CN103172052B - The large-scale producing method of the adjustable amorphous carbon nanotube of a kind of length-to-diameter ratio - Google Patents
The large-scale producing method of the adjustable amorphous carbon nanotube of a kind of length-to-diameter ratio Download PDFInfo
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- CN103172052B CN103172052B CN201310150972.4A CN201310150972A CN103172052B CN 103172052 B CN103172052 B CN 103172052B CN 201310150972 A CN201310150972 A CN 201310150972A CN 103172052 B CN103172052 B CN 103172052B
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Abstract
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, being utilize vacuum intermediate-frequency induction melting furnace to prepare non-crystal carbon nano tube on a large scale, is the preparing technical field belonging to low-dimension nano material.Method is as follows: by iron protochloride and tetrafluoroethylene raw material ball milling, adopts the power of 5-80 kilowatt, and insulation 5-30 minute, after reaction terminates, black product is non-crystal carbon nano tube.Described iron protochloride and the mass ratio of tetrafluoroethylene are 1:(8.0-9.5).Beneficial effect of the present invention is: preparation method and preparation process are very simple, and the processing parameter in preparation process easily controls, one-step synthesis, can realize a large amount of preparation.
Description
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, being utilize vacuum intermediate-frequency induction melting furnace to prepare non-crystal carbon nano tube on a large scale, is the preparing technical field belonging to low-dimension nano material.
Background technology
Since Japanese S.Iijima in 1991 formally finds carbon nanotube (S.IijimaNature1991), carbon nanotube has caused extensive concern and the great interest of various countries investigator in worldwide.Carbon nanotube is the body of seamless, the hollow that the graphite flake layer formed by carbon atom is rolled into.Generally can be divided into Single Walled Carbon Nanotube and multi-walled carbon nano-tubes.
Non-crystal carbon nano tube is different with multilayer carbon nanotube from the individual layer that structural pipe wall is made up of good graphite flake layer, and its tube wall is made up of the carbon atom of many complete random arrangements, is characterized in short range order, longrange disorder.Therefore non-crystal carbon nano tube is even better in the Application Areas such as gas adsorption, support of the catalyst, also more easily carries out finishing with further functionalization.Therefore, the research and development of a large amount of, controlled, high-purity technology of preparing of non-crystal carbon nano tube are seemed extremely important.
At present, the method preparing non-crystal carbon nano tube 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 the challenges such as aftertreatment, length-to-diameter ratio be non-adjustable.Also do not see and use simple device, efficient, extensive, the report of preparing the adjustable non-crystal carbon nano tube of length-to-diameter ratio without any aftertreatment, a step.
Summary of the invention
For Problems existing in current non-crystal carbon nano tube material preparation process, the object of the invention is to, a kind of length-to-diameter ratio adjustable port is provided, directly prepares the technology of preparing of non-crystal carbon nano tube material on a large scale; The method comprises the following steps:
(1) polytetrafluorethylepowder powder is mixed in certain mass ratio with iron protochloride; Wherein the mass ratio of iron protochloride and tetrafluoroethylene is 1:(8.0-9.5)
(2) in mixed powder, add the dehydrated alcohol of certain volume, the volume ratio of dehydrated alcohol and mixed powder is (1-3): 1;
(3) slip of step (2) is poured in ball grinder, ball material mass ratio (2-6): 1, ball milling 2-10 hour;
(4) by the slurry filtration after ball milling, and between 60 ~ 90 DEG C 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 heating and thermal insulation after 5-30 minute, obtained 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 easily controls, one-step synthesis, can realize a large amount of preparation.
Accompanying drawing explanation
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
The present invention is further illustrated below in conjunction with embodiment
Embodiment 1
In the present embodiment, the iron protochloride adopted is analytical pure, and tetrafluoroethylene is micro mist.
1, preparation raw material
A certain amount of iron protochloride of precise and ptfe micropowder, make iron protochloride and ptfe micropowder mass ratio be 1:9.2.
