CN109678198A - A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film - Google Patents
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film Download PDFInfo
- Publication number
- CN109678198A CN109678198A CN201811542623.6A CN201811542623A CN109678198A CN 109678198 A CN109678198 A CN 109678198A CN 201811542623 A CN201811542623 A CN 201811542623A CN 109678198 A CN109678198 A CN 109678198A
- Authority
- CN
- China
- Prior art keywords
- solution
- zncl
- nano
- zinc stannate
- deionized water
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of synthetic methods of nano-zinc stannate material for N-shaped transparent semiconductor film, zinc chloride, stannic chloride and tetrabutylammonium are co-precipitated with certain proportion, then prepare partial size adjustable zine stannate nano material in 30~300 nanometer ranges using the hydrothermal synthesis with stirring.Zinc stannate has high stability, high electron mobility, chemical composition and band structure are easily controllable advantages as novel semiconductor material.Compared with zinc oxide, stannic oxide, zinc stannate is more with potential applications in the film photovoltaic cells such as dye-sensitized solar cells field.
Description
Technical field
The invention belongs to application field of the novel N-shaped transparent oxide semiconductor material in photoelectric conversion technology, specifically
It is related to a kind of preparation of semiconductor nano zinc stannate.
Background technique
Dye-sensitized solar cells because of its simple production process, cost of manufacture is cheap, spectral region is adjustable receives state
The extensive concern of inside and outside researcher.In past 30 years, the research of dye-sensitized solar cells is absorbed around width always
Light-sensitive coloring agent, high conductivity light anode, different oxidation-reduction potential electrolyte and low cost and high catalytic activity are to electrode exhibition
It opens.
Light anode is usually made of broad stopband nanocrystal metal oxide, for collecting in dye-sensitized solar cells
Light induced electron.So far, zinc oxide and tin oxide are the more non-titanium dioxide class wide-band gap materials of research.But it aoxidizes
Zinc is unstable to the dyestuff containing carboxylic acids anchoring group and excitation charge injection is difficult, and tin oxide then has Interface composites speed
Rate is too fast, the uppity defect of preparation process grain diameter.Relative to above-mentioned material, the chemical composition of zinc stannate is stable, carries
It is high to flow transport factor, and grain diameter has very strong adjustable type, is ideal dye-sensitized solar cell anode
Material.
The nano-zinc stannate preparation method reported at present is chiefly used in photocatalysis and fire proofing field, prepared nanometer
There are a large amount of reunions in grain, seriously affected the light transmittance of prepared nano-crystal film.For this purpose, developing a kind of suitable for dye sensitization
The nano-zinc stannate synthetic technology of battery light anode preparation is of great significance.
Summary of the invention
Particle size range is prepared as raw material using zinc chloride/stannic chloride/tetrabutylammonium the purpose of the present invention is to provide one kind to exist
The stirring hydrothermal synthesis method of zinc stannate between 30~300 nanometers.The zine stannate nano grain diameter synthesized using this method
It is adjustable, pattern is uniform, is easy to disperse in water, ethyl alcohol isopolarity solvent, can be used for preparing N-shaped transparent metal oxide semiconductor
Light anode of the film as dye-sensitized cell.
Technical solution of the present invention:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
Weigh a certain amount of SnCl4, according to SnCl4Amount determine ZnCl2Amount.ZnCl2It easily deliquesces, weighing is had to
Fastly, the ZnCl that will be weighed up2With appropriate amount of deionized water dissolution, (amount of deionized water dissolves ZnCl enough2), stirring is cooled to room
Wen Hou, by SnCl4With ZnCl2Aqueous solution quickly mixes, and stirring and dissolving is uniformly mixed and is cooled to room temperature, then plus deionization in right amount
Water, which is uniformly mixed, makees presoma；
It is above-mentioned to prepare precursor solution, it is desirable that molar ratio Zn:Sn=2:1, quantitative ZnCl2For 100mmol, i.e. 13.63g,
Quantitative SnCl4For 50mmol, i.e. 13.03g, it is finally configured to 100g precursor solution.
2) preparation of zine stannate nano material
Scheme one
Quantitative precursor solution is taken, quantitative deionized water is added and dilutes to obtain solution a, weighs four quantitative fourths by a certain percentage
Base Ammonia (40wt.%), the amount of reordering deionized water dilute to obtain solution b, solution b are poured into solution a and is quickly mixed
It shakes up rapidly, is fitted into reaction kettle, be stirred to react at high temperature 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.
