CN205645738U - Coaxial nanotube field emission negative pole of nitrogen doping graphite xi @SiO2 - Google Patents
Coaxial nanotube field emission negative pole of nitrogen doping graphite xi @SiO2 Download PDFInfo
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- CN205645738U CN205645738U CN201620255673.6U CN201620255673U CN205645738U CN 205645738 U CN205645738 U CN 205645738U CN 201620255673 U CN201620255673 U CN 201620255673U CN 205645738 U CN205645738 U CN 205645738U
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000002071 nanotube Substances 0.000 title claims abstract description 38
- 229910052681 coesite Inorganic materials 0.000 title claims abstract description 37
- 229910052906 cristobalite Inorganic materials 0.000 title claims abstract description 37
- 229910052682 stishovite Inorganic materials 0.000 title claims abstract description 37
- 229910052905 tridymite Inorganic materials 0.000 title claims abstract description 37
- 229910002804 graphite Inorganic materials 0.000 title abstract description 20
- 239000010439 graphite Substances 0.000 title abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 title abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims description 64
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 3
- 239000002114 nanocomposite Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- -1 graphite alkene Chemical class 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000005286 illumination Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 10
- 239000007789 gas Substances 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000005253 cladding Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 230000005684 electric field Effects 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000004320 controlled atmosphere Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 229910008065 Si-SiO Inorganic materials 0.000 description 2
- 229910008062 Si-SiO2 Inorganic materials 0.000 description 2
- 229910006405 Si—SiO Inorganic materials 0.000 description 2
- 229910006403 Si—SiO2 Inorganic materials 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229920000344 molecularly imprinted polymer Polymers 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Abstract
The utility model provides a coaxial nanotube field emission negative pole of nitrogen doping graphite xi @SiO2, includes conductive substrate, the nitrogen doping graphite xi @SiO2 coaxial nanotube of growth in the basement. The central core of the coaxial nanotube of nitrogen doping graphite alkene that this scheme provided is a graphite alkene nanotube, and its pipe diameter is 150~250nm, and the skin is the siO2 coating, and its thickness is 6~8nm, and nitrogen foreign atom percent content is 3.2at%. This structure composition considered one -dimensional tubular structure, N element mix, with multifactor synergism to improving graphite alkene field emission performance such as other materials compound, make coaxial nanotube field emission negative pole of nitrogen doping graphite xi @SiO2, show excellent field emission performance, be applicable to the electron source among field emission flat -panel display, vacuum electron device, large screen LCD backlight unit and the field emission source of illumination etc..
Description
Technical field
This utility model relates to a kind of field emission component, specifically a kind of nitrogen-doped graphene@SiO2Coaxial Nanotubes field-transmitting cathode.
Background technology
Graphene is as a kind of new carbon, due to the electrical and mechanical performance of its excellence, is expected to become a kind of preferably filed emission cathode material.Multi-walled carbon nano-tubes is shelled solution by a kind of simple hydrothermal method and is become graphene nanobelt by Khare et al., the field emission performance test result of product shows that its threshold electric field is 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.)；Chinese invention patent (ZL201110292565.8) discloses a kind of patterned Graphene field emission electrode and preparation method thereof, it is thus achieved that graphene field emission cathode to have electron emission current density big, launch stable and uniform.
Have the field-transmitting cathode of actual application value to make Graphene become, researcher reduces threshold electric field and the threshold field of Graphene further by different approaches.Wherein nitrogen atom doping is a kind of effective way improving Graphene field emission performance.Soin et al. uses microwave plasma to strengthen chemical vapour deposition technique and has prepared few layer of nitrogen-doped graphene nanometer sheet (FLGs), and compared to pure FLGs, the field emission characteristic of N doping FLGs has had and is obviously improved, its threshold electric field is reduced to 1.0V/ μm (N.Soin, S.S.Roy, S.Roy by 1.94V/ μm, K.S.Hazra, D.S.Misra, T.H.Lim, C.J.Hetherington, J.A.McLaughlin, J.Phys.Chem.C 2011,115,5366.).It is combined another effective way being also to improve its field emission performance additionally, Graphene is carried out unlike material.Chinese invention patent (application number 201410465528.6 graphene field emission cathode preparation method and graphene field emission cathode) discloses the graphene film of a kind of doping metals granule as field-transmitting cathode, metal nanoparticle enhances the local electric field intensity of graphenic surface, significantly reduces the threshold electric field of its field-transmitting cathode.
