CN106629680A - Preparation method of graphene metal composite material - Google Patents
Preparation method of graphene metal composite material Download PDFInfo
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- CN106629680A CN106629680A CN201611224266.XA CN201611224266A CN106629680A CN 106629680 A CN106629680 A CN 106629680A CN 201611224266 A CN201611224266 A CN 201611224266A CN 106629680 A CN106629680 A CN 106629680A
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
Abstract
The invention discloses a preparation method of a graphene metal composite material. The preparation method comprises following steps: a graphene derivative is dispersed in a solvent, and is mixed with particles so as to obtain a mixed material; the mixed material is dried, and is delivered through a microwave heating at a preset atmosphere at a preset speed for heating so as to convert the graphene derivative in the mixture into graphene, and a mixture of graphene and the particles is obtained via cooling; the mixture and metal are subjected to fusion, high temperature sintering, and extrusion moulding for recombination so as to obtain a graphene-metal compound. The preparation method is capable of solving problems that dispersing of graphene is difficult to realize, and the performance of the graphene derivative is poor, mass production of the graphene-metal compound can be realized conveniently and rapidly, and further development and applications of graphene and metal materials are realized.
Description
Technical field
The invention belongs to Material Field, is related to a kind of Graphene metallic composite easy in particular with Graphene derivative
In dispersion and have Microwave Absorption Properties, first Graphene derivative is formulated as into solution, then Graphene derivative solution with
In metal material can homodisperse particulate solid be mixed to form mixture, subsequent mixture is dried and is simultaneously existed with setting speed
Carry out microwave heating treatment the Graphene derivative in mixture is converted into graphite by heating using microwave area under setting atmosphere
Alkene, then by the mixture of Graphene and particulate solid and metal be combined and formed Graphene being capable of scattered stone very well
Black alkene-metal composite.
Background technology
Used as a kind of two-dimensional material, it has excellent mechanical property (Young's modulus is up to 1.0TPa), electricity to Graphene
(electron mobility is up to 10 to property6cm2.v-1s-1), (thermal conductivity coefficient is up to 5000w.m to thermal property-1.k-1), optical property
(visible absorption of single-layer graphene only have 2.3% and excellent locked mode characteristic), the theoretical specific surface area (2630m of super large2.g-1) and monolithic Rotating fields give the chemistry and electro-chemical activity of its uniqueness so that Graphene is in electronics, information, the energy, material and life
Thing medicine and other fields have great application prospect.The application significant proportion of Graphene is presented by the form of compound.For
This global scientist and enterprise scientific research personnel have carried out a large amount of explorations in terms of graphene complex and have obtained remarkable progress.So
And also there is conflict graphene powder i.e. of good performance at present and be easy to reunite and do not have in graphene complex research and development aspect
There is good solvent therefore, it is difficult to forming finely dispersed compound；Although and Graphene derivative can by good solvent dispersion and can
To form finely dispersed compound, but because the performance of Graphene derivative then has a long way to go compared to Graphene, so
Graphene derivative compound can not give full play to the excellent properties of Graphene.For metallic composite, current people
Still in the technology for exploring the compound rear performance improvement of method and Graphene derivative for improving the raising of graphene powder dispersive property,
But effect need to be improved.For example it is attempted to for graphene powder and metal dust to improve graphene powder by ball grinding technique
Dispersive property in metal dust, is subsequently further combined and is formed Graphene-metallic composite.But ball milling
Low yield makes it be difficult to large-scale application.And the property of the compound of Graphene derivative and metal restricted Graphene derivative all the time
Can and make slow progress.So in the urgent need to exploitation can by Graphene in metal material homodisperse technology and improve at present
The present situation of Graphene-metallic composite.Propose first in the world to be first dispersed in Graphene derivative for this application
Solution is formed in solvent, then will in metal material can homodisperse particulate solid mix with Graphene derivative solution
Conjunction forms homogeneous mixture, is being set in mixture using Graphene derivative Microwave Absorption Properties after subsequently mixture is dried
Heated for the Graphene derivative in mixture to be converted into stone by heating using microwave area with setting speed under atmosphere
Black alkene, subsequent Graphene leaves heating using microwave area and is cooled down with the mixture of particulate solid, then Graphene and solid-state
The mixture of particulate matter homodisperse characteristic can be assisted and consolidated using particulate solid with metal material in metal material
The Graphene that state particulate matter is mutually mixed is combined and is obtained Graphene homodisperse graphite in metal material with metal
Alkene-metallic composite.The method of the present invention fully utilizes Graphene derivative solution and can uniformly mix with particulate solid
The characteristics of the characteristics of conjunction, particulate solid can be dispersed in metal material, Graphene derivative tool Microwave Absorption Properties
Heating can be converted into Graphene under setting atmosphere with microwave tool fast selective heat characteristic, Graphene derivative
Feature and mixture can be uneven with precise control microwave heating time and improvement heating by heating using microwave area with setting speed
The characteristics of, Graphene-metallic composite is prepared such that it is able to convenient, fast, low energy consumption ground batch, it is expected to as Graphene-gold
The further genralrlization development of category composite and application are made contributions.
