CN102190294A - Preparation method for carbon nanotube or graphene nano-carbon material - Google Patents
Preparation method for carbon nanotube or graphene nano-carbon material Download PDFInfo
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Abstract
The invention discloses a novel preparation method for nano-carbon material without metal catalyst. The method is a silicon carbide high temperature thermal decomposition method, wherein the high-efficiency and controllable preparation of carbon nanotube and graphene nano-carbon material is realized through modulating the atmosphere in the preparation process. According to the method, high purity nano-carbon material without metal catalyst is produced, thus the influence of metal on the physicochemical property of nano-carbon material is overcome fundamentally. The method is a simple high-efficiency novel method with good repeatability for producing nano-carbon material.
Description
Technical field
The present invention relates to a kind of method that metal catalytic prepares carbon nanotube or graphene nano carbon material of not having.
Background technology
Since carbon nanotube is found,, demonstrated wide application prospect in various fields such as microelectronics, feds, storage hydrogen and catalysis because it has unique electronic structure and physicochemical property.The made of carbon nanotubes of high purity, high yield is the prerequisite and the basis of it being carried out structural characterization, performance test and further applied research.Preparation method of carbon nano-tube commonly used at present mainly contains: arc discharge method, laser evaporation method and metal catalytic chemical Vapor deposition process.Wherein, the arc-over law technology is simple, fast growth, but needs the temperature height, and impurity in products is more; The product quality of laser evaporation method preparation is high but yield poorly; The metal catalytic chemical Vapor deposition process has advantages such as cost is low, output big, be produced on a large scale, and is present most widely used a kind of synthetic method.But the introducing of metal catalyst in the preparation process (being generally Fe-series catalyst: Fe, Co, Ni) has brought many problems for the research and the application of later stage carbon nanotube.For example, the metal remained nanoparticle can change the magnetic of carbon nanotube, stability, even can strengthen toxicity to organism.In addition, the non-compatibility of kish and Si semiconductor technology has hindered the development of carbon nanotube related electronic devices greatly.In order to avoid the influence of metal catalyst as far as possible, adopt very complicated last handling process such as oxidation, pickling, filtration to come purifying carbon nano-tube at present mostly.Even now still can't be got rid of the existence of minute quantity metal nanoparticle fully.And purification process is all very big to the loss and the infringement of sample, can produce a large amount of defectives.This shows that no metal catalytic prepares carbon nanotube can fundamentally avoid this problem.If utilize this method can further realize high quality, large batch of production, can promote the application of carbon nanotube greatly in association area.
At present, the non-metal catalyst preparation method of carbon nanotube can be divided into two kinds.A kind of is the non-metallic catalyst chemical Vapor deposition process.It is under the situation that carbon source (ethanol or methane) is provided, and utilizes semi-conductor (Si, Ge, SiC) or isolator (Al
2O
3, diamond) nanoparticle prepares carbon nanotube as nucleation site.The carbon nanotube that this method makes yields poorly, and it is more mixed and disorderly to distribute, poor orientation.Another is the silicon carbide high-temperature decomposition, promptly makes silicon carbide decompose in rough vacuum condition high temperature (＞1200 ℃) annealing.The carbon nanotube structure that this method obtains is regular, the purity height.But because it is a lot of to influence the factor of carbon nano tube growth, this method repeated poor also is difficult to realize controllably carbon nano-tube structure.
The people such as Geim of Britain Manchester university in 2004 have found the another dazzling star-Graphene of nano-carbon material.In recent years, it becomes the research focus in fields such as Materials science and Condensed Matter Physics rapidly.The bi-dimensional cellular shape lattice structure that Graphene is made up of the carbon six-ring is the elementary cell that makes up other nano-carbon material (as soccerballene, carbon nanotube, graphite).It not only has the advantageous property such as high heat conductance, high mechanical strength of above nano-carbon material concurrently, and electronic structure and electrical properties with uniqueness, as perfect quantum tunneling effect, half integral quantum hall effect, the specific conductivity that never disappears etc., will be expected to obtain widespread use in fields such as high-performance nano electron device, matrix material, field emmision material, gas sensor and energy storages.Therefore, the efficient production of Graphene becomes one of present problem demanding prompt solution.At present, the preparation of Graphene mainly contains the preparation mutually of mechanically peel, solution, chemical vapour deposition and silicon carbide thermal decomposition method.Simple to operate but the poor controllability of mechanically peel method; Solution prepares mutually that system is simple to operate, output is big but the less and skewness of Graphene size; Chemical Vapor deposition process can prepare the high quality Graphene, but complex process, efficient are low, product shifts difficulty.Present silicon carbide thermal decomposition method also is difficult to obtain big area, high-quality Graphene, and still, the silicon carbide elevated temperature heat decomposition method that improves among the present invention has the quality height, size is big, can scale operation etc. characteristics.
