CN103754953A - Preparation method of multi-morphologynano-sized zinc ferrite - Google Patents

Preparation method of multi-morphologynano-sized zinc ferrite Download PDF

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CN103754953A
CN103754953A CN201410041672.7A CN201410041672A CN103754953A CN 103754953 A CN103754953 A CN 103754953A CN 201410041672 A CN201410041672 A CN 201410041672A CN 103754953 A CN103754953 A CN 103754953A
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zinc ferrite
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CN103754953B (en
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黄啸谷
赖敏
程国生
张其土
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Nanjing University of Information Science and Technology
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Nanjing University of Information Science and Technology
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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

The preparation method of multi-morphology nano zinc ferrite
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 reports, pattern is to affect 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 for 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 compared with consequence.For example: the application for a patent for invention that application number is 201010512661.4 adopts chemical coprecipitation-local structured legal system 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) utilize solvent-thermal method to prepare spherical ZnFe 2o 4, and point out that this material can be used as sorbing material field; < < material wall bulletin > > (Materials Letters, 2006,60:154-158) has utilized 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) utilize method of electrostatic spinning to prepare fibrous ZnFe 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; The journal > > of < < Xinan Science and Technology Univ. (Xinan Science and Technology Univ.'s journal, 2009,24:16-22) adopts solid phase method to prepare bar-shaped ZnFe 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 make a kind of product of pattern, can not effectively control the variation of pattern, as need obtain the ZnFe of different morphologies 2o 4, needing to adopt diverse ways, device fabrication, operation and inconvenience thereof, seriously limited 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, can the regulation and control by the control of proportioning raw materials and thermal treatment process obtain the nanometer zinc ferrite with spherical, fibrous, chain pearl and Rod-like shape, and preparation method is simple, simple operation, with low cost, is 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 to electrostatic spraying, obtain presoma;
(3) presoma is warming up to 350 ~ 500 ℃ and be incubated 2 ~ 4h with pre-burning temperature rise rate, and then is warming up to 700 ~ 1000 ℃ and be incubated 1 ~ 5h with calcining temperature rise rate, naturally cooling, obtains 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 quality percentage composition of metal-salt is 5 ~ 13%, the quality percentage composition of organic linear molecule polymkeric substance is 3 ~ 12%, when pre-burning temperature rise rate is 1 ~ 5 ℃/min, obtains the spherical zinc ferrite of nanometer; In described mixing solutions, the quality percentage composition of metal-salt is 5 ~ 13%, the quality percentage composition of organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 1 ~ 5 ℃/min, obtains nanometer fibrous zinc ferrite; In described mixing solutions, the quality percentage composition of metal-salt is 14 ~ 17%, and the quality percentage composition of described organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 1 ~ 5 ℃/min, obtains the zinc ferrite of nano chain pearl; In described mixing solutions, the quality percentage composition of metal-salt is 5 ~ 13%, and the quality percentage composition of organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 7 ~ 10 ℃/min, obtains the zinc ferrite of nano bar-shape.
Described calcining temperature rise rate is 1 ~ 5 ℃/min.
During described electrostatic spraying, electrostatic potential is 10 ~ 20 kV, spray distance 8 ~ 20 cm.
beneficial effect:
