CN105800670B - A kind of ZnS/Ag2The preparation method of the hollow micro-nano ball of S hetero-junctions - Google Patents
A kind of ZnS/Ag2The preparation method of the hollow micro-nano ball of S hetero-junctions Download PDFInfo
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- C01G9/08—Sulfides
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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Abstract
The invention discloses a kind of preparation method of the hollow micro-nano ball of ZnS/Ag2S hetero-junctions, by silver nitrate solution and equimolar zinc nitrate solution according to 1:1 is pressed after 1 ratio mixing with equimolar hypo solution again:3 mixing, are subsequently poured into annealing in reactor（200 DEG C, 24h）Washing afterwards is taken out to dry again and obtains the hollow micro-nano ball of ZnS/Ag2S hetero-junctions.The inventive method is to complete ZnS/Ag in the case where any surfactant is not added with2The preparation of the hollow micro-nano ball of S hetero-junctions, equipment is simple, and energy consumption is low, and synthesis step is few, and good quality of product is simple to operate, at room temperature（25 DEG C or so）Can reaction, suitable large-scale production.
Description
Technical field
The present invention is attributable to inorganic functional material preparing technical field, and it particularly relates to a kind of ZnS/Ag2S hetero-junctions
The preparation method of hollow micro-nano ball.
Background technology
Micro-nano sphere material is a class size in nano-micro level, the material with special construction.Because it has specific surface
Product is high, the low characteristic of density, and such material has great application value at aspects such as opto-electronic conversion, photocatalysis, electrode materials.
At present, continuing to bring out with correlative study achievement, have become Material Field one grinds for the preparation of micro-nano sphere material
Study carefully focus
Hollow ball-shape sulfide is a kind of important Transition-metal dichalcogenide, even more a kind of important semiconductor material
Material, silver sulfide be the semi-conducting material of narrow band gap and zinc sulphide be direct broad-band gap semi-conducting material, when both are compounded to form
The semi-conducting material of hetero-junctions has more preferable photoelectric properties.Nanoscale silver sulfide and zinc sulphide are due to its unique physical chemistry
Characteristic, such as low-density, high-specific surface area, comprising inner space and the features such as surface penetration, particularly both are compounded to form ZnS/
Ag2Their performance advantage is preferably manifested after S heterojunction materials, thus opto-electronic conversion, photocatalysis, hydrogen storage property,
The aspects such as electrode material, nonlinear optics show excellent special nature.Therefore the ZnS/Ag of nanostructured2S hetero-junctions half
Conductor is in fields such as photocatalysis, photoelectric conversion, solar cell, solar energy irradiation receiver, lithium-hydrogen battery and optical-electrical converters
It is with a wide range of applications.And then ZnS/Ag2The hollow micro-nano ball of S hetero-junctions turns into material, physics, chemistry, photoelectricity etc.
Numerous disciplinary study person concerns and the focus of research.At present, the light of multicomponent is obtained by simple and feasible synthetic method
Electric material and corresponding experiment condition can be changed control the pattern of synthetic, particularly synthesize nanometer spherical, square
With the interest that interconnection shape nano material more causes lot of materials physical and chemical performance researcher.There are many experimental technique quilts now
Apply in multicomponent（ZnS/Ag2S hetero-junctions）In the preparation of semi-conducting material, such as：Chemical deposition, hydro-thermal method, electro-deposition
Method, solvent-thermal method, template contral method in situ, microwave assisting method etc..
The invention of this row is that the common hydro-thermal method for using prepares ZnS/Ag2The hollow micro-nano ball of S hetero-junctions, this is synthesis
Nano material is most common, simplest method, but prior art synthesis Nano microsphere is not just so simple, it can be common that
Under conditions of HTHP and add surfactant（CTAB）Nano particle, nano wire, nanometer rods etc. could be prepared.
The content of the invention
In view of prior art is not enough above, it is an object of the present invention to provide ZnS/Ag prepared by this preparation method2S is heterogeneous
But the degree of purity for tying hollow micro-nano ball be not it is very high can be to obtain desired purity through filter centrifugation, the method equipment letter
Single, energy consumption is low, and synthesis step is few, simple to operate, at room temperature（25 DEG C or so）Can react, be adapted to large-scale production, and system
Obtain the function admirable of silver sulfide.
