CN110002432A - A kind of multilevel structure graphene and its preparation method and application - Google Patents
A kind of multilevel structure graphene and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to nanocomposite technical fields more particularly to a kind of multilevel structure graphene and its preparation method and application.The preparation method of a kind of multilevel structure graphene provided by the invention, comprising the following steps: utilize chemical oxidization method vertical-growth Kocide SD nanometer rods on copper-based bottom, obtain copper-based bottom/Kocide SD nano-rod array material；Copper-based bottom/Kocide SD the nano-rod array material is placed in atmosphere of inert gases and is calcined, copper-based bottom/cupric oxide nano rod array material is obtained；Copper-based bottom/cupric oxide nano the rod array material is restored using hydrothermal reduction method, obtains copper-based bottom/copper nano-rod array material；Chemical vapor deposition graphene is utilized on the copper-based bottom/copper nanometer stick array, obtains copper-based bottom/grapheme material；Corrode the copper-based bottom in the copper-based bottom/grapheme material, obtains multilevel structure graphene, curling will not occur, stack phenomenon for multilevel structure graphene and electric conductivity is excellent.
Description
Technical field
The invention belongs to nanocomposite technical fields more particularly to a kind of multilevel structure graphene and preparation method thereof
And application.
Background technique
Graphene nanometer sheet is the hexagonal honeycomb shape sheet layer material that carbon atom is constituted with sp2 hybridized orbit, and graphene is received
Rice this structure of piece assign its many excellent physical and chemical properties, as superelevation specific surface area, good mechanical property, lead
Conductance hot property and chemical stability etc., thus graphene nanometer sheet is since 2004 are found, and is always the heat of research
Point, application field also relate to the every aspect in life.
Single layer or the graphene nanometer sheet of few number of plies are due to easily occurring curling, stacking with big surface energy and reuniting
Phenomenon, this greatly limits the performances of its physicochemical property, therefore while how to guarantee the electric conductivity of composite material, design
A kind of graphene composite material of the micro nano structure of morphology controllable is particularly important.
Summary of the invention
The purpose of the present invention is to provide a kind of multilevel structure graphene and its preparation method and application, the multilevel structures
Curling will not occur, stack phenomenon for graphene and electric conductivity is excellent.
To achieve the above object, one aspect of the present invention provides a kind of preparation method of multilevel structure graphene, including with
Lower step:
Using chemical oxidization method on copper-based bottom vertical-growth Kocide SD nanometer rods, obtain copper-based bottom/Kocide SD and receive
Rice rod array material；
Copper-based bottom/Kocide SD the nano-rod array material is placed in atmosphere of inert gases and is calcined, obtain copper-based bottom/
Cupric oxide nano rod array material；
Copper-based bottom/cupric oxide nano the rod array material is restored using hydrothermal reduction method, obtains copper-based bottom/copper nanometer rods
Array material；
Chemical vapor deposition graphene is utilized on the copper-based bottom/copper nano-rod array material, is obtained copper-based
Bottom/grapheme material；
Corrode the copper-based bottom in the copper-based bottom/grapheme material, obtains multilevel structure graphene.
Preferably, the multilevel structure graphene includes graphene nano pipe and graphene nanometer sheet, and the graphene is received
The length of mitron be 20~50nm, the graphene nanometer sheet with a thickness of 5~10nm.
Preferably, it is described using chemical oxidization method in vertical-growth Kocide SD nanometer rods on copper-based bottom the step of it
Before, it further include alternately washing copper-based bottom hydrochloric acid and water for several times, the copper-based bottom is copper sheet, copper mesh or copper foam.
