CN107675028A - A kind of single-layer graphene/aluminium composite material and preparation method thereof - Google Patents
A kind of single-layer graphene/aluminium composite material and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- C22C1/10—Alloys containing non-metals
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- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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Abstract
The present invention relates to a kind of single-layer graphene/aluminium composite material and preparation method thereof, specific preparation method step is as follows：1) single-layer graphene powder is added in absolute ethyl alcohol, single-layer graphene dispersion liquid is obtained by ultrasonic disperse；2) aluminium powder is added in single-layer graphene dispersion liquid, then mixing and ball milling and then vacuum drying treatment obtain single-layer graphene/aluminium composite granule under argon gas protection；3) single-layer graphene/aluminium precast body is prepared by discharge plasma sintering method in single-layer graphene/aluminium composite granule；4) fine aluminium block or aluminium alloy block melting are obtained into aluminium liquid, the single-layer graphene/aluminium precast body under agitation that then heats up is dispersed with stirring in aluminium liquid, is then cast into billet, then obtain single-layer graphene/aluminium composite material through hot extrusion molding.Single-layer graphene provided by the invention/aluminium composite material composition is uniform, and intensity is high with electrical conductivity, simple production process, and industrialized production can be achieved.
Description
Technical field
The present invention relates to metal-base composites technical field, and in particular to a kind of single-layer graphene/aluminium composite material and
Its preparation method.
Background technology
Because aerial suspension span is big, overhead high voltage transmission line in addition to it there are certain requirements to the electric conductivity of leader cable,
The intensity of leader cable also there are certain requirements.Domestic and international more common overhead high voltage electricity transmission conductive wire includes copper conductor and aluminium at present
Wire.Compared with aluminum conductor, the good conductivity of copper conductor, intensity is high, but the cost of copper conductor is higher, and copper belongs to strategic money
Source, and bauxite resource enriches, widely distributed, cost is low, therefore, it is necessary to increase the exploitation of overhead high voltage power transmission aluminum conductor cable
Using.The aluminum conductor cable material of commercial Application includes fine aluminium and aluminium composite material, its electric conductivity and copper-based material ratio at present
Compared with matching is relatively low.In recent years, it is increasing with the suspension span of overhead high voltage transmission line, to the electric hardness of aluminum conductor, prolong
Stretch rate, electric conductivity etc. and propose higher requirement.
Single-layer graphene is the semiconductor that there is linear energy to be distributed for a kind of lamellar spacing 2nm or so, no energy gap, in list
In layer graphene, each carbon atom contributes the electronics of a non-bonding, and the tapered distribution of electronics, these electronics can be in crystalline substance
Moved freely in body, assign the extraordinary electric conductivity of graphene.Therefore it is graphene and aluminum metal is compound, prepare graphene aluminium base
Composite, there will be the excellent properties such as high-strength light and high heat conductance, and meet the needs of actual overhead high voltage transmission line field.
Chinese patent (CN201410280611.6) reports a kind of preparation method of graphene/aluminum composite, uses
The method of mechanical ball mill prepares graphene/aluminum composite powder, then stirs into base substrate obtained by composite powder cold moudling in aluminum melt simultaneously
Ingot casting is cast into, but the combination property of gained composite improves and unobvious, because graphene/aluminum composite powder is cold-pressed
During stirring is dissolved in aluminium liquid, floating of reuniting occurs obtained by molding base substrate for graphene film, and is not up to dispersed in aluminium
The Expected Results of matrix.
The content of the invention
The technical problems to be solved by the invention are for above shortcomings in the prior art, there is provided a kind of hardness,
Elongation percentage, single-layer graphene/aluminium composite material with good conductivity and preparation method thereof.
