissolution sufficiently, mixed liquor is reacted 4 hours under the conditions of 35 DEG C, is then used
The dilution of 1L deionized water, adds 1L deionized water, by 30% H of 100ml2O2It is added dropwise in mixed liquor, filters, gained produces
Object is washed using the HCl solution of 2L；Filtering, is washed with 2L deionized water, obtains graphene oxide after vacuum drying oven is dry.
In the above method, in step (3) mechanical milling process, ratio of grinding media to material 4.5:1, revolving speed is 310~510rpm, when ball milling
Between be 0.2~3.0 hour.After ball milling, the granularity of mixed-powder is 100-500 mesh.
In above-mentioned mechanical milling process, Al is added by amount4C3Powder further strengthens graphene coated aluminium powder interface cohesion；
In the above method, during step (4) compression moulding, pressure is 660MPa~980MPa, under this pressing pressure
Cold moudling after 0.4~60min of pressure maintaining.
In the above method, in step (5) sintering process, the blank after cold moudling is put into inert gas shielding
It is sintered in heating equipment, sintering temperature is 500~650 DEG C, and sintering time is 0.8h~6h.
Further, the inert gas is Ar gas.
The graphene is the two dimensional crystal for only one layer of atomic thickness that carbon atom is constituted, and graphene can be used common
Method such as mechanical stripping method, oxidation-reduction method, the SiC epitaxial growth method of graphite composite powder production.
The principle of the present invention: (1) aluminium powder in cryogenic freezing and is used into ball-milling method, so that of graphene coated aluminium powder
Granularity is more tiny, and the dispersibility of graphene is more preferable；(2) Al4C3Addition so that the interface cohesion of graphene and aluminium powder is more
Closely, because the oxidation process of graphite and the thermal vibration technology for peeling away graphene from graphite oxide can allow graphite
Alkenyl face is defective, and defect can expose the prismatic surface of graphene, this is created condition for graphene with reacting for aluminium；(3)
Graphene oxide can be adsorbed above aluminium flake in mechanical milling process, and graphene oxide can pass through electron exchange part in adsorption process
Reduction.
Beneficial effects of the present invention: the present invention is formed in such a way that sintering combines using normal pressure, is had simple process, is set
Standby investment is low, can fast implement aluminum substrate sintering densification；Playing graphene itself excellent mechanical performance enhancement aluminum substrate
While, additionally it is possible to enhance aluminum substrate using the processing hardening of matrix, grain refining strengthening collective effect, so that composite material
Comprehensive performance increases substantially, and has extensive prospects for commercial application, and can widely be answered in aluminium alloy cable industry
With.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Embodiment 1:
(1) pure aluminium powder -150 DEG C of temperature are frozen in first to be kept for 2.0 hours.(2) after aluminium powder and graphene being mixed,
Ball milling is carried out to above-mentioned mixed freezing aluminium powder using high energy ball mill, Ball-milling Time is 0.22 hour, and the additive amount of graphene is
0.2%, ratio of grinding media to material 4.5:1, revolving speed 420rpm make its granularity be maintained at 300 ~ 400 mesh.In above-mentioned mechanical milling process, by
The Al of amount addition 0.08%4C3Powder further strengthens graphene coated aluminium powder interface cohesion.(3) by graphene packet obtained
It covers aluminium mixed-powder to be formed, pressure is in 680MPa, and the cold moudling after pressure maintaining 10min under this pressing pressure.(4) will
Blank after cold moudling is put into the heating equipment with inert gas Ar gas shielded and is sintered, sintering temperature 500
DEG C, sintering time 1.0h.After tested, consistency is up to 99.2%, hardness number 33HV.
Embodiment 2
(1) pure aluminium powder -200 DEG C of temperature are frozen in first to be kept for 1.0 hours.(2) by aluminium powder and a certain amount of graphene
After mixing, ball milling is carried out to above-mentioned mixed freezing aluminium powder using high energy ball mill, Ball-milling Time is 0.2 hour, and graphene adds
Dosage is 0.3%, ratio of grinding media to material 4.5:1, and revolving speed 310rpm is maintained at its granularity between 100-500 mesh.(3) in aluminium powder
While with ball milling is carried out after the mixing of a certain amount of graphene, by the Al of amount addition 0.10%4C3Powder makes graphene coated aluminium powder
Interface cohesion further strengthens.(4) graphene coated aluminium mixed-powder obtained is formed, pressure between 730MPa,
And the cold moudling after pressure maintaining 20min under this pressing pressure.(5) blank after cold moudling is put into inert gas Ar
It is sintered in the heating equipment of gas shielded, sintering temperature is 520 DEG C, sintering time 1.5h.After tested, consistency reaches
99.6%, hardness number 34HV.
Embodiment 3
(1) pure aluminium powder -120 DEG C of temperature are frozen in first to be kept for 2.5 hours.(2) by aluminium powder and a certain amount of graphene
After mixing, ball milling is carried out to above-mentioned mixed freezing aluminium powder using high energy ball mill, Ball-milling Time is 0.26 hour, and graphene adds
Dosage is 0.5%, ratio of grinding media to material 4.5:1, and revolving speed 450rpm is maintained at its granularity between 100-500 mesh.(3) in aluminium powder
While with ball milling is carried out after the mixing of a certain amount of graphene, by the Al of amount addition 0.16%4C3Powder makes graphene coated aluminium powder
Interface cohesion further strengthens.(4) graphene coated aluminium mixed-powder obtained is formed, pressure between 750MPa,
And the cold moudling after pressure maintaining 30min under this pressing pressure.(5) blank after cold moudling is put into inert gas Ar
It is sintered in the heating equipment of gas shielded, sintering temperature is 550 DEG C, sintering time 2.0h.After tested, consistency reaches
99.9%, hardness number 38HV.
