CN109794615A - A kind of preparation method of graphene-based composite material - Google Patents
A kind of preparation method of graphene-based composite material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of graphene-based composite material, grapheme material is mixed with compound precursor through liquid phase and solid phase mixing uniformly obtains mixing material, then adjuvant is added into mixing material, intermittent or continous way is taken to handle graphene using microwave, a step realizes graphene punching, doping and recombination process during the reaction, and graphene-based composite material is quickly made.Operation of the present invention method wide adaptation range, simple process, heating rate is fast, and with short production cycle, low energy consumption, environmental-friendly, can most complete the preparation of graphene-based composite material within tens of seconds fastly, and compared to conventional method, cost reduces obvious.
Description
Technical field
The invention belongs to novel C-base composte material technical fields, and in particular to a kind of quick, low energy consumption, green method system
Standby graphene-based composite material.
Background technique
Graphene has many excellent physical chemistry as a kind of two-dimension nano materials being made of single layer of carbon atom
Can, such as outstanding conduction, heating conduction, strong mechanical performance and high stability, thus there is it all extensively in numerous areas
Wealthy application prospect.
Wherein, in the fields such as energy storage and catalysis, researcher is in order to reach body of the limitation material granule in electrochemical reaction
Product expansion usually prepares stone by graphene and metal oxide, metal nanoparticle etc. the effects of promoting conduction or be catalyzed
Mertenyl composite material.But the method for preparing graphene-based composite material at present need to mostly be come in fact by traditional heat resolve method
It is existing, there is heating slowly, the operating time is long, and energy consumption is high, leads to the problems such as material production cycle is too long, and cost is excessively high, limits it
Practical application.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that providing one kind, low energy consumption,
Period is short, environmental-friendly, the method that can quickly prepare graphene-based composite material.
The invention adopts the following technical scheme:
A kind of preparation method of graphene-based composite material, grapheme material is mixed with compound precursor through liquid phase and
Solid phase mixing uniformly obtains mixing material, and adjuvant is then added into mixing material, is taken using microwave intermittent or continuous
Formula handles graphene, and a step realizes graphene punching, doping and recombination process during the reaction, and graphite is quickly made
Alkenyl composite material.
Specifically, grapheme material and the mass ratio of compound precursor are (0.1~20): 1.
Specifically, liquid phase, which is mixed into, is dissolved or dispersed in solvent for compound precursor, then grapheme material is sufficiently divided
It dissipates in above-mentioned solution, is then directly evaporated or the drying and processing after filtration washing；Solid phase mixing be by grapheme material with it is compound
It is uniform that carbonate, acetate and hydroxide in object presoma carry out direct mechanical mixture.
Further, solvent be deionized water, acid solution, aqueous slkali, methanol, ethyl alcohol, ethylene glycol, glycerine, glacial acetic acid,
One of ether and acetone or multicomponent solvent.
Further, grapheme material be pure graphene, slightly restore graphene oxide, through nitrogen phosphate and sulfur, fluorine or chlorine
At least one of graphene and the graphene of surface modification of doping；The graphene of surface modification is amino graphite
One or more of alkene, sulfonates graphene and sulfhydrylation graphene.
Further, compound precursor be magnesium, germanium, indium, tin, bismuth, antimony, lead, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel,
One or more of copper, zinc, rare earth metal and salt, oxide and the hydroxide of noble metal.
Specifically, the mass ratio of mixing material and adjuvant is (4~35): 1.
Further, adjuvant is in graphene oxide, carbon nanotube, carbon fiber, Ketjen black, acetylene black and Super P
One or more.
Specifically, the power of microwave treatment be 100~5000 watts, the processing time be 2~120s, work atmosphere be air,
One of nitrogen, argon gas, helium, ammonia, hydrogen, carbon monoxide and carbon dioxide or various mixed gases, divide as 0.1~
1 atmospheric pressure.
Further, work atmosphere further includes vacuum or oxygen.
