CN101402856B - Surface finishing method for copper ion doped zinc sulfide nano-material - Google Patents

Surface finishing method for copper ion doped zinc sulfide nano-material Download PDF

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Publication number
CN101402856B
CN101402856B CN2008101596026A CN200810159602A CN101402856B CN 101402856 B CN101402856 B CN 101402856B CN 2008101596026 A CN2008101596026 A CN 2008101596026A CN 200810159602 A CN200810159602 A CN 200810159602A CN 101402856 B CN101402856 B CN 101402856B
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China
Prior art keywords
copper ion
ion doped
zinc sulfide
sulfide nano
doped zinc
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CN2008101596026A
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CN101402856A (en
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曹立新
孙远光
苏革
柳伟
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Ocean University of China
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Ocean University of China
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Abstract

The invention discloses a surface decoration method for a zinc sulphide nanometer material mixed with copper ions and is characterized by including the steps of: weighing a zinc sulphide nanometer grain sample mixed with the copper ions, adding the sample into de-ionized water, dispersing the sample by ultra audible sound, adjusting the pH value, dropping ethylsilicate under stirring and continuously stirring after finishing dropping; growing the silicon dioxide generated by hydrolyzing the ethylsilicate on the surface of the zinc sulphide nanometer grain by taking the zinc sulphide nanometer grain mixed with the copper ions as a crystal nucleus for beginning to realize the decoration of the silicon dioxide to the surface of the zinc sulphide nanometer grain mixed with the copper ions; then obtaining a deposit through centrifugation, using the de-ionized water and absolute ethyl alcohol to wash for removing unreacted matters and byproducts; and obtaining the zinc sulphide nanometer material mixed with copper ions and decorated by the silicon dioxide through vacuum drying. The surface decoration method has the advantages that the surface states of the zinc sulphide nanometer material mixed with copper ions are reduced through surface decoration, luminescent idlertransition channels are reduced and the luminescent intensity can achieve 1.82 to 5.72 times than that before decoration.

Description

A kind of surface modification method of copper ion doped zinc sulfide nano-material
Technical field
The present invention relates to a kind of luminescent material, specifically relate to a kind of surface modification method of copper ion doped zinc sulfide nano-material.
Background technology
Nano luminescent material makes it have advantage in application in form and qualitative characteristics, as can significantly improving the homogeneity that cathode tube is coated with screen, helps to improve the sharpness that is coated with screen quality and demonstration; Can be complementary etc. with nano electron device.But the exhibiting high surface attitude that the nano luminescent material particle surface exists is mostly to luminous quenching effect, cause the luminous efficiency of nano material extremely low, seriously hindered the practicalization of nano luminescent material, realized that therefore the control to nano luminescent material particle surface attitude is the key that improves the nano material luminous efficiency.Existing copper ion doped zinc sulphide materials has a wide range of applications in the demonstration field as green luminescent material, but behind the nanometer, because the quenching effect of surface state, luminous efficiency is very low, and how the control surface attitude improves luminous intensity and becomes problem anxious to be solved.
Summary of the invention
The surface modification method that the purpose of this invention is to provide a kind of copper ion doped zinc sulfide nano-material, can reduce the surface state of copper ion doped zinc sulfide nano-material particle to luminous quenching effect, to improve the luminous intensity of copper ion doped zinc sulfide nano-material.
A kind of surface modification method of copper ion doped zinc sulfide nano-material, it is characterized in that at first taking by weighing copper ion doped Zinc sulfide nano-particle sample, add in the deionized water, ultra-sonic dispersion 1-3h, regulate the pH value with alkali then, under agitation drip tetraethyl silicate, after being added dropwise to complete, continue to stir 20-40min; The silicon-dioxide that is generated by silicate hydrolyzate is that nucleus is grown in its surface with copper ion doped Zinc sulfide nano-particle, begins to realize the modification of silicon-dioxide to copper ion doped Zinc sulfide nano-particle surface; Centrifugal with the rotating speed of 4000-6000rpm then, obtain throw out, and wash 3-5 time respectively, to remove unreacted matters and byproduct with deionized water and dehydrated alcohol; At 60-80 ℃ of following vacuum-drying 2-5h, promptly obtain silicon dioxide modified copper ion doped zinc sulfide nano-material at last.
The invention has the advantages that copper ion doped zinc sulfide nano-material surface modification has reduced surface state, reduced luminous radiationless transition channel, luminous intensity can reach 1.82-5.72 times before modifying.
Embodiment
During operation, at first taking by weighing copper ion doped concentration is that 0.1-2.5mol%, grain size are the copper ion doped Zinc sulfide nano-particle sample of 1-80nm, join in the deionized water, controlling the copper ion doped concentration of Zinc sulfide nano-particle in water is 0.005-0.05mol/L, ultra-sonic dispersion 1-3h, regulating pH with alkali then is 9.5-10.5, under agitation the speed with 10-30 second/drip drips tetraethyl silicate, the mol ratio of tetraethyl silicate and copper ion doped ZnS nanoparticle is controlled at 2-12:1, after being added dropwise to complete, continue to stir 20-40min.The silicon-dioxide that is generated by the TEOS hydrolysis is that nucleus is grown on its surface with the ZnS:Cu nanoparticle, begins to realize SiO 2Modification to the ZnS:Cu nanoparticle surface.Centrifugal with the rotating speed of 4000-6000rpm then, obtain throw out, and wash 3-5 time respectively, to remove unreacted matters and byproduct with deionized water and dehydrated alcohol.At 60-80 ℃ of following vacuum-drying 2-5h, promptly obtain silicon dioxide modified copper ion doped zinc sulfide nano-material at last.
Embodiment 1
At first taking by weighing copper ion doped concentration is that 0.2mol%, grain size are the copper ion doped ZnS nanoparticle sample of 4.6nm, join in the deionized water, controlling the copper ion doped concentration of ZnS nanoparticle in water is 0.01mol/L, ultra-sonic dispersion 2h, regulating pH with ammoniacal liquor then is 10, under agitation dropwise drips tetraethyl silicate with the 20 seconds/speed of dripping, and the mol ratio of tetraethyl silicate and copper ion doped ZnS nanoparticle is controlled at 4.5:1, after being added dropwise to complete, continue to stir 30min.Centrifugal with the rotating speed of 5000rpm then, obtain throw out, and wash respectively 3 times, to remove unreacted matters and byproduct with deionized water and dehydrated alcohol.At last at 80 ℃ of following vacuum-drying 3h, the SiO that obtains 2The copper ion doped zinc sulfide nano-material of modifying, its luminous enhancing that is positioned at 530-550nm are 2.85 times before the finishing.
Under similarity condition, the mol ratio that only changes tetraethyl silicate and copper ion doped ZnS nanoparticle is 6.75:1 and 9.0:1, the SiO that obtains 2The copper ion doped zinc sulfide nano-material of modifying, its luminous enhancing that is positioned at 530-550nm are 5.72 and 3.96 times before the finishing.As seen, the mol ratio of tetraethyl silicate and copper ion doped ZnS nanoparticle is not to be the bigger the better.
Embodiment 2
According to the condition of embodiment 1, the rate of addition that only changes tetraethyl silicate is 10 seconds/, the SiO that obtains 2The copper ion doped zinc sulfide nano-material of modifying, its luminous enhancing that is positioned at 530-550nm are 1.92 times before the finishing.
Embodiment 3
According to the condition of embodiment 1, only changing pH is 9.5, the SiO that obtains 2The copper ion doped zinc sulfide nano-material of modifying, its luminous enhancing that is positioned at 530-550nm are 2.43 times before the finishing.

