CN107445195A - A kind of preparation method of zine stannate nano cube or nanometer sheet material - Google Patents
A kind of preparation method of zine stannate nano cube or nanometer sheet material Download PDFInfo
- Publication number
- CN107445195A CN107445195A CN201710783924.7A CN201710783924A CN107445195A CN 107445195 A CN107445195 A CN 107445195A CN 201710783924 A CN201710783924 A CN 201710783924A CN 107445195 A CN107445195 A CN 107445195A
- Authority
- CN
- China
- Prior art keywords
- preparation
- zinc
- sheet material
- nanometer sheet
- ion salt
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to technical field of nano material, and in particular to a kind of preparation method of zine stannate nano cubic block or nanometer sheet material.The present invention uses the synthetic method of higher temperature hydro-thermal, directly obtains nano cubic block or the metal oxide materials of nanometer chip architecture.The present invention is additional acid source by using neopelex, tetraethylamine hydroxide is additional alkali source, the different hydro-thermal times are adjusted to regulate and control the size of cubic block, and the dosage of modulation neopelex optimizes the pattern of material, regular appearance, constitutionally stable metal oxide hierarchical structure nano material are finally obtained.The inventive method experiment condition is gently controllable, practical, and favorable reproducibility.
Description
Technical field
The invention belongs to nano composite material technical field, and in particular to a kind of new zine stannate nano cube is received
The preparation of rice sheet material.
Background technology
With developing rapidly for economic society, environmental degradation that fossil energy is triggered, lack of energy by various countries height
Degree concern, the key for alleviating energy environment issues is to find new material, by existing energy storage or pollution degradation.And
In numerous materials, zinc stannate has unique optics, electrochemistry, photoelectrochemical as a kind of important ternary semiconductor oxide
Etc. property, therefore get more and more people's extensive concerning.For example, early-stage Study finds that the material is due to high electron transfer
Rate and quick electron transfer rate, can be as the working electrode of fuel sensitization solar battery；Due to high theory
Electric capacity and reversible capacitance, can be as the anode material of lithium battery.Also, because its selectivity to gas with various is high, response
Speed is fast, can be used as gas sensor material；Due to the induction of Surface Oxygen vacant state, there is high separation of charge ability,
Photocatalytic degradation can be carried out to organic dyestuff in liquid-phase system.
On the other hand, why zinc stannate has the application of maturation in numerous areas, and not only have benefited from zinc stannate has in itself
Spinel structure, more benefit from the technique synthesis of stannic acid Zinc material.However, the synthetic method of most of stannic acid Zinc materials is all adopted
It is higher with traditional high temperature solid state reaction, energy consumption.Therefore, Research Significance of the invention is using low, the simple step that consumes energy
Hydro-thermal method, the differential responses time is adjusted, prepare pattern uniqueness, finely dispersed zine stannate nano cube.In addition, originally
Invention has also regulated and controled the dosage of surfactant, synthesizes the zinc stannate of another nanometer sheet pattern.This is zinc stannate and other materials
The preparation of material and physical property regulation and control method provide reference, the also research for zine stannate nano material on electricity, optics, magnetic performance
Experimental basis is provided with exploitation, is the basis in terms of the device in future is ready with laying material.
The content of the invention
The purpose of the present invention aims to provide a kind of preparation of simple reliable zinc stannate cube or nanometer sheet material.
To achieve the above object, the technical solution adopted by the present invention is by a certain amount of zinc acetate, butter of tin, dodecane
Base benzene sulfonic acid sodium salt, which adds, to be contained in a certain amount of water and alcohol mixeding liquid, and stirring in water bath at a certain temperature.Then, above-mentioned molten
A certain amount of tetraethylamine hydroxide is added dropwise in liquid to be well mixed, is transferred in the reactor of polytetrafluoroethylsubstrate substrate, through high-temperature water
After thermal response, product is repeatedly washed.Finally, zine stannate nano material is obtained.
A kind of preparation method of zinc stannate cube or nanometer sheet material, is comprised the following steps that：
(1) preparation of zinc stannate precursor solution：
By a certain amount of soluble zinc ion salt, tin ion salt, neopelex, water and ethanol are added to
In mixed solution, to being completely dissolved, stirring in water bath 30min~120min at 30~60 DEG C, tetraethylamine hydroxide is then added dropwise, instead
60~90min is answered, obtains zinc stannate precursor solution；
(2) preparation of zinc stannate cube or nanometer sheet：
Zinc stannate precursor solution obtained by step (1) is poured into the reactor of polytetrafluoroethylsubstrate substrate, seals, is placed in
In baking oven, hydro-thermal reaction is carried out, after reaction terminates, is cooled to room temperature, repeatedly washing, vacuum drying, produce zine stannate nano material
Material.
