CN103754953A - Preparation method of multi-morphologynano-sized zinc ferrite - Google Patents
Preparation method of multi-morphologynano-sized zinc ferrite Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- zinc ferrite
- preparation
- temperature rise
- percentage composition
- rise rate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
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 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.
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;
mixing solutions is carried out to electrostatic spraying, make the presoma of spherical pattern, wherein, electrostatic potential is 10 kV, spray distance 8cm;
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
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;
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
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;
mixing solutions is carried out to electrostatic spraying, obtain chain pearl pattern presoma, wherein, electrostatic potential is 20 kV, spray distance 20cm;
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
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;
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.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410041672.7A CN103754953B (en) | 2014-01-28 | 2014-01-28 | Preparation method of multi-morphologynano-sized zinc ferrite |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410041672.7A CN103754953B (en) | 2014-01-28 | 2014-01-28 | Preparation method of multi-morphologynano-sized zinc ferrite |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103754953A true CN103754953A (en) | 2014-04-30 |
CN103754953B CN103754953B (en) | 2015-07-22 |
Family
ID=50522321
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201410041672.7A Expired - Fee Related CN103754953B (en) | 2014-01-28 | 2014-01-28 | Preparation method of multi-morphologynano-sized zinc ferrite |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103754953B (en) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101289228A (en) * | 2008-06-03 | 2008-10-22 | 浙江理工大学 | Method for preparing porous zinc ferrite nano-rods |
-
2014
- 2014-01-28 CN CN201410041672.7A patent/CN103754953B/en not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
---|
W. PONHAN, ET AL.: "Fabrication and magnetic properties of electrospun zinc ferrite (ZnFe2O4) nanofibres", 《MATERIALS SCIENCE AND TECHNOLOGY》 * |
Cited By (13)
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 |
Also Published As
Publication number | Publication date |
---|---|
CN103754953B (en) | 2015-07-22 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103754953B (en) | Preparation method of multi-morphologynano-sized zinc ferrite | |
Boldrin et al. | Direct synthesis of nanosized NiCo2O4 spinel and related compounds via continuous hydrothermal synthesis methods | |
CN103956473A (en) | CuO-Cu2O/graphene nano compound material and preparation method thereof | |
CN104505508A (en) | Preparation method of nickel cobalt oxide electrode material | |
Davar et al. | Synthesis and optical properties of pure monoclinic zirconia nanosheets by a new precursor | |
CN103073065B (en) | Alpha-Fe2O3 nanometer sphere preparation method | |
CN105060351B (en) | Flower-like cobaltosic oxide material composed of nanoparticles and preparation method thereof | |
CN102674898B (en) | Cerium oxide/ aluminium oxide micro-nanostructure ceramic pigment and preparation method thereof | |
Jing et al. | Solvothermal synthesis of morphology controllable CoCO3 and their conversion to Co3O4 for catalytic application | |
CN109264787B (en) | ZnFe2O4Preparation method of cubic block structure and obtained product | |
CN102531015A (en) | Method for preparing porous aluminum oxide superfine powder | |
CN101804318A (en) | Preparation of lanthanum doping cerium dioxide porous microspheres and application thereof to Cr<6+> removal | |
CN106811832A (en) | A kind of pearl-decorated curtain shape BiFeO3The preparation method and products obtained therefrom of micro nanometer fiber | |
CN103435097B (en) | Preparation method and application of nano zirconia | |
CN106882845A (en) | A kind of mesoporous sea urchin shape NiCo2O4The preparation method of meter Sized Materials | |
CN104528803A (en) | Preparation method of ZnO flaky porous nanometer material | |
Zou et al. | Ultrasound-assisted synthesis of CuO nanostructures templated by cotton fibers | |
CN105206816B (en) | A kind of preparation method of nickel sulfide graphene nanocomposite material | |
CN102502849A (en) | Method for preparing Mn3O4 and composite nano material thereof by using manganous salt as raw material | |
CN105731518A (en) | Octahedron cuprous oxide crystal and normal-temperature crystallization preparation method thereof | |
CN106186045A (en) | A kind of preparation method of flower shape zinc oxide nano-particle cluster | |
CN102962470A (en) | Method for preparing spherical ultrafine nickel powder at room temperature | |
CN104466166A (en) | Preparation method of nickel-manganese spinel high-voltage positive material of lithium secondary battery | |
CN104326500B (en) | A kind of preparation method of fluffy state nano yttrium oxide powder | |
CN103920873B (en) | Be coated with the preparation method of the compound nano nickel particles of inertia shell |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150722 Termination date: 20180128 |