CN107311148A - Carbon nano pipe array section of length diameter controllable precise and its preparation method and application - Google Patents

Carbon nano pipe array section of length diameter controllable precise and its preparation method and application Download PDF

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CN107311148A
CN107311148A CN201710657476.6A CN201710657476A CN107311148A CN 107311148 A CN107311148 A CN 107311148A CN 201710657476 A CN201710657476 A CN 201710657476A CN 107311148 A CN107311148 A CN 107311148A
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carbon nano
nano pipe
pipe array
preparation
section
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彭慧胜
邓珏
官国振
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Fudan University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/08—Aligned nanotubes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/22—Electronic properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/34—Length
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/36—Diameter
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13—Nanotubes
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention belongs to electrode technology field, the carbon nano pipe array section of specially a kind of length diameter controllable precise and its preparation method and application.Preparation method of the present invention includes：Pass through chemical vapour deposition technique orientation of growth carbon nano pipe array；It is carbon source with ethene using aligned carbon nanotube array as template, one layer of coaxial graphene layer is gone out in its superficial growth by chemical vapour deposition technique, obtains the orientation carbon nano-array with core shell structure；Various hetero atoms can be introduced by doping way in growth course；The mode of freezing microtome section is finally used, diametrically above-mentioned carbon nano pipe array is sheared, by the regulation and control to feed distance, highly controllable carbon nano pipe array section is obtained.Using the section of such carbon nano pipe array as electrode material, the lithium ion battery of preparation has excellent energy-storage property, and its specific capacity reaches as high as 2450 mAh/g.