The content of the invention
Technical problem：It is an object of the invention to provide a kind of preparation method of Graphene metallic composite, particularly profit
With Graphene derivative can with homodisperse particulate solid can be uniformly mixed to form mixture in metal material, so
Rapidly and efficiently added by microwave under setting speed with mixture using Graphene derivative microwave absorbing property, heating using microwave afterwards
Hot-zone can be with the heating in the case where atmosphere is set with Graphene derivative the characteristics of precise control heat time, improvement heating inequality
The mixture of Graphene derivative and particulate solid is converted into Graphene and solid-state by the characteristics of being converted into Graphene
The mixture of grain thing, the fine dispersion performance followed by particulate solid in metal material is assisted and its mixed uniformly stone
Black alkene it is dispersed in metal material and obtain Graphene-metallic composite.The method is convenient, fast, low energy consumption, can
Batch prepares Graphene-metallic composite, hence helps to Graphene-metallic composite preferably service society.
Technical scheme：
A kind of preparation method of Graphene metallic composite of the present invention is：Graphene derivative solution is prepared first,
Then Graphene derivative solution and particulate solid are carried out being mixed to form mixture, is subsequently dried, then in setting
The mixture being dried under atmosphere is heated by heating using microwave area with setting speed and is derived Graphene in mixture
Thing is converted into Graphene, and subsequent Graphene leaves heating using microwave area and cooled down with the mixture of particulate solid, then will
Mixture is combined as reinforcement and metal material and is obtained Graphene-metallic composite.
Wherein：
The Graphene derivative refers to that the oxide of Graphene includes graphene oxide and redox graphene and stone
Black alkene edge derivative.
The particulate solid can be dispersed in metal material, including powder and chopped fiber.
The graphene carbon content is more than 90%.
The Graphene derivative is converted into Graphene and refers to that Graphene derivative absorbs microwave and heats up and in setting gas
Cause the Graphene for aoxidizing to be reduced under atmosphere and be converted into Graphene, and then there is off-clip edge functional group in graphene edge derivative
React and be converted into Graphene.
The setting atmosphere refers to inert atmosphere, reducing atmosphere or vacuum state.Inert atmosphere refer to gas not with
Gas such as nitrogen, helium, the argon gas of Graphene derivative reaction；Reducing atmosphere is referred in gas containing being capable of reduced graphene
The gas of derivative such as hydrogen, alcohols, alkanes gas；Vacuum state refer to air pressure less than 4KPa (relative degree of vacuum less than-
20KPa)。
The mixture is with setting speed by heating using microwave area according to the heating using microwave area size Control heat time.
The mixture leaves heating using microwave area and cooled referring to cools down mixture by cold atmosphere.
The microwave heating treatment can repeat that repeatedly mixture can be processed by microwave high-temperature.
The mixture and metal carry out it is compound refer to be combined by mixture and motlten metal, mixture and metal
Particle is combined after being well mixed by high temperature sintering, mixture is answered after being well mixed with metallic particles by extrusion molding
Close.
