CN100548887C - A kind of preparation method of micron zinc sulfide powder - Google Patents
A kind of preparation method of micron zinc sulfide powder Download PDFInfo
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- CN100548887C CN100548887C CNB2007100142002A CN200710014200A CN100548887C CN 100548887 C CN100548887 C CN 100548887C CN B2007100142002 A CNB2007100142002 A CN B2007100142002A CN 200710014200 A CN200710014200 A CN 200710014200A CN 100548887 C CN100548887 C CN 100548887C
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Abstract
The invention provides a kind of preparation method of micron order ZnS powder.The concrete steps of this method are: (1) in molar ratio 1: (1.0～2.0) are dissolved in zinc chloride or zinc nitrate and thioacetamide in the deionized water, with hydrochloric acid or nitric acid regulator solution pH value between 1.5～4; (2) ageing at room temperature of above-mentioned solution after 24～48 hours, was refluxed 30～60 minutes at 80～100 ℃, obtain white depositions; (3) the gained throw out is filtered, washs,, obtain the ZnS powder of median size 0.5～3.0 μ m 80 ℃ of oven dry 6 hours.Aqueous solution circumfluence method preparation technology of the present invention is simple, safety, does not need pyroreaction, adopts the ZnS powder diameter of the present invention's preparation bigger, belong to micron order, particle size distribution is even, and granule-morphology is all spherical in shape or subsphaeroidal, can be used as the substrate material of high quality fluorescent material.
Description
Technical field
The present invention relates to the preparation method of micrometre zinc sulphide ZnS powder, belong to the inorganic materials preparing technical field.
Figure viewed from behind technology
Fluorescent material comes into one's own owing to the widespread use in information demonstration and lighting engineering always.Zinc sulphide (ZnS) is a kind of fluorescence host material of unique properties, can obtain the efficient visible radiation of different-waveband by change doping agent wherein.Present stage is that the luminescent material of matrix has been widely used in the multiple instrument with ZnS, as flat-panel monitor, optical excitation diode, solar cell etc.
The size and the distribution of material granule form, granularity are very big to the Effect on Performance of ZnS based luminescent material.In actual applications, the fluorescent material especially granule-morphology of fluorescent powder material has crucial meaning, and the quality of fluorescent material depends on the uniformity coefficient and the particulate pattern of the granularity of powder fully.Basically the requirement to high-quality fluorescent material is that pattern is spherical, and particle size distribution is narrow.At present, the method for preparing nano level ZnS powder is more, is broadly divided into three kinds: solid phase method, liquid phase method and vapor phase process.Yet, showing and lighting field is widely applied is still micron order macrobead (median size＞2 μ m) doped ZnS powder that in information this mainly is because the nanometer ZnS defective is more, various defectives interactions have reduced the luminous efficiency of ZnS fluorescent material.Preparation micron order ZnS powder except that solid phase synthesis at high temperature, do not have additive method, and the size distribution that the high temperature solid-state synthetic method is prepared is inhomogeneous, and pattern is irregular, is difficult to realize the control to granule-morphology and size.
Summary of the invention
The present invention is directed to existing high temperature solid-state method and prepare granule-morphology and the big or small unmanageable problem that micron order ZnS powder exists, the preparation method of a kind of even particle size distribution, granule-morphology micron order ZnS powder spherical in shape is provided.
The present invention adopts aqueous solution circumfluence method to prepare micron order ZnS spherical powder, and concrete steps are as follows:
(1) in molar ratio 1: (1.0～2.0) are dissolved in zinc chloride or zinc nitrate and thioacetamide (TAA) in the deionized water, with hydrochloric acid or nitric acid regulator solution pH value between 1.5～4;
(2) ageing at room temperature of above-mentioned solution after 24～48 hours, was refluxed 30～60 minutes at 80～100 ℃, obtain white depositions;
(3) the gained throw out is filtered, washs,, promptly obtain the ZnS powder of median size 0.5～3.0 μ m 80 ℃ of oven dry 6 hours.
The present invention with zinc chloride or zinc nitrate as the zinc source, with thioacetamide as the sulphur source, adopt aqueous solution circumfluence method, preparation technology is simple, safety, does not need pyroreaction, adopts the ZnS powder diameter of the present invention's preparation bigger, belong to micron order, particle size distribution is even, and granule-morphology is all spherical in shape or subsphaeroidal, can be used as the substrate material of high quality fluorescent material.