Preferably, it is described utilize chemical oxidization method vertical-growth Kocide SD nanometer rods on copper-based bottom, obtain copper-based bottom/
The step of Kocide SD nano-rod array material, specifically includes, by copper-based bottom be immersed in 8~12mol/L sodium hydroxide solution and
In the mixed liquor of 20~30wt% ammonium hydroxide, it is stored at room temperature 1~for 24 hours, with water and ethyl alcohol, alternately washing is for several times, dry, obtains copper-based
Bottom/Kocide SD nano-rod array material；Wherein the volume ratio of the sodium hydroxide solution and ammonium hydroxide is 1~3:1.
It is preferably, described that the copper-based bottom/Kocide SD nano-rod array material is placed in atmosphere of inert gases and is calcined,
The step of obtaining copper-based bottom/cupric oxide nano rod array material specifically includes, by the copper-based bottom/Kocide SD nanometer stick array
Material is placed in 500~600 DEG C of 1~3h of calcining in argon atmosphere, obtains copper-based bottom/cupric oxide nano rod array material.
Preferably, described to restore the copper-based bottom/cupric oxide nano rod array material using hydrothermal reduction method, it obtains copper-based
The step of bottom/copper nano-rod array material, specifically includes,
Sodium hydroxide, reducing agent, water are configured into reducing agent solution；
Copper-based bottom/cupric oxide nano the rod array material is added in the reducing agent solution, in microwave reactor,
Microwave hydrothermal reacts 0.5~2h at 120~200 DEG C, is cooled to room temperature, and with water and ethyl alcohol, alternately washing is for several times, dry, obtains
Copper-based bottom/copper nano-rod array material.
Preferably, the reducing agent is one of glucose, hydrazine hydrate, sodium borohydride, ascorbic acid, oxalic acid.
Preferably, described that chemical vapor deposition graphite is utilized on the copper-based bottom/copper nano-rod array material
Alkene, the step of obtaining copper-based bottom/grapheme material, specifically include,
It is cleaned by ultrasonic the copper-based bottom/copper nano-rod array material；
Copper-based bottom/copper the nano-rod array material is placed in CVD tube furnace after ultrasonic cleaning, it is mixed in hydrogen and argon gas
It closes in atmosphere, the CVD tube furnace is warming up to 800~1000 DEG C with 5 DEG C/min heating rate, wherein the flow velocity of the hydrogen is
10~30sccm, the flow velocity of the argon gas are 600~1000sccm；
Adjusting hydrogen flow rate be 80~120sccm, be passed through carbon-source gas, wherein the flow velocity of carbon-source gas be 10~
50sccm turns off hydrogen and carbon-source gas after keeping the temperature 10~20min；
In argon atmosphere, the CVD tube furnace is down to room temperature, obtains copper-based bottom/grapheme material.
Another aspect of the present invention provides a kind of multilevel structure graphene, and the multilevel structure graphene is by any of the above-described system
Preparation Method prepares.
Another aspect of the invention provides the multilevel structure graphene in supercapacitor, conductive coating or electrically conductive ink
In application.
Compared with prior art, the invention has the following advantages:
The present invention provides the preparation methods of multilevel structure graphene, in copper substrate surfaces vertical-growth Kocide SD nanometer
Kocide SD nanometer rods are reduced to copper nanometer rods through multiple reduction treatment by stick, are deposited at copper-based bottom and the surface of copper nanometer rods
Graphene, copper substrate surfaces deposit to obtain graphene sheet layer structure, and copper nanorod surfaces deposit to obtain graphene tubular structure, stone
The vertical graphene tubular structure of black alkene lamellar structure, graphene sheet layer structure and graphene tubular structure are chemical vapour deposition technique
One step is made, and deposition thickness is uniform, and graphene sheet layer structure and graphene tubular structure are integrated, and is not two kinds of structures
Simple concatenation, be not in graphene stack, agglomeration, also reduce grapheme material simultaneously and the probability of defect occur.
And graphene sheet layer structure and graphene tubular structure form the three-dimensional conductive network system, electronics can either be in graphite
Free migration in alkene lamellar structure, also can be along graphene tubulose axis of no-feathering to quick transmitting, and electric conductivity is excellent.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to embodiment or description of the prior art
Needed in attached drawing be briefly described, it should be apparent that, the accompanying drawings in the following description is only of the invention some
Embodiment for those of ordinary skill in the art without any creative labor, can also be according to these
Attached drawing obtains other attached drawings.