Embodiment 4
(1) pure aluminium powder -100 DEG C of temperature are frozen in first to be kept for 3.0 hours.(2) by aluminium powder and a certain amount of graphene
After mixing, ball milling is carried out to above-mentioned mixed freezing aluminium powder using high energy ball mill, Ball-milling Time is 3.0 hours, and graphene adds
Dosage is between 0.6%, and ratio of grinding media to material 4.5:1, revolving speed 510rpm are maintained at its granularity between 100-500 mesh.(3) exist
While carrying out ball milling after aluminium powder and the mixing of a certain amount of graphene, by the Al of amount addition 0.30%4C3Powder makes graphene coated
Aluminium powder interface cohesion further strengthens.(4) graphene coated aluminium mixed-powder obtained is formed, pressure 900MPa it
Between, and the cold moudling after pressure maintaining 40min under this pressing pressure.(5) blank after cold moudling is put into inert gas
It is sintered in the heating equipment of Ar gas shielded, sintering temperature is 650 DEG C, sintering time 6.0h.After tested, consistency
Up to 99.7%, hardness number 36HV.
Claims (5)
1. a kind of Al4C3The preparation method of Modification on Al based composites, the Al4C3Modification on Al based composites are by following weight hundred
Divide the raw material composition of ratio: graphene oxide: 0.20-0.60%, Al4C3: 0.06-0.30%, Al:99.1-99.74%；Its feature exists
In: the following steps are included:
(1) graphene oxide is prepared；
(2) then pure aluminium powder is freezed 2.0~5.0 hours in temperature -200~-50 DEG C；
(3) after aluminium powder and graphene oxide mixing will be freezed, high energy ball mill is utilized to carry out ball milling；In mechanical milling process, by amount
Add Al4C3Powder；
In mechanical milling process, ratio of grinding media to material 4.5:1, revolving speed is 310~510rpm, and Ball-milling Time is 0.2~3.0 hour；
(4) graphene coated aluminium mixed-powder obtained is pressed, carries out pressure maintaining；
During compression moulding, pressure is 660MPa~980MPa, is cold-pressed into after 0.4~60min of pressure maintaining under this pressing pressure
Type；
(5) blank after cold moudling is put into the heating equipment with inert gas shielding and is sintered；
In sintering process, the blank after cold moudling is put into the heating equipment with inert gas shielding and is sintered, burnt
Junction temperature is 500~650 DEG C, and sintering time is 0.8h~6h.
2. the Al according to claim 14C3The preparation method of Modification on Al based composites, it is characterised in that: described compound
For material density up to 99.% or more, hardness number is 33HV or more.
3. Al according to claim 14C3The preparation method of Modification on Al based composites, it is characterised in that: step (1) system
The process of standby graphene oxide are as follows: first by 4.0g graphite, 6.0g K2S2O8And 6.0gP2O5It is scattered in the 30ml concentrated sulfuric acid, oil
After acid bath 6 hours, mixed liquor is cooled to room temperature, is diluted with 2L deionized water, overnight, filtering, product spontaneously dries；It will locate in advance
The graphite that reason obtains is added in 0 DEG C of 300ml of the concentrated sulfuric acid, and 35g KMnO is added4, ice bath, holding temperature is lower than 20 DEG C；It is molten
After solution is abundant, mixed liquor is reacted 4 hours under the conditions of 35 DEG C, is then diluted using 1L deionized water, adds 1L deionization
Water, by 30% H of 100ml2O2It is added dropwise in mixed liquor, filters, products therefrom is washed using the HCl solution of 2L；Filtering is used
The washing of 2L deionized water obtains graphene oxide after vacuum drying oven is dry.
4. Al according to claim 14C3The preparation method of Modification on Al based composites, it is characterised in that: in step (3),
After ball milling, the granularity of mixed-powder is 100-500 mesh.
5. Al according to claim 14C3The preparation method of Modification on Al based composites, it is characterised in that: the indifferent gas
Body is Ar gas.
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| JP6782678B2 (en) * | 2017-10-20 | 2020-11-11 | 矢崎総業株式会社 | Aluminum-based composite material, electric wire using it, and manufacturing method of aluminum-based composite material |
| CN109338167B (en) * | 2018-10-22 | 2021-09-14 | 昆明理工大学 | Preparation method of carbon nano tube composite material |
| CN109825744B (en) * | 2019-04-09 | 2021-03-26 | 河南科技大学 | In-situ generated nano tetra-aluminum carbide reinforced aluminum-based composite material and preparation method thereof |
| CN111235436B (en) * | 2020-01-16 | 2021-02-02 | 上海交通大学 | In-situ synthesized aluminum carbide reinforced aluminum-based composite material and preparation method thereof |
| CN112974842B (en) * | 2021-02-05 | 2022-05-03 | 南京航空航天大学 | Nano multiphase reinforced aluminum matrix composite material and preparation method thereof |
| CN114855021B (en) * | 2022-05-26 | 2022-12-30 | 山东省科学院新材料研究所 | Preparation method of fullerene raw ash modified diamond/aluminum composite material |
| CN115464140B (en) * | 2022-09-27 | 2023-06-27 | 天蔚蓝电驱动科技(江苏)有限公司 | Graphene conducting bar of motor and preparation method and application thereof |
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| CN102864345B (en) * | 2012-09-06 | 2015-02-18 | 安徽和电普华电气有限公司 | Preparation method of carbon nanotube composite aluminum conductor |
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