CN109987624A - The preparation method of ZnS nanosheet - Google Patents
The preparation method of ZnS nanosheet Download PDFInfo
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- CN109987624A CN109987624A CN201910389618.4A CN201910389618A CN109987624A CN 109987624 A CN109987624 A CN 109987624A CN 201910389618 A CN201910389618 A CN 201910389618A CN 109987624 A CN109987624 A CN 109987624A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01G9/08—Sulfides
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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
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 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
- C01P2004/62—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
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- Inorganic Chemistry (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention relates to a kind of preparation method of ZnS nanosheet, the preparation method includes the following steps: for ZnS- (L) n presoma to be dispersed in water, and obtains suspension；The suspension is placed under illumination, be stirred continuously and is reacted in certain temperature；Solution after reaction is washed, separated and precipitated, the dry precipitating obtains ZnS nanosheet；Wherein, the L in ZnS- (L) n is the compound comprising mono amino or polyamino, n 0.5-1.The preparation method reaction condition is mild, simple process and environmental-friendly.ZnS nanosheet made from the preparation method has huge application prospect in preparing optical device, electricity device and catalyst.
Description
Technical field
The present invention relates to the preparation technical fields of nano material, more particularly, to a kind of preparation side of ZnS nanosheet
Method.
Background technique
ZnS is a kind of semiconductor material with wide forbidden band with significant application value, with excellent fluorescent effect and electroluminescent
Light-emitting function shows huge application prospect in terms of Application Optics, electronics and electronic device.And for nanostructure
ZnS, due to the dependency characteristic of quantum confined effect and light emitting property and size, pattern, in electricity, magnetics, optics, power
It learns and the fields such as catalysis shows many excellent performances.In recent years especially by the concern of researchers.It grinds in the recent period simultaneously
Study carefully discovery, wurtzite-type ZnS has more superior optical property compared to zinc blende-type ZnS.However the high-temperature-phase as ZnS,
Wurtzite-type ZnS is but difficult to synthesize under cryogenic.
Traditionally, the preparation of wurtzite-type ZnS nanostructure (such as nano wire, nanometer rods, nanometer sheet) is mainly adopted
With thermal evaporation, reaction usually requires to carry out at 900~1600 DEG C.Not only energy consumption is larger for this method, and yield is not high, Er Qiegong
Skill process is complicated.
Summary of the invention
Based on this, one object of the present invention is just to provide a kind of preparation method of ZnS nanosheet, preparation method reaction
Mild condition, simple process and environmental-friendly.
To achieve the above object, it adopts the following technical scheme that
A kind of preparation method of ZnS nanosheet, includes the following steps:
ZnS- (L) n presoma is dispersed in water, suspension is obtained；
The suspension is placed under illumination, be stirred continuously and is reacted in certain temperature；
Solution after reaction is washed, separated and precipitated, the dry precipitating obtains ZnS nanosheet；
Wherein, the L in ZnS- (L) n is the compound comprising mono amino or polyamino, n 0.5-1.
The L in ZnS- (L) n is selected from the one of ethylenediamine, cyclohexanediamine and o-phenylenediamine in one of the embodiments,
Kind is a variety of.
The n in ZnS- (L) n is 0.5 in one of the embodiments,.
The n in ZnS- (L) n is 1 in one of the embodiments,.
The suspension is placed in the light source under illumination in one of the embodiments, and is selected from mercury lamp, xenon lamp and the sun
One of light or multiple combinations.
It is 2-50h that the suspension, which is placed in the light application time under illumination, in one of the embodiments,.
It is 2-24h that the suspension, which is placed in the light application time under illumination, in one of the embodiments,.
The certain temperature is 2-30 DEG C in one of the embodiments,.
The certain temperature is 15-25 DEG C in one of the embodiments,.
In one of the embodiments, the ZnS nanosheet with a thickness of 0.5-20nm, planar dimension is 10nm-10 μm.
In one of the embodiments, the ZnS nanosheet with a thickness of 6nm, planar dimension 120nm.
The quality of ZnS- (L) the n presoma is 5-500mg in one of the embodiments,.
The quality of ZnS- (L) the n presoma is 5-200mg in one of the embodiments,.
The volume of the suspension is 10-1000mL in one of the embodiments,.
The volume of the suspension is 10-500mL in one of the embodiments,.
In a kind of one embodiment, the volume of the suspension is 200-500mL.