Embodiment
Embodiment 1
Take by weighing 1.40 gram zinc chloride (ZnCl respectively
2) and 1 the gram thioacetamide be dissolved in 100 ml deionized water, with hydrochloric acid conditioning solution pH value is 3, ageing is transferred to after 30 hours in the there-necked flask and refluxed 30 minutes at 100 ℃, with the gained throw out filter, washing, 80 ℃ of oven dry got final product in 6 hours the ZnS powder of median size 1.0～1.5 μ m.
Embodiment 2
Take by weighing 1.77 gram zinc chloride (ZnCl respectively
2) and 1 the gram thioacetamide be dissolved in 100 ml deionized water, with nitric acid regulator solution pH value is 2, ageing is transferred to after 30 hours in the there-necked flask at 80 ℃ and refluxed 30 minutes, with the gained throw out filter, washing, 80 ℃ of oven dry got final product in 6 hours the ZnS powder of median size 1.0～2.0 μ m.
Embodiment 3
Take by weighing 3.0 gram zinc nitrate (Zn (NO respectively
3)
26H
2O) and 1 gram thioacetamide be dissolved in 100 ml deionized water, be 2 with the nitric acid adjust pH, ageing refluxed 40 minutes at 100 ℃ after 24 hours, with the gained throw out filter, washing, 80 ℃ dry got final product in 6 hours the ZnS powder of median size 1.0～2.5 μ m.
Embodiment 4
Take by weighing 4.0 gram zinc nitrate (Zn (NO respectively
3)
26H
2O) and 1 gram thioacetamide be dissolved in 100 ml deionized water, be 3 with the hydrochloric acid adjust pH, ageing refluxed 40 minutes at 100 ℃ after 30 hours, with the gained throw out filter, washing, 80 ℃ dry got final product in 6 hours the ZnS powder of median size 0.5～1.5 μ m.
Claims (1)
1. the preparation method of a micron zinc sulfide powder, it is characterized in that: concrete steps are as follows:
(1) in molar ratio 1: (1.0～2.0) are dissolved in zinc chloride or zinc nitrate and thioacetamide in the deionized water, are 1.5～4 with hydrochloric acid or nitric acid regulator solution pH value;
(2) ageing at room temperature of above-mentioned solution after 24～48 hours, was refluxed 30～60 minutes at 80～100 ℃, obtain white depositions;
(3) the gained throw out is filtered, washs,, promptly obtain the ZnS powder of median size 0.5～3.0 μ m 80 ℃ of oven dry 6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100142002A CN100548887C (en) | 2007-04-23 | 2007-04-23 | A kind of preparation method of micron zinc sulfide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100142002A CN100548887C (en) | 2007-04-23 | 2007-04-23 | A kind of preparation method of micron zinc sulfide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101037222A CN101037222A (en) | 2007-09-19 |
| CN100548887C true CN100548887C (en) | 2009-10-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100142002A Expired - Fee Related CN100548887C (en) | 2007-04-23 | 2007-04-23 | A kind of preparation method of micron zinc sulfide powder |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515255A (en) * | 2012-01-09 | 2012-06-27 | 西南大学 | Method for preparing zinc sulfide nanospheres |
| CN103143371A (en) * | 2013-03-18 | 2013-06-12 | 新疆大学 | Solid phase preparation of heterostructured zinc sulfide photocatalyst |
| CN107128940A (en) * | 2017-04-25 | 2017-09-05 | 安徽博硕科技有限公司 | A kind of preparation method of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide |
| CN116947089B (en) * | 2023-09-20 | 2024-01-30 | 广东鑫达新材料科技有限公司 | Metal sulfide, use thereof, and resin composition containing the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462258A (en) * | 2001-05-08 | 2003-12-17 | Lg化学株式会社 | Method for preparing single crystalline ZnS powder for phosphor |
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2007
- 2007-04-23 CN CNB2007100142002A patent/CN100548887C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462258A (en) * | 2001-05-08 | 2003-12-17 | Lg化学株式会社 | Method for preparing single crystalline ZnS powder for phosphor |
| US7153485B2 (en) * | 2001-05-08 | 2006-12-26 | Lg Chem, Ltd. | Method for preparing single crystalline zinc sulfide powder for phosphor |
Non-Patent Citations (2)
| Title |
|---|
| Preparation and Properties of Spherical Zinc SulfideParticles. Richard Williams, P. N. Yocom, F. S. Stofko.J. collid. interface sci.,Vol.106 No.2. 1985 |
| Preparation and Properties of Spherical Zinc SulfideParticles. Richard Williams, P. N. Yocom, F. S. Stofko.J. collid. interface sci.,Vol.106 No.2. 1985 * |
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| CN101037222A (en) | 2007-09-19 |
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