CN103832999B - Carbon nanometer wall and prepared the method for graphene nanobelt by it - Google Patents
Carbon nanometer wall and prepared the method for graphene nanobelt by it Download PDFInfo
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- CN103832999B CN103832999B CN201210490930.0A CN201210490930A CN103832999B CN 103832999 B CN103832999 B CN 103832999B CN 201210490930 A CN201210490930 A CN 201210490930A CN 103832999 B CN103832999 B CN 103832999B
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Abstract
The present invention relates to a kind of carbon nanometer wall and prepared the method for graphene nanobelt by it, comprise the steps: etched substrate; Prepare carbon nanometer wall; Prepare carbonoxide nanometer wall slurry; Prepare graphene nanobelt.The preparation method of carbon nanometer wall of the present invention, etching method and photochemical catalysis chemical Vapor deposition process is utilized to prepare vertical carbon nanometer wall, preparation technology is simple, condition is easily controlled, and effectively can avoid produced problem in the plasma method preparation process in existing method, make the thickness of carbon nanometer wall evenly, structure is more complete, the preparation of graphene nanobelt then have employed hot reducing method and peels off carbonoxide nanometer wall, splitting time is short, and preparation efficiency is high, and technique is simple.
Description
Technical field
The present invention relates to chemical material synthesis field, particularly relate to a kind of carbon nanometer wall and preparation method thereof.The invention still further relates to the graphene nanobelt and preparation method that utilize this carbon nanometer wall to prepare.
Background technology
The kind of carbon material comprises the soccerballene (C of zero dimension
60deng), the carbon nanotube, carbon nanofiber etc. of one dimension, the Graphene of two dimension, three-dimensional graphite, diamond etc.Carbon nanometer wall (english abbreviation CNW) is the carbon nano structure with two-dimensional diffusion structure, its most typical shape characteristic can grow perpendicular to substrate material surface exactly, and be greater than the wall-like structure of Graphene for thickness, they are completely different from the feature of soccerballene, carbon nanotube, Graphene etc., can be used as the raw material of other carbon material of preparation.
Before Graphene finds, people just in the preparation method of research carbon nanometer wall, just had the preparation of carbon nanometer wall and the reported in literature of related application thereof as far back as 2002.But no matter be early stage or recent preparation method, all can relate to reaction and carry out under plasma atmosphere, this will cause certain destruction to the structure of CNW.
Graphene nanobelt not only has the performance of Graphene, also possesses the performance that some are special, and such as its length-to-diameter ratio is very large, can up to thousands of times, can copper conductor be replaced at integrated circuit connection, to improve integrated level further, also can carry out modification to its structure and be prepared into switch device.But at present due to the problem that there is size control difficulty in graphene nanobelt preparation process, yield poorly, thus limit its application.
Summary of the invention
First goal of the invention of the present invention is to solve above-mentioned prior art Problems existing and deficiency, a kind of carbon nanometer wall and preparation method thereof is provided, etching method and photochemical catalysis chemical Vapor deposition process is utilized to prepare vertical carbon nanometer wall, its preparation technology is simple, condition is easily controlled, and effectively can avoid produced problem in the plasma method preparation process in existing method, make the thickness of carbon nanometer wall evenly, structure is more complete.
Second goal of the invention of the present invention is to provide a kind of graphene nanobelt and preparation method thereof, and adopt hot reducing method to peel off carbonoxide nanometer wall, splitting time is short, and preparation efficiency is high, and technique is simple.
For reaching the first goal of the invention of the present invention, the first technical scheme that the present invention adopts is: a kind of preparation method of carbon nanometer wall, comprises the steps: (a) etched substrate: the dilute acid soln of substrate 0.01 ~ 1mol/L etching cleaned up after 0.5 ~ 10 minute.
B () prepares carbon nanometer wall: described substrate is placed in oxygen-free environment and is heated to 600 ~ 900 DEG C; then substrate surface described in UV-irradiation is opened; pass into carbonaceous material and protective gas again and keep 30 ~ 300 minutes, obtaining carbon nanometer wall at described substrate surface.
