CN103754953B - Preparation method of multi-morphologynano-sized zinc ferrite - Google Patents
Preparation method of multi-morphologynano-sized zinc ferrite Download PDFInfo
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- CN103754953B CN103754953B CN201410041672.7A CN201410041672A CN103754953B CN 103754953 B CN103754953 B CN 103754953B CN 201410041672 A CN201410041672 A CN 201410041672A CN 103754953 B CN103754953 B CN 103754953B
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Abstract
The invention provides a preparation method, and relates to the field of nano inorganic non-metallic materials. The preparation method comprises the following steps: adding a metal salt and an organic linear polymer into a solvent, and uniformly stirring the mixture so as to obtain a mixed solution; electrostatically spraying the mixed solution, and obtaining a precursor; heating the precursor to a temperature of 350-500 DEG C at a presintering heating rate and keeping the temperature for 2-4h, and heating the precursor to reach the temperature of 700-1000 DEG C at a calcining heating rate and keeping the temperature for 1-5h, naturally cooling the recursor, and obtaining the nanoZnFe2O4. According to the invention, nanoZnFe2O4 materials with one system and multi-morphology are synthetized by the same method, ZnFe2O4with sphere-shaped, fibre-shaped, chain bead-shaped and rod-shaped morphology is obtained by controlling the raw material ratio and regulating and controlling the heat treatment process, the production cost is effectively reduced, the production efficiency is improved, and the operation is convenient, therefore, the preparation method is suitable for industrial production of a certain scale.
Description
Technical field
The present invention relates to Nanosized Inorganic Non-Metal Materials field, be specifically related to the preparation method of multi-morphology nano zinc ferrite.
Background technology
In recent years, nanometer zinc ferrite (ZnFe
2o
4) material is widely used in the territories such as magneticsubstance, new energy materials, stealth material, environmentally conscious materials, is a kind of important functional materials.According to numerous research report, pattern affects nanometer Zn Fe
2o
4the important factor in order of magnetic performance, absorbing property, absorption property, catalytic performance, chemical property, therefore large quantity research all concentrates on the nanometer Zn Fe preparing different-shape
2o
4.
At present, at numerous nanometer Zn Fe
2o
4preparation method in, coprecipitation method, solid phase method, solvent-thermal method, sol-gel method, template, method of electrostatic spinning etc. occupy more important status.Such as: application number is that application for a patent for invention employing chemical coprecipitation-local structured's legal system of 201010512661.4 is for bar-shaped ZnFe
2o
4, and point out that this material can be used for field of magnetic material; " hazardous material magazine " (Journal of Hazardous Materials, 2013,250-251:229-237) spherical ZnFe that utilized solvent-thermal method to prepare
2o
4, and point out that this material can be used as sorbing material field; " material bulletin " (Materials Letters, 2006,60:154-158) utilizes template synthesis nanometer wire ZnFe
2o
4, and point out that this material can be used as field of magnetic material; " application material and interface " (ACS APPLIED MATERIALS & INTERFACES, 2013,5:5461-5467) fibrous ZnFe that utilized method of electrostatic spinning to prepare
2o
4, and point out that the anode material that this material can be used as lithium ion battery is applied in new energy materials field; " Xinan Science and Technology Univ.'s journal " (Xinan Science and Technology Univ.'s journal, 2009,24:16-22) bar-shaped ZnFe that adopted solid phase method to prepare
2o
4, and point out that this material can be used as photocatalysis field.
Can find out, pattern is to ZnFe
2o
4performance important, the ZnFe of different-shape
2o
4can be applied within the scope of different field.But existing method all can only obtain a kind of product of pattern, effectively can not control the change of pattern, as the ZnFe of different morphologies need be obtained
2o
4, then need to adopt diverse ways, device fabrication, operation and inconvenience thereof, seriously limit ZnFe
2o
4industrial applications and production efficiency.
Summary of the invention
The object of this invention is to provide the preparation method of different-shape nano zinc ferrite, the nanometer zinc ferrite with spherical, fibrous, chain pearl and Rod-like shape can be obtained by the regulation and control of the control of proportioning raw materials and thermal treatment process, and preparation method is simple, simple operation, with low cost, be applicable to large-scale industrial production.
