CN105810530B - Nitrogen-doped graphene@SiO2The preparation method and application of Coaxial Nanotubes - Google Patents
Nitrogen-doped graphene@SiO2The preparation method and application of Coaxial Nanotubes Download PDFInfo
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- CN105810530B CN105810530B CN201610192237.3A CN201610192237A CN105810530B CN 105810530 B CN105810530 B CN 105810530B CN 201610192237 A CN201610192237 A CN 201610192237A CN 105810530 B CN105810530 B CN 105810530B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/30—Cold cathodes, e.g. field-emissive cathode
- H01J1/304—Field-emissive cathodes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
Abstract
The invention discloses a kind of nitrogen-doped graphene@SiO2The preparation method and application of Coaxial Nanotubes.The present invention is using melamine and methane as reaction raw materials, Si SiO2Mixed powder is auxiliary material, and nickel nitrate is catalyst, using no one step chemical gas-phase reaction method of template, in vacuum atmosphere oven, prepares nitrogen-doped graphene SiO2Coaxial Nanotubes.One step chemical gas-phase reaction method of no template provided by the invention has simple process and low cost, easily controllable, favorable repeatability, the nitrogen-doped graphene@SiO of acquisition2The caliber of Coaxial Nanotubes is 150~250nm, SiO2The thickness of clad is 6~8nm, and with excellent field emission performance, it can be made to have broad application prospects in fields such as field emission flat panel display, vacuum electron device, large screen LCD backlight module and field emission illuminating light sources.
Description
Technical field
The invention belongs to nano materials to prepare and Flied emission technical field, and in particular to nitrogen-doped graphene@SiO2Coaxially
The preparation method of nanotube and its application as filed emission cathode material.
Background technology
Graphene, due to its excellent electrical and mechanical performance, is expected to become a kind of ideal as a kind of new carbon
Filed emission cathode material.Khare et al. is received multi-walled carbon nanotube stripping solution into graphene by a kind of simple hydrothermal method
Rice band, the field emission performance test result of product show its threshold electric field for 2.8V/ μm (Khare R., Shinde D.B.,
Bansode S.,More M.A.,Majumder M.,Pillai V.K.,Late D.J.Applied Physics
Letters,2015,106(2):023111.);Stratakis et al. has synthesized in the convex surfaces that Si substrates are inlayed from branch
Few layer graphene piece of support, researches show that graphene film is extraordinary electron emitter, threshold electric field is 2.3V/ μm
(Stratakis E.,Eda G.,Yamaguchi H.,Kymakis E.,Fotakis C.,Chhowalla
M..Nanoscale,2012,4(10):3069-3074.);Chinese invention patent (ZL201110292565.8) discloses one kind
Patterned graphene field emission electrode and preparation method thereof, the graphene field emission cathode of acquisition are close with electron emission current
Degree is big, emits stable and uniform.
In order to make graphene become with actual application value filed emission cathode material, researcher by different approaches into
One step reduces the threshold electric field and threshold field of graphene.Wherein nitrogen atom doping is a kind of raising graphene field emission performance
Effective way.Soin et al. has prepared few layer of nitrogen-doped graphene using microwave plasma enhancing chemical vapour deposition technique and has received
Rice piece (FLGs), compared to pure FLGs, the field emission characteristic of N doping FLGs, which has, to be obviously improved, and threshold electric field is by 1.94V/
μm be reduced to 1.0V/ μm (N.Soin, S.S.Roy, S.Roy, K.S.Hazra, D.S.Misra, T.H.Lim,
C.J.Hetherington,J.A. McLaughlin,J.Phys.Chem.C 2011,115,5366.).In addition, to graphene
It is also another effective way for improving its field emission performance to carry out the compound of unlike material.Ding et al. is by graphene and metal oxygen
The progress of compound nano-particle is compound, can obtain threshold electric field (Ding, the J.J. lower than single component material;Yan,X.B.;
Li,J.;Shen,B.S.;Yang,J..Chen, J.T.;Xue,Q.J..ACS Appl.Mater.Interfaces 2011,3:
4299-4305.) Chinese invention patent (201410465528.6 graphene field emission cathode preparation method of application number and graphene
Field-transmitting cathode) a kind of graphene film of doping metals particle is disclosed as field-transmitting cathode, metal nanoparticle enhancing
The local electric field intensity of graphene surface significantly reduces the threshold electric field of its field-transmitting cathode.
