CN102583315A - Method for preparing ferroferric oxide/ carbon nano tube composite material - Google Patents
Method for preparing ferroferric oxide/ carbon nano tube composite material Download PDFInfo
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- CN102583315A CN102583315A CN2012100343750A CN201210034375A CN102583315A CN 102583315 A CN102583315 A CN 102583315A CN 2012100343750 A CN2012100343750 A CN 2012100343750A CN 201210034375 A CN201210034375 A CN 201210034375A CN 102583315 A CN102583315 A CN 102583315A
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Abstract
The invention discloses a method for preparing a ferroferric oxide/ carbon nano tube composite material, which is used for solving the technical problem that the nano Fe3O4 particle diameter of the coating prepared by the conventional method for preparing the ferroferric oxide/ carbon nano tube composite material is not uniform. According to the technical scheme, multi-wall carbon nano tubes, ammonium ferrous sulfate, ferric chloride and sodium hydroxide are used as raw materials, polyvinyl alcohol is used as a surfactant, the ferroferric oxide/ carbon nano tube magnetic nano composite material is obtained by adopting a reverse co-precipitation method, and nano Fe3O4 coatings with different particle diameters are obtained by changing the reaction temperature and the concentration of the reaction solution. The nano Fe3O4 particle diameter of the coating of the ferroferric oxide/ carbon nano tube composite material prepared by the method is uniform, the average nano particle diameter is less than 10 nanometers, and the synthesis process and the production equipment are simple.
Description
Technical field
The present invention relates to a kind of preparation method of matrix material, particularly relate to a kind of preparation method of Z 250/carbon nano tube compound material.
Background technology
Carbon nanotube is widely used in numerous areas such as hydrogen storage material, electrode materials, support of the catalyst and matrix material because of it has particular structure and excellent electricity, mechanics and hydrogen storage property.In one, the new features that produced make it receive much concern as a kind of special functional materials to magnetic Nano material with the advantages of nano material and magneticsubstance.Use the magnetic Nano material enveloped carbon nanometer tube, can show more excellent electrically, magnetic and microwave absorbing property, become one of focus that this area research person pays close attention to, have broad application prospects in industry and high-tech area.
Preparing Z 250/carbon nano-tube magnetic nanometer composite material adopts more method that hydrothermal method, polyvalent alcohol method, solvent-thermal method and chemical coprecipitation etc. are arranged.
Document 1 " Xuzhen Wang, Zongbin Zhao, Jiangying Qu, Zhiyu Wang, Jieshan Qiu, Fabrication and characterization of magnetic Fe
3O
4-CNT composites; Journal of Physics and Chemistry of Solids.71 (2010) 673-676 " the hot method of a kind of employing situ solvent disclosed; and ferrocene is made presoma, and benzene is made solvent, 500 ℃ of methods that prepare Z 250/carbon nanotube; the median size that obtains magnetic nanoparticle on the carbon nanotube is 14nm, and the saturation magnetization of its magnetic composite is 32.5emug
-1, coercive force is 110Oe, has good magnetic.
Document 2 " Yang He, Ling Huang, Jinshu Cai, Xiaomei Zheng, Shigang Sun, Structure and electrochemical performance of nanostructured Fe
3O
4/ carbon nanotube composites as anodes for lithium ion batteries; Electrochimica Acta.55 (2010) 1140-1144 " a kind of method that adopts the forward coprecipitation method to prepare Z 250/carbon nanotube disclosed; and the particle diameter of magnetic nanoparticle is 10-25nm on the carbon nanotube of preparation, and test result shows that magnetic composite has excellent chemical property as lithium ion battery.
Yet, preparing in Z 250/carbon nanotube magnetic composite material method commonly used, solvent-thermal method and hydrothermal method need autoclave; Reaction requires temperature higher; Raw material is simple though the polyvalent alcohol method needs, experimentation is prone to control, compares with chemical coprecipitation, and reaction requires temperature high.Chemical coprecipitation is simple because of its experiment condition, and process is prone to control, and is with low cost and be widely used.But the general chemical coprecipitation that adopts is the forward coprecipitation method normally, and there is the dimensional homogeneity control difficult problem of carbon nanotube coating layer nano particle in its method.