In described step (a), described substrate is a kind of in iron foil, nickel foil, cobalt paper tinsel, and described dilute acid soln is the one in hydrochloric acid, nitric acid, sulfuric acid, and the concentration of described dilute acid soln is 0.1 ~ 0.5mol/L.
In described step (a), the time of described etching is 1 ~ 3 minute, and described substrate deionized water, ethanol, acetone clean successively.
In described step (b); described carbonaceous material is the one in methane, ethane, propane, acetylene, ethanol; described protective gas is the one in helium, nitrogen, argon gas; the flow velocity passing into described carbonaceous material is 10 ~ 1000sccm, and the volume ratio of described carbonaceous material and described protective gas is (2 ~ 10): 1.
The present invention also comprises the carbon nanometer wall utilizing above-mentioned preparation method to obtain.
For reaching the second goal of the invention of the present invention, the second technical scheme that the present invention adopts comprises and utilizes above-mentioned carbon nanometer wall to prepare the method for graphene nanobelt, draw together following steps: (c) prepares carbonoxide nanometer wall slurry: get described carbon nanometer wall and join in the vitriol oil, add potassium permanganate again and stir, add deionized water again and carry out suction filtration, afterwards with hydrochloric acid carry out washing, suction filtration in neutral, obtains carbonoxide nanometer wall slurry to filtrate.
D () prepares graphene nanobelt: after described carbonoxide nanometer wall slurry drying to constant weight, transfers in the protective atmosphere of 500 ~ 1000 DEG C to heat after 10 ~ 300 minutes and peels off, after being cooled to room temperature, namely obtain graphene nanobelt.
In described step (c), the mass volume ratio of described carbon nanometer wall, the described vitriol oil, described potassium permanganate and described hydrogen peroxide is: 50g:1150mL:150g:250mL.
In described step (d), described drying is carried out in vacuum drying oven, and the temperature of described drying is 60 ~ 100 DEG C.
In described step (d), described protective atmosphere is at least one in hydrogen, helium, nitrogen, argon gas.
The present invention also comprises the graphene nanobelt utilizing above-mentioned preparation method to obtain.
Compared with prior art, carbon nanometer wall of the present invention and prepared the method for graphene nanobelt by it, there is following advantage: 1. adopt etching method to prepare vertical carbon nanometer wall with photochemical catalysis chemical Vapor deposition process, its preparation technology is simple, condition is easily controlled, shorten etching time while improve production efficiency, and photochemical catalysis effectively can reduce temperature of reaction, reduce energy consumption, reduce production cost, and effectively can avoid produced problem in the plasma method preparation process in existing method, make the thickness of carbon nanometer wall evenly, structure is more complete.
2. adopt hot reducing method to peel off carbonoxide nanometer wall, splitting time is short, and preparation efficiency is high, and technique is simple.
3. the high and raw material of the productive rate of graphene nanobelt can be prepared voluntarily, lessens production cost like this.
4. equipment required in preparation process is all common chemical industry equipment, can save research and development equipment cost, is applicable to scale operation.
Accompanying drawing explanation
Fig. 1 is that the carbon nanometer wall SEM prepared by the embodiment of the present invention 1 schemes.
Fig. 2 is that the graphene nanobelt SEM prepared by the embodiment of the present invention 1 schemes.
Embodiment
Below in conjunction with embodiment, elaboration is further given to the present invention.
The preparation process of nanometer wall of the present invention is roughly divided into following steps.
Prepare carbon nanometer wall: (a) etched substrate: substrate is put into the dilute acid soln etching 0.5 ~ 10 minute that concentration is 0.01 ~ 1mol/L, etch rear deionized water, ethanol, acetone cleans.
This step object is: by making metal liner end eclipse surface produce defect to metal substrate etching, effectively can improve the surface tissue of metal substrate, carbon nanometer wall energy is enough grown at this metal substrate surface.
Wherein, the preferred time etching this metal substrate is 60 ~ 180 seconds, and the preferred dilute acid soln concentration of etching metal substrate is 0.1 ~ 0.5mol/L.Preferred etching condition, can reach the effect of good etching above, improves the growth efficiency of carbon nanometer wall.