Compared with prior art, the present invention at least has the advantages that
A kind of preparation method of graphene-based composite material of the present invention regulates and controls reaction process by addition adjuvant, such as adds
Play reaction, improves temperature and heating rate, accelerates reaction, while increasing the toughness of composite material, the performances such as intensity and electric conductivity；
By controlling the process conditions of composite material preparation process, a step graphene punching, doping and multiple can be realized during the reaction
Conjunction process improves the preparation efficiency of material；Also different composite materials is made in controllable process etc., such as simultaneously realize punching and
It is compound, or doping and compound etc. is realized simultaneously.
Further, the mass ratio of graphene and composite precursor selection is specifically selected according to required composite material to be prepared
It selects.The method that this microwave prepares graphene-based composite material can be suitble to the matter of wide range of graphene and compound precursor
Amount ratio.
Further, solid phase mixing simple process is easy to operate, and liquid phase mixing can make predecessor and graphene compound more
Uniformly.
Further, according to the difference of used presoma, selection is more conducive to the molten of dissolution presoma and dispersed graphite alkene
Agent, to achieve the purpose that presoma is compound with graphene uniform.
Further, different types of graphene has different property, and can be prepared by microwave method has difference
The graphene composite material of property or purposes.
Further, compound precursor can be varied, has a wide range of application.
Further, the reaction that the use of adjuvant can prepare graphene composite material with assisted microwave synthesis is gone on smoothly.It is auxiliary
Auxiliary agent uses too down to the effect for causing microwave reaction less than it.Adjuvant uses too high, can make the graphene finally prepared
Adjuvant accounting is too high in composite material, influences composite material quality.Comprehensive consideration is by graphene in mixing material and adjuvant
Mass ratio be set as (4~35): 1.
Further, the optional range of adjuvant is wide, is not limited to graphene, can be various carbon materials.It can be according to difference
Mixing material and to be realized composite properties selection adjuvant.
Further, the power selection of microwave treatment is advisable with that can reach under microblogging fast reaction and reduce the reaction time,
Preferably, it can be set near 1000 watts, can not only make most material normal reactions, but also easy to accomplish.
Further, the use of atmosphere can be there are many selection, and the effect of atmosphere is mainly at two aspects: first is that protection is mixed
Condensation material makes it that unnecessary reaction occur during the reaction；Second is that reaching graphene doping or punching using special gas
Purpose.
In conclusion operation of the present invention method wide adaptation range, simple process, heating rate is fast, with short production cycle, energy consumption
It is low, it is environmental-friendly, the preparation of graphene-based composite material can be most completed within tens of seconds fastly, compared to conventional method, cost drop
It is low obvious.
Below by embodiment, technical scheme of the present invention will be described in further detail.
Specific embodiment
The present invention provides a kind of preparation methods of graphene-based composite material, first by grapheme material and compound forerunner
Body uniformly combines, and adds adjuvant, the effect using microwave to graphene, take intermittent or continous way the short time (2~
Corresponding graphene-based composite material is quickly made in 120s).Specific step is as follows:
S1, grapheme material and compound precursor A are pressed (5~20): 1 mass ratio mixes, and obtains mixing material a；
Grapheme material is pure graphene, the graphene oxide slightly restored, the stone through doping such as nitrogen phosphate and sulfur, fluorine, chlorine
At least one of black alkene and the graphene of surface modification；The graphene of surface modification includes but is not limited to amino graphite
Alkene, sulfonates graphene, one or more of sulfhydrylation graphene.
Compound precursor A include magnesium, germanium, indium, tin, bismuth, antimony, lead, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc,
One or more of the salt of rare earth metal and noble metal, oxide, hydroxide.
Hybrid mode includes liquid phase mixing and solid phase mixing.
Liquid phase mixing step is as follows:
Compound precursor is first dissolved or dispersed in coordinative solvent, then grapheme material is well-dispersed in above-mentioned molten
Then liquid evaporates under stirring or is evaporated or dries after filtration washing, drying temperature and time are Bu Tong specific according to solvent
Selection, temperature are usually no more than 100 DEG C.