The zinc stannate for being 100nm or more by the available partial size of scheme one, is mostly 100-300nm or so.
Scheme two
Quantitative precursor solution is taken, quantitative deionized water is added and dilutes to obtain solution a, weighs four quantitative fourths by a certain percentage
Base Ammonia (40wt.%), the amount of reordering deionized water dilute to obtain solution b, weigh suitable ZnCl by a certain percentage2,
Quantitative deionized water dissolving is added and obtains solution c, solution c is added in solution a and is uniformly mixed to obtain solution d, solution b is poured into solution
Quickly mixing shakes up rapidly in d, is fitted into reaction kettle, is stirred to react at high temperature 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.
Obtaining partial size by scheme two is 100nm zinc stannate below, is mostly 50nm or so.
The ZnCl2、SnCl4、H2O, the mass ratio of final precursor solution is 13.63g:13.03g:73.34g:100g.
The solution a mass ratio that precursor solution, dilution obtain in the scheme one is 5g:40g；In precursor solution
ZnCl2、SnCl4It is 2:1:10-16 with tetrabutylammonium hydroxide molar ratio；The solution that tetrabutylammonium hydroxide solution, dilution obtain
B mass ratio is 16.2163g-25.95g:60g.180 DEG C -200 DEG C of reaction temperature.
The solution a mass ratio that precursor solution, dilution obtain in the scheme two is 5g:40g；(b, d are mixed for reaction mixture
Solution after conjunction) in ZnCl2、SnCl4It is 2-2.4:1:9-10 with tetrabutylammonium hydroxide molar ratio；Tetrabutylammonium hydroxide is molten
The solution b mass ratio that liquid, dilution obtain is 14.59g-16.22g:60g；ZnCl2, solution c ratio be 0g-0.1363g:20-
40ml；180 DEG C -200 DEG C of reaction temperature.
The advantages and positive effects of the present invention:
The present invention method of stirring hydrothermal synthesis, can prepare the zine stannate nano material of different-grain diameter size, tin
Sour zinc is as ternary oxide, compared with the binary oxides such as tin oxide, zinc oxide, with more high electron mobility, highly conductive
Property and attracting optical characteristics.Zinc stannate as novel N-shaped transparent conductive oxide can be widely applied to solar battery,
The fields such as gas sensing, catalysis and lithium battery.
Detailed description of the invention
Fig. 1 is nano-zinc stannate SEM figure prepared by embodiment 1.
Fig. 2 is nano-zinc stannate SEM figure prepared by embodiment 2.
Fig. 3 is nano-zinc stannate SEM figure prepared by embodiment 3.
Fig. 4 is nano-zinc stannate SEM figure prepared by embodiment 4.
Fig. 5 is nano-zinc stannate SEM figure prepared by embodiment 5.
Fig. 6 is nano-zinc stannate SEM figure prepared by embodiment 6.
Fig. 7 is nano-zinc stannate SEM figure prepared by embodiment 7.
Fig. 8 is nano-zinc stannate SEM figure prepared by embodiment 8.
Specific embodiment
Embodiment 1:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
Weigh SnCl412.547g, in above-mentioned precursor solution each component ratio according to SnCl4Amount determine ZnCl2's
Amount.ZnCl2It easily deliquesces, fast, title ZnCl is had in weighing213.12g and with appropriate amount of deionized water dissolution (amount of deionized water is no more than
Final configuration precursor solution quality, the general ZnCl of dissolution enough2), after stirring is cooled to room temperature, by SnCl4With ZnCl2
Aqueous solution quickly mixes, and stirring and dissolving is uniformly mixed and is cooled to room temperature, then plus appropriate amount of deionized water (final solution quality is by upper
State precursor solution each component ratio-dependent, this solution quality should be 96.29g, that is, plus deionized water stir to 96.29g)
It mixes and is uniformly mixed that make presoma spare.
2) preparation of zine stannate nano material
5g precursor solution is taken, addition deionized water to 40g dilutes to obtain solution a, in molar ratio Zn:Sn: tetrabutyl hydrogen-oxygen
Change ammonium=2:1:16 ratio and weigh 25.95g tetrabutylammonium hydroxide solution (40wt.%), deionized water is added to dilute to 60g
Solution b is poured into solution a quickly mixing and shaken up rapidly, is fitted into reaction kettle, it is small to be stirred to react 12 at 180 DEG C by solution b
When.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.The nano-zinc stannate SEM figure of preparation is as shown in Fig. 1.