Claims (2)

1. the surface modification method of a copper ion doped zinc sulfide nano-material, it is characterized in that at first taking by weighing copper ion doped Zinc sulfide nano-particle sample, add in the deionized water, ultra-sonic dispersion 1-3h, regulate the pH value with alkali then, under agitation drip tetraethyl silicate, after being added dropwise to complete, continue to stir 20-40min; The silicon-dioxide that is generated by silicate hydrolyzate is that nucleus is grown in its surface with copper ion doped Zinc sulfide nano-particle, begins to realize the modification of silicon-dioxide to copper ion doped Zinc sulfide nano-particle surface; Centrifugal with the rotating speed of 4000-6000rpm then, obtain throw out, and wash 3-5 time respectively, to remove unreacted matters and byproduct with deionized water and dehydrated alcohol; At 60-80 ℃ of following vacuum-drying 2-5h, promptly obtain silicon dioxide modified copper ion doped zinc sulfide nano-material at last; The described copper ion doped concentration of Zinc sulfide nano-particle in deionized water is 0.005-0.05mol/L; The mol ratio of described tetraethyl silicate and copper ion doped Zinc sulfide nano-particle is 2-12: 1; The speed of described dropping tetraethyl silicate is 10-30 second/drip.
2. the surface modification method of copper ion doped zinc sulfide nano-material according to claim 1 is characterized in that described pH value scope is 9.5-10.5.
CN2008101596026A 2008-11-01 2008-11-01 Surface finishing method for copper ion doped zinc sulfide nano-material Expired - Fee Related CN101402856B (en)

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CN101402856B true CN101402856B (en) 2011-07-27

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EP2527309B1 (en) 2011-05-24 2016-08-03 Rohm and Haas Company Improved quality multi-spectral zinc sulfide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1632050A (en) * 2004-11-16 2005-06-29 彩虹集团电子股份有限公司 Method for producing phosphor powder
CN101177551A (en) * 2007-11-15 2008-05-14 电子科技大学 Method for preparing silica modified zinc sulfide nano material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1632050A (en) * 2004-11-16 2005-06-29 彩虹集团电子股份有限公司 Method for producing phosphor powder
CN101177551A (en) * 2007-11-15 2008-05-14 电子科技大学 Method for preparing silica modified zinc sulfide nano material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
吴峰 等.pH值对电致发光粉表面包覆SiO2膜的影响.《河北大学学报(自然科学版)》.2003,第23卷(第1期),25-28. *
姚渊 等.微乳液法制备二氧化硅包覆ZnS:Mn/CdS纳米晶.《人工晶体学报》.2006,第35卷(第2期), *

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