Summary of the invention
In order to overcome the coating layer nanometer Fe of existing Z 250/carbon nano tube compound material preparation method preparation
3O
4The uneven deficiency of particle diameter, the present invention provides a kind of preparation method of Z 250/carbon nano tube compound material.This method is a raw material with multi-walled carbon nano-tubes, ferrous ammonium sulphate, iron(ic)chloride and sodium hydroxide; Z 150PH is as tensio-active agent; Adopt reverse coprecipitation method to obtain Z 250/carbon nano-tube magnetic nanometer composite material; Through changing the concentration of temperature of reaction and reaction soln, can obtain the nanometer Fe of different-grain diameter size
3O
4Coating layer.The coating layer nanometer Fe of the Z 250/carbon nano tube compound material of this method preparation
3O
4Particle diameter is even, and synthesis technique and production unit are simple.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of Z 250/carbon nano tube compound material is characterized in may further comprise the steps:
(1) carbon nanotube is joined in the polyvinyl alcohol solution according to mass ratio 0.31～1.02, carry out ultrasonic and dispersed with stirring, obtain the aaerosol solution of carbon nanotube;
(2) divalent iron salt and trivalent iron salt are used the zero(ppm) water wiring solution-forming respectively, divalent iron salt and trivalent iron salt mol ratio are 1: 1.7～2, and it is added in the suspension-s of step (1) preparation, obtain containing the mixed solution of divalent iron salt, trivalent iron salt and carbon nanotube;
(3) mixed solution with step (2) carries out ultra-sonic dispersion;
(4) sodium hydroxide is used the zero(ppm) water wiring solution-forming; Sodium hydroxide and divalent iron salt mol ratio are 8～12: 1; To mix with the solution that contains sodium hydroxide through the mixing drop behind step (3) ultra-sonic dispersion; Logical nitrogen protection in the mixing process, induction stirring under 50～80 ℃ of reaction conditionss, ageing of solution after reaction is accomplished;
(5) solution after step (4) ageing filters under the magnet effect, is precipitated to neutrality with zero(ppm) water and absolute ethanol washing, obtains nano ferriferrous oxide coated carbon nanotube magnetic composite through vacuum-drying;
(6) product that step (5) is obtained is heated to 280～300 ℃, N with the speed of 1～2 ℃/min
21～2h is preserved in protection down makes product stable, and the speed with 3～5 ℃/min continues to be heated to 480～520 ℃ again, at N
2Atmosphere is preserved 3～5h and is made Fe
3O
4Crystallization and Z 150PH carbonization.
Said carbon nanotube is the multi-walled carbon nano-tubes that contains carboxyl functional group.
Said divalent iron salt is FeCl
2Or (NH
4)
2Fe (SO
4)
2Any.
Said trivalent iron salt is FeCl
3
The invention has the beneficial effects as follows: owing to be raw material with multi-walled carbon nano-tubes, ferrous ammonium sulphate, iron(ic)chloride and sodium hydroxide; Z 150PH is as tensio-active agent; Adopt reverse coprecipitation method to obtain Z 250/carbon nano-tube magnetic nanometer composite material; Through changing the concentration of temperature of reaction and reaction soln, obtained the nanometer Fe of different-grain diameter size
3O
4Coating layer.The coating layer nanometer Fe of the Z 250/carbon nano tube compound material of this method preparation
3O
4Particle diameter is even, and the nano particle median size is less than 10nm, and synthesis technique and production unit are simple.
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
Description of drawings
Fig. 1 is the XRD figure of the prepared Z 250/carbon nano tube compound material of the embodiment of the invention 1.
Fig. 2 is the TEM figure of the prepared Z 250/carbon nano tube compound material of the embodiment of the invention 1.
Fig. 3 is a nanometer Fe in Z 250/carbon nano tube compound material
3O
4Particulate TEM figure, Fig. 3 (a) is the background technology methods and results, Fig. 3 (b) is the result of the inventive method embodiment 1.
Fig. 4 is the magnetism testing photo of the prepared Z 250/carbon nano tube compound material of the embodiment of the invention 1.
Embodiment
Embodiment 1: the 122.1mg carbon nanotube is added in the polyvinyl alcohol solution (mass ratio of carbon nanotube and polyvinyl alcohol solution is 0.31), carry out ultrasonic and dispersed with stirring, obtain the aaerosol solution of carbon nanotube.
With divalent iron salt FeCl
2With trivalent iron salt FeCl
3Use the zero(ppm) water wiring solution-forming respectively, divalent iron salt FeCl
2With trivalent iron salt FeCl
3Mol ratio is 1: 2, and it is added in the suspension-s of carbon nanotube and Z 150PH, obtains containing divalent iron salt FeCl
2, trivalent iron salt FeCl
3With the mixed solution of carbon nanotube, ultra-sonic dispersion.
Sodium hydroxide is used the zero(ppm) water wiring solution-forming, sodium hydroxide and divalent iron salt FeCl
2Mol ratio is 8: 1, will contain divalent iron salt FeCl
2, trivalent iron salt FeCl
3Mix with the solution that contains sodium hydroxide with the mixing drop of carbon nanotube; Logical nitrogen protection in the mixing process; Induction stirring under 50 ℃ of reaction conditionss, the reaction 40min after solution through ageing, filtration washing under the magnet effect; Be precipitated to neutrality with zero(ppm) water and absolute ethanol washing, obtain nano ferriferrous oxide coated carbon nanotube magnetic composite through vacuum-drying.