The washing uses deionized water and/or ethyl alcohol in one of the embodiments,.
Reaction principle of the invention is shown below:
ZnS-(L)n+hυ→ZnS-(L)n*+h++e-
ZnS-(L)n*+h++O2→ZnS+CO2+H2O+N2
ZnS-(L)n*+e-+O2→ZnS+CO2+H2O+N2
That is the excitation of ZnS- (L) n light generates electron-hole pair, is then respectively provided with oxidation, the hole of reducing power, electricity
The L ligand that son directly or indirectly aoxidizes in ZnS- (L) n finally obtains ZnS nanosheet with the continuous consumption of L ligand.
Compared with prior art, the present invention has energy consumption small, and reaction is simple, at low cost, simple process and environmentally friendly
The advantages of.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method of ZnS nanosheet of the invention；
(A) and (B) is the SEM figure of ZnS nanosheet obtained by the embodiment of the present invention 2 in Fig. 2；
Fig. 3 is the XRD diagram of ZnS nanosheet obtained by the embodiment of the present invention 2.
Specific embodiment
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention.But the present invention can be with
Much it is different from other way described herein to implement, those skilled in the art can be without prejudice to intension of the present invention the case where
Under do similar improvement, therefore the present invention is not limited to the specific embodiments disclosed below.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
The present invention provides a kind of preparation methods of ZnS nanosheet, include the following steps:
S1, ZnS- (L) n presoma is dispersed in water, obtains suspension；
S2, the suspension is placed under illumination, is stirred continuously and is reacted in certain temperature；
S3, the solution after reaction is washed, separated and is precipitated, the dry precipitating obtains ZnS nanosheet；
Wherein, the L in ZnS- (L) n is the compound comprising mono amino or polyamino, n 0.5-1.
The present invention does not have special limitation to the source of all raw materials, is commercially available.
The organic compound containing amido functional group that L in ZnS- (L) n is well known to those skilled in the art is i.e.
Can, have no it is specifically limited, the present invention in L be preferably the one or more of ethylenediamine (en), cyclohexanediamine and o-phenylenediamine, more
Preferably ethylenediamine；N in ZnS- (L) n is preferably 0.5 or 1, more preferably 0.5；The quality of ZnS- (L) n presoma is according to reality
The demand of testing is adjusted correspondingly, and the quality of ZnS- (L) n presoma is preferably 5-500mg in the present invention, more preferably 5-
200mg, most preferably 5mg, 200mg or 500mg.
The light source that the light source that the suspension is placed under illumination is well known to those skilled in the art, has no spy
Different limitation, light source in the present invention is preferably one of mercury lamp, xenon lamp and sunlight or a variety of, more preferably mercury lamp；Its
Light application time is preferred 2-50h, more preferably 2-24h, most preferably 2h, for 24 hours or 50h.
The rate of stirring can be adjusted correspondingly according to experimental conditions, and the rate stirred in the present invention is preferably
1600r/min。
The volume of the suspension is adjusted correspondingly according to experiment demand, and the volume of suspension in the present invention is excellent
It is selected as 10-1000mL, more preferably 10-500mL, most preferably 200-500mL.
In the prior art, thermal evaporation is mainly used for the preparation of wurtzite-type ZnS nanostructure, reacting usually needs
It to be carried out at 900~1600 DEG C, this method energy consumption is larger.In the present invention, zinc ore type ZnS is prepared at a lower temperature to receive
Rice piece.Certain temperature in the present invention is preferably 2-30 DEG C, and more preferably 15-25 DEG C.
The method of carrying out washing treatment can make method well-known to those skilled in the art, in the present invention, washup
Reason uses deionized water or ethyl alcohol, or is cleaned after being first washed with deionized water with ethyl alcohol, and the cleaning sequence of the two can be exchanged.
Separation, precipitating and the dry conventional technical means being well known to the skilled person.
The thickness of ZnS nanosheet can be adjusted according to demand, and ZnS nanometers of thickness is preferably 0.5- in the present invention
20nm, more preferably 6nm；Its planar dimension is preferably 10nm-10 μm, more preferably 120nm.
In order to further illustrate the present invention, with reference to embodiments to a kind of preparation of ZnS nanosheet provided by the invention
Method is described in detail.
Reagent used in following embodiment is commercially available.
