WO2011150547A1 - 含有导电氧化物的掺杂稀土元素的氧化钇发光薄膜及其制备方法 - Google Patents
含有导电氧化物的掺杂稀土元素的氧化钇发光薄膜及其制备方法 Download PDFInfo
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- WO2011150547A1 WO2011150547A1 PCT/CN2010/073400 CN2010073400W WO2011150547A1 WO 2011150547 A1 WO2011150547 A1 WO 2011150547A1 CN 2010073400 W CN2010073400 W CN 2010073400W WO 2011150547 A1 WO2011150547 A1 WO 2011150547A1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
- C04B41/4519—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application application under an other specific atmosphere
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7784—Chalcogenides
Definitions
- Y 2 O 3 Re is a widely used phosphor, and how to make it The film has excellent uniformity, stability and excellent adhesion to the substrate, and has been an important part of research on rare earth luminescent materials in the fields of material chemistry and material physics.
- the technical problem to be solved by the present invention is to provide a rare earth element-doped cerium oxide luminescent film containing a conductive oxide and a method for preparing the same, which has good stability and high luminous intensity.
- a technical solution to solve the technical problem of the present invention is: a rare earth element-doped yttria luminescent film containing a conductive oxide having a composition formula of Y 2 O 3 : Re, Zn 1-x Al x O, wherein x has a value range of 0 ⁇ x ⁇ 0.05, and Re is a rare earth element lanthanum or cerium.
- Step 1 preparing a colloid containing rare earth elements lanthanum and cerium or a colloid containing rare earth elements lanthanum and cerium;
- a compound of ruthenium and osmium or a compound of ruthenium and osmium is selected and the doping concentration of ruthenium or osmium is 0.1% to 10%, and the solution concentration is 0. 1 mol/L to 2.00 mol/L of a solution of ruthenium and osmium or a solution of ruthenium and osmium, and then a mixed solution of an alcohol and water containing citric acid, and an alcohol solution of lanthanum and cerium of 0.1 mol/L to 1.00 mol/L.
- the aqueous solution of hydrazine and hydrazine the volume ratio of water to ethanol is 1:1 ⁇ 1:7, and the molar ratio of citric acid to strontium ions and strontium ions or strontium ions and strontium ions is 1:1 ⁇ 5:1.
- polyethylene glycol is added to the aqueous alcohol solution to make the concentration of the polyethylene glycol 0.05-0.20 g/mL, and the aqueous solution of the hydrazine and hydrazine or the aqueous solution of hydrazine and hydrazine in the water bath of 40-60 ° C is placed.
- the ratio of the sum of the moles of zinc and aluminum to the sum of the moles of lanthanum and cerium or lanthanum and cerium is 0.01:1 to 2:1, and the mixture is stirred in a water bath at 15 ° C to 80 ° C. The mixed colloid was formed in ⁇ 4 hours.
- the mixed colloid is spin-coated for 3 to 10 times, and after each coating, the film is dried at a temperature of 100 ° C to 150 ° C for 5 to 30 minutes, and the coating is applied.
- the formed film is heated to 700 ° C to 1200 ° C at 1 ° C ⁇ 5 ° C / min in an air atmosphere or a reducing atmosphere, and kept for 1 to 3 hours.
- the present invention provides a rare earth element-doped yttria luminescent film containing a conductive oxide having a composition formula of Y 2 O 3 : Re, Zn 1-x Al x O , wherein x The value ranges from 0 ⁇ x ⁇ 0.05, and Re is a rare earth element lanthanum or cerium.
- Step S01 preparing a colloid containing rare earth elements lanthanum and cerium or a colloid containing rare earth elements lanthanum and cerium;
- Step S02 preparing a colloid of a conductive oxide Zn 1-x Al x O (AZO);
- Step S03 mixing the colloid of step S01 and the colloid of step S02 to form a mixed colloid
- Step S04 The mixed colloidal coating film of the step S03 is obtained by obtaining a rare earth element-doped cerium oxide light-emitting film containing a conductive oxide Zn 1-x Al x O.
- a compound of lanthanum and cerium or a compound of lanthanum and cerium is selected and configured to have a doping concentration of cerium or lanthanum of 0.1% to 10%, and the solution concentration is 0. 1 mol/L to 2.00 mol/L of a solution of ruthenium and osmium or a solution of ruthenium and osmium, and then a mixed solution of an alcohol and water containing citric acid, and an alcohol solution of lanthanum and cerium of 0.1 mol/L to 1.00 mol/L.