1. the present invention has realized by the nanometer zinc ferrite material of the synthetic a kind of system of preparation method of the same race, different morphologies, can the regulation and control by the control of proportioning raw materials and thermal treatment process obtain the nanometer zinc ferrite with spherical, fibrous, chain pearl and Rod-like shape, effectively reduce production cost, improved production efficiency, and simple operation, the suitability for industrialized production of applicable 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 figure of material 1.
Fig. 3 is the X-ray diffractogram of material 2.
Fig. 4 is the cold field emission scanning electron microscope figure of material 2.
Fig. 5 is the X-ray diffractogram of material 3.
Fig. 6 is the cold field emission scanning electron microscope figure of material 3.
Fig. 7 is the X-ray diffractogram of material 4.
Fig. 8 is the cold field emission scanning electron microscope figure 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
Figure 2014100416727100002DEST_PATH_IMAGE001
take 2.2g bis-hydration zinc acetates, 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;
Figure 986427DEST_PATH_IMAGE002
mixing solutions is carried out to electrostatic spraying, make the presoma of spherical pattern, wherein, electrostatic potential is 10 kV, spray distance 8cm;
Figure 2014100416727100002DEST_PATH_IMAGE003
the presoma of spherical pattern is warming up to 350 ℃ and be incubated 2h with the pre-burning temperature rise rate of 5 ℃/min, and then is warming up to 1000 ℃ and be incubated 1h with the calcining temperature rise rate of 5 ℃/min, naturally cooling, obtains material 1.
Adopt X-ray diffraction analysis instrument (XRD, Model X ' TRAX) to carry out phase composite analysis, result as shown in Figure 1, can be found out the zinc ferrite (ZnFe of material 1 for 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 the spherical pattern of nanometer.
embodiment 2
Figure 662128DEST_PATH_IMAGE001
take 1.36g zinc chloride, 7.06g ferric acetyl acetonade and 18g PVP K-30 (Chemical Reagent Co., Ltd., Sinopharm Group) and join in 100ml ethanolic soln, stir, obtain mixing solutions;
Figure 602402DEST_PATH_IMAGE002
mixing solutions is carried out to electrostatic spraying, obtain the presoma of fibrous morphology, wherein, electrostatic potential is 15 kV, spray distance 13cm;
the presoma of fibrous morphology is warming up to 500 ℃ and be incubated 4h with the pre-burning temperature rise rate of 1 ℃/min, and then is warming up to 700 ℃ and be incubated 5h with the calcining temperature rise rate of 1 ℃/min, naturally cooling, obtains material 2 4.
Adopt X-ray diffraction analysis instrument (XRD, Model X ' TRAX) to carry out phase composite analysis, result as shown in Figure 3, can find out that material 2 is for 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
Figure 927870DEST_PATH_IMAGE001
take 2.2 g bis-hydration zinc acetates, 5.41g ferric chloride hexahydrate and 10g polyoxyethylene (molecular weight 1000000, Shanghai Lian Sheng Chemical Co., Ltd.), join 35mlN, in dinethylformamide solution, stir, obtain mixing solutions;
Figure 169496DEST_PATH_IMAGE002
mixing solutions is carried out to electrostatic spraying, obtain chain pearl pattern presoma, wherein, electrostatic potential is 20 kV, spray distance 20cm;
Figure 897149DEST_PATH_IMAGE003
the presoma of Rod-like shape is warming up to 400 ℃ and be incubated 3h with the pre-burning temperature rise rate of 3 ℃/min, and then is warming up to 900 ℃ and be incubated 3h with the calcining temperature rise rate of 3 ℃/min, naturally cooling, obtains material 3.
Adopt X-ray diffraction analysis instrument (XRD, Model X ' TRAX) to carry out phase composite analysis, result as shown in Figure 5, can find out that material 3 is for 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
Figure 540620DEST_PATH_IMAGE001
take 2.97 g zinc nitrate hexahydrates, 7.06g ferric acetyl acetonade and 19g PVP K-30 (Chemical Reagent Co., Ltd., Sinopharm Group) and join in 118ml ethanolic soln, stir, obtain mixing solutions;
mixing solutions is carried out to electrostatic spraying and make Rod-like shape presoma, wherein, electrostatic potential is 14 kV, spray distance 12cm;
Figure 276812DEST_PATH_IMAGE003
the presoma of Rod-like shape is warming up to 450 ℃ and be incubated 3h with the pre-burning temperature rise rate of 9 ℃/min, and then is warming up to 800 ℃ and be incubated 2h with the calcining temperature rise rate of 2 ℃/min, naturally cooling, obtains material 4.
Adopt X-ray diffraction analysis instrument (XRD, Model X ' TRAX) to carry out phase composite analysis, result as shown in Figure 7, can find out that material 4 is for 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 (7)