Embodiment 2:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
It is consistent with 1 scheme of embodiment
Weigh SnCl412.55g, in above-mentioned precursor solution each component ratio according to SnCl4Amount determine ZnCl2's
Amount.ZnCl2It easily deliquesces, fast, title ZnCl is had in weighing213.12g and with appropriate amount of deionized water dissolution (amount of deionized water is no more than
Final configuration precursor solution quality, the general ZnCl of dissolution enough2), after stirring is cooled to room temperature, by SnCl4With ZnCl2
Aqueous solution quickly mixes, and stirring and dissolving is uniformly mixed and is cooled to room temperature, then plus appropriate amount of deionized water (final solution quality is by upper
State precursor solution each component ratio-dependent, this solution quality should be 96.29g, that is, plus deionized water stir to 96.29g)
It mixes and is uniformly mixed that make presoma spare.
2) preparation of zine stannate nano material
5g precursor solution is taken, addition deionized water to 40g dilutes to obtain solution a, by Zn:Sn: tetrabutylammonium hydroxide=
The ratio of 2:1:12 weighs 19.46g tetrabutylammonium hydroxide solution (40wt.%), and deionized water is added to dilute to obtain solution b to 60g,
Solution b is poured into quickly to mix in solution a and is shaken up rapidly, is fitted into reaction kettle, is stirred to react at 200 DEG C 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.The nano-zinc stannate SEM figure of preparation is as shown in Fig. 2.
Embodiment 3:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
It is consistent with 1 scheme of embodiment
Weigh SnCl412.547g, in above-mentioned precursor solution each component ratio according to SnCl4Amount determine ZnCl2's
Amount.ZnCl2It easily deliquesces, fast, title ZnCl is had in weighing213.12g and with appropriate amount of deionized water dissolution (amount of deionized water is no more than
Final configuration precursor solution quality, the general ZnCl of dissolution enough2), after stirring is cooled to room temperature, by SnCl4With ZnCl2
Aqueous solution quickly mixes, and stirring and dissolving is uniformly mixed and is cooled to room temperature, then plus appropriate amount of deionized water (final solution quality is by upper
State precursor solution each component ratio-dependent, this solution quality should be 96.29g, that is, plus deionized water stir to 96.29g)
It mixes and is uniformly mixed that make presoma spare.
2) preparation of zine stannate nano material
5g precursor solution is taken, addition deionized water to 40g dilutes to obtain solution a, by Zn:Sn: tetrabutylammonium hydroxide=
The ratio of 2:1:11 weighs 17.84g tetrabutylammonium hydroxide solution (40wt.%), and deionized water is added to dilute to obtain solution b to 60g,
Solution b is poured into quickly to mix in solution a and is shaken up rapidly, is fitted into reaction kettle, is stirred to react at 200 DEG C 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.The nano-zinc stannate SEM figure of preparation is as shown in Fig. 3.
Embodiment 4:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
It is consistent with 1 scheme of embodiment
Weigh SnCl412.55g, in above-mentioned precursor solution each component ratio according to SnCl4Amount determine ZnCl2's
Amount.ZnCl2It easily deliquesces, fast, title ZnCl is had in weighing213.12g and with appropriate amount of deionized water dissolution (amount of deionized water is no more than
Final configuration precursor solution quality, the general ZnCl of dissolution enough2), after stirring is cooled to room temperature, by SnCl4With ZnCl2
Solution quickly mixes, and stirring and dissolving is uniformly mixed and is cooled to room temperature, then plus appropriate amount of deionized water (final solution quality is by above-mentioned
Precursor solution each component ratio-dependent, this solution quality should be 96.29g, that is, plus deionized water stir to 96.29g)
It is uniformly mixed that make presoma spare.
2) preparation of zine stannate nano material
5g precursor solution is taken, addition deionized water to 40g dilutes to obtain solution a, by Zn:Sn: tetrabutylammonium hydroxide=
The ratio of 2:1:10 weighs 16.22g tetrabutylammonium hydroxide solution (40wt.%), and deionized water is added to dilute to obtain solution b to 60g,
Solution b is poured into quickly to mix in solution a and is shaken up rapidly, is fitted into reaction kettle, is stirred to react at 200 DEG C 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.The nano-zinc stannate SEM figure of preparation is as shown in Fig. 4.
