CN109161715A - A kind of metallic graphite carbon alkene composite material and preparation method and preparation facilities - Google Patents
A kind of metallic graphite carbon alkene composite material and preparation method and preparation facilities Download PDFInfo
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- CN109161715A CN109161715A CN201811018859.XA CN201811018859A CN109161715A CN 109161715 A CN109161715 A CN 109161715A CN 201811018859 A CN201811018859 A CN 201811018859A CN 109161715 A CN109161715 A CN 109161715A
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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
- C22C1/1026—Alloys containing non-metals starting from a solution or a suspension of (a) compound(s) of at least one of the alloy constituents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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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
- C22C1/08—Alloys with open or closed pores
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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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
Abstract
The present invention discloses a kind of metallic graphite carbon alkene composite material and preparation method and preparation facilities, composite material are prepared from the following raw materials: copper foil, dilute hydrochloric acid, hydrogen, methane, PMMA, Fecl3Solution, deionized water, charcoal-aero gel, metalliferous chemical plating fluid, acetone and inert gas, preparation method includes: to prepare nano porous metal, graphene is pulled out from deionized water with nano porous metal, graphene is put into drying box and is heated, obtain metallic graphite carbon alkene composite material, the metallic graphite carbon alkene that the preparation method of metallic graphite carbon alkene composite material of the invention is formed, the graphene for thering is metal to support by Experimental comparison and the graphene without metal support, it can be seen that the graphene specific capacity for having metal to support significantly improves, chemical property is preferable, it is preferable as electrode of super capacitor effect.
Description
Technical field
The present invention relates to carbon processing technique field, in particular to a kind of metallic graphite carbon alkene composite material and preparation method and
Preparation facilities.
Background technique
Carbon material is to be used as electrode material for super capacitor earliest, has stability and electric conductivity good, specific surface area
The advantages that high.Since carbon material is by being formed on its surface electric double layer capacitance, the specific surface area of material gets over the electricity of large capacitor
Capacitive can be better, and therefore, the specific surface area for improving carbon material is to improve the effective way of carbon electrode material capacitor specific capacity.Stone
Black alkene is a kind of two-dimensional slice structure, only one carbon atom of thickness is thick, the hexagonal network knot that surface is made of carbon atom
Structure.Graphene has special physical and chemical properties, and graphene is as a kind of carbon material, and specific surface area is high, in super capacitor
The application of device electrode material above has good prospect.But graphene specific capacity is lower, and chemical property is poor, as super capacitor
Device electrode effect is poor.
Summary of the invention
To overcome the problems in correlation technique, the present invention provide a kind of graphene composite material and preparation method thereof and
Device.
According to the first aspect of the embodiments of the present disclosure, a kind of metallic graphite carbon alkene composite material is provided, which is characterized in that described
Metallic graphite carbon alkene composite material is prepared from the following raw materials: copper foil, dilute hydrochloric acid, hydrogen, methane, PMMA, Fecl3Solution, deionization
Water, charcoal-aero gel, metalliferous chemical plating fluid, acetone and inert gas.
Optionally, the inert gas is helium, neon, one of argon and krypton.
According to the second aspect of the disclosure, a kind of preparation method of metallic graphite carbon alkene composite material, including following step are provided
It is rapid:
Copper foil is impregnated in dilute hydrochloric acid, 4~6min is ultrasonically treated in ultrasonic particle oscillator, obtains pretreatment copper foil；
Pretreatment copper foil is put into vacuum tank, hydrogen and methane is passed through into the vacuum tank, obtains being deposited with graphite
The copper foil of alkene；
PMMA is coated in the copper foil surface for being deposited with graphene, obtains the copper foil of coating PMMA；
The copper foil of the coating PMMA is placed in Fecl3In solution, standing 5~after ten minutes, it is cleaned, is gone with deionized water
The graphene of copper foil；
Charcoal-aero gel is placed in metalliferous chemical plating fluid, metal-carbon aerogel composite is obtained；
The metal-carbon aerogel composite is subjected to solvent displacement with acetone, obtains the metal-carbon aeroge of replacement Treatment
Composite material；
The metal-carbon aerogel composite of the replacement Treatment is heat-treated under inert gas protection, obtains nanoporous
Metal；
Graphene is pulled out from deionized water with the nano porous metal, and the graphene is put into drying box and is heated, is added
Hot temperature is 120~140 DEG C, and heating time is 40~50min, obtains metal-graphite alkene composite material preform；
The metal-graphite alkene composite material preform is placed in acetone and impregnates 20~30min, is impregnated after the acetone more renewed
10~12h obtains the metallic graphite carbon alkene composite material.
