CN103922319A - Boron-doped graphene nanoribbons and preparation method thereof - Google Patents
Boron-doped graphene nanoribbons and preparation method thereof Download PDFInfo
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Abstract
The invention relates to boron-doped graphene nanoribbons and a preparation method thereof. The preparation method comprises the following steps: preparation of oxidized carbon nano wall slurry; and preparation of the boron-doped graphene nanoribbons. The boron-doped graphene nanoribbons belong to P-type doping, the hole concentration can be increased, at the same time, the potential for lithium can be improved, moreover, the yield of the boron-doped graphene nanoribbons is high, raw materials can be self-prepared, and the production cost is reduced. Devices required in the preparation process are all common chemical devices, so that the cost of the research and development devices can be saved, and mass production is fitted.
Description
Technical field
The present invention relates to the synthetic field of chemical material, relate in particular to a kind of boron doped graphene nano belt and preparation method thereof.
Background technology
The kind of carbon material comprises the soccerballene (C of zero dimension
60deng), carbon nanotube, the 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 be grown perpendicular to substrate material surface exactly, and for thickness is greater than the wall shape structure of Graphene, 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.
Just the begin one's study preparation of carbon nanometer wall of people before finding early than Graphene, just had preparation and the related application thereof of reported in literature carbon nanometer wall in 2002.Graphene nanobelt not only has the performance of Graphene, also possesses some special performances, and for example its length-to-diameter ratio is very large, can be up to thousands of times, can replace copper conductor at integrated circuit connection, further to improve integrated level, also can carry out modification to its structure and be prepared into switch device.But no matter be early stage preparation method or nearest preparation method, all can relate under plasma atmosphere and react, this will cause certain destruction to the structure of CNW.In addition, the problem that have size control difficulty in graphene nanobelt preparation process, yields poorly, this has also limited its application.
Summary of the invention
Goal of the invention of the present invention is to solve the problem and shortage that above-mentioned prior art exists, a kind of boron doped graphene nano belt and preparation method thereof is provided, boron doped graphene nano belt belongs to N-type doping, can increase electron density, the electroconductibility that also can improve graphene nanobelt simultaneously more has superiority it in switch device as conductive additive.
For reaching goal of the invention of the present invention, the technical solution used in the present invention is: a kind of preparation method of boron doped graphene nano belt, comprise the steps: that (a) prepares carbonoxide nanometer wall slurry: get carbon nanometer wall and join in the vitriol oil, add potassium permanganate and stir, add again deionized water to carry out suction filtration, wash with hydrochloric acid afterwards, suction filtration is neutral to filtrate, obtains carbonoxide nanometer wall slurry.
(b) prepare boron doped graphene nano belt: after described carbonoxide nanometer wall slurry is mixed in the ratio of 1:0.01 ~ 0.5 with boron-doping agent, stir; then directly transfer to temperature and be in the protective atmosphere of 500～1000 DEG C and heat 10～300 minutes, obtain boron doped graphene nano belt after being cooled to room temperature.
Boron doped graphene nano belt belongs to N-type doping, can increase electron density, also can improve the electroconductibility of graphene nanobelt simultaneously, and it is more had superiority as conductive additive in switch device.
In described step (a), 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 (b), described boron-doping agent is at least one in urea, ammonium nitrate, volatile salt or bicarbonate of ammonia.
In described step (b), described protective atmosphere is at least one in helium, nitrogen, argon gas.
Described carbon nanometer wall is prepared by following steps: (c) etched substrate: substrate etching was cleaned up after 0.5～10 minute with the dilute acid soln of 0.01～1mol/L;
(d) prepare carbon nanometer wall: described substrate is placed in to oxygen-free environment and is heated to 600～900 DEG C; then open substrate surface described in UV-irradiation; pass into again carbonaceous material and protective gas and keep 30～300 minutes, obtaining carbon nanometer wall at described substrate surface.
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, improved production efficiency when shortening etching time, and photochemical catalysis can effectively reduce temperature of reaction, reduce energy consumption, reduce production costs, and can effectively avoid the problem occurring in the plasma method preparation process in existing method, and make the thickness of carbon nanometer wall more even, structure is more complete.
In described step (c), 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 (c), the time of described etching is 1～3 minute, described for substrate deionized water, ethanol, acetone clean successively.
In described step (d); described carbonaceous material is at least one in methane, ethane, propane, acetylene, ethanol steam; described protective gas is at least one in helium, nitrogen, argon gas; the flow velocity that passes 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 boron doped graphene nano belt of utilizing above-mentioned preparation method to make.
