CN1468936A - Electroluminescent composite coated ZnS:Cu/Cu.Mn material and its prepn process - Google Patents
Electroluminescent composite coated ZnS:Cu/Cu.Mn material and its prepn process Download PDFInfo
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- CN1468936A CN1468936A CNA031124127A CN03112412A CN1468936A CN 1468936 A CN1468936 A CN 1468936A CN A031124127 A CNA031124127 A CN A031124127A CN 03112412 A CN03112412 A CN 03112412A CN 1468936 A CN1468936 A CN 1468936A
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- electroluminescent
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Abstract
The composite coated electroluminescent ZnS:Cu/Cu.Mn material has spherical crystalline electroluminescent ZnS:xCu.yMn material of 15-30 micron size coated with amorphous compact alumina layer. The coating alumina layer has the weight of 4-8 % of the electroluminescent ZnS:xCu.yMn material and is formed 60-80 % weight via liquid phase chemical deposition process and 20-40 % weight via metal organic compound vapor chemical deposition process. The coated electroluminescent ZnS:Cu/Cu.Mn material has low cost, and less failure caused by the action of water molecule.
Description
(1) technical field
The invention belongs to the inorganic materials scientific domain, particularly the employed coated ZnS of electroluminescent device: Cu or ZnS: Cu.Mn luminescent material and preparation method thereof.
(2) background technology
With ZnS: Cu or ZnS: Cu.Mn is that the AC electroluminescence display device of luminescent material has distinguishing features such as the emission of surface cold light, reduce power consumption, size be thin, in light weight and obtains increasingly extensive application.But this class material owing to water molecules and action of ultraviolet ray in the outside atmosphere, is separated out sulphur or zinc easily from lattice when alternating electric field excites work, cause the electroluminescent miopragia, even loses efficacy.Adopt coating technology, at ZnS: Cu or ZnS: it is to improve the electroluminescent device photoelectric transformation efficiency, the effective way that prolongs the effective luminescent lifetime of device that the Cu.Mn particle surface forms fine and close integument.The processing method that U.S. patent of invention US5958591 adopts the chemical vapour deposition of organometallics trimethyl aluminium is to ZnS: Cu or ZnS: the Cu.Mn material has obtained the higher compactness surface covered effect of transmittance; U.S. patent of invention US5593782 has introduced the method that adopts the vapour deposition of organometallics trimethyl aluminium hydrolysis reaction to prepare the coated electroluminescent material.Above-mentioned technological method causes cladded type electroluminescent material production cost higher owing to adopt expensive organometallics and complicated vapor deposition apparatus to realize all coating production.
(3) summary of the invention
The present invention is directed to the shortcoming of prior art, provide a kind of compound coated ZnS: Cu/Cu.Mn electroluminescent material and preparation method thereof.
Technical scheme of the present invention is as follows:
Compound coated ZnS of the present invention: the Cu/Cu.Mn electroluminescent material is to be the ball-type crystalline state ZnS of 15 μ m～30 μ m at particle diameter: the particle surface of xCu.yMn electroluminescent material has coated non-type aluminum oxide (Al
2O
3) fine and close integument.X=0.001～0.010 wherein, y=0.000～0.005, aluminum oxide (Al
2O
3) weight of integument is ZnS: 4%～8% of xCu.yMn electroluminescent material weight.
Above-mentioned aluminum oxide (Al
2O
3) the parcel amount 60%～80%, finish by the liquid phase chemical deposition method for coating, 20%～40%, finish by organometallics chemical vapor deposition method for coating.
