CN103193217B - Method for preparing boron-doped diamond and carbon nanotube composite nanocone - Google Patents
Method for preparing boron-doped diamond and carbon nanotube composite nanocone Download PDFInfo
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- CN103193217B CN103193217B CN201310077328.9A CN201310077328A CN103193217B CN 103193217 B CN103193217 B CN 103193217B CN 201310077328 A CN201310077328 A CN 201310077328A CN 103193217 B CN103193217 B CN 103193217B
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Abstract
Carbon nanotubes have a relatively high geometric field enhancement effect, low threshold voltage and high field emission performance. Diamond has a negative electron affinity and field emission stability. The two materials can be widely used in field emission display devices. The invention provides a method for preparing a boron-doped diamond and carbon nanotube composite nanocone. By an electrostatic spraying method, a suspension of nanodiamond mixed with methanol is sprayed and coated on vertical orientation growth multi-walled carbon nanotube surfaces to pre-deposite nanocrystalline diamond particles. The adjacent carbon nanotube tips gather into a cone structure under the role of static electricity. Further, a hot filament chemical vapor deposition method is used for depositing a layer of boron-doped diamond thin film on carbon nanotube cone structures to form the neat, uniform, and size and density-controllable boron-doped diamond and carbon nanotube composite nanocone. The composite nanocone has the advantages of low field emission threshold voltage, long electron emission life and stable performance, and can be applied to field emission devices, electrochemical electrodes and hydrogen storage devices.
Description
Technical field
The present invention relates to nano material technology, particularly a kind of can be applicable to high-performance and long lifetime feds, electrochemical electrode and hydrogen storage device boron-doped diamond and the preparation method that bores of carbon nanotube composite Nano.
Background technology
Carbon nanotube has the mechanical property that tip curvature radius is little, length-to-diameter ratio is large, excellent, good chemical stability and electroconductibility, thus there is higher end geometric field reinforcing effect, low threshold voltage and efficient field emission performance, since being found, people are applied to field emission display to carbon nanotube as electron source and create great interest.Single and many carbon nanotubes and carbon nano-tube film Flied emission research obtains common concern, but the Flied emission electric current of carbon nanotube is unstable, and work-ing life is shorter, is not suitable for large-scale commercial applications.When working under certain vacuum environment, surface adsorption gas molecule, can cause carbon nanotube end to be damaged, electron emission reduced capability, causes the Flied emission of carbon nanotube to produce persistence and degenerates.
Along with the fast development of information technology and vaccum microelectronics, less energy-consumption, high-resolution, ultra-thin over-large screen display system visual organ more and more come into one's own, and vacuum microelectronics technique requires also more and more higher to the cathode material as device core.Therefore, the material that energy consumption is little, field emission performance is superior and stable becomes more and more important.The wide bandgap material (as cBN, AlN etc.) taking diamond as representative, owing to having good chemistry and thermostability, high-melting-point and thermal conductivity, little specific inductivity, large carrier mobility and high voltage breakdown and negative electron affinity (NEA) (when surface is stopped by hydrogen atom), has broad prospect of application in feds.Document (A comparative study of the field emission properties of aligned carbon nanostructures films, from carbon nanotubes to diamond, Eur. Phys. J. Appl. Phys. 38,115,2007) utilize the advantages such as the lower effective work function of adamantine negative electron affinity (NEA) and surface, prepared the diamond thin with better field emission performance by chemical gaseous phase depositing process.In addition, the field emission characteristic of diamond thin can also be strengthened further by other method, as reduce film grain-size, mix boron or nitrogen unit in the film and usually improve the electroconductibility of film or produce defect level, adopt different functional groups (as CsO, LiO) to carry out chemically modified to diamond surface to there is sharp-pointed end to improve the methods such as field reinforcing effect to increase surperficial negative electron affinity (NEA) and to be constructed by diamond thin.Although diamond field emission performance can be improved by these methods, the problems such as but diamond thin prepared by chemical vapour deposition exists, and electroconductibility is relatively poor, columnar crystal structure, low resistance back contacts and nanostructure preparation difficulty, cause higher than the feds threshold voltage of carbon nanotube based on adamantine feds under the same conditions, emission efficiency is lower.But adamantine feds is longer for work-ing life, and electron emission tip is not easily burnt.