Fig. 1 is the structural schematic diagram of copper-based bottom/grapheme material provided in an embodiment of the present invention；
Fig. 2 is the structural schematic diagram of multilevel structure graphene provided in an embodiment of the present invention；
Wherein, the copper-based bottom 100-/copper nano-rod array material；200- multilevel structure graphene.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
On the one hand the embodiment of the invention provides a kind of preparation method of multilevel structure graphene, packets combined with Figure 1 and Figure 2,
Include following steps:
S01, using chemical oxidization method on copper-based bottom vertical-growth Kocide SD nanometer rods, obtain copper-based bottom/hydroxide
Copper nano-rod array material；
S02, the copper-based bottom/Kocide SD nano-rod array material is placed in atmosphere of inert gases and is calcined, obtain copper
Substrate/cupric oxide nano rod array material；
S03, the copper-based bottom/cupric oxide nano rod array material is restored using hydrothermal reduction method, obtains copper-based bottom/copper and receives
Rice rod array material；
S04, chemical vapor deposition graphene is utilized on the copper-based bottom/copper nano-rod array material, obtain
Copper-based bottom/grapheme material；
Copper-based bottom in S05, the corrosion copper-based bottom/grapheme material, obtains multilevel structure graphene.
The embodiment of the invention provides the preparation methods of multilevel structure graphene, in copper substrate surfaces vertical-growth hydroxide
Kocide SD nanometer rods are reduced to copper nanometer rods through multiple reduction treatment, the table at copper-based bottom and copper nanometer rods by copper nanometer rods
Face deposits graphene, and copper substrate surfaces deposit to obtain graphene sheet layer structure, and copper nanorod surfaces deposit to obtain graphene tubulose
Structure, graphene sheet layer structure vertical graphene tubular structure, graphene sheet layer structure and graphene tubular structure are chemical gas
One step of phase sedimentation is made, and deposition thickness is uniform, and graphene sheet layer structure and graphene tubular structure are integrated, and is not
The simple concatenation of two kinds of structures is not in graphene stacking, agglomeration, and also reducing grapheme material defect occurs simultaneously
Probability.
And graphene sheet layer structure and graphene tubular structure form the three-dimensional conductive network system, electronics can either be in graphite
Free migration in alkene lamellar structure, also can be along graphene tubulose axis of no-feathering to quick transmitting, and electric conductivity is excellent.
For the present embodiment through chemical vapour deposition technique in copper-based bottom/copper nanometer rods, a step deposits the graphite of multilevel structure
Alkene, obtained multilevel structure graphene is not in stacking phenomenon, and electric conductivity is excellent.
Wherein, the multilevel structure graphene includes graphene nano pipe and graphene nanometer sheet, the graphene nano
The length of pipe be 20~50nm, the graphene nanometer sheet with a thickness of 5~10nm.
Specifically, graphene tubular structure is graphene nano pipe, and the graphene sheet layer structure is graphene nanometer sheet,
The graphene nanometer sheet with a thickness of 5~10nm, graphene nanometer sheet is single-layer graphene nanostructure, is further prevented out
Now stack phenomenon；The length of the graphene nano pipe is 20~50nm, and the length of graphene nano pipe is less than 20nm, length
It is too short, it is bigger to there is a possibility that stacking phenomenon；The length of graphene nano pipe is greater than 50nm, and length is excessively high, and graphene is received
Being broken occurs in mitron or a possibility that defect is bigger.
It wherein, before step S01, further include alternately washing copper-based bottom hydrochloric acid and water for several times, the copper-based bottom is
Copper sheet, copper mesh or copper foam.