SiO2It is commonly used for being combined with other nano material, it is thus achieved that there is the functional material of different qualities.Literature research shows, Nano-meter SiO_22It is combined with flake graphite alkene, contributes to improving the multiple performance of Graphene.Meng et al. is prepared for SiO2Cladding lamellar graphene composite material, and have studied this composite selective adsorption capacity to uranium, show 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, and by introducing vinyl group to this composite material surface, construct Graphene/SiO2-molecularly imprinted polymer electrochemical sensor, the advantages such as this sensor demonstrates higher response current, shorter response time.Separately there are some researches show, the SiO of suitable thickness2Clad can promote 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 relevant Graphene/SiO2Composite is as the report of field-transmitting cathode.
Research to Graphene field emission performance at present is concentrated mainly on two-dimensional sheet Graphene, has no the research to one-dimensional tubular graphene alkene field emission performance.And one-dimensional tubular structure, due to advantages such as the orientation of growth of its uniqueness, big draw ratios, in the more guidance quality of the electron transport along product production direction, consequently, it is possible to make it have the field emission performance more excellent than flake graphite alkene.Therefore this utility model considers the multifactor synergism to raising Graphene field emission performance such as one-dimensional tubular structure, N element doping and other Material cladding, synthesizes a kind of nitrogen-doped graphene@SiO2Coaxial Nanotubes composite, while obtaining grapheme tube, completes N doping and SiO2Cladding, make prepared nitrogen-doped graphene@SiO2Coaxial Nanotubes has more excellent field emission performance, and it can be made to have broad application prospects in fields such as EED, vacuum electron device, giant-screen LCD backlight module and field emission illuminating light sources.
Utility model content
The purpose of this utility model is to provide a kind of nitrogen-doped graphene@SiO2Coaxial Nanotubes field-transmitting cathode, while obtaining grapheme tube, completes N doping and SiO2Cladding, make obtained nitrogen-doped graphene@SiO2Coaxial Nanotubes has the field emission performance of excellence.
The technical solution of the utility model is: a kind of nitrogen-doped graphene@SiO2Coaxial Nanotubes field-transmitting cathode, including, conductive substrates, is grown in suprabasil nitrogen-doped graphene@SiO2Coaxial Nanotubes.
As further program of the utility model: described conductive substrates is graphite substrate.
As further program of the utility model: described nitrogen-doped graphene@SiO2The growing method of Coaxial Nanotubes field-transmitting cathode is without template one step chemical gas-phase reaction method.
As further program of the utility model: described nitrogen-doped graphene@SiO2The N doping atomic percentage conc of Coaxial Nanotubes is 3.2at%.
As further program of the utility model: described nitrogen-doped graphene@SiO2The central core of Coaxial Nanotubes field-transmitting cathode is graphene nano pipe, and its caliber is 150～250nm, and outer layer is SiO2Clad, its thickness is 6～8nm.
The beneficial effects of the utility model are:
Novel in structural design of the present utility model, with grapheme tube as base, completes N doping and SiO2Cladding, and SiO2Clad is uniform, defines the amorphous clad of 6 coaxial with grapheme tube～8nm；This structure composition considers the multifactor synergism to raising Graphene field emission performance such as one-dimensional tubular structure, N element doping and other Material cladding, makes nitrogen-doped graphene@SiO2Coaxial Nanotubes field-transmitting cathode, shows the field emission performance of excellence, and its threshold electric field and threshold field are respectively 0.8～1V/ μm and 3.4～3.8V/ μm.