B () prepares carbon nanometer wall.
(b
1) cleaned substrate is placed in oxygen-free environment is heated to 600 ~ 900 DEG C; open ultraviolet source equipment again; make UV-irradiation at substrate surface; then by volume (2 ~ 10): 1 passes into carbonaceous material (flow is 10 ~ 1000sccm) and protective gas, and keeps 30 ~ 300 minutes.
This step object is: the air got rid of in reaction chamber can remove the oxygen in reaction chamber, and avoid the participation of oxygen and affect the growth of carbon nanometer wall, the growth for carbon nanometer wall provides a stable environment.
(b
2) reacted after, stop pass into carbonaceous material, stop silicon; and close ultraviolet source equipment, stop after question response room is cooled to room temperature passing into protective gas, namely obtain carbon nanometer wall at substrate surface; it is scraped from substrate surface, just obtains pulverous carbon nanometer wall.
Wherein, substrate is a kind of in iron foil, nickel foil, cobalt paper tinsel, and dilute acid soln is the one in hydrochloric acid, nitric acid, sulfuric acid.
Protective gas is the one in helium, nitrogen, argon gas, and carbonaceous material is the one in methane, ethane, propane, acetylene, ethanol.
The preparation process of graphene nanobelt of the present invention is roughly divided into following steps:
Prepare graphene nanobelt: (c) prepares carbonoxide nanometer wall slurry: by above-mentioned steps (b
2) in pulverous carbon nanometer wall join in the vitriol oil of 0 DEG C, add potassium permanganate again, keep the temperature of mixture to remain on less than 10 DEG C, after stirring 2h, 24h is stirred in room-temperature water bath, under condition of ice bath, slowly add deionized water again, after 15min, then add the deionized water suction filtration containing 30% concentration hydrogen peroxide, mixture color becomes glassy yellow afterwards, wash with the hydrochloric acid that concentration is 10% again, after suction filtration is neutrality to filtrate, namely obtain carbonoxide nanometer wall slurry.
Wherein, the mass volume ratio of carbon nanometer wall, the vitriol oil, potassium permanganate and hydrogen peroxide is: 50g:1150mL:150g:250mL.
D () prepares graphene nanobelt: transfer in vacuum drying oven by carbonoxide nanometer wall slurry; be dried to constant weight at 60 ~ 100 DEG C after; transferring to temperature is again heat in the protective atmosphere of 500 ~ 1000 DEG C after 10 ~ 300 minutes to peel off, and to be cooledly can obtain graphene nanobelt to room temperature.
Wherein, protective atmosphere is at least one in hydrogen, helium, nitrogen, argon gas.
The present invention also comprises the carbon nanometer wall and graphene nanobelt that utilize above-mentioned preparation method to obtain.
Be specifically described with the preparation process of embodiment 1 ~ 3 to carbon nanometer wall of the present invention and graphene nanobelt below.
Embodiment 1 prepares carbon nanometer wall: (a) etched substrate: nickel foil is put into the dilute hydrochloric acid solution etching 0.5 minute that concentration is 1mol/L, the good rear deionized water of etching, ethanol, acetone clean.
B () prepares carbon nanometer wall.
(b
1) cleaned nickel foil is put into reaction chamber; and after getting rid of the air in reaction chamber, nickel foil is heated to 900 DEG C; then ultraviolet source equipment is opened; make UV-irradiation on nickel foil surface; then carbonaceous material methane (flow is 200sccm) and protective gas nitrogen is passed into; the volume ratio of methane and nitrogen is 2:1, and keeps 100 minutes.
(b
2) reacted after, stop pass into carbonaceous material methane, stop to nickel foil heating and close light source; stop after question response room is cooled to room temperature passing into protective gas nitrogen; carbon nanometer wall can be obtained on nickel foil surface, it is scraped from nickel foil surface, just obtain carbon nanometer wall powder.