Copper-based bottom alternately is washed with hydrochloric acid and water, the surface at copper-based bottom is cleaned, to remove the impurity on its surface；The hydrochloric acid
Concentration 2~5mol/L can be used.
Wherein, step S01 is specifically included, by copper-based bottom be immersed in 8~12mol/L sodium hydroxide solution and 20~
In the mixed liquor of 30wt% ammonium hydroxide, it is stored at room temperature 1~for 24 hours, with water and ethyl alcohol, alternately washing is for several times, dry, obtains copper-based bottom/hydrogen
Cupric oxide nano rod array material；Wherein the volume ratio of the sodium hydroxide solution and ammonium hydroxide is 1~3:1.Wherein, the ethyl alcohol
Dehydrated alcohol can be used；The drying can use dries in air.
Wherein, step S02 is specifically included, and the copper-based bottom/Kocide SD nano-rod array material is placed in argon atmosphere
In 500~600 DEG C of 1~3h of calcining, obtain copper-based bottom/cupric oxide nano rod array material.It calcines, prevents in atmosphere of inert gases
Other miscellaneous by-products are only generated, sintered structure is more stable.
Wherein, step S03 is specifically included, and sodium hydroxide, reducing agent, water are configured reducing agent solution；
Copper-based bottom/cupric oxide nano the rod array material is added in the reducing agent solution, in microwave reactor,
Microwave hydrothermal reacts 0.5~2h at 120~200 DEG C, is cooled to room temperature, and with water and ethyl alcohol, alternately washing is for several times, dry, obtains
Copper-based bottom/copper nano-rod array material.By microwave hydrothermal, reaction system is heated more evenly, and reduces the reaction time, further
By the control of temperature and time, so that reaction sufficiently carries out.
Preferably, the reducing agent is one of glucose, hydrazine hydrate, sodium borohydride, ascorbic acid, oxalic acid.Raw material
It is easy to get, preparation is more convenient.
Wherein, step S04 is specifically included: the ultrasonic cleaning copper-based bottom/copper nano-rod array material；
Copper-based bottom/copper the nano-rod array material is placed in CVD tube furnace after ultrasonic cleaning, it is mixed in hydrogen and argon gas
It closes in atmosphere, the CVD tube furnace is warming up to 800~1000 DEG C with 5 DEG C/min heating rate, wherein the flow velocity of the hydrogen is
10~30sccm, the flow velocity of the argon gas are 600~1000sccm；
Adjusting hydrogen flow rate be 80~120sccm, be passed through carbon-source gas, wherein the flow velocity of carbon-source gas be 10~
50sccm turns off hydrogen and carbon-source gas after keeping the temperature 10~20min；
In argon atmosphere, the CVD tube furnace is down to room temperature, obtains copper-based bottom/grapheme material.The graphene of deposition
The film thickness of material is uniform, and membrane structure is stablized.
Preferably, the carbon-source gas is one of methane, ethylene, acetylene；Carbon-source gas is easy to get, easy to operate.
On the other hand the embodiment of the present invention provides a kind of multilevel structure graphene, by implementation any in the various embodiments described above
The preparation method of multilevel structure graphene described in example is prepared.
The multilevel structure graphene, thickness is uniform, is not susceptible to stack, reunite, compared to traditional graphene film
Layer, electric conductivity are excellent.
The another aspect of the embodiment of the present invention provides multilevel structure graphene in supercapacitor, conductive coating or conductive oil
Application in ink.
