CN102091627B - Method for preparing CNT/Fe3O4@ZnO one-dimensional nanocomposite by polyol one-pot method - Google Patents
Method for preparing CNT/Fe3O4@ZnO one-dimensional nanocomposite by polyol one-pot method Download PDFInfo
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- CN102091627B CN102091627B CN201010563497XA CN201010563497A CN102091627B CN 102091627 B CN102091627 B CN 102091627B CN 201010563497X A CN201010563497X A CN 201010563497XA CN 201010563497 A CN201010563497 A CN 201010563497A CN 102091627 B CN102091627 B CN 102091627B
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Abstract
The invention relates to a method for preparing a CNT/Fe3O4@ZnO one-dimensional nanocomposite by a polyol one-pot method. The method comprises the following steps: 1, weighing and then mixing a multiwall nanotube, ferric acetylacetonate and triethylene glycol, then carrying out ultrasonic dispersion on the mixture until the mixture is uniform, then introducing argon, then heating the mixture to the boiling point of triethylene glycol and then carrying out reflux; and 2, then cooling the product to the room temperature, then throwing zinc acetate, then slowing heating the mixture to the boiling point of triethylene glycol, then carrying out reflux, carrying out magnetic separation after cooling, washing the product with ethanol and drying the product to obtain the CNT/Fe3O4@ZnO composite. The composite is applied in the fields of photoelectric device assembly and photocatalysis.
Description
Technical field
The present invention relates to a kind of CNT/Fe
3O
4The preparation method of ZnO one-dimensional nano-composite material.
Background technology
CNT (CNT) has characteristic and one-dimensional nano structures such as good mechanics, calorifics, electricity, has broad application prospects at nano electron device, reinforced composite, hydrogen storage material, bio-medical, catalytic field.Ferriferrous oxide nano-particle has excellent magnetism ability and excellent biological compatibility, can be used for fields such as magnetic fluid, target administration, cancer thermotherapy, magnetic resonance imaging, magnetic recovery carrier.At present, there is the researcher on CNT, to assemble Fe
3O
4Nano particle is given CNT good magnetic responsiveness, and it is prepared into magnetic flow liquid, electrode material, target medicine carrier etc.
Existing CNT/Fe
3O
4Exist only to have magnetic, do not have optical characteristics such as photocatalysis.
Summary of the invention
The present invention will provide the polyalcohol one kettle way to prepare CNT/Fe
3O
4The method of ZnO one-dimensional nano-composite material; (give monodimension nanometer material magnetic and optics double function characteristic simultaneously.
The polyalcohol one kettle way prepares CNT/Fe
3O
4The method of ZnO one-dimensional nano-composite material is characterized in that the polyalcohol one kettle way prepares CNT/Fe
3O
4The method of ZnO one-dimensional nano-composite material is undertaken by following step: one, take by weighing 100mg multi-walled carbon nano-tubes (one dimension matrix), 100～400mg ferric acetyl acetonade (presoma) and 25ml triethylene glycol (solvent) back and mix; Ultrasonicly then be dispersed to even back and feed argon gas, be heated to the triethylene glycol boiling point 30～60min that refluxes again; Two, be cooled to room temperature then, drop into 100～300mg zinc acetate (presoma) again, slowly be heated to the triethylene glycol boiling point then, the 30～60min that refluxes, cooling back magnetic separates, and uses washing with alcohol again 4 times, and drying obtains CNT/Fe
3O
4The ZnO composite.
The present invention adopts the polyalcohol one kettle way to prepare CNT/Fe
3O
4ZnO magneto-optic double-function one-dimensional nano-composite material.This method is easy and simple to handle, can control the load capacity of ZnO through changing the presoma input amount.In the prepared one-dimensional nano-composite material that goes out, Fe
3O
4Even at the CNT area load with ZnO, the composite average diameter is about 60nm.Composite presents superparamagnetism, self is difficult for reuniting; The maximum saturation intensity of magnetization can reach 22emu/g, and good response is arranged under externally-applied magnetic field.And composite has photocatalytic, as a kind of catalyst with magnetic, can also use the magnetic field recycling after the photocatalysis, has saved resource.At the assembling photoelectric device, photocatalysis field all has application prospect.