In addition, the many distinctive physicochemical property that have of silicon carbide will make it might be widely used in industry such as semiconductor electronic replacing silicon in the future.The silicon carbide high-temperature decomposition organically combines nano-carbon materials such as carbon nanotube, Graphene and manufacturing silicon carbide semiconductor.This type material might be obtained application in a lot of fields.
Summary of the invention
The objective of the invention is to invent a kind of method that metal catalytic prepares carbon nanotube or graphene nano carbon material of not having, realized the preparation of high quality, extensive Graphene or carbon nanotube.
For achieving the above object, the technical solution used in the present invention comprises the steps:
A kind of method for preparing carbon nanotube or graphene nano carbon material,
1) treating processes of SiC sample: to the high-purity alpha-SiC sample, for example the 6H-SiC monocrystalline carries out surface cleaning processing; Adopt the method for solution chemistry that the pollutant removal of SiC sample surfaces is clean;
2) preparation of Graphene: the SiC sample after will handling places in the vacuum chamber, vacuumizes to make vacuum tightness in the vacuum chamber≤5 * 10
-10Mbar or in vacuumizing the back feeds inertia in vacuum chamber or reducing gas makes the vacuum tightness in the vacuum chamber keep 10
-4～10
-10Mbar, heating is heated to high temperature 1200-2000 ℃ with the SiC sample, and is incubated 〉=3 minutes; Sample is reduced to room temperature in inertia or reducing atmosphere, get Graphene;
Or the preparation of carbon nanotube: the SiC sample after will handling places in the vacuum chamber, vacuumizes to make vacuum tightness in the vacuum chamber≤5 * 10
-10Feeding oxygen-containing gas behind the mbar in vacuum chamber makes the vacuum tightness in the vacuum chamber keep 10
-4～10
-8Mbar, heating is heated to high temperature 1300-2000 ℃ with the SiC sample, and is incubated 〉=3 minutes; Sample is reduced to room temperature in inertia or reducing atmosphere, get carbon nanotube.
The treating processes of SiC sample: soaked 〉=5 minutes with mass concentration 5-25% hydrogen fluoride solution earlier, use deionized water, ethanol, acetone rinsing then successively, after importing in the vacuum chamber, the SiC sample is carried out degassing processing (500-900 ℃ was heated 1-10 hour under the vacuum condition); Be mainly the removal surface impurity, for example SiO
2Deng.
Specimen in use is high-purity SiC material of purity 99.9%.
Described inert atmosphere is helium (He), nitrogen (N
2), in the argon gas (Ar) one or more;
Also described originality atmosphere is hydrogen (H
2), ammonia (NH
3), in the alkane of C1-C4 one or more; Heating is heated to 1500-1700 ℃ with the SiC sample.
Described oxygen-containing gas is oxygen (O
2), water (H
2O), in hydrogen peroxide, alcohols, phenols, ketone, acids and the ester class one or more; Heating is heated to 1500-1700 ℃ with the SiC sample.
1, the preparation of nano-carbon materials such as concrete carbon nanotube, Graphene
A. inert atmosphere: in vacuum chamber, feed rare gas element (as argon gas, nitrogen) by leaking valve control, reach 10
-4～10
-10The vacuum tightness of mbar.Utilize the DC heating method that the SiC sample is heated to high temperature (＞1300 ℃), and insulation for some time.Sample is being reduced to room temperature in inert atmosphere, close leakage valve.Obtain high-quality grapheme material thus.
B. reducing atmosphere: in vacuum chamber, feed reducing gas (as hydrogen, methane) by leaking valve control, reach 10
-4～10
-8The vacuum tightness of mbar.Utilize the DC heating method that the SiC sample is heated to high temperature (＞1300 ℃), and insulation for some time.Sample is reduced to room temperature in reducing atmosphere, close leakage valve.Obtain high-quality grapheme material thus.
C. oxygen-containing atmosphere: by leak valve control in vacuum chamber, feed oxygen-containing gas (as oxygen, water, methyl alcohol, ethanol), reach 10
-4～10
-8The vacuum tightness of mbar.Utilize the DC heating method that the SiC sample is heated to high temperature (＞1300 ℃), and insulation for some time.Sample is reduced to room temperature in oxygen-containing atmosphere, close leakage valve.Obtain highly purified carbon nano-tube material thus.