Diamond and carbon nano tube compound material is prepared in conjunction with the satisfactory electrical conductivity of carbon nanotube and the feature such as the stability on boron-doped diamond surface and emission lifetime length, and be built into cone structure, will be a kind of efficient, long-life field emission cold-cathode material.But there is not the technology of preparing that boron-doped diamond and carbon nanotube composite Nano are bored in prior art.
Summary of the invention
The object of the invention is, by the feature in field emission performance in conjunction with carbon nanotube and boron-doped diamond, to provide the preparation method that a kind of boron-doped diamond and carbon nanotube composite Nano are bored.
The technical solution realizing the object of the invention is: the preparation method that a kind of boron-doped diamond and carbon nanotube composite Nano are bored, by the multi-wall carbon nano-tube tube-surface pre-deposition Nano diamond particle of electrostatic coating method at vertical oriented growth, and carbon nanotube is made to be gathered into cone structure under electrostatic forcing; Further employing hot-wire chemical gas-phase deposition method deposits one deck Boron-doped diamond on carbon mitron cone structure, is formed to have the boron-doped diamond of good field emission performance and carbon nanotube composite Nano is bored, and specifically comprises the following steps:
Step 1, surface cleaning processing is carried out to monocrystalline substrate; Be specially: first substrate is immersed ultrasonic cleaning in the miscible fluid of acetone and ethanol, then put into deionized water for ultrasonic cleaning, cold wind dries up afterwards.
Step 2, in the clean monocrystalline substrate of surface cleaning sputtering sedimentation SiO successively
2film and Ni film; Described SiO
2film thickness is 30-50nm, Ni film thickness is 5-15nm.
Step 3, sample is placed in plasma enhanced chemical vapor deposition reaction vessel, by heated substrate, Ni film is melted, substrate is formed the Ni nanoparticle of dispersion; Described underlayer temperature is 650-750 DEG C, and heat-up time is 5-15min.
Step 4, using plasma strengthen chemical gaseous phase depositing process, take Ni as catalyzer, at C
2h
2/ NH
3regulate direct current (DC) bias to prepare the array of multi-walled carbon nanotubes of vertical orientation in mixed gas; The direct current (DC) bias of described preparation array of multi-walled carbon nanotubes is 550-750V, C
2h
2/ NH
3gas flow is 50sccm/200sccm.
Step 5, by Nano diamond Granular composite in methanol solution, be mixed with suspension liquid, afterwards by the multi-walled carbon nano-tubes on the surface in advance coated with nano diamond particles of electrostatic spraying in preparation, and carbon nanotube is made to be gathered into cone structure under electrostatic forcing; Described Nano diamond particle diameter is 3-10nm, and electrostatic spraying Nano diamond particle suspension liquid time institute biasing is 35kV, deposits the rotary sample speed 1500rpm of multi-walled carbon nano-tubes.
Step 6, surface-coated there is the multi-walled carbon nano-tubes sample of Nano diamond particle to be placed in hot filament chemical vapor deposition reactor container, pass into CH
4/ H
2/ B
2h
6mixed gas, controls hot-wire temperature, CH
4/ H
2ratio, B/C ratio, deposition pressure and these processing parameters of depositing time, many walls carbon mitron cone structure of forming core in advance deposits one deck Boron-doped diamond, forms boron-doped diamond and carbon nanotube composite Nano is bored.Described hot-wire chemical gas-phase deposition prepares diamond thin condition: deposition pressure is 20-30Torr, CH
4/ H
2gas ratio is 1-5%, and in mixed gas, B/C ratio is 2000-10000ppm, Ta flight lead sample surfaces distance is 3-5mm, and hot-wire temperature is 2300-2400 DEG C, and substrate temperature is about 800-900 DEG C, and depositing time is 30-60min.
