CN105060277A - Preparing technology for carbon nano tube - Google Patents
Preparing technology for carbon nano tube Download PDFInfo
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- CN105060277A CN105060277A CN201510519847.5A CN201510519847A CN105060277A CN 105060277 A CN105060277 A CN 105060277A CN 201510519847 A CN201510519847 A CN 201510519847A CN 105060277 A CN105060277 A CN 105060277A
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Abstract
The invention discloses a preparing technology for a carbon nano tube. Xylene serves as a carbon source, and a carbon nano tube array is prepared through a chemical vapor deposition method. The preparing technology comprises the steps of preparing a mixing solution of a catalyst and a carbon source, carrying heating gasification, controlling the gasification flow, carrying out vacuum pumping, carrying out heating and introducing protection gas. The amount of ferrocene is 10 g, the amount of the xylene solution is 150 ml, and magnetic stirring is carried out for 5 min. The heating gasification temperature is 200-220 DEG C, and the gasification flow is 0.6-0.8 ml/min. The vacuum degree is 2-5 Pa, the heating temperature is 800-900 DEG C, and the protection gas is hydrogen and nitrogen. The carbon nano tube is high in growth speed and stable in quality, the technological parameters are convenient to control, and the prepared carbon nano tube has very good antioxidant ability.
Description
Technical field
The present invention relates to a kind of preparation technology of carbon nanotube.
Background technology
Earlier 1990s .KratschmerI etc. adopt graphite acr method first time to produce C60, and they are by studying its structure, find that it is the another kind of ppolymorphism crystal of carbon.Along with the development of science and technology, 1991, when Japan NEC Corporation basic research laboratories electron microscope expert lijimal observes C60 structure under high resolution transmission electron microscope, find diameter 4nm-30nm, reached, am magnitude, tube wall is the multilayer carbon molecule of graphite-structure, Here it is today by the carbon nanotube of extensive concern, but the fact to be lijima found at that time is not Single Walled Carbon Nanotube, but minimum number of plies is the multi-walled carbon nano-tubes of 2.1993, the research group of Iijima seminar and IBM successfully synthesized the carbon nanotube of individual layer respectively.Say in some sense, it is Single Walled Carbon Nanotube that carbon truly receives art pipe.Due to the structure of Single Walled Carbon Nanotube uniqueness, high mechanical property, unique electrical property and chemical stability, cause the great interest that worldwide many scientists comprise physicist, chemist and material scholar, started an abundant carbon nanotube research tide.In the last few years, along with each technique of carbon nanotube system development, prepare carbon nanotube on a large scale to become a reality, the potential using value of carbon nanotube receives publicity day by day, from current applied research situation. carbon nano-tube material is expected to the industrial application realizing scale in the near future, for mankind's productive life brings convenience.
It is because be sp2 hydridization between the carbon atom of graphite synusia that alkali nanotube and graphite have good conductivity equally, on two tracks that each carbon atom has a unpaired electron to be positioned at perpendicular to synusia.Graphite synusia curls into the determinative that the diameter of tubulose and helix angle are its electroconductibility, and carbon nano-tube conductive is between conductor and semi-conductor.Along with the difference of helical vector, the energy gap width of carbon nanotube can change to from zero can be identical with the energy gap width of silicon.Also can not find any one material people in the world can accomplish so to follow one's bent when modulating its conductivity.The diameter of carbon nanotube generally in several nanometer to tens nanometers, length is even longer about several micron greatly, and the diameter of Single Walled Carbon Nanotube is only about lnm, and electronics motion wherein has quantum behavior.In fact, the multi-walled carbon nano-tubes (about 25nm) that a part of diameter is less shows the characteristic of Quantum Teleportation too.Usually containing paired pentagon and heptagon on the tube wall of carbon nanotube, the existence of these defects can produce new electrical conductive behavior again, and therefore everywhere defect can regard a nanodevice be made up of the carbon atom (tens) of little number as.Heterojunction between carbon nanotube and " T " shape knot can be regarded as metal and metal, or the connection between metal and semi-conductor.
