CN101962169A - Method for preparing carbon nanotubes filled with metallic oxide - Google Patents
Method for preparing carbon nanotubes filled with metallic oxide Download PDFInfo
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- CN101962169A CN101962169A CN2010102825710A CN201010282571A CN101962169A CN 101962169 A CN101962169 A CN 101962169A CN 2010102825710 A CN2010102825710 A CN 2010102825710A CN 201010282571 A CN201010282571 A CN 201010282571A CN 101962169 A CN101962169 A CN 101962169A
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Abstract
The invention relates to the technical field of lithium ion batteries, in particular to a method for preparing carbon nanotubes filled with metallic oxide. The method comprises the following steps of: modifying the surfaces of the carbon nanotubes, namely adding the carbon nanotubes into aqueous solution of sodium dodecyl benzene sulfonate, scattering the carbon nanotubes in the solution by ultrasonication, and then removing deposits by separation so as to obtain solution of carbon nanotube-sodium dodecyl benzene sulfonate; filling the carbon nanotubes, namely preparing solution of metallic nitrate, then dropping the prepared solution of metallic nitrate to the solution of carbon nanotube-sodium dodecyl benzene sulfonate for ultrasonic treatment, and standing to obtain black deposits; and performing thermal treatment, namely performing the thermal treatment on the obtained black deposits at a high temperature to obtain the carbon nanotubes filled with the metallic oxide. The method for preparing the carbon nanotubes filled with the metallic oxide avoids an acid treatment procedure in the prior art and the damage of the acid treatment to the structures of the carbon nanotubes, and has a simple preparation process and wide application prospect.
Description
Technical field
The present invention relates to the lithium ion battery electrode material technical field, especially a kind of preparation method who fills the CNT of metal oxide.
Background technology
CNT has the one-dimensional space of nanoscale, many morphosis, physical property and the chemical property of filler is not only far different with macrostate, and also influenced the character of CNT to a certain extent, so carbon nano-tube filled technology becomes the focus of people's research.
After in CNT (CNTs), filling metals such as Sn, Ag, Fe, Co, Al, these metals or its oxide can form alloy with lithium, and the existence of CNT can also suppress the volumetric expansion of above-mentioned metal in the embedding lithium process or its oxide, is applied to the lithium ion battery industrial circle so can be used as the active material with height ratio capacity and good circulation performance; CNT behind the metals such as filling Fe, Ni, Co will have the magnetic of 430oe～1070oe to be rectified stupid value and has good single shaft magnetic domain anisotropic along filling direction, is one of manufacturing focal point of high density magnetic storage; In addition, because outer field carbon pipe can prevent to manage inner catalyst and material on every side reacts, can also be with the carrier of carbon pipe as the nanoscale catalyst; Moreover the nanoscale cavity that can also utilize CNT is as template, and the metal nanometer line of preparation one dimension form to be applied to constructing of nanometer circuit and nanoelectronic components and parts, is applied to following electronics industry, as aspects such as computer chips.
Hence one can see that, and the development prospect of carbon nano-tube filled technology is very wide, all has ample scope for one's abilities in all fields.The filling technique of carbon current nanotube mainly comprises original position completion method and capillarity completion method two big classes; The former fills foreign substance in the preparation CNT, promptly directly prepare the composite that CNT coats foreign substance; The latter then utilizes the capillarity of carbon nanotubes lumen that foreign substance is filled and enters CNT.The original position completion method need be carried out under the temperature of several Baidu even thousands of degree, though can fill foreign substance more continuously in the CNTs the inside, should not control the growth of CNT, operates also not easy.Thereby, commonplace by the use that capillarity is filled the method enter CNT with foreign substance.The solid phase fusion completion method that grown up at present and liquid phase wet-chemical completion method, the solid phase fusion completion method can only be packed into CNT by the material that surface tension is less, and suitable material is less relatively; And liquid phase wet-chemical completion method condition is relatively gentle, and is wider to the adaptability of filler.People utilize the method to obtain being filled with the CNT of the oxide of Fe, Co, Ni, U, Mo, Sn, Nb, Sm, Eu, La, Ce, Pr, Y, Zr, Cd etc. and simple metal Pd, Ag, Au.
Yet present nearly all capillarity fill method all will though this step has reached the purpose of purifying, activation and opening, also destroy the structure of CNT simultaneously through the step of peracid treatment opening.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide provides a kind of and can avoid under the acid-treated prerequisite that external metal oxide is filled the method that enters CNT, and its preparation process is simple, has a extensive future.