The present invention also has following advantage except that the characteristics of non-metal catalyst previously discussed:
1, good reproducibility, controllability is strong.The present invention has considered various possible influence factors, has realized the controlled preparation of dissimilar nano-carbon materials.
2, carbon nanotube quality height, output is big.The carbon nanotube that the present invention obtains is that the form with array covers on the whole silicon carbide, but also can regulate and control the tube wall layer number and the length of carbon nanotube by the dividing potential drop that changes temperature, temperature rise rate and particular atmosphere.
3, technology is simple, easily operation.
Description of drawings
The scanning electron microscope sectional view of the Graphene array for preparing under Fig. 1, the UHV condition;
The transmission electron microscope photo of the Graphene for preparing under Fig. 2, the UHV condition;
Fig. 3, hydrogen atmosphere be the scanning electron microscope sectional view of the Graphene array of preparation down;
Fig. 4, steam atmosphere be the carbon nano pipe array scanning electron microscope sectional view of preparation down;
Fig. 5, steam atmosphere be the carbon nanotube transmission electron microscope photo of preparation down;
Fig. 6, oxygen atmosphere be the carbon nanotube scanning electron microscope sectional view of preparation down.
Embodiment
The 6H-SiC single crystal samples that the present invention adopts is bought in the BeiJing TianKeHeDa blue light Semiconductor Co., Ltd.Doping type is the n type, doping content 10
18Atoms/cm
3, resistivity is 0.02～0.1 Ω cm.Sample is cut into 3 * 10 * 0.33mm
3, or 5 * 10 * 0.33mm
3Rectangular-shaped pieces.The single-crystal silicon carbide sheet has two dissimilar polarity faces: silicon face SiC (0001) and carbon face SiC (000-1).What adopt among the present invention is 6H-SiC (000-1) single crystal samples of carbon mirror polish, but the present invention also not only is confined to this single crystal samples.
Give detailed explanation below by embodiment for this invention process, but claim scope of the present invention is not subjected to the restriction of these embodiment.Following treating processes is carried out in vacuum chamber.
Embodiment 1
At first 6H-SiC (000-1) surface is cleaned, in 20% hydrofluoric acid solution, soaked 5 minutes, wash successively with deionized water, ethanol, acetone then, remove the hydrofluoric acid and the organism of remained on surface to remove oxide on surface.Put into after the vacuum chamber, be heated to 650 ℃ of left and right sides degasification a few hours.
Embodiment 2
The 6H-SiC sample clean and degasification after, under vacuum condition (3.0 * 10
-10Mbar) DC heating to 1700 ℃ kept 60 minutes.At this moment, color sample becomes black by light green, and formation thickness is several microns surperficial carbon-coating structure.
Fig. 1 is the scanning electron microscope sectional view of the grapheme material of this examples preparation.Can know the interface of telling surperficial carbon-coating and silicon carbide substrates by the figure below.Carbon-coating structure thick about 2.4 μ m in surface are made up of vertical graphene-structured.
Fig. 2 is the transmission electron microscope photo of Graphene.
Embodiment 3
The 6H-SiC sample is after cleaning and degasification, and control is leaked valve and fed argon gas to vacuum chamber, and vacuum keeps 1.3 * 10
-5Mbar.DC heating sample to 1700 ℃ kept 60 minutes then.Sample becomes black by light green.The surface is the thick Graphene array structure in the 1 μ m left and right sides.
Embodiment 4
The 6H-SiC sample is after cleaning and degasification, and control is leaked valve and feed methane in vacuum chamber, and vacuum keeps 1.3 * 10
-5Mbar.DC heating sample to 1700 ℃ kept 60 minutes then.The surface is the thick Graphene array structures in the 2 μ m left and right sides.
Embodiment 5
The 6H-SiC sample is after cleaning and degasification, and control is leaked valve and feed hydrogen in vacuum chamber, and vacuum keeps 1.3 * 10
-5Mbar.DC heating sample to 1700 ℃ kept 60 minutes then.Sample becomes black.The surface is the thick Graphene array structures in the 1.6 μ m left and right sides, but embodiment 2 structures are than irregularity relatively.Graphene curls mostly, sees Fig. 3.
Embodiment 6
The 6H-SiC sample is after cleaning and degasification, and control is leaked valve and feed water vapour in vacuum chamber, and vacuum keeps 1.3 * 10
-5Mbar.DC heating sample to 1700 ℃ kept 60 minutes then.Sample becomes black, obtains carbon nano tube array structure.