Products therefrom is heated to 280 ℃, N with the speed of 1 ℃/min
22h is preserved in protection down makes product stable, and the speed with 3 ℃/min continues to be heated to 480 ℃ at N again
2Atmosphere is preserved 5h, makes Fe
3O
4Crystallization and Z 150PH carbonization.
After tested, utilize the Scherrer formula to calculate the nano ferriferrous oxide average grain diameter that coats on the CNT and be 8.9nm.
From the XRD figure of Fig. 1 Z 250/carbon nano tube compound material, can see the diffraction peak of Z 250 and carbon nanotube, show that this matrix material is Z 250/carbon nano tube compound material.
Can find out from the TEM photo of Fig. 2 Z 250/carbon nano tube compound material: a large amount of nanometer Fe
3O
4Particle evenly is coated on the carbon nanotube, and the nanoparticle size evenly.
From Fig. 3 (b) nanometer Fe
3O
4The TEM photo of particle can be found out, compares the nanometer Fe of embodiment 1 preparation with Fig. 3 (a)
3O
4Particle diameter is littler, and size is more even.
Can find out from the magnetism testing photo of Fig. 4 Z 250/carbon nano tube compound material; In the extremely short time; Turbid solution in Fig. 4 (a) beaker promptly can present the phenomenon among Fig. 4 (b); Magnetic composite is fully by the sidewall of attraction to beaker, and the magnetic induction sensitivity of the Z 250/carbon nano tube compound material of illustrative embodiment 1 preparation is very strong.
Embodiment 2: the 257.8mg carbon nanotube is added in the polyvinyl alcohol solution (mass ratio of carbon nanotube and polyvinyl alcohol solution is 0.64), carry out ultrasonic and dispersed with stirring, obtain the aaerosol solution of carbon nanotube.
With divalent iron salt (NH
4)
2Fe (SO
4)
2With trivalent iron salt FeCl
3Use the zero(ppm) water wiring solution-forming respectively, divalent iron salt (NH
4)
2Fe (SO
4)
2With trivalent iron salt FeCl
3Mol ratio is 1: 1.85, and it is added in the suspension-s of carbon nanotube and Z 150PH, obtains containing divalent iron salt (NH
4)
2Fe (SO
4)
2, trivalent iron salt FeCl
3With the mixed solution of carbon nanotube, ultra-sonic dispersion.
Sodium hydroxide is used the zero(ppm) water wiring solution-forming, sodium hydroxide and divalent iron salt (NH
4)
2Fe (SO
4)
2Mol ratio is 10: 1, will contain divalent iron salt (NH
4)
2Fe (SO
4)
2, trivalent iron salt FeCl
3Mix with the solution that contains sodium hydroxide with the mixing drop of carbon nanotube; Logical nitrogen protection in the mixing process; Induction stirring under 65 ℃ of reaction conditionss, the reaction 30min after solution through ageing, filtration washing under the magnet effect; Be precipitated to neutrality with zero(ppm) water and absolute ethanol washing, obtain nano ferriferrous oxide coated carbon nanotube magnetic composite through vacuum-drying.
Products therefrom is heated to 290 ℃, N with the speed of 1.5 ℃/min
21.5h is preserved in protection down makes product stable, and the speed with 4 ℃/min continues to be heated to 500 ℃ at N again
2Atmosphere is preserved 4h, makes Fe
3O
4Crystallization and Z 150PH carbonization.
After tested, utilize the Scherrer formula to calculate the nano ferriferrous oxide average grain diameter that coats on the CNT and be 9.3nm.
Embodiment 3: the 409.4mg carbon nanotube is added in the polyvinyl alcohol solution (mass ratio of carbon nanotube and polyvinyl alcohol solution is 1.02), carry out ultrasonic and dispersed with stirring, obtain the aaerosol solution of carbon nanotube.
With divalent iron salt FeCl
2With trivalent iron salt FeCl
3Use the zero(ppm) water wiring solution-forming respectively, divalent iron salt FeCl
2With trivalent iron salt FeCl
3Mol ratio is 1: 1.7, and it is added in the suspension-s of carbon nanotube and Z 150PH, obtains containing divalent iron salt FeCl
2, trivalent iron salt FeCl
3With the mixed solution of carbon nanotube, ultra-sonic dispersion.
