CN101049923A - Method for making opening and short cutting on single wall Nano carbon tube - Google Patents
Method for making opening and short cutting on single wall Nano carbon tube Download PDFInfo
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- CN101049923A CN101049923A CN 200610046231 CN200610046231A CN101049923A CN 101049923 A CN101049923 A CN 101049923A CN 200610046231 CN200610046231 CN 200610046231 CN 200610046231 A CN200610046231 A CN 200610046231A CN 101049923 A CN101049923 A CN 101049923A
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- walled carbon
- carbon nanotube
- single walled
- opening
- koh
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Abstract
This invention relates to a method for opening and cutting single-walled carbon nanotubs with a high efficiency. The method comprises: mixing single-walled carbon nanotubs and KOH at a ratio of 1 :( 4-7), ball-milling in a planetary ball mill under 500 rpm for 1-3 h, treating at 900 deg.C in Ar for 1-3 h, washing with HCl, and rinsing with deionized water to obtain purified, opened and cut single-walled carbon nanotubs. The method avoids strong acid refluxing and oxygen-containing atmosphere oxidation.
Description
Technical field:
The present invention relates to the post-processing technology of CNT (carbon nano-tube), a kind of opening and short blanking method of Single Walled Carbon Nanotube is provided especially.
Background technology:
Be prepared as in a large number its physics of research and chemical property and practical application of Single Walled Carbon Nanotube provide possibility at present.But the Single Walled Carbon Nanotube for preparing usually, length are tens microns or longer, and two ends are normally sealed.When Single Walled Carbon Nanotube is applied to gas adsorption or support of the catalyst, requires Single Walled Carbon Nanotube to have particular length and the port opened, thereby help entering and deviating from of particle.So cutting with opening, the weak point of Single Walled Carbon Nanotube has meaning of the utmost importance for its practical application.
There is the scholar to propose to adopt in oxygen-containing atmosphere the method weak point of oxidation and strong acid backflow poach to cut Single Walled Carbon Nanotube.But there is following shortcoming in this method: degree of oxidation is not easy control and consuming time longer in the oxygen-containing atmosphere; Lack the purpose of cutting with opening though strong acid backflow poach can reach, this technological process is serious to the structure deteriorate of Single Walled Carbon Nanotube, makes a part of Single Walled Carbon Nanotube change the carbonaceous fragment into, and yield is very low.Therefore people make great efforts to cut and hatch method at a kind of simple, effective, quick and high efficiency weak point of searching always.
Summary of the invention:
The object of the present invention is to provide a kind of opening and short blanking method of Single Walled Carbon Nanotube, realize the opening of Single Walled Carbon Nanotube and shortly cut and improve yield.
The invention provides a kind of treatment process that does not relate to strong acid backflow and oxygen-containing atmosphere oxidation.Concrete technology is: the Single Walled Carbon Nanotube behind the purifying is mixed by a certain percentage with solid-state KOH, through processing such as ball milling, pyroprocessing, HCl cleaning, deionized water rinsings, finally obtain pure opening and short Single Walled Carbon Nanotube of cutting.
Single Walled Carbon Nanotube of the present invention and KOH mixing and ball milling are meant by both by the mixed of 1/ (4～7); Described rare gas element is meant high-purity argon gas; Rotational speed of ball-mill is 500 rev/mins, time 1～3h; Pyroreaction is carried out under argon shield, and temperature is 900 ℃, time 1～3h.
The present invention has following characteristics:
1 with Single Walled Carbon Nanotube and the solid KOH mixed with 1/ (4～7), is ball milling on 500 rev/mins the planetary ball mill at rotating speed then, can reduce the granularity of KOH on the one hand, increases the contact area with Single Walled Carbon Nanotube; Single Walled Carbon Nanotube is mixed fully with KOH contact, for next step reaction is got ready.
Pyroprocessing under 2 argon shields makes the reaction of KOH and Single Walled Carbon Nanotube, and the mouth of pipe of etching tube wall and sealing generates carbon monoxide or carbonic acid gas, thereby reaches opening and short purpose of cutting.The reaction formula is as follows:
KOH+C＝CO(CO
2)+K+H
2
It is for metal and KOH Impurity removal that 3HCl cleans.