SiO2It is commonly used for carrying out compound, functional material of the acquisition with different characteristics with other nano materials.Document is ground
Study carefully and show Nano-meter SiO_22It is compound with flake graphite alkene, help to improve the multiple performance of graphene.Meng et al. is prepared for SiO2
Sheet graphene composite material is coated, and has studied selective adsorption capacity of the composite material to uranium, is shown good
Repeatability and stability (Meng, H.;Li,Z.;Ma,F.Y.;Wang,X.N.;Zhou,W.;Zhang,L..RSC Adv.,
2015,5, 67662–67668.);Zeng et al. is successfully prepared graphene/SiO2Composite material, and pass through introducing vinyl
Group constructs graphene/SiO to the composite material surface2- molecularly imprinted polymer electrochemical sensor, the sensor are shown
Go out higher response current, the advantages that the shorter response time.Separately some researches show that the SiO of suitable thickness2Clad can carry
Rise field emission performance (Zhang, the M. of the materials such as SiC;Li,Z.J.;Zhao,J.;Meng,A.L.;Ma,F.L.;Gong,
L..RSC Adv.2014,4, 55224–55228.).But have not yet to see related graphene/SiO2The preparation of composite material and
The report of its field emission performance research.
Two-dimensional sheet graphene is concentrated mainly on to the research of graphene field emission performance at present, is had no to one-dimensional tubulose stone
The research of black alkene field emission performance.And one-dimensional tubular structure, the advantages that due to its unique orientation of growth, big draw ratio,
Guidance quality is being had more along the electron transport on product production direction, consequently, it is possible to making it have more superior than flake graphite alkene
Field emission performance.Therefore the present invention considers one-dimensional tubular structure, N element doping, compound etc. multifactor right with other materials
The synergistic effect of graphene field emission performance is improved, synthesizes a kind of nitrogen-doped graphene@SiO2Coaxial Nanotubes composite material,
No one step chemical gas-phase reaction method of template is invented, while grapheme tube is obtained, completes N doping and SiO2Cladding, make
Prepared nitrogen-doped graphene@SiO2Coaxial Nanotubes have superior field emission performance, can make it in field emission plane
Before the fields such as display, vacuum electron device, large screen LCD backlight module and field emission illuminating light source have wide application
Scape.
The content of the invention
It is an object of the invention to provide a kind of nitrogen-doped graphene@SiO2Coaxial Nanotubes and preparation method thereof, system
Standby process simply, efficiently, while grapheme tube is obtained, completes N doping and SiO without template2Cladding, gained
Nitrogen-doped graphene@SiO2Coaxial Nanotubes have excellent field emission performance.