Below by way of specific embodiment, the invention will be further described:
Embodiment 1
A kind of preparation method of multilevel structure graphene, comprising the following steps:
S101, copper sheet is alternately washed for several times with the hydrochloric acid and water of 4mol/L, the copper sheet after washing is immersed in 200mL
In the mixed liquor of 10mol/L sodium hydroxide solution and 100mL 25wt% ammonium hydroxide, 12h is stood under room temperature；Then with water and
Dehydrated alcohol washs copper sheet for several times respectively, dries in air, obtains copper-based bottom/Kocide SD nano-rod array material；
S102, the copper-based bottom/Kocide SD nano-rod array material is placed in the lower 550 DEG C of calcinings 2h of argon atmosphere, obtained
To copper-based bottom/cupric oxide nano rod array material；
S103, by 8g sodium hydroxide and 8g glucose mixed dissolution in 80mL water, the copper-based bottom/oxygen is added thereto
Change copper nano-rod array material, and be transferred in microwave reactor, microwave hydrothermal reacts 1h at 160 DEG C, to after reaction
It is cooled to room temperature, takes out the solid obtained after reaction, washed respectively for several times with water and dehydrated alcohol, the dry 40min at 60 DEG C,
Obtain copper-based bottom/copper nano-rod array material；
S104, the copper-based bottom/copper nano-rod array material is successively cleaned by ultrasonic in water, dehydrated alcohol and acetone
Then 20min is put it into CVD tube furnace, flow velocity be 20sccm hydrogen and flow velocity be 800sccm argon gas gaseous mixture
Under atmosphere, after CVD tube furnace is warming up to 1000 DEG C with the rate of 5 DEG C/min, then adjusting hydrogen flow rate is 100sccm, and with
The flow velocity of 30sccm is passed through methane gas, after keeping the temperature 15min, turns off hydrogen and methane gas, room temperature is down in argon atmosphere,
Sample is taken out, copper-based bottom/grapheme material is obtained；
S105, the copper-based bottom/grapheme material is immersed in 0.5mol/L ferric chloride solution and is corroded, stand two
It is centrifuged after the disappearance of copper substrate corrosion, and is washed with water for several times, and obtained black solid is dry at 60 DEG C
30min obtains multilevel structure graphene.
Embodiment 2
A kind of preparation method of multilevel structure graphene, comprising the following steps:
S201, copper sheet is alternately washed for several times with the hydrochloric acid and water of 4mol/L, the copper sheet after washing is immersed in 100mL
In the mixed liquor of 10mol/L sodium hydroxide solution and 100mL 25wt% ammonium hydroxide, 12h is stood under room temperature；Then with water and
Dehydrated alcohol washs copper sheet for several times respectively, dries in air, obtains copper-based bottom/Kocide SD nano-rod array material；
S202, the copper-based bottom/Kocide SD nano-rod array material is placed in the lower 500 DEG C of calcinings 3h of argon atmosphere, obtained
To copper-based bottom/cupric oxide nano rod array material；
S203, by 4g sodium hydroxide and 8g ascorbic acid mixed dissolution in 80mL water, be added thereto the copper-based bottom/
Cupric oxide nano rod array material, and be transferred in microwave reactor, microwave hydrothermal reacts 2h at 120 DEG C, to the end of reacting
After be cooled to room temperature, take out obtained solid after reaction, washed respectively for several times with water and dehydrated alcohol, it is dry at 50 DEG C
60min obtains copper-based bottom/copper nano-rod array material；
S204, the copper-based bottom/copper nano-rod array material is successively cleaned by ultrasonic in water, dehydrated alcohol and acetone
Then 10min is put it into CVD tube furnace, flow velocity be 10sccm hydrogen and flow velocity be 600sccm argon gas gaseous mixture
Under atmosphere, after CVD tube furnace is warming up to 800 DEG C with the rate of 5 DEG C/min, then adjusting hydrogen flow rate is 80sccm, and with
The flow velocity of 10sccm is passed through ethylene gas, after keeping the temperature 20min, turns off hydrogen and ethylene gas, room temperature is down in argon atmosphere,
Sample is taken out, copper-based bottom/grapheme material is obtained；
S205, the copper-based bottom/grapheme material is immersed in 0.1mol/L ferric chloride solution and is corroded, stand two
It is centrifuged after the disappearance of copper substrate corrosion, and is washed with water for several times, and obtained black solid is dry at 50 DEG C
50min obtains multilevel structure graphene.