Beneficial effect：The present invention compared with prior art, with advantages below：
The application comprehensively utilizes first Graphene derivative solution can be with the mixed uniformly feature of particulate solid, solid-state
The characteristics of particulate matter can be dispersed in metal material, Graphene derivative tool Microwave Absorption Properties and the quick choosing of microwave tool
Selecting property heat characteristic, Graphene derivative are heating the characteristics of being converted into Graphene and mixture under setting atmosphere
The characteristics of can heating uneven with precise control microwave heating time and improvement by heating using microwave area with setting speed, prepares first
Graphene with can in metal material homodisperse particulate solid homogeneous mixture, then nationality by particulate solid assist
Help Graphene dispersed in metal material.This method is not only convenient, fast, low energy consumption, and can in batches prepare graphite
Alkene-metallic composite, hence helps to Graphene-metallic composite preferably service society and its further development and answers
With making contributions.
Specific embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment one：
Graphene oxide powder and redox graphene powder are prepared first.30 grams of graphite mixing 15g sodium nitrate and 750
The milliliter concentrated sulfuric acid.Mixture is cooled in ice bath 0 degree Celsius, and is stirred after 2h, be slowly added to 90 grams of potassium permanganate, kept
Mixture temperature is less than 5 degrees Celsius in mixed process.The mixture is stirred for a hour, and is heated to by removing ice bath
Room temperature.Add 1 liter of distilled water in mixture and the temperature in oil bath increases to 90 degrees Celsius.Add 300 milliliters of water in addition, and
It is stirred for one and a half hours.The color of mixture becomes brown.Mixture and then 300 milliliters of hydrogen peroxide with 30% and 30 liters
Hot water treatment and dilution.The mixture further with excessive water washing, until the pH value of filtrate is almost neutral so as to obtain
Obtain graphene oxide.Then graphene oxide is disperseed and is reduced 12 hours at 80 degrees Celsius with hydrazine hydrate in water.Oxygen reduction
Graphite alkene is formed with black precipitate, is collected by filtration with 0.45 μm of PTFE film, and is rinsed with substantial amounts of water.Product by methyl alcohol,
Tetrahydrofuran (THF) and water are further purified with soxhlet extraction.Finally, the redox graphene for being obtained is at 0.05 millimeter
Subzero 120 degrees Celsius freeze under Hg vacuum environment.Subsequently deionized water prepares the redox graphene of 1 mg/ml
The aqueous solution.
Secondly pure copper powder is obtained, then redox graphene Graphene is scaled into and with pure copper powder and Graphene quality
Than 10:1 ratio is added in the redox graphene aqueous solution of 1 mg/ml and is uniformly mixed.Then filter,
It is dried and obtains the mixture that redox graphene is well mixed with pure copper powder.Subsequently mixture nationality is protected by conveyer belt in argon gas
Power is passed through as 1000 watts with the speed of 0.1 meter per second under shield, a diameter of 20 centimetres of heating using microwave area carries out heating using microwave about 2
Second, subsequently enter and cooled down by the room temperature atmosphere cooled region of circulating cooling water management.Mixture repeats microwave heating treatment 3
Redox graphene is converted into Graphene in secondary rear mixture.The carbon content of Graphene is more than 90% wherein in mixture.With
Afterwards by Graphene fine copper powder mixture with its with molten copper with mass ratio 1:50 ratio is added in the copper water of melting and mixes
Uniformly, subsequently cooling can obtain Graphene-carbon/carbon-copper composite material that graphene uniform is dispersed in metallic copper.
Embodiment two：
By the Graphene in embodiment one-fine copper powder mixture with mass ratio 1:After 10 ratio uniformly mixes with brass powder
Sintering in 5 kilowatts of sintering furnaces is added to obtain Graphene-brass wire composite.
Embodiment three：
By the Graphene in embodiment one-fine copper powder mixture with mass ratio 1:20 ratio uniformly mixes logical with brass powder
Cross extrusion forming technology and be prepared as Graphene-brass wire composite.
Example IV：
Nickel powder is obtained first, then graphene oxide is scaled into Graphene and with nickel powder and Graphene mass ratio 15:1
Ratio is added in the aqueous solution of 10 mg/mls and is uniformly mixed.Then filter, be dried acquisition graphene oxide and nickel
The mixture that powder is well mixed.Subsequent is 55 in nitrogen and hydrogen ratio by conveyer belt by mixture nationality:Under 1 atmosphere protection with
It is 1000 watts that the speed of 0.01 meter per second is entered by the power that hot-air temperature control is 250 degrees Celsius, a diameter of 20 centimetres of micro-wave oven
The thermal treatment zone carries out heating using microwave about 10 seconds, subsequently enters and is cooled down by the room temperature atmosphere cooled region of circulating cooling water management.