The surperficial carbon-coating structure that we prepare under steam atmosphere as can be seen by Fig. 4 scanning electron microscope sectional view can be divided into two parts.For being similar to front embodiment 2～5 resulting graphene-structured, and an approaching surperficial end is a carbon nano pipe array near an end of silicon carbide substrates, and is more neat, fine and close.Surface carbon-coating thick altogether about 1.2 μ m, wherein to be about 200nm thick for carbon nano pipe array.Fig. 5 is the transmission electron microscope photo of corresponding carbon nano pipe array, mostly is multi-walled carbon nano-tubes greatly.
Embodiment 7
The 6H-SiC sample is after cleaning and degasification, and control is leaked valve and feed methyl alcohol in vacuum chamber, and vacuum keeps 1.3 * 10
-5Mbar.DC heating sample to 1700 ℃ kept 60 minutes then, obtained the carbon nano tube array structure of similar embodiment 6.
Embodiment 8
The 6H-SiC sample is after cleaning and degasification, and control is leaked valve and fed ethanol to vacuum chamber, and vacuum keeps 1.3 * 10
-5Mbar.DC heating sample to 1700 ℃ kept 60 minutes then, obtained the carbon nano tube array structure of similar embodiment 6.
Embodiment 9
The 6H-SiC sample is after cleaning and degasification, and control is leaked valve to the vacuum chamber aerating oxygen, and vacuum keeps 1.3 * 10
-5Mbar.DC heating sample to 1700 ℃ kept 60 minutes then.Equally also can obtain the carbon nano tube array structure (see figure 6).
The present invention adopts silicon carbide elevated temperature heat decomposition method, has realized comprising efficient, the controlled preparation of nano-carbon materials such as carbon nanotube and Graphene by the atmosphere in the modulation preparation process.This method can prepare the not high pure phase nano-carbon material of containing metal catalyzer, has fundamentally overcome the influence of metal pair nano-carbon material physicochemical property.It is a kind of novel method of preparation nano-carbon material of simple, efficient, good reproducibility.
Claims (5)
1. method for preparing carbon nanotube or graphene nano carbon material is characterized in that:
1) treating processes of SiC sample: adopt the method for solution chemistry that the pollutant removal of SiC sample surfaces is clean;
2) preparation of Graphene: the SiC sample after will handling places in the vacuum chamber, vacuumizes to make vacuum tightness in the vacuum chamber≤5 * 10
-10Mbar or in vacuumizing the back feeds inertia in vacuum chamber or reducing gas makes the vacuum tightness in the vacuum chamber keep 10
-4～10
-10Mbar, heating is heated to high temperature 1300-2000 ℃ with the SiC sample, and is incubated 〉=3 minutes; Sample is reduced to room temperature in inertia or reducing atmosphere, get Graphene;
Or the preparation of carbon nanotube: the SiC sample after will handling places in the vacuum chamber, vacuumizes to make vacuum tightness in the vacuum chamber≤5 * 10
-10Feeding oxygen-containing gas behind the mbar in vacuum chamber makes the vacuum tightness in the vacuum chamber keep 10
-4～10
-8Mbar, heating is heated to high temperature 1300-2000 ℃ with the SiC sample, and is incubated 〉=3 minutes; Sample is reduced to room temperature in inertia or reducing atmosphere, get carbon nanotube.
2. method according to claim 1, it is characterized in that: the treating processes of SiC sample: soaked 〉=5 minutes with mass concentration 5-25% hydrogen fluoride solution earlier, use deionized water, ethanol, acetone rinsing then successively, at last under vacuum condition 500-900 ℃ the heating 1-10 hour.
3. method according to claim 1 is characterized in that: specimen in use is high-purity SiC material of purity 99.9%.
4. method according to claim 1 is characterized in that:
Described inert atmosphere is helium (He), nitrogen (N
2), in the argon gas (Ar) one or more;
Also described originality atmosphere is hydrogen (H
2), ammonia (NH
3), in the alkane of C1-C4 one or more; Heating is heated to 1500-1700 ℃ with the SiC sample.
5. method according to claim 1 is characterized in that:
Described oxygen-containing gas is oxygen (O
2), water (H
2O), in hydrogen peroxide, alcohols, phenols, ketone, acids and the ester class one or more; Heating is heated to 1500-1700 ℃ with the SiC sample.