With the inventive method Single Walled Carbon Nanotube is carried out opening and short cutting, purity still can reach more than the 98wt%, and 40～50um before the length of Single Walled Carbon Nanotube tube bank is cut by weak point is reduced between 2～3um, and the sample opening rate can reach 70～90%.
Description of drawings:
The opening of accompanying drawing 1 Single Walled Carbon Nanotube and the short process flow sheet of cutting;
Accompanying drawing 2 openings and the short transmission electron microscope photo of cutting the back Single Walled Carbon Nanotube.
Embodiment:
It is that the Single Walled Carbon Nanotube of 1.85nm is mixed with KOH that embodiment of the present invention is mean diameter behind the purifying, through ball milling, pyroprocessing, HCl clean, deionized water rinsing handles, and finally obtains opening and short Single Walled Carbon Nanotube of cutting.Its technical process such as Fig. 1.
Embodiment 1
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; mix with the KOH of 600mg; at rotating speed ball milling 2h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 2h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing finally obtains pure opening and short Single Walled Carbon Nanotube of cutting.Through the projection electron microscopic observation, tube bank length is between the 2-3um, and the sample opening rate is 85%.
Embodiment 2
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; mix with the KOH of 400mg; at rotating speed ball milling 2h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 2h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing finally obtains pure opening and short Single Walled Carbon Nanotube of cutting.Through the projection electron microscopic observation, tube bank length is between the 2-3um, and the sample opening rate is 80%.
Embodiment 3
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; mix with the KOH of 400mg; at rotating speed ball milling 2h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 2h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing finally obtains pure opening and short Single Walled Carbon Nanotube of cutting.Through the projection electron microscopic observation, tube bank length is between the 2-3um, and the sample opening rate is 80%.
Embodiment 4
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; mix with the KOH of 600mg; at rotating speed ball milling 2h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 1h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing finally obtains pure opening and short Single Walled Carbon Nanotube of cutting.Through the projection electron microscopic observation, tube bank length is between the 2-3um, and the sample opening rate is 83%.
Embodiment 5
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; mix with the KOH of 600mg; at rotating speed ball milling 2h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 3h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing finally obtains pure opening and short Single Walled Carbon Nanotube of cutting.Through the projection electron microscopic observation, tube bank length is between the 2-3um, and the sample opening rate is 88%.
Embodiment 6
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; mix with the KOH of 600mg; at rotating speed ball milling 1h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 2h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing finally obtains pure opening and short Single Walled Carbon Nanotube of cutting.Through the projection electron microscopic observation, tube bank length is between the 2-3um, and the sample opening rate is 78%.
Embodiment 7
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; mix with the KOH of 600mg; at rotating speed ball milling 3h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 2h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing finally obtains pure opening and short Single Walled Carbon Nanotube of cutting.Through the projection electron microscopic observation, tube bank length is between the 2-3um, and the sample opening rate is 87%.
In order to verify the validity of above-mentioned method of purification, the present invention has carried out simultaneous test to above-mentioned Single Walled Carbon Nanotube, promptly changes the ratio of Single Walled Carbon Nanotube and KOH, the temperature and time of pyroprocessing etc., and test-results shows that embodiment 1 is preferred plan.
Comparative example 1
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; being blended in rotating speed with the KOH of 100mg is ball milling 2h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 2h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing is through transmission electron microscope observing; the tube bank mean length is 35um still, and aperture opening ratio is 10%.
Comparative example 2
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; being blended in rotating speed with the KOH of 800mg is ball milling 2h on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 2h under argon shield then, naturally cools to room temperature, and HCl cleans; deionized water rinsing; through transmission electron microscope observing, the tube bank mean length is 2um, and aperture opening ratio is 95%; but more carbon fragment is arranged in the sample, and purity is very low.