Compared with prior art, boron doped graphene nano belt of the present invention and preparation method thereof, there is following advantage: 1. boron doped graphene nano belt belongs to N-type doping, can increase electron density, the electroconductibility that also can improve graphene nanobelt simultaneously more has superiority it in switch device as conductive additive.The productive rate of boron doped graphene nano belt is high, and the specific conductivity of nano belt is also improved, and raw material can be prepared voluntarily, has reduced production cost.
2. 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, improved production efficiency when shortening etching time, and photochemical catalysis can effectively reduce temperature of reaction, reduce energy consumption, reduce production costs, and can effectively avoid the problem occurring in the plasma method preparation process in existing method, and make the thickness of carbon nanometer wall more even, structure is more complete.
3. in preparation process, required equipment is all common chemical industry equipment, can save research and development equipment cost, is applicable to scale operation.
Brief description of the drawings
Fig. 1 is the prepared carbon nanometer wall SEM figure of the embodiment of the present invention 1.
Fig. 2 is the prepared boron doped graphene nano belt SEM figure of the embodiment of the present invention 1.
Embodiment
Below in conjunction with embodiment, the present invention is given to elaboration further.
The preparation process of boron doped graphene nano belt of the present invention is roughly divided into following steps: 1. etched substrate: substrate is put into the dilute acid soln etching 0.5～10 minute that concentration is 0.01～1mol/L, after etching, clean with deionized water, ethanol, acetone.
This step object is: by etching makes metal liner end eclipse surface produce defect to metal substrate, can effectively improve the surface tissue of metal substrate, make carbon nanometer wall energy enough in this metal substrate surface growth.
Wherein, the preferred time of this metal substrate of etching is 60～180 seconds, and the preferred acid strength of etching metal substrate is 0.1～0.5mol/L.Preferred etching condition above, can reach the effect of good etching, improves the growth efficiency of carbon nanometer wall.
2. prepare carbon nanometer wall: cleaned substrate is put into reaction chamber and get rid of the air of reaction chamber; then substrate is heated to 600～900 DEG C; open again ultraviolet source equipment; make UV-irradiation at substrate surface; follow (2～10) by volume: 1 passes into carbonaceous material (flow is 10～1000sccm) and protective gas, and keeps 30～300 minutes.
This step object is: the air of getting rid of in reaction chamber can be removed the oxygen in reaction chamber, avoids the participation of oxygen and affects the growth of carbon nanometer wall, for the growth of carbon nanometer wall provides a stable environment.
After having reacted, stop passing into carbonaceous material, stop substrate heating; and close ultraviolet source equipment, question response chamber stops passing into protective gas after being cooled to room temperature, obtains carbon nanometer wall at substrate surface; it is scraped from substrate surface, just obtain 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 at least one in helium, nitrogen, argon gas, and carbonaceous material is at least one in methane, ethane, propane, acetylene, ethanol steam.
3. prepare carbonoxide nanometer wall slurry: pulverous carbon nanometer wall that above-mentioned steps 2 is prepared joins in the vitriol oil of 0 DEG C, add again potassium permanganate, keep the temperature of mixture to remain on below 10 DEG C, stir after 2h, stir 24h in room-temperature water bath, under condition of ice bath, slowly add again deionized water, after 15min, add again the deionized water suction filtration that contains 30% concentration hydrogen peroxide, mixture color becomes glassy yellow afterwards, wash with the hydrochloric acid that concentration is 10%, suction filtration is after neutrality to filtrate again, obtains 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.
4. prepare boron doped graphene nano belt: be 1:(0.01～0.5 in mass ratio by carbonoxide nanometer wall slurry and boron-doping agent) stir after mixing; transfer to again temperature and be in the protective atmosphere of 500～1000 DEG C and heat 10～300 minutes; high temperature can make carbonoxide nanometer wall and nitrating agent decompose, and the effect to the reduction of carbonoxide nanometer wall is also played in nitrating agent simultaneously.In the process of decomposing, realize peeling off and the doping reaction of nitrogen of carbonoxide nanometer wall.To be cooledly to room temperature, collect, just obtain boron doped graphene nano belt.
Wherein, boron-doping agent is at least one in urea, ammonium nitrate, volatile salt or bicarbonate of ammonia.Protective atmosphere is at least one in helium, nitrogen, argon gas.
The present invention also comprises the boron doped graphene nano belt of utilizing above-mentioned preparation method to make.
Be specifically described with the preparation process of 1 ~ 3 pair of boron doped graphene nano belt of the present invention of embodiment below.
Embodiment 1:1. etched substrate: nickel foil is put into the dilute hydrochloric acid solution etching 0.5 minute that concentration is 1mol/L, and etching is well cleaned with deionized water, ethanol, acetone afterwards.