In order to solve the above technical problems, technical scheme provided by the invention is：
A kind of preparation method of single-layer graphene/aluminium composite material is provided, its step is as follows：
1) single-layer graphene dispersion liquid is prepared：Single-layer graphene powder is added in absolute ethyl alcohol, obtained by ultrasonic disperse
To the single-layer graphene dispersion liquid that mass concentration is 0.5~2%；
2) single-layer graphene/aluminium composite granule is prepared：Aluminium powder is added in single-layer graphene dispersion liquid obtained by step 1), its
Middle aluminium powder is 0.5~1 with single-layer graphene mass ratio：99~99.5, then argon gas protection under 6~12h of mixing and ball milling, ball milling
Rotating speed is 200~400r/min, and then vacuum drying treatment obtains single-layer graphene/aluminium composite granule；
3) Fast Sintering prepares single-layer graphene/aluminium precast body：Single-layer graphene/aluminium composite granule obtained by step 2) is led to
Single-layer graphene/aluminium precast body is prepared in overdischarge plasma agglomeration method；
4) single-layer graphene/aluminium composite material is prepared：The melting at 720~760 DEG C by fine aluminium block or aluminium alloy block
Aluminium liquid is obtained, then heats to 760~800 DEG C, single-layer graphene/aluminium precast body obtained by step 3) is mixed with aluminium liquid, 100
Stirring makes single-layer graphene/aluminium precast body fusing be scattered in aluminium liquid under~300r/min stir speed (S.S.), is then cast into circle
Ingot, then obtain single-layer graphene/aluminium composite material through hot extrusion molding.
By such scheme, step 3) aluminium powder purity >=99.9%, the mesh of mesh number >=600.
By such scheme, step 3) the discharge plasma sintering method process conditions are：Sintering temperature is 400~500
DEG C, sintering time is 5~10min, and additional axial compressive force is 5~20MPa.
By such scheme, step 4) the aluminium alloy block is Al-Mg-Si-Cu systems alloy.
By such scheme, step 4) the hot extrusion molding process conditions are：Extrusion temperature is 420~480 DEG C, extrusion ratio
For 10~14.
The present invention also provides the single-layer graphene/aluminium composite material being prepared according to the above method.
And the application of above-mentioned single-layer graphene/aluminium composite material in the cable.
The beneficial effects of the present invention are：It is molten that the present invention by ultra-sonic dispersion method prepares low concentration single-layer graphene alcohol
Liquid, disperse single-layer graphene；Then single-layer graphene/aluminium composite powder is prepared by mechanical ball mill, and utilizes plasma discharging
Fast Sintering is molded, and single-layer graphene is evenly coated at superfine aluminium power surface, then finally make stone by the method for stirring casting
Black alkene is dispersed in aluminum substrate, so as to finally improve the intensity of aluminium and electrical conductivity.Instant component reasonable mixture ratio, production
Technique is simple, security reliability is high, cost is cheap.
Brief description of the drawings
Fig. 1 is the single-layer graphene/aluminium composite powder (a) and As-extruded single-layer graphene/aluminium prepared by the embodiment of the present invention 1
The tissue of composite (b)；
Fig. 2 is the Raman spectrogram of single-layer graphene/aluminium composite powder prepared by embodiment 2.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made below in conjunction with the accompanying drawings into
One step is described in detail.
The present invention obtains low concentration graphene alcohol dispersion liquid using ultrasonic disperse single-layer graphene powder, and mechanical ball mill obtains
Single-layer graphene/aluminium composite granule, the graphite for obtaining single-layer graphene and coating then is molded by plasma discharging Fast Sintering
Alkene/aluminium precast body, block single-layer graphene/aluminium composite material is then obtained by Melt Stirring casting and hot extrusion deformation.It is multiple
The intensity of condensation material has exceeded matrix material with electrical conductivity, and plastic deformation ability does not substantially reduce.
Comparative example 1
Fine aluminium sample, preparation method are：First fine aluminium is put into smelting furnace, is warming up to 720 DEG C, round casting is cast into after fusing
Ingot, after the machining of ingot casting surface, bar is squeezed into extrusion ratio 14 at 450 DEG C, then the tensile property and conductance of test material
Rate.The alloy property index of the embodiment of the present invention and comparative example is shown in Table 1.
Comparative example 2
Aluminum alloy sample, aluminium alloy nominal composition (mass fraction, %) are：Al-0.1Si-0.2%Cu-0.05Mg-
0.3%Fe, preparation method：Raw metal powder is fully melted into stirring at 760 DEG C, 10min is incubated in 720 DEG C, makes
Improving uniformity of melt, round ingot casting is cast into after fusing, bar is squeezed into extrusion ratio 14 at 450 DEG C after the machining of ingot casting surface, then
The tensile property and electrical conductivity of test material.