Compared with prior art, its remarkable advantage is in the present invention: 1) composite Nano cone material of the present invention is made up of the multi-walled carbon nano-tubes being coated with boron-doped diamond; 2) the vertical orientation multi-walled carbon nano-tubes carbon prepared of the present invention, can make adjacent carbon nanotubes assemble by Electrostatic Spray Technology and form nanocone structures; 3) nanocone end can cover by the Boron-doped diamond that the present invention adopts hot-wire chemical gas-phase deposition method to prepare, and does not affect the configuration of nanocone simultaneously; 4) the technology of the present invention can prepare the controlled boron-doped diamond of neatly homogeneous, size and density and carbon nanotube composite Nano is bored, and this composite Nano cone has the long and stable performance of low Flied emission threshold voltage, emission lifetime; 5) boron-doped diamond prepared of the present invention and carbon nanotube composite Nano are bored and are not only applicable to high-performance field emission display, also can be used for electrochemical electrode and hydrogen storage device simultaneously.
Below in conjunction with accompanying drawing, further detailed description is done to the present invention.
Accompanying drawing explanation
Fig. 1 is the carbon nanotube scanning electron microscope (SEM) photograph of the vertical oriented growth of example 1 of the present invention preparation.
Fig. 2 is the carbon nanotube pyramidal structure scanning electron microscope (SEM) photograph that example 1 of the present invention is formed after electrostatic spraying Nano diamond particle suspension liquid.
Fig. 3 is boron-doped diamond and the carbon nanotube composite Nano scanning electron microscope (SEM) photograph of boring of example 1 of the present invention preparation.
Fig. 4 is the field emission characteristic curve that boron-doped diamond and carbon nanotube composite Nano bore array.
Embodiment
The invention provides the preparation method that a kind of boron-doped diamond and carbon nanotube composite Nano are bored, by the multi-wall carbon nano-tube tube-surface pre-deposition Nano diamond particle of electrostatic coating method at vertical oriented growth, and carbon nanotube is made to be gathered into cone structure under electrostatic forcing; Further employing hot-wire chemical gas-phase deposition method deposits one deck Boron-doped diamond on carbon mitron cone structure, is formed to have the boron-doped diamond of good field emission performance and carbon nanotube composite Nano is bored, and specifically comprises the following steps:
Step 1, surface cleaning processing is carried out to monocrystalline substrate.Concrete operations are: first substrate is immersed ultrasonic cleaning in the miscible fluid of acetone and ethanol, and then put into deionized water for ultrasonic cleaning, cold wind dries up afterwards;
Step 2, in the clean monocrystalline substrate of surface cleaning, sputtering sedimentation a layer thickness is the SiO of 30-50nm successively
2film and thickness are the Ni film of 5-15nm;
Step 3, be placed in plasma enhanced chemical vapor deposition reaction vessel by sample, by silicon to 650-750 DEG C, heat-up time is 5-15min, makes the Ni film fusing on substrate form the Ni nanoparticle of dispersion;
Step 4, using plasma strengthen chemical gaseous phase depositing process, take Ni as catalyzer, at C
2h
2/ NH
3the array of multi-walled carbon nanotubes of vertical orientation is prepared in mixed gas; Concrete growth parameter(s) is direct current (DC) bias is 550-750V, C
2h
2/ NH
3gas flow is 50sccm/200sccm.
Step 5, by the Nano diamond Granular composite of diameter 3-10nm in methanol solution, be mixed with suspension liquid.By the multi-walled carbon nano-tubes on the surface in advance coated with nano diamond particles of electrostatic spraying in preparation, electrostatic spraying Nano diamond particle suspension liquid time institute biasing is 35kV, deposits the rotary sample speed 1500rpm of multi-walled carbon nano-tubes.And residual wetted with methanol array of multi-walled carbon nanotubes end surface, and by electrostatic attraction, many carbon nanotube tips are flocked together formation cone structure.