Using the preparation method for the metallic graphite carbon alkene composite material that second aspect provides, copper foil first is impregnated by dilute hydrochloric acid
After ultrasonic treatment, the pore size of copper foil surface can be increased, graphene is facilitated to be deposited on copper foil surface；Graphene is in vacuum
In the hole for growing the graphene that can prevent other substances in air from entering generation in pipe, the purity of graphene is improved,
Increase the probability that metal enters graphene hole；Use PMMA as protective layer be graphene surface coating prevent Fecl3It is right
The graphene of generation causes to damage, Fecl3The graphene of copper foil is obtained after solution removal copper foil；Charcoal-aero gel is one kind by ball
Light nanoporous material made of shape nanoparticle is interconnected, it has pore structure abundant, by charcoal-aero gel and containing gold
After the chemical plating fluid mixing of category, then metal-carbon aerogel composite is obtained after being replaced with acetone soln, high temperature goes down carbon removal gas
Gel complex material just forms nano porous metal, and the nano porous metal material of formation is in block shape, later nanoporous
Metal with graphene is compound combines closely at high temperature, finally remove PMMA using acetone, it is multiple to obtain final metallic graphite carbon alkene
Condensation material；The metallic graphite carbon alkene that the preparation method for the metallic graphite carbon alkene composite material that second aspect provides is formed passes through experiment pair
Than the graphene for thering is metal to support and the graphene supported without metal, it can be seen that the graphene specific capacity for having metal to support is significant
It improves, chemical property is preferable, preferable as electrode of super capacitor effect.
Optionally, described to be passed through hydrogen and methane into the vacuum tank, the ratio of hydrogen and methane is 15:25.
Optionally, the metal-carbon aerogel composite by the replacement Treatment under inert gas protection heat at
Before reason, further includes: by the metal-carbon aerogel composite merging autoclave of the replacement Treatment, carry out CO2It is overcritical
Dry, temperature condition is 50~60 DEG C, and pressure condition is 12~15MPa.
Optionally, it is described the metal-carbon aerogel composite is subjected to solvent displacement with acetone after, third after exchange
The content of moisture is lower than 2500ppm in ketone.
According to the third aspect of the disclosure, a kind of preparation facilities of metallic graphite carbon alkene composite material is provided, is used for institute
It states nano porous metal to be dried the graphene after pulling graphene in deionized water out, which is characterized in that the system
Standby device includes: drying box body, heating device and vacuum evacuation device, and the drying box body is internally provided with dry appearance
Chamber is set, the heating device and the vacuum evacuation device are connected with the dry accommodating cavity respectively；
The heating device includes outlet pipe, cold water storage cistern, suction pump, communicating pipe, boiler, water inlet pipe and S bend pipe, the S
One end of the inside of type pipe setting and the dry accommodating cavity, the S bend pipe is connected by the outlet pipe with the cold water storage cistern
Logical, the other end of the S bend pipe is connected by the water inlet pipe with the boiler, and the cold water storage cistern and the boiler are logical
It crosses and is connected the communicating pipe, one end of the suction pump is connected with the cold water storage cistern, the other end of the suction pump and institute
It states boiler to be connected, the boiler is internally provided with heating device；
The vacuum evacuation device includes vacuum-pumping tube and vacuum pumping pump, one end of the vacuum-pumping tube and the dry accommodating cavity phase
Connection, the other end of the vacuum-pumping tube are connected with the vacuum pumping pump.
Optionally, every section of top of the S bend pipe is provided with vessel accommodation groove.
Optionally, the vacuum evacuation device is set as multiple.
Optionally, heating tube is provided on the inner wall of the dry accommodating cavity, the heating tube is in the dry accommodating cavity
Inner wall on be evenly distributed.