Embodiment 3
A kind of preparation method of multilevel structure graphene, comprising the following steps:
S301, copper sheet is alternately washed for several times with the hydrochloric acid and water of 4mol/L, the copper sheet after washing is immersed in 300mL
In the mixed liquor of 10mol/L sodium hydroxide solution and 100mL 25wt% ammonium hydroxide, 1h is stood under room temperature；Then water and nothing are used
Water-ethanol washs copper sheet for several times respectively, dries in air, obtains copper-based bottom/Kocide SD nano-rod array material；
S302, the copper-based bottom/Kocide SD nano-rod array material is placed in the lower 600 DEG C of calcinings 1h of argon atmosphere, obtained
To copper-based bottom/cupric oxide nano rod array material；
S303, by 16g sodium hydroxide and 8g oxalic acid mixed dissolution in 80mL water, the copper-based bottom/oxygen is added thereto
Change copper nano-rod array material, and be transferred in microwave reactor, microwave hydrothermal reacts 0.5h at 200 DEG C, to the end of reacting
After be cooled to room temperature, take out obtained solid after reaction, washed respectively for several times with water and dehydrated alcohol, it is dry at 80 DEG C
20min obtains copper-based bottom/copper nano-rod array material；
S304, the copper-based bottom/copper nano-rod array material is successively cleaned by ultrasonic in water, dehydrated alcohol and acetone
Then 30min is put it into CVD tube furnace, flow velocity be 30sccm hydrogen and flow velocity be 1000sccm argon gas mixing
Under atmosphere, after CVD tube furnace is warming up to 900 DEG C with the rate of 5 DEG C/min, then adjusting hydrogen flow rate is 120sccm, and with
The flow velocity of 50sccm is passed through acetylene gas, after keeping the temperature 10min, turns off hydrogen and acetylene gas, room temperature is down in argon atmosphere,
Sample is taken out, copper-based bottom/grapheme material is obtained；
S305, the copper-based bottom/grapheme material is immersed in 1mol/L ferric chloride solution and is corroded, stand two days,
It after the disappearance of copper substrate corrosion, is centrifuged, and is washed with water for several times, obtained black solid is dried into 20min at 80 DEG C,
Obtain multilevel structure graphene.
Above-described specific embodiment, has been further described the present invention, it should be understood that more than
It is described to be merely a preferred embodiment of the present invention, it is not intended to limit the scope of protection of the present invention, it is all in spirit and original of the invention
Within then, any modification, equivalent substitution, improvement and etc. done, all belong to the scope of protection of the present invention within.
Claims (10)
1. a kind of preparation method of multilevel structure graphene, which comprises the following steps:
Using chemical oxidization method on copper-based bottom vertical-growth Kocide SD nanometer rods, obtain copper-based bottom/Kocide SD nanometer rods
Array material；
Copper-based bottom/Kocide SD the nano-rod array material is placed in atmosphere of inert gases and is calcined, copper-based bottom/oxidation is obtained
Copper nano-rod array material；
Copper-based bottom/cupric oxide nano the rod array material is restored using hydrothermal reduction method, obtains copper-based bottom/copper nanometer stick array
Material；
Chemical vapor deposition graphene is utilized on the copper-based bottom/copper nano-rod array material, obtains copper-based bottom/stone
Black alkene material；
Corrode the copper-based bottom in the copper-based bottom/grapheme material, obtains multilevel structure graphene.
2. a kind of preparation method of multilevel structure graphene according to claim 1, which is characterized in that the multilevel structure
Graphene includes graphene nano pipe and graphene nanometer sheet, and the length of the graphene nano pipe is 20~50nm, the stone
Black alkene nanometer sheet with a thickness of 5~10nm.