- the aqueous solution of hydrazine and hydrazine the volume ratio of water to ethanol is 1:1 ⁇ 1:7, and the molar ratio of citric acid to strontium ions and strontium ions or strontium ions and strontium ions is 1:1 ⁇ 5:1.
- polyethylene glycol is added to the aqueous alcohol solution to make the concentration of the polyethylene glycol 0.05-0.20 g/mL, and the aqueous solution of the hydrazine and hydrazine or the aqueous solution of hydrazine and hydrazine in the water bath at 40 ° C to 60 ° C is placed.
- the ruthenium and osmium compounds or the ruthenium and osmium compounds are also selected from metal oxides or oxalates, and the metal oxides or oxalates are analyzed with pure hydrochloric acid or analyzed under stirring at 15 ° C to 100 ° C. Pure nitric acid is dissolved in a container and configured as a solution.
- the step of preparing the colloid of the conductive oxide Zn 1-x Al x O includes: according to the chemical formula Zn 1-x Al x O, wherein the value of x ranges from 0 ⁇ x ⁇ 0.05, respectively Zinc salt and aluminum salt, adding stabilizer, using ethylene glycol methyl ether or alcohol aqueous solution as a solvent to form a solution, stirring in a water bath at 40 ° C ⁇ 70 ° C for 4-8 hours to obtain a uniform precursor solution, the resulting precursor The solution was aged at a temperature of 50 ° C to 80 ° C for 56 to 90 hours to obtain a Zn 1-x Al x O colloid.
- the stabilizer is one or more of monoethanolamine, diethanolamine or triethanolamine.
- the ratio of the sum of the moles of zinc and aluminum to the sum of the moles of lanthanum and cerium or lanthanum and cerium is 0.01:1 to 2:1, and the mixture is stirred in a water bath at 15 ° C to 80 ° C. The mixed colloid was formed in ⁇ 4 hours.
- FIG. 2 is a spectrum diagram of a light-emitting film Y 2 O 3 :Eu with a thickness of 100 nm added to AZO prepared by the method of the present invention under the excitation of a cathode ray, and the curve b is the same under the experimental conditions, and is not added.
- AZ is a spectrum of a light-emitting film Y 2 O 3 :Eu having a thickness of 100 nm under the excitation of a cathode ray, wherein the integrated area of the curve a is 1.44 times the integrated area of the curve b.
- the spectrogram was analyzed using a Shimadzu RF-5301PC spectrometer under 5KV voltage test conditions.
- 6.7 mL of the prepared AZO colloid was added to the Y and Eu colloids, and the mixture was stirred for 2 hours in a water bath at 60 ° C, and the obtained colloid was spin-coated for 8 times. After each application, the film was placed in an oven at 120 ° C. Dry in 15 minutes. The spin-formed film was placed in a temperature-programmed oven at a temperature of 3 ° C/min to 1200 ° C and held for 1 hour to obtain a light-emitting film Y 2 O 3 :Eu having a thickness of 1.5 ⁇ m added to AZO.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Luminescent Compositions (AREA)