Prepare graphene nanobelt: (c) prepares carbonoxide nanometer wall slurry: 50g carbon nanometer wall is added 0 DEG C, in the vitriol oil of 1.15L, add 150g potassium permanganate again, the temperature of mixture remains on less than 10 DEG C, stir 2h, then after room-temperature water bath stirs 24h, 4.6L deionized water is slowly added under condition of ice bath, after 15min, add 14L deionized water (wherein containing 250mL concentration is the hydrogen peroxide of 30%) again, mixture color becomes glassy yellow afterwards, suction filtration, wash with the hydrochloric acid that 2.5L concentration is 10% again, suction filtration, until filtrate is in neutral.
D () prepares graphene nanobelt: carbonoxide nanometer wall slurry to be transferred in vacuum drying oven 60 DEG C be dried to constant weight after, transferring to temperature is again heat 30 minutes in the hydrogen atmosphere of 800 DEG C, to be cooledly to collect to room temperature, just obtain graphene nanobelt.
Embodiment 2 prepares carbon nanometer wall: (a) etched substrate: iron foil is put into the dilution heat of sulfuric acid etching 4 minutes that concentration is 0.5mol/L, the good rear deionized water of etching, ethanol, acetone clean.
B () prepares carbon nanometer wall.
(b
1) cleaned nickel foil is put into reaction chamber; after getting rid of the air in reaction chamber, iron foil is heated to 600 DEG C; then ultraviolet source equipment is opened; make UV-irradiation on iron foil surface; then carbonaceous material ethane (flow is 100sccm) and protective gas argon gas is passed into; the volume ratio of methane and argon gas is 5:1, and keeps 200 minutes.
(b
2) reacted after, stop pass into carbonaceous material ethane, stop to iron foil heating and close light source; stop after question response room is cooled to room temperature passing into protective gas argon gas; carbon nanometer wall can be obtained on iron foil surface, it is scraped from iron foil surface, just obtain carbon nanometer wall powder.
Prepare graphene nanobelt: (c) prepares carbonoxide nanometer wall slurry: 50g carbon nanometer wall is added 0 DEG C, in the vitriol oil of 1.15L, add 150g potassium permanganate again, the temperature of mixture remains on less than 10 DEG C, stir 2h, then after room-temperature water bath stirs 24h, 4.6L deionized water is slowly added under condition of ice bath, after 15min, add 14L deionized water (wherein containing 250mL concentration is the hydrogen peroxide of 30%) again, mixture color becomes glassy yellow afterwards, suction filtration, wash with the hydrochloric acid that 2.5L concentration is 10% again, suction filtration, until filtrate is in neutral.
D () prepares graphene nanobelt: carbonoxide nanometer wall slurry to be transferred in vacuum drying oven 80 DEG C be dried to constant weight after, transferring to temperature is again heat 10 minutes in the nitrogen atmosphere of 500 DEG C, to be cooledly to collect to room temperature, just obtain graphene nanobelt.
Embodiment 3 prepares carbon nanometer wall: (a) etched substrate: cobalt paper tinsel is put into the dilute nitric acid solution etching 10 minutes that concentration is 0.01mol/L, the good rear deionized water of etching, ethanol, acetone clean.
B () prepares carbon nanometer wall.
(b
1) cleaned cobalt paper tinsel is put into reaction chamber; after getting rid of the air in reaction chamber, cobalt paper tinsel is heated to 700 DEG C; then ultraviolet source equipment is opened; make UV-irradiation on cobalt paper tinsel surface; then carbonaceous material acetylene (flow is 10sccm) and protective gas helium is passed into; the volume ratio of acetylene and helium is 8:1, and keeps 300 minutes.
(b
2) reacted after, stop pass into carbonaceous material acetylene, stop to cobalt paper tinsel heating and close light source; stop after question response room is cooled to room temperature passing into protective gas helium; carbon nanometer wall can be obtained on cobalt paper tinsel surface, it is scraped from cobalt paper tinsel surface, just obtain carbon nanometer wall powder.