Above-mentioned ball-type crystalline state ZnS: the xCu.yMn electroluminescent material can pass through prior art for preparing, also can obtain as follows:
(1) preparation of the mixing solutions of activator and auxiliary agent, activator are CuCl
2, CuSO
4Or MnCl
2, press ZnS: the xCuyMn mol ratio, x=0.001～0.010, y=0.000～0.005, auxiliary agent is NaCl, MgCl
2Or BaCl
2, auxiliary agent and ZnS weight ratio 0.005～0.02: 1; With this mixing solutions and ZnS powder mixing, drying and dehydrating adds the solid sulfur powder again, and activator, auxiliary agent and ZnS mixed powder and solid sulfur powder weight be than 1: 0.02～0.05, compound;
(2) in compound was packed the high purity aluminium oxide crucible into, in 1100 ℃～1150 ℃ insulations 2.5～3.5 hours, naturally cooling got the luminescent material work in-process; Work in-process luminescent material ball milling, pickling, water rinse, drying gets the work in-process fine powder;
(3) with ZnO or ZnSO
4Powder adds in the work in-process fine powder in the ratio of 3%～7% weight percent of work in-process fine powder and reacts, and perhaps again and press the work in-process fine powder: activator=1: 0.001～0.002 weight ratio adds activator CuCl
2, CuSO
4, CuBr
2Or MnCl
2, mixing, drying, the porcelain boat of packing into is in atmosphere furnace, at N
2+ H
2Twice firing under the S atmosphere; Twice firing products obtained therefrom superoxol and ammonia scrubbing, the rinsed with deionized water after drying promptly obtains ball-type crystalline state ZnS: the xCuyMn electroluminescent material.
The compound coated ZnS of the present invention: the preparation method of Cu/Cu.Mn electroluminescent material comprises that step is as follows:
1. crystalline state ZnS: xCu.yMn electroluminescent powder surface preparation
The organo-silicon coupling agent of hydrophobic nature is dissolved in dehydrated alcohol or the acetone by 0.5%～2% weight ratio, the UV light absorber that adds the 2%-3% of weight of solvent again stirs in this solution, makes its dissolving obtain a kind of solution that contains coupling agent and UV light absorber; Will be through the crystalline state ZnS of thorough drying: xCu.yMn electroluminescent powder and above-mentioned solution be by 0.3～0.6: 1 weight ratio mix stir 15～30 minutes after, centrifugal solid-liquid separates, and uses Vacuumdrier at 40 ℃～60 ℃ temperature dryings subsequently.Obtain ZnS: xCu.yMn electroluminescent powder through surface preparation.
Above-mentioned organo-silicon coupling agent is: Trimethoxy silane.
Above-mentioned UV light absorber is: Switzerland CGY company's T inuvin-P UV light absorber or Switzerland CGY company's T inuvin-327 UV light absorber.
2. liquid phase chemical deposition coats
Will be through giving the ZnS of processing: the xCu.yMn electroluminescent powder forms uniform suspension by 2%～5% weight percent and deionized water thorough mixing in reactor.With concentration is the buffered soln that 3%～8% acetic acid (HAc) and sodium-acetate are mixed with pH=5.1～5.4, and adds in the aforesaid reaction vessel, fully mixes with suspension.The volume ratio of buffered soln and suspension is 0.7～1: 1.Then, dropping concentration is 15%～25% Al (NO
3)
3.9H
2The O aqueous solution.Buffered soln and Al (NO
3)
3.9H
2The volume ratio of O solution is 10～11: 1.After fully stirring, with the NH of concentration 8%～15%
3H
2O solution is regulated the pH value 7～7.5 of above-mentioned mixing liquid.Continue to stir 25～35 minutes, and after leaving standstill supernatant liquor was separated, the centrifuge dewatering and in 60 ℃～80 ℃ dryings of packing into then obtains the pre-ZnS that coats of liquid phase method: xCu.yMn electroluminescent powder.At this moment, aluminum oxide (Al
2O
3) integument weight is ZnS: 3%～6% of xCu.yMn luminescent powder weight.
3. chemical vapor deposition coats
With the ZnS that coats in advance: the xCu.yMn electroluminescent powder is encased in the reaction chamber of the vapor phase growing apparatus that has revolution gravity fluidized-bed, and the nitrogen of the bubbling bottle that metallic aluminium organic compound and superoxol is housed by flowing through is respectively brought metallic aluminium organic compound and hydrogen peroxide steam into reaction chamber and carried out chemical vapor deposition and coat.Reaction chamber temperature is: 40 ℃～80 ℃.Nitrogen flow is 600ml/min～1000ml/min, and the vapour deposition coating time is: 6～10 hours.The acquisition coating layer is ZnS: the fine and close coated electroluminescent material of xCu.yMn luminescent powder weight ratio 4%～8%.