The preparation facilities of the metallic graphite carbon alkene composite material of the third aspect, in use, the heater in boiler heats heat
Hot water is pumped into S bend pipe by Water in Water Tanks, suction pump, realizes that carrying out heating to the substance being placed in the vessel on S bend pipe does
It is dry, while being flowed into cold water storage cistern after the hot water cooling in S bend pipe, and flowed back in boiler via communicating pipe, and under entrance
One circulation realizes the effect of the heat drying of S bend pipe so that the temperature of S bend pipe keeps higher state, meanwhile, it takes out
Vacuum plant carries out vacuumize process to the inside of dry accommodating cavity, prevents the impurity in air from generating shadow to substance to be dried
It rings；The whole process that the preparation facilities that the third aspect provides is dried all realizes the effect of stable drying process to graphene
Fruit can significantly improve the production efficiency of metallic graphite carbon alkene composite material and the electrode effect of metallic graphite carbon alkene.
Detailed description of the invention
In order to illustrate more clearly of technical solution of the present invention, letter will be made to attached drawing needed in the embodiment below
Singly introduce, it should be apparent that, for those of ordinary skills, without any creative labor,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 is that the process of the preparation method of the metallic graphite carbon alkene composite material provided according to an exemplary embodiment is illustrated
Figure；
Fig. 2 is the overall schematic of the preparation facilities of the metallic graphite carbon alkene composite material provided according to an exemplary embodiment.
Specific embodiment
Example embodiments are described in detail here, and the example is illustrated in the accompanying drawings.Following description is related to
When attached drawing, unless otherwise indicated, the same numbers in different drawings indicate the same or similar elements.Following exemplary embodiment
Described in embodiment do not represent all embodiments consistented with the present invention.On the contrary, they be only with it is such as appended
The example of device and method being described in detail in claims, some aspects of the invention are consistent.
According to the first aspect of the embodiments of the present disclosure, a kind of metallic graphite carbon alkene composite material is provided, which is characterized in that described
Metallic graphite carbon alkene composite material is prepared from the following raw materials: copper foil, dilute hydrochloric acid, hydrogen, methane, PMMA, Fecl3Solution, deionization
Water, charcoal-aero gel, metalliferous chemical plating fluid, acetone and inert gas.
A kind of metallic graphite carbon alkene composite material of first aspect, by preparing nano porous metal and the life of the invention used
The method of long graphene and screen clean surface, graphene continuous, single layer is good, enable nano porous metal with beat
The graphene in hole is combined closely, and the graphene for having metal to support by Experimental comparison and the graphene without metal support can be seen
The graphene specific capacity for having metal to support out significantly improves, and chemical property is preferable, and seat is that electrode of super capacitor effect is preferable.
As preferred embodiment, the inert gas is helium, neon, one of argon and krypton.Inert gas can prevent
Metal is reacted with the oxygen in air, and prepared nano porous metal is caused to contain impurity, to reduce nano porous metal
Degree is tightly combined with graphene.
Embodiment one
Fig. 1 is the flow diagram of the preparation method for the metallic graphite carbon alkene composite material that embodiment one provides, and is included the following steps:
In step sl, copper foil is impregnated in dilute hydrochloric acid, 4~6min is ultrasonically treated in ultrasonic particle oscillator, is obtained pre-
Handle copper foil.
In step s 2, pretreatment copper foil is put into vacuum tank, is passed through hydrogen and methane into the vacuum tank,
Obtain the copper foil for being deposited with graphene.
In step s3, PMMA is coated in the copper foil surface for being deposited with graphene, obtains the copper foil of coating PMMA.
In step s 4, the copper foil of the coating PMMA is placed in Fecl3In solution, stand 5~after ten minutes, spend from
Sub- water cleaning, obtains the graphene of copper foil.
In step s 5, charcoal-aero gel is placed in metalliferous chemical plating fluid, obtains metal-carbon aeroge composite wood
Material.
In step s 6, the metal-carbon aerogel composite is subjected to solvent displacement with acetone, obtains replacement Treatment
Metal-carbon aerogel composite.
It in the step s 7, will be at the metal-carbon aerogel composite of the replacement Treatment under inert gas protection heat
Reason, obtains nano porous metal.
In step s 8, graphene is pulled out from deionized water with the nano porous metal, the graphene is put into
It is heated in drying box, heating temperature is 120~140 DEG C, and heating time is 40~50min, obtains metal-graphite alkene composite material
Preform.
