CN103757748A - Preparation of tubular zinc stannate (ZnSnO3) material by using electrostatic spinning process - Google Patents
Preparation of tubular zinc stannate (ZnSnO3) material by using electrostatic spinning process Download PDFInfo
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- CN103757748A CN103757748A CN201310414741.XA CN201310414741A CN103757748A CN 103757748 A CN103757748 A CN 103757748A CN 201310414741 A CN201310414741 A CN 201310414741A CN 103757748 A CN103757748 A CN 103757748A
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Abstract
The present invention relates to preparation of a tubular ZnSnO3 material by using an electrostatic spinning process, and belongs to the technical field of composite metal chloride material preparation processes. According to the present invention, zinc nitrate and tin tetrachloride are adopted as precursors and polyvinylpyrrolidone is adopted as a fiber template to prepare an electrospinning solution, and electrostatic spinning and a heat treatment process are performed to prepare ZnSnO3; the method has characteristics of simple device, easy operation, moderate heat treatment temperature and short thermal insulation time; preliminary study results show that: the ZnSnO3 sample prepared by using the method presents the micron-scale thin tube shape, the length is 3-7 mum, and the diameter is 1-2 mum; and the material is expected to be used in the fields of photocatalysis, sensor manufacturing and the like.
Description
Technical field
The present invention relates to utilize electrostatic spinning process to prepare tubulose zinc stannate (ZnSnO
3) material, belong to composite metal chloride material preparation process technical field.
Background technology
ZnSnO
3be a kind of N-shaped composite oxide of metal semiconductor, can be used as the quick material of wine, there is the features such as highly sensitive, cost is low and the life-span is long.Method of electrostatic spinning is a kind of simple, cheap technology.Utilize electrostatic spinning process, can prepare low cost, high-quality micron and nano-fiber material, under the condition such as low in heat treatment temperature, temperature retention time is short, can prepare and there is d
10the metal oxide materials of electron configuration.Primary Study is found, is utilized the standby ZnSnO of this legal system
3sample has micron order tubule macroscopic features, and length is between 3-7 μ m, and diameter is between 1-2 μ m.This kind of material is expected to be applied to the fields such as photocatalysis, sensor manufacture.
Summary of the invention
The present invention aims to provide that a kind of to take zinc nitrate hexahydrate and Tin tetrachloride pentahydrate be presoma, take polyvinylpyrrolidone as stay in place form, utilizes method of electrostatic spinning to prepare tubulose ZnSnO
3the method of material.Its preparation process and step are as described below:
A. the preparation of electrospinning liquid
(1) take 1.2818 g zinc nitrate hexahydrate Zn (NO
3)
26H
2o and 1.5106 g Tin tetrachloride pentahydrate SnCl
45H
2o, puts into 100 ml beakers, adds successively 10 ml ethanol and 10 ml acetylacetone,2,4-pentanediones, is stirred to dissolving; Be precursor solution;
(2) take 1.2 g polyvinylpyrrolidones (K90), under lasting stirring, slowly pour in above-mentioned precursor solution in batches.Beaker is put into baking oven, in 83 ℃ of heating, every half an hour, take out, stir 5 min, then put back to.Repeat this step, until decorating film all dissolves, stop heat treatment, take out standing; This is electrolyte, standby;
B. tubulose ZnSnO
3preparation
(1) pipette the above-mentioned electrospinning liquid of 20 ml in syringe, syringe is fixed on computer micro-injection pump; Choose the propelling speed of 0.5 ml/h, at the uniform velocity promoting dispersion liquid is that electrolyte arrives spinning-nozzle through polytetrafluoroethylene (PTFE) tubule;
(2) nozzle is set as to 15 cm with collecting aluminium foil distance, regulating high-voltage power voltage is 10 kV; Spray silk temperature is 25 ℃, and nozzle inside diameter is 1mm; Carry out electrospinning spray silk; After spinning process finishes, spinning was dried and is processed through 4 hours in vacuum desiccator;
(3) will be dried spinning and put into a crucible, then the speed with 3 ° of C/min heats up in Muffle furnace; Rise to 650 ° of C in air atmosphere after, be incubated 2 hours, naturally cool to room temperature, obtain tubulose ZnSnO
3material.
The ZnSnO that utilizes above-mentioned technique to prepare
3material has following pattern and topological characteristic:
ZnSnO
3nanofiber length is between 5-10 μ m, and diameter is 1 μ m left and right.