Step 6, surface-coated there is the multi-walled carbon nano-tubes sample of Nano diamond particle to be placed in hot filament chemical vapor deposition reactor container, pass into CH
4/ H
2/ B
2h
6mixed gas, controls hot-wire temperature, CH
4/ H
2ratio, B/C ratio, deposition pressure and these processing parameters of depositing time, many walls carbon mitron cone structure of forming core in advance deposits one deck Boron-doped diamond, forms boron-doped diamond and carbon nanotube composite Nano is bored.Concrete technology parameter is: pressure is 20-30Torr, CH
4/ H
2gas ratio is 1-5%, and in mixed gas, B/C ratio is 2000-10000ppm, Ta flight lead sample surfaces distance is 3-5mm, and hot-wire temperature is 2300-2400 DEG C, and substrate temperature is about 800-900 DEG C, and depositing time is 30-60min.
Below in conjunction with embodiment, further detailed description is done to the present invention:
embodiment 1:
Using plasma strengthens chemical gaseous phase depositing process and prepares multi-walled carbon nano-tubes, by the multi-wall carbon nano-tube tube-surface pre-deposition Nano diamond particle of electrostatic coating method at vertical oriented growth, and carbon nanotube is made to be gathered into cone structure under electrostatic forcing; Further employing hot-wire chemical gas-phase deposition method deposits one deck Boron-doped diamond on carbon mitron cone structure, is formed to have the boron-doped diamond of good field emission performance and carbon nanotube composite Nano is bored, and specifically comprises the following steps:
Step 1, surface cleaning processing is carried out to monocrystalline substrate.Concrete operations are: first substrate is immersed ultrasonic cleaning in the miscible fluid of acetone and ethanol, and then put into deionized water for ultrasonic cleaning, cold wind dries up afterwards;
Step 2, in the clean monocrystalline substrate of surface cleaning, sputtering sedimentation a layer thickness is the SiO of 40nm successively
2film and thickness are the Ni film of 7nm;
Step 3, be placed in plasma enhanced chemical vapor deposition reaction vessel by sample, by silicon to 700 DEG C, heat-up time is 10min, makes the Ni film fusing on substrate form the Ni nanoparticle of dispersion;
Step 4, using plasma strengthen chemical gaseous phase depositing process, take Ni as catalyzer, C
2h
2/ NH
3gas flow is 50sccm/200sccm, direct current (DC) bias 650V, prepares the array of multi-walled carbon nanotubes of vertical oriented growth.
Step 5, by the Nano diamond Granular composite of diameter 5nm in methanol solution, be mixed with suspension liquid.By the multi-walled carbon nano-tubes on the surface in advance coated with nano diamond particles of electric spraying method in preparation, electrostatic spraying Nano diamond particle suspension liquid time institute biasing is 35kV, deposits the rotary sample speed 1500rpm of multi-walled carbon nano-tubes.Residual wetted with methanol array of multi-walled carbon nanotubes end surface, and by electrostatic attraction, adjacent many carbon nanotube tips are flocked together formation cone structure.
Step 6, surface-coated there is the multi-walled carbon nano-tubes sample of Nano diamond particle to be placed in hot filament chemical vapor deposition reactor container, pass into CH
4/ H
2/ B
2h
6mixed gas, pressure is 25Torr, CH
4/ H
2gas ratio is 2%, in mixed gas, B/C ratio is 5000ppm, Ta flight lead sample surfaces distance is 4mm, hot-wire temperature is 2350 DEG C, substrate temperature is about 850 DEG C, depositing time is 45min, and many walls carbon mitron cone structure of forming core in advance deposits one deck Boron-doped diamond, forms boron-doped diamond and carbon nanotube composite Nano is bored.