In step S, the metal-graphite alkene composite material preform is placed in acetone and impregnates 20~30min, replacement
10~12h is impregnated after new acetone, obtains the metallic graphite carbon alkene composite material.
The preparation method of metallic graphite carbon alkene composite material provided in this embodiment, first copper foil are impregnated and are surpassed by dilute hydrochloric acid
After sonication, the pore size of copper foil surface can be increased, graphene is facilitated to be deposited on copper foil surface；Graphene is in vacuum tube
In the hole for growing the graphene that can prevent other substances in air from entering generation, the purity of graphene is improved, is increased
Metal enters the probability of graphene hole；Use PMMA as protective layer be graphene surface coating prevent Fecl3To generation
Graphene cause to damage, Fecl3The graphene of copper foil is obtained after solution removal copper foil；Charcoal-aero gel is that one kind is received by spherical
Light nanoporous material made of rice corpuscles is interconnected, it has pore structure abundant, by charcoal-aero gel with it is metalliferous
After chemical plating fluid mixing, then metal-carbon aerogel composite is obtained after being replaced with acetone soln, high temperature goes down except charcoal-aero gel
Composite material just forms nano porous metal, and the nano porous metal material of formation is in block shape, later nano porous metal
With graphene is compound combines closely at high temperature, finally remove PMMA using acetone, obtain final metallic graphite carbon alkene composite wood
Material；The metallic graphite carbon alkene that the preparation method for the metallic graphite carbon alkene composite material that second aspect provides is formed, has by Experimental comparison
The graphene of metal support and the graphene supported without metal, it can be seen that the graphene specific capacity for having metal to support significantly mentions
Height, chemical property is preferable, and seat is that electrode of super capacitor effect is preferable.
As preferred embodiment, in aqueous mixed raw material described in step S3 the content of water be 30%~40%, it is described
It is added before deionized water in the mixed raw material, the deionized water is heated.It was proved that in mixed raw material
Water content be 30%~40% be optimum moisture content, the very few mixing for being unfavorable for raw material of water content, water content is excessively unfavorable for mixing
Close the press strip processing of raw material.It also needs to detect the water content in mixed raw material after mixed raw material, so that it is determined that deionized water adds
Deionized water is heated before in addition adding, is equivalent to and is indirectly heated to mixed raw material, be conducive to subsequent by water
Press strip processing, molding is more preferable.
Embodiment two
Include the following steps:
In step sl, copper foil is impregnated in dilute hydrochloric acid, 4~6min is ultrasonically treated in ultrasonic particle oscillator, is obtained pre-
Handle copper foil.
In step s 2, pretreatment copper foil is put into vacuum tank, is passed through hydrogen and methane into the vacuum tank,
Obtain the copper foil for being deposited with graphene.
Wherein, described to be passed through hydrogen and methane into the vacuum tank, the ratio of hydrogen and methane is 15:25.
In step s3, PMMA is coated in the copper foil surface for being deposited with graphene, obtains the copper foil of coating PMMA.
In step s 4, the copper foil of the coating PMMA is placed in Fecl3In solution, stand 5~after ten minutes, spend from
Sub- water cleaning, obtains the graphene of copper foil.
In step s 5, charcoal-aero gel is placed in metalliferous chemical plating fluid, obtains metal-carbon aeroge composite wood
Material.
In step s 6, the metal-carbon aerogel composite is subjected to solvent displacement with acetone, obtains replacement Treatment
Metal-carbon aerogel composite.
It in the step s 7, will be at the metal-carbon aerogel composite of the replacement Treatment under inert gas protection heat
Reason, obtains nano porous metal.
In step s 8, graphene is pulled out from deionized water with the nano porous metal, the graphene is put into
It is heated in drying box, heating temperature is 120~140 DEG C, and heating time is 40~50min, obtains metal-graphite alkene composite material
Preform.
In step S, the metal-graphite alkene composite material preform is placed in acetone and impregnates 20~30min, replacement
10~12h is impregnated after new acetone, obtains the metallic graphite carbon alkene composite material.
It was proved that the graphene single-layer type of growth is more preferable when the ratio of methane and hydrogen being passed through is 15:25,
Crystal grain is big, is more advantageous to combining closely for graphene and nano porous metal.
