CN102674433A - Method for preparing zinc sulfide nanopowder - Google Patents
Method for preparing zinc sulfide nanopowder Download PDFInfo
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- CN102674433A CN102674433A CN2012101916961A CN201210191696A CN102674433A CN 102674433 A CN102674433 A CN 102674433A CN 2012101916961 A CN2012101916961 A CN 2012101916961A CN 201210191696 A CN201210191696 A CN 201210191696A CN 102674433 A CN102674433 A CN 102674433A
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Abstract
The invention discloses method for preparing zinc sulfide nanopowder and relates to the technical field of processes for chemically synthesizing nano materials by a hydrothermal method. The zinc sulfide nanopowder is prepared through steps of reaction, heating, washing, drying and the like by taking two kinds of solid powder, namely ZnCl2.H2O and S powder as raw materials and hydrazine as a reducing agent. The prepared zinc sulfide powder has the advantages of high purity, uniform size, high dispersibility, environment friendliness and the like; the process is safe; assisting solutions and a product are easily treated in the process; and therefore, the method is very wide in application prospect.
Description
Technical field
The present invention relates to hydrothermal chemistry nano materials Technology field, relate in particular to the preparation method of the synthetic zinc sulfide nano powder of hydrothermal method.
Background technology
Nano material is meant the material that in three-dimensional space, has at least one dimension to be in nanoscale scope 1～100nm or to be made up of as elementary cell them.Nano material is that Condensed Matter Physics has proposed many new problems because the nano material size is little, quantum size effect very significantly, this makes that the physical propertiess such as light, heat, electricity, magnetic of nano material system are different with conventional material, many new kink characteristics occur; Another important feature of nano material is a surface effects in addition.Along with size reduces, specific surface increases greatly, causes the chemical property of nanometer system and Chemical Equilibria Systems very big difference to occur.Nanometer synthesizes the development type material new approach and new thinking is provided.Nano semiconductor material is that the superior semiconducter device of processability provides the foundation.
ZnS is an II-VI family wide bandgap semiconductor compound-material; The white powder solid; Six sides and cube two kinds of crystalline structure are arranged; Energy gap is about 3.5～3.8eV, and ZnS is widely used in fields such as flat-panel monitor, electroluminescent, nonlinear optics device, cathodoluminescence, light emitting diode, solar cell, photochemical catalysis, transmitter and laser.Other there are some researches show that the ZnS particulate band gap of 3nm is 4.13eV, and tangible blue shift takes place, and be a kind of potential photonic material, and nanometer ZnS also has outstanding photochemical catalysis effect.So the preparation research of nanometer ZnS has crucial meaning to the photoelectric device industry.
The method for preparing at present nano material has a lot, like liquid phase methods such as vapor phase process such as physical vapor deposition, chemical vapour deposition, sputtering method and the precipitator method, spray method, sol-gel method, chemical radiations.The complex process that these methods have; Temperature of reaction and long reaction time; The method reaction process toxic that has is big, environmental pollution is serious; The method gained nano material that has is prone to reunite, bad dispersibility, the pattern of wayward nano material and dimensional homogeneity, and the nano-zinc sulfide phase composite of the concrete prepared that is adopted in the method that has is impure.Shape and the inhomogeneous specific surface area that affects nano material of size, thereby performance has than big difference; When purity difference, because the dephasign that occurs is another kind of material, thereby its performance can be different with single-phase material, have than big-difference at aspects such as optical characteristics, conductivities, and these physicalies are crucial to semiconductor material.
The prior art approaching with this patent has:
[1]R.Saravanan，S.Saravanakumar，S.Lavanya，Growth?and?local?structure?analysis?of?ZnS?nanoparticles，Physica?B?405(2010)3700-3703.
Reported in the literary composition with sol-gel method to prepare the ZnS nano particle, and the ZnS nano particle has been characterized with XRD and SEM.
[2]Cun?Li，Xiaogang?Yang，Baojun?Yang，Growth?of?microtubular?complexes?as?precursors?to?synthesize?nanocrystalline?ZnS?and?CdS，Journal?of?Crystal?Growth?291(2006)45-51.
Article has reported that with compound microtubule be precursor, with ZnCl
2, CdCl
2Reaching S simple substance is raw material, synthesizes ZnS, CdS nanocrystal with hydrothermal method respectively at 120 ℃ of insulation 12-24h.
[3]Feng?Wei，Guicun?Li，Zhikun?Zhang，Hydrothermal?synthesis?of?spindle-like?ZnS?hollow?nanostructures，Materials?Research?Bulletin?40(2005)1402-1407.
Mainly reported spindle shape ZnS nanometer, and the structure and the pattern of its microcosmic characterized with the synthetic hollow of hydrothermal method.
[4]Ondrej?Kozák，Petr?Praus，Kamila?Kocí，Preparation?and?characterization?of?ZnS?nanoparticles?deposited?onmontmorillonite，Journal?of?Colloid?and?Interface?Science?352(2010)244-251.
