CN105967225B - A kind of stannic oxide nanometer flower and preparation method thereof - Google Patents
A kind of stannic oxide nanometer flower and preparation method thereof Download PDFInfo
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- CN105967225B CN105967225B CN201610314087.9A CN201610314087A CN105967225B CN 105967225 B CN105967225 B CN 105967225B CN 201610314087 A CN201610314087 A CN 201610314087A CN 105967225 B CN105967225 B CN 105967225B
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- stannic oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- 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
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- 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
Abstract
The present invention relates to a kind of tin oxide nano flower and preparation method thereof.The stannic oxide nanometer flower is made up of nanometer sheet, and between 10 nanometers ~ 20 nanometers, multi-disc stannic oxide nanometer piece stacks monolithic lamellar spacing in the same direction, forms a kind of multilayer, orderly stacked body.The nano flower is graded structure, and monodispersity and crystallinity are good, and specific surface area is big.Its specific preparation method is as follows：Tin salt or pink salt are dissolved in stirring and dissolving in deionized water, then add alkali lye, after stirring, the stannic oxide nanometer that multilevel hierarchy is obtained by a step hydro-thermal process is spent.The preparation method technique and simple flow, Parameter adjustable scope is wide, and repeatability is strong, and cost is low, and process is environmentally safe without using toxic organic solvents, is a kind of preparation method for possessing commercial promise.Prepared stannic oxide nanometer flower has higher application value in fields such as dusty gas detection, energy storage, new energy preparations.
Description
Technical field
The present invention relates to a kind of stannic oxide nanometer flower and preparation method thereof, particularly a kind of tin ash stacked in the same direction
Nano flower, belong to inorganic nano material and synthesis technical field.
Background technology
In modern society's life, around miscellaneous gas around the mankind, some are needed by human, such as oxygen
Deng, but also have some be harmful pollution environment gas, such as NOx、SOxDeng.Detection to these pernicious gases,
Not only the health of human body, the also sound development to entire society are had great significance.Therefore, high performance gas is developed to pass
Sensor electronic component, which just seems detecting various gas componants, to be even more important.
At present, metal oxide semiconductor nano material（Such as ZnO, SnO2、TiO2Deng）, it is widely used in sensing, urges
The fields such as change, photoelectricity, energy storage.Wherein, tin ash SnO2It is a kind of important n-type semiconductor transition metal oxide material
Material, there is wider energy gap, higher vapor sensitivity, preferable optical property, and its chemical stability is good, corrosion-resistant
Property is strong, to gas absorption desorption time section and high sensitivity, the advantages that absorptivity in visible-range is almost nil and it is standby
Paid close attention to by scientists, and can be widely applied to lithium ion battery, ultracapacitor, sensor and be used as the side such as catalyst
Face.But for how to improve ZnO sensitivity, it is selective the problems such as, need further to study.
In recent years, having focused on for research is prepared the metal oxygen with different crystal morphology by more research workers
In compound.At present, tin ash SnO is prepared2Method mainly have：Hydro-thermal method, coprecipitation, vapour deposition process etc..Vapor phase method
The equipment of costliness is needed, thus cost is higher.And synthesis has the nanocrystalline of controllable appearance and structure, based on pattern and knot
The change of structure makes nano material be improved in the performance of numerous application fields, and is the basic challenge in nanoscale science and technology field.
The present invention is prepared for the stannic oxide nanometer flower gas sensing materials of multilevel hierarchy using one step hydro thermal method, obtains new structure shape
Looks, there is technology and the novelty and creativeness of application.
The content of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of stannic oxide nanometer flower and preparation method thereof.
A kind of stannic oxide nanometer flower, it is characterised in that nano flower is made up of nanometer sheet, and monolithic lamellar spacing is 10-20
Nanometer, multi-disc stannic oxide nanometer flower are stacked along same specific direction, form a kind of multilayer, orderly stacked body.
A kind of preparation method of stannic oxide nanometer flower, it is characterised in that comprise the following steps：
（1）Tin salt or pink salt are dissolved in deionized water, stirring to dissolve, solution concentration be 0.008-0.02 moles/
Rise；
（2）Aqueous slkali is added drop-wise in the aqueous solution dissolved with tin salt, is stirred when being added dropwise, forms uniform suspension；
（3）Then suspension is carried out to hydro-thermal reaction processing 10-16 in autoclave small at a temperature of 373-473K
When, after stopping reaction, precipitated product will be obtained using the method for filtering or centrifugation, be then washed with deionized, after drying
Obtained object.
Step（1）Described in water-soluble tin salt be anhydrous or with the crystallization water stannous chloride, stannous oxalate
Or one kind in butter of tin, and concentration is and concentration is 0.008-0.02 mol/Ls.
Step（2）Described in the aqueous slkali that adds, alkali source is one kind in sodium hydroxide NaOH or potassium hydroxide KOH.
