CN107058833A - A kind of graphene composite armour material and preparation method thereof - Google Patents
A kind of graphene composite armour material and preparation method thereof Download PDFInfo
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- CN107058833A CN107058833A CN201610977815.4A CN201610977815A CN107058833A CN 107058833 A CN107058833 A CN 107058833A CN 201610977815 A CN201610977815 A CN 201610977815A CN 107058833 A CN107058833 A CN 107058833A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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Abstract
The invention provides a kind of graphene composite armour material and preparation method thereof, the composite armour material includes following components by mass percentage：Si≤0.01%；Fe≤0.005%；Cu≤0.002%；Ni≤0.005%；Al：2.5%~3.5%, Zn：0.6%~1.4%；Mn：0.1%~0.3%；Surplus is Mg and inevitable impurity.The preparation method of the composite armour material comprises the following steps：Prepare the graphene nanometer sheet organic solution that the number of plies is less than 10；Graphene coated magnesium and/or magnesium alloy powder；20~100min is mixed to the graphene after cladding/magnesium alloy powder in mixer, graphene/magnesium alloy composite armour material is produced.The method and device that the present invention is provided makes graphene spread more evenly across in metal-powder, and graphene nanometer sheet is uniformly coated on magnesium alloy powder surface, forms high quality interface and combines；Technique is simple, production efficiency is high, beneficial to extensive industrialization.
Description
Technical field
The present invention relates to a kind of preparation method of composite and device, and in particular to a kind of graphene composite armour material
And preparation method thereof.
Background technology
Graphene is a kind of two-dimension nano materials being made up of carbon atom, and in individual layer laminated structure, (thickness is only several receive
Rice).Due to its unique bi-dimensional cellular crystal structure and high bond strength, graphene is the specific strength in the world being currently known
Highest, most hard nano material, its fracture strength are up to 130Gpa.Therefore, using the high intensity of graphene, and by itself and gold
Belong to Material cladding, be prepared into graphene metallic composite, be a kind of new high-strength and high ductility metal-base composites.
The process of current graphene and metal composite mainly has two kinds：Melt casting and powder metallurgic method.Using
When melt casting prepares graphene magnesium base composite material, because both graphenes density variation is big, graphene is difficult in magnesium liquid
Portion is dispersed, in addition, the two reacts in material preparation process it is also possible to occurring high-temperature interface, deteriorates material property.Cause
This graphene magnesium base composite material is less to be prepared using melt casting.Graphene magnesium base composite material is prepared using powder metallurgic method
When, it is necessary to obtain graphene and the mixed uniformly powder of magnesium alloy first, graphite is then prepared by follow-up pressure processing
Alkene magnesium composite block material, the high-temperature interface reaction for inhibiting conventional melt casting to bring to greatest extent.Therefore, graphene
Magnesium base composite material is typically prepared using powder metallurgic method.
At present, LAV uses steel bulletproof armour always, and gunship uses titanium alloy bulletproof armour.But
It is that future war all proposes higher and higher want to the long-range delivery ability of ground force, the payload capability of gunship
Ask, this just proposes rigors to equipment weight so that the steel armor and titanium alloy armor used in the past can not be met
The need for following Weapon Development.Therefore need to provide that a kind of density is low, cost is low, the composite armour material easily produced in batches
Material.
For magnesium-based composite material, strengthen whether the distribution in magnesium matrix is uniform, strengthens and mutually whether rolls into a ball
Whether poly-, interface cohesion is close, directly decides the quality of composite property.It is small to there is size in graphene, and specific surface area is big,
It is difficult to scattered, it is easy to the problem of reuniting, therefore, how dispersed in magnesium matrix of graphene is realized, is to prepare graphite
Alkene magnesium base composite material needs the key technology broken through.When preparing graphene magnesium base composite material in particular by powder metallurgic method, such as
What obtains graphene mixed powder dispersed in magnesium alloy-powder, prepares before high-quality graphene magnesium base composite material
Carry and basis.