Embodiment 5:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
It is consistent with 1 scheme of embodiment
Weigh SnCl412.55g, in above-mentioned precursor solution each component ratio according to SnCl4Amount determine ZnCl2's
Amount.ZnCl2It easily deliquesces, fast, title ZnCl is had in weighing213.12g and with appropriate amount of deionized water dissolution (amount of deionized water is no more than
Final configuration precursor solution quality, the general ZnCl of dissolution enough2), after stirring is cooled to room temperature, by SnCl4With ZnCl2
Aqueous solution quickly mixes, and stirring and dissolving is uniformly mixed and is cooled to room temperature, then plus appropriate amount of deionized water (final solution quality is by upper
State precursor solution each component ratio-dependent, this solution quality should be 96.29g, that is, plus deionized water stir to 96.29g)
It mixes and is uniformly mixed that make presoma spare.
2) preparation of zine stannate nano material
5g precursor solution is taken, addition deionized water to 40g dilutes to obtain solution a, in molar ratio Sn: tetrabutylammonium hydroxide
The ratio of=1:10 weighs 16.22g tetrabutylammonium hydroxide solution (40wt.%), and deionized water is added to dilute to obtain solution b to 60g,
Zn:Sn=2.05:1 ratio claims the ZnCl of 0.01704g again in molar ratio2, 10ml deionized water dissolving is added and obtains solution c, it will be molten
Liquid c is added in solution a and is uniformly mixed to obtain solution d, and solution b is poured into solution d quickly mixing and is shaken up rapidly, loading reaction kettle
In, it is stirred to react at 200 DEG C 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.The nano-zinc stannate SEM figure of preparation is as shown in Fig. 5.
Embodiment 6:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
It is consistent with 1 scheme of embodiment
Weigh SnCl412.55g, in above-mentioned precursor solution each component ratio according to SnCl4Amount determine ZnCl2's
Amount.ZnCl2It easily deliquesces, fast, title ZnCl is had in weighing213.12g and with appropriate amount of deionized water dissolution (amount of deionized water is no more than
Final configuration precursor solution quality, the general ZnCl of dissolution enough2), after stirring is cooled to room temperature, by SnCl4With ZnCl2
Quickly mixing, stirring and dissolving are uniformly mixed and are cooled to room temperature, then plus appropriate amount of deionized water (final solution quality is by above-mentioned forerunner
Liquid solution each component ratio-dependent, this solution quality should be 96.29g, that is, plus deionized water be stirred to 96.29g)
It is spare uniformly to make presoma.
2) preparation of zine stannate nano material
5g precursor solution is taken, addition deionized water to 40g dilutes to obtain solution a, in molar ratio Sn: tetrabutylammonium hydroxide
The ratio of=1:10 weighs 16.22g tetrabutylammonium hydroxide solution (40wt.%), and deionized water is added to dilute to obtain solution b to 60g,
Zn:Sn=2.4:1 ratio claims the ZnCl of 0.1363g again in molar ratio2, 20ml deionized water dissolving is added and obtains solution c, by solution
C is added in solution a and is uniformly mixed to obtain solution d, and solution b is poured into solution d quickly mixing and is shaken up rapidly, is fitted into reaction kettle,
It is stirred to react at 200 DEG C 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.The nano-zinc stannate SEM figure of preparation is as shown in Fig. 6.
Embodiment 7:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
It is consistent with 1 scheme of embodiment
Weigh SnCl412.55g, in above-mentioned precursor solution each component ratio according to SnCl4Amount determine ZnCl2's
Amount.ZnCl2It easily deliquesces, fast, title ZnCl is had in weighing213.12g and with appropriate amount of deionized water dissolution (amount of deionized water is no more than
Final configuration precursor solution quality, the general ZnCl of dissolution enough2), after stirring is cooled to room temperature, by SnCl4With ZnCl2
Aqueous solution quickly mixes, and stirring and dissolving is uniformly mixed and is cooled to room temperature, then plus appropriate amount of deionized water (final solution quality is by upper
State precursor solution each component ratio-dependent, this solution quality should be 96.29g, that is, plus deionized water stir to 96.29g)
It mixes and is uniformly mixed that make presoma spare.