Description
Claims (10)
- 一种含有导电氧化物的掺杂稀土元素的氧化钇发光薄膜,其特征在于:所述氧化钇发光薄膜的组成式为Y2O3: Re,Zn1-xAlxO,其中,x的取值范围为0<x≤0.05,Re为稀土元素铕或者铽。
- 一种含有导电氧化物的掺杂稀土元素的氧化钇发光薄膜的制备方法,其包括如下步骤:步骤一:制备含有稀土元素钇和铕的胶体或者含有稀土元素钇和铽的胶体;步骤二:制备导电氧化物Zn1-xAlxO的胶体;步骤三:将步骤一的胶体和步骤二的胶体混合形成混合胶体;步骤四:将步骤三的混合胶体镀膜得到含有导电氧化物Zn1-xAlxO的掺杂稀土元素的氧化钇发光薄膜。
- 如权利要求2所述的制备方法,其特征在于:在所述步骤一中,选用钇和铕的化合物或者选用钇和铽的化合物并配置成铕或者铽的掺杂浓度为0.1%~10%,溶液浓度为0. 1mol/L~2.00mol/L的钇和铕的溶液或者钇和铽的溶液,然后加入含有柠檬酸的醇水混合溶液,配置成0.1mol/L~1.00mol/L的钇和铕的醇水溶液或者钇和铽的醇水溶液,水与乙醇的体积比为1:1~1:7,保持柠檬酸与钇离子和铕离子或钇离子和铽离子的摩尔比为1:1~5:1,再在醇水溶液中加入聚乙二醇,使聚乙二醇的浓度为0.05~0.20g/mL,将所配置的钇和铕的醇水溶液或者钇和铽的醇水溶液在40℃~60℃水浴中搅拌4~6小时,再于60℃~90℃烘箱中陈化40~60小时,得到含有钇和铕的胶体或者含有钇和铽的胶体。
- 如权利要求3所述的制备方法,其特征在于:所述钇和铕的化合物或者钇和铽的化合物选用硝酸盐类或盐酸盐类可溶性盐,用去离子水溶解于容器中形成溶液。
- 如权利要求3所述的制备方法,其特征在于:所述钇和铕的化合物或者钇和铽的化合物选用金属氧化物或者草酸盐,在15℃~100℃搅拌条件下,将所述金属氧化物或草酸盐用分析纯的盐酸或分析纯硝酸溶解于容器中配置成溶液。
- 如权利要求2所述的制备方法,其特征在于:在所述步骤二中,制备导电氧化物Zn1-xAlxO的胶体的步骤包括:按化学式Zn1-xAlxO,其中x的取值范围为0<x≤0.05,分别称取锌盐及铝盐,加入稳定剂,用乙二醇甲醚或醇水溶液做溶剂配置成溶液,于40℃~70℃水浴搅拌4~8小时后得到均匀的前驱体溶液,将所得的前驱体溶液置于温度为50℃~80℃的条件下陈化56~90小时得到Zn1-xAlxO胶体。
- 如权利要求6所述的制备方法,其特征在于:所述稳定剂为单乙醇胺、二乙醇胺或三乙醇胺中的一种或几种。
- 如权利要求2所述的制备方法,其特征在于:在所述步骤三中,锌和铝的摩尔数之和与钇和铕或者钇和铽的摩尔数之和的比例为0.01:1~2:1,并于15℃~80℃下水浴搅拌1~4小时形成所述混合胶体。
- 如权利要求2所述的制备方法,其特征在于:在所述步骤四中,镀膜时,将混合胶体旋转涂敷3~10次,每次涂敷完后将薄膜置于温度为100℃~150℃条件下烘干5~30分钟,将旋涂成型的薄膜置于空气气氛或还原气氛中以1℃~5℃/min升温至700℃~1200℃,并保温1~3小时。
- 如权利要求9所述的制备方法,其特征在于:所述还原气氛为碳粉形成的一氧化碳还原气氛或者氮气和氢气的混合气体。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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CN201080065466.XA CN102812106B (zh) | 2010-05-31 | 2010-05-31 | 含有导电氧化物的掺杂稀土元素的氧化钇发光薄膜及其制备方法 |
US13/700,656 US20130071689A1 (en) | 2010-05-31 | 2010-05-31 | Rare earth elements doping on yttrium oxide luminescent thin film containing conductive oxides and preparation methods thereof |
EP10852346.5A EP2578662A4 (en) | 2010-05-31 | 2010-05-31 | Rare Terpenation on a Luminescent Yttrium Oxide Thinnable Layer with Conductive Oxides and Preparation Method Therefor |
PCT/CN2010/073400 WO2011150547A1 (zh) | 2010-05-31 | 2010-05-31 | 含有导电氧化物的掺杂稀土元素的氧化钇发光薄膜及其制备方法 |
JP2013512713A JP5749798B2 (ja) | 2010-05-31 | 2010-05-31 | 導電酸化物を含有する、希土元素ドーピングされた酸化イットリウム発光フィルム及びその調製方法 |
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PCT/CN2010/073400 WO2011150547A1 (zh) | 2010-05-31 | 2010-05-31 | 含有导电氧化物的掺杂稀土元素的氧化钇发光薄膜及其制备方法 |
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US (1) | US20130071689A1 (zh) |
EP (1) | EP2578662A4 (zh) |
JP (1) | JP5749798B2 (zh) |
CN (1) | CN102812106B (zh) |
WO (1) | WO2011150547A1 (zh) |
Cited By (1)
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CN115895656A (zh) * | 2021-08-24 | 2023-04-04 | 浙江理工大学 | 光致发光铽掺杂氧化锡薄膜及其制备方法 |
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CN102906217B (zh) * | 2010-06-12 | 2014-07-23 | 海洋王照明科技股份有限公司 | 氧化钇荧光粉及其制备方法 |
