CN101499341A - Preparation of carbon nano-tube(MWCNTs)/manganese-zinc ferrite(Mn1-xZnxFe2O4) magnetic nano material by alcohol-thermal method - Google Patents
Preparation of carbon nano-tube(MWCNTs)/manganese-zinc ferrite(Mn1-xZnxFe2O4) magnetic nano material by alcohol-thermal method Download PDFInfo
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- CN101499341A CN101499341A CNA2008102021666A CN200810202166A CN101499341A CN 101499341 A CN101499341 A CN 101499341A CN A2008102021666 A CNA2008102021666 A CN A2008102021666A CN 200810202166 A CN200810202166 A CN 200810202166A CN 101499341 A CN101499341 A CN 101499341A
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Abstract
The invention relates to an alcohol-thermal method for preparing a carbon nano tube (MWCNTs)/ manganese-zinc ferrite (Mn1-xZnxFe2O4) magnetic nano-material. The method is mainly characterized in that the carbon nano tube, soluble malysite, zinc salt and manganese salt are taken as initial raw materials, and acid with strong oxidizing property is firstly used for acidizing the surface of the MWCNTs,; the acidized MWCNTs is dispersed into glycol solution, and then the malysite, the zinc salt, the manganese salt, anhydrous sodium acetate and dispersant polyethylene glycol are added in; and the lcohol-thermal method is adopted for preparing the (MWCNTs)/ Mn1-xZnxFe2O4 magnetic nano composite material. The prepared (MWCNTs)/ Mn1-xZnxFe2O4 magnetic nano composite material has pure crystalling phase, good dispersivity, high magnetization, strong magnetic induction sensitivity and simple preparing technique, and is not easy to agglomerate, thus being simple in the requirements for the production equipment and easy for commercial process.
Description
Technical field
The invention belongs to carbon nano-tube (MWCNTs)/manganese-zinc ferrite (Mn
1-xZn
xFe
2O
4) preparation field of magnetic nanometer composite material, particularly relate to pure hot legal system and be equipped with carbon nano-tube (MWCNTs)/manganese-zinc ferrite (Mn
1-xZn
xFe
2O
4) method of magnetic Nano material.
Background technology
Carbon nano-tube has performances such as particular structure, electricity, mechanics, Chu Qing because of it, extensive in many frontier application prospects such as nano electron device, superpower composite material, hydrogen storage material, catalyst carriers.Carbon nano-tube is a kind of monodimension nanometer material of hollow structure, has higher draw ratio, and the magnetic carbon-nano tube composite material of therefore assembling the 1-dimention nano level becomes one of research focus.Cao etc. are at Journal of Macromolecular Science, Part B:Physics, and 541,45, (2006) go up report by the synthetic Ni that makes of hydro-thermal
0.75Zn
0.25Fe
2O
4/ CNTs magnetic composite; Yu Huarong etc. are at Chinese Journal of Inorganic Chemistry, and 1651,21, [11], (2005) are gone up report and are adopted liquid-phase chemistry deposition technique to prepare Fe
2O
3/ CNTs composite material.This shows that carbon nano-tube magnetic nanometer composite material has a extensive future in industry and high-tech area because of the various performances of its uniqueness.Mn
1-xZn
xFe
2O
4It is a kind of important magnetic material.Mn
1-xZn
xFe
2O
4It is soft magnet material with spinel structure, it has higher magnetic permeability, higher magnetic saturation intensity, characteristics such as high resistivity, medium-high frequency loss, thereby be widely used in the signal transmission system of filter, wide-band transformer, various communication and transmission equipment, in this external biomaterial and the drug targeting material important application is arranged also.Fan etc. are at Journal of the European Ceramic Society, and 2743,20, (2000) are gone up report and are made the identical manganese-zinc ferrite (Mn of composition respectively with citrate gel method and traditional china-clay method
0.57Zn
0.35Fe
2.08O
4).People such as Darko are in Journal of the European Ceramic Society, 1945,21, (2001) go up the soluble-salt of reporting a certain proportion of iron, manganese, zinc and add the water mixing, the pH value of adjusting solution with NaOH is put into hydrothermal reaction kettle more than 10, reacts to make Mn
1-xZn
xFe
2O
4Makovec etc. are at Nanotechnology160, and 15, (2004) are gone up report and are prepared the manganese-zinc ferrite nano particle of particle diameter at 2～5nm by microemulsion method.Lai etc. are at Nanoscale Review Letter 40,2, and (2007) are gone up report and prepared the manganese-zinc ferrite nano particle by microwave method.This shows Mn
1-xZn
xFe
2O
4Because of its unique magnetic property, absorbing property, in industry, fields such as military affairs have a wide range of applications.Do not see at present and adopt pure hot legal system to be equipped with MWCNTs/Mn
1-xZn
xFe
2O
4The report of magnetic nanometer composite material.