Comparative example 3
The graphene/aluminum composite that graphene volume is 0.1% is prepared, preparation method is：1) by ultrasonic disperse side
It is 0.5% single-layer graphene alcohol dispersion liquid that method, which prepares mass fraction concentration,；2) graphene of mass fraction 0.5% is pressed：99.5%
Superfine aluminium power proportions, pure aluminium powder are 600 mesh, and pure aluminium powder is added in the single-layer graphene alcohol dispersion liquid in step 1),
And ball milling mixing 6h, rotational speed of ball-mill 200r/min under argon gas protection, then 50 DEG C of drying process in vacuum drying chamber, obtain
To graphene/aluminum composite powder；3) fine aluminium is melted at a temperature of 720 DEG C, and degasification removes the gred；4) in 200r/min stir speed (S.S.)
Under, the graphene/aluminum composite powder in step 2) is dispersed with stirring in 760 DEG C of aluminium liquid, cast molding ingot casting；5) step 4)
In the graphene/aluminum ingot casting for preparing be squeezed into bar under 420 DEG C of extrusion temperature, extrusion ratio 14, then test material
Tensile property and electrical conductivity.
Comparative example 4
The graphene/aluminum composite that graphene volume is 0.1% is prepared, preparation method is：1) by ultrasonic disperse side
It is 0.5% single-layer graphene alcohol dispersion liquid that method, which prepares mass fraction concentration,；2) graphene of mass fraction 0.1% is pressed：99.5%
Superfine aluminium power proportions, pure aluminium powder are 600 mesh, and pure aluminium powder is added in the single-layer graphene alcohol dispersion liquid in step 1),
And ball milling mixing 24h, rotational speed of ball-mill 300r/min under argon gas protection, then 50 DEG C of drying process in vacuum drying chamber,
Obtain 0.1% graphene/aluminum composite powder；3) by 0.1% graphene/aluminum composite powder in 600 DEG C of temperature, sintering pressure 5MPa and burning
Tie Thermocompressed sintering and forming blank under time 2h；4) the graphene/aluminum blank prepared in step 3) in extrusion temperature 420
DEG C, be squeezed into bar under extrusion ratio 14.Then the tensile property and electrical conductivity of test material.
Embodiment 1
The graphene/aluminum composite that graphene volume is 0.1% is prepared, preparation method is：1) by ultrasonic disperse side
It is 0.5% single-layer graphene alcohol dispersion liquid that method, which prepares mass fraction concentration,；2) graphene of mass fraction 0.5% is pressed：99.5%
The proportions of superfine aluminium power, fine aluminium powder purity are 99.9%, and mesh number is 600 mesh, the individual layer that pure aluminium powder is added in step 1)
In graphene alcohol dispersion liquid, and the ball milling mixing 6h under argon gas protection, rotational speed of ball-mill 200r/min, then it is being dried in vacuo
50 DEG C of drying process obtain single-layer graphene/aluminium composite granule in case；3) single-layer graphene in step 2)/aluminium composite granule is led to
Overdischarge plasma agglomeration is prepared into precast body, and sintering temperature is 400 DEG C, sintering time 5min, additional axial compressive force 5MPa；4)
Fine aluminium is melted at a temperature of 720 DEG C, and degasification removes the gred；5) under 100r/min stir speed (S.S.), by electric discharge etc. in step 3)
The precast body fusing that ion sintering is prepared is scattered in 760 DEG C of aluminium liquid, cast molding ingot casting；6) preparation in step 5)
The graphene/aluminum ingot casting of acquisition is squeezed into bar under 420 DEG C of extrusion temperature, extrusion ratio 14.Then the draftability of test material
Energy and electrical conductivity.
Single-layer graphene/aluminium composite granule (a) and step 6) as shown in Figure 1 obtained by the present embodiment step 2) are through hot extrusion
Suppress the SEM photograph of standby single-layer graphene/aluminium composite material (b), it can be seen that graphene coated is ultra-fine in composite granule
Aluminium powder surface, and after hot extrusion, graphene uniform is distributed on aluminium crystal boundary.