EP2607450A4 (en) * | 2010-08-16 | 2017-01-25 | Ocean's King Lighting Science&Technology Co., Ltd. | Color-adjustable luminescent powder and preparation method thereof |
CN110628062A (zh) * | 2019-10-24 | 2019-12-31 | 泉州师范学院(石狮)生态智能织物工程技术研究院 | 一种光色可调的稀土基纳米高分子复合纤维素薄膜及其制备方法 |
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US4208613A (en) * | 1975-06-30 | 1980-06-17 | Dai Nippon Toryo Co., Ltd. | Low-velocity electron excited fluorescent display device |
JPS54106085A (en) * | 1978-02-07 | 1979-08-20 | Nec Corp | Luminous material |
JPS5586877A (en) * | 1978-12-22 | 1980-07-01 | Nec Corp | Light-emitting material |
JPH0326781A (ja) * | 1989-06-23 | 1991-02-05 | Nichia Chem Ind Ltd | 蛍光体 |
JP2959817B2 (ja) * | 1990-08-03 | 1999-10-06 | 日亜化学工業株式会社 | 顔料付き蛍光体 |
JP2001019952A (ja) * | 1999-07-09 | 2001-01-23 | Tokyo Kagaku Kenkyusho:Kk | 赤色蛍光体及び三波長域発光形蛍光ランプ |
KR100730122B1 (ko) * | 2004-12-24 | 2007-06-19 | 삼성에스디아이 주식회사 | 전도성 물질을 포함하는 이트륨계 형광체, 그의 제조방법및 이를 채용한 표시소자 |
JP4938999B2 (ja) * | 2005-06-14 | 2012-05-23 | 株式会社アルバック | 導電性蛍光体薄膜の形成方法及び薄膜蛍光体基板の作製方法 |
KR100792279B1 (ko) * | 2006-06-28 | 2008-01-08 | 한국지질자원연구원 | 솔-젤 공정 및 열처리에 의한 젤 분말로부터 분쇄 및소성공정에 의한 나노크기의 적색형광체 제조방법 |
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2010
- 2010-05-31 EP EP10852346.5A patent/EP2578662A4/en not_active Withdrawn
- 2010-05-31 JP JP2013512713A patent/JP5749798B2/ja not_active Expired - Fee Related
- 2010-05-31 CN CN201080065466.XA patent/CN102812106B/zh not_active Expired - Fee Related
- 2010-05-31 WO PCT/CN2010/073400 patent/WO2011150547A1/zh active Application Filing
- 2010-05-31 US US13/700,656 patent/US20130071689A1/en not_active Abandoned
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Title |
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See also references of EP2578662A4 * |
TAKAHASHI R ET AL.: "Development of a New Combinatorial Mask for Addressable Ternary Phase Diagramming: Application to Rare Earth Doped Phosphors", APPLIED SURFACE SCIENCE, vol. 223, no. 1-3, 2004, pages 249 - 252, XP055069096 * |
ZENG D. M. ET AL.: "Preparation of Y2O3:Eu Fluorescent Film by Sol-Gel Process", PHOTOGRAPHIC SCIENCE AND PHOTOCHEMISTRY, vol. 21, no. 4, 2003, pages 280 - 284, XP008169181 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115895656A (zh) * | 2021-08-24 | 2023-04-04 | 浙江理工大学 | 光致发光铽掺杂氧化锡薄膜及其制备方法 |
CN115895656B (zh) * | 2021-08-24 | 2024-05-03 | 浙江理工大学 | 光致发光铽掺杂氧化锡薄膜及其制备方法 |
Also Published As
Publication number | Publication date |
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EP2578662A4 (en) | 2014-12-24 |
EP2578662A1 (en) | 2013-04-10 |
CN102812106A (zh) | 2012-12-05 |
JP5749798B2 (ja) | 2015-07-15 |
JP2013532203A (ja) | 2013-08-15 |
CN102812106B (zh) | 2014-11-05 |
US20130071689A1 (en) | 2013-03-21 |
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