CN108439458B - A kind of preparation method of two dimension foliaceous nano zinc oxide material - Google Patents
A kind of preparation method of two dimension foliaceous nano zinc oxide material Download PDFInfo
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- CN108439458B CN108439458B CN201810446334.XA CN201810446334A CN108439458B CN 108439458 B CN108439458 B CN 108439458B CN 201810446334 A CN201810446334 A CN 201810446334A CN 108439458 B CN108439458 B CN 108439458B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of preparation methods of two-dimentional foliaceous nano zinc oxide material, are related to the preparation field of nano zine oxide.The present invention is sequentially added using zinc sulfate, urea and the cetyl trimethylammonium bromide of certain mass ratio and forms certain density aqueous solution in water, then it is washed and is centrifugated after reactor constant temperature reacts a period of time, and after certain temperature drying and high-temperature heat treatment, the nano oxidized zinc product of two dimension foliaceous is made.In the preparation method, primary raw material is cheap and easy to get, and simple process is easy to operate, is suitable for large-scale production；And product piece shape full-size obtained, less than 1 micron, thickness is less than 40 nanometers, and the edge of piece has broached-tooth design, and pattern is similar to leaf.Product obtained by the present invention can be used as gas sensing material tests low-concentration ethanol amine, be demonstrated by higher selectivity in ammonium hydroxide, dimethylamine, trimethylamine and diethylamine.
Description
Technical field
The present invention relates to the preparation field of nano zine oxide, specially a kind of system of two-dimentional foliaceous nano zinc oxide material
Preparation Method.
Background technique
The structure and pattern of nano material have a great impact to the performance of nano material and application.Prepare specific structure
Nano material for develop nano ZnO frontier have important academic significance and application value.It is received in numerous
In rice material, the nanostructure of zinc oxide is had received widespread attention.The zinc oxide of nanostructure is due to having compared with Large ratio surface
Long-pending and good magnetic, light, electrical property and have attracted much attention, be expected to be applied to photocatalysis, gas sensor, moisture sensor, pressure-sensitive
The various fields such as resistance, transparent electrode, have broad application prospects.
Therefore, it develops and prepares cheap, simple, the novel pattern of damage Nano-class zinc oxide preparation method with important
Scientific meaning.
Summary of the invention
The present invention provides a kind of two-dimentional foliaceous and receives to solve the problems, such as to prepare the nano zinc oxide material of novel pattern
The preparation method of rice zinc oxide material.
The present invention is achieved by the following technical solution: a kind of preparation side of two dimension foliaceous nano zinc oxide material
Method is achieved by the steps of:
(1) by the zinc sulfate solution of zinc sulfate soluble in water for obtaining 14 ~ 15g/L, then it is according to zinc sulfate mass ratio
The urea and cetyl trimethylammonium bromide of 1:0.41:0.13, urea and cetyl trimethylammonium bromide are sequentially added
In solution of zinc sulfate, stirring is made it completely dissolved, and forms mixed solution；
(2) mixed solution in step (1) is transferred in reaction kettle, in 100 DEG C ~ 140 DEG C constant temperature 4-10h；
(3) after the reaction was completed, reactant is taken out to be washed and be centrifugated；
(4) by the reactant of step (3) in 70 DEG C ~ 80 DEG C dryings, and in 380 DEG C ~ 420 DEG C heat treatment 2h, two dimension is made
The nano oxidized zinc product of foliaceous.
Using zinc sulfate as zinc source in the present invention, zinc sulfate is completely dissolved, and the solution of zinc sulfate of 14 ~ 15g/L is in two dimension
Sufficient zinc ion is provided in foliaceous nano zine oxide forming process, cetyl trimethylammonium bromide plays dispersion and limit
The effect that nanometer sheet processed is grown up, in combination with urea slow release precipitating reagent, symplastic growth is somebody's turn to do in specific reaction environment
Product.Cetyl trimethylammonium bromide plays the role of the pattern of nano zine oxide main.The zinc sulfate of 14 ~ 15g/L
Solution and urea, cetyl trimethylammonium bromide have codetermined nano oxygen according to mass ratio, preparation parameter (temperature, time)
Change the pattern of zinc.Product zinc oxide is the nanometer sheet being evenly distributed, with two-dimensional structure, and piece shape full-size is thick less than 1 micron
Degree is less than 40 nanometers, and the edge of piece has broached-tooth design, and pattern is similar to leaf.
In addition, the present invention, which prepares resulting two-dimentional foliaceous nano zinc oxide material, can be used as gas sensing material tests
Low-concentration ethanol amine is demonstrated by higher selectivity in ammonium hydroxide, dimethylamine, trimethylamine and diethylamine.