The purpose of the present invention is be achieved through the following technical solutions:
1) solid melamine is selected as reaction raw materials, Si-SiO2(its molar ratio is Si to mixed powder:SiO2=1.5:1)
It is in molar ratio 1.5~2 for auxiliary material:1 weighs melamine and Si-SiO2Mixed powder is placed it in agate mortar and mixed
Grind 40min;
2) graphite substrate after cleaning, drying, is immersed into the Ni (NO of 0.01mol/L in supersonic wave cleaning machine3)2Ethanol solution
In 5 minutes, take out naturally dry, obtain being soaked with the substrate of catalyst;
3) mixed raw material is placed on two layers of carbon cloth, and graphite substrate is placed on the top of mixed raw material, and with raw material interval 3~
Then 5mm is put into togerther in graphite reative cell, then graphite reative cell is placed in vacuum atmosphere oven;
4) 50~80Pa is evacuated to vacuum atmosphere oven, furnace temperature is risen to 1200 with the heating rate of 15 DEG C/min~
1250 DEG C, keep the temperature 20~30min, then methane gas be passed through with the Ventilation Rate of 0.10~0.15sccm, duration of ventilation for 25~
30 minutes, gas valve is closed, stopping is passed through methane, closes power supply, cools to room temperature with the furnace, realizes prepared by no masterplate one-step method
Nitrogen-doped graphene@SiO2Coaxial Nanotubes;
5) nitrogen-doped graphene@SiO2Application of the Coaxial Nanotubes as filed emission cathode material.It is sent out in ultrahigh vacuum field
It penetrates in test system, the nitrogen-doped graphene@SiO obtained with step (4)2Coaxial Nanotubes are as cathode, the copper of a diameter of 3mm
Stick is anode, and the distance between adjustment anode and cathode is 500 μm, and the size of Flied emission electric current is come by adjusting the size of load voltage
It adjusts, load voltage is controlled between 0~3kV, and the vacuum degree of ultrahigh vacuum Flied emission test system is 1.0 × 10-6~2.0 ×
10-6Pa。
No template disclosed in this invention, a step chemical gas-phase reaction method prepare nitrogen-doped graphene@SiO2Co-axial nano
The method of pipe compared with prior art, is advantageous in that:
(1) template is not required, it is simple for process, efficient, the preparation of template and removing step in template are avoided, and is kept away
Exempt to destroy caused by tubular structure during removing template is removed;One step chemical gas-phase reaction method, mixes preparing nitrogen
While miscellaneous grapheme tube, SiO is obtained2Clad structure, repeatability is good, batch growth easy to implement;
(2) the nitrogen-doped graphene pipe obtained, product purity is high, and pattern is homogeneous, SiO2Clad is uniform, form with
The coaxial thickness of grapheme tube is the amorphous clad of 6~8nm;
(3) the nitrogen-doped graphene@SiO obtained2Coaxial Nanotubes, as filed emission cathode material, threshold electric field
It is respectively 0.8~1V/ μm and 3.4~3.8V/ μm with threshold field, shows excellent field emission performance.
Description of the drawings
Fig. 1 is the nitrogen-doped graphene@SiO obtained by embodiment 12The SEM photograph of Coaxial Nanotubes.
Fig. 2 is the nitrogen-doped graphene@SiO obtained by embodiment 12TEM the and HRTEM photos of Coaxial Nanotubes.
Fig. 3 is the nitrogen-doped graphene@SiO obtained by embodiment 12The infrared FTIR spectrograms of Coaxial Nanotubes.
Fig. 4 is the nitrogen-doped graphene@SiO obtained by embodiment 12The XPS spectrum figure of Coaxial Nanotubes.
Fig. 5 obtains nitrogen-doped graphene@SiO by embodiment 1, embodiment 22The field emission performance of Coaxial Nanotubes.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but these embodiments are not with any side
Formula limits the scope of the invention.