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 to electrostatic spraying, obtain presoma;
(3) presoma is warming up to 350 ~ 500 ℃ and be incubated 2 ~ 4h with pre-burning temperature rise rate, and then is warming up to 700 ~ 1000 ℃ and be incubated 1 ~ 5h with calcining temperature rise rate, naturally cooling, obtains nanometer Zn Fe 2o 4.
2. the preparation method of multi-morphology nano zinc ferrite according to claim 1, is characterized in that described metal-salt is one or more in nitrate, chlorate, acetate and acetylacetonate.
3. the preparation method of multi-morphology nano zinc ferrite according to claim 2, is characterized in that described organic linear polymeric polymkeric substance is polyoxyethylene, polyvinylpyrrolidone or polyvinyl alcohol.
4. the preparation method of multi-morphology nano zinc ferrite according to claim 3, is characterized in that described solvent is ethanol, water or DMF.
5. the preparation method of multi-morphology nano zinc ferrite according to claim 4, it is characterized in that: in described mixing solutions, the quality percentage composition of metal-salt is 5 ~ 13%, the quality percentage composition of organic linear molecule polymkeric substance is 3 ~ 12%, when pre-burning temperature rise rate is 1 ~ 5 ℃/min, obtain the spherical zinc ferrite of nanometer; In described mixing solutions, the quality percentage composition of metal-salt is 5 ~ 13%, the quality percentage composition of organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 1 ~ 5 ℃/min, obtains nanometer fibrous zinc ferrite; In described mixing solutions, the quality percentage composition of metal-salt is 14 ~ 17%, and the quality percentage composition of described organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 1 ~ 5 ℃/min, obtains the zinc ferrite of nano chain pearl; In described mixing solutions, the quality percentage composition of metal-salt is 5 ~ 13%, and the quality percentage composition of organic linear molecule polymkeric substance is 13 ~ 20%, when pre-burning temperature rise rate is 7 ~ 10 ℃/min, obtains the zinc ferrite of nano bar-shape.
6. the preparation method of multi-morphology nano zinc ferrite according to claim 4, is characterized in that: described calcining temperature rise rate is 1 ~ 5 ℃/min.
7. according to the preparation method of the described multi-morphology nano zinc ferrite of one of claim 1-6, 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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Cited By (8)

* Cited by examiner, † Cited by third party
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CN104016414A (en) * 2014-06-23 2014-09-03 湖南大学 Preparation method of ferrite nanowire
CN104310459A (en) * 2014-10-22 2015-01-28 上海大学 Novel preparation method of zinc oxide nano-rod
CN106896146A (en) * 2017-01-05 2017-06-27 扬州大学 A kind of coating production of zinc ferrite acetone gas sensing layer
CN108793261A (en) * 2018-08-22 2018-11-13 浙江理工大学 It is a kind of using monheimite as the preparation method of the nanometer zinc ferrite of raw material
CN109231340A (en) * 2018-10-22 2019-01-18 沈阳理工大学 A kind of preparation method of lightweight diatomite material for water treatment
CN109264787A (en) * 2018-09-20 2019-01-25 济南大学 A kind of ZnFe2O4The preparation method and products obtained therefrom of cube block structure
CN110639529A (en) * 2019-09-12 2020-01-03 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
CN111977696A (en) * 2020-08-13 2020-11-24 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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W. PONHAN, ET AL.: "Fabrication and magnetic properties of electrospun zinc ferrite (ZnFe2O4) nanofibres", 《MATERIALS SCIENCE AND TECHNOLOGY》 *

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104016414B (en) * 2014-06-23 2015-11-18 湖南大学 A kind of preparation method of ferrite nano line
CN104016414A (en) * 2014-06-23 2014-09-03 湖南大学 Preparation method of ferrite nanowire
CN104310459A (en) * 2014-10-22 2015-01-28 上海大学 Novel preparation method of zinc oxide nano-rod
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
CN106896146A (en) * 2017-01-05 2017-06-27 扬州大学 A kind of coating production of zinc ferrite acetone gas sensing layer
CN108793261A (en) * 2018-08-22 2018-11-13 浙江理工大学 It is a kind of using monheimite as the preparation method of the nanometer zinc ferrite of raw material
CN109264787A (en) * 2018-09-20 2019-01-25 济南大学 A kind of ZnFe2O4The preparation method and products obtained therefrom of cube block structure
CN109231340A (en) * 2018-10-22 2019-01-18 沈阳理工大学 A kind of preparation method of lightweight diatomite material for water treatment
CN109231340B (en) * 2018-10-22 2021-05-14 沈阳理工大学 Preparation method of light diatomite water treatment material
CN110639529A (en) * 2019-09-12 2020-01-03 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
CN111977696A (en) * 2020-08-13 2020-11-24 吉林化工学院 Preparation method and application of pomegranate-shaped magnetic visible light heterogeneous Fenton catalyst material
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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