CN105112732A - Graphene/aluminium alloy composite - Google Patents
Graphene/aluminium alloy composite Download PDFInfo
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- CN105112732A CN105112732A CN201510387953.2A CN201510387953A CN105112732A CN 105112732 A CN105112732 A CN 105112732A CN 201510387953 A CN201510387953 A CN 201510387953A CN 105112732 A CN105112732 A CN 105112732A
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Abstract
The invention provides a graphene/aluminium alloy composite. The additive amount of graphene in the composite accounts for 0.1-5.0 percent by weight of the total amount of the composite. Compared with the tensile strength of aluminium alloy not added with graphene, the mechanical property and electric property of the graphene/aluminium alloy composite are improved to different extents. Owing to the existence of intermediate alloy in the graphene/aluminium alloy composite, graphene can be added into molten aluminum liquid in the form of a 'graphene/aluminium alloy' intermediate alloy, so that the dispersion uniformity of graphene in the aluminum liquid is improved to the maximum extent, and accordingly, the industrial lot production of modified graphene aluminium conductor cables can be realized by a melt-casting method. A preparation method of the composite comprises the steps of mechanical mixing, low-temperature ball milling, vacuum degassing, hot isostatic pressing, hot extrusion and the like, and is simple and controllable in process, low in production cost, suitable for industrial production and favorable in market prospect.
Description
Technical field
The present invention relates to a kind of matrix material and preparation method thereof, specifically relate to a kind of preparation method of graphene/aluminum alloy composite materials.
Background technology
Large owing to hanging span in the air, overhead high voltage transmission line, except there are certain requirements the electroconductibility of leader cable, also there are certain requirements the intensity of leader cable.Overhead high voltage electricity transmission conductive wire comparatively conventional both at home and abroad at present comprises copper conductor and aluminium conductor.Compared with aluminium conductor, the good conductivity of copper conductor, intensity is high.But the cost of copper conductor is higher, and copper belongs to strategic resource, and bauxite resource enriches, and widely distributed, cost is low.Although some places transmitting line almost more than 90% uses aluminum composite conductor, the application quantity of some local aluminum composite conductor is less than 1%.Therefore, in order to reduce costs, be necessary the Application and Development strengthening overhead high voltage power transmission aluminium conductor cable.
The aluminium conductor cable material of industrial application comprises fine aluminium and aluminum composite at present, but the matching of the intensity of the two and electroconductibility is all lower.The good conductivity of fine aluminium, but intensity is lower.Existing aluminum composite is on the basis of fine aluminium, and the alloying elements such as interpolation Mg, Si obtain, and obtained matrix material, while the raising strength of materials, but brings the reduction of electroconductibility.In recent years, along with the suspension span of overhead high voltage transmission line is increasing, the performance of aluminium conductor cable is had higher requirement.
Graphene is a kind of two-dimension nano materials be made up of carbon atom, in individual layer sheet structure (thickness is only several nanometer).Due to bi-dimensional cellular crystalline structure and the high bonding strength of its uniqueness, Graphene is the nano material that specific tenacity is high, the hardest in the world known at present, and its breaking tenacity is up to 130Gpa.(ChangguLee, XiaodingWei, JeffreyW.Kysar, etc. JamesHone) people is at " science " (Science, Vol.321, issue18, July2008,385-388) on delivered about " mensuration of single-layer graphene retractility and inherent strength " (Measurementoftheelasticpropertiesandintrinsicstrengthonm onolayergraphene).The more important thing is, material that Graphene or in the world specific conductivity are the highest (resistivity only about 10
-8Ω m), be about 100 times of copper.Therefore, utilize the high strength of Graphene and good electroconductibility, and by itself and fine aluminium or aluminum composite compound, be prepared into graphene/aluminum alloy composite materials, be expected the intensity for improving aluminium cable and electroconductibility, the mechanical property of aluminium conductor and electric property are better mated.