Summary of the invention
Technical problem to be solved by this invention provides pure hot legal system and is equipped with carbon nano-tube (MWCNTs)/manganese-zinc ferrite (Mn
1-xZn
xFe
2O
4) method of (0＜x＜1) magnetic Nano material, the method process is simple, is easy to suitability for industrialized production.
The hot legal system of alcohol of the present invention is equipped with carbon nano-tube (MWCNTs)/manganese-zinc ferrite (Mn
1-xZn
xFe
2O
4) magnetic Nano material, comprising:
(1) MWCNTs acidification
The acid with strong oxidizing property adding is equipped with in the three-neck flask of MWCNTs, wherein the mass ratio of carbon nano-tube and acid with strong oxidizing property is 1:400～1:200, ultrasonic then dispersion 30～60min, be warming up to 100～120 ℃, acidification 18～30h, make carbon nano tube surface oxidized, and contain a large amount of electronegative groups;
(2) MWCNTs/Mn
1-xZn
xFe
2O
4The preparation of magnetic nanometer composite material
Under the room temperature, MWCNTs after the acidification is distributed in the ethylene glycol solution, ethylene glycol solution is 1/3～2/3 of a reactor volume, takes by weighing molysite, zinc salt, manganese salt then and comprises that iron, manganese, the chloride of zinc, nitrate, the sulfate of solubility are dissolved in the ethylene glycol solution, wherein Zn
2+And Mn
2+Mole ratio be 1:4～4:1; Zn
2+And Mn
2+Molal quantity sum and Fe
3+The ratio of molal quantity be 1:2, treat to dissolve fully the back and add polyethylene glycol (13000～20000), wherein the volume ratio of polyethylene glycol and ethylene glycol solution is 1:25-50, adds anhydrous sodium acetate again, wherein anhydrous sodium acetate and Fe
3+The ratio of molal quantity be 8:1～12:1, mechanical agitation 20～40min, mixing speed is 500～800 commentaries on classics/min, after treating to dissolve fully mixture is put into reactor, be warming up to 180～220 ℃, reaction 9～12h is cooled to room temperature, collect product with magnet, use deionized water wash again, oven dry.
The acid with strong oxidizing property of described step (1) is selected from one or both nitration mixture in red fuming nitric acid (RFNA), the concentrated sulfuric acid.
The acid with strong oxidizing property of described step (1) is a red fuming nitric acid (RFNA).
The amount that described step (2) adds ethylene glycol solution is 1/2～3/4 of a reactor volume.
The volume ratio of described step (2) ethylene glycol solution and acid with strong oxidizing property is 1:1.
The iron of described step (2), manganese, the chloride of zinc, nitrate, sulfate are respectively iron chloride FeCl
36H
2The sulfate MnSO of O, manganese
4H
2Nitrate Zn (the NO of O, zinc
3)
26H
2O.
Described step (2) Zn
2+And Mn
2+Molal quantity sum and Fe
3+The ratio of molal quantity be 1:2.
By regulating the ratio of molysite, zinc salt, manganese salt, can obtain the different MWCNTs/Mn that form
1-xZn
xFe
2O
4Magnetic nanometer composite material.