To achieve these goals, technical scheme of the present invention is as follows:
A kind of preparation method who fills the CNT of metal oxide, this method comprise carbon nano tube surface modification operation, carbon nano-tube filled and heat treatment step;
Described carbon nano tube surface is modified operation:
Take by weighing CNT earlier and join in the sodium dodecyl benzene sulfonate aqueous solution, with ultrasonic under power 50W～300W, CNT is fully disperseed in solution with Ultrasonic Cell Disruptor;
Then, separate, remove sediment, make CNT-neopelex solution with the centrifugal speed of 3000r/min～20000r/min;
Described carbon nano-tube filled operation is:
Elder generation's preparing metal nitrate solution, getting the metal-nitrate solutions for preparing splashes in CNT-neopelex solution, use Ultrasonic Cell Disruptor ultrasonic again, obtain black precipitate behind static 10h～24h and be the CNT of having filled metal nitrate with power 50W～300W;
Described heat treatment step is:
The CNT of having filled metal nitrate is carried out high-temperature heat treatment in inert atmospheres such as nitrogen, argon gas, treatment temperature is 300～800 ℃.After decomposing, metal nitrate obtained filling the CNT of metal oxide.
Preferably, described carbon nano tube surface is modified in the operation, and the mass concentration of sodium dodecyl benzene sulfonate aqueous solution is 2%～15%.
Preferably, described carbon nano tube surface is modified in the operation, is 3～8 hours with ultrasonic time.
Preferably, described carbon nano tube surface is modified in the operation, and the centrifugation time is 0.5～3 hour.
Preferably, in the described carbon nano-tube filled operation, metal-nitrate solutions is 20%～100% a metal-nitrate solutions of saturated concentration.
Preferably, in the described carbon nano-tube filled operation, ultrasonic time is 0.5h～5h.
Preferably, in the described heat treatment step, heat treatment temperature is 300～800 ℃.
The present invention includes carbon nano tube surface and modify operation and carbon nano-tube filled operation; Take by weighing CNT earlier and join in the sodium dodecyl benzene sulfonate aqueous solution, CNT is disperseed in solution with ultrasonication; Separate the removal sediment then and make CNT-neopelex solution; Follow the preparing metal nitrate solution, getting the metal-nitrate solutions for preparing again splashes in CNT-neopelex solution ultrasonic, obtain black precipitate after static and be the CNT of having filled metal nitrate, the CNT that will obtain having filled metal nitrate at last carries out elevated temperature heat and goes out the CNT that has promptly obtained filling metal oxide in inert atmosphere; The present invention has not only avoided acid treatment operation of the prior art, avoided the destruction of acid treatment to carbon nano tube structure, and its preparation process is simple, has a extensive future; Especially the metal oxide filling carbon nano-pipe material of the li-ion electrode materials of a kind of high electrochemistry capacitance realized by technical scheme of the present invention and good circulation performance, carbon nano-tube material not only can be filled by comparatively continuous material, and external substance can enter the CNT depths, in addition from an end to an other end; Its electrochemistry capacitance is 400～600mAhg after testing
-1, and have excellent cycle performance.
The specific embodiment
Embodiment 1
(1) preparation of CNT-SDS solution
Take by weighing 120.4mgSDS, add 7000 μ L H
2O makes the SDS dissolving.Take by weighing the 14.2mg CNT and add in the SDS solution, in ice-water bath, use the power ultrasonic 6h of Ultrasonic Cell Disruptor with 50W.Solution is overnight leave standstill after, ultrasonic 2h under same condition again is centrifugation 3 hours under the speed of 3000r/min at rotating speed then, obtains CNT-SDS solution.
(2) Co (NO
3)
2The preparation of solution
Get Co (NO
3)
2(chemical pure) 2781.0mg adds 2000 μ L distilled water, utilizes ultrasonic cleaning instrument ultrasound condition to make Co (NO
3)
2Fully dissolving.
(3) filling of CNT
Get 500 μ L Co (NO
3)
2Solution adds in 1400 μ L CNT-SDS solution, adds 3200 μ L H again
2The O dilution.Then, mixed solution is used the power ultrasonic 5h of Ultrasonic Cell Disruptor with 50W in ice-water bath, obtain muddy suspension.Get black precipitate after leaving standstill 10h, and the several washing and precipitating.
(4) heat treatment
With putting into tube furnace after the deposit oven dry, under nitrogen atmosphere, be heated to 350 ℃, decompose Co (NO
3)
2After obtain having filled Co
3O
4CNT.