Having described with zinc acetate, zinc sulfate and sodium sulphite etc. is raw material, on smectite, deposit the ZnS nano particle, through measuring particulate diameter 3～5nm.
[5]S.D.Sartale，B.R.Sankapal，M.Lux-Steiner，Preparation?of?nanocrystalline?ZnS?by?a?new?chemical?bath?deposition?route，Thin?Solid?Films?480-481(2005)168-172.
Reported with chemical bath deposition and prepared fine and close, uniform nano-crystal film.Raw material is zinc salt, thiocarbamide etc., and wherein thiocarbamide is the effect that complexing agent is played in the sulphur source again.
Though the present invention and above technology preparation all are the nanometer ZnSs of preparation, very big difference are all arranged, so product has very big difference on structure, pattern, size in raw material, technical process.
Summary of the invention
The present invention is in order to solve the deficiency of prior art, and the preparation method who has invented a kind of zinc sulfide nano powder.
The present invention adopts the hydrothermal method synthesis technique to prepare the zinc sulfide nano powder, with ZnCl
22H
2O, sulphur simple substance powder are raw material, and the stoichiometric ratio and the concentration of strict control raw material are reductive agent with the hydrazine, and heating at a lower temperature makes raw material carry out the reaction of the concurrent intercrescence one-tenth of coreduction, and can obtain title product through cleaning, filter and drying.
Concrete preparation method of the present invention comprises the step of following order:
A. with 2.0～5.0 parts of ZnCl
22H
2O, two kinds of pressed powder uniform mixing of 1.0～2.5 parts of sulphur powder are incorporated as 20～45 parts of hydrochloric acid, 140～160 parts of absolute ethyl alcohols and 350～380 parts of deionized waters again;
B. pour said mixture solution into autoclave, add 20～45 parts of hydrazines again;
C. aforesaid reaction vessel is heated between 160～200 ℃, soaking time 20～90 hours, cool to room temperature takes out then;
D. with reacted solution through the water system filtering with microporous membrane, successively use deionized water and absolute ethyl alcohol repetitive scrubbing, filtering separation, removal impurity washs till the neutrality;
E. gains after the above-mentioned washing are dry, obtain the zinc sulfide nano powder.
Mix powder uniform mixing in deionized water among the above-mentioned steps a, it is more abundant that employing ultrasonic vibration and the mode that stirs make it dissolving.
The purity of the hydrazine among the above-mentioned steps b adopts 85% or 80%.
Autoclave among the above-mentioned steps b adopts the teflon-lined reaction kettle.
The drying of washing back gains is 50～80 ℃ of oven dry down among the above-mentioned steps e.
Drying among the above-mentioned steps e adopts vacuum drying oven to carry out drying.
Facies analysis and morphology analysis show that gained zinc sulfide nano powder of the present invention is single-phase powder, and its shape is even with size, and particle diameter is between 80～100nm.With similar compared with techniques, gained zinc sulfide nano powder purity of the present invention is high, good dispersivity, and technological process safety, process assisted solution and product be prone to handle, pollution-free etc., so this method has boundless application prospect.
Description of drawings
Embodiment
With 4.242 parts of ZnCl
22H
2O and two kinds of pressed powder uniform mixing of 1.000 parts of sulphur powder add 30.303 parts hydrochloric acid again, 151.515 parts of ethanol, and 363.636 parts of deionized waters adopt ultrasonic vibration and the mode that stirs makes it uniform mixing.Pour said mixture solution into the teflon-lined autoclave, add 30.303 parts of 85% hydrazines again.Aforesaid reaction vessel is heated between 200 ℃, soaking time 90 hours, cool to room temperature takes out then.Reacted solution through the water system filtering with microporous membrane, is successively used deionized water and absolute ethyl alcohol repetitive scrubbing, filtering separation, and removal impurity washs till the neutrality.With dry in the vacuum drying oven of gains under 70 ℃ after the above-mentioned washing, obtain zinc sulfide powder.Through detecting, the purity of gained ZnS is 100%.
Embodiment 2
With 4.242 parts of ZnCl
22H
2O and two kinds of pressed powder uniform mixing of 1.000 parts of sulphur powder add 30.303 parts hydrochloric acid again, 151.515 parts of ethanol, and 363.636 parts of deionized waters adopt ultrasonic vibration and the mode that stirs makes it uniform mixing.Pour said mixture solution into the teflon-lined autoclave, add 30.303 parts of 85% hydrazines again.Aforesaid reaction vessel is heated between 200 ℃, soaking time 45 hours, cool to room temperature takes out then.Reacted solution through the water system filtering with microporous membrane, is successively used deionized water and absolute ethyl alcohol repetitive scrubbing, filtering separation, and removal impurity washs till the neutrality.With dry in the vacuum drying oven of gains under 70 ℃ after the above-mentioned washing, obtain zinc sulfide powder.Through detecting, the purity of gained ZnS is 100%.