Description of drawings
Fig. 1 is CNT/Fe
3O
4The XRD figure of ZnO composite, ■ representes Fe among the figure
3O
4, ↓ expression ZnO, a representes CNT: Fe
3O
4: ZnO=1: 2: 4, b represented CNT: Fe
3O
4: ZnO=1: 2: 2, c represented CNT: Fe
3O
4: ZnO=1: 2: 1; Fig. 2 is CNT/Fe
3O
4The infrared absorption spectra of ZnO (1: 2: 4) composite; Fig. 3 is CNT/Fe
3O
4The SEM pattern of ZnO (1: 2: 4) composite; Fig. 4 is CNT/Fe
3O
4The ability spectrogram of ZnO (1: 2: 4) composite; Fig. 5 is CNT/Fe
3O
4The TEM photo of composite; Fig. 6 is CNT/Fe
3O
4The TEM photo of ZnO (1: 2: 4) composite; Fig. 7 is CNT/Fe
3O
4And CNT/Fe
3O
4The hysteresis curve figure of ZnO (1: 2: 4) composite; Fig. 8 does not add magnetic field composite deployment conditions figure in ethanol; Fig. 9 adds magnetic field composite deployment conditions figure in ethanol; Figure 10 is that the UV, visible light of methyl orange aqueous solution after by composite photocatalysis different time absorbs spectrogram.
The specific embodiment
The specific embodiment one: the polyalcohol one kettle way prepares CNT/Fe in this embodiment
3O
4The method of ZnO one-dimensional nano-composite material is undertaken by following step: one, take by weighing 100mg multi-walled carbon nano-tubes (one dimension matrix), 100～400mg ferric acetyl acetonade (presoma) and 25ml triethylene glycol (solvent) back and mix; Ultrasonicly then be dispersed to even back and feed argon gas, be heated to the triethylene glycol boiling point 30～60min that refluxes again; Two, be cooled to room temperature then, drop into 100～300mg zinc acetate (presoma) again, slowly be heated to the triethylene glycol boiling point then, the 30～60min that refluxes, cooling back magnetic separates, and uses washing with alcohol again 4 times, and drying obtains CNT/Fe
3O
4The ZnO composite.
The specific embodiment two: what this embodiment and the specific embodiment one were different is: the frequency of ultrasonic dispersion is 80KHz in the step 1.
The specific embodiment three: what this embodiment and the specific embodiment one were different is: the firing rate in the step 2 be 5 ℃/min).
The specific embodiment four: what this embodiment and the specific embodiment one were different is: the temperature of the said drying of step 2 is 45 ℃, and the dry time is 10 hours.
The specific embodiment five: the polyalcohol one kettle way prepares CNT/Fe in this embodiment
3O
4The method of ZnO one-dimensional nano-composite material is undertaken by following step: one, take by weighing 100mg multi-walled carbon nano-tubes (one dimension matrix), 170mg ferric acetyl acetonade (presoma) and 25ml triethylene glycol (solvent) back and mix; Ultrasonicly then be dispersed to even back and feed argon gas (1L), be heated to triethylene glycol boiling point backflow 30min again; Two, be cooled to room temperature then, drop into about 200mg zinc acetate (presoma) again, slowly be heated to the triethylene glycol boiling point then, backflow 30min, cooling back magnetic separates, and uses washing with alcohol again 4 times, and drying is 10 hours under 45 ℃ of conditions, obtains CNT/Fe
3O
4The ZnO composite.
This embodiment prepares CNT in the product: Fe
3O
4: ZnO=1: 2: 4 (pressing mass ratio).
The specific embodiment six: the polyalcohol one kettle way prepares CNT/Fe in this embodiment
3O
4The method of ZnO one-dimensional nano-composite material is undertaken by following step: one, take by weighing 100mg multi-walled carbon nano-tubes (one dimension matrix), 170mg ferric acetyl acetonade (presoma) and 25ml triethylene glycol (solvent) back and mix; Ultrasonicly then be dispersed to even back and feed argon gas (1L), be heated to triethylene glycol boiling point backflow 30min again; Two, be cooled to room temperature then, drop into 100mg zinc acetate (presoma) again, slowly be heated to the triethylene glycol boiling point then, backflow 30min, cooling back magnetic separates, and uses washing with alcohol again 4 times, and drying obtained CNT/Fe in 10 hours under 45 ℃ of conditions
3O
4The ZnO composite.
