CN103172052A - Large-scale preparation method of amorphous carbon nanotubes with adjustable length-diameter ratio - Google Patents
Large-scale preparation method of amorphous carbon nanotubes with adjustable length-diameter ratio Download PDFInfo
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- CN103172052A CN103172052A CN2013101509724A CN201310150972A CN103172052A CN 103172052 A CN103172052 A CN 103172052A CN 2013101509724 A CN2013101509724 A CN 2013101509724A CN 201310150972 A CN201310150972 A CN 201310150972A CN 103172052 A CN103172052 A CN 103172052A
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Abstract
The invention relates to a large-scale preparation method of amorphous carbon nanotubes with adjustable length-diameter ratio and particularly relates to large-scale preparation of the amorphous carbon nanotubes by utilizing a vacuum medium-frequency induction smelting furnace, belonging to the technical field of preparation of low-dimensional nanomaterials. The method is as follows: performing ball milling on ferrous chloride and polytetrafluoroethylene raw materials, adopting the power of 5-80kw, performing heat preservation for 5-30 minutes, and obtaining black products, namely the amorphous carbon nanotubes after the end of reaction. The weight ratio of the ferrous chloride to the polytetrafluoroethylene is 1:(8.0-9.5). The preparation method disclosed by the invention has the beneficial effects that the preparation method and the preparation steps are very simple, process parameters in the preparation process are easy to control, and one-step synthesis and large-scale preparation can be realized.
Description
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Technical field
The present invention relates to the large-scale producing method of the adjustable non-crystal carbon nano tube of a kind of length-to-diameter ratio, particularly, is to utilize the vacuum intermediate-frequency induction melting furnace to prepare on a large scale non-crystal carbon nano tube, is the preparing technical field that belongs to low-dimension nano material.
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Background technology
Since Japanese S. Iijima in 1991 formally finds carbon nanotube (S. Iijima Nature 1991), carbon nanotube has caused various countries investigators' extensive concern and very big interest in worldwide.Carbon nanotube is the body of seamless, the hollow that is rolled into by the graphite flake layer that carbon atom forms.Generally can be divided into Single Walled Carbon Nanotube and multi-walled carbon nano-tubes.
Non-crystal carbon nano tube is different by individual layer and multilayer carbon nanotube that good graphite flake layer forms from structural pipe wall, and its tube wall is that the carbon atom by many complete random arrangements is consisted of, and is characterized in that short range order, long-range are unordered.Therefore non-crystal carbon nano tube is even better in Application Areass such as gas adsorption, support of the catalyst, also more easily carries out finishing with further functionalization.Therefore, the research and development a large amount of, controlled, high-purity technology of preparing of non-crystal carbon nano tube seemed extremely important.
At present, the method for preparing non-crystal carbon nano tube of having reported mainly contains arc-over [1-2], chemical vapour deposition [3-4], thermolysis organism solvent method [5-6] and electron cyclotron resonace advocate approach [7] etc.; But these methods all exist and yield poorly, energy consumption is high, equipment is complicated, must extra catalyst, must aftertreatment, the challenge such as length-to-diameter ratio is non-adjustable.Also do not see use simple device, efficient, extensive, without the report of any aftertreatment, an adjustable non-crystal carbon nano tube of step preparation length-to-diameter ratio.
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Summary of the invention
Problem for existing in present non-crystal carbon nano tube material preparation process the object of the invention is to, and a kind of length-to-diameter ratio adjustable port is provided, directly extensive preparation non-crystal carbon nano tube material preparation technology; The method comprises the following steps:
(1) polytetrafluorethylepowder powder is mixed in the certain mass ratio with iron protochloride; Wherein the mass ratio of iron protochloride and tetrafluoroethylene is 1:(8.0-9.5)
(2) add the dehydrated alcohol of certain volume in the mixed powder, the volume ratio of dehydrated alcohol and mixed powder is (1-3): 1;
(3) slip of step (2) is poured in ball grinder into ball material mass ratio (2-6): 1, ball milling 2-10 hour;
(4) with the slurry filtration after ball milling, and between 60～90 ℃ dry 5～12 hours;
(5) dried powder in step (4) is inserted in plumbago crucible, and put in vacuum medium frequency induction furnace, under vacuum state, use 5-80 kw of power heat tracing after 5-30 minute, make non-crystal carbon nano tube.
Further: in described step (3), drum's speed of rotation is 300r/min.
Further: in described step (5), vacuum tightness is 0.01 MPa.
Beneficial effect of the present invention is: preparation method and preparation process are very simple, and the processing parameter in preparation process is easily controlled, and one-step synthesis can be realized a large amount of preparations.
Description of drawings
Fig. 1 is the typical Raman spectrum schematic diagram of non-crystal carbon nano tube of preparation.
When Fig. 2 is 8 kilowatts of induction heating, the surface topography schematic diagram of non-crystal carbon nano tube.
When Fig. 3 is 30 kilowatts of induction heating, the surface topography schematic diagram of non-crystal carbon nano tube.
When Fig. 4 is 60 kilowatts of induction heating, the surface topography schematic diagram of non-crystal carbon nano tube (carbon hollow nanospheres).
Fig. 5 is the typical high-resolution-ration transmission electric-lens schematic diagram of non-crystal carbon nano tube.
Embodiment
Further illustrate the present invention below in conjunction with embodiment
Embodiment 1
In the present embodiment, the iron protochloride that adopts is analytical pure, and tetrafluoroethylene is micro mist.
1, preparation raw material
Accurate a certain amount of iron protochloride of weighing and ptfe micropowder, making iron protochloride and ptfe micropowder mass ratio is 1:9.2.