Mixture repeats after microwave heating treatment 10 times that graphene oxide is converted into Graphene in mixture.Wherein Graphene in mixture
Carbon content be more than 90%.Subsequently by Graphene nickel powder mixture with its with fusion electrolysis aluminium with mass ratio 1:30 ratio addition
To in the aluminium water of melting and it is well mixed, subsequently cooling can obtain Graphene-aluminium that graphene uniform is dispersed in metallic aluminium
Composite.
Embodiment five：
Steel chip is obtained first, then graphene oxide is scaled into Graphene and with steel chip and Graphene mass ratio
10:1 ratio is added in the aqueous solution of 8 mg/mls and is uniformly mixed.Then filter, be dried acquisition graphite oxide
The mixture that alkene is well mixed with steel chip.Subsequently mixture 95 degrees Celsius of process in hydrazine hydrate steam are mixed for 24 hours with reducing
Graphene oxide in compound.It is by power with the speed of 0.1 meter per second under helium protection by conveyer belt by mixture nationality subsequently
1000 watts, a diameter of 20 centimetres of heating using microwave area carries out heating using microwave about 2 seconds, subsequently enters by the room of circulating cooling water management
Wet atmosphere cooled region is cooled down.Mixture repeats redox graphene conversion in mixture after microwave heating treatment 5 times
For Graphene.The carbon content of Graphene is more than 90% wherein in mixture.Subsequently by Graphene steel crumb mixture with its with it is molten
Melt molten steel with mass ratio 1:100 ratio is added in the molten steel of melting and is well mixed, and subsequently cooling can obtain Graphene
Graphene-the steel composite material being dispersed in metallic steel.
Embodiment six：
The graphene platelet of edge carboxylated is prepared first.5 grams of graphite and 100 grams of dry ice are added containing 1000 grams of diameter
In the stainless steel capsule of 5 millimeters of stainless steel balls.Container is sealed and is fixed on planetary ball mill (F-P4000), and with 500rpm
(rev/min) speed is stirred 48 hours.Subsequently, internal pressure is slowly discharged by a gas vent.Pass through at the end of ball milling
Container cover is opened in atmosphere, is caused carboxylate that violent hydration reaction generation carboxylic acid occurs by the wet steam in air and is sent out and dodge
Light.Products obtained therefrom 1M hydrochloric acid solutions carry out soxhlet type to be thoroughly acidified carboxylate and remove presumable metal impurities.Most
Eventually under 0.05 millimetres of mercury vacuum environment subzero 120 degrees Celsius obtain edge carboxylated graphene nanometer sheet within lyophilized 48 hours
Furvous powder.The edge carboxylated graphene nanometer sheet of 0.1wt% is obtained into uniform for 30 minutes by the ultrasound in isopropanol
Scattered solution.
Next Huo Qu Magnesium powder.Then edge carboxylated Graphene is scaled into Graphene Bing Yi Magnesium powder and Graphene mass ratio
10:1 ratio is added in 0.1wt% edges carboxylated graphene nanometer sheet aqueous isopropanol and is uniformly mixed.Then
Filter, be dried the mixture that acquisition edge carboxylated Graphene is well mixed Yu Magnesium powder.Subsequently by mixture 2KPa vacuum
10 centimetres of thermals treatment zone of micro-wave oven diameter under environment with the speed of 0.05 meter per second in room temperature condition by power as 800W carry out adding
Heat about 2 seconds, subsequently enters room temperature region and is cooled down, you can obtain the mixture that Graphene is well mixed Yu Magnesium powder.
Subsequently by Graphene Yu Magnesium powder mixtures and magnesium alloy powder with mass ratio 1:30 ratio is well mixed and is led to
Burning freezing of a furnace is sintered and forms Graphene-Magnesium alloy composite materials.