Accompanying drawing explanation
Fig. 1 (a) is the nitrogen-doped graphene@SiO of embodiment 12Low multiple transmission electron microscope (TEM) photo of Coaxial Nanotubes field-transmitting cathode；Fig. 1 (b) is the nitrogen-doped graphene@SiO of embodiment 12High multiple transmission electron microscope (TEM) photo of Coaxial Nanotubes field-transmitting cathode；Fig. 1 (c) is embodiment 1 nitrogen-doped graphene@SiO2The amorphous SiO of Coaxial Nanotubes field-transmitting cathode tube wall2High-resolution-ration transmission electric-lens (HRTEM) photo of clad；Fig. 1 (d) is embodiment 1 nitrogen-doped graphene@SiO2High-resolution-ration transmission electric-lens (HRTEM) photo of the graphene layer of Coaxial Nanotubes field-transmitting cathode tube wall；Fig. 1 (e) is embodiment 1 nitrogen-doped graphene@SiO2High-resolution-ration transmission electric-lens (HRTEM) photo of the internal Graphene separate layer of Coaxial Nanotubes field-transmitting cathode pipe.
Fig. 2 is embodiment 1 nitrogen-doped graphene@SiO2The infrared FTIR spectrogram of Coaxial Nanotubes field-transmitting cathode.
Fig. 3 is embodiment 1 nitrogen-doped graphene@SiO2The XPS spectrum figure of Coaxial Nanotubes field-transmitting cathode.
Fig. 4 is the nitrogen-doped graphene@SiO of embodiment 1, embodiment 22The field emission performance of Coaxial Nanotubes field-transmitting cathode.
Detailed description of the invention
Below in conjunction with specific embodiment, this utility model is described in further detail, but these embodiments limit the scope of the present invention never in any form.
Embodiment 1
Selecting commercially available analytical pure tripolycyanamide is reaction raw materials, as carbon source and nitrogen source, high-purity CH4Gas (purity > 99.99%) it is supplementary carbon source, Si-SiO2(amount of material compares Si:SiO to ball milling mixed powder2=1.5:1) it is adjuvant.12.6g tripolycyanamide and 2.04g Si-SiO is weighed in molar ratio for 2:12Ball milling mixed powder, puts into grinding 40min in agate mortar；Select a diameter of 7cm, thickness be 1mm and any surface finish circular graphite sheets as reaction substrate, graphite substrate after cleaning, drying, is immersed in the Ni (NO that molar concentration is 0.01mol prepared in advance in ultrasonic washing unit3)2Ethanol solution takes out after 5min, dries standby in air；Mixing raw material grinding obtained is placed on carbon cloth, the graphite substrate being soaked with catalyst is placed on mixing raw material top, and and raw material interval 3～5mm, be placed in the most together in graphite reative cell, then graphite reative cell put into vacuum controlled atmosphere furnace；Starting vacuum system, vacuum controlled atmosphere furnace is evacuated to 50～80Pa, high-purity argon gas is passed through vacuum drying oven and makes furnace pressure close to normal pressure, being again started up mechanical pump, evacuation, this process in triplicate, makes furnace pressure be maintained at 50～80Pa；With the heating rate of 15 DEG C/min, furnace temperature is first risen to 1250 DEG C, be incubated 25min, be passed through methane gas with the Ventilation Rate of 0.10～0.15sccm, duration of ventilation is 30 minutes, closes gas valve, stops being passed through methane, close power supply, cool to room temperature with the furnace, it is achieved nitrogen-doped graphene@SiO2The preparation of Coaxial Nanotubes.TEM, HRTEM, FTIR, XPS characterization result of product is shown in Fig. 1 (a～e), Fig. 2, Fig. 3 respectively.Result shows: the nitrogen-doped graphene@SiO of preparation2Coaxial Nanotubes pattern even one, caliber is about 150～200nm, and Graphene wall thickness is 8～10nm, amorphous SiO2It is evenly coated at Graphene tube wall outer layer, forms the clad that thickness is about 6nm.From XPS spectrum figure, containing N, C and O element in product, illustrate that nitrogen-atoms is successfully incorporated in product, form nitrogen-doped graphene nanotube.
The nitrogen-doped graphene@SiO that will be obtained2Coaxial Nanotubes, as field-transmitting cathode, carries out field emission performance test to it.By the J-E relation curve of accompanying drawing 4 it can be seen that current density, J strengthens along with the enhancing of field intensity E.It is opened and threshold field is respectively 0.8V/ μm and 3.4V/ μm, shows nitrogen-doped graphene@SiO2Coaxial Nanotubes, as field-transmitting cathode, has the field emission performance of excellence.