Based on above Discuss and analyse, need to provide a kind of preparation technology to obtain graphene/aluminum alloy composite materials, and the high quality interface realizing the dispersed and graphene/aluminum of Graphene in aluminum substrate combines.Preparation method's mainly melt casting and powder metallurgic method of aluminum current based composites.If graphene/aluminum alloy composite materials adopts the preparation of conventional melt casting, because the two density variation is large, Graphene is difficult in the dispersion of aluminium liquid inner homogeneous, and in addition, the two also high-temperature interface reaction likely occurs in material preparation process, generates Al
4c
3brittlement phase, worsens material property.And adopt powder metallurgic method, graphene nanometer sheet and aluminum composite powder then can be made at room temperature to realize Homogeneous phase mixing, then prepare Graphene by follow-up press working and strengthen aluminum-base composite block materials, the high-temperature interface that inhibit conventional melt casting to bring to greatest extent reacts.
But, fact proved, because graphene nanometer sheet and aluminum composite powder (atomization) all also exist very large difference (see table 1) in pattern, size and density etc., consistency both causing when Material cladding is very poor, even if the aluminium of nonmetallic Graphene and metal is also difficult to form good interface cohesion under powder metallurgical technique.(BARTOLUCCISF, PARAS.J, RAFIEEMA, etc. etal.) people is at " Materials science and engineering " periodical [[J] .MaterialScienceandEngineeringA, 2011,528:7933-7937.)] on disclose Graphene-aluminium nano-composition " Graphene-aluminumnanocomposites ".And for aluminum matrix composite, whether the distribution of wild phase in aluminum substrate be even, whether wild phase reunites, whether interface cohesion is tight, directly decide the quality of composite property.Therefore, how dispersed in aluminum substrate of Graphene realizes, and the high quality interface of graphene/aluminum combines and how to obtain, and is the gordian technique preparing the breakthrough of graphene/aluminum alloy composite materials needs.
The difference of table 1 graphene nanometer sheet and aluminum composite powder
The low temperature ball-milled powder metallurgical technology occurred in recent years is compared with traditional powder metallurgic method, in the dispersiveness improving wild phase and interface cohesion, have obvious advantage.The powder of wild phase and matrix phase just mixes by mechanical ball milling that conventional powder metallurgical technique adopts equably, is difficult to just form interface cohesion between powder in mechanical milling process; And the metallurgical rule of low temperature ball-milled powder introduces the inertia cryogenic medias such as liquid nitrogen (or liquid argon) in traditional Mechanical Milling Process, the milling atmosphere (low temperature and inert media) of its uniqueness makes it have plurality of advantages.Pertinent literature shows (YEJC, HEJH, SCHOENUNGJM.CryomillingforthefabricationofaparticulateB
4creinforcedAlnanocomposite:PartI.Effectsofprocessconditi onsonstructure [J] .MetallurgicalandMaterialsTransactionA, 2006,37A:3099-3109.), ceramic particle/aluminium mixed powder is through low temperature ball milling, while the nanocrystalline aluminum substrate of acquisition, achieve dispersed in aluminium of ceramic particle, also ceramic particle can be coated on aluminium inside, form high-quality interface cohesion.Therefore, can attempt realizing graphene nanometer sheet being uniformly distributed in aluminium by low temperature ball grinding technique, obtaining high-quality graphene/aluminum interface.
Fact proved, adopt low temperature ball-milled powder metallurgy method not only can realize effective interpolation of high quality mark Graphene (1.0%), but also greatly can improve the dispersiveness of Graphene in aluminium and the interface cohesion situation of graphene/aluminum.(LIJL, XIONGYC, WANGXD, YANSJ, YANGC, HEWW, CHENJZ, WANGSQ, ZHANGXY, etc. DAISL.) people has delivered the obtained nanostructure aluminium/graphene complex microtexture of cryogrinding and extension property " Microstructureandtensilepropertiesofbulknanostructuredal uminum/graphenecompositespreparedviacryomilling [J] .MaterialsScienceandEngineeringA, 2015,626:400-405) " on " Materials science and engineering " periodical.But, though adopt low temperature ball-milled powder metallurgy method can realize the improvement of the interface cohesion of the dispersed and graphene/aluminum of Graphene in aluminium, but, the method complex process, cost is higher, is not suitable for applying in the large-scale engineeringization of low value-added field (such as electrical equipment, cable etc.).