3. a kind of preparation method of multilevel structure graphene according to claim 1, which is characterized in that in the utilizationization
Before oxidizing process is learned the vertical-growth Kocide SD nanometer rods on copper-based bottom the step of, further include, by copper-based bottom hydrochloric acid and water
Alternately for several times, the copper-based bottom is copper sheet, copper mesh or copper foam for washing.
4. a kind of preparation method of multilevel structure graphene according to claim 1, which is characterized in that described to utilize chemistry
Oxidizing process vertical-growth Kocide SD nanometer rods on copper-based bottom obtain copper-based bottom/Kocide SD nano-rod array material step
Suddenly it specifically includes, copper-based bottom is immersed in the sodium hydroxide solution of 8~12mol/L and the mixed liquor of 20~30wt% ammonium hydroxide,
It is stored at room temperature 1~for 24 hours, with water and ethyl alcohol, alternately washing is for several times, dry, obtains copper-based bottom/Kocide SD nano-rod array material；
Wherein the volume ratio of the sodium hydroxide solution and ammonium hydroxide is 1~3:1.
5. a kind of preparation method of multilevel structure graphene according to claim 1, which is characterized in that described by the copper
Substrate/Kocide SD nano-rod array material is placed in atmosphere of inert gases and calcines, and obtains copper-based bottom/cupric oxide nano-rod array
The step of material, specifically includes, and the copper-based bottom/Kocide SD nano-rod array material is placed in 500~600 in argon atmosphere
DEG C calcining 1~3h, obtain copper-based bottom/cupric oxide nano rod array material.
6. a kind of preparation method of multilevel structure graphene according to claim 1, which is characterized in that described to utilize hydro-thermal
The step of reduction method restores the copper-based bottom/cupric oxide nano rod array material, obtains copper-based bottom/copper nano-rod array material tool
Body includes,
Sodium hydroxide, reducing agent, water are configured into reducing agent solution；
Copper-based bottom/cupric oxide nano the rod array material is added in the reducing agent solution, in microwave reactor,
Microwave hydrothermal reacts 0.5~2h at 120~200 DEG C, is cooled to room temperature, and with water and ethyl alcohol, alternately washing is for several times, dry, obtains copper
Substrate/copper nano-rod array material.
7. a kind of preparation method of multilevel structure graphene according to claim 6, which is characterized in that the reducing agent is
One of glucose, hydrazine hydrate, sodium borohydride, ascorbic acid, oxalic acid.
8. a kind of preparation method of multilevel structure graphene according to claim 1, which is characterized in that described in the copper
Chemical vapor deposition graphene is utilized on substrate/copper nano-rod array material, obtains the step of copper-based bottom/grapheme material
Suddenly it specifically includes,
It is cleaned by ultrasonic the copper-based bottom/copper nano-rod array material；
Copper-based bottom/copper the nano-rod array material is placed in CVD tube furnace after ultrasonic cleaning, in hydrogen and argon gas gaseous mixture
In atmosphere, the CVD tube furnace is warming up to 800~1000 DEG C with 5 DEG C/min heating rate, wherein the flow velocity of the hydrogen be 10~
30sccm, the flow velocity of the argon gas are 600~1000sccm；
Adjusting hydrogen flow rate is 80~120sccm, is passed through carbon-source gas, and wherein the flow velocity of carbon-source gas is 10~50sccm, is protected
After 10~20min of temperature, turn off hydrogen and carbon-source gas；
In argon atmosphere, the CVD tube furnace is down to room temperature, obtains copper-based bottom/grapheme material.
9. a kind of multilevel structure graphene, which is characterized in that the multilevel structure graphene is by any right of claim 1~8
It is required that the preparation method of the multilevel structure graphene is prepared.
10. multilevel structure graphene answering in supercapacitor, conductive coating or electrically conductive ink according to claim 9
With.
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| CN114530606A (en) * | 2022-01-06 | 2022-05-24 | 清华大学深圳国际研究生院 | Three-dimensional lithium-philic carbon interface modified copper-based current collector and preparation method and application thereof |
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