The technical scheme adopted by the invention for realizing the object of the invention is：A kind of hollow micro-nano ball of ZnS/Ag2S hetero-junctions
Preparation method, its specific practice is：
A, preparation mixed solution
Prepare certain density silver nitrate solution；The zinc nitrate solution of same concentration is prepared again；Then equivalent volumes are taken
Two kinds of solution make its uniform mixing；
B, annealing
Prepare the hypo solution of same concentration；Then the mixed solution for a being walked is added in hypo solution,
Consumption volume ratio is the mixed solution of a steps：Hypo solution=1:3；Gained mixed solution is placed on magnetic stirrer stirring
, there are the suspended things of grey in 30min；The mixed solution poured into hydrothermal reaction kettle again afterwards and locking is sealed, finally dress
The reactor for having mixed solution is put into Muffle furnace, and 24h is made annealing treatment at a temperature of 200 DEG C；
C, washing and drying
After the completion of the reactor equipped with mixed solution is annealed in Muffle furnace, reaction solution therein is put into beaker,
Black precipitate first is removed into salt ion with deionized water supersound washing to be defined, then with absolute ethanol washing, then will cleaned
Black precipitate is put into vacuum drying chamber, and 5h is dried at 60 DEG C can obtain dry target product.
The inventive method prepares ZnS/Ag2The substantially mechanism of the hollow micro-nano ball of S hetero-junctions：ZnS/Ag2S hetero-junctions is hollow
Micro-nano ball be by interfacial reaction synthesize, after silver nitrate solution mixes with zinc nitrate solution again with hypo solution
Mixing, three's mixed liquor is in faintly acid, at room temperature sodium thiosulfate hydrolysis S2O3 2-, S2O3 2--With Ag+Reaction generation Ag2S2O3 2-
Complex compound simultaneously further decomposes into silver sulfide molecule, and silver sulfide molecule is assembled to form nano particle, at high temperature under high pressure Zn2+With
S2O3 2-Reaction ultimately generates ZnS molecules and assembles to form microballoon as core with silver sulfide nano particle, while Zn2+It is high in high temperature
Pressure and silver sulfide reaction are that the silver sulfide nanometer particles particle in core is gradually decreased and forms hollow microballoon, but hollow micro-
Silver sulfide is also being generated during ball is formed, and the relative zinc sulphide of amount is less, ultimately forms ZnS/Ag2S hetero-junctions hollow structures are micro-
Nanosphere.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention uses hydro-thermal method, with inorganic silver nitrate and nitric acid
Zinc hydrolysis provides silver-colored source and zinc source, and being hydrolyzed to sulphur source with sodium thiosulfate participates in the reaction with silver-colored source and zinc source and then form ZnS/
Ag2The hollow micro-nano ball of S hetero-junctions, this reaction is added without any activating agent and stabilizer, in 200 DEG C and 2 ~ 3 atmospheric pressures
Lower reaction can obtain ZnS/Ag2The hollow micro-nano ball of S hetero-junctions, its preparation method is simple, and reaction is gentle, consumes energy small, synthesis step
It is rapid few, it is simple to operate, to equipment without particular/special requirement, it is adapted to large-scale production.It is demonstrated experimentally that obtained is ZnS/Ag2S hetero-junctions
Hollow micro-nano ball, a diameter of 1 ~ 5um.
The inventive method can obtained various patterns nanometer sulfide.Such as：Synthesis CuS nanosheet and nanosphere, Ag2S
Nano particle, nano wire, nanosphere and nanometer rods, the single inorganic sulphide such as ZnS nanospheres and PbS nano particles；Can also make
For polynary nanometer sulfide is gone out, such as：CdS-PbS, CdS-FeS, CuS-ZnS and CuZnInS3Deng.Vulcanization is obtained after the completion of synthesis
The structure determination of thing, degree of purity are good, controllable, stable performance.The sulfide and compound of these micro-nano structures have extensive use
On the way, can be used as the electrode material and the photoelectric conversion material of solar panel of the Li/S batteries of height ratio capacity.
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is further detailed explanation.
Brief description of the drawings
Fig. 1 is ZnS/Ag prepared by the embodiment of the present invention one2The XRD spectrum of the hollow micro-nano ball of S hetero-junctions.
Fig. 2 is ZnS/Ag prepared by the embodiment of the present invention one2The scanning electron microscopic picture of the hollow micro-nano ball of S hetero-junctions, its
In, figure A is scanning electron microscope (SEM) photograph, and figure B is the partial enlarged drawing of figure A.
Fig. 3 is ZnS/Ag prepared by the embodiment of the present invention two2The scanning electron microscopic picture of the hollow micro-nano ball of S hetero-junctions, its
In, figure A is scanning electron microscope (SEM) photograph, and figure B is the partial enlarged drawing of figure A.