2. prepare carbon nanometer wall: by cleaned nickel foil put into reaction chamber and and get rid of the air of described reaction chamber after nickel foil is heated to 900 DEG C; then open ultraviolet source equipment; make UV-irradiation on nickel foil surface; then pass into carbonaceous material methane (flow is 200sccm) and protective gas nitrogen; the volume ratio of methane and nitrogen is 2:1, and keeps 100 minutes.
After having reacted, stop passing into carbonaceous material, stop nickel foil heating and close light source, question response chamber stops passing into nitrogen after being cooled to room temperature, can obtain carbon nanometer wall on nickel foil surface, and it is scraped from nickel foil surface, just obtains carbon nanometer wall powder.
3. prepare carbonoxide nanometer wall slurry: prepare carbonoxide nanometer wall slurry: 50g carbon nanometer wall is added to 0 DEG C, in the vitriol oil of 1.15L, add again 150g potassium permanganate, the temperature of mixture remains on below 10 DEG C, stir 2h, then stir after 24h in room-temperature water bath, under condition of ice bath, slowly add 4.6L deionized water, after 15min, add again 14L deionized water (wherein contain 250ml concentration be 30% hydrogen peroxide), 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 neutral.
4. prepare boron doped graphene nano belt: by carbonoxide nanometer wall slurry and urea in mass ratio for 1:0.5 stirs after mixing, directly transfer to temperature and be in the nitrogen atmosphere of 800 DEG C and heat 30 minutes, to be cooledly to room temperature, collect, just obtain boron doped graphene nano belt.
Embodiment 2:1. etched substrate: iron foil is put into the dilution heat of sulfuric acid etching 4 minutes that concentration is 0.5mol/L, and etching is well cleaned with deionized water, ethanol, acetone afterwards.
2. prepare carbon nanometer wall: by cleaned nickel foil put into reaction chamber and and get rid of the air of described reaction chamber after iron foil is heated to 600 DEG C; then open ultraviolet source equipment; make UV-irradiation on iron foil surface; then pass into carbonaceous material ethane (flow is 100sccm) and protective gas argon gas; the volume ratio of methane and argon gas is 5:1, and keeps 200 minutes.
After having reacted, stop passing into carbonaceous material, stop iron foil heating and close light source; question response chamber stops passing into protective gas after being cooled to room temperature; can obtain carbon nanometer wall on iron foil surface, it is scraped from iron foil surface, just obtain carbon nanometer wall powder.
3. prepare carbonoxide nanometer wall slurry: prepare carbonoxide nanometer wall slurry: 50g carbon nanometer wall is added to 0 DEG C, in the vitriol oil of 1.15L, add again 150g potassium permanganate, the temperature of mixture remains on below 10 DEG C, stir 2h, then stir after 24h in room-temperature water bath, under condition of ice bath, slowly add 4.6L deionized water, after 15min, add again 14L deionized water (wherein contain 250ml concentration be 30% hydrogen peroxide), 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 neutral.
4. prepare boron doped graphene nano belt: by carbonoxide nanometer wall slurry and ammonium nitrate in mass ratio for 1:0.1 stirs after mixing, directly transfer to temperature and be in the helium atmosphere of 500 DEG C and heat 10 minutes, to be cooledly to room temperature, collect, just obtain boron doped graphene nano belt.
Embodiment 3:1. etched substrate: cobalt paper tinsel is put into the dilute nitric acid solution etching 10 minutes that concentration is 0.011mol/L, and etching is well cleaned with deionized water, ethanol, acetone afterwards.
2. prepare carbon nanometer wall: by cleaned cobalt paper tinsel put into reaction chamber and and get rid of the air of described reaction chamber after cobalt paper tinsel is heated to 700 DEG C; then open ultraviolet source equipment; make UV-irradiation on cobalt paper tinsel surface; then pass into carbonaceous material acetylene (flow is 10sccm) and protective gas helium; the volume ratio of acetylene and helium is 8:1, and keeps 300 minutes.
After having reacted, stop passing into carbonaceous material, stop the heating of cobalt paper tinsel and close light source; question response chamber stops passing into protective gas after being cooled to room temperature; can obtain carbon nanometer wall on nickel foil surface, it is scraped from cobalt paper tinsel surface, just obtain carbon nanometer wall powder.
3. prepare carbonoxide nanometer wall slurry: prepare carbonoxide nanometer wall slurry: 50g carbon nanometer wall is added to 0 DEG C, in the vitriol oil of 1.15L, add again 150g potassium permanganate, the temperature of mixture remains on below 10 DEG C, stir 2h, then stir after 24h in room-temperature water bath, under condition of ice bath, slowly add 4.6L deionized water, after 15min, add again 14L deionized water (wherein contain 250ml concentration be 30% hydrogen peroxide), 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 neutral.
