WO2012009845A1 - 一种发光材料及其制备方法 - Google Patents
一种发光材料及其制备方法 Download PDFInfo
- Publication number
- WO2012009845A1 WO2012009845A1 PCT/CN2010/075254 CN2010075254W WO2012009845A1 WO 2012009845 A1 WO2012009845 A1 WO 2012009845A1 CN 2010075254 W CN2010075254 W CN 2010075254W WO 2012009845 A1 WO2012009845 A1 WO 2012009845A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- luminescent material
- source compound
- geo
- nay
- material according
- Prior art date
Links
Images
Classifications
-
- 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
- C09K11/7793—Germanates
-
- 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
- C09K11/7775—Germanates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/30—Cold cathodes, e.g. field-emissive cathode
- H01J1/304—Field-emissive cathodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J31/00—Cathode ray tubes; Electron beam tubes
- H01J31/08—Cathode ray tubes; Electron beam tubes having a screen on or from which an image or pattern is formed, picked up, converted, or stored
- H01J31/10—Image or pattern display tubes, i.e. having electrical input and optical output; Flying-spot tubes for scanning purposes
- H01J31/12—Image or pattern display tubes, i.e. having electrical input and optical output; Flying-spot tubes for scanning purposes with luminescent screen
- H01J31/123—Flat display tubes
- H01J31/125—Flat display tubes provided with control means permitting the electron beam to reach selected parts of the screen, e.g. digital selection
- H01J31/127—Flat display tubes provided with control means permitting the electron beam to reach selected parts of the screen, e.g. digital selection using large area or array sources, i.e. essentially a source for each pixel group
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B41/00—Circuit arrangements or apparatus for igniting or operating discharge lamps
- H05B41/14—Circuit arrangements
- H05B41/36—Controlling
Definitions
- the invention belongs to the technical field of luminescent materials, and in particular relates to a luminescent material and a preparation method thereof.
- Field emission display is a flat panel display newly developed in recent years. It belongs to low voltage cold cathode emission. This special emission feature gives FED Many different performances than other flat panel displays: low operating voltage (200 ⁇ 5000V), low power consumption, high brightness, thin, small size, light weight, good stability, long life, fast response, full color display, no Perspective limitations and compatibility with the environment.
- the fluorescent materials used in field emission devices are mainly sulfide series, oxide series and sulfur oxide series phosphors used in conventional cathode ray tubes and projection television tubes.
- the luminescence brightness is higher and has certain conductivity, but it is easily decomposed under the bombardment of large beam electron beams, releasing the elemental sulfur "poisoning" cathode tip and generating other
- the precipitate covers the surface of the phosphor, which reduces the luminous efficiency of the phosphor and shortens the service life of the field emission device.
- the oxide phosphor has good stability, but the luminous efficiency is not high enough, and the material is generally an insulator, and both properties have to be improved and improved.
- the present invention provides a citrate luminescent material doped with a rare earth element, which has high conductivity, stability, and high luminous efficiency.
- the mixed powder was subjected to a sintering treatment, and then cooled to room temperature and ground to obtain the above-mentioned luminescent material.
- the luminescent material is doped with rare earth elements and sodium ions to form a ceric acid luminescent material containing rare earth elements, which effectively improves the stability and luminescent properties of the luminescent material. Moreover, due to the presence of sodium ions, the conductive property of the luminescent material is effectively improved; the presence of the rare earth element enables the luminescent material to selectively emit red, green, blue and other colors under the excitation of the cathode ray, which can be better
- the invention is applied to a field emission device.
- the luminescent materials are obtained by directly mixing and sintering the respective source components, thereby making the preparation process simple, the cost is low, and the invention has broad application prospects.
- Example 1 is a luminescence spectrum of a luminescent material prepared in Example 2 of the present invention under excitation of a cathode ray at an acceleration voltage of 5 kV;
- Example 2 is a luminescence spectrum of a luminescent material prepared in Example 5 of the present invention under excitation of a cathode ray at an acceleration voltage of 5 kV;
- Example 3 is a luminescence spectrum of a luminescent material prepared in Example 6 of the present invention under excitation of a cathode ray at an acceleration voltage of 5 kV;
- FIG. 4 is a flow chart of a method for preparing a luminescent material according to the present invention.
- the luminescent material of the embodiment of the invention has the chemical formula: NaY 1-x Ln x GeO 4 , wherein Ln is a rare earth element, and x has a value ranging from 0 ⁇ x ⁇ 0.2.
- the Ln includes one of Eu, Tb, Tm, Sm, Dy, and Bi;
- the value range of x is preferably 0.001 ⁇ x ⁇ 0.15.
- the luminescent material is doped with a rare earth element to form a strontium silicate material containing a rare earth element and a sodium ion, thereby effectively improving the stability and luminescent properties of the luminescent material, and appropriately adjusting the ratio of each element in the luminescent material, such as
- NaY 1-x Ln x GeO 4 preferably has a value range of 0.001 ⁇ x ⁇ 0.15, and when Ln is preferably one of Eu, Tb, Tm, Sm, Dy, and Bi, it can be further improved.
- the stability and luminous efficiency of the luminescent material is doped with a rare earth element to form a strontium silicate material containing a rare earth element and a sodium ion, thereby effectively improving the stability and luminescent properties of the luminescent material, and appropriately adjusting the ratio of each element in the luminescent material, such as
- NaY 1-x Ln x GeO 4 preferably has a value range of 0.001 ⁇ x ⁇ 0.
