CN100439242C - Method of preparing spiral nanometer carbon fiber - Google Patents
Method of preparing spiral nanometer carbon fiber Download PDFInfo
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- CN100439242C CN100439242C CNB2006101480069A CN200610148006A CN100439242C CN 100439242 C CN100439242 C CN 100439242C CN B2006101480069 A CNB2006101480069 A CN B2006101480069A CN 200610148006 A CN200610148006 A CN 200610148006A CN 100439242 C CN100439242 C CN 100439242C
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- carbon fiber
- nanometer carbon
- baseplate material
- spiral nanometer
- organic solvent
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Abstract
This invention discloses a preparation method that prepares spiral nanometer carbon fiber. It includes following steps: spread predecessor solution of catalytic agent on surface of baseplate material, dry, burn in flame of organic solvent, collect black fine powder product, which is spiral nanometer carbon fiber. Above predecessor solution of catalytic agent is chloride alcoholic solution which contains tin; fiber diameter of spiral nanometer carbon fiber is 50-70nm, spiral diameter is 80-110nm, pitch is 80-200nm.
Description
Technical field
The present invention relates to prepare the method for spiral nanometer carbon fiber, particularly prepare the method for carbon nanotube by phase carbon source.
Technical background
Helical carbon fiber not only has excellent properties such as the low density, high specific strength, thermotolerance, electric heating conductivity, chemical stability of common straight charcoal fiber, also have the special spirane structure (the maximum characteristics of chiral material are the cross-polarization performance with electromagnetic field) of different chiralitys, thereby it might be applied at numerous areas such as energy storage material, catalyst base, microelectronic device, Microsprings especially radio-radar absorber.
The U.S., Japan and some European countries have carried out many research work in this respect." Materials science magazine " (Journal of Material Science 1995,30 (5): 5049-5055) reported that professor Motojima adopts acetylene gas as raw material, wherein comprise a spot of sulfocompound (as the saliva fen, hydrogen sulfide), active transition metal powders (nickel, titanium and tungsten) is as catalyzer, thermolysis acetylene has successfully been prepared coiled carbon fibers.They have studied the absorbing property of different size helical carbon fiber in great detail, and by the size that changes helical carbon fiber absorption peak are moved.
" SCI " (2005,26 (1): 5-8) employing hydrogen arc plasma process such as report professor Cui Zuolin etc. has prepared the nanometer copper-nickel alloy as catalyzer, has prepared the spiral nanometer carbon fiber of symmetric growth by the catalyse pyrolysis of acetylene.Human catalytic pyrolysis substrate methods such as Zhao Donglin have successfully prepared volution conductive magnetism fiber, and have studied its microwave electromagnetic performance.But the existing remarkable defective of aforesaid method is to need expensive device, complicated operation, cost height, can't realize suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing spiral nanometer carbon fiber, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
The precursor solution of catalyzer is coated on the baseplate material surface, and drying places the flame of organic solvent to burn then, collects the black powder shape product after burning, and is spiral nanometer carbon fiber.
The precursor solution of said catalyzer is the muriatic ethanolic soln that contains tin;
Said baseplate material is the pure nickel tinsel, and thickness is preferably 0.2～0.6mm, most preferably 0.4mm;
The muriate of said tin is tin tetrachloride (SnCl
45H
2O), the concentration of the muriate of tin in ethanolic soln is 0.08～0.2M;
The said baseplate material drying temperature that scribbles the tin tetrachloride ethanolic soln is 85～95 ℃;
Said baseplate material combustion time in organic solvent flame is 5～15 minutes;
Said organic solvent is selected from the monohydroxy-alcohol of C2～C3 or the alkane of C5～C6, preferred alcohol.
Adopt method of the present invention to prepare spiral nanometer carbon fiber, need not expensive device, simple to operate, with low cost, be easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is for adopting JSM-5600LV type scanning electronic microscope to embodiment 1 product observations.
Fig. 2 is for adopting JSM-5600LV type scanning electronic microscope to embodiment 2 product observationss.
Fig. 3 is for adopting JEM-100CXII type transmission electron microscope to embodiment 2 product observationss.
Fig. 4 is for adopting JEM-100CXII type transmission electron microscope to embodiment 3 product observationss.
Embodiment
Embodiment 1
Employing thickness is that the pure nickel sheet of 0.4mm is made baseplate material, and compound concentration is the tin tetrachloride ethanolic soln of 0.8M, evenly is applied to the baseplate material surface, and dry down in 90 ℃.Then baseplate material was burnt 15 minutes in n-propyl alcohol flame, collect the product after burning, obtain spiral nanometer carbon fiber.The Fibre diameter of spiral nanometer carbon fiber is 50nm, and screw diameter is 80-100nm, and pitch is 80-120nm.
Adopt JSM-5600LV type scanning electronic microscope that products of combustion is observed, scanned photograph as shown in Figure 1.As can be seen from the figure except spiral nanometer carbon fiber, also contain straight type carbon fiber of part and impurity in the product.
Embodiment 2
Employing thickness is that the pure nickel sheet of 0.4mm is made baseplate material, and compound concentration is the tin tetrachloride ethanolic soln of 1M, evenly is applied to the baseplate material surface, and dry down in 90 ℃.Then baseplate material was burnt in ethanol flames 10 minutes, collect the product after burning, obtain spiral nanometer carbon fiber.The Fibre diameter of spiral nanometer carbon fiber is 70nm, and screw diameter is 110nm, and pitch is 200nm.Adopt JSM-5600LV type scanning electronic microscope that products of combustion is observed, scanned photograph as shown in Figure 2.As can be seen from Figure 2 the content of straight type carbon fiber and impurity obviously is less than example 1 in example 2 products.