4. prepare boron doped graphene nano belt: by carbonoxide nanometer wall slurry and ammonium nitrate in mass ratio for 1:0.2 stirs after mixing, directly transfer to temperature and be in the argon gas atmosphere of 1000 DEG C and heat 100 minutes, to be cooledly to room temperature, collect, just obtain boron doped graphene nano belt.
In carbon nanometer wall SEM figure from Fig. 1, can find out, the carbon nanometer wall thickness that adopts photochemical catalysis chemical Vapor deposition process to prepare is even, is 20～40nm, and basic vertical substrates growth, and high consistency is good.As shown in the boron doped graphene nano belt SEM figure of Fig. 2, carbon nanometer wall is stripped from into after boron doped graphene nano belt, and width is even, is about 30～60nm, and length is about 0.5～5um.Length-to-diameter ratio reaches as high as 130.
Following table 1 is the design parameter of embodiment 4～11, and the processing step of embodiment 4～11 is identical with embodiment 1～3, and difference is processing parameter and processing condition, at this, its processing step is repeated no more.
Boron doped graphene nano belt of the present invention and preparation method thereof, there is following advantage: 1. boron doped graphene nano belt belongs to N-type doping, can increase electron density, also can improve the electroconductibility of graphene nanobelt simultaneously, it is more had superiority as conductive additive in switch device.The productive rate of boron doped graphene nano belt is high, and the specific conductivity of nano belt is also improved, and raw material can be prepared voluntarily, has reduced production cost.
2. 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, improved production efficiency when shortening etching time, and photochemical catalysis can effectively reduce temperature of reaction, reduce energy consumption, reduce production costs, and can effectively avoid the problem occurring in the plasma method preparation process in existing method, and make the thickness of carbon nanometer wall more even, structure is more complete.
3. in preparation process, required equipment is all common chemical industry equipment, can save research and development equipment cost, is applicable to scale operation.
Foregoing; it is 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 main design of the present invention and spirit; can carry out very easily corresponding flexible or amendment, therefore protection scope of the present invention should be as the criterion with the desired protection domain of claims.
Claims (9)
1. a preparation method for boron doped graphene nano belt, is characterized in that, comprises the steps:
(a) prepare carbonoxide nanometer wall slurry: get carbon nanometer wall and join in the vitriol oil, add potassium permanganate and stir, then adding deionized water to carry out suction filtration, wash afterwards with hydrochloric acid, suction filtration is neutral to filtrate, obtains carbonoxide nanometer wall slurry;
(b) prepare boron doped graphene nano belt: after described carbonoxide nanometer wall slurry is mixed in the ratio of 1:0.01 ~ 0.5 with boron-doping agent, stir; then directly transfer to temperature and be in the protective atmosphere of 500～1000 DEG C and heat 10～300 minutes, obtain boron doped graphene nano belt after being cooled to room temperature.
2. preparation method according to claim 1, it is characterized in that, in described step (a), the mass volume ratio of described carbon nanometer wall, the described vitriol oil, described potassium permanganate and described hydrogen peroxide is: 50g:1150ml:150g:250 ml.
3. preparation method according to claim 1, is characterized in that, in described step (b), described boron-doping agent is at least one in boron trioxide or boric acid.
4. preparation method according to claim 1, is characterized in that, in described step (b), described protective atmosphere is at least one in helium, nitrogen, argon gas.
5. preparation method according to claim 1, is characterized in that, in described step (a), described carbon nanometer wall is prepared by following steps:
(c) etched substrate: substrate etching was cleaned up after 0.5～10 minute with the dilute acid soln of 0.01～1mol/L;
(d) prepare carbon nanometer wall: described substrate is placed in to oxygen-free environment and is heated to 600～900 DEG C; then open substrate surface described in UV-irradiation; pass into again carbonaceous material and protective gas and keep 30～300 minutes, obtaining carbon nanometer wall at described substrate surface.
6. preparation method according to claim 5, it is characterized in that, in described step (c), described substrate is a kind of in iron foil, nickel foil, cobalt paper tinsel, 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.
7. preparation method according to claim 5, is characterized in that, in described step (c), the time of described etching is 1～3 minute, described for substrate deionized water, ethanol, acetone clean successively.
8. preparation method according to claim 5; it is characterized in that; in described step (d); described carbonaceous material is at least one in methane, ethane, propane, acetylene, ethanol steam; described protective gas is at least one in helium, nitrogen, argon gas; the flow velocity that passes into described carbonaceous material is 10～1000 sccm, and the volume ratio of described carbonaceous material and described protective gas is (2～10): 1.
9. the boron doped graphene nano belt that the arbitrary described preparation method of claim 1 to 8 makes.
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