Bore the boron-doped diamond prepared and carbon nanotube composite Nano and carried out analysis and characterization, Fig. 1 is length about 5 μm, diameter 20-50nm, density about 1 × 10
9cm
-2the multi-walled carbon nano-tubes of vertical oriented growth.Fig. 2 is the scanning electron microscope (SEM) photograph of array of multi-walled carbon nanotubes after electrostatic spraying Nano diamond particle, and residual methyl alcohol is distributed in carbon nano pipe array end surface, and electrostatic attraction makes 30-40 follow carbon nanotube tip to be gathered into a little, forms density about 1 × 10
7cm
-2conical structure.Fig. 3 is the scanning electron microscope (SEM) photograph that boron-doped diamond after surface deposition diamond thin and carbon nanotube composite Nano bore array, the top of cone and surface cover by skim boron-doped diamond, density about 1 × 10
7cm
-2.Fig. 4 is the field emission characteristic curve that boron-doped diamond and carbon nanotube composite Nano bore array, shows that this composite Nano cone has low threshold electric field (about 3.0V μm
-1), emitting performance is stable and the life-span is long.
embodiment 2:
Using plasma strengthens chemical gaseous phase depositing process and prepares multi-walled carbon nano-tubes, by the multi-wall carbon nano-tube tube-surface pre-deposition Nano diamond particle of electrostatic coating method at vertical oriented growth, and carbon nanotube is made to be gathered into cone structure under electrostatic forcing; Further employing hot-wire chemical gas-phase deposition method deposits one deck Boron-doped diamond on carbon mitron cone structure, is formed to have the boron-doped diamond of good field emission performance and carbon nanotube composite Nano is bored, and specifically comprises the following steps:
Step 1, surface cleaning processing is carried out to monocrystalline substrate.Concrete operations are: first substrate is immersed ultrasonic cleaning in the miscible fluid of acetone and ethanol, and then put into deionized water for ultrasonic cleaning, cold wind dries up afterwards;
Step 2, in the clean monocrystalline substrate of surface cleaning, sputtering sedimentation a layer thickness is the SiO of 50nm successively
2film and thickness are the Ni film of 15nm;
Step 3, be placed in plasma enhanced chemical vapor deposition reaction vessel by sample, by silicon to 750 DEG C, heat-up time is 15min, makes the Ni film fusing on substrate form the Ni nanoparticle of dispersion;
Step 4, using plasma strengthen chemical gaseous phase depositing process, take Ni as catalyzer, C
2h
2/ NH
3gas flow is 50sccm/200sccm, direct current (DC) bias 750V, prepares the array of multi-walled carbon nanotubes of vertical oriented growth.
Step 5, by the Nano diamond Granular composite of diameter 10nm in methanol solution, be mixed with suspension liquid.By the multi-walled carbon nano-tubes on the surface in advance coated with nano diamond particles of electric spraying method in preparation, electrostatic spraying Nano diamond particle suspension liquid time institute biasing is 35kV, deposits the rotary sample speed 1500rpm of multi-walled carbon nano-tubes.Residual wetted with methanol array of multi-walled carbon nanotubes end surface, and by electrostatic attraction, adjacent many carbon nanotube tips are flocked together formation cone structure.
Step 6, surface-coated there is the multi-walled carbon nano-tubes sample of Nano diamond particle to be placed in hot filament chemical vapor deposition reactor container, pass into CH
4/ H
2/ B
2h
6mixed gas, pressure is 30Torr, CH
4/ H
2gas ratio is 5%, and in mixed gas, B/C ratio is 10000ppm, Ta flight lead sample surfaces distance is 5mm, and hot-wire temperature is 2400 DEG C, and substrate temperature is about 900 DEG C, and depositing time is 60min.
