CN1473657A - Method for opening multi-wall nano carbon tube end by directly ball milling - Google Patents
Method for opening multi-wall nano carbon tube end by directly ball milling Download PDFInfo
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- CN1473657A CN1473657A CNA031296858A CN03129685A CN1473657A CN 1473657 A CN1473657 A CN 1473657A CN A031296858 A CNA031296858 A CN A031296858A CN 03129685 A CN03129685 A CN 03129685A CN 1473657 A CN1473657 A CN 1473657A
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Abstract
The present invention provides the direct ball milling process for opening multi-wall carbon nanotube end with large 20 mm diameter milling ball and small 10 mm diameter milling ball, with the ratio between the large milling ball number and the small milling ball number being 1-4 to 10-26. After all the large milling ball, the small milling ball and carbon nanotube are set inside ball mill, the ball mill is twice vacuum pumped and protective gas is led into the ball mill, and ball milling is performed at rotation speed of 100-400 rpm for 4-90 hr. The ball milling process to modify multi-wall carbon nanotube is simple and high in repeatability, has most of the carbon nanotube opened and no damage to the structure of carbon nanotube as shown as the XRD data.
Description
Technical field
The present invention relates to a kind ofly make the open-ended method of CNT with the common multiple-wall carbon nanotube of the direct ball milling of ball mill.
Background technology
CNT is because its good electricity, mechanics and thermal property all have good application prospects in storage hydrogen, an emission, a lot of fields such as ripple, electrode material of inhaling.CNT being carried out modification, connect organic group at the two ends of carbon pipe, carry out compoundly with other materials such as high molecular polymer and other big molecules then, make full use of the property of CNT, is a focus of current CNT study on the modification.But CNT is because its arc discharge method, the growth pattern that laser evaporation method and chemical vapour deposition technique are special, and its pipe end does not have the opening that is used to connect organic group.
Summary of the invention
The present invention aims to provide the one or both ends opening that the method for using ball milling makes common multiple-wall carbon nanotube, and the further modification for multiple-wall carbon nanotube connects organic group and provides convenience.
Direct ball milling of the present invention makes the open-ended method of multiple-wall carbon nanotube; be that steel ball with external diameter 20mm is big abrading-ball; the steel ball of 10mm is little abrading-ball; in big abrading-ball number: little abrading-ball number: CNT quality (gram)=1～4: 10～26: 0.5～2.5 ratio; big abrading-ball, little abrading-ball, CNT are put into ball grinder; vacuumize twice; exhaust vacuum at every turn and in ball grinder, feed protective gas; carry out ball milling then; the rotating speed of ball milling is 100～400 rev/mins, and the ball milling time is 4～90 hours.When generally needing long-time ball milling, in mechanical milling process, stopped 1 hour every 2～3 hours.
The present invention, best proportioning is big abrading-ball number: little abrading-ball number: CNT quality (gram)=2～4: 15～24: 0.8～1.5.Preferred rotational speed of ball-mill is 200～300 rev/mins, and the ball milling time is 8～30 hours.Above-mentioned protective gas is nitrogen or argon gas, helium inert gas.
The present invention uses ball milling that multiple-wall carbon nanotube is carried out modification, and is simple to operate, good reproducibility, and the multiple-wall carbon nanotube overwhelming majority opening of ball milling, the data of XRD show that the structure of carbon pipe is not damaged.
Description of drawings
Fig. 1 is the XRD experimental result of CNT before and after having ground;
Fig. 2 is transmission electron microscopy (TEM) photo of CNT behind the ball milling.
The specific embodiment
Embodiment is 10nm～25nm with the diameter of chemical vapour deposition technique preparation, and purity is example at the common multiple-wall carbon nanotube more than 80%.