The content of the invention
To overcome the drawbacks described above that prior art is present, the invention provides a kind of graphene composite armour material and its system
Standby device, this method and device are improved to graphene with magnesium and/or magnesium alloy powder mixed method, are a kind of new technique
And method, graphene nanometer sheet can be uniformly coated on the surface of metal-powder, realize graphene and gold by this method and device
Belong to the uniform mixing of powder.
For achieving the above object, the technical scheme taken of the present invention is：
A kind of graphene composite armour material, it is characterised in that the magnesium alloy includes following groups by mass percentage
Point：Si≤0.01%；Fe≤0.005%；Cu≤0.002%；Ni≤0.005%；Al：2.5%~3.5%, Zn：0.6%~
1.4%；Mn：0.1%~0.3%；Surplus is Mg and inevitable impurity.
Further, the magnesium alloy includes following components by mass percentage：Zn≤0.2；Mn≤0.15；Si≤
0.01；Fe≤0.01；Cu≤0.03；Ni≤0.005；RE:2.4~4.4%；Zr:0.3~1.0%；Y:3.7~4.3%；It is remaining
Measure as Mg and inevitable impurity.
Further, the magnesium alloy includes following components by mass percentage：RE:3.0%.
Further, the magnesium alloy includes following components by mass percentage：Zr:0.7%.
Further, the magnesium alloy includes following components by mass percentage：Y:4.0%
A kind of preparation method of graphene composite armour material, it is characterised in that as follows the step of preparation：
1) the nanometer sheet organic solution that the graphene number of plies is less than 10 is prepared：In 7000~9000rpm rotating speeds, linear velocity 85~
In Double-plate high speed dispenser under 115m/s, the graphene for being scattered in organic solution is handled；
2) graphene coated magnesium and/or magnesium alloy powder：It will be walked for 60~280 μm of spray equipment with gondola water faucet mesh size
Rapid graphene nanometer sheet organic solution atomized spray 1) is on the magnesium and/or magnesium alloy powder rotated in mixer high speed；
3) 20~100min is mixed to the graphene after cladding/magnesium alloy powder in mixer, produces graphene and be combined
Armour material.
Further, in the magnesium alloy powder of graphene coated prepared by methods described, contain by mass percentage：Graphite
Alkene 0.05%~9%, magnesium and/or magnesium alloy 91%~99.95%；The particle diameter of the magnesium and/or magnesium alloy powder is 10~100
μm；The gondola water faucet mesh size is 100 μm~200 μm.
Further, the rotating speed of the Double-plate high speed dispenser is 8000rpm, and linear velocity is 100m/s；The mixer
Rotating speed be 1000rpm.
Further, the organic solvent in the nanometer sheet organic solution be include ethanol, NPM, polyethylene glycol and/or
One or more in PVP, the concentration of the organic solvent is 20%~100%.
Further, the organic solvent in the nanometer sheet organic solution is absolute ethyl alcohol.
With immediate prior art ratio, the technical scheme that the present invention is provided has the advantages that：
1st, a kind of graphene composite armour material that the present invention is provided and preparation method thereof, realizes graphene in magnesium alloy
The cladding of powder surface, is conducive to forming high-quality graphene metal interface combination in graphene metallic composite.
2nd, group is less likely to occur a kind of graphene composite armour material that the present invention is provided and preparation method thereof, graphene
It is poly-, no secondary agglomeration and scattered phenomenon is solidified again.
3rd, a kind of graphene composite armour material that the present invention is provided and preparation method thereof, without solidification, need not roll, keep away
Exempt to be formed hardened or reunite.
4th, a kind of graphene composite armour material that the present invention is provided and preparation method thereof, without vibrating and sieving, so that
Avoid the skewness of the graphene thus brought and magnesium alloy powder.
5th, a kind of graphene composite armour material that the present invention is provided and preparation method thereof, technological operation is simple, be manufactured into
This cheap, production efficiency is high.