2) preparation of zine stannate nano material
5g precursor solution is taken, addition deionized water to 40g dilutes to obtain solution a, in molar ratio Sn: tetrabutylammonium hydroxide
The ratio of=1:9 weighs 14.59g tetrabutylammonium hydroxide solution (40wt.%), and deionized water is added to dilute to obtain solution b to 60g,
Zn:Sn=2:1 ratio separately takes ZnCl in molar ratio20g, only taking 40ml deionized water is solution c, and solution c is added in solution a
It is uniformly mixed to obtain solution d, solution b is poured into solution d quickly mixing and is shaken up rapidly, is fitted into reaction kettle, is stirred instead at 200 DEG C
It answers 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.The nano-zinc stannate SEM figure of preparation is as shown in Fig. 7.
Embodiment 8:
A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, steps are as follows:
1) preparation of molar ratio Zn:Sn=2:1 presoma
It is consistent with 1 scheme of embodiment
Weigh SnCl412.55g, in above-mentioned precursor solution each component ratio according to SnCl4Amount determine ZnCl2's
Amount.ZnCl2It easily deliquesces, fast, title ZnCl is had in weighing213.12g and with appropriate amount of deionized water dissolution (amount of deionized water is no more than
Final configuration precursor solution quality, the general ZnCl of dissolution enough2), after stirring is cooled to room temperature, by SnCl4With ZnCl2
Aqueous solution quickly mixes, and stirring and dissolving is uniformly mixed and is cooled to room temperature, then plus appropriate amount of deionized water (final solution quality is by upper
State precursor solution each component ratio-dependent, this solution quality should be 96.29g, that is, plus deionized water stir to 96.29g)
It mixes and is uniformly mixed that make presoma spare.
2) preparation of zine stannate nano material
5g precursor solution is taken, addition deionized water to 40g dilutes to obtain solution a, in molar ratio Sn: tetrabutylammonium hydroxide
The ratio of=1:9 weighs 14.59g tetrabutylammonium hydroxide solution (40wt.%), and deionized water is added to dilute to obtain solution b to 60g,
Zn:Sn=2.4:1 ratio claims the ZnCl of 0.1363g again in molar ratio2, 40ml deionized water dissolving is added and obtains solution c, by solution
C is added in solution a and is uniformly mixed to obtain solution d, and solution b is poured into solution d quickly mixing and is shaken up rapidly, is fitted into reaction kettle,
It is stirred to react at 200 DEG C 12 hours.
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, i.e.,
Preliminary target product can be obtained.The nano-zinc stannate SEM figure of preparation is as shown in Fig. 8.
Claims (6)
1. a kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film, using stirring hydrothermal synthesis method,
It is characterized by the following steps:
1) preparation of molar ratio Zn:Sn=2:1 presoma
Weigh a certain amount of SnCl4, according to SnCl4Amount determine ZnCl2Amount, the ZnCl that will be weighed up2Use appropriate amount of deionized water
Dissolution, the amount of deionized water dissolve ZnCl enough2, after stirring is cooled to room temperature, by SnCl4With ZnCl2Quickly mixing is stirred molten
Solution is uniformly mixed and is cooled to room temperature, then plus appropriate amount of deionized water be uniformly mixed and make presoma；
It is above-mentioned to prepare precursor solution, it is desirable that molar ratio Zn:Sn=2:1；
2) preparation of zine stannate nano material
Quantitative precursor solution is taken, quantitative deionized water is added and dilutes to obtain solution a, weighs quantitative 40wt.% by a certain percentage
Tetrabutylammonium hydroxide solution, the amount of reordering deionized water dilute to obtain solution b, and solution b is poured into quickly to mix in solution a and is shaken rapidly
It is even, it is fitted into reaction kettle, is stirred to react at high temperature 12 hours；
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, can be obtained
To preliminary target product.
2. the synthetic method of the nano-zinc stannate material according to claim 1 for N-shaped transparent semiconductor film, special
Sign is, in step 2) zine stannate nano material prepare it is as follows:
Quantitative precursor solution is taken, appropriate amount of deionized water is added and dilutes to obtain solution a, weighs quantitative 40wt.% by a certain percentage
Tetrabutylammonium hydroxide solution adds appropriate amount of deionized water to dilute to obtain solution b, weighs suitable ZnCl by a certain percentage2, it is added suitable
Amount deionized water dissolving obtains solution c, and solution c is added in solution a and is uniformly mixed to obtain solution d, solution b is poured into fast in solution d
Speed mixing shakes up rapidly, is fitted into reaction kettle, is stirred to react at high temperature 12 hours；
Lye after reaction is outwelled, product is washed 3-5 times, in aqueous solution by the zinc stannate dispersion after washing, can be obtained
To preliminary target product.