Accompanying drawing explanation
Fig. 1 is ZnSnO
3scanning electronic microscope (SEM) photo.
Fig. 2 is ZnSnO
3scanning electronic microscope (SEM) photo.
Fig. 3 is ZnSnO
3x-ray diffraction (XRD) collection of illustrative plates.
The specific embodiment
After now instantiation of the present invention being specified in.
Embodiment
the present embodiment is prepared ZnSnO
3
process and the step of nanofiber are as described below:
Take 1.2818 g zinc nitrate hexahydrate Zn (NO
3)
26H
2o and 1.5106 g Tin tetrachloride pentahydrate SnCl
45H
2o, puts into 100 ml beakers, adds successively 10 ml ethanol and 10 ml acetylacetone,2,4-pentanediones, is stirred to dissolving; Take 1.2 g polyvinylpyrrolidones (K90), under lasting stirring, slowly pour in above-mentioned precursor solution in batches.Beaker is put into baking oven, in 83 ℃ of heating, every half an hour, take out, stir 5 min, then put back to.Repeat this step, until decorating film all dissolves, stop heat treatment, take out standing.This is electrolyte, standby;
Pipette the above-mentioned electrospinning liquid of 20 ml in syringe; Syringe is fixed on computer micro-injection pump; Choose the propelling speed of 0.5 ml/h, at the uniform velocity promoting dispersion liquid is that electrolyte arrives spinning-nozzle through polytetrafluoroethylene (PTFE) tubule; Nozzle is set as to 15 cm with collecting aluminium foil distance, and regulating high-voltage power voltage is 10 kV; Spray silk temperature is 25 ℃, and nozzle inside diameter is 1mm; Carry out electrospinning spray silk; After spinning process finishes, spinning was dried and is processed through 4 hours in vacuum desiccator.To be dried spinning and put into a crucible, then the speed with 3 ° of C/min heats up in Muffle furnace; Rise to 650 ° of C in air atmosphere after, be incubated 2 hours, naturally cool to room temperature; Obtain tubulose ZnSnO
3material.
Test result is shown by following accompanying drawing:
Fig. 1 and Fig. 2 are ZnSnO
3sample SEM photo.Can find out ZnSnO
3sample presents micron order " tubule " dispersing character, and every tubule is piled up and formed by nanoscale " sheet " solid again, and tubule length and thickness are uneven respectively, and length is between 3-7 μ m, and diameter is being between 1-2 μ m.
Fig. 3 is ZnSnO
3sample X-ray diffraction (XRD) collection of illustrative plates.In 2 θ=32.053 °, 33.928 °, 52.078 ° of crystal face diffraction of locating, corresponding to ZnSnO
3tetragonal system (104), (110), (116) crystal face.The ZnSnO that utilizes method of electrostatic spinning to prepare is described
3there is higher degree, formed the ZnSnO with perovskite structure
3crystalline phase.
Claims (1)
1. one kind is utilized electrostatic spinning process to prepare tubulose ZnSnO
3material, is characterized in that having following preparation process and step:
A. the preparation of electrospinning liquid
(1) take 1.2818 g zinc nitrate hexahydrate Zn (NO
3)
26H
2o and 1.5106 g Tin tetrachloride pentahydrate SnCl
45H
2o, puts into 100 ml beakers, adds successively 10 ml ethanol and 10 ml acetylacetone,2,4-pentanediones, is stirred to dissolving; Be precursor liquid solution;
(2) take 1.2 g polyvinylpyrrolidones (K90), continuing, under stirring, slowly to pour in batches in above-mentioned precursor solution; Beaker is put into baking oven, in 83 ℃ of heating, every half an hour, take out, stir 5 min, then put back to; Repeat this step, until decorating film all dissolves, stop heat treatment, take out standing; This is electrolyte, standby;
B. tubulose ZnSnO
3preparation
(1) pipette the above-mentioned electrospinning liquid of 20 ml in syringe, syringe is fixed on computer micro-injection pump; Choose the propelling speed of 0.5 ml/h, at the uniform velocity promoting dispersion liquid is that electrolyte arrives spinning-nozzle through polytetrafluoroethylene (PTFE) tubule;
(2) nozzle is set as to 15 cm with collecting aluminium foil distance, regulating high-voltage power voltage is 10 kV; Spray silk temperature is 25 ℃, and nozzle inside diameter is 1mm; Carry out electrospinning spray silk; After spinning process finishes, spinning was dried and is processed through 4 hours in vacuum desiccator;