Fig. 4 is ZnS/Ag prepared by the embodiment of the present invention three2The scanning electron microscopic picture of the hollow micro-nano ball of S hetero-junctions, its
In, figure A is scanning electron microscope (SEM) photograph, and figure B is the partial enlarged drawing of figure A.
Fig. 5 is ZnS/Ag prepared by the embodiment of the present invention four2The scanning electron microscopic picture of the hollow micro-nano ball of S hetero-junctions, its
In, figure A is scanning electron microscope (SEM) photograph, and figure B is the partial enlarged drawing of figure A.
Specific embodiment
In the narration of this paper, each reactant in addition to special declaration, is chemistry pure.
Embodiment one
A kind of specific embodiment of the invention is：
A kind of ZnS/Ag2The preparation method of the hollow micro-nano ball of S hetero-junctions, its specific practice is：
A, preparation mixed solution
Solution is prepared as container with beaker, silver nitrate solution is first prepared, concentration is 0.20M, measure 5ml；Nitric acid is prepared again
Zinc solution, concentration is 0.20M, measures 5ml；Then two kinds of solution of corresponding concentration are mixed makes its uniform.Then thio sulphur is prepared
Acid sodium solution, concentration is 0.20M, measures 30ml；
B, annealing
The mixed solution that a is walked is poured into the hypo solution of corresponding concentration respectively and is ceaselessly stirred, then by three
Person's mixed solution is placed on magnetic stirrer stirring 30min, and the suspended things of grey are occurred in that in mixed solution；Afterwards again mixing
Solution is poured into hydrothermal reaction kettle and seals locking, and finally the reactor equipped with mixed solution is put into Muffle furnace, at 200 DEG C
At a temperature of make annealing treatment 24h；
C, washing and drying
After the completion of the reactor equipped with mixed solution is annealed in Muffle furnace, reaction solution therein is put into beaker,
Now mixed liquor is to clarify and have black precipitate；Black precipitate is first used into deionized water supersound washing for several times（Gone salt from
Son is defined）Again with absolute ethanol washing several times；Clean black precipitate sample is put into vacuum drying chamber again, in 60 DEG C of bakings
Dry 5h can obtain dry sample.
The ZnS/Ag prepared with this method in terms of the XRD spectrum of sample from Fig. 12The X-ray of the hollow micro-nano ball of S hetero-junctions
Diffraction maximum position can correspond to silver sulfide and zinc sulphide PDF respectively（Powder Diffraction File）The peak position of diffraction maximum on standard card, this
Illustrate that the sample is ZnS/Ag2S composites, are that the heterojunction structure that is compounded to form of silver sulfide phase and zinc sulphide phase has no other
Dephasign.
Fig. 2 is by this example reaction generation ZnS/Ag2The hollow micro-nano ball of S hetero-junctions is sonicated（Ultrasound 1 is small in water
When, power 100w）Scanning electron microscope (SEM) photograph afterwards.ZnS/Ag can be seen from A figures2The diameter dimension of S hetero-junctions micro-nano balls be 1 ~
In the range of 4.0um, but from terms of B figures it is known that ZnS/Ag2S hetero-junctions micro-nano balls center is empty, and hollow is micro-nano
Ball inner surface be it is very rough there are many tiny nanoparticle aggregates to form rough surface, outer surface is smoother,
This explanation ZnS/Ag2S hetero-junctions micro-nano balls are unconventional whole ZnS/Ag2The hollow micro-nano ball of S hetero-junctions.
Embodiment two
A kind of specific embodiment of the invention is：
A kind of ZnS/Ag2The preparation method of the hollow micro-nano ball of S hetero-junctions, its specific practice is：
A, preparation mixed solution
Solution is prepared as container with beaker, silver nitrate solution is first prepared, concentration is 0.25M, measure 5ml；Nitric acid is prepared again
Zinc solution, concentration is 0.25M, measures 5ml；Then two kinds of solution of corresponding concentration are mixed makes its uniform.Then thio sulphur is prepared
Acid sodium solution, concentration is 0.25M, measures 30ml；
B, annealing
The mixed solution that a is walked is poured into the hypo solution of corresponding concentration respectively and is ceaselessly stirred, then by three
Person's mixed solution is placed on magnetic stirrer stirring 30min, and the suspended things of grey are occurred in that in mixed solution；Afterwards again mixing
Solution is poured into hydrothermal reaction kettle and seals locking, and finally the reactor equipped with mixed solution is put into Muffle furnace, at 200 DEG C
At a temperature of make annealing treatment 24h；
C, washing and drying
After the completion of the reactor equipped with mixed solution is annealed in Muffle furnace, reaction solution therein is put into beaker,
Now mixed liquor is to clarify and have black precipitate；Black precipitate is first used into deionized water supersound washing for several times（Gone salt from
Son is defined）Again with absolute ethanol washing several times；Clean black precipitate sample is put into vacuum drying chamber again, in 60 DEG C of bakings
Dry 5h can obtain dry sample.