Apply for the through engineering approaches realizing graphene/aluminum alloy composite materials and adapt to the large-scale production of aluminium conductor cable product, just must adopt the method that melting is cast.But, directly join in aluminium liquid if Graphene is left intact, then can observe serious defect (pore, Graphene reunion etc.) in the ingot casting finally obtained, worsen material property.
Summary of the invention
In order to overcome the above-mentioned deficiency of prior art, the invention provides the technical scheme of the relative merits of a kind of consolidated powder metallurgy method and melt casting, prepared a kind of graphene/aluminum alloy composite materials of Graphene modified aluminium leader cable by powder metallurgy in conjunction with the method that melting is cast.In technical scheme provided by the invention: first, adopt low temperature ball grinding technique to prepare Graphene in conjunction with Hot-extrusion to be uniformly distributed in aluminum substrate and good " graphene/aluminum " matrix material extruded bars (or silk material) of interface cohesion, then it can be used as the master alloy of " graphene/aluminum ", make Graphene can join in the aluminium liquid of melting by the form of " graphene/aluminum " master alloy, farthest improve the dispersing uniformity of Graphene in aluminium liquid, thus make the suitability for industrialized production of graphitic modified aluminium leader cable become possibility.
Adopt low temperature ball grinding technique to prepare Graphene in conjunction with Hot-extrusion to be uniformly distributed in aluminum substrate (fine aluminium or aluminum composite) and good " graphene/aluminum " matrix material extruded bars (or silk material) of interface cohesion, it can be used as the master alloy of " graphene/aluminum ".
The object of the invention is to realize by the following technical solutions:
The invention provides a kind of graphene/aluminum alloy composite materials, its improvements are: described matrix material take aluminium as matrix, and Graphene addition is 0.1 ~ 5.0wt.% of described graphene/aluminum alloy composite materials.
Another kind of graphene/aluminum alloy provided by the invention, its improvements are: Graphene addition is 0.1 ~ 3.0wt.% of described graphene/aluminum alloy composite materials.
Another graphene/aluminum alloy provided by the invention, its improvements are: Graphene addition is 0.2 ~ 3.0wt.% of described graphene/aluminum alloy composite materials.
4th kind of graphene/aluminum alloy composite materials provided by the invention, its improvements are: Graphene addition is 0.4 ~ 5.0wt.% of described graphene/aluminum alloy composite materials.
5th kind of graphene/aluminum alloy composite materials provided by the invention, its improvements are: Graphene addition is 1.0 ~ 3.0wt.% of described graphene/aluminum alloy composite materials.
6th kind of graphene/aluminum alloy composite materials provided by the invention, its improvements are: Graphene addition is the 3.0wt.% of described graphene/aluminum alloy composite materials.
7th all graphene/aluminum alloy composite materials provided by the invention, its improvements are, described aluminium alloy chemical composition is by mass percentage: silicon Si:0.30 ~ 0.7, iron Fe :≤0.50, copper Cu :≤0.10, manganese Mn :≤0.03, magnesium Mg:0.35 ~ 0.8, chromium Cr :≤0.03, zinc Zn :≤0.10, boron :≤0.06; Other elements unspecified: often kind :≤0.03; Add up to :≤0.10 and aluminium Al (minimum value): surplus.