3. the synthetic method of the nano-zinc stannate material according to claim 1 for N-shaped transparent semiconductor film, special
Sign is:
In the hydrothermal synthesis reaction for preparing zinc stannate using tetrabutylammonium hydroxide as raw material, Zn, Sn, tetrabutylammonium hydroxide mole
Ratio is 2-2.4:1:10-16；The reaction temperature is 180 DEG C -200 DEG C.
4. the synthesis of the nano-zinc stannate material according to claim 1-3 for N-shaped transparent semiconductor film
Method, it is characterised in that:
The present invention using stirring hydrothermal synthesis method, be built in reaction kettle stir oil bath heating under conditions of complete it is anti-
It answers, guarantees crystallinity.
5. the synthetic method of the nano-zinc stannate material according to claim 1 or 2 for N-shaped transparent semiconductor film,
It is characterized by:
The uniform zinc stannate of small particle is prepared in step 2), in addition to low tetrabutylammonium hydroxide amount, key is to add appropriate
ZnCl2And reaction system concentration is reduced in right amount, by dissolved ZnCl2Solution be added to Zn be uniformly mixed in Sn presoma, mend
Add ZnCl2And solution c ratio is 0g-0.1363g:20-40ml after dissolution.
6. the synthetic method of the nano-zinc stannate material according to claim 1 for N-shaped transparent semiconductor film, special
Sign is: in step 1) precursor solution, quantitative ZnCl2For 100mmol, i.e. 13.63g, quantitative SnCl4For 50mmol, i.e.,
13.03g is finally configured to 100g precursor solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811542623.6A CN109678198A (en) | 2018-12-17 | 2018-12-17 | A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811542623.6A CN109678198A (en) | 2018-12-17 | 2018-12-17 | A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109678198A true CN109678198A (en) | 2019-04-26 |
Family
ID=66187894
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811542623.6A Pending CN109678198A (en) | 2018-12-17 | 2018-12-17 | A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109678198A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110172733A (en) * | 2019-06-20 | 2019-08-27 | 山东大学 | A kind of high quality zinc stannate monocrystal thin films and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1907862A (en) * | 2005-08-04 | 2007-02-07 | 河南大学 | Method of preparing nano hydroxyl zinc stannate and nano zinc stannate |
| CN103265065A (en) * | 2013-04-22 | 2013-08-28 | 中山大学 | Preparation method of graded zinc stannate macroporous materials |
| CN103601234A (en) * | 2013-10-23 | 2014-02-26 | 三棵树涂料股份有限公司 | Preparation method for nanometer zinc stannate |
| CN104891556A (en) * | 2015-05-29 | 2015-09-09 | 吉林大学 | Zinc hydroxystannate in double-layer hollow cubic structure and preparation method thereof |
| CN107445195A (en) * | 2017-09-04 | 2017-12-08 | 江苏大学 | A kind of preparation method of zine stannate nano cube or nanometer sheet material |
| CN107803196A (en) * | 2017-11-01 | 2018-03-16 | 大连民族大学 | A kind of synthesis has visible light-responded photochemical catalyst Zn2SnO 4/Bi 2WO 6The preparation method of nanometer sheet |
| CN108039472A (en) * | 2017-12-11 | 2018-05-15 | 西北大学 | A kind of preparation method and application of the hollow micron cube composite material of carbon coating zinc metastannate |
| CN108097233A (en) * | 2017-12-11 | 2018-06-01 | 河南师范大学 | A kind of preparation method for the cube structure zinc stannate photochemical catalyst for responding sunlight |
-
2018
- 2018-12-17 CN CN201811542623.6A patent/CN109678198A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1907862A (en) * | 2005-08-04 | 2007-02-07 | 河南大学 | Method of preparing nano hydroxyl zinc stannate and nano zinc stannate |
| CN103265065A (en) * | 2013-04-22 | 2013-08-28 | 中山大学 | Preparation method of graded zinc stannate macroporous materials |
| CN103601234A (en) * | 2013-10-23 | 2014-02-26 | 三棵树涂料股份有限公司 | Preparation method for nanometer zinc stannate |
| CN104891556A (en) * | 2015-05-29 | 2015-09-09 | 吉林大学 | Zinc hydroxystannate in double-layer hollow cubic structure and preparation method thereof |