Fig. 3 is by this example reaction generation ZnS/Ag2The hollow micro-nano ball of S hetero-junctions is sonicated（Ultrasound 2 is small in water
When, power 100w）Scanning electron microscope (SEM) photograph afterwards.ZnS/Ag can be seen from A figures2The diameter dimension of S hetero-junctions micro-nano balls be 1 ~
In the range of 4.0um, but from terms of B figures it is known that ZnS/Ag2The inside of S hetero-junctions micro-nano balls is empty, smooth outer surface
, this explanation ZnS/Ag2S hetero-junctions micro-nano ball is unconventional whole ZnS/Ag2The hollow micro-nano ball of S hetero-junctions.
Embodiment three
A kind of specific embodiment of the invention is：
A kind of ZnS/Ag2The preparation method of the hollow micro-nano ball of S hetero-junctions, its specific practice is：
A, preparation mixed solution
Solution is prepared as container with beaker, silver nitrate solution is first prepared, concentration is 0.30M, measure 5ml；Nitric acid is prepared again
Zinc solution, concentration is 0.30M, measures 5ml；Then two kinds of solution of corresponding concentration are mixed makes its uniform.Then thio sulphur is prepared
Acid sodium solution, concentration is 0.30M, measures 30ml；
B, annealing
The mixed solution that a is walked is poured into the hypo solution of corresponding concentration respectively and is ceaselessly stirred, then by three
Person's mixed solution is placed on magnetic stirrer stirring 30min, and the suspended things of grey are occurred in that in mixed solution；Afterwards again mixing
Solution is poured into hydrothermal reaction kettle and seals locking, and finally the reactor equipped with mixed solution is put into Muffle furnace, at 200 DEG C
At a temperature of make annealing treatment 24h；
C, washing and drying
After the completion of the reactor equipped with mixed solution is annealed in Muffle furnace, reaction solution therein is put into beaker,
Now mixed liquor is to clarify and have black precipitate；Black precipitate is first used into deionized water supersound washing for several times（Gone salt from
Son is defined）Again with absolute ethanol washing several times；Clean black precipitate sample is put into vacuum drying chamber again, in 60 DEG C of bakings
Dry 5h can obtain dry sample.
Fig. 4 is by this example reaction generation ZnS/Ag2The hollow micro-nano ball of S hetero-junctions is sonicated（Ultrasound 3 is small in water
When, power 100w）Scanning electron microscope (SEM) photograph afterwards.ZnS/Ag can be seen from A figures2The diameter dimension of S hetero-junctions micro-nano balls be 1 ~
In the range of 4.0um, but from terms of B figures it is known that ZnS/Ag2S hetero-junctions micro-nano balls center is empty, and hollow is micro-nano
Ball inner surface be it is very rough there are many tiny nanoparticle aggregates to form rough surface, outer surface is that have smaller nanometer
Particle packing is formed and relatively smooth rounder and more smooth, this explanation ZnS/Ag2S hetero-junctions micro-nano balls are unconventional whole ZnS/
Ag2The hollow micro-nano ball of S hetero-junctions.
Example IV
A kind of specific embodiment of the invention is：
A kind of ZnS/Ag2The preparation method of the hollow micro-nano ball of S hetero-junctions, its specific practice is：
A, preparation mixed solution
Solution is prepared as container with beaker, silver nitrate solution is first prepared, concentration is 0.35M, measure 5ml；Nitric acid is prepared again
Zinc solution, concentration is 0.35M, measures 5ml；Then two kinds of solution of corresponding concentration are mixed makes its uniform.Then thio sulphur is prepared
Acid sodium solution, concentration is 0.35M, measures 30ml；
B, annealing
The mixed solution that a is walked is poured into the hypo solution of corresponding concentration respectively and is ceaselessly stirred, then by three
Person's mixed solution is placed on magnetic stirrer stirring 30min, and the suspended things of grey are occurred in that in mixed solution；Afterwards again mixing
Solution is poured into hydrothermal reaction kettle and seals locking, and finally the reactor equipped with mixed solution is put into Muffle furnace, at 200 DEG C
At a temperature of make annealing treatment 24h；
C, washing and drying
After the completion of the reactor equipped with mixed solution is annealed in Muffle furnace, reaction solution therein is put into beaker,
Now mixed liquor is to clarify and have black precipitate；Black precipitate is first used into deionized water supersound washing for several times（Gone salt from
Son is defined）Again with absolute ethanol washing several times；Clean black precipitate sample is put into vacuum drying chamber again, in 60 DEG C of bakings
Dry 5h can obtain dry sample.