Step（2）Described in the alkali lye that adds, measured according to the ratio between amount of substance of hydroxide ion and tin ion, should
Ratio is 4 ~ 6:1.
Step（3）Described in drying means for constant pressure and dry, vacuum drying or spray drying etc..
The tin ash obtained by above-mentioned preparation method is SnO2Type, its crystal formation and standard powder diffraction card
(JCPDS:73-1126) match.Pattern is square nanometer sheet, monolithic lamellar spacing between 10 nanometers -100 nanometers,
It is long and wide between 1 micron -20 microns.Multi-disc stannic oxide nanometer flower is stacked along the vertical direction of lamella, forms one
Kind multilayer, square ordered stacks body.The product pollution control, environmental protection, hygiene medical treatment, new energy prepare etc. field all
With very high potential using value.The preparation method technique and simple flow, Parameter adjustable scope is wide, and repeatability is strong, into
This is low, and process is environmentally safe without using toxic organic solvents, is a kind of preparation method for possessing commercial promise.It is prepared
Stannic oxide nanometer flower dusty gas detection, energy storage, new energy prepare etc. field have higher application value.
Brief description of the drawings
Fig. 1：The stereoscan photograph that the stannic oxide nanometer as made from embodiment 2 is spent.
Embodiment
Below by embodiment, the present invention is further elaborated, and its purpose, which is only that, is best understood from present disclosure.
Therefore, the cited case is not intended to limit protection scope of the present invention.
Embodiment 1：
（1）Configuration concentration is the butter of tin SnCl of 0.017 mol/L4Solution；
（2）Certain density potassium hydroxide solution is configured, wherein the amount of material hydroxy:The amount of the material of tin ion=
4:1；
（3）In whipping process, potassium hydroxide solution is added in butter of tin solution, and continues to stir 30 min, shape
Into uniform suspension；
（4）Suspension is put into the stainless steel autoclave of teflon lined, it is small that 10 are reacted at a temperature of 423K
When.Precipitated product is washed with deionized after terminating for reaction, is then dried in vacuo under 323K, obtains stannic oxide nanometer
Flower.
Embodiment 2：
（1）Configuration concentration is the stannous chloride SnCl of 0.008 mol/L2Solution；
（2）Certain density sodium hydroxide solution is configured, wherein the amount of material hydroxy:The amount of the material of tin ion=
4:1；
（3）In whipping process, sodium hydroxide solution is added in stannous chloride solution, and continues to stir 30 min, shape
Into uniform suspension；
（4）Suspension is put into the stainless steel autoclave of teflon lined, it is small that 16 are reacted at a temperature of 393K
When.Precipitated product is washed with deionized after terminating for reaction, and then the constant pressure and dry under 343K, obtains stannic oxide nanometer
Flower.
Obtained stannic oxide nanometer flower is made up of nanometer sheet, about 20 nanometers of monolithic lamellar spacing, multi-disc tin ash
Nano flower is stacked along the vertical direction of lamella, forms a kind of multilayer, orderly stacked body.
Embodiment 3：
（1）Configuration concentration is the stannous chloride SnCl of 0.02 mol/L2Solution；
（2）Certain density sodium hydroxide solution is configured, wherein the amount of material hydroxy:The amount of the material of tin ion=
5:1；
（3）In whipping process, sodium hydroxide solution is added in stannous chloride solution, and continues to stir 30 min, shape
Into uniform suspension；
（4）Suspension is put into the stainless steel autoclave of teflon lined, is reacted 16 hours at a temperature of 403K.
Precipitated product is washed with deionized after terminating for reaction, then the constant pressure and dry under 353K, obtains stannic oxide nanometer flower.
Embodiment 4：
（1）Configuration concentration is the stannous oxalate solution of 0.008 mol/L；
（2）Certain density potassium hydroxide solution is configured, wherein the amount of material hydroxy:The amount of the material of tin ion=
6:1；
（3）In whipping process, potassium hydroxide solution is added in stannous oxalate solution, and continues to stir 30 min, shape
Into uniform suspension；
（4）Suspension is put into the stainless steel autoclave of teflon lined, it is small that 12 are reacted at a temperature of 473K
When.Precipitated product is washed with deionized after terminating for reaction, is then dried in vacuo under 333K, obtains stannic oxide nanometer
Flower.
Embodiment 5：
（1）Configuration concentration is the stannous oxalate solution of 0.02 mol/L；
（2）Certain density potassium hydroxide solution is configured, wherein the amount of material hydroxy:The amount of the material of tin ion=
6:1；
（3）In whipping process, potassium hydroxide solution is added in stannous oxalate solution, and continues to stir 30 min, shape
Into uniform suspension；
（4）Suspension is put into the stainless steel autoclave of teflon lined, it is small that 16 are reacted at a temperature of 373K
When.Precipitated product is washed with deionized after terminating for reaction, is then dried in vacuo under 323K, obtains stannic oxide nanometer
Flower.