Solvent include deionized water, acid solution, aqueous slkali, methanol, ethyl alcohol, ethylene glycol, glycerine, glacial acetic acid, ether and
One of acetone or multicomponent solvent.
Solid phase mixing is that carbonate, acetate, hydroxide in grapheme material and compound precursor A etc. is easily high
The warm direct mechanical mixture of decomposition product is uniform.
Preferably, incorporation time is in 0.5~12h.
S2, adjuvant B is added in gained mixing material a in step sl, obtains mixing material b, is mixed in mixing material b
The mass ratio of material a and adjuvant B are (4~10): 1；
Adjuvant B is in graphene oxide, carbon nanotube, carbon fiber, Ketjen black, acetylene black and conductive black Super P
One or more.
S3, by step S2 gained mixing material b be placed in microwave reaction equipment, adjust work atmosphere, plant capacity and
Time is reacted, and a step can be realized graphene punching, doping and recombination process during the reaction, be obtained corresponding graphene
Based composites.
Work atmosphere is one in air, nitrogen, argon gas, helium, ammonia, hydrogen, oxygen, carbon monoxide and carbon dioxide
Kind or various mixed gases, partial pressure are as follows: 0.1~1 atmospheric pressure.
Preferably, work atmosphere further includes vacuum environment.
The power of microwave reaction equipment be 100~5000 watts, microwave treatment time be 2~120s, can be used it is intermittent or
Continuity preparation method.
Preferably, the material in composite material outside graphene is stable in the air, is not easy to be oxidized.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.The component for being usually described herein as the embodiment of the present invention with shown in can pass through
A variety of different configurations are to arrange and design.Therefore, the detailed description of the embodiment of the present invention of offer is not intended to below
The range of claimed invention is limited, but is merely representative of selected embodiment of the invention.Based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
Embodiment 1
(1) 5 milligrams of silver nitrates are dissolved in 20 ml deionized waters, then 25 milligrams of redox graphenes are placed in above-mentioned molten
Liquid stirs evenly, and is evaporated at 50 DEG C；
(2) sample after being evaporated and 1 milligram of carbon nanotube grinding is uniform；
(3) material in step (2) is placed in microwave reaction equipment, adjusting work atmosphere is argon gas, is divided as 1 atmosphere
Pressure, plant capacity are 800 watts, and the microwave reaction time is 30 seconds.
Occur apparent arc phenomenon, spark and combustion phenomena in reaction process, it is compound that silver/graphite alkene is just obtained after reaction
Material.
Embodiment 2
(1) 5 milligrams of silver nitrates are dissolved in 20 ml deionized waters, then 25 milligrams of redox graphenes are placed in above-mentioned molten
Liquid stirs evenly, and is evaporated at 50 DEG C；
(2) sample after being evaporated is mixed with 1 milligram of graphene oxide；
(3) material in step (2) is placed in microwave reaction equipment, adjusting work atmosphere is argon gas, is divided as 1 atmosphere
Pressure, plant capacity are 800 watts, and the microwave reaction time is 10 seconds.
Occur apparent electric arc, spark and combustion phenomena in reaction process, silver/graphite alkene composite wood is just obtained after reaction
Material.
Embodiment 3
(1) 5 milligrams of silver nitrates are dissolved in 20 ml deionized waters, then 25 milligrams of redox graphenes are placed in above-mentioned molten
Liquid stirs evenly, and is evaporated at 50 DEG C；
(2) sample after being evaporated is mixed with 1 milligram of graphene oxide；
(3) material in step (2) is placed in microwave reaction equipment, adjusting work atmosphere is argon gas, is divided big for 0.1
Air pressure, plant capacity are 100 watts, and the microwave reaction time is 120s, using 20s intermittent type microwave.
Occur apparent electric arc, spark and combustion phenomena in reaction process, increase with time, reacting phenomenon slowly dies down,
Just silver/graphite alkene composite material is obtained after reaction.
