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CN104609392A - Method for directly growing carbon nano spirals or carbon nanospheres on surface of alumina substrate - Google Patents

Method for directly growing carbon nano spirals or carbon nanospheres on surface of alumina substrate Download PDF

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Publication number
CN104609392A
CN104609392A CN201510034619.9A CN201510034619A CN104609392A CN 104609392 A CN104609392 A CN 104609392A CN 201510034619 A CN201510034619 A CN 201510034619A CN 104609392 A CN104609392 A CN 104609392A
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Prior art keywords
alumina substrate
carbon
spirals
temperature
research
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CN201510034619.9A
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Chinese (zh)
Inventor
祁小四
顼建乐
钟伟
都有为
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Guizhou University
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Guizhou University
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Priority to CN201510034619.9A priority Critical patent/CN104609392A/en
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Abstract

The invention discloses a method for directly growing carbon nano spirals or carbon nanospheres on the surface of an alumina substrate. By taking acetylene as a carbon source and utilizing a high-temperature pyrolysis method, the carbon nano spirals or carbon nanospheres with high selectivity are controllably synthesized on the alumina substrate under the catalytic action of non-transition metals by adjusting and controlling the reaction temperature, so that the technological problem of the functional material in the research of electronics field caused by the existence of transition metal catalysts is well solved, and the experimental process is greatly simplified and the cost is reduced. A solid experimental basis is established for the electronics field research and product development of the material. The good repeatability, simplicity in operation and environmental protection are achieved, and the research and potential application of the type in the field of nanometer devices are widened. The method is simple and good in using effect.