Embodiment 1:
Get 4 of big abrading-balls in proportion, 20 of little abrading-balls, CNT 1.0 grams are put in the ball grinder, vacuumize one time 10 minutes, pour helium then in ball grinder, vacuumize one time 5 minutes again, pour helium again in ball grinder, can carry out ball milling.Ball milling speed is 250 rev/mins, and the ball milling time is 8 hours, in mechanical milling process, stops 1 hour every 2 hours, restarts again.Sample takes out uses transmission electron microscope observing, and finding has a large amount of CNT openings, mainly is an end opening.The XRD diffraction experiment shows that the structure of CNT is not destroyed.Fig. 1 is the XRD experimental result of CNT before and after having ground.
Embodiment 2:
Get 4 of big abrading-balls in proportion, 24 of little abrading-balls, CNT 2.0 grams are put in the ball grinder, vacuumize one time 10 minutes, pour helium then in ball grinder, vacuumize one time 5 minutes again, pour helium again in ball grinder, can carry out ball milling.Ball milling speed is 250 rev/mins, and the ball milling time is 20 hours, in the mechanical milling process, stops 1 hour every 3 hours.Sample takes out uses transmission electron microscope observing, finds to have a large amount of CNT opening (mainly being both ends open).The XRD diffraction experiment shows that the structure of CNT is not destroyed.Fig. 2 has shown transmission electron microscopy analysis (TEM) photo of CNT behind the ball milling.
Experiment shows, CNT is mainly in the majority with both ends open more than 18 hours the time ball milling time usually.
Claims (6)
1. directly ball milling makes the open-ended method of multiple-wall carbon nanotube; it is characterized in that the steel ball with external diameter 20mm is big abrading-ball; the steel ball of 10mm is little abrading-ball; in big abrading-ball number: little abrading-ball number: CNT quality (gram)=1～4: 10～26: 0.5～2.5 ratio; big abrading-ball, little abrading-ball, CNT are put into ball grinder; vacuumize twice; exhaust vacuum at every turn and in ball grinder, feed protective gas; carry out ball milling then; the rotating speed of ball milling is 100～400 rev/mins, and the ball milling time is 4～90 hours.
2. direct ball milling according to claim 1 makes the open-ended method of multiple-wall carbon nanotube, it is characterized in that big abrading-ball number: little abrading-ball number: CNT quality (gram)=2～4: 1 5～24: 0.8～1.5.
3. direct ball milling according to claim 1 makes the open-ended method of multiple-wall carbon nanotube, it is characterized in that said protective gas is nitrogen or argon gas, helium inert gas.
4. direct ball milling according to claim 1 makes the open-ended method of multiple-wall carbon nanotube, and the rotating speed that it is characterized in that ball milling is 200～300 rev/mins.
5. the open-ended method of multiple-wall carbon nanotube that makes according to claim 1, the time that it is characterized in that ball milling is 8～30 hours.
6. the open-ended method of multiple-wall carbon nanotube that makes according to claim 1 is characterized in that in mechanical milling process, stops 1 hour every 2～3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031296858A CN1473657A (en) | 2003-06-30 | 2003-06-30 | Method for opening multi-wall nano carbon tube end by directly ball milling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031296858A CN1473657A (en) | 2003-06-30 | 2003-06-30 | Method for opening multi-wall nano carbon tube end by directly ball milling |
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| Publication Number | Publication Date |
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| CN1473657A true CN1473657A (en) | 2004-02-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CNA031296858A Pending CN1473657A (en) | 2003-06-30 | 2003-06-30 | Method for opening multi-wall nano carbon tube end by directly ball milling |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058721B (en) * | 2006-04-21 | 2010-09-29 | 清华大学 | Method of preparing heat interfacial material |
| CN110721776A (en) * | 2019-12-17 | 2020-01-24 | 广东欧文莱陶瓷有限公司 | Secondary ball milling method |
-
2003
- 2003-06-30 CN CNA031296858A patent/CN1473657A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058721B (en) * | 2006-04-21 | 2010-09-29 | 清华大学 | Method of preparing heat interfacial material |
| CN110721776A (en) * | 2019-12-17 | 2020-01-24 | 广东欧文莱陶瓷有限公司 | Secondary ball milling method |
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