Embodiment 6：
（1）Configuration concentration is the stannous chloride SnCl of 0.008 mol/L2Solution；
（2）Certain density potassium hydroxide solution is configured, wherein the amount of material hydroxy:The amount of the material of tin ion=
6:1；
（3）In whipping process, potassium hydroxide solution is added in stannous oxalate solution, and continues to stir 30 min, shape
Into uniform suspension；
（4）Suspension is put into the stainless steel autoclave of teflon lined, it is small that 8 are reacted at a temperature of 453K
When.Precipitated product is washed with deionized after terminating for reaction, and then the constant pressure and dry under 353K, obtains stannic oxide nanometer
Flower.
Embodiment 7：
（1）Configuration concentration is the stannic chloride SnCl of 0.02 mol/L4Solution；
（2）Certain density potassium hydroxide solution is configured, wherein the amount of material hydroxy:The amount of the material of tin ion=
5:1；
（3）In whipping process, potassium hydroxide solution is added in butter of tin solution, and continues to stir 30 min, shape
Into uniform suspension；
（4）Suspension is put into the stainless steel autoclave of teflon lined, it is small that 12 are reacted at a temperature of 393K
When.Precipitated product is washed with deionized after terminating for reaction, then by spray drying, obtains stannic oxide nanometer flower.
Claims (3)
1. a kind of preparation method of stannic oxide nanometer flower, it is characterised in that comprise the following steps：
（1）Tin salt or pink salt are dissolved in deionized water, to dissolving, solution concentration is 0.008-0.02 mol/Ls for stirring；
（2）Aqueous slkali is added drop-wise to dissolved with the aqueous solution of tin salt or pink salt, stirred when being added dropwise, forms uniform suspend
Liquid；
（3）Then suspension is subjected to hydro-thermal reaction processing 10-16 hours in autoclave at a temperature of 373-473K, stopped
After only reacting, precipitated product will be obtained using the method for filtering or centrifugation, be then washed with deionized, obtain after drying
Object；
Step（1）Described in tin salt or pink salt be anhydrous or with the crystallization water stannous chloride, stannous oxalate or four chlorinations
One kind in tin, and concentration is 0.008-0.02 mol/Ls；
Step（2）The aqueous slkali of middle addition, measured according to the ratio between amount of material of hydroxide ion and tin ion, the ratio
For 4-6:1.
A kind of 2. preparation method of stannic oxide nanometer flower according to claim 1, it is characterised in that step（2）In plus
The aqueous slkali entered, alkali source are one kind in sodium hydroxide NaOH or potassium hydroxide KOH.
A kind of 3. preparation method of stannic oxide nanometer flower according to claim 1, it is characterised in that step（3）Middle institute
The drying stated is constant pressure and dry, vacuum drying or spray drying.
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179491B (en) * | 2018-11-09 | 2021-02-26 | 五邑大学 | SnO capable of growing rapidly2Method of nanosheet |
| CN109879307B (en) * | 2019-03-18 | 2021-01-19 | 武汉理工大学 | Mesoporous SnO in perovskite solar cell2Preparation method of (1) |
| CN113860360A (en) * | 2021-11-17 | 2021-12-31 | 云南锡业锡化工材料有限责任公司 | Preparation method of nano flower-ball-shaped tin dioxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823703A (en) * | 2009-03-06 | 2010-09-08 | 中国科学院宁波材料技术与工程研究所 | Controllable preparation method for petaliform tin oxide nano powder |
| CN102942215A (en) * | 2012-09-10 | 2013-02-27 | 重庆大学 | Three-dimensional SnO2 nano flower-like material grown on titanium substrate and preparation method thereof |
| CN103101967A (en) * | 2011-11-14 | 2013-05-15 | 南开大学 | Preparation method three-dimensional multistage SnO2 nanoflowers |
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2016
- 2016-05-13 CN CN201610314087.9A patent/CN105967225B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823703A (en) * | 2009-03-06 | 2010-09-08 | 中国科学院宁波材料技术与工程研究所 | Controllable preparation method for petaliform tin oxide nano powder |
| CN103101967A (en) * | 2011-11-14 | 2013-05-15 | 南开大学 | Preparation method three-dimensional multistage SnO2 nanoflowers |
| CN102942215A (en) * | 2012-09-10 | 2013-02-27 | 重庆大学 | Three-dimensional SnO2 nano flower-like material grown on titanium substrate and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Hydrothermal synthesis and characterization of novel flower-like zinc-doped SnO2 nanocrystals;Zirong Li et al.;《Journal of Crystal Growth》;20030419;第291卷;第258-261页 * |
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