Embodiment three
Include the following steps:
In step sl, copper foil is impregnated in dilute hydrochloric acid, 4~6min is ultrasonically treated in ultrasonic particle oscillator, is obtained pre-
Handle copper foil.
In step s 2, pretreatment copper foil is put into vacuum tank, is passed through hydrogen and methane into the vacuum tank,
Obtain the copper foil for being deposited with graphene.
In step s3, PMMA is coated in the copper foil surface for being deposited with graphene, obtains the copper foil of coating PMMA.
In step s 4, the copper foil of the coating PMMA is placed in Fecl3In solution, stand 5~after ten minutes, spend from
Sub- water cleaning, obtains the graphene of copper foil.
In step s 5, charcoal-aero gel is placed in metalliferous chemical plating fluid, obtains metal-carbon aeroge composite wood
Material.
In step s 6, the metal-carbon aerogel composite is subjected to solvent displacement with acetone, obtains replacement Treatment
Metal-carbon aerogel composite.
It in the step s 7, will be at the metal-carbon aerogel composite of the replacement Treatment under inert gas protection heat
Reason, obtains nano porous metal.
In step s 8, graphene is pulled out from deionized water with the nano porous metal, the graphene is put into
It is heated in drying box, heating temperature is 120~140 DEG C, and heating time is 40~50min, obtains metal-graphite alkene composite material
Preform.
In step S, the metal-graphite alkene composite material preform is placed in acetone and impregnates 20~30min, replacement
10~12h is impregnated after new acetone, obtains the metallic graphite carbon alkene composite material.
Wherein, before step S7, further includes: be placed in the metal-carbon aerogel composite of the replacement Treatment high
It presses in kettle, carries out CO2Supercritical drying, temperature condition are 50~60 DEG C, and pressure condition is 12~15MPa.By carrying out CO2
Supercritical drying, on the one hand can be with CO2It is liquid, the CO of liquid under supercriticality2As liquid solvent can make metal with
Charcoal-aero gel mixes more abundant, the CO of another aspect liquid2It is easier to flow between metal and charcoal-aero gel, improves gold
Belong to the efficiency in conjunction with charcoal-aero gel.
Example IV
Include the following steps:
In step sl, copper foil is impregnated in dilute hydrochloric acid, 4~6min is ultrasonically treated in ultrasonic particle oscillator, is obtained pre-
Handle copper foil.
In step s 2, pretreatment copper foil is put into vacuum tank, is passed through hydrogen and methane into the vacuum tank,
Obtain the copper foil for being deposited with graphene.
In step s3, PMMA is coated in the copper foil surface for being deposited with graphene, obtains the copper foil of coating PMMA.
In step s 4, the copper foil of the coating PMMA is placed in Fecl3In solution, stand 5~after ten minutes, spend from
Sub- water cleaning, obtains the graphene of copper foil.
In step s 5, charcoal-aero gel is placed in metalliferous chemical plating fluid, obtains metal-carbon aeroge composite wood
Material.
In step s 6, the metal-carbon aerogel composite is subjected to solvent displacement with acetone, obtains replacement Treatment
Metal-carbon aerogel composite.
Wherein, it is described the metal-carbon aerogel composite is subjected to solvent displacement with acetone after, the acetone after exchange
The content of middle moisture is lower than 2500ppm.Water content carries out solvent displacement completely using acetone lower than 2500ppm explanation in acetone,
Form the higher metal-carbon aerogel composite of purity.
It in the step s 7, will be at the metal-carbon aerogel composite of the replacement Treatment under inert gas protection heat
Reason, obtains nano porous metal.
In step s 8, graphene is pulled out from deionized water with the nano porous metal, the graphene is put into
It is heated in drying box, heating temperature is 120~140 DEG C, and heating time is 40~50min, obtains metal-graphite alkene composite material
Preform.
In step S, the metal-graphite alkene composite material preform is placed in acetone and impregnates 20~30min, replacement
10~12h is impregnated after new acetone, obtains the metallic graphite carbon alkene composite material.