The preparation method of a kind of graphene/aluminum alloy composite materials provided by the invention, the method comprises following processing step:
(1) be the aluminium alloy atomization powder of 30 ~ 70 μm and Graphene addition by granularity be 0.1 ~ 5.0wt.% mixture of graphene/aluminum alloy composite materials amount, mix in powder machine in " V " type of rotating speed 10 ~ 30r/min and mix 24 ~ 48h;
(2) mixed powder that step (1) is obtained is put into the VC high efficient mixer mixing 10 ~ 30min of rotating speed 100 ~ 200r/min;
(3) made mixed powder, abrading-ball and stearic acid are placed in stirring ball mill, are filled with liquid nitrogen, when liquid nitrogen submergence whole abrading-ball, start ball milling, ratio of grinding media to material is 30 ~ 40: 1;
(4) low temperature ball milling is after 2 ~ 4 hours, and take out powder and be placed in protection of inert gas case, after its temperature return to room temperature, load intracavity diameter is 80 ~ 120mm, and cavity heights is in the aluminum composite jacket of 85 ~ 300mm;
(5) in 300 ~ 350 DEG C and 2.0 × 10
-3under Pa vacuum tightness, to jacket vacuum stripping 2 ~ 4h, after degasification terminates, jacket is pounded flat, heal seal;
(6) under 400 ~ 500 DEG C and 100 ~ 120MPa pressure, hot isostatic pressing is carried out to the described jacket dwell time 2 ~ 4h of sealing;
(7) jacket after hot isostatic pressing is carried out mechanical workout, remove jacket skin, obtain cylindrical press blank, diameter is 55 ~ 85mm, is highly 55 ~ 200mm;
(8) by the extrusion billet of gained at 300 ~ 350 DEG C with tonnage be the extrusion machine of 200 ~ 500t with the extrusion ratio hot extrusion of 15: 1 ~ 20: 1, obtain described graphene/aluminum alloy composite materials bar.
Another kind provided by the invention prepares the method for graphene/aluminum alloy composite materials, the method comprises following processing step: its improvements are, described V-arrangement mixing machine is the not contour mixing staving combined after cuing open into 40 degree of angles by staving, by the mixing machine of pedestal two tanks bearing center axle, in mixing tank, be provided with mandatory whipping appts; Mix in powder machine in " V " type of rotating speed 20 ~ 30r/min and mix 15 ~ 24h.
It is provided by the invention that separately another prepares the method for graphene/aluminum alloy composite materials, the method comprises following processing step: its improvements are, the described VC high efficient mixer of described step (2) is conical shell, and Tong Nei is equipped with at center stirring main shaft.
Another kind provided by the invention prepares the method for graphene/aluminum alloy composite materials, and the method comprises following processing step: its improvements are, the described abrading-ball of described step (3) is high-carbon-chromium bearing steel material abrading-ball.
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
(1) adopt low temperature ball grinding technique in conjunction with hot isostatic pressing, Hot-extrusions etc. are prepared Graphene and are uniformly distributed in alloy matrix aluminum and good " graphene/aluminum alloy " the matrix material extruded bars (or silk material) of interface cohesion, then it can be used as the master alloy of " graphene/aluminum alloy ", make Graphene can join in the aluminum alloy melt of melting by the form of " graphene/aluminum alloy " master alloy, farthest improve the dispersing uniformity of Graphene in aluminum alloy melt, thus make the suitability for industrialized production of graphitic modified aluminium alloy lead wire cable become possibility.
(2) material preparation process is simple, and it is controlled that technique is adjustable.Material preparation cost is lower, is applicable to suitability for industrialized production, good market prospects.
(3) the present invention uses V-arrangement mixing machine, VC high efficient mixer and high-carbon-chromium bearing steel material abrading-ball are conducive to Graphene being uniformly distributed and interface cohesion therebetween in alloy matrix aluminum.
Embodiment
Prepare to provided by the invention detailed, the specific description that aluminium alloy/graphene composite material does indefiniteness below by specific embodiments.