Black powder shape product of the present invention is scattered in the ethanol, behind the ultra-sonic dispersion, drops in sample preparation on the copper mesh, adopt then HRTEM (HITACHI, JEM-2010F, JEOL) type transmission electron microscope observing sample topography, pattern as shown in Figure 3.
Embodiment 3
Employing thickness is that the pure nickel sheet of 0.4mm is made baseplate material, and compound concentration is the tin tetrachloride ethanolic soln of 0.9M, evenly is applied to the baseplate material surface, and dry down in 93 ℃.Then baseplate material was burnt 5 minutes in normal hexane flame, collect the product after burning, obtain spiral nanometer carbon fiber.The Fibre diameter of spiral nanometer carbon fiber is 60nm, and screw diameter is 100nm, and pitch is 140nm.Black powder shape product of the present invention is scattered in the ethanol, behind the ultra-sonic dispersion, drops in sample preparation on the copper mesh, adopt JEM-100CXII type transmission electron microscope observing sample topography then, pattern as shown in Figure 4.
Claims (9)
1. prepare the method for spiral nanometer carbon fiber, comprise the steps:
The precursor solution of catalyzer is coated on the baseplate material surface, and drying places the flame of organic solvent to burn then, collects the black powder shape product after burning, and is spiral nanometer carbon fiber.
The precursor solution of said catalyzer is the muriatic ethanolic soln that contains tin.
2. method according to claim 1 is characterized in that, said baseplate material is the pure nickel tinsel.
3. method according to claim 2 is characterized in that, said pure nickel sheet thicknesses is 0.2～0.6mm.
4. method according to claim 1 is characterized in that, the muriate of said tin is SnCl
45H
2O.
5. method according to claim 4 is characterized in that, the concentration of the muriate of tin in ethanolic soln is 0.08～0.2M.
6. method according to claim 1 is characterized in that, the said baseplate material drying temperature that scribbles the tin tetrachloride ethanolic soln is 85～95 ℃.
7. method according to claim 1 is characterized in that, said baseplate material combustion time in organic solvent flame is 5～15 minutes.
8. method according to claim 1 is characterized in that, said organic solvent is selected from the monohydroxy-alcohol of C2～C3 or the alkane of C5～C6.
9. method according to claim 8 is characterized in that, said organic solvent is an ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101480069A CN100439242C (en) | 2006-12-26 | 2006-12-26 | Method of preparing spiral nanometer carbon fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101480069A CN100439242C (en) | 2006-12-26 | 2006-12-26 | Method of preparing spiral nanometer carbon fiber |
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| CN100999315A CN100999315A (en) | 2007-07-18 |
| CN100439242C true CN100439242C (en) | 2008-12-03 |
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| CNB2006101480069A Expired - Fee Related CN100439242C (en) | 2006-12-26 | 2006-12-26 | Method of preparing spiral nanometer carbon fiber |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093712A (en) * | 2010-11-13 | 2011-06-15 | 中国石油大学(华东) | Preparation method of composite super capacitor electrode material |
| CN102515092B (en) * | 2011-12-02 | 2014-06-25 | 中国科学院化学研究所 | Method for manufacturing micro-spring |
| CN104157834B (en) * | 2014-08-26 | 2017-03-08 | 四川理工学院 | Spiral sodium rice carbon fiber is used as application and the GND preparation method of lithium ion battery negative material |
| CN111112596B (en) * | 2018-11-01 | 2021-12-28 | 国家纳米科学中心 | Chiral noble metal nano-particles and preparation method and application thereof |
| CN113149550B (en) * | 2021-04-12 | 2022-03-22 | 武汉三源特种建材有限责任公司 | Nano carbon fiber cement-based toughened and reinforced composite material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327093A (en) * | 2000-06-07 | 2001-12-19 | 华侨大学 | High elastic screw carbon fibre and its preparing method |
| US6986877B2 (en) * | 2002-01-08 | 2006-01-17 | Futaba Corporation | Method for preparing nano-carbon fiber and nano-carbon fiber |
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2006
- 2006-12-26 CN CNB2006101480069A patent/CN100439242C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327093A (en) * | 2000-06-07 | 2001-12-19 | 华侨大学 | High elastic screw carbon fibre and its preparing method |
| US6986877B2 (en) * | 2002-01-08 | 2006-01-17 | Futaba Corporation | Method for preparing nano-carbon fiber and nano-carbon fiber |
Non-Patent Citations (4)
| Title |
|---|
| Catalytic effects of metal carbides, oxides and Ni singlecrystal on the vapor growth of micro-coiled carbon fibers. S. Motojima, S Asakura,K Kasemura,et al.Carbon,Vol.34 No.3. 1996 |
| Catalytic effects of metal carbides, oxides and Ni singlecrystal on the vapor growth of micro-coiled carbon fibers. S. Motojima, S Asakura,K Kasemura,et al.Carbon,Vol.34 No.3. 1996 * |
| 螺旋纳米碳纤维的制备与表征. 于立岩，张乾，崔作林.高等化学学报，第26卷第1期. 2005 |
| 螺旋纳米碳纤维的制备与表征. 于立岩，张乾，崔作林.高等化学学报，第26卷第1期. 2005 * |
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