(3) will be dried spinning and put into a crucible, then the speed with 3 ° of C/min heats up in Muffle furnace; Rise to 650 ° of C in air atmosphere after, be incubated 2 hours, naturally cool to room temperature, obtain tubulose ZnSnO
3material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310414741.XA CN103757748A (en) | 2013-09-12 | 2013-09-12 | Preparation of tubular zinc stannate (ZnSnO3) material by using electrostatic spinning process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310414741.XA CN103757748A (en) | 2013-09-12 | 2013-09-12 | Preparation of tubular zinc stannate (ZnSnO3) material by using electrostatic spinning process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103757748A true CN103757748A (en) | 2014-04-30 |
Family
ID=50525058
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044843A (en) * | 2016-06-02 | 2016-10-26 | 景德镇学院 | Preparing method of porous zinc metastannate nanosheet |
| CN110865099A (en) * | 2019-12-02 | 2020-03-06 | 陕西师范大学 | ZnO-SnO2-Zn2SnO4Preparation method and application of porous nanofiber gas-sensitive material |
| CN113337900A (en) * | 2021-06-02 | 2021-09-03 | 西安交通大学 | Photocatalytic fabric and preparation method and application thereof |
| CN117696045A (en) * | 2024-02-05 | 2024-03-15 | 浙江师范大学杭州校区 | S-type heterojunction catalyst with high-efficiency photocatalysis and piezocatalysis as well as preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126745A (en) * | 2011-01-24 | 2011-07-20 | 济南大学 | Nano zinc metastannate air-sensitive material with hollow fiber structure and preparation method thereof |
| KR20120102840A (en) * | 2011-03-09 | 2012-09-19 | 한국과학기술원 | Gas sensors using metal oxide tube of multilayered structures and it's fabrication method |
| CN102733000A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院过程工程研究所 | Preparation method for hollow polymer nanofibers |
| KR20120124673A (en) * | 2011-05-04 | 2012-11-14 | 한국과학기술원 | Porous zinc stannate nanofibers, fabrication method for the same, and gas sensors using the same |
-
2013
- 2013-09-12 CN CN201310414741.XA patent/CN103757748A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126745A (en) * | 2011-01-24 | 2011-07-20 | 济南大学 | Nano zinc metastannate air-sensitive material with hollow fiber structure and preparation method thereof |
| KR20120102840A (en) * | 2011-03-09 | 2012-09-19 | 한국과학기술원 | Gas sensors using metal oxide tube of multilayered structures and it's fabrication method |
| KR20120124673A (en) * | 2011-05-04 | 2012-11-14 | 한국과학기술원 | Porous zinc stannate nanofibers, fabrication method for the same, and gas sensors using the same |
| CN102733000A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院过程工程研究所 | Preparation method for hollow polymer nanofibers |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044843A (en) * | 2016-06-02 | 2016-10-26 | 景德镇学院 | Preparing method of porous zinc metastannate nanosheet |
| CN106044843B (en) * | 2016-06-02 | 2017-06-23 | 景德镇学院 | The preparation method of porous zinc metastannate nanometer sheet |
| CN110865099A (en) * | 2019-12-02 | 2020-03-06 | 陕西师范大学 | ZnO-SnO2-Zn2SnO4Preparation method and application of porous nanofiber gas-sensitive material |
| CN113337900A (en) * | 2021-06-02 | 2021-09-03 | 西安交通大学 | Photocatalytic fabric and preparation method and application thereof |
| CN113337900B (en) * | 2021-06-02 | 2023-05-26 | 西安交通大学 | Photocatalytic fabric and preparation method and application thereof |
| CN117696045A (en) * | 2024-02-05 | 2024-03-15 | 浙江师范大学杭州校区 | S-type heterojunction catalyst with high-efficiency photocatalysis and piezocatalysis as well as preparation method and application thereof |
| CN117696045B (en) * | 2024-02-05 | 2024-04-12 | 浙江师范大学杭州校区 | S-type heterojunction catalyst with high-efficiency photocatalysis and piezocatalysis as well as preparation method and application thereof |
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Application publication date: 20140430 |