Through verification experimental verification, many walls carbon mitron cone structure of forming core in advance deposited one deck Boron-doped diamond, and form boron-doped diamond and carbon nanotube composite Nano is bored.
embodiment 3:
Using plasma strengthens chemical gaseous phase depositing process and prepares multi-walled carbon nano-tubes, by the multi-wall carbon nano-tube tube-surface pre-deposition Nano diamond particle of electrostatic coating method at vertical oriented growth, and carbon nanotube is made to be gathered into cone structure under electrostatic forcing; Further employing hot-wire chemical gas-phase deposition method deposits one deck Boron-doped diamond on carbon mitron cone structure, is formed to have the boron-doped diamond of good field emission performance and carbon nanotube composite Nano is bored, and specifically comprises the following steps:
Step 1, surface cleaning processing is carried out to monocrystalline substrate.Concrete operations are: first substrate is immersed ultrasonic cleaning in the miscible fluid of acetone and ethanol, and then put into deionized water for ultrasonic cleaning, cold wind dries up afterwards;
Step 2, in the clean monocrystalline substrate of surface cleaning, sputtering sedimentation a layer thickness is the SiO of 30nm successively
2film and thickness are the Ni film of 5nm;
Step 3, be placed in plasma enhanced chemical vapor deposition reaction vessel by sample, by silicon to 650 DEG C, heat-up time is 5min, makes the Ni film fusing on substrate form the Ni nanoparticle of dispersion;
Step 4, using plasma strengthen chemical gaseous phase depositing process, take Ni as catalyzer, C
2h
2/ NH
3gas flow is 50sccm/200sccm, direct current (DC) bias 550V, prepares the array of multi-walled carbon nanotubes of vertical oriented growth.
Step 5, by the Nano diamond Granular composite of diameter 3nm in methanol solution, be mixed with suspension liquid.By the multi-walled carbon nano-tubes on the surface in advance coated with nano diamond particles of electric spraying method in preparation, electrostatic spraying Nano diamond particle suspension liquid time institute biasing is 35kV, deposits the rotary sample speed 1500rpm of multi-walled carbon nano-tubes.Residual wetted with methanol array of multi-walled carbon nanotubes end surface, and by electrostatic attraction, adjacent many carbon nanotube tips are flocked together formation cone structure.
Step 6, surface-coated there is the multi-walled carbon nano-tubes sample of Nano diamond particle to be placed in hot filament chemical vapor deposition reactor container, pass into CH
4/ H
2/ B
2h
6mixed gas, pressure is 20Torr, CH
4/ H
2gas ratio is 1%, and in mixed gas, B/C ratio is 2000ppm, Ta flight lead sample surfaces distance is 3mm, and hot-wire temperature is 2300 DEG C, and substrate temperature is about 800 DEG C, and depositing time is 30min.
Through verification experimental verification, many walls carbon mitron cone structure of forming core in advance deposited one deck Boron-doped diamond, and form boron-doped diamond and carbon nanotube composite Nano is bored.
Claims (5)
1. the preparation method that bores of a boron-doped diamond and carbon nanotube composite Nano, it is characterized in that, by the multi-wall carbon nano-tube tube-surface pre-deposition Nano diamond particle of electrostatic coating method at vertical oriented growth, and carbon nanotube is made to be gathered into cone structure under electrostatic forcing; Further employing hot-wire chemical gas-phase deposition method deposits one deck Boron-doped diamond on carbon mitron cone structure, is formed to have the boron-doped diamond of good field emission performance and carbon nanotube composite Nano is bored, and specifically comprises the following steps:
Step 1, surface cleaning processing is carried out to monocrystalline substrate;
Step 2, in the clean monocrystalline substrate of surface cleaning sputtering sedimentation SiO successively
2film and Ni film;
Step 3, sample is placed in plasma enhanced chemical vapor deposition reaction vessel, by heated substrate, Ni film is melted, substrate is formed the Ni nanoparticle of dispersion;