Under normal circumstances, along with the difference of diameter and helicity, Single Walled Carbon Nanotube can have metallicity (namely conductive capability is very strong), also semiconductive can be had: when n=is little, carbon nanotube is metallicity, and be narrow-band semiconductor pipe time m=0, n=3q (q is integer), other type be broadband semiconductor pipe, its energy gap and radius are roughly in inverse relation.R.A.Jiahi etc. to Single Walled Carbon Nanotube resistance be studied, adopt 4 bayonet points directly to measure the resistivity of single tube bank.Adopt 4 methods to measure the sheet Single Walled Carbon Nanotube of pressure simultaneously.
In addition, because the internal diameter of carbon pipe can be as small as nanometer scale, make its electronic band structure more special, wave vector is defined to axis, in the carbon nanotube of minor diameter, quantum effect is particularly evident, therefore can be used as quantum pipe electronic energy is run through unobstructedly, in experiment, oneself is through finding that Single Walled Carbon Nanotube is real quantum wire.
Carbon nanotube has field emission effect, in short: field emission effect refers to that, under sufficiently high electric field action, the electronics near Fermi surface overcomes potential barrier and becomes the phenomenon of unbound electron.Compared with traditional heat emission source hot-cathode, field emitting electronic source cold cathode has the features such as electronic beam current is high, zero energy discrete little (aberration is little), job stability is high, the life-span is long, is widely used in scanning tunnel microscope (STM) and novel electron microscope and microwave amplifier.Although people broadly studied the field emission characteristic of various material, not yet set up a perfect field emission theory, be especially applicable to the theory of semi-conductor and nano material, current comparative maturity be still the field emission theory of metal.
Result of study shows: the people such as carbon nanotube has supraconductivity, Kasumov adopt special technology to allow single-walled pipe (bundle) grow between the slit of two superconducting metal pads, when temperature is lower than having occurred superconducting phenomenon during 1K.Tang etc. have studied magnetic properties and the transport property of the Single Walled Carbon Nanotube embedded in zeolite matrix, find that lower than at the temperature of 20K, the carbon nanotube of 4A shows and shows as anisotropic Meisser effect.In addition, ServiceRobert is thought by Theoretical Calculation, can produce very high superconducting temperature with soccerballene filling carbon nano-pipe, even can reach room temperature.In addition, field electron emission materials also has very important application in the preparation process of vacuum microelectronic device, such as microwave amplifier etc.A hot fields in microelectronic material research had been become in the last few years for the research of field emmision material aspect, along with the development of field emmision material technology, people expect using some wide bandgap materials as field electron emission materials naturally, as a series of wide-band gap semiconductor thin films such as diamond, quasi-diamond, cubic boron nitride, aluminium nitride, silicon carbide, mainly because these materials possess: the chemistry that (1) is good and thermostability; (2) high-melting-point; (3) high heat conductance; (4) high-breakdown-voltage; (5) large carrier mobility, especially has minimum electron affinity, or even negative electron affinity, and this reduces the voltage of Flied emission to a great extent.In addition, in nanometer system, electronics also has unique transportation function, and therefore, this field emmision material will have very wide development potentiality and application prospect.Early stage field emmision material many employings metal tip is as field emmision material, as the advantage of field emmision material, metal tip is that emission mechanism is clearer, and technique is more ripe, but because metallic substance Flied emission threshold voltage own is higher, greatly limit the application of metallic substance, therefore metallic substance is faced with the situation be eliminated.Certainly, metal field emitter array (FEA) its emission characteristic is more stable, but metal field emitter difficulty of preparation technology is larger, and technique is also relatively complicated.In the last few years, nanometer field emmision material progressively attract attention, and the interest of people to carbon nanotube derives from the potential outstanding representation in its transmitting aspect on the scene.Carbon nanotube compares to metal more stable field emission characteristic, and its transmitter current of single multi-walled carbon nano-tubes even reaches the magnitude of 0.1mA, and some are also shaping according to the flat-panel monitor of its emission principle, and has been converted into finished product production.Obviously, in nanometer field emmision material, carbon nanotube receives much attention and attention especially.