Fig. 2 is the overall schematic of the preparation facilities for the metallic graphite carbon alkene composite material that exemplary embodiment provides, the system
Standby device is used to for the nano porous metal being dried the graphene after pulling graphene in deionized water out, described
Preparation facilities includes: drying box body 1, heating device 11 and vacuum evacuation device 12, and being internally provided with for drying box body 1 is dry
Dry accommodating cavity 13, heating device 11 and vacuum evacuation device 12 are connected with dry accommodating cavity 13 respectively；
Heating device 11 includes outlet pipe 111, cold water storage cistern 112, suction pump 113, communicating pipe 114, boiler 115, water inlet pipe 116
And S bend pipe 117, the inside of S bend pipe 117 setting and dry accommodating cavity 13, one end of S bend pipe 117 by outlet pipe 111 with it is cold
Water tank 112 is connected, and the other end of S bend pipe 117 is connected by water inlet pipe 116 with boiler 115, cold water storage cistern 112 and hot water
By being connected communicating pipe 114, one end of suction pump 113 is connected case 115 with cold water storage cistern 112, the other end of suction pump 113 and
Boiler 115 is connected, and boiler 115 is internally provided with heating device；
Vacuum evacuation device 12 includes vacuum-pumping tube 121 and vacuum pumping pump 122, one end and the drying accommodating cavity 13 of vacuum-pumping tube 121
It is connected, the other end of vacuum-pumping tube 121 is connected with vacuum pumping pump 122.
In use, water in heater heat hot water case 15 first in boiler 15, hot water is pumped into S type by suction pump 113
In pipe 117, realization is thermally dried the substance in the vessel being placed on S bend pipe 117, while by S bend pipe 117
It flows into cold water storage cistern 112 after hot water cooling, and is flowed back in boiler 115 via communicating pipe 114, and enter next circulation, from
And the temperature of S bend pipe 117 is made to keep higher state, realize the effect of the heat drying of S bend pipe 117, meanwhile, vacuum means
The inside for setting 12 pairs of dry accommodating cavities 13 carries out vacuumize process, prevents the impurity in air from generating shadow to substance to be dried
It rings；The whole process that the preparation facilities that the third aspect provides is dried all realizes the effect of stable drying process to graphene
Fruit can significantly improve the production efficiency of metallic graphite carbon alkene composite material and the electrode effect of metallic graphite carbon alkene.
Another kind embodiment shown in fig. 1, every section of top of S bend pipe 117 are provided with vessel accommodation groove 118, so that
The vessel for being placed on 117 surface of S bend pipe are more stable, prevent substance to be dried from pouring out.
Another kind embodiment shown in fig. 1, vacuum evacuation device 12 are set as multiple, enhance the effect vacuumized.
Another kind embodiment shown in fig. 1, dries and is provided with heating tube 119 on the inner wall of accommodating cavity 13, heating tube 119 exists
It is evenly distributed on the inner wall of dry accommodating cavity 13, heating tube 119 can be further improved the efficiency of drying process.
Those skilled in the art after considering the specification and implementing the invention disclosed here, will readily occur to of the invention its
Its embodiment.This application is intended to cover any variations, uses, or adaptations of the invention, these modifications, purposes or
Person's adaptive change follows general principle of the invention and including the undocumented common knowledge in the art of the disclosure
Or conventional techniques.The description and examples are only to be considered as illustrative, and true scope and spirit of the invention are by following
Claim is pointed out.
It should be understood that the present invention is not limited to the precise structure already described above and shown in the accompanying drawings, and
And various modifications and changes may be made without departing from the scope thereof.The scope of the present invention is limited only by the attached claims.
Claims (10)
1. a kind of metallic graphite carbon alkene composite material, which is characterized in that the metallic graphite carbon alkene composite material is prepared from the following raw materials:
Copper foil, dilute hydrochloric acid, hydrogen, methane, PMMA, Fecl3Solution, deionized water, charcoal-aero gel, metalliferous chemical plating fluid, acetone
And inert gas.
2. a kind of metallic graphite carbon alkene composite material as described in claim 1, which is characterized in that the inert gas is helium, neon,
One of argon and krypton.