A preparation method for multi-morphology nano zinc ferrite, comprises the steps:
(1) metal-salt and organic linear polymeric polymkeric substance are joined in solvent, stir, obtain mixing solutions;
(2) described mixing solutions is carried out electrostatic spraying, obtain presoma;
(3) presoma be warming up to 350 ~ 500 DEG C with pre-burning temperature rise rate and be incubated 2 ~ 4h, and then be warming up to 700 ~ 1000 DEG C and be incubated 1 ~ 5h to calcine temperature rise rate, naturally cooling, obtaining nanometer Zn Fe
2o
4.
Described metal-salt is one or more in nitrate, chlorate, acetate and acetylacetonate.
Described organic linear polymeric polymkeric substance is polyoxyethylene, polyvinylpyrrolidone or polyvinyl alcohol.
Described solvent is ethanol, water or DMF.
In described mixing solutions, the mass percentage of metal-salt is 5 ~ 13%, the mass percentage of organic linear molecule polymkeric substance is 3 ~ 12%, when pre-burning temperature rise rate is 1 ~ 5 DEG C/min, obtains the zinc ferrite that nanometer is spherical; In described mixing solutions, the mass percentage of metal-salt is 5 ~ 13%, the mass percentage of organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 1 ~ 5 DEG C/min, obtains nanometer fibrous zinc ferrite; In described mixing solutions, the mass percentage of metal-salt is 14 ~ 17%, and the mass percentage of described organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 1 ~ 5 DEG C/min, obtains the zinc ferrite of nano chain pearl; In described mixing solutions, the mass percentage of metal-salt is 5 ~ 13%, and the mass percentage of organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 7 ~ 10 DEG C/min, obtains the zinc ferrite of nano bar-shape.
Described calcining temperature rise rate is 1 ~ 5 DEG C/min.
During described electrostatic spraying, electrostatic potential is 10 ~ 20 kV, spray distance 8 ~ 20 cm.
beneficial effect:
1. present invention achieves the nanometer zinc ferrite material being synthesized a kind of system, different morphologies by preparation method of the same race, the nanometer zinc ferrite with spherical, fibrous, chain pearl and Rod-like shape can be obtained by the regulation and control of the control of proportioning raw materials and thermal treatment process, effectively reduce production cost, improve production efficiency, and simple operation, is applicable to the suitability for industrialized production of certain scale.
2. the different morphologies nanometer zinc ferrite that prepared by the inventive method can be applied in the territories such as magneticsubstance, new energy materials, stealth material, environmentally conscious materials, has broad application market and prospect.
accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of material 1
Fig. 2 is the cold field emission scanning electron microscope (SEM) photograph of material 1.
Fig. 3 is the X-ray diffractogram of material 2.
Fig. 4 is the cold field emission scanning electron microscope (SEM) photograph of material 2.
Fig. 5 is the X-ray diffractogram of material 3.
Fig. 6 is the cold field emission scanning electron microscope (SEM) photograph of material 3.
Fig. 7 is the X-ray diffractogram of material 4.
Fig. 8 is the cold field emission scanning electron microscope (SEM) photograph of material 4.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but should not limit the scope of the invention with this.
embodiment 1
take 2.2g bis-acetate hydrate zinc, 8.08g Fe(NO3)39H2O and 13g polyvinyl alcohol (model is 1750 ± 50, Chemical Reagent Co., Ltd., Sinopharm Group), join in 105ml deionized water, stir, obtain mixing solutions;
mixing solutions is carried out electrostatic spraying, the presoma of obtained spherical morphology, wherein, electrostatic potential is 10 kV, spray distance 8cm;
the presoma of spherical morphology be warming up to 350 DEG C with the pre-burning temperature rise rate of 5 DEG C/min and be incubated 2h, and then is warming up to 1000 DEG C and is incubated 1h with the calcining temperature rise rate of 5 DEG C/min, naturally cooling, obtaining material 1.