Above-mentioned characteristic is to a great extent based on the result that single-root carbon nano-tube is measured, and the actual carbon nano-tube macroscopic body obtained, above-mentioned performance is subject to the impact of the factor such as interaction, spatial relation between its actual length-to-diameter ratio and carbon nanotube and does not embody so excellent performance completely.By the method such as CVD and silk screen printing, carbon nano tube field-emission application aspect is made some progress.Wang Chengwei, Li Mengke, the height-oriented Carbon Nanotube Array film of Template synthesis such as power Hulin, but need to improve on Flied emission theoretical modeling, the Flied emission model setting up science carries out theoretical modeling, the result in experiment can better be applied in actual production life.
Xi'an Communications University Zhu length is pure, history Yongsheng group to the large quantifier elimination of carbon nanotube cathod Flied emission big area silk screen printing, and achieves good achievement in research.They have prepared novel carbon nanotube cathod printing slurry according to carbon nano tube field-emission theory.Research shows, make massfraction and be about the printing slurry that the purifying carbon nano-tube of 20% and the conductive oxide matrix material of 4.2% be mixed to form, its negative electrode has the transmitting uniform properties of excellence.Big area (12.5cm is greater than for the line length) negative electrode be made into screen printing technique, then through Fast Sintering technology and two step aftertreatment technologys, the matrix material on above it can not only be removed and can reach make carbon nanotube well and substrate fix, with seasonal carbon nanotube portion, upright and fully exposure, can improve field transmitting uniformity further.
Making carbon nanotube field emission cold cathode method conventional in practical study has CVD.The diameter of the carbon nanotube grown by CVD, by the impact of catalyst particle diameter, is changed along with catalyst particle diameter change.When there is not template, the direction of growth is random, but the poor stability that larger current is launched, but show that current density is but very large, more stable by the carbon nanotube field emission cathode current emission of method for printing screen making equally, the electric current obtained is also very large, but current density is but very low.CVD prepares carbon nano pipe array process means as a kind of low cost, by the method for many computer MSR Information system as structure flat field emission body, carbon nano pipe array technology of preparing mainly prepares carbon nanotube basis at catalytic pyrolysis method grows up, although at present for the understanding that the growth mechanism of array is also ununified, what the key factor of array growth was mainly reflected in the preparation of catalyzer and energy feeds mode.Utilize electrolytic anodization aluminium as template, in duct, grow the good CNTs of orientation.Domestic also have many research to adopt the structure controlling array in this way further, such as, occupy gorgeous grade by regulating the pore structure of altering anodization parameters regulation and control template, and then can the pattern that grows in duct of control CNTs.Generally speaking, the carbon nanotube that the catalyzer of unordered accumulation grows presents certain aggregate structure, is wound around seriously, in lack of alignment state, and under certain condition, carbon nanotube can be made to have remarkable orientation, realize arranged in parallel, namely form carbon nano pipe array.In carbon nano pipe array, all carbon nanotubes have more consistent length-to-diameter ratio, preferably orientation, higher purity, and these are all conducive to playing its excellent performance, have very important meaning to the research of carbon nano pipe array.The arrangement of carbon nanotube is the maximum difference of carbon nano pipe array and agglomerate carbon nanotube.The bending of carbon nanotube has two kinds of reasons: one is the character due to carbon nanotube itself oneself, especially multi-walled carbon nano-tubes, and the defect of itself makes it in process of growth, form the shape such as spiral tube, curved tube.This defect is difficult to by means cut-ofves such as general drawing-off, high-temperature heat treatment; Two is because the great length-to-diameter ratio of carbon nanotube, caused bending under stressed condition.Because carbon nanotube deformability is strong, general this bending radius-of-curvature can reach 100nm--mono-500nm.This bending generally can pass through some post-treating method, as by polymer chips, stretching; Electric field, magnetic field, chemical bonding householder method orientation; By methods such as gas or liquid-flow shearings, orientation is carried out to unordered carbon nanotube.But this physical method can not make the less carbon nanotube containing native defect of radius-of-curvature straighten, and the usual complex process of post-treating method, be difficult to extensive preparation in enormous quantities, also can introduce other media and assist, be not easy the carbon nano pipe array obtaining very high purity.