Description

Carbon nano pipe array section of length diameter controllable precise and its preparation method and application
Technical field
The invention belongs to electrode technology field, and in particular to a kind of carbon nano pipe array section of length diameter controllable precise And its preparation method and application.
Background technology
It is heavy to closing with application to its property by the adjusted and controlled pattern of preparation technology for nano material Will[1-4].On the other hand, the accurate control of the aggregated structure of nano material, can be by its excellent behavior extension to macroscopical chi Degree[5,6].Although researcher is directed to the research and development to nano material processing method always, in application field, to nanometer material Material realizes that inexpensive, efficient processing is still challenging[7-9].For example, 1-dimention nano pipe is used as the main nanometer of a class Material, is widely used in the application field in various forward positions.However, in order to by the excellent specific property of 1-dimention nano pipe from micro-scale Macroscopic arts are expanded to, it is necessary to control its size, composition and aggregated structure exactly, but realize that this point is extremely difficult. Therefore, seek conveniently and efficiently to prepare length diameter controllable, the adjustable carbon nano pipe array of composition, for nano material should It is very significant with the demand in field.
The content of the invention
It is an object of the invention to provide a kind of section of the carbon nano pipe array of length diameter controllable precise and its preparation side Method, and carbon nano pipe array section are used as the application of the electrode material of lithium ion battery.
The present invention provides the preparation method of the carbon nano pipe array section of length diameter controllable precise, comprises the following steps that：
（1）First, chemical vapour deposition technique orientation of growth carbon nano pipe array is passed through；
（2）Then, using the aligned carbon nanotube array of above-mentioned preparation as template, it is carbon source with ethene, passes through chemical vapor deposition Area method goes out one layer of coaxial graphene layer in its superficial growth, obtains the orientation carbon nano-array with core shell structure, the orientation The length of carbon nano pipe array, diameter controllable precise；
（3）Finally, using the mode of freezing microtome section, diametrically above-mentioned carbon nano pipe array is sheared, cut through Cheng Zhong, by the regulation and control to feed distance, obtains highly controllable carbon nano pipe array section.
Step of the present invention（2）In, can be further, to contain the material of nitrogen-atoms, boron atom and sulphur atom as raw material, The doping of nitrogen, boron or sulphur is carried out to the graphene layer coaxially grown respectively, shell is prepared respectively for nitrogen, boron, sulfur doping, stratum nucleare The carbon nano pipe array not mixed, the carbon nano pipe array length and diameter also controllable precise.
Step of the present invention（2）In, carbon nano pipe array diameter passes through growth time accuracy controlling, general carbon nano pipe array Diameter control is in 10nm between 130nm（Referring to Fig. 2 d-g）.
Step of the present invention（3）In, the height of gained carbon nano pipe array section is accurately controlled between 50nm to 80 μm （Referring to Fig. 2 a-c）.
As shown in Figure 2, obtained piece cutting structure is complete, highly consistent and has for the pattern of gained carbon nano pipe array section There is opening（Referring to Fig. 3 a-c）, this characteristic this for material transport and store it is most important.
The carbon nano pipe array section of above-mentioned preparation, as the electrode material of lithium ion battery, shows excellent energy storage Performance.Carbon nano pipe array section and lithium metal are assembled into half-cell, electrochemical analysis is carried out.With a chemical vapor deposition Template CNT（Diameter 10nm, 250 μm of height）Compare, the length diameter controllable precise CNT prepared by the present invention Array slice has higher high rate performance, cycle performance and coulombic efficiency（Referring to Fig. 4 a, b）.Under 0.2A/g multiplying power, Specific capacity highly for a diameter of 60nm of 500nm array slice is about 1380 mAh/g, is seven times of original carbon nanotubes.And The specific capacity of nitrogen-doped carbon nanometer pipe array slice under the same terms is more up to 2450 mAh/g.And in different electric discharge electricity Flow down, coulombic efficiency is held in more than 98%.
Brief description of the drawings
The preparation flow schematic diagram that Fig. 1 cuts into slices for the carbon nano pipe array of length diameter controllable precise.
Fig. 2 is carbon nano pipe array section shape appearance figure.Wherein, a-c, the carbon nano pipe array section scanning electricity of different height Mirror figure；D-g, when graphene layer growth time is 0,10,30 and 45 minute, diameter is respectively that 8,15,35 and 50 nm carbon is received Mitron array slice stereoscan photograph.
The cross-sectional scans electromicroscopic photograph that Fig. 3 cuts into slices for a diameter of 20,45 and 90nm carbon nano pipe array.
Fig. 4 is that the energy storage characteristic that carbon nano pipe array is cut into slices is characterized.Wherein, a, first lap, second when multiplying power is 0.2A/g The charging and discharging curve of the nitrogen-doped carbon nanometer pipe array slice of circle, the 5th circle and the tenth circle；B, nitrogen-doped carbon nanometer pipe is forthright again Can be with coulombic efficiency curve（Nitrogen-doped carbon nanometer pipe diameter 60nm, slice height is 500nm）.
Embodiment
First, the preparation of aligned carbon nanotube array mould plate
By way of magnetron sputtering, 10nm alumina layer and 1nm iron layer are prepared on silicon chip successively.As catalysis Agent, is placed in tube furnace quartz ampoule, is synthesized by typical chemical vapour deposition technique.Wherein ethene (30sccm) is as carbon Source, argon gas (400sccm) and hydrogen (90sccm) set 750 °C of furnace temperature as carrier gas.Aligned carbon nanotube array after growth Highly it is about 2mm.
2nd, the preparation of the carbon nano pipe array with core shell structure and controlled diameter
Above-mentioned aligned carbon nanotube array is transferred on another clean silicon chip, with same tubular quartz stove, is being passed through Carrier gas argon gas（Flow velocity 100-200sccm）Under conditions of, furnace temperature rose to 1060 °C in 23 minutes.Keeping the bar of the temperature Under part, carbon source is further passed through（Such as methane, ethene, acetylene etc.）And reducing gas（Such as hydrogen）, coutroi velocity is 10- 30sccm.By controlling the time of high growth temperature, the thickness of shell graphene layer can be accurately controlled, so that orientation carbon nanometer The controlled diameter of pipe array.When growth time is 10-120min, diameter can be controlled in 15-130nm.When the carbon source being passed through contains There is hetero atom, can make effectively to be doped shell.Such as using acetonitrile, carbon disulfide and boron chloride as nitrogen, boron With the doped source of sulphur, nitrogen, sulphur, boron doped carbon nanometer pipe array are prepared.
3rd, highly controllable aligned carbon nanotube array slice
In the mixed solution that obtained array is immersed to water and methanol, by liquid nitrogen frozen to -120 °C.By regulating and controlling water and first The ratio of alcohol, can regulate and control hardness and toughness, use slicer（Leica RM2265, Leica LN22）It can be taken above-mentioned Cutting flakiness is diametrically carried out to carbon nano pipe array.By controlling the distance of feed, the orientation carbon nanometer after cutting Pipe slice height can be controlled at 0.5-50 μm.
4th, the carbon nano pipe array section based on length diameter controllable precise builds lithium ion battery
Above-mentioned carbon nano-pipe array is classified as working electrode, by the lithium hexafluoro phosphate containing ethylene carbonate, diethyl carbonate（1 M） It is that electrolyte and lithium piece are assembled into button cell（CR2032）, by electrochemical test system, test chemical property.
Bibliography
[1]Y. Tang, M. Ouyang, Nature Mater.2007, 6, 754.
[2]F. Yang, X. Wang, D. Zhang, J. Yang, D. Luo, Z. Xu, J. Wei, J. Wang, Z. Xu, F. Peng, X. Li, R. Li, Y. Li, M. Li, X. Bai, F. Ding, Y. Li,Nature2014, 510, 522.
[3]Q. Cao, S.-j. Han, G. S. Tulevski, Y. Zhu, D. D. Lu, W. Haensch,Nature Nanotechnol.2013, 8, 180.
[4]L. Xu, W. Ma, L. Wang, C. Xu, H. Kuang, N. A. Kotov, Chem. Soc. Rev.2013, 42, 3114.
[5] M. Pumera, Chem. Soc. Rev.2010, 39, 4146.
[6]W. Yang, K. R. Ratinac, S. P. Ringer, P. Thordarson, J. J. Gooding, F. Braet, Angew. Chem. In. Ed.2010, 49, 2114.
[7]R. H. Baughman, A. A. Zakhidov, W. A. de Heer, Science2002, 297, 787.
[8]K. Gong, F. Du, Z. Xia, M. Durstock, L. Dai, Science2009, 323, 760.
[9] M. F. L. De Volder, S. H. Tawfick, R. H. Baughman, A. J. Hart,Science2013, 339, 535。