Step 4, using plasma strengthen chemical gaseous phase depositing process, take Ni as catalyzer, at C
2h
2/ NH
3regulate direct current (DC) bias to prepare the array of multi-walled carbon nanotubes of vertical orientation in mixed gas;
Step 5, by Nano diamond Granular composite in methanol solution, be mixed with suspension liquid, afterwards by the multi-walled carbon nano-tubes on the surface in advance coated with nano diamond particles of electrostatic spraying in preparation, and carbon nanotube is made to be gathered into cone structure under electrostatic forcing;
Step 6, surface-coated there is the multi-walled carbon nano-tubes sample of Nano diamond particle to be placed in hot filament chemical vapor deposition reactor container, pass into CH
4/ H
2/ B
2h
6mixed gas, controls hot-wire temperature, CH
4/ H
2ratio, B/C ratio, deposition pressure and these processing parameters of depositing time, many walls carbon mitron cone structure of forming core in advance deposits one deck Boron-doped diamond, forms boron-doped diamond and carbon nanotube composite Nano is bored;
In step 5, Nano diamond particle diameter is 3-10nm, and electrostatic spraying Nano diamond particle suspension liquid time institute biasing is 35kV, deposits the rotary sample speed 1500rpm of multi-walled carbon nano-tubes;
In step 6, hot-wire chemical gas-phase deposition prepares diamond thin condition: deposition pressure is 20-30Torr, CH
4/ H
2gas ratio is 1-5%, and in mixed gas, B/C ratio is 2000-10000ppm, Ta flight lead sample surfaces distance is 3-5mm, and hot-wire temperature is 2300-2400 DEG C, and substrate temperature is about 800-900 DEG C, and depositing time is 30-60min.
2. the preparation method that bores of boron-doped diamond according to claim 1 and carbon nanotube composite Nano, it is characterized in that, step 1 pair silicon substrate carries out surface cleaning processing and is specially: first substrate is immersed ultrasonic cleaning in the miscible fluid of acetone and ethanol, then put into deionized water for ultrasonic cleaning, cold wind dries up afterwards.
3. the preparation method that bores of boron-doped diamond according to claim 1 and carbon nanotube composite Nano, is characterized in that, SiO in step 2
2film thickness is 30-50nm, Ni film thickness is 5-15nm.
4. the preparation method that bores of boron-doped diamond according to claim 1 and carbon nanotube composite Nano, it is characterized in that, in step 3, underlayer temperature is 650-750 DEG C, and heat-up time is 5-15min.
5. the preparation method that bores of boron-doped diamond according to claim 1 and carbon nanotube composite Nano, it is characterized in that, the direct current (DC) bias preparing array of multi-walled carbon nanotubes in step 4 is 550-750V, C
2h
2/ NH
3gas flow is 50sccm/200sccm.
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| CN103496689B (en) * | 2013-09-23 | 2015-04-15 | 同济大学 | Preparation method of boron-doped p type carbon nanotube with high seebeck coefficient |
| CN104090011B (en) * | 2014-07-09 | 2017-04-05 | 东南大学 | The preparation method of nanometer gold nanofiber function and service thing modified electrode |
| CN104709872A (en) * | 2015-02-06 | 2015-06-17 | 中国科学院物理研究所 | Diamond nanowire array and preparation method thereof, and electrode for electrochemical analysis |
| CN108335916A (en) * | 2017-12-20 | 2018-07-27 | 肇庆市华师大光电产业研究院 | A kind of multi-walled carbon nanotube@X combination electrodes and its preparation method and application |
| CN108609695B (en) * | 2018-05-14 | 2020-06-30 | 环境保护部华南环境科学研究所 | Fluorine-tin modified boron-doped diamond film electrode and preparation method and application thereof |
| CN110734726B (en) * | 2018-10-23 | 2021-10-29 | 嘉兴学院 | Preparation method of carbon nanotube/diamond composite heat-conducting adhesive material |
| CN111378956B (en) * | 2020-03-24 | 2021-08-03 | 南京航空航天大学 | Preparation method of orderly-arranged diamond micro-nano cone array tool |
| CN113604792B (en) * | 2021-06-21 | 2022-11-04 | 北京大学 | Preparation method of diamond nano burr structure |
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