Fig. 5 is by this example reaction generation ZnS/Ag2The hollow micro-nano ball of S hetero-junctions is sonicated（Ultrasound 5 is small in water
When, power 100w）Scanning electron microscope (SEM) photograph afterwards.ZnS/Ag can be seen from A figures2The diameter dimension of S hetero-junctions micro-nano balls be 1 ~
In the range of 4.0um, but from terms of B figures it is known that ZnS/Ag2S hetero-junctions micro-nano balls center is empty, and hollow is micro-nano
Ball inner surface be it is very rough there are many tiny nanoparticle aggregates to form rough surface, outer surface nor very smooth,
This explanation ZnS/Ag2S hetero-junctions micro-nano balls are unconventional whole ZnS/Ag2The hollow micro-nano ball of S hetero-junctions, even if in ultrasound
Treatment a few hours still can guarantee that the integrality of micro-nano ball.
Claims (3)
1. a kind of ZnS/Ag2The preparation method of the hollow micro-nano ball of S hetero-junctions, its specific practice is：
A, preparation mixed solution
Prepare certain density silver nitrate solution；The zinc nitrate solution of same concentration is prepared again；Then two kinds of equivalent volumes are taken
Solution makes its uniform mixing；
B, annealing
Prepare the hypo solution of same concentration；Then the mixed solution for a being walked is added in hypo solution, consumption
Volume ratio is the mixed solution of a steps：Hypo solution=1:3；Gained mixed solution is placed on magnetic stirrer stirring
, there are the suspended things of grey in 30min；The mixed solution poured into hydrothermal reaction kettle again afterwards and locking is sealed, finally dress
The reactor for having mixed solution is put into Muffle furnace, and 24h is made annealing treatment at a temperature of 200 DEG C；
C, washing and drying
After the completion of the reactor equipped with mixed solution is annealed in Muffle furnace, reaction solution therein is put into beaker, will be black
Color sediment has first removed salt ion and has been defined with deionized water supersound washing, then with absolute ethanol washing, then will be clean black
Sediment is put into vacuum drying chamber, and drying 5h at 60 DEG C obtains a diameter of 1 ~ 5um target products.
2. ZnS/Ag as claimed in claim 12The preparation method of the hollow micro-nano ball of S hetero-junctions, it is characterised in that：Described a
The concentration of silver nitrate solution and zinc nitrate solution is controlled in 0.20-35M in step.
3. a kind of ZnS/Ag as claimed in claim 1 or 22The preparation method of the hollow micro-nano ball of S hetero-junctions, it is characterised in that：
Hypo solution concentration is controlled in 0.20-35M in described b steps.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103586051A (en) * | 2013-11-28 | 2014-02-19 | 中国石油大学(华东) | Composite metal sulfide photocatalyst, and preparation method and application thereof |
| CN105170165A (en) * | 2015-09-07 | 2015-12-23 | 武汉理工大学 | Flake Ag2S-loaded Ag3PO4 nano-sphere composite visible light catalyst and preparation method thereof |
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2016
- 2016-03-21 CN CN201610159432.6A patent/CN105800670B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103586051A (en) * | 2013-11-28 | 2014-02-19 | 中国石油大学(华东) | Composite metal sulfide photocatalyst, and preparation method and application thereof |
| CN105170165A (en) * | 2015-09-07 | 2015-12-23 | 武汉理工大学 | Flake Ag2S-loaded Ag3PO4 nano-sphere composite visible light catalyst and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| D. Amaranatha Reddya et al..Reduced graphene oxide wrapped ZnS–Ag2S ternary compositessynthesized via hydrothermal method: Applications in photocatalystdegradation of organic pollutants.《Applied Surface Science》.2014,第324卷第725-735页. * |
| V. G. Debabov et al..Bacterial Synthesis of Silver Sulfide Nanoparticles.《Nanotechnologies in Russia》.2013,第8卷(第3-4期),第269-276页. * |
| 李小兵 等.ZnS纳米粒子的水热法和溶剂热法制备.《压电与声光》.2002,第24卷(第4期),第306-308、311页. * |
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