Comparative example 3
Take that mean diameter is the Single Walled Carbon Nanotube 100mg of 1.85nm behind the purifying; being blended in rotating speed with the KOH of 600mg is ball milling 30 minutes on 500 rev/mins the planetary ball mill; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 2h under argon shield then; naturally cool to room temperature; HCl cleans, and deionized water rinsing is through transmission electron microscope observing; the tube bank mean length is 25um, and aperture opening ratio is 25%.
Comparative example 4
Take that mean diameter is that the Single Walled Carbon Nanotube 100mg of 1.85nm and the KOH of 600mg are blended in ball milling 2h on the planetary ball mill that rotating speed is 500rm/min behind the purifying; temperature rise rate with 15 ℃/min is warmed up to 750 ℃ of constant temperature 2h under argon shield then; naturally cool to room temperature; HCl cleans; deionized water rinsing; through transmission electron microscope observing, the tube bank mean length is 30um, and aperture opening ratio is 30%.
Comparative example 5
Take that mean diameter is that the Single Walled Carbon Nanotube 100mg of 1.85nm and the KOH of 600mg are blended in ball milling 2h on the planetary ball mill that rotating speed is 500rm/min behind the purifying; temperature rise rate with 15 ℃/min is warmed up to 900 ℃ of constant temperature 30min under argon shield then; naturally cool to room temperature; HCl cleans; deionized water rinsing; through transmission electron microscope observing, the tube bank mean length is 35um, and aperture opening ratio is 40%.
Claims (4)
1, a kind of opening of Single Walled Carbon Nanotube and short blanking method mix Single Walled Carbon Nanotube behind the purifying by a certain percentage with KOH, handle through ball milling, pyroreaction, HCl cleaning, deionized water rinsing, finally obtain opening and short Single Walled Carbon Nanotube of cutting.
2, by the opening and the short blanking method of the described Single Walled Carbon Nanotube of claim 1, it is characterized in that: described Single Walled Carbon Nanotube and KOH blended proportional range by a certain percentage are 1: (4～7) mass ratio.
3, by the opening of the described Single Walled Carbon Nanotube of claim 1 and short blanking method, it is characterized in that: it is the mixture of ball milling Single Walled Carbon Nanotube and KOH on 500 rev/mins the planetary ball mill that described ball milling is meant at rotating speed, and the ball milling time is 1～3h.
4, by the opening and the short blanking method of the described Single Walled Carbon Nanotube of claim 1, it is characterized in that: described pyroprocessing is meant that temperature is in 900 ℃ of constant temperature 1～3h under the high-purity argon gas protection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610046231 CN101049923A (en) | 2006-04-03 | 2006-04-03 | Method for making opening and short cutting on single wall Nano carbon tube |
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|---|---|---|---|
| CN 200610046231 CN101049923A (en) | 2006-04-03 | 2006-04-03 | Method for making opening and short cutting on single wall Nano carbon tube |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106976868A (en) * | 2017-06-05 | 2017-07-25 | 国家纳米科学中心 | The low-dimensional method of CNT |
| CN112978717A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for shortening carbon nano tube |
| CN114890408A (en) * | 2022-05-12 | 2022-08-12 | 湖南金天铝业高科技股份有限公司 | Preparation method of carbon nano tube with controllable size distribution and preparation method of carbon nano tube reinforced aluminum matrix composite |
-
2006
- 2006-04-03 CN CN 200610046231 patent/CN101049923A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106976868A (en) * | 2017-06-05 | 2017-07-25 | 国家纳米科学中心 | The low-dimensional method of CNT |
| CN112978717A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for shortening carbon nano tube |
| CN114890408A (en) * | 2022-05-12 | 2022-08-12 | 湖南金天铝业高科技股份有限公司 | Preparation method of carbon nano tube with controllable size distribution and preparation method of carbon nano tube reinforced aluminum matrix composite |
| CN114890408B (en) * | 2022-05-12 | 2023-08-22 | 湖南湘投轻材科技股份有限公司 | Preparation method of carbon nano tube with controllable size distribution and preparation method of carbon nano tube reinforced aluminum matrix composite material |
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