Claims (4)
1. the preparation method of a zinc sulfide nano powder, this method comprises the step of following order:
A. with 2.0～5.0 parts of ZnCl
22H
2O, two kinds of pressed powder uniform mixing of 1.0～2.5 parts of sulphur powder add hydrochloric acid, absolute ethyl alcohol and deionized water equal solvent uniform mixing again;
B. pour said mixture solution into autoclave, add 20～45 parts of hydrazines again;
C. aforesaid reaction vessel is heated between 160～200 ℃, soaking time 20～90 hours, cool to room temperature takes out then;
D. with reacted solution through the water system filtering with microporous membrane, successively use deionized water and absolute ethyl alcohol repetitive scrubbing, filtering separation, removal impurity washs till the neutrality;
E. gains after the above-mentioned washing are dry, obtain the zinc sulfide nano powder.
2. a kind of according to claim 1 preparation method of zinc sulfide nano powder; The solvent that in mixed powder, adds among the wherein said step a is 20～45 parts of hydrochloric acid; 140～160 parts of absolute ethyl alcohols and 350～380 parts of deionized waters, employing ultrasonic vibration and the mode that stirs make it to dissolve more fully and mix.
3. a kind of according to claim 1 preparation method of zinc sulfide nano powder, the drying of washing back gains is 50～80 ℃ of oven dry down among the wherein said step e.
4. like the preparation method of claim 1 or 3 said a kind of zinc sulfide nano powder, the drying among the wherein said step e adopts vacuum drying oven to carry out drying.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400894A (en) * | 2013-07-09 | 2013-11-20 | 山东建筑大学 | Method for preparing zinc sulfide optoelectronic film |
| CN105016376A (en) * | 2014-04-21 | 2015-11-04 | 渤海大学 | Preparation method of zinc sulfide twin nanobelt |
| CN106006717A (en) * | 2016-05-11 | 2016-10-12 | 南阳理工学院 | Preparing method of ZnS nano aerogel |
| CN107456980A (en) * | 2017-07-07 | 2017-12-12 | 国家纳米科学中心 | A kind of ZnS/ZnO core shell structures and its preparation method and application |
| CN112397671A (en) * | 2019-08-19 | 2021-02-23 | Tcl集团股份有限公司 | Modified zinc sulfide, preparation method thereof and quantum dot light-emitting diode |
| CN113104883A (en) * | 2021-05-06 | 2021-07-13 | 竹山县秦巴钡盐有限公司 | Preparation method of pigment-grade zinc sulfide |
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| CN101575117A (en) * | 2009-05-26 | 2009-11-11 | 陕西师范大学 | Method for thermally preparing solvent of high-orientating diameter adjustable ZnS nano-rod array |
| CN101691241A (en) * | 2009-10-19 | 2010-04-07 | 新疆大学 | Method for growing ZnS single-crystal nanowire bundle |
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2012
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| CN101575117A (en) * | 2009-05-26 | 2009-11-11 | 陕西师范大学 | Method for thermally preparing solvent of high-orientating diameter adjustable ZnS nano-rod array |
| CN101691241A (en) * | 2009-10-19 | 2010-04-07 | 新疆大学 | Method for growing ZnS single-crystal nanowire bundle |
Non-Patent Citations (6)
| Title |
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| 《J. Phys. Chem. C》 20070804 Lanlan Chai et al. "Synthesis of Wurtzite ZnS Nanowire Bundles Using a Solvothermal Technique" 第12658-12662页 1-4 , * |
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| 郑梅琴等: ""不同方法制备的ZnS粉体的光催化性能"", 《福建农林大学学报（自然科学版）》, 15 April 2009 (2009-04-15), pages 439 - 443 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400894A (en) * | 2013-07-09 | 2013-11-20 | 山东建筑大学 | Method for preparing zinc sulfide optoelectronic film |
| CN103400894B (en) * | 2013-07-09 | 2015-12-09 | 山东建筑大学 | A kind of method preparing zinc sulfide optoelectronic film |
| CN105016376A (en) * | 2014-04-21 | 2015-11-04 | 渤海大学 | Preparation method of zinc sulfide twin nanobelt |
| CN105016376B (en) * | 2014-04-21 | 2016-08-24 | 渤海大学 | The preparation method of zinc sulphide twin nanobelt |
| CN106006717A (en) * | 2016-05-11 | 2016-10-12 | 南阳理工学院 | Preparing method of ZnS nano aerogel |
| CN107456980A (en) * | 2017-07-07 | 2017-12-12 | 国家纳米科学中心 | A kind of ZnS/ZnO core shell structures and its preparation method and application |
| CN112397671A (en) * | 2019-08-19 | 2021-02-23 | Tcl集团股份有限公司 | Modified zinc sulfide, preparation method thereof and quantum dot light-emitting diode |
| CN113104883A (en) * | 2021-05-06 | 2021-07-13 | 竹山县秦巴钡盐有限公司 | Preparation method of pigment-grade zinc sulfide |
| CN113104883B (en) * | 2021-05-06 | 2022-06-17 | 竹山县秦巴钡盐有限公司 | Preparation method of pigment-grade zinc sulfide |
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Application publication date: 20120919 |