Embodiment 1
Weigh homemade 5mg ZnS (en)0.5Presoma is scattered in the water of 10mL, obtains suspension；By gained suspension
It is placed under low pressure mercury lamp and irradiates 2h, it is room temperature that suspension, which is stirred continuously and keeps temperature of reaction system, in irradiation process；Then
With deionized water and ethyl alcohol by washing, separation collects precipitating, is dried to obtain ZnS nanosheet sample.
Embodiment 2
Weigh homemade 200mg ZnS (en)0.5Presoma is scattered in the water of 200mL, obtains suspension；Gained is hanged
Turbid, which is placed under low pressure mercury lamp, irradiates for 24 hours, and it is room temperature that suspension, which is stirred continuously and keeps temperature of reaction system, in irradiation process；
Then with deionized water and ethyl alcohol by washing, separation collects precipitating, is dried to obtain ZnS nanosheet sample.
Embodiment 3
Weigh homemade 500mg ZnS (en)0.5Presoma is scattered in the water of 500mL, obtains suspension；Gained is hanged
Turbid, which is placed under low pressure mercury lamp, irradiates 50h, and it is room temperature that suspension, which is stirred continuously and keeps temperature of reaction system, in irradiation process；
Then with deionized water and ethyl alcohol by washing, separation collects precipitating, is dried to obtain ZnS nanosheet sample.
Comparative example 1
Weigh homemade 500mg ZnS (en)0.5Presoma is laid in porcelain boat, is placed it in Muffle furnace, is warming up to
350 DEG C, it is naturally cooling to room temperature after keeping the temperature 10h, obtains ZnS nanosheet sample.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (9)
1. a kind of preparation method of ZnS nanosheet, which comprises the steps of:
ZnS- (L) n presoma is dispersed in water, suspension is obtained；
The suspension is placed under illumination, be stirred continuously and is reacted in certain temperature；
Solution after reaction is washed, separated and precipitated, the dry precipitating obtains ZnS nanosheet；
Wherein, the L in ZnS- (L) n is the compound comprising mono amino or polyamino, n 0.5-1.
2. preparation method according to claim 1, which is characterized in that the n in ZnS- (L) n is 0.5.
3. preparation method according to claim 1, which is characterized in that the n in ZnS- ((the L)) n is 1.
4. preparation method according to claim 1, which is characterized in that the suspension is placed in the choosing of the light source under illumination
From one of mercury lamp, xenon lamp and sunlight or multiple combinations.
5. preparation method according to claim 1, which is characterized in that the suspension is placed in the light application time under illumination
For 2-50h.
6. preparation method according to claim 1, which is characterized in that the certain temperature is 2-30 DEG C.
7. preparation method according to claim 1, which is characterized in that the ZnS nanosheet with a thickness of 0.5-20nm, put down
Face is having a size of 10nm-10 μm.
8. preparation method according to claim 1, which is characterized in that the quality of ZnS- (L) the n presoma is 5-
500mg。
9. preparation method according to claim 1, which is characterized in that the washing uses deionized water and/or ethyl alcohol.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015137511A1 (en) * | 2014-03-11 | 2015-09-17 | Nitto Denko Corporation | Photocatalytic element |
| CN107265495A (en) * | 2017-07-20 | 2017-10-20 | 济南大学 | Non-template method prepares zinc sulphide microballoon |
| CN107381620A (en) * | 2017-08-07 | 2017-11-24 | 中国科学技术大学 | A kind of zinc sulphide/diethylenetriamine hydridization and zinc sulphide ultrathin nanometer band and preparation method thereof |
-
2019
- 2019-05-10 CN CN201910389618.4A patent/CN109987624A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015137511A1 (en) * | 2014-03-11 | 2015-09-17 | Nitto Denko Corporation | Photocatalytic element |
| CN107265495A (en) * | 2017-07-20 | 2017-10-20 | 济南大学 | Non-template method prepares zinc sulphide microballoon |
| CN107381620A (en) * | 2017-08-07 | 2017-11-24 | 中国科学技术大学 | A kind of zinc sulphide/diethylenetriamine hydridization and zinc sulphide ultrathin nanometer band and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| AGILEO HERNA´NDEZ-GORDILLO ET AL.: "An efficient ZnS-UV photocatalysts generated in situ from ZnS(en)0.5 hybrid during the H2 production in methanole water solution", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》 * |
| WENHUI FENG ET AL.: "Grain boundary engineering in organic-inorganic hybrid semiconductor ZnS(en)0.5 for visible-light photocatalytic hydrogen production", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
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