In step (1), the soluble zinc ion salt is any in zinc acetate, zinc nitrate or zinc chloride
In step (1), the tin ion salt is butter of tin.
In step (1), in the mixed solution of the water and ethanol, the volume ratio of water and ethanol is 1:1.
In step (1), soluble zinc ion salt, tin ion salt, neopelex and the tetraethylammonium hydroxide
The usage ratio of amine is：1mmol：0.5mmol：0~1mmol：3mL,
In step (2), the temperature of hydro-thermal reaction is 180~220 DEG C, and the time of hydro-thermal reaction is 5~8 hours.
When the addition of neopelex is：
The soluble zinc ion salt, tin ion salt, the amount ratio of neopelex and tetraethylamine hydroxide
Example be：1mmol：0.5mmol：1mmol：3mL, what is obtained is zine stannate nano cubic materials；
When the addition of neopelex is：
The soluble zinc ion salt, tin ion salt, the amount ratio of neopelex and tetraethylamine hydroxide
Example be：1mmol：0.5mmol：0mmol：3mL, what is obtained is zine stannate nano sheet material.
Component, pattern and the size of the nano material prepared using this method, are respectively adopted X-ray diffraction analysis figure
(XRD) characterized with ESEM (SEM).
Beneficial effects of the present invention are：
The present invention proposes a kind of preparation method of stannic acid Zinc material, and the pattern of material is cube or nanometer sheet, the material
Expect that pattern uniqueness is regular, materials wide material sources are cheap.
Present invention process is simple, favorable reproducibility, cheap, meets environment-friendly requirement, is easy to produce in batches.
Brief description of the drawings
Fig. 1 is the X-ray diffraction analysis figure (XRD) of the gained zine stannate nano material of the embodiment of the present invention 1,2,3；
Fig. 2 is the cubical scanning electron microscope (SEM) photograph of gained zinc stannate (SEM) of the embodiment of the present invention 1；
Fig. 3 is the cubical scanning electron microscope (SEM) photograph of gained large scale zinc stannate (SEM) of the embodiment of the present invention 2；
Fig. 4 is the scanning electron microscope (SEM) photograph (SEM) of the gained zine stannate nano piece of the embodiment of the present invention 3.
Embodiment
The present invention is expanded on further below by example, but protection scope of the present invention is not limited to these examples.This
Raw material in invention example is purchased from Shanghai Chinese medicines group, is that analysis is pure.
Embodiment 1
1mmoL zinc acetates, 0.5mmoL butters of tin and 1mmoL neopelexes are added containing 15mL water and
In the 50mL conical flasks of 15mL alcohol mixeding liquids, and the stirring in water bath 120min at 30 DEG C.Then, it is added dropwise in above-mentioned solution
3mL tetraethylamine hydroxide, 90min is reacted, it is stand-by.Above-mentioned zinc stannate precursor solution is poured into 50mL polytetrafluoroethylsubstrate substrates
Reactor in, sealing, be placed in baking oven, control baking oven temperature be 180 DEG C, react 5 hours, be cooled to room temperature, repeatedly wash
Wash, be dried in vacuo, produce zinc stannate cube.Each diffraction maximum position and relative intensity are cubical with zinc stannate in Fig. 1
JPCDS cards (24-1470) match, and show that product zinc stannate has highly crystalline.The stannic acid prepared as can be seen from Figure 2
Zinc cube is uniformly dispersed, regular appearance, and cubical average rib is about 650nm.
Embodiment 2
1mmoL zinc nitrates, 0.5mmoL butters of tin and 1mmoL neopelexes are added containing 15mL water and
In the 50mL conical flasks of 15mL alcohol mixeding liquids, and the stirring in water bath 30min at 60 DEG C.Then, 3mL is added dropwise in above-mentioned solution
Tetraethylamine hydroxide, react 1h, it is stand-by.Above-mentioned zinc stannate precursor solution is poured into the reaction of 50mL polytetrafluoroethylsubstrate substrates
In kettle, sealing, it is placed in baking oven, the temperature for controlling baking oven is 220 DEG C, reacts 8 hours, is cooled to room temperature, repeatedly washing, vacuum
Dry, produce large-sized zinc stannate cube.Each diffraction maximum position and relative intensity are cubical with zinc stannate in Fig. 1
JPCDS cards (24-1470) match, and show that product zinc stannate has highly crystalline.From figure 3, it can be seen that with reaction
The extension of time, cubic block little by little grow, and prepare large-sized zinc stannate cube and are uniformly dispersed, regular appearance, cube
The rib of body is about 2.5 μm.