Used metallic aluminium organic compound is trimethyl aluminium or triisobutyl aluminium in the above-mentioned vapour deposition.
The present invention adopts liquid phase to coat and gas phase coats the process combined method, electroluminescent material surface liquid phase is coated, the gas phase sealing, to obtain the low multiple fine and close ZnS that coats of cost: the Cu/Cu.Mn electroluminescent material, reduce the ZnS that causes because of the water molecules effect: the luminous inefficacy of Cu/Cu.Mn electroluminescent material.
(4) embodiment
The invention will be further described below in conjunction with embodiment, but be not limited thereto.
Embodiment 1:
Compound coated ZnS: the xCu.yMn electroluminescent material, be the ball-type crystalline state ZnS of 15 μ m～30 μ m at particle diameter: the particle surface of xCu.yMn electroluminescent material has coated non-type aluminum oxide (Al
2O
3) fine and close integument.X=0.005 wherein, y=0.001, aluminum oxide (Al
2O
3) weight of integument is ZnS: 8% of xCu.yMn electroluminescent material weight.Aluminum oxide (Al
2O
3) the parcel amount 68～72%, finish by the liquid phase chemical deposition method for coating, 28～32%, finish by organometallics chemical vapor deposition method for coating.
The preparation method is as follows:
1. pre-treatment
Take by weighing organo-silicon coupling agent Trimethoxy silane 60 grams, UV light absorber is: Switzerland CGY company's T inuvin-P UV light absorber 92 grams successively are dissolved in 4000 milliliters of dehydrated alcohols; Take by weighing crystalline state ZnS through thorough drying: xCu.yMn electroluminescent powder 2000 grams, join in the above-mentioned mixing solutions, stir after 30 minutes, centrifugal solid-liquid separates, and uses Vacuumdrier 50 ℃ of dryings subsequently.Obtain the ZnS that processing is given on the process surface: xCu.yMn electroluminescent powder.
2. liquid phase chemical deposition coats
Restrain the ZnS that processing is given on the surface with 2000: xCu.yMn electroluminescent powder and 50 liters of deionized waters join in the reactor, and thorough mixing forms uniform suspension; Subsequently, in suspension, drip, slowly drip concentration and be 20% Al (NO by 50 liters in acetic acid (HAc) and sodium-acetate buffered soln that be mixed with, pH=5.4
3)
3.9H
25 liters of the O aqueous solution are after fully stirring, with the NH of concentration 15%
3H
2O solution is regulated the pH value 7.5 of above-mentioned mixing liquid; Continue to stir 30 minutes, static, separate clear liquid, at centrifuge dewatering and in 80 ℃ of dryings, obtain the ZnS that liquid phase method gives coating: xCu.yMn electroluminescent powder.
3. chemical vapor deposition coats
The ZnS that 2000 grams are given coating: the xCu.yMn electroluminescent powder is encased in the reaction chamber of the vapor phase growing apparatus that has revolution gravity fluidized-bed, and the nitrogen of the bubbling bottle that trimethyl aluminium and superoxol is housed by flowing through is respectively brought trimethyl aluminium and hydrogen peroxide steam into reaction chamber and carried out chemical vapour deposition and coat.Reaction chamber temperature is 80 ℃.Nitrogen flow is 800ml/min, and vapour deposition coats 8 hours time.The acquisition coating layer is ZnS: the fine and close coated electroluminescent material of xCu.yMn luminescent powder weight ratio 8%.
Adopt 5% silver nitrate solution that the fine and close coated electroluminescent material that obtains through said process is carried out the covered effect check, soak and do not have the blackout phenomenon in 2 hours; The 140V/400Hz reference power supply is surveyed powder box and is detected, and initial luminosity is 176Cd/m
2, luminance test phase half-life is 1140 hours.