Embodiment 2
(1) preparation of CNT-SDS solution
Take by weighing 122.4mgSDS, add 7500 μ L H
2O makes the SDS dissolving.Take by weighing the 14.2mg CNT and add in the SDS solution, in ice-water bath, use the power ultrasonic 3h of Ultrasonic Cell Disruptor with 200W.Solution is overnight leave standstill after, ultrasonic 2h under same condition again is centrifugation 1 hour under the speed of 13000r/min at rotating speed then, obtains CNT-SDS solution.
(2) Co (NO
3)
2The preparation of solution
Get Co (NO
3)
2(chemical pure) 2791.0mg adds 3000 μ L distilled water, utilizes ultrasonic cleaning instrument ultrasound condition to make Co (NO
3)
2Fully dissolving.
(3) filling of CNT
Get 500 μ L Co (NO
3)
2Solution adds in 1400 μ L CNT-SDS solution, adds 3200 μ L H again
2The O dilution.Then, mixed solution is used the power ultrasonic 2h of Ultrasonic Cell Disruptor with 180W in ice-water bath, obtain muddy suspension.Get black precipitate after leaving standstill 24h, and the several washing and precipitating.
(4) heat treatment
With putting into tube furnace after the deposit oven dry that obtains, under nitrogen atmosphere, be heated to 500 ℃, decompose Co (NO
3)
2After obtain Co
3O
4The carbon nano-tube material of filling.CNT is blocked in ultrasonic procedure, and external substance has entered in the CNT.
(6) electro-chemical test
Get above-mentioned material 100mg, sneak into 10mg Kynoar (PVDF), drip the N-methyl pyrrolidone and transfer to pulpous state, ultrasonic dispersion 30 minutes is coated in the slurry that obtains on the Copper Foil collector, 100 ℃ of oven dry in 10 hours.Using the lithium sheet is to electrode, and polyethylene is a barrier film, and the organic solution of lithium hexafluoro phosphate is electrolyte, is assembled into the buckle type lithium-ion battery in being full of the glove box of argon gas.Place 24 tests as a child.Material specific capacity is 478mAhg
-1, still can keep 432mAhg after 30 circulations
-1
Embodiment 3
(1) preparation of CNT-SDS solution
Take by weighing 122.4mgSDS, add 7500 μ L H
2O makes the SDS dissolving.Take by weighing the 14.2mg CNT and add in the SDS solution, in ice-water bath, use the power ultrasonic 3h of Ultrasonic Cell Disruptor with 200W.Solution is overnight leave standstill after, ultrasonic 2h under same condition again is centrifugation 1 hour under the speed of 13000r/min at rotating speed then, obtains CNT-SDS solution.
(2) Fe (NO
3)
3The preparation of solution
Get Fe (NO
3)
3(chemical pure) 3810.4mg adds 4000 μ L distilled water, utilizes ultrasonic cleaning instrument ultrasound condition to make Fe (NO
3)
3Fully dissolving.
(3) filling of CNT
Get 500 μ L Fe (NO
3)
3Solution joins in 1000 μ L CNT-SDS solution, and it is muddy that settled solution becomes, and suspension occurs.With solution left standstill 24h, make that molecule fully adsorbs in the solution.Afterwards, the black precipitate of cleaning gained for several times.
(5) heat treatment
With putting into tube furnace after the sediment oven dry that obtains, in argon gas atmosphere, be heated to 650 ℃, decompose Fe (NO
3)
3After obtain Fe
2O
3The carbon nano-tube material of filling.CNT is blocked in ultrasonic procedure, and external substance has entered in the CNT.
(6) electro-chemical test
Get above-mentioned material 80mg, sneak into 8mg Kynoar (PVDF), drip the N-methyl pyrrolidone and transfer to pulpous state, ultrasonic dispersion 20 minutes is coated in the slurry that obtains on the Copper Foil collector, 100 ℃ of oven dry in 10 hours.Using the lithium sheet is to electrode, and polyethylene is a barrier film, and the organic solution of lithium hexafluoro phosphate is electrolyte, is assembled into the buckle type lithium-ion battery in being full of the glove box of argon gas.Place 24 tests as a child.Material specific capacity is 426mAhg
-1, still can keep 388mAhg after 30 circulations
-1
Embodiment 4
(1) preparation of CNT-SDS solution
Take by weighing 132.4mgSDS, add 8000 μ L H
2O makes the SDS dissolving.Take by weighing 15.4mg CNT (sample IRM-B) and add in the SDS solution, in ice-water bath, use the power ultrasonic 2h of Ultrasonic Cell Disruptor with 300W.Solution is overnight leave standstill after, ultrasonic 1h under same condition again is centrifugation 0.5 hour under the speed of 20000r/min at rotating speed then, obtains CNT-SDS solution.