Sodium hydroxide is used the zero(ppm) water wiring solution-forming, sodium hydroxide and divalent iron salt FeCl
2Mol ratio is 12: 1, will contain divalent iron salt FeCl
2, trivalent iron salt FeCl
3Mix with the solution that contains sodium hydroxide with the mixing drop of carbon nanotube; Logical nitrogen protection in the mixing process; Induction stirring under 80 ℃ of reaction conditionss, the reaction 20min after solution through ageing, filtration washing under the magnet effect; Be precipitated to neutrality with zero(ppm) water and absolute ethanol washing, obtain nano ferriferrous oxide coated carbon nanotube magnetic composite through vacuum-drying.
Products therefrom is heated to 300 ℃, N with the speed of 2 ℃/min
21h is preserved in protection down makes product stable, and the speed with 5 ℃/min continues to be heated to 520 ℃ at N again
2Atmosphere is preserved 3h, makes Fe
3O
4Crystallization and Z 150PH carbonization.
After tested, utilize the Scherrer formula to calculate the nano ferriferrous oxide average grain diameter that coats on the CNT and be 9.7nm.
Embodiment 1～3 used carbon nanotube is the multi-walled carbon nano-tubes that contains carboxyl functional group.
Claims (4)
1. the preparation method of a Z 250/carbon nano tube compound material is characterized in that may further comprise the steps:
(1) carbon nanotube is joined in the polyvinyl alcohol solution according to mass ratio 0.31～1.02, carry out ultrasonic and dispersed with stirring, obtain the aaerosol solution of carbon nanotube;
(2) divalent iron salt and trivalent iron salt are used the zero(ppm) water wiring solution-forming respectively, divalent iron salt and trivalent iron salt mol ratio are 1: 1.7～2, and it is added in the suspension-s of step (1) preparation, obtain containing the mixed solution of divalent iron salt, trivalent iron salt and carbon nanotube;
(3) mixed solution with step (2) carries out ultra-sonic dispersion;
(4) sodium hydroxide is used the zero(ppm) water wiring solution-forming; Sodium hydroxide and divalent iron salt mol ratio are 8～12: 1; To mix with the solution that contains sodium hydroxide through the mixing drop behind step (3) ultra-sonic dispersion; Logical nitrogen protection in the mixing process, induction stirring under 50～80 ℃ of reaction conditionss, ageing of solution after reaction is accomplished;
(5) solution after step (4) ageing filters under the magnet effect, is precipitated to neutrality with zero(ppm) water and absolute ethanol washing, obtains nano ferriferrous oxide coated carbon nanotube magnetic composite through vacuum-drying;
(6) product that step (5) is obtained is heated to 280～300 ℃, N with the speed of 1～2 ℃/min
21～2h is preserved in protection down makes product stable, and the speed with 3～5 ℃/min continues to be heated to 480～520 ℃ again, at N
2Atmosphere is preserved 3～5h and is made Fe
3O
4Crystallization and Z 150PH carbonization.
2. the preparation method of Z 250/carbon nano tube compound material according to claim 1, it is characterized in that: said carbon nanotube is the multi-walled carbon nano-tubes that contains carboxyl functional group.
3. the preparation method of Z 250/carbon nano tube compound material according to claim 1, it is characterized in that: said divalent iron salt is FeCl
2Or (NH
4)
2Fe (SO
4)
2Any.
4. the preparation method of Z 250/carbon nano tube compound material according to claim 1, it is characterized in that: said trivalent iron salt is FeCl
3
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| CN103007887A (en) * | 2013-01-08 | 2013-04-03 | 长沙矿冶研究院有限责任公司 | Carbon-nanotube-loaded multi-stage nanometer ferroferric oxide adsorbent and preparation method and application thereof |
| CN103157438A (en) * | 2013-04-10 | 2013-06-19 | 哈尔滨工业大学 | Preparation method of carbon microsphere/nanometer iron oxide magnetic composite material |
| CN103346291A (en) * | 2013-07-10 | 2013-10-09 | 肖辉 | Carbon nano-paper-based in-situ loaded ferroferric oxide lithium-ion battery negative electrode and preparation method thereof |
| CN103559970A (en) * | 2013-10-11 | 2014-02-05 | 苏州英芮诚生化科技有限公司 | Superparamagnetism nanocomposite material with carbon nano tubes coated with metallic oxide crystals, preparation method and application |
| CN103825019A (en) * | 2014-02-21 | 2014-05-28 | 浙江大学 | Fe3O4/C composite material, its preparation method and its application in lithium ion battery |
| CN105036115A (en) * | 2015-07-29 | 2015-11-11 | 桂林电子科技大学 | Carbon nanotube uniformly and stably loaded with iron-containing nano particles and preparation method of carbon nanotube |
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