Embodiment 4
(1) 5 milligrams of cobalt nitrates are dissolved in 20 milliliters of ethyl alcohol, then the graphene oxide that 25 milligrams slightly restore are placed in above-mentioned
Solution stirs evenly, and is evaporated at 50 DEG C；
(2) sample after being evaporated is mixed with 2 milligrams of graphene oxides；
(3) material in step (2) is placed in microwave reaction equipment, adjusting work atmosphere is ammonia, is divided big for 0.5
Air pressure, plant capacity are 800 watts, and the microwave reaction time is 15 seconds.
Embodiment 5
(1) 5 milligrams of cobalt nitrates are dissolved in 20 milliliters of ethyl alcohol, then the graphene oxide that 25 milligrams slightly restore are placed in above-mentioned
Solution stirs evenly, and is evaporated at 50 DEG C；
(2) sample after being evaporated is mixed with 5 milligrams of redox graphenes；
(3) material in step (2) is placed in microwave reaction equipment, adjusting work atmosphere is ammonia, is divided big for 0.2
Air pressure, plant capacity are 5000 watts, and the microwave reaction time is 2 seconds.Occurs apparent electric arc, pyrophoric behavio(u)r in reaction process, instead
Just cobalt/nitrogen-doped graphene composite material is obtained after answering.
By embodiment, appropriate microwave power and auxiliary agent quality are selected, reaction can be made to complete within 1min, and
Relative to conventional heat treatment, heat loss is few, and low energy consumption.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (10)
1. a kind of preparation method of graphene-based composite material, which is characterized in that pass through grapheme material and compound precursor
Liquid phase mixing and solid phase mixing uniformly obtain mixing material, adjuvant are then added into mixing material, between taking using microwave
Formula of having a rest or continous way handle graphene, and a step realizes graphene punching, doping and recombination process during the reaction, fastly
Graphene-based composite material is made in speed.
2. the preparation method of graphene-based composite material according to claim 1, which is characterized in that grapheme material and multiple
The mass ratio for closing object presoma is (0.1~20): 1.
3. the preparation method of graphene-based composite material according to claim 1 or 2, which is characterized in that liquid phase is mixed into
Compound precursor is dissolved or dispersed in solvent, then grapheme material is well-dispersed in above-mentioned solution, is then directly evaporated
Or the drying and processing after filtration washing；Solid phase mixing is by carbonate, the acetate in grapheme material and compound precursor
It is uniform that direct mechanical mixture is carried out with hydroxide.
4. the preparation method of graphene-based composite material according to claim 3, which is characterized in that solvent is deionization
One of water, acid solution, aqueous slkali, methanol, ethyl alcohol, ethylene glycol, glycerine, glacial acetic acid, ether and acetone or multicomponent solvent.
5. the preparation method of graphene-based composite material according to claim 3, which is characterized in that grapheme material is pure
Graphene, the graphene oxide slightly restored, through nitrogen phosphate and sulfur, fluorine or chlorine doping graphene and surface modification graphene
At least one of；The graphene of surface modification is in amination graphene, sulfonates graphene and sulfhydrylation graphene
It is one or more of.
6. the preparation method of graphene-based composite material according to claim 3, which is characterized in that compound precursor is
Salt, the oxidation of magnesium, germanium, indium, tin, bismuth, antimony, lead, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, rare earth metal and noble metal
One or more of object and hydroxide.
7. the preparation method of graphene-based composite material according to claim 1, which is characterized in that mixing material and auxiliary
The mass ratio of agent is (4~35): 1.
8. the preparation method of graphene-based composite material according to claim 1 or claim 7, which is characterized in that adjuvant is oxygen
One or more of graphite alkene, carbon nanotube, carbon fiber, Ketjen black, acetylene black and Super P.
9. the preparation method of graphene-based composite material according to claim 1, which is characterized in that the power of microwave treatment
It is 100~5000 watts, the processing time is 2~120s, and work atmosphere is air, nitrogen, argon gas, helium, ammonia, hydrogen, an oxygen
Change one of carbon and carbon dioxide or various mixed gases, divides as 0.1~1 atmospheric pressure.
10. the preparation method of graphene-based composite material according to claim 9, which is characterized in that work atmosphere also wraps
Include vacuum or oxygen.
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