Adopt X-ray diffraction analysis instrument (XRD, Model X ' TRAX) to carry out crystal species analysis, result as shown in Figure 1, can find out that material 1 is the zinc ferrite (ZnFe of pure phase
2o
4).Adopt cold field emission scanning electron microscope (FESEM, S-4800) to carry out microscopic appearance test, result as shown in Figure 2, can find out that zinc ferrite presents nanometer spherical morphology.
embodiment 2
take 1.36g zinc chloride, 7.06g ferric acetyl acetonade and 18g PVP K-30 (Chemical Reagent Co., Ltd., Sinopharm Group) to join in 100ml ethanolic soln, stir, obtain mixing solutions;
mixing solutions is carried out electrostatic spraying, obtains the presoma of fibrous morphology, wherein, electrostatic potential is 15 kV, spray distance 13cm;
the presoma of fibrous morphology be warming up to 500 DEG C with the pre-burning temperature rise rate of 1 DEG C/min and be incubated 4h, and then is warming up to 700 DEG C and is incubated 5h with the calcining temperature rise rate of 1 DEG C/min, naturally cooling, obtaining material 2
4.
Adopt X-ray diffraction analysis instrument (XRD, Model X ' TRAX) to carry out crystal species analysis, result as shown in Figure 3, can find out that material 2 is pure phase zinc ferrite (ZnFe
2o
4).Adopt cold field emission scanning electron microscope (FESEM, S-4800) to carry out microscopic appearance test, result as shown in Figure 4, can find out that material 2 presents nanometer fibrous pattern.
embodiment 3
take 2.2 g bis-acetate hydrate zinc, 5.41g ferric chloride hexahydrate and 10g polyoxyethylene (molecular weight 1000000, Shanghai Liansheng Chemical Co., Ltd.), join 35mlN, in dinethylformamide solution, stir, obtain mixing solutions;
mixing solutions is carried out electrostatic spraying, obtains chain pearl pattern presoma, wherein, electrostatic potential is 20 kV, spray distance 20cm;
the presoma of Rod-like shape be warming up to 400 DEG C with the pre-burning temperature rise rate of 3 DEG C/min and be incubated 3h, and then is warming up to 900 DEG C and is incubated 3h with the calcining temperature rise rate of 3 DEG C/min, naturally cooling, obtaining material 3.
Adopt X-ray diffraction analysis instrument (XRD, Model X ' TRAX) to carry out crystal species analysis, result as shown in Figure 5, can find out that material 3 is pure phase zinc ferrite (ZnFe
2o
4).Adopt cold field emission scanning electron microscope (FESEM, S-4800) to carry out microscopic appearance test, result as shown in Figure 6, can find out that material 3 presents nano chain pearl pattern.
embodiment 4
take 2.97 g zinc nitrate hexahydrates, 7.06g ferric acetyl acetonade and 19g PVP K-30 (Chemical Reagent Co., Ltd., Sinopharm Group) to join in 118ml ethanolic soln, stir, obtain mixing solutions;
mixing solutions is carried out electrostatic spraying and obtains Rod-like shape presoma, wherein, electrostatic potential is 14 kV, spray distance 12cm;
the presoma of Rod-like shape be warming up to 450 DEG C with the pre-burning temperature rise rate of 9 DEG C/min and be incubated 3h, and then is warming up to 800 DEG C and is incubated 2h with the calcining temperature rise rate of 2 DEG C/min, naturally cooling, obtaining material 4.
Adopt X-ray diffraction analysis instrument (XRD, Model X ' TRAX) to carry out crystal species analysis, result as shown in Figure 7, can find out that material 4 is pure phase zinc ferrite (ZnFe
2o
4).Adopt cold field emission scanning electron microscope (FESEM, S-4800) to carry out microscopic appearance test, result as shown in Figure 8, can find out that material 4 presents nano bar-shape pattern.
