CN106319632A - Zinc sulfide twin nanosphere and preparation method thereof - Google Patents

Zinc sulfide twin nanosphere and preparation method thereof Download PDF

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Publication number
CN106319632A
CN106319632A CN201610619304.5A CN201610619304A CN106319632A CN 106319632 A CN106319632 A CN 106319632A CN 201610619304 A CN201610619304 A CN 201610619304A CN 106319632 A CN106319632 A CN 106319632A
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twin
nanosphere
zinc sulfide
preparation
lamellae
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CN106319632B (en
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张俊
胡光
崔玉
蒋青松
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Huaiyin Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
    • 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
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a zinc sulfide twin nanosphere and a preparation method thereof. The twin nanosphere is prepared by dissolving L-cysteine and zinc acetate into deionized water through a hydrothermal method. The microstructure of the twin nanosphere is composed of closely-layered nanocrystals, high-density twin lamellae with different orientations exist in the crystals, the twin lamellae with the same orientation are mutually parallel, and the length of the twin lamellae ranges from 10 nm to 20 nm. The twin nanosphere can be conveniently prepared, and the yield is high; a reference method is provided for preparation of other twin nanospheres, and a certain material basis is provided for research on the twin nanospheres.

Description

A kind of zinc sulfide twin nanosphere and preparation method thereof
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of zinc sulfide twin nanosphere and preparation method thereof.
Background technology
Nano material has big specific surface area, and along with the decline of particle diameter, surface atom number, surface energy and surface tension are anxious Sharp increase adds, and shows the feature of small-size effect, quantum size effect, skin effect and macro quanta tunnel effect etc., material Magnetic performance, electric property, optical property and the mechanical property etc. of material have the biggest difference with macroscopic material, at dye cell, light The aspects such as electronic sensor have broad application prospects, so the synthetic method that exploitation nano material is new, develop new capability side There is great meaning in face.In metal-oxide semiconductor (MOS), introduce suitable defect such as dislocation, twin etc. also to affect or strengthen Its performance, to constructing, nano-device based on this kind of material is extremely important.
As a kind of important semi-conducting material, ZnS is always the focus of scientific research.Material about zinc sulfide has ZnS nano wire, ZnS nano belt etc..ZnS nano material can be prepared by multiple method, such as template, hydro-thermal method, chemistry gas Phase sedimentation etc., but the most relatively difficult in terms of twin growth, and growth cost is the highest.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of zinc sulfide twin nanosphere and preparation method thereof, this Bright by simple one-step preppn process, can the most controllably prepare zinc sulfide twin nanosphere, twin for other The preparation of brilliant nanosphere provides a reference method.
The present invention is achieved by the following technical solutions:
A kind of zinc sulfide twin nanosphere, its microstructure is made up of laminar nano crystal grain, exists highdensity at intra-die The twin lamellae structure of different orientation, is parallel to each other between equally oriented twin lamellae, twin lamellae a length of 10～20nm, Width is 2～5nm.
The further improvement project of the present invention is:
The preparation method of a kind of zinc sulfide twin nanosphere, comprises the steps:
Step one, is dissolved in zinc acetate and Cys deionized water, after aqueous slkali regulation pH value, stirs；
Step 2, puts in reactor by above-mentioned mixed solution, reacting by heating, reaction terminate after, cooling, centrifuge washing, be dried, receipts The solid of collection is zinc sulfide twin nanosphere.
The mol ratio of described zinc acetate and Cys is 1:2.5～3.6.
The aqueous slkali of described regulation pH value is ammonia spirit.
Described pH value range is 9～11.
The temperature of described reacting by heating is 140 DEG C～160 DEG C, and the time is 4～12h.
The invention have the benefit that
Preparation method of the present invention is simple, uses one-step method to complete, and repeatability preferably, can the most controllably be prepared Zinc sulfide twin nanosphere, low cost, yield is big and pollution-free, and sample purity is high, favorable repeatability, it is not necessary to add other and urge Agent.
Zinc sulfide twin nanosphere prepared by the present invention, good stability, at absorbed layer, the photoelectron device of solaode The field such as part, semiconductor transducer has bigger application potential.
Preparation method of the present invention is that the research of the growth mechanism of zinc sulfide twin nanosphere provides material base, for research The twin nanosphere of other material provides a Research foundation.
Accompanying drawing explanation
The zinc sulfide twin nanosphere scanning electron microscope diagram of Fig. 1 embodiment 1 preparation.
The zinc sulfide twin nanosphere transmission electron microscope figure of Fig. 2 embodiment 1 preparation.
The zinc sulfide twin nanosphere twin structure high resolution transmission electron microscopy figure of Fig. 3 embodiment 1 preparation.
The zinc sulfide twin nanosphere X-ray diffraction spectrogram of Fig. 4 embodiment 1 to 3 preparation.
Detailed description of the invention
Embodiment 1
The Cys of the zinc acetate of 1mol Yu 2.5mol is dissolved in deionized water, until completely dissolved, with the ammonia of 25% Regulation pH value, to 9, continues to stir half an hour, is put into by above-mentioned mixed solution in 60ml tetrafluoroethene water heating kettle, and at 140-160 In DEG C muffle electric furnace, after reacting 6 hours, close heating power supply, naturally cool to room temperature.Prepared by said method products obtained therefrom spend After ionized water and washes of absolute alcohol are clean, gained white powder is zinc sulfide twin nanosphere.
As it is shown on figure 3, the microstructure of zinc sulfide twin nanosphere is made up of laminar nano crystal grain, exist at intra-die The twin lamellae structure of highdensity different orientation, is parallel to each other between equally oriented twin lamellae, and twin lamellae is a length of 10～20nm, width is 2～5nm.
Embodiment 2
The Cys of the zinc acetate of 1mol Yu 3mol is dissolved in deionized water, until completely dissolved, with 35% ammonia Regulation pH value, to 10, continues to stir half an hour, is put into by above-mentioned mixed solution in 60ml tetrafluoroethene water heating kettle, and at 140- In 160 DEG C of muffle electric furnaces, after reacting 8 hours, close heating power supply, naturally cool to room temperature.Said method is prepared products obtained therefrom With deionized water and washes of absolute alcohol clean after, gained white powder is zinc sulfide twin nanosphere.
Embodiment 3
The Cys of the zinc acetate of 1mol Yu 3.6mol is dissolved in deionized water, until completely dissolved, with the ammonia of 30% Regulation pH value, to 11, continues to stir half an hour, is put into by above-mentioned mixed solution in 60ml tetrafluoroethene water heating kettle, and at 140- In 160 DEG C of muffle electric furnaces, after reacting 12 hours, close heating power supply, naturally cool to room temperature.Said method is prepared products obtained therefrom With deionized water and washes of absolute alcohol clean after, gained white powder is zinc sulfide twin nanosphere.