Embodiment seven：
Short steel fibre is obtained first.Then graphene oxide is scaled into Graphene and with steel fibre and Graphene mass ratio
10:1 ratio is added in the aqueous solution of 8 mg/mls and is uniformly mixed.Then filter, be dried acquisition graphite oxide
The mixture that alkene is well mixed with steel fibre.Subsequently mixture 95 degrees Celsius of process in hydrazine hydrate steam are mixed for 24 hours with reducing
Graphene oxide in compound.It is by power with the speed of 0.1 meter per second under helium protection by conveyer belt by mixture nationality subsequently
1000 watts, a diameter of 20 centimetres of heating using microwave area carries out heating using microwave about 2 seconds, subsequently enters by the room of circulating cooling water management
Wet atmosphere cooled region is cooled down.Mixture repeats redox graphene conversion in mixture after microwave heating treatment 5 times
For Graphene.The carbon content of Graphene is more than 90% wherein in mixture.Subsequently by Graphene-short steel fibre mixture with its with
Molten steel is with mass ratio 1:100 ratio is added in the molten steel of melting and is well mixed, and subsequently cooling can obtain graphite
Alkene is dispersed in the Graphene-steel composite material in metallic steel.
Claims (9)
1. a kind of preparation method of Graphene metallic composite, it is characterised in that prepare Graphene derivative solution first, so
Afterwards Graphene derivative solution and particulate solid are carried out being mixed to form mixture, be subsequently dried, then in setting gas
The mixture being dried under atmosphere is heated and by Graphene derivative in mixture with setting speed by heating using microwave area
Graphene is converted into, subsequent Graphene leaves heating using microwave area and cooled down with the mixture of particulate solid, then will be mixed
Compound is combined as reinforcement and metal material and is obtained Graphene-metallic composite.
2. a kind of preparation method of Graphene metallic composite according to claim 1, it is characterised in that the graphite
Ene derivative refers to that the oxide of Graphene includes graphene oxide and redox graphene and graphene edge derivative.
3. a kind of preparation method of Graphene metallic composite according to claim 1, it is characterised in that the solid-state
Particulate matter can be dispersed in metal material, including powder and chopped fiber.
4. a kind of preparation method of Graphene metallic composite according to claim 1, it is characterised in that the graphite
Olefinic carbon content is more than 90%.
5. a kind of preparation method of Graphene metallic composite according to claim 1, it is characterised in that the graphite
Ene derivative be converted into Graphene refer to Graphene derivative absorb microwave and heat up and setting atmosphere under cause aoxidize stone
Black alkene is reduced and is converted into Graphene, and graphene edge derivative then occurs the reaction of off-clip edge functional group and is converted into graphite
Alkene.
6. a kind of preparation method of Graphene metallic composite according to claim 1, it is characterised in that the setting
Atmosphere refers to inert atmosphere, reducing atmosphere or vacuum state.Inert atmosphere refers to that gas does not react with Graphene derivative
Gas；Reducing atmosphere is referred in gas containing the gas of reduced graphene derivative；Vacuum state refers to that air pressure is less than
4KPa, relative degree of vacuum is less than -20KPa.
7. a kind of preparation method of Graphene metallic composite according to claim 1, it is characterised in that the mixing
Thing is with setting speed by heating using microwave area according to the heating using microwave area size Control heat time.
8. a kind of preparation method of Graphene metallic composite according to claim 1, it is characterised in that the mixing
Thing leaves heating using microwave area and cooled referring to cools down mixture by cold atmosphere.
9. a kind of preparation method of Graphene metallic composite according to claim 1, it is characterised in that the microwave
Heat that can repeat i.e. can multiple microwave heating treatment mixture.
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Cited By (3)
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| CN109794615A (en) * | 2018-12-25 | 2019-05-24 | 西安交通大学 | A kind of preparation method of graphene-based composite material |
| CN112955586A (en) * | 2018-10-29 | 2021-06-11 | C2Cnt有限责任公司 | Continuous, easily separated molten carbonate electrolysis cathode products |
| RU2803865C1 (en) * | 2022-12-26 | 2023-09-21 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский политехнический университет Петра Великого" (ФГАОУ ВО "СПбПУ") | Method for obtaining a nickel-graphene nanocomposite with increased plasticity |
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