(2) Fe (NO
3)
3The preparation of solution
Get Fe (NO
3)
3(chemical pure) 3920.4mg adds 5000 μ L distilled water, utilizes ultrasonic cleaning instrument ultrasound condition to make Fe (NO
3)
3Fully dissolving.
(3) filling of CNT
Get 500 μ L Fe (NO
3)
3Solution joins in 1000 μ L CNT-SDS solution, and it is muddy that settled solution becomes, and suspension occurs, adds 3200 μ L H again
2The O dilution.Then, mixed solution is used the power ultrasonic 0.5h of Ultrasonic Cell Disruptor with 300W in ice-water bath, obtain muddy suspension.With solution left standstill 15h, make that molecule fully adsorbs in the solution.Afterwards, the black precipitate of cleaning gained for several times.
(4) heat treatment
The composite that obtains is heated to 750 ℃ in inert atmosphere, decomposes Fe (NO
3)
3After obtain Fe
2O
3, the carbon nano-tube material of filling.
Use transmission electron microscope observing the present invention, (diameter about 3～4nm) is filled by comparatively continuous material can obviously to find out the double-walled carbon nano-tube of single existence.Carbon nano tube surface is wrapped up by foreign substance; The carbon pipe is also filled by foreign substance, and single-root carbon nano-tube obviously as can be seen.In addition, a port of this CNT is not blocked, and can infer that an other end is by opening.Adopt this kind method, external substance can enter the CNT depths, in addition from an end to an other end.CNT is filled discontinuously by foreign substance as can be seen.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting the scope of the present invention, so all equivalences of being done with described feature of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
Claims (7)
1. a preparation method who fills the CNT of metal oxide is characterized in that, this method comprises carbon nano tube surface modification operation, carbon nano-tube filled operation and heat treatment step;
Described carbon nano tube surface is modified operation:
Take by weighing CNT earlier and join in the sodium dodecyl benzene sulfonate aqueous solution, with ultrasonic under power 50W～300W, CNT is fully disperseed in solution with Ultrasonic Cell Disruptor;
Then, separate, remove sediment, make CNT-neopelex solution with the centrifugal speed of 3000r/min～20000r/min;
Described carbon nano-tube filled operation is:
Elder generation's preparing metal nitrate solution, getting the metal-nitrate solutions for preparing splashes in CNT-neopelex solution, use Ultrasonic Cell Disruptor ultrasonic again, obtain black precipitate behind static 10h～24h and be the CNT of having filled metal nitrate with power 50W～300W;
Described heat treatment step is:
The CNT of having filled metal nitrate is carried out high-temperature heat treatment in inert atmospheres such as nitrogen, argon gas, treatment temperature is 300～800 ℃.After decomposing, metal nitrate obtained filling the CNT of metal oxide.
2. the preparation method of the CNT of filling metal oxide according to claim 1 is characterized in that, described carbon nano tube surface is modified in the operation, and the mass concentration of sodium dodecyl benzene sulfonate aqueous solution is 2%～15%.
3. the preparation method of the CNT of filling metal oxide according to claim 1 is characterized in that, described carbon nano tube surface is modified in the operation, is 3～8 hours with ultrasonic time.
4. the preparation method of the CNT of filling metal oxide according to claim 1 is characterized in that, described carbon nano tube surface is modified in the operation, and the centrifugation time is 0.5～3 hour.
5. the preparation method of the CNT of filling metal oxide according to claim 1 is characterized in that, in the described carbon nano-tube filled operation, metal-nitrate solutions is that saturated concentration is 20%～100% metal-nitrate solutions.
6. the preparation method of the CNT of filling metal oxide according to claim 1 is characterized in that, in the described carbon nano-tube filled operation, ultrasonic time is 0.5h～5h.
7. the preparation method of the CNT of filling metal oxide according to claim 1 is characterized in that, in the described heat treatment step, heat treatment temperature is 300～800 ℃.
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Cited By (3)
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| CN103560018A (en) * | 2013-11-13 | 2014-02-05 | 北京化工大学 | Carbon nano-tube/ nickel oxide composite material and supercapacitor made of the material |
| CN109273726A (en) * | 2018-02-08 | 2019-01-25 | 成都理工大学 | A kind of carbon coated air electrode material and its preparation method and application |
| EP3395761A4 (en) * | 2015-12-17 | 2019-08-21 | Zeon Corporation | Fibrous carbon nanostructure dispersion |
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Cited By (5)
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| CN109273726A (en) * | 2018-02-08 | 2019-01-25 | 成都理工大学 | A kind of carbon coated air electrode material and its preparation method and application |
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Application publication date: 20110202 |