Embodiment 3
1mmoL zinc chloride, 0.5mmoL butters of tin and 0mmoL neopelexes are added containing 15mL water and
In the 50mL conical flasks of 15mL alcohol mixeding liquids, and the stirring in water bath 30min at 60 DEG C.Then, 3mL is added dropwise in above-mentioned solution
Tetraethylamine hydroxide, react 1h, it is stand-by.Above-mentioned zinc stannate precursor solution is poured into the reaction of 50mL polytetrafluoroethylsubstrate substrates
In kettle, sealing, it is placed in baking oven, the temperature for controlling baking oven is 220 DEG C, reacts 8 hours, is cooled to room temperature, repeatedly washing, vacuum
Dry, produce zine stannate nano piece.
JPCDS cards (24-1470) kissing of each diffraction maximum position and relative intensity with zine stannate nano piece in Fig. 1
Close, show that product zinc stannate has highly crystalline.From fig. 4, it can be seen that when other reaction conditions keep constant, structure directing
When agent neopelex is not added to reaction, it is nano-sheet to prepare zinc stannate pattern, and the size of nanometer sheet is about
1.5~2 μm.
Description to examples detailed above is understood that for ease of those skilled in the art and using the present invention.It is ripe
Know the personnel of art technology obviously can easily make various modifications to these examples, and General Principle described herein
It is applied in other examples without by performing creative labour.Therefore, the invention is not restricted to example here, art technology
For personnel according to the announcement of the present invention, the improvement made for the present invention and modification all should be within protection scope of the present invention.
Claims (7)
1. the preparation method of a kind of zine stannate nano cubic block or nanometer sheet material, it is characterised in that comprise the following steps：
(1) preparation of zinc stannate precursor solution：
By a certain amount of soluble zinc ion salt, tin ion salt, neopelex, the mixing of water and ethanol is added to
In solution, to being completely dissolved, stirring in water bath 30min~120min at 30~60 DEG C, tetraethylamine hydroxide, reaction 60 is then added dropwise
~90min, obtain zinc stannate precursor solution；
(2) preparation of zinc stannate cube or nanometer sheet：
Zinc stannate precursor solution obtained by step (1) is poured into the reactor of polytetrafluoroethylsubstrate substrate, seals, is placed in baking oven
In, hydro-thermal reaction is carried out, after reaction terminates, is cooled to room temperature, repeatedly washing, vacuum drying, produce zine stannate nano material.
2. the preparation method of a kind of zine stannate nano cubic block according to claim 1 or nanometer sheet material, its feature exist
In in step (1), the soluble zinc ion salt is any in zinc acetate, zinc nitrate or zinc chloride.
3. the preparation method of a kind of zine stannate nano cubic block according to claim 1 or nanometer sheet material, its feature exist
In in step (1), the tin ion salt is butter of tin.
4. the preparation method of a kind of zine stannate nano cubic block according to claim 1 or nanometer sheet material, its feature exist
In in step (1), in the mixed solution of the water and ethanol, the volume ratio of water and ethanol is 1:1.
5. the preparation method of a kind of zine stannate nano cubic block according to claim 1 or nanometer sheet material, its feature exist
In, in step (1), the soluble zinc ion salt, tin ion salt, the use of neopelex and tetraethylamine hydroxide
Amount ratio is：1mmol：0.5mmol：0~1mmol：3mL.
6. the preparation method of a kind of zine stannate nano cubic block according to claim 1 or nanometer sheet material, its feature exist
In in step (2), the temperature of hydro-thermal reaction is 180~220 DEG C, and the time of hydro-thermal reaction is 5~8 hours.