Embodiment 2:
The add-on of each raw material and preparation method are with embodiment 1, different is that step (1) middle-ultraviolet lamp absorption agent is: Switzerland CGY company's T inuvin-327 UV light absorber, the metallic aluminium organic compound that adopts in step (3) vapour deposition coating process is a triisobutyl aluminium, and the vapour deposition coating time is 10 hours.Obtain the multiple fine and close ZnS that coats: the Cu.Mn electroluminescent powder.
Adopt 5% silver nitrate solution that the fine and close coated electroluminescent material that obtains through said process is carried out the covered effect check, soak and do not have the blackout phenomenon in 2 hours; The 140V/400Hz reference power supply is surveyed powder box and is detected, and initial luminosity is 164Cd/m
2, luminance test phase half-life is 1080 hours.
Embodiment 3:
Compound coated ZnS: the xCu electroluminescent material, be the ball-type crystalline state ZnS of 15 μ m～30 μ m at particle diameter: the particle surface of xCu electroluminescent material has coated non-type aluminum oxide (Al
2O
3) fine and close integument.X=0.0010 wherein,, aluminum oxide (Al
2O
3) weight of integument is ZnS: 4.6～5% of xCu electroluminescent material weight.Aluminum oxide (Al
2O
3) the parcel amount 58～60%, finish by the liquid phase chemical deposition method for coating, 38～40%, finish by organometallics chemical vapor deposition method for coating.
Pre-treatment among the preparation method is with embodiment 1, step 2 that different is, 3 as follows:
Step 2. liquid phase chemical deposition coats
Will be through giving the ZnS of processing: the xCu electroluminescent powder forms uniform suspension by 2% weight percent and deionized water thorough mixing in reactor.With concentration is the buffered soln that 5% acetic acid (HAc) and sodium-acetate are mixed with pH=5.3, and adds in the aforesaid reaction vessel, fully mixes with suspension.The volume ratio of buffered soln and suspension is 0.8: 1.Then, dropping concentration is 18% Al (NO
3)
3.9H
2The O aqueous solution.Buffered soln and Al (NO
3)
3.9H
2The volume ratio of O solution is 11: 1.After fully stirring, with the NH of concentration 12%
3H
2O solution is regulated the pH value 7.4 of above-mentioned mixing liquid.Continue to stir-35 minutes, and after leaving standstill supernatant liquor was separated, the centrifuge dewatering and in 70 ℃ of dryings of packing into then obtains the pre-ZnS that coats of liquid phase method: xCu electroluminescent powder.At this moment, aluminum oxide (Al
2O
3) integument weight is ZnS: 4.6～5% of xCu. luminescent powder weight.
3. chemical vapor deposition coats
With the ZnS that coats in advance: the xCu. electroluminescent powder is encased in the reaction chamber of the vapor phase growing apparatus that has revolution gravity fluidized-bed, and the nitrogen of the bubbling bottle that triisobutyl aluminium and superoxol is housed by flowing through is respectively brought triisobutyl aluminium and hydrogen peroxide steam into reaction chamber and carried out chemical vapor deposition and coat.Reaction chamber temperature is: 70 ℃.Nitrogen flow is 700ml/min, and the vapour deposition coating time is: 6 hours.The acquisition coating layer is ZnS: the fine and close coated electroluminescent material of xCu luminescent powder weight ratio 5%.Obtain the multiple fine and close ZnS that coats: the Cu electroluminescent powder.
The initial luminosity of fine and close coated electroluminescent material that is obtained is 170Cd/m
2, luminance test phase half-life is 1120 hours.
Claims (5)
1. compound coated ZnS: the Cu/Cu.Mn electroluminescent material is characterized in that be to be the ball-type crystalline state ZnS of 15 μ m～30 μ m at particle diameter: the particle surface of xCu.yMn electroluminescent material has coated non-type aluminum oxide (Al
2O
3) fine and close integument, x=0.001～0.010 wherein, y=0.000～0.005, aluminum oxide (Al
2O
3) weight of integument is ZnS: 4%～8% of xCu.yMn electroluminescent material weight.