| CN107445195A (en) * | 2017-09-04 | 2017-12-08 | 江苏大学 | A kind of preparation method of zine stannate nano cube or nanometer sheet material |
| CN107803196A (en) * | 2017-11-01 | 2018-03-16 | 大连民族大学 | A kind of synthesis has visible light-responded photochemical catalyst Zn2SnO 4/Bi 2WO 6The preparation method of nanometer sheet |
| CN108039472A (en) * | 2017-12-11 | 2018-05-15 | 西北大学 | A kind of preparation method and application of the hollow micron cube composite material of carbon coating zinc metastannate |
| CN108097233A (en) * | 2017-12-11 | 2018-06-01 | 河南师范大学 | A kind of preparation method for the cube structure zinc stannate photochemical catalyst for responding sunlight |
Non-Patent Citations (1)
| Title |
|---|
| YA-QI JIANG ET AL.: "Hydrothermal synthesis and gas sensing properties of cubic and quasi-cubic Zn2SnO4", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110172733A (en) * | 2019-06-20 | 2019-08-27 | 山东大学 | A kind of high quality zinc stannate monocrystal thin films and preparation method thereof |
| CN110172733B (en) * | 2019-06-20 | 2020-11-27 | 山东大学 | High-quality zinc stannate single crystal film and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104332560B (en) | Preparation method of chlorine-bromine-iodine-mixing perovskite light absorption layer material | |
| CN106477633B (en) | A kind of bimetal-doped group vib metal oxide nano-material and the preparation method and application thereof | |
| CN107511154B (en) | Sea urchin-shaped CeO 2 /Bi 2 S 3 Composite visible light catalyst and preparation method thereof | |
| CN101914310B (en) | Environmental-friendly pigment bismuth yellow and production method thereof | |
| CN103894177B (en) | A kind of synthetic method with the rear-earth-doped metatitanic acid potassium powder of photocatalytic activity | |
| CN105668633B (en) | Sea urchin shape tungsten bronze particle prepared by a kind of utilization template and preparation method thereof | |
| CN105957966A (en) | REO (rare earth oxide) down-conversion material perovskite solar cell and preparation method | |
| CN102491408A (en) | Preparation method of antimony-doped tin dioxide nano-slurry | |
| CN100593019C (en) | Tin dioxide powder body doped with antimony and preparing method thereof | |
| CN105382268B (en) | The preparation method of the vanadium pentoxide nanowires of Ag doping, its preparation method and electrochromic device | |
| CN104505521A (en) | Cathode catalyst for air battery and preparation method of cathode catalyst | |
| Bao et al. | One-step synthesis and stabilization of gold nanoparticles and multilayer film assembly | |
| CN106881078B (en) | Z-type junction ZnO-WO3Electrode, preparation method thereof and application thereof in photoelectrocatalysis | |
| CN109678198A (en) | A kind of synthetic method of the nano-zinc stannate material for N-shaped transparent semiconductor film | |
| CN101708820A (en) | Method for manufacturing nano antimony doped tin oxide | |
| CN109663615A (en) | A kind of g-C3N4/ppy/Bi2WO6Solid-state Z-type photochemical catalyst and preparation method | |
| CN109678211A (en) | A kind of tantalum doping caesium tungsten bronze and the preparation method and application thereof | |
| CN109768275A (en) | A kind of preparation method for mixing titanium lithium ion anode material presoma | |
| CN106430289A (en) | Method for low temperature preparation of high specific surface area nanometer gallate spinel | |
| CN107986334A (en) | A kind of preparation method of Ti-Mo codopes tungsten trioxide photoelectrode | |
| CN105417575B (en) | A kind of preparation method of the single dispersing tin dioxide quantal-point hydrosol | |
| CN109133168B (en) | Preparation method of monoclinic phase truncated octahedral bismuth vanadate crystal | |
| CN111185245A (en) | Graphene oxide loaded bismuth vanadate nanocomposite and preparation method thereof | |
| CN110499158A (en) | A kind of rare earth samarium doped tin oxide nano hollow ball sensitized luminescence body, preparation method and application | |
| CN107188225B (en) | A kind of indium-doped antimony oxidation tin nano-powder and preparation method thereof |
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 | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190426 |