This method is solvent with ethylene glycol, and ethylene glycol is as a kind of strong reducible agent and have higher boiling point, and with respect to common liquid phase method, magnetic Nano microsphere is more stable in organic facies, is difficult for generating the impurity phase.In addition, because in liquid phase, magnetic nano-particle is very easily reunited because of the effect that is subjected to the strong electrostatic attraction of solion, so this method selects electrostatic stabilization for use good anhydrous sodium acetate adds as alkaline reagent, to prevent Mn
1-xZn
xFe
2O
4Extensive reunion.
Beneficial effect
(1) prepared MWCNTs/Mn
1-xZn
xFe
2O
4The magnetic nanometer composite material crystalline phase is pure, good dispersion, be difficult for to reunite, and magnetization height and magnetic induction sensitivity are very strong;
(2) preparation technology is simple, and production equipment is required simply to be easy to suitability for industrialized production.
Description of drawings
Fig. 1 .MWCNTs/Mn
1-xZn
xFe
2O
4The magnetic nanometer composite material stereoscan photograph;
Fig. 2 .MWCNTs/Mn
1-xZn
xFe
2O
4The transmission electron microscope photo of magnetic nanometer composite material;
Fig. 3 .MWCNTs/Mn
1-xZn
xFe
2O
4The X-ray diffractogram of magnetic nanometer composite material;
Fig. 4 .MWCNTs/Mn
1-xZn
xFe
2O
4The magnetic hysteresis loop figure of magnetic nanometer composite material, lower right corner illustration is MWCNTs/Mn
1-xZn
xFe
2O
4Nano composite material magnetism testing photo.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are used to illustrate the present invention, limit the scope of the invention and be not used in.Should be understood that in addition those skilled in the art can make various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Take by weighing 0.15g MWCNTs and add three-neck flask, add 50ml (18mol/L) red fuming nitric acid (RFNA) again, ultrasonic dispersion 40min is warming up to 100 ℃, acidification reaction 24h then.Reaction finishes the back carbon pipe suspension is carried out suction filtration, washing, drying, obtains the MWCNTs after the acidification.Take by weighing the high iron chloride of 1.351g, 0.1487g zinc nitrate hexahydrate, 0.338g manganese sulfate monohydrate then, add three-neck flask, add 50ml ethylene glycol again, add the MWCNTs of above-mentioned acidifying, ultrasonic dispersion 45min again.After treating that ultrasonic dispersion finishes, add 3.6g anhydrous sodium acetate, 1.2ml Macrogol 200 again, be 500 rev/mins of following mechanical agitation 30min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 200 ℃, reaction 10h at revolution.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 45 ℃ of following vacuumize 24h, obtain MWCNTs/Mn
1-xZn
xFe
2O
4Nano composite material.Fig. 3 is the synthetic magnetic Nano microsphere X-ray diffractogram of present embodiment, and the diffraction maximum among the figure shows: this nano composite material is MWCNTs/Mn
1-xZn
xFe
2O
4As seen from Figure 1: a large amount of Mn are arranged
1-xZn
xFe
2O
4Nano microsphere is coated on the carbon nano-tube, and microspherulite diameter is at 50～150nm.As seen from Figure 2: Mn
1-xZn
xFe
2O
4Nano microsphere is that a plurality of Mn are arranged
1-xZn
xFe
2O
4The directed gathering of nanocrystal forms, and is coated on the carbon nano-tube.The magnetization by this nano composite material of Fig. 4 is higher, and magnetic induction sensitivity is very strong.