This embodiment prepares CNT in the product: Fe
3O
4: ZnO=1: 2: 2 (pressing mass ratio).
The specific embodiment seven: the polyalcohol one kettle way prepares CNT/Fe in this embodiment
3O
4The method of ZnO one-dimensional nano-composite material is undertaken by following step: one, take by weighing 100mg multi-walled carbon nano-tubes (one dimension matrix), 170mg ferric acetyl acetonade (presoma) and 25ml triethylene glycol (solvent) back and mix; Ultrasonicly then be dispersed to even back and feed argon gas (1L), be heated to triethylene glycol boiling point backflow 30min again; Two, be cooled to room temperature then, drop into 50mg zinc acetate (presoma) again, slowly be heated to the triethylene glycol boiling point then, backflow 30min, cooling back magnetic separates, and uses washing with alcohol again 4 times, and drying obtained CNT/Fe in 10 hours under 45 ℃ of conditions
3O
4The ZnO composite.
This embodiment prepares CNT in the product: Fe
3O
4: ZnO=1: 2: 1 (pressing mass ratio).
Fig. 1 is the XRD figure of composite.The peak of 2 θ=26 ° is the peak of CNT; 2 θ=30.28 °, 2 θ=43.40 °, 2 θ=53.28 °, the diffraction maximum of 2 θ=57.14 ° and 2 θ=62.76 ° is corresponding Fe respectively
3O
4(220), (400), (422), (511), (440) crystal face.31.90 °, (100), (101) of 36.10 °, 47.34 °, 56.52 °, 62.96 °, the 67.98 ° corresponding buergerites of difference, (102), (110), (103), (112) crystal face.Visible from Fig. 1, the presoma zinc acetate is many more, and the ZnO characteristic peak is obvious more.Explanation is through increasing the load capacity that the presoma rate of charge just can increase ZnO.
Fig. 2 is CNT/Fe
3O
4The infrared spectrum of ZnO nano composite material.467cm wherein
-1The peak at place is the characteristic peak of ZnO, 580cm
-1The peak at place is Fe
3O
4Characteristic peak.Consistent with XRD, the ZnO characteristic peak is the most obvious the most for a long time for the zinc acetate rate of charge.
Fig. 3 is CNT/Fe
3O
4The SEM pattern and the power spectrum of ZnO composite.The whole uniform depositions of ZnO nano particle are not free in outside ZnO particle on the magnetic carbon nano-tube surface.From power spectrum, can find out has the Zn element.
4 figure are CNT/Fe
3O
4The TEM pattern photo of magnetic carbon nano-tube.5 and 6 figure are CNT/Fe
3O
4The pattern of ZnO nano composite material.ZnO all evenly is coated on the magnetic carbon nano-tube surface.Compare with magnetic carbon tube, it is big that the caliber of composite becomes, and average diameter is about 60nm.
Fig. 9 is the hysteresis curve of composite.All CNT/Fe
3O
4The ZnO composite all presents ultra paramagnetic characteristic, maximum saturation intensity of magnetization 22emu/g.ZnO content is many more, and saturation magnetization is more little.This is because ZnO occupies a part of quality, and inner magnetic carbon tube is had shielding action.Fig. 8 and 9 is for adding composite deployment conditions in ethanolic solution before and after the magnetic field, add magnetic field before composite be dispersed in the ethanol; After adding magnetic field, composite gathers near the magnet, can find out that composite has good magnetic response characteristic.
Figure 10 is through behind the composite photocatalysis different time, the UV, visible light absorption spectra of methyl orange aqueous solution.Under the high-voltage ultraviolet mercury lamp illuminate condition, use CNT/Fe
3O
4ZnO (1: 2: 4) composite carries out photocatalytic degradation to methyl orange.Find out that from figure along with the photocatalysis time increases, the absworption peak that methyl orange is positioned at the 467nm place weakens to zero gradually, explains that methyl orange has been degraded under the catalysis of composite.Composite has catalysis.