Embodiment 1
It is reaction raw materials to select commercially available analysis pure melamine, as carbon source and nitrogen source, high-purity CH4Gas (purity>
99.99%) it is supplementary carbon source, Si-SiO2(amount of substance compares Si to ball milling mixing powder:SiO2=1.5:1) it is auxiliary material.By mole
Than for 2:1 weighs 12.6g melamines and 2.04g Si-SiO2Ball milling mixing powder, is put into agate mortar and grinds 40min;
A diameter of 7cm is selected, thickness is 1mm and the circular graphite sheets of any surface finish are as reaction substrate, by graphite substrate in ultrasonic wave
In cleaning machine after cleaning, drying, the Ni (NO that the molar concentration prepared in advance is 0.01mol are immersed in3)2In ethanol solution after 5min
It takes out, is dried in air spare;The mixed raw material that grinding obtains is placed on carbon cloth, the graphite substrate of catalyst will be soaked with
Be placed on the top of mixed raw material, and with 3~5mm of raw material interval, be then placed in together in graphite reative cell, then by graphite reative cell
It is put into vacuum controlled atmosphere furnace;Start vacuum system, vacuum controlled atmosphere furnace is carried out to be evacuated to 50~80Pa, it will be high-purity
Argon gas is passed through vacuum drying oven and furnace pressure is made to be again started up mechanical pump close to normal pressure, vacuumize, this process was repeated three times, makes stove
Internal pressure power is maintained at 50~80Pa;Furnace temperature is first risen to 1250 DEG C with the heating rate of 15 DEG C/min, 25min is kept the temperature, with 0.10
The Ventilation Rate of~0.15sccm is passed through methane gas, and duration of ventilation is 30 minutes, closes gas valve, and stopping is passed through methane,
Power supply is closed, cools to room temperature with the furnace, realizes nitrogen-doped graphene@SiO2The preparation of Coaxial Nanotubes.The SEM characterization knots of product
Fruit sees Fig. 1, and TEM characterization results are shown in Fig. 2 (a, b), and HRTEM characterization results are shown in Fig. 2 (c, d, e), and FTIR characterization results are shown in Fig. 3,
XPS characterization results are shown in Fig. 4.The result shows that:The nitrogen-doped graphene@SiO of preparation2Coaxial Nanotubes pattern even one, caliber are
150~200nm, graphene wall thickness are 8~10nm, amorphous SiO2Graphene tube wall outer layer is evenly coated at, forming thickness is about
The clad of 6nm.By XPS spectrum figure as it can be seen that containing N, C and O element in product, illustrate that nitrogen-atoms is successfully incorporated into product, shape
Into nitrogen-doped graphene nanotube.
The nitrogen-doped graphene@SiO that will be obtained2Coaxial Nanotubes carry out field hair as filed emission cathode material to it
Penetrate performance test.Current density, J enhances with the enhancing of field strength E it can be seen from the J-E relation curves of attached drawing 5.It is opened
It is respectively 0.8V/ μm and 3.4V/ μm with threshold field, shows nitrogen-doped graphene@SiO2Coaxial Nanotubes have excellent field
Emitting performance.In 5 illustration of attached drawing F-N curves present approximately linear, belong to field-electron emission, illustrate Flied emission electric current essentially from
In the product of synthesis.
Embodiment 2
It is reaction raw materials to select commercially available analysis pure melamine, as carbon source and nitrogen source, high-purity CH4Gas (purity>
99.99%) it is supplementary carbon source, Si-SiO2(amount of substance compares Si to ball milling mixing powder:SiO2=1.5:1) it is auxiliary material.By mole
Than for 1.5:1 weighs 9.45g melamines and 2.04g Si-SiO2Ball milling mixing powder, is put into agate mortar and grinds
40min;A diameter of 7cm is selected, thickness is 1mm and the circular graphite sheets of any surface finish are as reaction substrate, and graphite substrate is existed
In supersonic wave cleaning machine after cleaning, drying, the Ni (NO that the molar concentration prepared in advance is 0.01mol are immersed in3)2In ethanol solution
It takes out, is dried in air spare after 5min;The mixed raw material that grinding obtains is placed on carbon cloth, the stone of catalyst will be soaked with
Black substrate is placed on the top of mixed raw material, and with 3~5mm of raw material interval, be then placed in together in graphite reative cell, graphite is anti-
Room is answered to be put into vacuum controlled atmosphere furnace;Start vacuum system, vacuum controlled atmosphere furnace is carried out to be evacuated to 50~80Pa, it will
High-purity argon gas is passed through vacuum drying oven and furnace pressure is made to be again started up mechanical pump, vacuumize close to normal pressure, and this process was repeated three times,
Furnace pressure is made to be maintained at 50~80Pa;Furnace temperature is first risen to 1250 DEG C with the heating rate of 15 DEG C/min, keeps the temperature 25min, with
The Ventilation Rate of 0.10~0.15sccm is passed through methane gas, and duration of ventilation is 30 minutes, closes gas valve, stops being passed through
Methane closes power supply, cools to room temperature with the furnace, realizes nitrogen-doped graphene@SiO2The preparation of co-axial nano structure.It is prepared
Nitrogen-doped graphene pipe@SiO2Co-axial nano structure and morphology even one, caliber are about 200~250nm, and graphene wall thickness is about
8nm, amorphous SiO2Graphene tube wall outer layer is evenly coated at, forms the clad that thickness is about 8nm.