2. compound coated ZnS as claimed in claim 1: the Cu/Cu.Mn electroluminescent material is characterized in that described aluminum oxide (Al
2O
3) the parcel amount 60%～80%, finish by the liquid phase chemical deposition method for coating, 20%～40%, finish by organometallics chemical vapor deposition method for coating.
3. the described compound coated ZnS of claim 1: the preparation method of Cu/Cu.Mn electroluminescent material, it is characterized in that, comprise as under the step:
(1) crystalline state ZnS: xCu.yMn electroluminescent powder surface preparation
The organo-silicon coupling agent of hydrophobic nature is dissolved in dehydrated alcohol or the acetone by 0.5%～2% weight ratio, 2%～3% the UV light absorber that adds weight of solvent again stirs in this solution, makes its dissolving obtain a kind of solution that contains coupling agent and UV light absorber; Will be through the crystalline state ZnS of thorough drying: xCu.yMn electroluminescent powder and above-mentioned solution be by 0.3～0.6: 1 weight ratio mix stir 15～30 minutes after, centrifugal solid-liquid separates, and uses Vacuumdrier at 40 ℃～60 ℃ temperature dryings subsequently;
(2) liquid phase chemical deposition coats
Will be through giving the ZnS of processing: the xCu.yMn electroluminescent powder mixes in reactor with deionized water by 2%～5% weight percent, form uniform suspension, with concentration is the buffered soln that 3%～8% acetic acid and sodium-acetate are mixed with pH=5.1～5.4, and in the adding aforesaid reaction vessel, mix, the volume ratio of buffered soln and suspension is 0.7～1: 1; Then, dropping concentration is 15%～25% Al (NO
3)
3.9H
2The O aqueous solution, buffered soln and Al (NO
3)
3.9H
2The volume ratio of O solution is 10～11: 1, after stirring, with the NH of concentration 8%～15%
3H
2O solution is regulated the pH value 7～7.5 of above-mentioned mixing liquid; Continue to stir 25～35 minutes, and after leaving standstill supernatant liquor was separated, the centrifuge dewatering and of packing into then in 60 ℃～80 ℃ dryings;
(3) chemical vapor deposition coats
ZnS with above-mentioned pre-coating: the xCu.yMn electroluminescent powder is encased in the reaction chamber of the vapor phase growing apparatus that has revolution gravity fluidized-bed, and the nitrogen of the bubbling bottle that metallic aluminium organic compound and superoxol is housed by flowing through is respectively brought metallic aluminium organic compound and hydrogen peroxide steam into reaction chamber and carried out chemical vapor deposition and coat; Reaction chamber temperature is: 40 ℃～80 ℃, nitrogen flow is 600ml/min～1000ml/min, and the vapour deposition coating time is 6～10 hours, and getting coating layer is ZnS: the fine and close coated electroluminescent material of xCu.yMn luminescent powder weight ratio 4%～8%.
4. compound coated ZnS as claimed in claim 3: the preparation method of Cu/Cu.Mn electroluminescent material, it is characterized in that, described organo-silicon coupling agent is: Trimethoxy silane, UV light absorber is: Tinuvin-P or Tinuvin-327 UV light absorber.
5. compound coated ZnS as claimed in claim 3: the preparation method of Cu/Cu.Mn electroluminescent material is characterized in that used metallic aluminium organic compound is trimethyl aluminium or triisobutyl aluminium in the described vapour deposition.