2, ball milling pretreatment
Above-mentioned 1 Raw is poured in ball grinder, added a certain amount of zirconia ball, making ball material mass ratio is 5:1, add again a certain amount of dehydrated alcohol, the volume ratio that makes dehydrated alcohol and ball material is 2:1, sets 300 rev/mins of drum'ss speed of rotation, and ball milling went out zirconia ball with strainer filtering after 8 hours;
3, drying and processing
Raw material in above-mentioned 2 is put into baking oven, 70 dry 10 hours of degree
4, Medium frequency induction prepares non-crystal carbon nano tube
With the raw material in above-mentioned 3, in the plumbago crucible of packing into, and be placed on the vacuum induction furnace the inside, be evacuated to 0.01Mpa, 8 kw of power heating 10 minutes are incubated 20 minutes, then naturally are cooled to room temperature; Take out black powder, namely make non-crystal carbon nano tube, its typical pattern such as Fig. 2, Fig. 5.Diameter 30-120 nanometer, length 10-20 micron.
Embodiment 2
Accurate a certain amount of iron protochloride of weighing and ptfe micropowder, making iron protochloride and ptfe micropowder mass ratio is 1:8.8, all the other steps equally also obtain the similar non-crystal carbon nano tube of size and pattern with embodiment 1.
Embodiment 3
With embodiment 1, the raw material after processing through step 3 in the plumbago crucible of packing into, and is placed on inside vacuum induction furnace, is evacuated to 0.01Mpa, and 30 kw of power heating 6 minutes are incubated 20 minutes, then naturally are cooled to room temperature; Take out black powder, namely make non-crystal carbon nano tube, its typical pattern such as Fig. 3, diameter 30-120 nanometer, length 1-2 micron.
Embodiment 4
With embodiment 1, the raw material after processing through step 3 in the plumbago crucible of packing into, and is placed on inside vacuum induction furnace, is evacuated to 0.01Mpa, and 60 kw of power heating 4 minutes are incubated 20 minutes, then naturally are cooled to room temperature; Take out black powder, namely make the peculiar non-crystal carbon nano tube of pattern, also claim the amorphous carbon nano-hollow ball, its typical pattern such as Fig. 4, diameter 60-120 nanometer, length 100-200 nanometer
Can find out from above 4 embodiment, as long as make various parameters in preparation process, as preparation raw material proportioning, power and time maintenance within the specific limits, just can controlled mass preparing amorphous.In specific implementation process, the process parameters range when those skilled in the art can be according to the ratio range of raw material and Frequency Induction Heating is carried out concrete enforcement, is not limited with given above-mentioned four embodiment of the present invention.
Abovely by four embodiment, the present invention is described in detail; those skilled in the art is to be understood that; in being no more than the present invention's spirit and essential scope; this the present invention makes certain modification and distortion; such as adopting different power and the different technical parameters such as intensification and soaking time; still can realize result of the present invention, and not break away from protection scope of the present invention.
Claims (3)
1. the large-scale producing method of the adjustable amorphous carbon nanotube of length-to-diameter ratio, described method comprises the steps:
(1) polytetrafluorethylepowder powder is mixed in the certain mass ratio with iron protochloride; Wherein the mass ratio of iron protochloride and tetrafluoroethylene is 1:(8.0-9.5)
(2) add the dehydrated alcohol of certain volume in the mixed powder, the volume ratio of dehydrated alcohol and mixed powder is (1-3): 1;
(3) slip of step (2) is poured in ball grinder into ball material mass ratio (2-6): 1, ball milling 2-10 hour;
(4) with the slurry filtration after ball milling, and between 60～90 ℃ dry 5～12 hours;
(5) dried powder in step (4) is inserted in plumbago crucible, and put in vacuum medium frequency induction furnace, under vacuum state, use 5-80 kw of power heat tracing after 5-30 minute, make non-crystal carbon nano tube.
2. method according to claim 1, it is characterized in that: in described step (3), drum's speed of rotation is 300r/min.
3. method according to claim 1, it is characterized in that: in described step (5), vacuum tightness is 0.01 MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036112A (en) * | 2015-07-24 | 2015-11-11 | 北京科技大学 | Preparation method of carbon nano-material having adjustable length to diameter ratio and mesoporous hollow structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6479028B1 (en) * | 2000-04-03 | 2002-11-12 | The Regents Of The University Of California | Rapid synthesis of carbon nanotubes and carbon encapsulated metal nanoparticles by a displacement reaction |
| CN101337667A (en) * | 2007-07-04 | 2009-01-07 | 中国科学院理化技术研究所 | Method for preparing carbon nanotube or magnetic nanometer carbon ball |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6479028B1 (en) * | 2000-04-03 | 2002-11-12 | The Regents Of The University Of California | Rapid synthesis of carbon nanotubes and carbon encapsulated metal nanoparticles by a displacement reaction |
| CN101337667A (en) * | 2007-07-04 | 2009-01-07 | 中国科学院理化技术研究所 | Method for preparing carbon nanotube or magnetic nanometer carbon ball |
Non-Patent Citations (2)
| Title |
|---|
| HITOSHI NISHINO, ET AL.: "Carbon nanotube with amorphous carbon wall: α-CNT", 《CARBON》 * |
| HITOSHI NISHINO, ET AL.: "Growth of amorphous carbon nanotube from poly(tetrafluoroethylene) and ferrous chloride", 《CARBON》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036112A (en) * | 2015-07-24 | 2015-11-11 | 北京科技大学 | Preparation method of carbon nano-material having adjustable length to diameter ratio and mesoporous hollow structure |
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