The nitrogen-doped graphene@SiO that will be obtained2Coaxial Nanotubes carry out field hair as filed emission cathode material to it
Penetrate performance test.Current density, J enhances with the enhancing of field strength E it can be seen from the J-E relation curves of attached drawing 5.It is opened
It is respectively 1.0V/ μm and 3.8V/ μm with threshold field, shows nitrogen-doped graphene@SiO2Coaxial Nanotubes have excellent field
Emitting performance.In 5 illustration of attached drawing F-N curves present approximately linear, belong to field-electron emission, illustrate Flied emission electric current essentially from
In the product of synthesis.
Claims (3)
1. nitrogen-doped graphene@SiO2The preparation method of Coaxial Nanotubes, which is characterized in that nitrogen is made using no template one-step method
Doped graphene@SiO2The key step of Coaxial Nanotubes is as follows:
Using solid melamine as reaction raw materials, Si-SiO2Mixed powder is auxiliary material, wherein Si powder and SiO2The amount ratio of amylaceous substance
For 1.5:1, reaction raw materials and auxiliary material are placed in mixed grinding 40min in agate mortar,
By graphite substrate in supersonic wave cleaning machine after cleaning, drying, the Ni (NO of 0.01mol/L are immersed3)2Ethanol solution 5 minutes,
Take out naturally dry,
By carbon cloth, the obtained reaction raw material of grinding and it is soaked with the graphite substrate of catalyst and is put into togerther in graphite reative cell,
Graphite reative cell is placed in vacuum atmosphere oven again,
50~80Pa is evacuated to vacuum atmosphere oven, furnace temperature is risen to 1200~1250 DEG C with the heating rate of 15 DEG C/min,
After keeping the temperature 20~30min, methane gas is passed through with the Ventilation Rate of 0.10~0.15sccm, after ventilating 25~30 minutes, is closed
Gas valve, stopping are passed through methane, cool to room temperature with the furnace, realize that no one step chemical gas-phase reaction method of template prepares N doping stone
Black alkene@SiO2Coaxial Nanotubes,
The nitrogen-doped graphene@SiO2The caliber of Coaxial Nanotubes is 150~250nm, and graphene wall thickness is 8~10nm, non-
Brilliant SiO2The thickness of clad is 6~8nm,
The nitrogen-doped graphene@SiO2Coaxial Nanotubes can be used for filed emission cathode material, threshold electric field and threshold field
Respectively 0.8~1V/ μm and 3.4~3.8V/ μm.
2. nitrogen-doped graphene@SiO according to claim 12The preparation method of Coaxial Nanotubes, it is characterised in that:It is used
Melamine reaction raw materials and Si-SiO2The molar ratio of mixed powder auxiliary material is:(1.5~2):1.
3. nitrogen-doped graphene@SiO according to claim 12The preparation method of Coaxial Nanotubes, it is characterised in that:Mixing
Raw material and graphite substrate with catalyst react indoor placement location in graphite and are:Mixed raw material is placed on two layers of carbon cloth,
Graphite substrate is placed on the top of mixed raw material, and with raw material at intervals of 3~5mm.
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CN112467113A (en) * | 2020-12-01 | 2021-03-09 | 南昌大学 | Preparation method of nitrogen-doped carbon-coated silicon dioxide nanotube composite material |
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