6th, a kind of graphene composite armour material that the present invention is provided and preparation method thereof, without heating without drying,
Graphene is set preferably in magnesium alloy-powder Surface coating, i.e. Environmental Safety, to shorten manufacturing cycle again.
Brief description of the drawings
Fig. 1 is scattered at a high speed for a kind of double plate of the preparation equipment of graphene composite armour material provided in an embodiment of the present invention
Machine structural representation；
Fig. 2 is the ESEM (SEM) of graphene composite armour material made from the embodiment of the present invention；
Fig. 3 is the ESEM (SEM) of graphene composite armour material made from comparative example of the present invention.
Embodiment
With reference to specific embodiment, the present invention will be described in detail.
Embodiment 1
The present embodiment provides a kind of preparation facilities of graphene/magnesium alloy composite armour material, and it is high that the device includes double plate
Fast dispersion machine, its structure is by head (1), main motor (2), guidance panel (3), hydraulic power unit (4), high-speed main spindle (5), double
Layer dispersion impeller (6), material cylinder (7), fixing device (8), base (9) part composition, it is characterised in that：Wherein the one of head (1)
End and main motor (2) screw connection, the other end are connected by screw with hydraulic power unit (4), main motor (2) and master at a high speed
Axle (5) is connected by belt, and hydraulic power unit (4) passes through screw connection, high-speed main spindle (5) and head with guidance panel (2)
(1) screw connection is used, head (1) is fixedly connected with double-layer disperse disk (6) with the dual high accuracy of screw key pin, base (9) and liquid
Press power apparatus (4) to be connected with bearing pin, base (9) is fixedly installed on ground.Embodiment 2：
The present embodiment provides a kind of preparation method of graphene/magnesium alloy composite armour material, comprises the following steps that：
Graphene coated magnesium alloy powder includes the component of following parts by weight meter：Graphene 9%, magnesium alloy 91%.Graphite
Alkene can be prepared by Hummer ' s methods.Magnesium alloy is following components by mass percentage：Si：0.01%；Ni：0.005%；
Al：3.5%, Zn：1.4%；Mn：0.3%；Surplus is Mg and inevitable impurity；The particle diameter of magnesium alloy powder is 60 μm.
1) by graphene after ultrasonic disperse during concentration is 90% alcoholic solution, rotating speed is subsequently placed in for 9000rpm, line
Speed for 115m/s Double-plate high speed dispenser in, obtain the graphene alcoholic solution after Centrifugal dispersion, the graphene alcohol
In solution the graphene nanometer sheet number of plies below 10 layers account for whole graphene nanometer sheets more than 90%；
2) the graphene nanometer sheet organic solution is passed under pressure through to the spray equipment mist of 60 μm of gondola water faucet mesh size
Droplet is melted into, is equably spilt to the magnesium and/or magnesium alloy powder rotated in 1200rpm high efficient mixer；Wherein it is possible to
Solvent flashing is reclaimed by condensate recycling device, recycling and reuse can also be realized by other means, does not do specific here
Limit.
3) after the completion of graphene alcoholic solution all sprays, high efficient mixer is kept to continue to run with 20min；
4) powder of well mixed graphene coated magnesium alloy is taken out from high efficient mixer.
Embodiment 3：
Graphene coated magnesium alloy powder includes the component of following parts by weight meter：Graphene 5%, magnesium alloy 95%.Magnesium is closed
Gold is following components by mass percentage：Fe：0.004%；Cu：0.001%；Ni：0.002%；Al：2.5%, Zn：
0.6%；Mn：0.1%；Surplus is Mg and inevitable impurity.The particle diameter of magnesium alloy powder is 100 μm.