Embodiment 1:
Get business aluminium alloy atomization powder (nitrogen atomization, purity >=99%) 999 grams, Graphene (Hummer ' s legal system standby) 1g, concrete preparation process is as follows:
(1) by granularity 30 μm, the Graphene addition of pure aluminum alloy atomization powder and interpolation is that the 0.1wt.% mixture of graphene/aluminum mixture total amount mixes in powder machine in " V " type of rotating speed 10r/min and mixes 24h;
(2) mixed powder is put into the VC high efficient mixer mixing 10min of rotating speed 100r/min;
(3) mixed powder, high-carbon-chromium bearing steel material abrading-ball and stearic acid are placed in stirring ball mill simultaneously, are filled with liquid nitrogen, when liquid nitrogen submergence whole abrading-ball, start ball milling.Wherein ratio of grinding media to material is 30: 1;
(4) low temperature ball milling is after 2 hours, and take out powder and be placed in protection of inert gas case, after its temperature return to room temperature, load material is 3A21 aluminum composite, thickness is 2mm, jacket intracavity diameter is Φ 80mm, and jacket cavity heights is in the jacket of 85mm;
(5) in vacuum tightness 2.0 × 10
-3at Pa and 300 DEG C, jacket is carried out vacuum stripping 2h, after degasification terminates, jacket is pounded flat, heal seal;
(6) in 400 DEG C, under 100MPa pressure, by the jacket hot isostatic pressing heat-insulation pressure keeping 2h after sealing;
(7) jacket skin is removed in turning, and obtaining diameter is Φ 55mm, is highly the cylindrical press blank of 55mm;
(8) by this extrusion billet at 300 DEG C, with the hot extrusion under for 15: 1 extrusion ratios of the extrusion machine of tonnage 200t, obtain " graphene/aluminum " compound walking spa-cial system, i.e. graphene/aluminum matrix material.
The bar room temperature tensile intensity of the graphene/aluminum alloy composite materials taking above technique to prepare is 270MPa, and elongation is 13%, and electric conductivity (IACS) is 65%.As compared to the aluminium alloy (tensile strength 150-200MPa, elongation is 10%, IACS49.9%) not adding Graphene, the tensile strength of graphene/aluminum alloy composite materials extruded bars improves, and elongation and electric conductivity all increase.
Embodiment 2 ~ 5 is listed in the table below, and sequence of process steps wherein and term implication and embodiment 1 are with, the different numerical value of the parameter corresponding from embodiment 1 that listed is:
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; those of ordinary skill in the field are to be understood that; can modify to the specific embodiment of the present invention with reference to above-described embodiment or equivalent replacement; these do not depart from any amendment of spirit and scope of the invention or equivalent replacement, and it all should be encompassed within claims of the present invention.
Claims (7)
1. a graphene/aluminum alloy composite materials, is characterized in that: described matrix material take aluminium alloy as matrix, and Graphene addition is 0.1 ~ 5.0wt.% of described graphene/aluminum alloy composite materials.
2. a kind of graphene/aluminum alloy composite materials according to claim 1, is characterized in that: Graphene addition is 0.1 ~ 3.0wt.% of described graphene/aluminum alloy composite materials.
3. a kind of graphene/aluminum alloy composite materials according to claim 1, is characterized in that: Graphene addition is 0.2 ~ 3.0wt.% of described graphene/aluminum alloy composite materials.
4. a kind of graphene/aluminum alloy composite materials according to claim 1, is characterized in that: Graphene addition is 0.4 ~ 5.0wt.% of described graphene/aluminum alloy composite materials.
5. a kind of graphene/aluminum alloy composite materials according to claim 1, is characterized in that: Graphene addition is 1.0 ~ 3.0wt.% of described graphene/aluminum alloy composite materials.
6. a kind of graphene/aluminum alloy composite materials according to claim 1, is characterized in that: Graphene addition is the 3.0wt.% of described graphene/aluminum alloy composite materials.