3. a kind of preparation method of metallic graphite carbon alkene composite material, which comprises the following steps:
Copper foil is impregnated in dilute hydrochloric acid, 4~6min is ultrasonically treated in ultrasonic particle oscillator, obtains pretreatment copper foil；
Pretreatment copper foil is put into vacuum tank, hydrogen and methane is passed through into the vacuum tank, obtains being deposited with graphite
The copper foil of alkene；
PMMA is coated in the copper foil surface for being deposited with graphene, obtains the copper foil of coating PMMA；
The copper foil of the coating PMMA is placed in Fecl3In solution, standing 5~after ten minutes, it is cleaned, is gone with deionized water
The graphene of copper foil；
Charcoal-aero gel is placed in metalliferous chemical plating fluid, metal-carbon aerogel composite is obtained；
The metal-carbon aerogel composite is subjected to solvent displacement with acetone, obtains the metal-carbon aeroge of replacement Treatment
Composite material；
The metal-carbon aerogel composite of the replacement Treatment is heat-treated under inert gas protection, obtains nanoporous
Metal；
Graphene is pulled out from deionized water with the nano porous metal, and the graphene is put into drying box and is heated, is added
Hot temperature is 120~140 DEG C, and heating time is 40~50min, obtains metal-graphite alkene composite material preform；
The metal-graphite alkene composite material preform is placed in acetone and impregnates 20~30min, is impregnated after the acetone more renewed
10~12h obtains the metallic graphite carbon alkene composite material.
4. a kind of preparation method of metallic graphite carbon alkene composite material as claimed in claim 3, which is characterized in that described to described
It is passed through hydrogen and methane in vacuum tank, the ratio of hydrogen and methane is 15:25.
5. a kind of preparation method of metallic graphite carbon alkene composite material as claimed in claim 3, which is characterized in that it is described will be described
Before the metal-carbon aerogel composite of replacement Treatment is heat-treated under inert gas protection, further includes: at the displacement
In the metal-carbon aerogel composite merging autoclave of reason, CO is carried out2Supercritical drying, temperature condition are 50~60 DEG C, pressure
Power condition is 12~15MPa.
6. a kind of preparation method of metallic graphite carbon alkene composite material as claimed in claim 3, which is characterized in that it is described will be described
After metal-carbon aerogel composite carries out solvent displacement with acetone, the content of moisture is lower than in the acetone after exchange
2500ppm。
7. a kind of preparation facilities of metallic graphite carbon alkene composite material, for fishing out the nano porous metal from deionized water
The graphene is dried after graphene out, which is characterized in that the preparation facilities includes: drying box body (1), heating
Device (11) and vacuum evacuation device (12), the drying box body (1) are internally provided with dry accommodating cavity (13), described to add
Thermal (11) and the vacuum evacuation device (12) are connected with the dry accommodating cavity (13) respectively)；
The heating device (11) includes outlet pipe (111), cold water storage cistern (112), suction pump (113), communicating pipe (114), hot water
Case (115), water inlet pipe (116) and S bend pipe (117), the S bend pipe (117) are set to the interior of the dry accommodating cavity (13)
The one end in portion, the S bend pipe (117) is connected by the outlet pipe (111) with the cold water storage cistern (112), the S bend pipe
(117) the other end is connected by the water inlet pipe (116) with the boiler (115), the cold water storage cistern (112) with it is described
Boiler (115) is connected by the communicating pipe (114), one end and the cold water storage cistern (112) phase of the suction pump (113)
Connection, the other end of the suction pump (113) are connected with the boiler (115), the inside setting of the boiler (115)
There is heating device；
The vacuum evacuation device (12) includes vacuum-pumping tube (121) and vacuum pumping pump (122), and the one of the vacuum-pumping tube (121)
End is connected with the dry accommodating cavity (13), and the other end of the vacuum-pumping tube (121) is connected with the vacuum pumping pump (122)
It is logical.
8. a kind of preparation facilities of metallic graphite carbon alkene composite material as claimed in claim 7, which is characterized in that the S type
Every section of top of pipe (117) is provided with vessel accommodation groove (118).
9. a kind of preparation facilities of metallic graphite carbon alkene composite material as claimed in claim 7, which is characterized in that described to take out very
Empty device (12) is set as multiple.
10. a kind of preparation of metallic graphite carbon alkene composite material as described in claim 7 to 9 any one claim fills
It sets, which is characterized in that be provided with heating tube (119) on the inner wall of the dry accommodating cavity (13), the heating tube (119) is in institute
It states and is evenly distributed on the inner wall of dry accommodating cavity (13).
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