1) by graphene after ultrasonic disperse during concentration is 95% alcoholic solution, rotating speed is subsequently placed in for 8000rpm, line
Speed for 100m/s Double-plate high speed dispenser in, obtain the graphene alcoholic solution after Centrifugal dispersion, the graphene alcohol
In solution the graphene nanometer sheet number of plies below 10 layers account for whole graphene nanometer sheets more than 90%；
2) the graphene nanometer sheet organic solution is passed under pressure through to the spray equipment mist of 100 μm of gondola water faucet mesh size
Droplet is melted into, is equably spilt to the magnesium and/or magnesium alloy powder rotated in 1000rpm high efficient mixer；
3) after the completion of graphene alcoholic solution all sprays, high efficient mixer is kept to continue to run with 60min；
4) powder of well mixed graphene coated magnesium alloy is taken out from the high efficient mixer.
Embodiment 4
Graphene coated magnesium alloy powder includes the component of following parts by weight meter：Graphene 0.05%, magnesium alloy
99.95%.Magnesium alloy is following components by mass percentage：Si：0.005%；Fe：0.005%；Cu：0.002%；Al：
2.9%, Zn：1.2%；Mn：0.2%；Surplus is Mg and inevitable impurity.The particle diameter of magnesium alloy powder is 10 μm.
1) by graphene in organic solvent (concentration be 40% alcoholic solution) after ultrasonic disperse, being subsequently placed in rotating speed is
7000rpm, linear velocity for 85m/s Double-plate high speed dispenser in, obtain the graphene nanometer sheet organic solution after Centrifugal dispersion,
The graphene nanometer sheet number of plies accounts for whole graphene nanometer sheets below 10 layers in the graphene nanometer sheet organic solution
More than 90%；
2) the graphene nanometer sheet organic solution is passed under pressure through to the spray equipment mist of 60 μm of gondola water faucet mesh size
Droplet is melted into, is equably spilt to the magnesium and/or magnesium alloy powder rotated in 1100rpm high efficient mixer；
3) after the completion of the graphene nanometer sheet organic solution is all sprayed, the high efficient mixer is kept to continue to run with
100min；
4) powder of well mixed graphene coated magnesium alloy is taken out from the high efficient mixer.
Embodiment 5
Graphene coated magnesium alloy powder includes the component of following parts by weight meter：Graphene 9%, magnesium alloy 91%.Magnesium is closed
Gold is following components by mass percentage：Zn：0.2；Mn：0.15；Cu：0.02；Ni：0.003；RE:2.4%；Zr:0.3%；
Y:3.7%；Surplus is Mg and inevitable impurity.The particle diameter of magnesium alloy powder is 50 μm.
1) graphene after ultrasonic disperse, is subsequently placed in and turned in organic solvent (concentration is 20% polyglycol solution)
Speed be 8000rpm, linear velocity for 100m/s Double-plate high speed dispenser in, obtain the graphene nanometer sheet after Centrifugal dispersion organic
The graphene nanometer sheet number of plies accounts for whole graphene nanometer sheets below 10 layers in solution, the graphene nanometer sheet organic solution
More than 90%；
2) the graphene nanometer sheet organic solution is passed under pressure through to the spray equipment mist of 280 μm of gondola water faucet mesh size
Droplet is melted into, is equably spilt to the magnesium and/or magnesium alloy powder rotated in 1000rpm high efficient mixer；
3) after the completion of the graphene nanometer sheet organic solution is all sprayed, the high efficient mixer is kept to continue to run with
20min；
4) powder of well mixed graphene coated magnesium alloy is taken out from the high efficient mixer.
Embodiment 6
Graphene coated magnesium alloy powder includes the component of following parts by weight meter：Graphene 0.05%, magnesium alloy
99.95%.Magnesium alloy is following component Zn by mass percentage：0.1；Si：0.01；Fe：0.01；Cu：0.03；RE:
4.4%；Zr:1.0%；Surplus is Mg and inevitable impurity.The particle diameter of magnesium alloy powder is 10 μm.