Embodiment 2
The graphene/aluminum composite that graphene volume is 0.2% is prepared, preparation method is：1) by ultrasonic disperse side
Method prepares the single-layer graphene alcohol dispersion liquid that mass fraction concentration is 1%；2) graphene of mass fraction 1% is pressed：99% is ultra-fine
The proportions of aluminium powder, pure aluminium powder are 600 mesh, and pure aluminium powder is added in the single-layer graphene alcohol dispersion liquid in step 1), and
Ball milling mixing 12h, rotational speed of ball-mill 400r/min under argon gas protection, then 80 DEG C of drying process obtain in vacuum drying chamber
Single-layer graphene/aluminium composite granule；3) single-layer graphene in step 2/aluminium composite granule is prepared by discharge plasma sintering
Into precast body, sintering temperature is 500 DEG C, sintering time 10min, additional axial compressive force 20MPa；4) by pure Al in 740 DEG C of temperature
Lower fusing, and degasification removes the gred；5) under 300r/min stir speed (S.S.), discharge plasma sintering in step 3) is prepared
Precast body fusing is scattered in 800 DEG C of aluminium liquid, cast molding ingot casting；6) graphene/aluminum prepared in step 5) is cast
Ingot is squeezed into bar under 450 DEG C of extrusion temperature, extrusion ratio 12.Then the tensile property and electrical conductivity of test material.
The Raman spectrum for the single-layer graphene/aluminium composite granule being illustrated in figure 2 prepared by the present embodiment step 2), in figure
2D is shown with 2G peaks contains single-layer graphene in composite powder.
Embodiment 3
Prepare the graphene/aluminum alloy composite materials that graphene volume is 0.1%, aluminium alloy Al-0.05Si-
0.03Cu-0.02Fe, composite material and preparation method thereof are：1) it is 1% individual layer to prepare mass fraction concentration by ultra-sonic dispersion method
Graphene alcohol dispersion liquid；2) graphene of mass fraction 1% is pressed：99% superfine aluminium power proportions, pure aluminium powder are 600 mesh, will
Pure aluminium powder is added in the single-layer graphene alcohol dispersion liquid in step 1), and the ball milling mixing 12h under argon gas protection, rotational speed of ball-mill
For 400r/min, then 80 DEG C of drying process obtain single-layer graphene/aluminium composite granule in vacuum drying chamber；3) step 2)
Middle single-layer graphene/aluminium composite granule is prepared into precast body by discharge plasma sintering, and sintering temperature is 500 DEG C, during sintering
Between 10min, additional axial compressive force 20MPa；4) it is that Al-0.1Si-0.07Cu-0.02Fe carries out dispensing by alloying component, dispensing exists
Melted at a temperature of 740 DEG C, and degasification removes the gred；5) under 200r/min stir speed (S.S.), by discharge plasma sintering in step 3)
The precast body fusing being prepared is scattered in 800 DEG C of aluminium liquid, cast molding ingot casting；6) the stone prepared in step 5)
Black alkene/aluminium ingot casting is squeezed into bar under 450 DEG C of extrusion temperature, extrusion ratio 12, then the tensile property and conductance of test material
Rate.
Embodiment 4
Prepare the graphene/aluminum alloy composite materials that graphene volume is 0.1%, aluminium alloy Al-0.6Mg-0.2Si-
0.16%Cu-0.03Mn, preparation method are：1) it is 2% single-layer graphene to prepare mass fraction concentration by ultra-sonic dispersion method
Alcohol dispersion liquid；2) graphene of mass fraction 0.75% is pressed：The proportions of 99.25% superfine aluminium power, pure aluminium powder are 1200 mesh,
Pure aluminium powder is added in the single-layer graphene alcohol dispersion liquid in step 1), and the ball milling mixing 8h under argon gas protection, ball milling turn
Speed is 300r/min, and then 70 DEG C of drying process obtain single-layer graphene/aluminium composite granule in vacuum drying chamber；3) step
2) single-layer graphene/aluminium composite granule is prepared into precast body by discharge plasma sintering in, and sintering temperature is 480 DEG C, sintering
Time 7min, additional axial compressive force 12MPa；4) it is that Al-1.8Mg-0.2Si-0.16%Cu-0.03Mn is matched somebody with somebody by alloying component
Material, dispensing melt at a temperature of 760 DEG C, and degasification removes the gred；5) under 150r/min stir speed (S.S.), by electric discharge etc. in step 3)
The precast body fusing that ion sintering is prepared is scattered in 800 DEG C of aluminium liquid, cast molding ingot casting；6) preparation in step 5)
The graphene/aluminum ingot casting of acquisition is squeezed into bar under 480 DEG C of extrusion temperature, extrusion ratio 13, then the draftability of test material
Energy and electrical conductivity.