Embodiment 2
Take by weighing 0.1g MWCNTs and add three-neck flask, add 60ml (15mol/L) red fuming nitric acid (RFNA) again, ultrasonic dispersion 20min is warming up to 120 ℃, acidification reaction 30h then.Reaction finishes the back carbon pipe suspension is carried out suction filtration, washing, drying, obtains the MWCNTs after the acidification.Take by weighing the high iron chloride of 1.486g, 0.655g zinc nitrate hexahydrate, 0.093g manganese sulfate monohydrate then, add three-neck flask, add 50ml ethylene glycol again, add the MWCNTs of above-mentioned acidifying, ultrasonic dispersion 45min again.After treating ultrasonic dispersion, add 4.42g anhydrous sodium acetate, 1ml Macrogol 200 again, be 700 rev/mins of following mechanical agitation 20min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 190 ℃, reaction 11h at revolution.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 60 ℃ of following vacuumize 18h, obtain MWCNTs/Mn
1-xZn
xFe
2O
4Nano composite material.The XRD test result shows: this nano composite material is MWCNTs/Mn
1-xZn
xFe
2O
4Scanning electron microscopic observation shows: a large amount of Mn are arranged
1-xZn
xFe
2O
4Nano microsphere is coated on the carbon nano-tube, and microspherulite diameter is at 50～150nm.Transmission electron microscope photo is observed and is shown: the Mn in this nano composite material
1-xZn
xFe
2O
4Nano microsphere is that a plurality of Mn are arranged
1-xZn
xFe
2O
4The directed gathering of nanocrystal forms, and is coated on the carbon nano-tube.The magnetic hysteresis loop figure and the magnetism testing photo of this magnetic nanometer composite material show: the magnetization of this nano composite material is higher, and magnetic induction sensitivity is very strong.
Embodiment 3
Take by weighing 0.12g MWCNTs and add three-neck flask, add 45ml (16mol/L) red fuming nitric acid (RFNA) again, ultrasonic dispersion 25min is warming up to 120 ℃, acidification reaction 24h then.Reaction finishes the back carbon pipe suspension is carried out suction filtration, washing, drying, obtains the MWCNTs after the acidification.Take by weighing the high iron chloride of 1.486g, 0.491g zinc nitrate hexahydrate, 0.186g manganese sulfate monohydrate then, add three-neck flask, add 50ml ethylene glycol again, add the MWCNTs of above-mentioned acidifying, ultrasonic dispersion 50min again.After treating ultrasonic dispersion, add 4.62g anhydrous sodium acetate, 1.1ml Macrogol 200 again, be 600 rev/mins of following mechanical agitation 40min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 210 ℃, reaction 9h at revolution.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 55 ℃ of following vacuumize 24h, obtain MWCNTs/Mn
1-xZn
xFe
2O
4Nano composite material.The XRD test result shows: this nano composite material is MWCNTs/Mn
1-xZn
xFe
2O
4Scanning electron microscopic observation shows: a large amount of Mn are arranged
1-xZn
xFe
2O
4Nano microsphere is coated on the carbon nano-tube, and microspherulite diameter is at 50～150nm.Transmission electron microscope photo is observed and is shown: the Mn in this nano composite material
1-xZn
xFe
2O
4Nano microsphere is that a plurality of Mn are arranged
1-xZn
xFe
2O
4The directed gathering of nanocrystal forms, and is coated on the carbon nano-tube.The magnetic hysteresis loop figure and the magnetism testing photo of this magnetic nanometer composite material show: the magnetization of this nano composite material is higher, and magnetic induction sensitivity is very strong.
Embodiment 4
Take by weighing 0.13g MWCNTs and add three-neck flask, add 55ml (20mol/L) red fuming nitric acid (RFNA) again, ultrasonic dispersion 30min is warming up to 120 ℃, acidification reaction 18h then.Reaction finishes the back carbon pipe suspension is carried out suction filtration, washing, drying, obtains the MWCNTs after the acidification.Take by weighing the high iron chloride of 1.486g, 0.233g zinc nitrate hexahydrate, 0.411g manganese sulfate monohydrate then, add three-neck flask, add 50ml ethylene glycol again, add the MWCNTs of above-mentioned acidifying, ultrasonic dispersion 45min again.After treating ultrasonic dispersion, add 4.95g anhydrous sodium acetate, 1.2ml Macrogol 200 again, be 800 rev/mins of following mechanical agitation 30min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 220 ℃, reaction 8h at revolution.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 60 ℃ of following vacuumize 24h, obtain MWCNTs/Mn
1-xZn
xFe
2O
4Nano composite material.The XRD test result shows: this nano composite material is MWCNTs/Mn
1-xZn
xFe
2O
4Scanning electron microscopic observation shows: a large amount of Mn are arranged
1-xZn
xFe
2O
4Nano microsphere is coated on the carbon nano-tube, and microspherulite diameter is at 50～150nm.Transmission electron microscope photo is observed and is shown: the Mn in this nano composite material
1-xZn
xFe
2O
4Nano microsphere is that a plurality of Mn are arranged
1-xZn
xFe
2O
4The directed gathering of nanocrystal forms, and is coated on the carbon nano-tube.The magnetic hysteresis loop figure and the magnetism testing photo of this magnetic nanometer composite material show: the magnetization of this nano composite material is higher, and magnetic induction sensitivity is very strong.