1) by graphene in organic solvent (concentration be 40% alcoholic solution) after ultrasonic disperse, being subsequently placed in rotating speed is
7000rpm, linear velocity for 85m/s Double-plate high speed dispenser in, obtain the graphene nanometer sheet organic solution after Centrifugal dispersion,
The graphene nanometer sheet number of plies accounts for whole graphene nanometer sheets below 10 layers in the graphene nanometer sheet organic solution
More than 90%；
2) the graphene nanometer sheet organic solution is passed under pressure through to the spray equipment mist of 200 μm of gondola water faucet mesh size
Droplet is melted into, is equably spilt to the magnesium and/or magnesium alloy powder rotated in 800rpm high efficient mixer；
3) after the completion of the graphene nanometer sheet organic solution is all sprayed, the high efficient mixer is kept to continue to run with
30min；
4) powder of well mixed graphene coated magnesium alloy is taken out from the high efficient mixer.
Embodiment 7
Graphene coated magnesium alloy powder includes the component of following parts by weight meter：Graphene 5%, magnesium alloy 99.5%.Magnesium
Alloy is following component Mn by mass percentage：0.1；Si：0.005；Fe：0.005；Ni：0.005；Y：4.3%；Surplus is
Mg and inevitable impurity.The particle diameter of magnesium alloy powder is 100 μm.
1) graphene after ultrasonic disperse, is subsequently placed in rotating speed in organic solvent (concentration is 100% alcoholic solution)
For 7000rpm, linear velocity is in 85m/s Double-plate high speed dispenser, obtains the graphene nanometer sheet after Centrifugal dispersion organic molten
The graphene nanometer sheet number of plies accounts for whole graphene nanometer sheets below 10 layers in liquid, the graphene nanometer sheet organic solution
More than 90%；
2) the graphene nanometer sheet organic solution is passed under pressure through to the spray equipment mist of 100 μm of gondola water faucet mesh size
Droplet is melted into, is equably spilt to the magnesium and/or magnesium alloy powder rotated in 800rpm high efficient mixer；
3) after the completion of the graphene nanometer sheet organic solution is all sprayed, the high efficient mixer is kept to continue to run with
100min；
4) powder of well mixed graphene coated magnesium alloy is taken out from the high efficient mixer.
Comparative example 1
1) magnesium alloy that granularity is 40 μm is atomized powder and graphene (addition is graphene/composite material of magnesium alloy
0.1~5.0wt.% of amount), 24~48h is mixed in 10~30r/min of rotating speed mixed powder machine；
2) by mixed powder made from step (1) be put into 100~200r/min of rotating speed mixer mixing 10~
30min；
3) made mixed powder, abrading-ball and stearic acid are placed in stirring ball mill, are filled with liquid nitrogen, treat that liquid nitrogen submergence is complete
Start ball milling during portion's abrading-ball, ratio of grinding media to material is 40: 1；
4) low temperature ball milling takes out powder and is placed in inert gas shielding case, treat that its temperature is recovered to room after 2~4 hours
Taken out after temperature.
As can be seen that the uncoated magnesium of graphene is closed in the mixed powder that the method that comparative example is provided is obtained from Fig. 2~3
Gold, and the mixed powder that method provided in an embodiment of the present invention is obtained, the surface for being coated on magnesium alloy of graphene completely, with base
Body forms good interface cohesion.
Method and device provided in an embodiment of the present invention, realizes cladding of the graphene on magnesium alloy-powder surface, favorably
Combined in forming high-quality graphene metal interface in graphene metallic composite；Graphene is less likely to occur to reunite,
Without secondary agglomeration and again scattered phenomenon is solidified；Without solidification, it need not roll, it is to avoid formed hardened or reunited；Without vibration
And screening, so as to avoid the skewness of the graphene thus brought and magnesium alloy powder；Technological operation is simple, manufacturing cost
Cheap, production efficiency is high；Without heating without drying, make graphene preferably in magnesium alloy-powder Surface coating, i.e. environmental protection
Safety, shortens manufacturing cycle again.
Finally it should be noted that：The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, to the greatest extent
The present invention is described in detail with reference to above-described embodiment for pipe, those of ordinary skills in the art should understand that：Still
The embodiment of the present invention can be modified or equivalent substitution, and without departing from any of spirit and scope of the invention
Modification or equivalent substitution, it all should cover among scope of the presently claimed invention.