Description

In alumina substrate surface direct growth carbon nanometer spiral or the method for Nano carbon balls
Technical field
The present invention relates to the technology of preparing of carbon nanomaterial, especially a kind of in alumina substrate surface direct growth carbon nanometer spiral or the method for Nano carbon balls.
Background technology
Since Kroto and Iijima finds and prepares carbon nanotube, carbon nanotube is with the process based prediction model of its uniqueness, and have very large potentiality application in fields such as Field Emission Display, microelectronic device, hydrogen storage material, composite additives, thus make dissimilar carbon nanomaterial enjoy paying close attention to of lot of domestic and foreign scientific worker at recent two decades always.With linear pattern carbon nanomaterial unlike, carbon nanometer spiral or Nano carbon balls can regard that introducing portion carbon pentagon or carbon heptagon are formed in carbon hexagonal mesh as.Carbon nanometer spiral is also seen as a kind of chiral carbon material because of its special helicoidal structure, research work shows that carbon nanometer spiral not only possesses the process based prediction model of carbon nanomaterial intrinsic, but also there is the advantage that himself spirane structure brings, have broad application prospects in micromechanical component fields such as high-performance reinforced composite, gaseous storage, biosynthesizing catalyzer, miniature inductance, Microsprings.In the last few years, due to microstructure feature, the excellent process based prediction model of its uniqueness, Nano carbon balls received paying close attention to of domestic and international researcher.A large amount of experimental study work shows that Nano carbon balls has powerful potentiality using value in the field such as electrode materials, lubricant, hydrogen storage of support of the catalyst, lithium cell.Based on the desirable physical of dissimilar carbon nanomaterial, chemical property and huge using value, the synthesis technique problem of its sample enjoys people to pay close attention to always.But up to now, without in the katalysis situation of magnesium-yttrium-transition metal material, on substrate, directly the carbon nanomaterial of synthesis highly selective remains a very large timely difficult problem.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of in alumina substrate surface direct growth carbon nanometer spiral or the method for Nano carbon balls, it can on alumina substrate surface directly the carbon nanometer spiral of controllable growth highly selective or Nano carbon balls, to overcome the deficiencies in the prior art.
The present invention is achieved in that the method at alumina substrate surface direct growth carbon nanometer spiral or Nano carbon balls, first alumina substrate is carried out cleaning and drying; Alumina substrate after clean is passed into acetylene in enclosed environment and carries out reacting by heating, Heating temperature is 490-510 DEG C or 640-660 DEG C, more than 30 minutes reaction times, obtains carbon nanometer spiral or Nano carbon balls in the deposited on silicon growth of alumina substrate.
Before alumina substrate and acetylene react, under first making alumina substrate be in protection of inert gas, from room temperature, temperature is increased to temperature of reaction, and then passes into acetylene and react, after having reacted, under protection of inert gas, make temperature be down to room temperature.
Compared with prior art, the present invention is using acetylene as carbon source, utilize the method for Pintsch process, by regulation and control temperature of reaction, achieve without under the katalysis of magnesium-yttrium-transition metal, alumina substrate controllably synthesizes carbon nanometer spiral or the Nano carbon balls of highly selective, solves this kind of functional materials in the past bringing due to the existence of the transition group metal catalyst Technology difficult problem in person in electronics research well, and significantly simplify experimentation and cost.In order to solid experiment basis has been established in the person in electronics research of this kind of material and product development.Originally show to have good repeatability, simple to operate and environmental friendliness, widen the research of the type in field of nanometer devices and the application of potentiality.The inventive method is simple, and result of use is good.
Accompanying drawing explanation
Accompanying drawing 1 is the FE-SEM photo of the product of embodiments of the invention 1;
Accompanying drawing 2 is the FE-SEM photo of the product of embodiments of the invention 2.
Accompanying drawing 3 is the FE-SEM photo of the product of embodiments of the invention 3.
Embodiment
Embodiments of the invention 1: in alumina substrate surface direct growth carbon nanometer spiral or the method for Nano carbon balls, choose the aluminum oxide lining substrate that one piece of 1cm × 1cm specifies, first alumina substrate is carried out cleaning for several times with deionized water and alcohol respectively, put into little porcelain boat after natural air drying in atmosphere, and push in tubular quartz pipe; Under the provide protection of argon gas, the temperature from ambient in silica tube is increased to 500 DEG C; close argon gas afterwards and switch immediately and pass into acetylene gas; then isothermal reaction 1 hour at remaining on 500 DEG C; close acetylene afterwards; in pipe, pass into argon gas simultaneously; after being cooled to room temperature in silica tube, obtain carbon nanometer spiral in the deposited on silicon growth of alumina substrate.
Detected by the product of embodiment 1, the statistical observation result of its field emission scanning electron microscope and transmission electron microscope all shows that carbon nanometer spiral is the primary structure of sample under this condition, and the selectivity of carbon nanometer spiral is about 90%, and its FE-SEM photo as shown in Figure 1.
Embodiments of the invention 2: in alumina substrate surface direct growth carbon nanometer spiral or the method for Nano carbon balls, choose the aluminum oxide lining substrate that one piece of 1cm × 1cm specifies, first alumina substrate is carried out cleaning for several times with deionized water and alcohol respectively, put into little porcelain boat after natural air drying in atmosphere, and push in tubular quartz pipe; Under the provide protection of argon gas, the temperature from ambient in silica tube is increased to 650 DEG C; close argon gas afterwards and switch immediately and pass into acetylene gas; then isothermal reaction 1 hour at remaining on 650 DEG C; close acetylene afterwards; in pipe, pass into argon gas simultaneously; after being cooled to room temperature in silica tube, obtain carbon nanometer spiral in the deposited on silicon growth of alumina substrate.
Detected by the product of embodiment 2, the statistical observation result of its field emission scanning electron microscope and transmission electron microscope all shows that Nano carbon balls is the primary structure of sample under this condition, and the selectivity of Nano carbon balls is about 97%, and its FE-SEM photo as shown in Figure 2.
Embodiments of the invention 3: in the method for alumina substrate surface direct growth carbon nanomaterial, choose the aluminum oxide lining substrate that one piece of 1cm × 1cm specifies, first alumina substrate is carried out cleaning for several times with deionized water and alcohol respectively, put into little porcelain boat after natural air drying in atmosphere, and push in tubular quartz pipe; Under the provide protection of argon gas, the temperature from ambient in silica tube is increased to 600 DEG C; close argon gas afterwards and switch immediately and pass into acetylene gas; then isothermal reaction 1 hour at remaining on 600 DEG C; close acetylene afterwards; in pipe, pass into argon gas simultaneously; after being cooled to room temperature in silica tube, obtain carbon nanomaterial in the deposited on silicon growth of alumina substrate.
Detected by the product of embodiment 3, the statistical observation result of its field emission scanning electron microscope and transmission electron microscope all shows that carbon nanometer spiral and Nano carbon balls are the primary structures of sample under this condition, and its FE-SEM photo as shown in Figure 3.