Claims (6)

1. a zinc sulfide twin nanosphere, it is characterised in that: microstructure is made up of laminar nano crystal grain, deposits at intra-die In the twin lamellae structure of different orientation, be parallel to each other between equally oriented twin lamellae, twin lamellae a length of 10～ 20nm, width is 2～5nm.
2. the preparation method of a zinc sulfide twin nanosphere, it is characterised in that comprise the steps:
Step one, is dissolved in zinc acetate and Cys deionized water, after aqueous slkali regulation pH value, stirs；
Step 2, puts in reactor by above-mentioned mixed solution, reacting by heating, reaction terminate after, cooling, centrifuge washing, be dried, receipts The solid of collection is zinc sulfide twin nanosphere.
The preparation method of a kind of zinc sulfide twin nanosphere the most according to claim 2, it is characterised in that: described zinc acetate It is 1:2.5～3.6 with the mol ratio of Cys.
The preparation method of a kind of zinc sulfide twin nanosphere the most according to claim 2, it is characterised in that: described regulation pH The aqueous slkali of value is ammonia spirit.
The preparation method of a kind of zinc sulfide twin nanosphere the most according to claim 2, it is characterised in that: described pH value model Enclose is 9～11.
The preparation method of a kind of zinc sulfide twin nanosphere the most according to claim 2, it is characterised in that: described heating is anti- The temperature answered is 140 DEG C～160 DEG C, and the time is 4～12h.
CN201610619304.5A 2016-08-02 2016-08-02 A kind of zinc sulphide twin nanosphere and preparation method thereof Active CN106319632B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109160538A (en) * 2018-11-08 2019-01-08 北京高压科学研究中心 The method for preparing superstructure twin material

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Publication number Priority date Publication date Assignee Title
CN1762823A (en) * 2005-09-02 2006-04-26 清华大学 Zinc sulfide microsphere synthesis method
CN101186816A (en) * 2007-11-16 2008-05-28 河南科技大学 Nano-crystal with core-shell structure and preparation method thereof
CN101519223A (en) * 2009-04-10 2009-09-02 武汉理工大学 One-step template-free method for preparing a great amount of monodisperse ZnS hollow nanospheres
CN102241976A (en) * 2011-05-12 2011-11-16 北京化工大学 Method for preparing ZnS quantum dot modified by mercaptoacetic acid
CN104108744A (en) * 2014-07-21 2014-10-22 陕西科技大学 Method for preparing ZnS nano-particles with microwave hydrothermal method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1762823A (en) * 2005-09-02 2006-04-26 清华大学 Zinc sulfide microsphere synthesis method
CN101186816A (en) * 2007-11-16 2008-05-28 河南科技大学 Nano-crystal with core-shell structure and preparation method thereof
CN101519223A (en) * 2009-04-10 2009-09-02 武汉理工大学 One-step template-free method for preparing a great amount of monodisperse ZnS hollow nanospheres
CN102241976A (en) * 2011-05-12 2011-11-16 北京化工大学 Method for preparing ZnS quantum dot modified by mercaptoacetic acid
CN104108744A (en) * 2014-07-21 2014-10-22 陕西科技大学 Method for preparing ZnS nano-particles with microwave hydrothermal method

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HUA TONG等: "Self-Assembled ZnS Nanostructured Spheres: Controllable Crystal Phase and Morphology", 《JOURNAL OF PHYSICAL CHEMISTRY C》 *
SULAWAN KAOWPHONG等: "The effect of solvents on ZnS nanostructures synthesized by biomolecule-assisted solvothermal method", 《MATERIALS LETTERS》 *
XIAO WU等: "Facile synthesis of ZnS nanostructured spheres and their photocatalytic properties", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
YANGPING HONG等: "Influence of lattice integrity and phase composition on the photocatalytic hydrogen production efficiency of ZnS nanomaterials", 《NANOSCALE》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109160538A (en) * 2018-11-08 2019-01-08 北京高压科学研究中心 The method for preparing superstructure twin material
CN109160538B (en) * 2018-11-08 2020-11-06 北京高压科学研究中心 Method for preparing superstructure twin crystal material

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