7. a kind of graphene/aluminum alloy composite materials according to claim 1, it is characterized in that, described aluminium alloy chemical composition is by mass percentage: silicon Si:0.30 ~ 0.7, iron Fe :≤0.50, copper Cu :≤0.10, manganese Mn :≤0.03, magnesium Mg:0.35 ~ 0.8, chromium Cr :≤0.03, zinc Zn :≤0.10, boron :≤0.06; Other elements unspecified: often kind :≤0.03; Add up to :≤0.10 and aluminium Al (minimum value): surplus.
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Cited By (9)
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| CN105112745A (en) * | 2015-06-25 | 2015-12-02 | 中国航空工业集团公司北京航空材料研究院 | Graphene/aluminum alloy composite material |
| CN105714229A (en) * | 2016-03-21 | 2016-06-29 | 刘崴崴 | Al-Zn-Si-C hot-dip coating liquid and hot-dip coating process |
| CN106448798A (en) * | 2016-11-25 | 2017-02-22 | 广东中德电缆有限公司 | Anti-pulling cable conductor and anti-pulling cable |
| CN106695165A (en) * | 2016-12-29 | 2017-05-24 | 安徽华众焊业有限公司 | Aluminum magnesium alloy welding flux and preparation method thereof |
| CN107475581A (en) * | 2017-07-28 | 2017-12-15 | 合肥泓定科技有限公司 | Graphene oxide Al alloy composite and preparation method thereof |
| CN107538016A (en) * | 2017-07-28 | 2018-01-05 | 天津大学 | A kind of method for the interface wellability for improving graphene and fine aluminium |
| CN107858571A (en) * | 2017-11-01 | 2018-03-30 | 内蒙古汇豪镁业有限公司 | A kind of magnesium alkene alloy preparation method |
| CN108220703A (en) * | 2017-12-04 | 2018-06-29 | 江苏大学 | A kind of cast Al-Si alloy of graphene and rare earth cooperative reinforcing and preparation method thereof |
| CN108359852A (en) * | 2018-03-22 | 2018-08-03 | 沈阳理工大学 | A kind of high silica/aluminum-based composite material and preparation method of graphene enhancing |
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| CN105112745A (en) * | 2015-06-25 | 2015-12-02 | 中国航空工业集团公司北京航空材料研究院 | Graphene/aluminum alloy composite material |
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| CN105714229B (en) * | 2016-03-21 | 2018-09-07 | 刘崴崴 | A kind of hot-dip aluminizing zinc silicon-carbon plating solution and or immersion |
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| CN107475581A (en) * | 2017-07-28 | 2017-12-15 | 合肥泓定科技有限公司 | Graphene oxide Al alloy composite and preparation method thereof |
| CN107538016A (en) * | 2017-07-28 | 2018-01-05 | 天津大学 | A kind of method for the interface wellability for improving graphene and fine aluminium |
| CN107858571A (en) * | 2017-11-01 | 2018-03-30 | 内蒙古汇豪镁业有限公司 | A kind of magnesium alkene alloy preparation method |
| CN108220703A (en) * | 2017-12-04 | 2018-06-29 | 江苏大学 | A kind of cast Al-Si alloy of graphene and rare earth cooperative reinforcing and preparation method thereof |
| CN108220703B (en) * | 2017-12-04 | 2020-01-24 | 江苏大学 | Cast aluminum-silicon alloy cooperatively reinforced by graphene and rare earth and preparation method thereof |
| CN108359852A (en) * | 2018-03-22 | 2018-08-03 | 沈阳理工大学 | A kind of high silica/aluminum-based composite material and preparation method of graphene enhancing |
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Address after: 100095 Haidian District hot springs town, Beijing Village Applicant after: AECC BEIJING INSTITUTE OF AERONAUTICAL MATERIALS Address before: 100095 Haidian District hot springs town, Beijing Village Applicant before: AVIC BEIJING INSTITUTE OF AERONAUTICAL MATERIALS |
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Application publication date: 20151202 |
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