Claims (6)

1. the preparation method of the carbon nano pipe array section of a kind of length diameter controllable precise, it is characterised in that specific steps are such as Under：
（1）First, chemical vapour deposition technique orientation of growth carbon nano pipe array is passed through；
（2）Then, using the aligned carbon nanotube array of above-mentioned preparation as template, it is carbon source with ethene, passes through chemical vapor deposition Area method goes out one layer of coaxial graphene layer in its superficial growth, obtains the orientation carbon nano-array with core shell structure, the orientation The length of carbon nano pipe array, diameter controllable precise；
（3）Finally, using the mode of freezing microtome section, diametrically above-mentioned carbon nano pipe array is sheared, cut through Cheng Zhong, by the regulation and control to feed distance, obtains highly controllable carbon nano pipe array section.
2. preparation method according to claim 1, it is characterised in that step（2）In, further, to contain nitrogen-atoms, boron The material of atom and sulphur atom carries out the doping of nitrogen, boron or sulphur to the graphene layer coaxially grown, prepared respectively as raw material Shell is nitrogen, boron, sulfur doping, and the carbon nano pipe array that stratum nucleare does not mix, the carbon nano pipe array length and diameter also accurately may be used Control.
3. preparation method according to claim 1 or 2, it is characterised in that step（2）In, by regulating and controlling growth time control Carbon nano pipe array diameter processed is in 10nm between 130nm.
4. preparation method according to claim 3, it is characterised in that step（3）In, the section of gained carbon nano pipe array Highly control is between 50 nanometers to 80 microns.
5. the carbon nano pipe array obtained by one of the claim 1-4 preparation methods is cut into slices.
6. carbon nano pipe array section as claimed in claim 5 is used as the application of the electrode material of lithium ion battery.
CN201710657476.6A 2017-08-03 2017-08-03 Carbon nano pipe array section of length diameter controllable precise and its preparation method and application Pending CN107311148A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1897205A (en) * 2005-07-15 2007-01-17 清华大学 Carbon-nano-tube array transmitting element and its production
CN101580243A (en) * 2009-06-03 2009-11-18 惠州市沃特新材料有限公司 Surface treatment method of carbon nanotube and method for preparing composite plastic by using the same
CN102092703A (en) * 2009-12-11 2011-06-15 北京富纳特创新科技有限公司 Preparation method of carbon nanotube structure
CN103515170A (en) * 2012-06-28 2014-01-15 清华大学 Preparation method for carbon nanotube field emitter
CN106904598A (en) * 2017-04-20 2017-06-30 国家纳米科学中心 A kind of CNT magnet and its preparation method and application

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1897205A (en) * 2005-07-15 2007-01-17 清华大学 Carbon-nano-tube array transmitting element and its production
CN101580243A (en) * 2009-06-03 2009-11-18 惠州市沃特新材料有限公司 Surface treatment method of carbon nanotube and method for preparing composite plastic by using the same
CN102092703A (en) * 2009-12-11 2011-06-15 北京富纳特创新科技有限公司 Preparation method of carbon nanotube structure
CN103515170A (en) * 2012-06-28 2014-01-15 清华大学 Preparation method for carbon nanotube field emitter
CN106904598A (en) * 2017-04-20 2017-06-30 国家纳米科学中心 A kind of CNT magnet and its preparation method and application

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JUE DENG ET AL.: "The Deformations of Carbon Nanotubes under Cutting", 《ACS NANO》 *
ZHIYONG PAN ET AL.: "Synthesizing Nitrogen-Doped Core–Sheath Carbon Nanotube Films for Flexible Lithium Ion Batteries", 《ADVENCED ENERGY MATERIALS》 *

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