In sum, the present invention has synthesized CNT/Fe with a kind of easy method
3O
4The ZnO one-dimensional nano-composite material.This composite has superparamagnetism and higher saturation magnetization, self is difficult for reuniting, and good magnetic response is arranged under externally-applied magnetic field.In addition, this composite also has photocatalysis performance.At the assembling photoelectric device, photocatalysis field has application prospect.
Claims (4)
1. the polyalcohol one kettle way prepares CNT/Fe
3O
4The method of ZnO one-dimensional nano-composite material is characterized in that the polyalcohol one kettle way prepares CNT/Fe
3O
4The method of ZnO one-dimensional nano-composite material is undertaken by following step: mix after one, taking by weighing 100mg multi-walled carbon nano-tubes, 100～400mg ferric acetyl acetonade and 25ml triethylene glycol; Ultrasonicly then be dispersed to even back and feed argon gas, be heated to the triethylene glycol boiling point 30～60min that refluxes again; Two, be cooled to room temperature then, drop into 100～300mg zinc acetate again, slowly be heated to the triethylene glycol boiling point then, the 30～60min that refluxes, cooling back magnetic separates, and uses washing with alcohol again 4 times, and drying obtains CNT/Fe
3O
4The ZnO composite.
2. polyalcohol one kettle way according to claim 1 prepares CNT/Fe
3O
4The method of ZnO one-dimensional nano-composite material, the frequency that it is characterized in that ultrasonic dispersion in the step 1 is 80KHz.
3. polyalcohol one kettle way according to claim 1 prepares CNT/Fe
3O
4The method of ZnO one-dimensional nano-composite material is characterized in that the 5 ℃/min of firing rate in the step 2.
4. polyalcohol one kettle way according to claim 1 prepares CNT/Fe
3O
4The method of ZnO one-dimensional nano-composite material, the temperature that it is characterized in that the said drying of step 2 is 45 ℃, the dry time is 10 hours.
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| CN102515281A (en) * | 2011-11-18 | 2012-06-27 | 内蒙古师范大学 | Preparation method for Fe3O4 magnetic fluid and water-soluble Fe3O4 powder |
| CN102773111B (en) * | 2012-07-06 | 2014-06-11 | 上海应用技术学院 | Magnetic solid super acid nanotube catalytic agent and preparation method thereof |
| CN105158217A (en) * | 2015-06-09 | 2015-12-16 | 济南大学 | Preparation method and application of Fe3O4@ZnO@L-Cys magnetic fluorescent probe used for detecting ferric ions |
| CN108079368A (en) * | 2018-02-09 | 2018-05-29 | 重庆医科大学附属永川医院 | A kind of magnetism calcium orthophosphate base bone cement and preparation method thereof |
| CN110724493B (en) * | 2019-09-29 | 2022-11-18 | 安徽理工大学 | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN114129724B (en) * | 2020-09-03 | 2023-07-28 | 天津大学 | Microwave-excited targeted sterilization nanoparticle, preparation method and application thereof |
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| CN100999319A (en) * | 2006-12-31 | 2007-07-18 | 哈尔滨工业大学 | Preparation method of magnetic controlled ultra paramagnetism nanometer carbon pipe |
| CN101239716A (en) * | 2008-03-19 | 2008-08-13 | 哈尔滨工业大学 | Preparation method of polymer grafting magnetic carbon nano-tube |
| CN101823689A (en) * | 2010-02-20 | 2010-09-08 | 哈尔滨工业大学 | Method for preparing porous metal oxide-coated carbon nanotube composite material |
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| CN100999319A (en) * | 2006-12-31 | 2007-07-18 | 哈尔滨工业大学 | Preparation method of magnetic controlled ultra paramagnetism nanometer carbon pipe |
| CN101239716A (en) * | 2008-03-19 | 2008-08-13 | 哈尔滨工业大学 | Preparation method of polymer grafting magnetic carbon nano-tube |
| CN101823689A (en) * | 2010-02-20 | 2010-09-08 | 哈尔滨工业大学 | Method for preparing porous metal oxide-coated carbon nanotube composite material |
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