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|---|---|---|---|
| CNA031124127A CN1468936A (en) | 2003-06-10 | 2003-06-10 | Electroluminescent composite coated ZnS:Cu/Cu.Mn material and its prepn process |
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|---|---|---|---|
| CNA031124127A CN1468936A (en) | 2003-06-10 | 2003-06-10 | Electroluminescent composite coated ZnS:Cu/Cu.Mn material and its prepn process |
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295297C (en) * | 2005-02-25 | 2007-01-17 | 东南大学 | Alumina coated fluorescent powder and its coating method |
| CN100363457C (en) * | 2005-11-04 | 2008-01-23 | 中国科学院长春应用化学研究所 | Low heat solid phase method for implementing nano-cladding on fluorescent pewder surface |
| CN102212360A (en) * | 2010-04-08 | 2011-10-12 | 海洋王照明科技股份有限公司 | Field emission fluorescent material and preparation method thereof |
| CN101445724B (en) * | 2008-11-04 | 2012-03-21 | 中国海洋大学 | Method for improving surface of zinc sulfide nano-material mixed with copper ion |
| CN101341228B (en) * | 2005-09-29 | 2013-03-13 | 国防研究与发展组织总干事 | Single-source precursor for semiconductor nanocrystals |
| CN103773084A (en) * | 2013-12-30 | 2014-05-07 | 福建师范大学 | Preparation method for synthesizing sheet-type cladding material by fluidized bed gas-phase method |
| CN101360803B (en) * | 2006-01-26 | 2014-05-28 | 奥斯兰姆施尔凡尼亚公司 | Moisture-resistant electroluminescent phosphor with high initial brightness and method of making |
| CN101360804B (en) * | 2006-01-26 | 2014-11-26 | 环球钨和粉末公司 | Moisture-resistant electroluminescent phosphor with high initial brightness and method of making |
| CN106590634A (en) * | 2016-11-30 | 2017-04-26 | 北京中科卓研科技有限公司 | Preparation of doped zinc sulfide with micro-nano composite structure and application thereof in augmented reality |
| CN108728081A (en) * | 2018-05-22 | 2018-11-02 | 温州中祥光电科技发展有限公司 | A kind of inorganic powder electroluminescent material and inorganic electroluminescence device |
| CN109103348A (en) * | 2018-08-10 | 2018-12-28 | 武汉艾特米克超能新材料科技有限公司 | A kind of OLED luminous organic material and preparation method thereof, OLED device and preparation method thereof |
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2003
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295297C (en) * | 2005-02-25 | 2007-01-17 | 东南大学 | Alumina coated fluorescent powder and its coating method |
| CN101341228B (en) * | 2005-09-29 | 2013-03-13 | 国防研究与发展组织总干事 | Single-source precursor for semiconductor nanocrystals |
| CN100363457C (en) * | 2005-11-04 | 2008-01-23 | 中国科学院长春应用化学研究所 | Low heat solid phase method for implementing nano-cladding on fluorescent pewder surface |
| CN101360804B (en) * | 2006-01-26 | 2014-11-26 | 环球钨和粉末公司 | Moisture-resistant electroluminescent phosphor with high initial brightness and method of making |
| CN101360803B (en) * | 2006-01-26 | 2014-05-28 | 奥斯兰姆施尔凡尼亚公司 | Moisture-resistant electroluminescent phosphor with high initial brightness and method of making |
| CN101445724B (en) * | 2008-11-04 | 2012-03-21 | 中国海洋大学 | Method for improving surface of zinc sulfide nano-material mixed with copper ion |
| CN102212360A (en) * | 2010-04-08 | 2011-10-12 | 海洋王照明科技股份有限公司 | Field emission fluorescent material and preparation method thereof |
| CN102212360B (en) * | 2010-04-08 | 2013-11-27 | 海洋王照明科技股份有限公司 | Field emission fluorescent material and preparation method thereof |
| CN103773084A (en) * | 2013-12-30 | 2014-05-07 | 福建师范大学 | Preparation method for synthesizing sheet-type cladding material by fluidized bed gas-phase method |
| CN103773084B (en) * | 2013-12-30 | 2015-05-20 | 福建师范大学 | Preparation method for synthesizing sheet-type cladding material by fluidized bed gas-phase method |
| CN106590634A (en) * | 2016-11-30 | 2017-04-26 | 北京中科卓研科技有限公司 | Preparation of doped zinc sulfide with micro-nano composite structure and application thereof in augmented reality |
| CN108728081A (en) * | 2018-05-22 | 2018-11-02 | 温州中祥光电科技发展有限公司 | A kind of inorganic powder electroluminescent material and inorganic electroluminescence device |
| CN109103348A (en) * | 2018-08-10 | 2018-12-28 | 武汉艾特米克超能新材料科技有限公司 | A kind of OLED luminous organic material and preparation method thereof, OLED device and preparation method thereof |
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