2, ball milling pretreatment
Above-mentioned 1 Raw is poured in ball grinder, adds a certain amount of zirconia ball, make ball material mass ratio be 5:1, add a certain amount of dehydrated alcohol again, make the volume ratio of dehydrated alcohol and ball material be 2:1, setting drum's speed of rotation 300 revs/min, 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, and 70 degree dry 10 hours
4, Medium frequency induction prepares non-crystal carbon nano tube
By the raw material in above-mentioned 3, load in plumbago crucible, and be placed on inside vacuum induction furnace, be evacuated to 0.01Mpa, 8 kw of power heat 10 minutes, and be incubated 20 minutes, then Temperature fall is to room temperature; Take out black powder, i.e. obtained non-crystal carbon nano tube, its typical pattern is as Fig. 2, Fig. 5.Diameter 30-120 nanometer, length 10-20 micron.
Embodiment 2
A certain amount of iron protochloride of precise and ptfe micropowder, make iron protochloride and ptfe micropowder mass ratio be 1:8.8, and all the other steps, with embodiment 1, equally also obtain size and the similar non-crystal carbon nano tube of pattern.
Embodiment 3
By embodiment 1, the raw material after step 3 processes, load in plumbago crucible, and be placed on inside vacuum induction furnace, be evacuated to 0.01Mpa, 30 kw of power heat 6 minutes, and be incubated 20 minutes, then Temperature fall is to room temperature; Take out black powder, i.e. obtained non-crystal carbon nano tube, its typical pattern as Fig. 3, diameter 30-120 nanometer, length 1-2 micron.
Embodiment 4
By embodiment 1, the raw material after step 3 processes, load in plumbago crucible, and be placed on inside vacuum induction furnace, be evacuated to 0.01Mpa, 60 kw of power heat 4 minutes, and be incubated 20 minutes, then Temperature fall is to room temperature; Take out black powder, the non-crystal carbon nano tube that namely obtained pattern is peculiar, also claim amorphous carbon nano-hollow ball, its typical pattern as Fig. 4, diameter 60-120 nanometer, length 100-200 nanometer
As can be seen from above 4 embodiments, as long as make various parameter in preparation process, as preparation raw material proportioning, power and time keep within the specific limits, just can controlled mass preparing amorphous.In specific implementation process, those skilled in the art can carry out concrete enforcement according to the process parameters range when ratio range of raw material and Frequency Induction Heating, is not limited with above-mentioned four embodiments given by the present invention.
Above by four embodiments to invention has been detailed description; those skilled in the art is to be understood that; be no more than the present invention spirit and essential scope in; this the present invention makes certain amendment and distortion; such as adopt different power and the different technical parameters such as intensification and soaking time; still can realize result of the present invention, and not depart from protection scope of the present invention.
Claims (1)
1. a large-scale producing method for the adjustable amorphous carbon nanotube of length-to-diameter ratio, described method comprises the steps:
(1) polytetrafluorethylepowder powder is mixed in certain mass ratio with iron protochloride; Wherein the mass ratio of iron protochloride and tetrafluoroethylene is 1:(8.0-9.5);
(2) in mixed powder, add the dehydrated alcohol of certain volume, the volume ratio of dehydrated alcohol and mixed powder is (1-3): 1;
(3) pour in ball grinder by the slip of step (2), ball material mass ratio (2-6): 1, ball milling 2-10 hour, drum's speed of rotation is 300r/min;
(4) by the slurry filtration after ball milling, and between 60 ~ 90 DEG C 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 heating and thermal insulation after 5-30 minute, obtained non-crystal carbon nano tube; Described vacuum tightness is 0.01 MPa.
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| 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 |
|---|
| Carbon nanotube with amorphous carbon wall: α-CNT;Hitoshi Nishino, et al.;《Carbon》;2003;第41卷;2165-2167 * |
| Growth of amorphous carbon nanotube from poly(tetrafluoroethylene) and ferrous chloride;Hitoshi Nishino, et al.;《carbon》;2003;第41卷;2819-2823 * |
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