Compared with prior art the invention has the following advantages: preparation method is raw materials used is easy to get, morphology controllable is produced
The quality of product is stablized, and each parameter is easily controllable, and production cost is low, does not both need to handle raw material with acid, also not need using organic
Solvent belongs to green synthesis techniques, and method is easy, high production efficiency, and pole is suitable for industrialized production, can be used for detecting low concentration
Ethanol amine has the characteristics that sensitivity is high, response is fast relative to conventional gas sensitive.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the two-dimentional foliaceous nano zinc oxide material of present invention preparation gained.
Fig. 2 is the stereoscan photograph of the two-dimentional foliaceous nano zinc oxide material of present invention preparation gained.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of two dimension foliaceous nano zinc oxide material, is achieved by the steps of:
(1) 1.4g zinc sulfate is dissolved in 100ml water and obtains the solution of zinc sulfate of 14g/L, then according to zinc sulfate matter
Amount is than the urea and cetyl trimethylammonium bromide for 1:0.41:0.13, by 0.58g urea and 0.18g cetyl front three
Base ammonium bromide sequentially adds in solution of zinc sulfate, and stirring makes it completely dissolved, and forms mixed solution；
(2) mixed solution in step (1) is transferred in reaction kettle, in 100 DEG C of constant temperature 4h；
(3) after the reaction was completed, reactant is taken out to be washed and be centrifugated；
(4) by the reactant of step (3) in 80 DEG C of dryings, and in 380 DEG C of heat treatment 2h, two dimension foliaceous nano oxygen is made
Change zinc product.
Embodiment 2
A kind of preparation method of two dimension foliaceous nano zinc oxide material, is achieved by the steps of:
(1) 1.44g zinc sulfate is dissolved in 100ml water and obtains the solution of zinc sulfate of 14.4g/L, then according to zinc sulfate
Mass ratio is the urea and cetyl trimethylammonium bromide of 1:0.41:0.13, by 0.59g urea and 0.19g cetyl three
Methyl bromide ammonium sequentially adds in solution of zinc sulfate, and stirring makes it completely dissolved, and forms mixed solution；
(2) mixed solution in step (1) is transferred in reaction kettle, in 120 DEG C of constant temperature 10h；
(3) after the reaction was completed, reactant is taken out to be washed and be centrifugated；
(4) by the reactant of step (3) in 70 DEG C of dryings, and in 400 DEG C of heat treatment 2h, two dimension foliaceous nano oxygen is made
Change zinc product.
Embodiment 3
A kind of preparation method of two dimension foliaceous nano zinc oxide material, is achieved by the steps of:
(1) 1.5g zinc sulfate is dissolved in 100ml water and obtains the solution of zinc sulfate of 15g/L, then according to zinc sulfate matter
Amount is than the urea and cetyl trimethylammonium bromide for 1:0.41:0.13, by 0.62g urea and 0.2g cetyl trimethyl
Ammonium bromide sequentially adds in solution of zinc sulfate, and stirring makes it completely dissolved, and forms mixed solution；
(2) mixed solution in step (1) is transferred in reaction kettle, in 140 DEG C of constant temperature 8h；
(3) after the reaction was completed, reactant is taken out to be washed and be centrifugated；
(4) by the reactant of step (3) in 75 DEG C of dryings, and in 420 DEG C of heat treatment 2h, two dimension foliaceous nano oxygen is made
Change zinc product.
Above-described is only the preferred embodiment of the present invention, it is noted that is come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, other embodiments can also be made, these belong to protection of the invention
Range.
Claims (1)
1. a kind of preparation method of two dimension foliaceous nano zinc oxide material, it is characterised in that: be achieved by the steps of:
(1) it is then 1 according to zinc sulfate mass ratio by the zinc sulfate solution of zinc sulfate soluble in water for obtaining 14 ~ 15g/L:
The urea and cetyl trimethylammonium bromide of 0.41:0.13, sequentially adds sulphur for urea and cetyl trimethylammonium bromide
In sour zinc solution, stirring is made it completely dissolved, and forms mixed solution；
(2) mixed solution in step (1) is transferred in reaction kettle, in 100 DEG C ~ 140 DEG C constant temperature 4-10h；
(3) after the reaction was completed, reactant is taken out to be washed and be centrifugated；
(4) by the reactant of step (3) in 70 DEG C ~ 80 DEG C dryings, and in 380 DEG C ~ 420 DEG C heat treatment 2h, two dimension blade is made
The nano oxidized zinc product of shape.
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| CN101591037B (en) * | 2009-07-03 | 2011-04-20 | 北京化工大学 | One-dimensional zinc oxide nanometer material and preparation method thereof |
| CN105417574A (en) * | 2014-09-05 | 2016-03-23 | 天津工业大学 | Preparation method of three-dimensional layered porous zinc oxide microspheres assembled from nano-sheets |
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