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| CN102502592A (en) * | 2011-10-02 | 2012-06-20 | 西安电子科技大学 | Method for realizing epitaxial growth of wafer level graphene on 4H/6H-SiC carbon surfaces |
| CN102569407A (en) * | 2012-02-14 | 2012-07-11 | 北京中瑞经纬科技有限公司 | Silicon-based graphene field effect transistor and production method thereof |
| CN102586869A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院上海硅酸盐研究所 | Three-dimensional grapheme tube and preparation method thereof |
| CN102627271A (en) * | 2012-04-27 | 2012-08-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Separating method for metallic carbon nanotube |
| CN102786049A (en) * | 2012-08-29 | 2012-11-21 | 电子科技大学 | System and method for preparing graphene by means of SiC thermal cracking |
| CN102936009A (en) * | 2012-10-11 | 2013-02-20 | 中国电子科技集团公司第五十五研究所 | Method for manufacturing low layer number graphene film on silicon carbide substrate |
| CN104717876A (en) * | 2013-12-11 | 2015-06-17 | 中扬动力股份有限公司 | Heat transfer catalytic heat dissipation method |
| CN106565263A (en) * | 2016-11-05 | 2017-04-19 | 天津大学 | Preparation method for carbon nano-tube/silicon carbide heat-conducting composite material |
| CN104217930B (en) * | 2013-06-05 | 2017-08-25 | 中芯国际集成电路制造(上海)有限公司 | A kind of forming method of graphene pattern |
| CN107601473A (en) * | 2017-09-30 | 2018-01-19 | 中国电子科技集团公司第十三研究所 | A kind of modified chemical vapor deposition process (MCVD) for the grapheme material for preparing uniformity |
| CN109553089A (en) * | 2018-12-29 | 2019-04-02 | 赛福纳米科技(徐州)有限公司 | Multi-purpose material heat treatment apparatus |
| CN112054185A (en) * | 2020-09-24 | 2020-12-08 | 东莞理工学院 | Preparation method of nitrogen-doped graphene-coated SiC nanoparticle lithium ion battery negative electrode material |
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| CN102502592A (en) * | 2011-10-02 | 2012-06-20 | 西安电子科技大学 | Method for realizing epitaxial growth of wafer level graphene on 4H/6H-SiC carbon surfaces |
| CN102586869B (en) * | 2012-01-20 | 2015-02-11 | 中国科学院上海硅酸盐研究所 | Three-dimensional grapheme tube and preparation method thereof |
| CN102586869A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院上海硅酸盐研究所 | Three-dimensional grapheme tube and preparation method thereof |
| CN102569407A (en) * | 2012-02-14 | 2012-07-11 | 北京中瑞经纬科技有限公司 | Silicon-based graphene field effect transistor and production method thereof |
| CN102627271A (en) * | 2012-04-27 | 2012-08-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Separating method for metallic carbon nanotube |
| CN102786049A (en) * | 2012-08-29 | 2012-11-21 | 电子科技大学 | System and method for preparing graphene by means of SiC thermal cracking |
| CN102786049B (en) * | 2012-08-29 | 2014-09-10 | 电子科技大学 | System and method for preparing graphene by means of SiC thermal cracking |
| CN102936009B (en) * | 2012-10-11 | 2014-05-21 | 中国电子科技集团公司第五十五研究所 | Method for manufacturing low layer number graphene film on silicon carbide substrate |
| CN102936009A (en) * | 2012-10-11 | 2013-02-20 | 中国电子科技集团公司第五十五研究所 | Method for manufacturing low layer number graphene film on silicon carbide substrate |
| CN104217930B (en) * | 2013-06-05 | 2017-08-25 | 中芯国际集成电路制造(上海)有限公司 | A kind of forming method of graphene pattern |
| CN104717876A (en) * | 2013-12-11 | 2015-06-17 | 中扬动力股份有限公司 | Heat transfer catalytic heat dissipation method |
| CN106565263A (en) * | 2016-11-05 | 2017-04-19 | 天津大学 | Preparation method for carbon nano-tube/silicon carbide heat-conducting composite material |
| CN107601473A (en) * | 2017-09-30 | 2018-01-19 | 中国电子科技集团公司第十三研究所 | A kind of modified chemical vapor deposition process (MCVD) for the grapheme material for preparing uniformity |
| CN107601473B (en) * | 2017-09-30 | 2019-08-27 | 中国电子科技集团公司第十三研究所 | A kind of modified chemical vapor deposition process (MCVD) preparing uniform grapheme material |
| CN109553089A (en) * | 2018-12-29 | 2019-04-02 | 赛福纳米科技(徐州)有限公司 | Multi-purpose material heat treatment apparatus |
| CN112054185A (en) * | 2020-09-24 | 2020-12-08 | 东莞理工学院 | Preparation method of nitrogen-doped graphene-coated SiC nanoparticle lithium ion battery negative electrode material |
| US11557752B2 (en) | 2020-09-24 | 2023-01-17 | Dongguan University Of Technology | Method for preparing anode material for lithium ion battery of SiC nanoparticle encapsulated by nitrogen-doped graphene |
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Application publication date: 20110921 |