Claims (8)
1. pure hot legal system is equipped with carbon nano-tube MWCNTs/ manganese-zinc ferrite Mn
1-xZn
xFe
2O
4Magnetic Nano material comprises:
(1) MWCNTs acidification
The acid with strong oxidizing property adding is equipped with in the three-neck flask of MWCNTs, and wherein the mass ratio of carbon nano-tube and acid with strong oxidizing property is 1:400～1:200, and ultrasonic then dispersion 30～60min is warming up to 100～120 ℃, acidification 18～30h;
(2) MWCNTs/Mn
1-xZn
xFe
2O
4The preparation of magnetic nanometer composite material
Under the room temperature, MWCNTs after the acidification is distributed in the ethylene glycol solution that concentration is 98～99.5wt%, the volume of ethylene glycol solution is 1/3～2/3 of a reactor volume, take by weighing molysite, zinc salt, manganese salt then and comprise that iron, manganese, the chloride of zinc, nitrate, the sulfate of solubility are dissolved in the ethylene glycol solution, wherein Zn
2+And Mn
2+Mole ratio be 1:4～4:1; Zn
2+And Mn
2+Molal quantity sum and Fe
3+The ratio of molal quantity be 1:2, treat to dissolve fully the back and add polyethylene glycol (13000～20000), wherein the volume ratio of polyethylene glycol and ethylene glycol solution is 1:25-50, adds anhydrous sodium acetate again, wherein anhydrous sodium acetate and Fe
3+The ratio of molal quantity be 8:1～12:1, mechanical agitation 20～40min, mixing speed is 500～800 commentaries on classics/min, after treating to dissolve fully mixture is put into reactor, be warming up to 180～220 ℃, reaction 9～12h is cooled to room temperature, collect product with magnet, use deionized water wash again, oven dry.
2. the hot legal system of alcohol according to claim 1 is equipped with carbon nano-tube MWCNTs/ manganese-zinc ferrite Mn
1-xZn
xFe
2O
4Magnetic Nano material is characterized in that: the acid with strong oxidizing property of described step (1) is selected from one or both nitration mixture in red fuming nitric acid (RFNA), the concentrated sulfuric acid.
3. the hot legal system of alcohol according to claim 1 is equipped with carbon nano-tube MWCNTs/ manganese-zinc ferrite Mn
1-xZn
xFe
2O
4Magnetic Nano material is characterized in that: the acid with strong oxidizing property of described step (1) is a red fuming nitric acid (RFNA).
4. the hot legal system of alcohol according to claim 1 is equipped with carbon nano-tube MWCNTs/ manganese-zinc ferrite Mn
1-xZn
xFe
2O
4Magnetic Nano material is characterized in that: the amount that described step (2) adds ethylene glycol solution is 1/2～3/4 of a reactor volume.
5. the hot legal system of alcohol according to claim 1 is equipped with carbon nano-tube MWCNTs/ manganese-zinc ferrite Mn
1-xZn
xFe
2O
4Magnetic Nano material is characterized in that: the volume ratio of described step (2) ethylene glycol solution and acid with strong oxidizing property is 1:1.
6. the hot legal system of alcohol according to claim 1 is equipped with carbon nano-tube MWCNTs/ manganese-zinc ferrite Mn
1-xZn
xFe
2O
4Magnetic Nano material is characterized in that: the iron of described step (2), manganese, the chloride of zinc, nitrate, sulfate are respectively iron chloride FeCl
36H
2The sulfate MnSO of O, manganese
4H
2Nitrate Zn (the NO of O, zinc
3)
26H
2O.