Summary of the invention
The object of the invention is to the preparation technology proposing a kind of carbon nanotube.
For reaching this object, the present invention by the following technical solutions:
A kind of preparation technology of carbon nanotube, take dimethylbenzene as carbon source, chemical gaseous phase depositing process is utilized to prepare carbon nano pipe array, comprise: the mixing solutions of Kaolinite Preparation of Catalyst and carbon source that---heating and gasifying---controls gasification flow and---vacuumizes that---heating---is logical protects gas, ferrocene is 10g, xylene solution 150ml, magnetic agitation 5min; Heating and gasifying temperature is 200---220 degree, gasification flow is 0.6---and 0.8ml/min, vacuum tightness is 2---5Pa, Heating temperature is 800---900 degree, protection gas is hydrogen and nitrogen.
Embodiment
Embodiment 1
A kind of preparation technology of carbon nanotube; take dimethylbenzene as carbon source; utilize chemical gaseous phase depositing process to prepare carbon nano pipe array, comprising: the mixing solutions of Kaolinite Preparation of Catalyst and carbon source that---heating and gasifying---controls gasification flow and---vacuumizes that---heating---is logical protects gas.Ferrocene is 10g, xylene solution 150ml, magnetic agitation 5min.Heating and gasifying temperature is 220 degree, and gasification flow is 0.8ml/min.Vacuum tightness is 5Pa, and Heating temperature is 900 degree, and protection gas is hydrogen and nitrogen.
Embodiment 2
A kind of preparation technology of carbon nanotube; take dimethylbenzene as carbon source; utilize chemical gaseous phase depositing process to prepare carbon nano pipe array, comprising: the mixing solutions of Kaolinite Preparation of Catalyst and carbon source that---heating and gasifying---controls gasification flow and---vacuumizes that---heating---is logical protects gas.Ferrocene is 15g, xylene solution 200ml, magnetic agitation 5min, places 1h.Heating and gasifying temperature is 210 degree, and gasification flow is 0.7ml/min.Vacuum tightness is 5Pa, and Heating temperature is 900 degree, and protection gas is hydrogen and nitrogen, and nitrogen flow is 3.0L/min, and hydrogen flowing quantity is 0.25L/min.
Claims (1)
1. the preparation technology of a carbon nanotube, it is characterized in that: take dimethylbenzene as carbon source, chemical gaseous phase depositing process is utilized to prepare carbon nano pipe array, comprise: the mixing solutions of Kaolinite Preparation of Catalyst and carbon source that---heating and gasifying---controls gasification flow and---vacuumizes that---heating---is logical protects gas, ferrocene is 10g, xylene solution 150ml, magnetic agitation 5min; Heating and gasifying temperature is 200---220 degree, gasification flow is 0.6---and 0.8ml/min, vacuum tightness is 2---5Pa, Heating temperature is 800---900 degree, protection gas is hydrogen and nitrogen.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757595A (en) * | 2005-10-29 | 2006-04-12 | 大连理工大学 | Method for preparing orientation micron tube by original self-assembling of multi-wall carbon nanometer tubes |
| CN1803594A (en) * | 2005-11-25 | 2006-07-19 | 清华大学 | Large-area ultra-thin carbon nanotube film and its preparation process |
| EP1919826A1 (en) * | 2005-08-29 | 2008-05-14 | University Of The Witwatersrand Johannesburg | A process for producing carbon nanotubes |
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- 2015-08-21 CN CN201510519847.5A patent/CN105060277A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1919826A1 (en) * | 2005-08-29 | 2008-05-14 | University Of The Witwatersrand Johannesburg | A process for producing carbon nanotubes |
| CN1757595A (en) * | 2005-10-29 | 2006-04-12 | 大连理工大学 | Method for preparing orientation micron tube by original self-assembling of multi-wall carbon nanometer tubes |
| CN1803594A (en) * | 2005-11-25 | 2006-07-19 | 清华大学 | Large-area ultra-thin carbon nanotube film and its preparation process |
Non-Patent Citations (1)
| Title |
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| 曾效舒等: "大规模生长定向排列多壁碳纳米管工艺研究", 《人工晶体学报》 * |
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