Claims (2)

1. in alumina substrate surface direct growth carbon nanometer spiral or the method for Nano carbon balls, it is characterized in that: first alumina substrate is carried out cleaning and drying; Alumina substrate after clean is passed into acetylene in enclosed environment and carries out reacting by heating, Heating temperature is 490-510 DEG C or 640-660 DEG C, more than 30 minutes reaction times, obtains carbon nanometer spiral or Nano carbon balls in the deposited on silicon growth of alumina substrate.
2. according to claim 1 in alumina substrate surface direct growth carbon nanometer spiral or the method for Nano carbon balls; it is characterized in that: before alumina substrate and acetylene react; under first making alumina substrate be in protection of inert gas; from room temperature, temperature is increased to temperature of reaction; and then pass into acetylene and react; after having reacted, under protection of inert gas, temperature is made to be down to room temperature.
CN201510034619.9A 2015-01-23 2015-01-23 Method for directly growing carbon nano spirals or carbon nanospheres on surface of alumina substrate Pending CN104609392A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017124659A1 (en) * 2016-01-19 2017-07-27 Institute Of Chemistry, Chinese Academy Of Sciences A modified 3d current collector, its application in lithium metal batteries and method for preparing said composite material
CN110395728A (en) * 2019-08-15 2019-11-01 四川轻化工大学 Preparation method of porous carbon sphere negative electrode material for lithium battery

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20040068026A (en) * 2003-01-23 2004-07-30 캐논 가부시끼가이샤 Method for producing nano-carbon materials
CN102020262A (en) * 2009-09-09 2011-04-20 中国科学院金属研究所 Method for growing single-walled carbon nanotubes in high efficiency without metal catalyst

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20040068026A (en) * 2003-01-23 2004-07-30 캐논 가부시끼가이샤 Method for producing nano-carbon materials
CN102020262A (en) * 2009-09-09 2011-04-20 中国科学院金属研究所 Method for growing single-walled carbon nanotubes in high efficiency without metal catalyst

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
XIAOSI QI ET AL.: "High yield synthesis and photoluminescence properties of carbon coils over Al2O3 substrates", 《DIAMOND AND RELATED MATERIALS》, vol. 51, 15 November 2014 (2014-11-15), pages 30 - 33 *
祁小四: "新颖碳基纳米材料的合成与性能研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》, 15 October 2011 (2011-10-15), pages 020 - 66 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017124659A1 (en) * 2016-01-19 2017-07-27 Institute Of Chemistry, Chinese Academy Of Sciences A modified 3d current collector, its application in lithium metal batteries and method for preparing said composite material
US10847804B2 (en) 2016-01-19 2020-11-24 Institute Of Chemistry, Chinese Academy Of Sciences Carbon nanosphere modified current collector for lithium metal battery and method for preparing the same
CN110395728A (en) * 2019-08-15 2019-11-01 四川轻化工大学 Preparation method of porous carbon sphere negative electrode material for lithium battery
CN110395728B (en) * 2019-08-15 2021-10-22 四川轻化工大学 Preparation method of porous carbon sphere negative electrode material for lithium battery

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