7. a kind of zine stannate nano cubic block or nanometer sheet material, it is characterised in that be by any one of claim 1~6 institute
State made from preparation method,
When the addition of neopelex is：
The soluble zinc ion salt, tin ion salt, the usage ratio of neopelex and tetraethylamine hydroxide are：
1mmol：0.5mmol：1mmol：3mL, what is obtained is zine stannate nano cubic materials；
When the addition of neopelex is：
The soluble zinc ion salt, tin ion salt, the usage ratio of neopelex and tetraethylamine hydroxide are：
1mmol：0.5mmol：0mmol：3mL, now, what is obtained is zine stannate nano sheet material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710783924.7A CN107445195A (en) | 2017-09-04 | 2017-09-04 | A kind of preparation method of zine stannate nano cube or nanometer sheet material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710783924.7A CN107445195A (en) | 2017-09-04 | 2017-09-04 | A kind of preparation method of zine stannate nano cube or nanometer sheet material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107445195A true CN107445195A (en) | 2017-12-08 |
Family
ID=60493554
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710783924.7A Pending CN107445195A (en) | 2017-09-04 | 2017-09-04 | A kind of preparation method of zine stannate nano cube or nanometer sheet material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107445195A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678198A (en) * | 2018-12-17 | 2019-04-26 | 天津理工大学 | A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film |
| CN110887871A (en) * | 2019-11-27 | 2020-03-17 | 哈尔滨师范大学 | Oxygen-enriched defect zinc stannate material, synthesis method thereof and hydrogen sulfide early warning sensor |
| CN113731395A (en) * | 2021-09-28 | 2021-12-03 | 杭州师范大学 | Zinc stannate photocatalyst rich in oxygen vacancies, preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105405656A (en) * | 2015-11-30 | 2016-03-16 | 福州大学 | Hierarchical structure Zn<2>SnO<4> and application thereof |
| CN106512978A (en) * | 2016-11-29 | 2017-03-22 | 洛阳理工学院 | Method for preparing visible-light response photocatalyst by utilizing nano Zn2SnO4 |
-
2017
- 2017-09-04 CN CN201710783924.7A patent/CN107445195A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105405656A (en) * | 2015-11-30 | 2016-03-16 | 福州大学 | Hierarchical structure Zn<2>SnO<4> and application thereof |
| CN106512978A (en) * | 2016-11-29 | 2017-03-22 | 洛阳理工学院 | Method for preparing visible-light response photocatalyst by utilizing nano Zn2SnO4 |
Non-Patent Citations (3)
| Title |
|---|
| QINQIN ZHAO等: "Polyhedral Zn2SnO4: Synthesis, enhanced gas sensing and photocatalytic performance", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
| YA-QI JIANG等: "Hydrothermal syntheses and gas sensing properties of cubic and quasi-cubic Zn2SnO4", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| YA-QI JIANG等: "Synthesis of Zn2SnO4 nanoplate-built hierarchical cube-like structures with enhanced gas-sensing property", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678198A (en) * | 2018-12-17 | 2019-04-26 | 天津理工大学 | A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film |
| CN110887871A (en) * | 2019-11-27 | 2020-03-17 | 哈尔滨师范大学 | Oxygen-enriched defect zinc stannate material, synthesis method thereof and hydrogen sulfide early warning sensor |
| CN113731395A (en) * | 2021-09-28 | 2021-12-03 | 杭州师范大学 | Zinc stannate photocatalyst rich in oxygen vacancies, preparation method and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107098403B (en) | NiCo2S4Nano material and preparation method thereof | |
| CN104393103B (en) | A kind of Cu2ZnSnS4The preparation method of semiconductive thin film and application thereof | |
| CN109650464A (en) | Preparation method of cobaltosic oxide nano linear array and products thereof and application | |
| CN107445195A (en) | A kind of preparation method of zine stannate nano cube or nanometer sheet material | |
| CN104588045A (en) | Ultra-thin BiOCl nano-sheet, preparation method and application thereof | |
| CN103145345B (en) | Chemical method for synthesising silver selenide semiconductor photoelectric film material in situ at room temperature | |
| CN110172711A (en) | Copper-based three-dimensional self-supporting electrocatalysis material and its preparation method and application | |
| CN102201498B (en) | Method for preparing Cu2ZnSnS4 nanocrystalline thin-film solar cell | |
| CN104016405A (en) | Flower-shaped mesoporous titanium dioxide material and preparation method and application thereof | |
| CN104785266A (en) | Preparation method of nanometer cobalt oxide/graphene composite material | |
| CN105489874A (en) | Stannic oxide nanoparticles with high electrical property and preparation method therefor | |
| CN106744728A (en) | A kind of method that room temperature liquid phase method prepares SnSe micron balls | |
| CN102659177A (en) | Method for preparing porous spherical stannous oxide nano material | |
| CN108101119A (en) | The preparation method of oxidation nanometer sheet material | |
| CN101121504A (en) | Dendritic silver selenide nano crystal thin film material and preparation method | |
| CN103474616A (en) | Sol precipitation preparation method for carbon-coated lithium iron silicate cathode material | |
| CN106542569A (en) | A kind of preparation method of flower ball-shaped tin ash | |
| CN107601441A (en) | A kind of method of hydro-thermal method synthesis stannic selenide micron crystalline flour body | |
| CN105731518B (en) | Normal-temperature crystallization preparation method of octahedron cuprous oxide crystal | |
| CN102897722B (en) | Alpha-In2Se3 nano-grade flower-ball solvothermal synthesizing method | |
| CN104979098A (en) | Counter electrode of dye-sensitized solar cell, preparation method thereof and application | |
| CN104628263A (en) | Method for preparing indium oxide octahedral nanocrystal film | |
| CN109133158A (en) | The SnS of selective oxidation2Preparation of sections method and products thereof and purposes | |
| CN102897835A (en) | Preparation method of BiVO4 | |
| CN102254701B (en) | Anodizing method capable of improving performance of titanium dioxide based dye sensitized solar cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171208 |
|
| RJ01 | Rejection of invention patent application after publication |