Claims (10)
1. a kind of graphene composite armour material, it is characterised in that the graphene composite armour material includes pressing quality percentage
Following components of ratio：Si≤0.01%；Fe≤0.005%；Cu≤0.002%；Ni≤0.005%；Al：2.5%~3.5%,
Zn：0.6%~1.4%；Mn：0.1%~0.3%；Surplus is Mg and inevitable impurity.
2. a kind of graphene composite armour material according to claim 1, it is characterised in that the graphene composite armour
Material includes following components by mass percentage：Zn≤0.2；Mn≤0.15；Si≤0.01；Fe≤0.01；Cu≤0.03；Ni
≤0.005；RE:2.4~4.4%；Zr:0.3~1.0%；Y:3.7~4.3%；Surplus is Mg and inevitable impurity.
3. a kind of graphene composite armour material according to claim 1, it is characterised in that the graphene composite armour
Material includes following components by mass percentage：RE:3.0%.
4. a kind of graphene composite armour material according to claim 1, it is characterised in that the graphene composite armour
Material includes following components by mass percentage：Zr:0.7%.
5. a kind of graphene composite armour material according to claim 1, it is characterised in that the graphene composite armour
Material includes following components by mass percentage：Y:4.0%.
6. a kind of preparation method of graphene composite armour material, it is characterised in that as follows the step of preparation：
1) the nanometer sheet organic solution that the graphene number of plies is less than 10 is prepared：In 7000~9000rpm rotating speeds, linear velocity 85~
In Double-plate high speed dispenser under 115m/s, the graphene for being scattered in organic solution is handled；
2) graphene coated magnesium and/or magnesium alloy powder：It is 60~280 μm of spray equipment by step 1 with gondola water faucet mesh size)
Graphene nanometer sheet organic solution atomized spray on the magnesium and/or magnesium alloy powder rotated in mixer high speed；
3) 20~100min is mixed to the graphene after cladding/magnesium alloy powder in mixer, produces graphene composite armour
Material.
7. a kind of preparation method of graphene composite armour material according to claim 6, it is characterised in that methods described
In the magnesium alloy powder of the graphene coated of preparation, contain by mass percentage：Graphene 0.05%~9%, magnesium and/or magnesium are closed
Gold 91%~99.95%；The particle diameter of the magnesium and/or magnesium alloy powder is 10~100 μm；The gondola water faucet mesh size is 100 μ
M~200 μm.
8. a kind of preparation method of graphene composite armour material according to claim 6, it is characterised in that the double plate
The rotating speed of high speed dispersor is 8000rpm, and linear velocity is 100m/s；The rotating speed of the mixer is 1000rpm.
9. a kind of preparation method of graphene composite armour material according to claim 6, it is characterised in that the nanometer
Organic solvent in piece organic solution is to include the one or more in ethanol, NPM, polyethylene glycol and/or PVP, described organic
The concentration of solvent is 20%~100%.
10. the preparation method of a kind of graphene composite armour material according to claim 6, it is characterised in that described to receive
Organic solvent in rice piece organic solution is absolute ethyl alcohol.
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| CN110681869A (en) * | 2019-10-15 | 2020-01-14 | 上海交通大学 | Method for preparing high-strength and high-toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology |
| CN111254332A (en) * | 2018-11-30 | 2020-06-09 | 华孚精密科技(马鞍山)有限公司 | High-thermal-conductivity magnesium alloy material and product thereof |
| CN115156525A (en) * | 2022-06-22 | 2022-10-11 | 广东省科学院新材料研究所 | Active modification spherical magnesium alloy powder based on electrostatic self-assembly and preparation method and application thereof |
| CN115948674A (en) * | 2023-03-14 | 2023-04-11 | 淄博国创中心先进车用材料技术创新中心 | Preparation method of graphene modified magnesium alloy hub |
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