Embodiment 2
Selecting commercially available analytical pure tripolycyanamide is reaction raw materials, as carbon source and nitrogen source, high-purity CH4Gas (purity > 99.99%) it is supplementary carbon source, Si-SiO2(amount of material compares Si:SiO to ball milling mixed powder2=1.5:1) it is adjuvant.9.45g tripolycyanamide and 2.04g Si-SiO is weighed in molar ratio for 1.5:12Ball milling mixed powder, puts into grinding 40min in agate mortar；Select a diameter of 7cm, thickness be 1mm and any surface finish circular graphite sheets as reaction substrate, graphite substrate after cleaning, drying, is immersed in the Ni (NO that molar concentration is 0.01mol prepared in advance in ultrasonic washing unit3)2Ethanol solution takes out after 5min, dries standby in air；Mixing raw material grinding obtained is placed on carbon cloth, the graphite substrate being soaked with catalyst is placed on mixing raw material top, and and raw material interval 3～5mm, be placed in the most together in graphite reative cell, graphite reative cell put into vacuum controlled atmosphere furnace；Starting vacuum system, vacuum controlled atmosphere furnace is evacuated to 50～80Pa, high-purity argon gas is passed through vacuum drying oven and makes furnace pressure close to normal pressure, being again started up mechanical pump, evacuation, this process in triplicate, makes furnace pressure be maintained at 50～80Pa；With the heating rate of 15 DEG C/min, furnace temperature is first risen to 1250 DEG C, be incubated 25min, be passed through methane gas with the Ventilation Rate of 0.10～0.15sccm, duration of ventilation is 30 minutes, closes gas valve, stops being passed through methane, close power supply, cool to room temperature with the furnace, it is achieved nitrogen-doped graphene@SiO2The preparation of co-axial nano structure.The nitrogen-doped graphene pipe@SiO prepared2Co-axial nano structure and morphology even one, caliber is about 200～250nm, and Graphene wall thickness is about 8nm, amorphous SiO2It is evenly coated at Graphene tube wall outer layer, forms the clad that thickness is about 8nm.
The nitrogen-doped graphene@SiO that will be obtained2Coaxial Nanotubes, as field-transmitting cathode, carries out field emission performance test to it.By the J-E relation curve of accompanying drawing 4 it can be seen that current density, J strengthens along with the enhancing of field intensity E.It is opened and threshold field is respectively 1.0V/ μm and 3.8V/ μm, shows nitrogen-doped graphene@SiO2Co-axial nano tube cathode has the field emission performance of excellence.
Claims (3)
1. a nitrogen-doped graphene SiO2Coaxial Nanotubes field-transmitting cathode, including conductive substrates, is grown in suprabasil nitrogen-doped graphene@SiO2Coaxial Nanotubes, it is characterised in that: amorphous SiO2Layer uniformly, is coaxially coated on grapheme tube outer wall, is graphene-based nano composite structure.
A kind of nitrogen-doped graphene@SiO the most according to claim 12Coaxial Nanotubes field-transmitting cathode, it is characterised in that: nitrogen-doped graphene@SiO2The central core of Coaxial Nanotubes is graphene nano pipe, and its caliber is 150～250nm, and outer layer is SiO2Clad, its thickness is 6～8nm.
A kind of nitrogen-doped graphene@SiO the most according to claim 12Coaxial Nanotubes field-transmitting cathode, it is characterised in that: the atomic percentage conc of nitrogen-doping is 3.2at%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108163842A (en) * | 2018-01-23 | 2018-06-15 | 内蒙古农业大学 | A kind of preparation method and application of graphene nano pipe |
| CN108987218A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting graphene film-silicon nanowire array composite material field emission performance |
-
2016
- 2016-03-30 CN CN201620255673.6U patent/CN205645738U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108163842A (en) * | 2018-01-23 | 2018-06-15 | 内蒙古农业大学 | A kind of preparation method and application of graphene nano pipe |
| CN108987218A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting graphene film-silicon nanowire array composite material field emission performance |
| CN108987218B (en) * | 2018-01-31 | 2019-12-31 | 天津师范大学 | Method for improving field emission performance of graphene sheet-silicon nanowire array composite material |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161012 Termination date: 20170330 |