Prepare graphene nanobelt: (c) prepares carbonoxide nanometer wall slurry: 50g carbon nanometer wall is added 0 DEG C, in the vitriol oil of 1.15L, add 150g potassium permanganate again, the temperature of mixture remains on less than 10 DEG C, stir 2h, then after room-temperature water bath stirs 24h, 4.6L deionized water is slowly added under condition of ice bath, after 15min, add 14L deionized water (wherein containing 250mL concentration is the hydrogen peroxide of 30%) again, mixture color becomes glassy yellow afterwards, suction filtration, wash with the hydrochloric acid that 2.5L concentration is 10% again, suction filtration, until filtrate is in neutral.
D () prepares graphene nanobelt: carbonoxide nanometer wall slurry to be transferred in vacuum drying oven 100 DEG C be dried to constant weight after, transferring to temperature is again heat 50 minutes in the argon gas atmosphere of 1000 DEG C, to be cooledly to collect to room temperature, just obtain graphene nanobelt.
As can be seen from the carbon nanometer wall SEM figure in Fig. 1, the carbon nanometer wall thickness adopting photochemical catalysis chemical Vapor deposition process to prepare is even, is 20 ~ 40nm, and basic vertical substrates growth, high consistency is good.As shown in the graphene nanobelt SEM figure of Fig. 2, after carbon nanometer wall is stripped into graphene nanobelt, even width, is about 30 ~ 60nm, and length is about 5 ~ 10um.
Following table 1 is the design parameter of embodiment 4 ~ 11, and the processing step of each embodiment is identical with embodiment 1 ~ 3, and difference is processing parameter and processing condition, repeats no more its processing step at this.
Carbon nanometer wall of the present invention and prepare the method for graphene nanobelt, there is following advantage: 1. adopt etching method to prepare vertical carbon nanometer wall with photochemical catalysis chemical Vapor deposition process, its preparation technology is simple, condition is easily controlled, shorten etching time while improve production efficiency, and photochemical catalysis effectively can reduce temperature of reaction, reduce energy consumption, reduce production cost, and effectively can avoid produced problem in the plasma method preparation process in existing method, make the thickness of carbon nanometer wall evenly, structure is more complete.
2. adopt hot reducing method to peel off carbonoxide nanometer wall, splitting time is short, and preparation efficiency is high, and technique is simple.
3. the high and raw material of the productive rate of graphene nanobelt can be prepared voluntarily, lessens production cost like this.
4. equipment required in preparation process is all common chemical industry equipment, can save research and development equipment cost, is applicable to scale operation.
Foregoing; be only preferred embodiment of the present invention; not for limiting embodiment of the present invention; those of ordinary skill in the art are according to central scope of the present invention and spirit; can carry out corresponding flexible or amendment very easily, therefore protection scope of the present invention should be as the criterion with the protection domain required by claims.
Table 1
Claims (4)
1. a method for graphene nanobelt prepared by carbon nanometer wall, it is characterized in that, comprises the steps:
C () prepares carbonoxide nanometer wall slurry: get described carbon nanometer wall and join in the vitriol oil, add potassium permanganate again and stir, add deionized water again and carry out suction filtration, afterwards with hydrochloric acid carry out washing, suction filtration in neutral, obtains carbonoxide nanometer wall slurry to filtrate;
D () prepares graphene nanobelt: after described carbonoxide nanometer wall slurry drying to constant weight, transfers in the protective atmosphere of 500 ~ 1000 DEG C to heat after 10 ~ 300 minutes and peels off, be cooled to room temperature and namely obtain graphene nanobelt.
2. the method for graphene nanobelt prepared by carbon nanometer wall according to claim 1, it is characterized in that, in described step (c), the mass volume ratio of described carbon nanometer wall, the described vitriol oil, described potassium permanganate and described hydrogen peroxide is: 50g:1150mL:150g:250mL.
3. the method for graphene nanobelt prepared by carbon nanometer wall according to claim 1, it is characterized in that, in described step (d), described drying is carried out in vacuum drying oven, and the temperature of described drying is 60 ~ 100 DEG C.
4. the method for graphene nanobelt prepared by carbon nanometer wall according to claim 1, it is characterized in that, in described step (d), described protective atmosphere is at least one in hydrogen, helium, nitrogen, argon gas.
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