7. the hot legal system of alcohol according to claim 1 is equipped with carbon nano-tube MWCNTs/ manganese-zinc ferrite Mn
1-xZn
xFe
2O
4Magnetic Nano material is characterized in that: described step (2) Zn
2+And Mn
2+Molal quantity sum and Fe
3+The ratio of molal quantity be 1:2.
8. the hot legal system of alcohol according to claim 1 is equipped with carbon nano-tube MWCNTs/ manganese-zinc ferrite Mn
1-xZn
xFe
2O
4Magnetic Nano material is characterized in that: by regulating the ratio of molysite, zinc salt, manganese salt, can obtain the different MWCNTs/Mn that form
1-xZn
xFe
2O
4Magnetic nanometer composite material.
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| CN101800105A (en) * | 2010-03-25 | 2010-08-11 | 东华大学 | Method for preparing MWCNTs/Co1-xZnxFe2O4 magnetic nanocomposite material |
| CN102205238A (en) * | 2011-04-11 | 2011-10-05 | 东华大学 | Method for preparing MWCNTs/ZnO (multi-wall carbon nano tubes/zinc oxide) nanometer composite material |
| CN102391830A (en) * | 2011-08-09 | 2012-03-28 | 中国科学院宁波材料技术与工程研究所 | Application of ferrite-carbon nano-tube composite material used as wave-absorbing material at low temperature |
| CN103613374A (en) * | 2013-11-26 | 2014-03-05 | 彭晓领 | Cobalt ferrite @ carbon nano tube composite material and preparation method thereof |
| CN103834361A (en) * | 2014-02-20 | 2014-06-04 | 钟春燕 | Carbon nanometer fiber/ferrite composite absorbing material and preparation method thereof |
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| CN105601263A (en) * | 2015-12-23 | 2016-05-25 | 苏州冠达磁业有限公司 | High-performance power soft-magnetic Mn-Zn ferrite material and preparation method thereof |
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| CN102205238A (en) * | 2011-04-11 | 2011-10-05 | 东华大学 | Method for preparing MWCNTs/ZnO (multi-wall carbon nano tubes/zinc oxide) nanometer composite material |
| CN102391830A (en) * | 2011-08-09 | 2012-03-28 | 中国科学院宁波材料技术与工程研究所 | Application of ferrite-carbon nano-tube composite material used as wave-absorbing material at low temperature |
| CN102391830B (en) * | 2011-08-09 | 2014-01-29 | 中国科学院宁波材料技术与工程研究所 | Application of ferrite-carbon nano-tube composite material used as wave-absorbing material at low temperature |
| CN103613374A (en) * | 2013-11-26 | 2014-03-05 | 彭晓领 | Cobalt ferrite @ carbon nano tube composite material and preparation method thereof |
| CN103613374B (en) * | 2013-11-26 | 2015-07-08 | 中国计量学院 | Cobalt ferrite @ carbon nano tube composite material and preparation method thereof |
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| CN103834361B (en) * | 2014-02-20 | 2016-03-23 | 钟春燕 | A kind of carbon nanofiber/ferrite composite wave-suction material and preparation method thereof |
| CN103834361A (en) * | 2014-02-20 | 2014-06-04 | 钟春燕 | Carbon nanometer fiber/ferrite composite absorbing material and preparation method thereof |
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| US11824189B2 (en) | 2018-01-09 | 2023-11-21 | South Dakota Board Of Regents | Layered high capacity electrodes |
| CN114524461A (en) * | 2022-01-10 | 2022-05-24 | 闽都创新实验室 | Manganese-zinc ferrite compound and preparation method and application thereof |
| CN114933297A (en) * | 2022-06-14 | 2022-08-23 | 河南农业大学 | Preparation method of nanocrystalline/carbon nano tube composite super microsphere |
| CN114933297B (en) * | 2022-06-14 | 2023-08-18 | 河南农业大学 | Preparation method of nanocrystalline/carbon nanotube composite super microsphere |
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