Embodiment 5
Prepare the graphene/aluminum alloy composite materials that graphene volume is 0.15%, aluminium alloy Al-0.5Mg-
0.18Si-0.14%Cu-0.09Cr, preparation method are：1) it is 1% individual layer to prepare mass fraction concentration by ultra-sonic dispersion method
Graphene alcohol dispersion liquid；2) graphene of mass fraction 1% is pressed：The proportions of 99% superfine aluminium power, pure aluminium powder are 600 mesh,
Pure aluminium powder is added in the single-layer graphene alcohol dispersion liquid in step 1, and the ball milling mixing 8h under argon gas protection, rotational speed of ball-mill
For 300r/min, then 80 DEG C of drying process in vacuum drying chamber；3) single-layer graphene in step 2/aluminium composite granule is led to
Overdischarge plasma agglomeration is prepared into precast body, and sintering temperature is 450 DEG C, sintering time 10min, sintering pressure 10MPa；4) press
Alloying component is that Al-1.74Mg-0.18Si-0.14%Cu-0.09Cr carries out dispensing, and dispensing melts at a temperature of 740 DEG C, and removes
Gas removes the gred；5) under 250r/min stir speed (S.S.), the precast body fusing that discharge plasma sintering in step 3 is prepared divides
Dissipate in 780 DEG C of aluminium liquid, cast molding ingot casting；6) the graphene/aluminum ingot casting prepared in step 5 in extrusion temperature
450 DEG C, be squeezed into bar under extrusion ratio 10.Then the tensile property and electrical conductivity of test material.
The alloy property index of the embodiment of the present invention and comparative example is shown in Table 1.
Table 1
The performance parameter value of embodiment and comparative example in comparison sheet 1, it can be seen that：Composite prepared by the present invention resists
Tensile strength is apparently higher than comparative example alloy, and electrical conductivity can meet overhead high voltage transmission line also above contrast material
Performance requirement.
Claims (7)
1. a kind of preparation method of single-layer graphene/aluminium composite material, it is characterised in that step is as follows：
1) single-layer graphene dispersion liquid is prepared：Single-layer graphene powder is added in absolute ethyl alcohol, matter is obtained by ultrasonic disperse
Measure the single-layer graphene dispersion liquid that concentration is 0.5~2%；
2) single-layer graphene/aluminium composite granule is prepared：Aluminium powder is added in single-layer graphene dispersion liquid obtained by step 1), wherein aluminium
Powder is 0.5~1 with single-layer graphene mass ratio：99~99.5, then argon gas protection under 6~12h of mixing and ball milling, rotational speed of ball-mill
For 200~400r/min, then vacuum drying treatment obtains single-layer graphene/aluminium composite granule；
3) Fast Sintering prepares single-layer graphene/aluminium precast body：By single-layer graphene/aluminium composite granule obtained by step 2) by putting
Single-layer graphene/aluminium precast body is prepared in electric plasma agglomeration method；
4) single-layer graphene/aluminium composite material is prepared：By fine aluminium block or aluminium alloy block, melting obtains at 720~760 DEG C
Aluminium liquid, 760~800 DEG C are then heated to, single-layer graphene/aluminium precast body obtained by step 3) is mixed with aluminium liquid, 100~
Stirring makes single-layer graphene/aluminium precast body fusing be scattered in aluminium liquid under 300r/min stir speed (S.S.), is then cast into billet,
Again single-layer graphene/aluminium composite material is obtained through hot extrusion molding.
2. preparation method according to claim 1, it is characterised in that：Step 3) aluminium powder purity >=99.9%, mesh number
>=600 mesh.
3. preparation method according to claim 1, it is characterised in that：Step 3) the discharge plasma sintering method technique
Condition is：Sintering temperature is 400~500 DEG C, and sintering time is 5~10min, and additional axial compressive force is 5~20MPa.
4. preparation method according to claim 1, it is characterised in that：Step 4) the aluminium alloy block is Al-Mg-Si-
Cu systems alloy.
5. preparation method according to claim 1, it is characterised in that：Step 4) the hot extrusion molding process conditions are：
Extrusion temperature is 420~480 DEG C, extrusion ratio is 10~14.
A kind of 6. single-layer graphene/aluminium composite material being prepared according to any methods describeds of claim 1-5.
A kind of 7. application of single-layer graphene/aluminium composite material in the cable described in claim 6.
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| WO2022088463A1 (en) * | 2020-10-30 | 2022-05-05 | 梁海 | Sub-superconductor material and preparation method therefor |
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| CN113718125B (en) * | 2021-08-11 | 2022-04-29 | 武汉材料保护研究所有限公司 | Graphene reinforced aluminum-based composite material with high conductivity and preparation method thereof |
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