Claims (4)
1. a preparation method for multi-morphology nano zinc ferrite, is characterized in that comprising the steps:
(1) metal-salt and organic linear polymeric polymkeric substance are joined in solvent, stir, obtain mixing solutions;
(2) described mixing solutions is carried out electrostatic spraying, obtain presoma;
(3) presoma be warming up to 350 ~ 500 DEG C with pre-burning temperature rise rate and be incubated 2 ~ 4h, and then be warming up to 700 ~ 1000 DEG C and be incubated 1 ~ 5h to calcine temperature rise rate, naturally cooling, obtaining nanometer Zn Fe
2o
4;
In described mixing solutions, the mass percentage of metal-salt is 5 ~ 13%, the mass percentage of organic linear polymeric polymkeric substance is 3 ~ 12%, and pre-burning temperature rise rate is 5 DEG C/min, and described metal-salt is zinc acetate and iron nitrate, obtains the zinc ferrite that nanometer is spherical; Or in described mixing solutions, the mass percentage of metal-salt is 5 ~ 13%, the mass percentage of organic linear polymeric polymkeric substance is 13 ~ 20%, pre-burning temperature rise rate is 1 DEG C/min, described metal-salt is zinc chloride and ferric acetyl acetonade, obtains nanometer fibrous zinc ferrite; Or the mass percentage of metal-salt is 14 ~ 17% in described mixing solutions, the mass percentage of described organic linear polymeric polymkeric substance is 13 ~ 20%, pre-burning temperature rise rate is 3 DEG C/min, and described metal-salt is zinc acetate and iron(ic) chloride, obtains the zinc ferrite of nano chain pearl; Or the mass percentage of metal-salt is 5 ~ 13% in described mixing solutions, the mass percentage of organic linear polymeric polymkeric substance is 13 ~ 20%, pre-burning temperature rise rate is 9 DEG C/min, and described metal-salt is zinc nitrate and ferric acetyl acetonade, obtains the zinc ferrite of nano bar-shape; Described organic linear polymeric polymkeric substance is polyoxyethylene, polyvinylpyrrolidone or polyvinyl alcohol.
2. the preparation method of multi-morphology nano zinc ferrite according to claim 1, is characterized in that described solvent is ethanol, water or DMF.
3. the preparation method of multi-morphology nano zinc ferrite according to claim 2, is characterized in that: described calcining temperature rise rate is 1 ~ 5 DEG C/min.
4. according to the preparation method of the described multi-morphology nano zinc ferrite of one of claim 1-3, it is characterized in that: in described electrostatic spray process, electrostatic potential is 10 ~ 20 kV, spray distance 8 ~ 20 cm.
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| CN104016414B (en) * | 2014-06-23 | 2015-11-18 | 湖南大学 | A kind of preparation method of ferrite nano line |
| CN104310459B (en) * | 2014-10-22 | 2017-01-18 | 上海大学 | Preparation method of zinc oxide nano-rod |
| CN106896146B (en) * | 2017-01-05 | 2019-03-01 | 扬州大学 | A kind of coating production of zinc ferrite acetone gas sensing layer |
| CN108793261B (en) * | 2018-08-22 | 2020-06-05 | 浙江理工大学 | Preparation method of nano zinc ferrite by taking calamine as raw material |
| CN109264787B (en) * | 2018-09-20 | 2020-10-30 | 济南大学 | ZnFe2O4Preparation method of cubic block structure and obtained product |
| CN109231340B (en) * | 2018-10-22 | 2021-05-14 | 沈阳理工大学 | Preparation method of light diatomite water treatment material |
| CN110639529B (en) * | 2019-09-12 | 2021-02-09 | 中国科学院高能物理研究所 | Catalyst for removing hexavalent uranium through visible light catalytic reduction, method and application |
| CN111977696B (en) * | 2020-08-13 | 2022-06-07 | 吉林化工学院 | Preparation method and application of pomegranate-shaped magnetic visible light heterogeneous Fenton catalyst material |
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| CN101289228A (en) * | 2008-06-03 | 2008-10-22 | 浙江理工大学 | Method for preparing porous zinc ferrite nano-rods |
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| CN101289228A (en) * | 2008-06-03 | 2008-10-22 | 浙江理工大学 | Method for preparing porous zinc ferrite nano-rods |
Non-Patent Citations (1)
| Title |
|---|
| Fabrication and magnetic properties of electrospun zinc ferrite (ZnFe2O4) nanofibres;W. Ponhan, et al.;《Materials Science and Technology》;20101231;第26卷(第11期);第1298-1303页 * |
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