- the conductive property of the luminescent material is effectively improved; the presence of rare earth elements enables the luminescent material to emit red, green, blue, etc. under the excitation of a cathode ray.
- Light of different colors such as a rare earth element containing Tm, Sm, Dy, Bi, etc., emits blue light, and the luminescent material containing a rare earth element such as Eu emits red light, and the luminescent material containing a rare earth element such as Tb emits green light. It can be preferably applied to field emission devices.
- the preparation process comprises the following steps:
- the mixed powder is subjected to a sintering treatment, and then cooled to room temperature and ground to obtain the luminescent material.
- the source compound of Na is preferably at least one of Na carbonate, sodium oxalate, sodium acetate, sodium fluoride, sodium chloride, and sodium bromide;
- the source compound is preferably at least one of an oxide, a nitrate, a carbonate, and an oxalate of Ln;
- the source compound of Y is preferably an oxide, a nitrate, a carbonate or an oxalate of Y.
- At least one of; the source compound of Ge is preferably an oxide of Ge.
- the Ln preferably includes one of Eu, Tb, Tm, Sm, Dy, and Bi; and the value of x is preferably 0.001 ⁇ x ⁇ 0.15.
- the respective source compounds are mixed and then ground to uniformly mix the respective source compounds.
- the method of grinding can be ball milling or other methods of grinding commonly used in the art.
- the sintering is performed in the presence of an air atmosphere, and the sintering temperature is preferably 900 to 1350 ° C, the time is preferably 2 to 20 h, and more preferably the temperature is 1100 to 1300 ° C, time. It is 2 ⁇ 10h.
- the luminescent material product of the present embodiment obtained after sintering can also be ground into a powder.
- the grinding method can be ball milling or other grinding methods commonly used in the art. In order to ensure that the molecular structure of the product is not destroyed, a ball milling method is preferably employed.
- the luminescent materials are obtained by directly mixing and sintering the respective source compounds, thereby making the preparation process simple, the cost is low, and the production and application prospects are broad.
- compositions of the luminescent materials and their preparation methods, as well as their properties and the like, are exemplified below by various embodiments.
- the NaY 0.999 Sm 0.001 GeO 4 luminescent material of this example emits blue light under the excitation of a cathode ray.
- the NaY 0.99 Bi 0.01 GeO 4 luminescent material of this example emits blue light under the excitation of a cathode ray.
- the luminescence spectrum of the NaY 0.99 Bi 0.01 GeO 4 luminescent material prepared in this example under the excitation of cathode ray is shown in FIG. 1 , and the citrate luminescent material prepared in this embodiment has high luminescence efficiency and excellent luminescence property.
- the weighed raw materials are ground and uniformly mixed in an agate mortar, and then placed in a corundum crucible, and the corundum crucible is placed in a high-temperature box furnace, and heated to 1350 ° C in an air atmosphere, and the calcination is performed under the conditions 2 After an hour, it was cooled to room temperature, and the cooled product was ground to obtain a NaY 0.8 Dy 0.2 GeO 4 luminescent material.
- the NaY 0.8 Dy 0.2 GeO 4 luminescent material of this example emits blue light under the excitation of a cathode ray.
- the NaY 0.99 Tm 0.01 GeO 4 luminescent material of this example emits blue light under the excitation of a cathode ray.
- the NaY 0.95 Eu 0.05 GeO 4 luminescent material of this example emits red light under the excitation of a cathode ray.
- the luminescence spectrum of the NaY 0.95 Eu 0.05 GeO 4 red luminescent material prepared by the embodiment of the present invention is excited by the cathode ray.
- the bismuth silicate luminescent material prepared in the embodiment has high luminescence efficiency and excellent luminescence property. .
- 0.4101 g of sodium acetate (CH 3 CO 2 Na), 0.4798 g of yttrium oxide (Y 2 O 3 ), 0.1402 g of lanthanum oxide (Tb 4 O 7 ), and 0.5230 g of cerium oxide (GeO 2 ) were weighed.
- the prepared raw materials are ground and uniformly mixed in an agate mortar, and then placed in a corundum crucible.
- the corundum crucible is placed in a high-temperature box furnace and heated to 1100 ° C in an air atmosphere. After the calcination for 10 hours under this condition, After cooling to room temperature, the cooled product was ground to obtain a NaY 0.85 Tb 0.15 GeO 4 luminescent material.
- the NaY 0.85 Tb 0.15 GeO 4 luminescent material of this example emits green light under the excitation of a cathode ray.
- the luminescence spectrum of the NaY 0.85 Tb 0.15 GeO 4 green luminescent material prepared by the embodiment of the present invention under the excitation of the cathode ray is shown in FIG. 3 , and the citrate luminescent material prepared in the embodiment has high luminescence efficiency and excellent luminescence property. .
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Description
Claims (10)
- 一种发光材料,其化学通式为:NaY1-xLnxGeO4,其中,Ln为稀土元素,x的取值范围为0<x≤0.2。
- 如权利要求1所述的发光材料,其特征在于:所述Ln包含Eu、Tb、Tm、Sm、Dy、Bi中的一种。
- 如权利要求1所述的发光材料,其特征在于:所述x的取值范围为0.001≤x≤0.15。
- 一种发光材料制备方法,其包括如下步骤:按照化学通式NaY1-xLnxGeO4中各元素的化学计量比,称取Na的源化合物、Ln的源化合物、Y的源化合物、Ge的源化合物,其中,Ln为稀土元素,x的取值范围为0<x≤0.2;将所述Na的源化合物、Ln的源化合物、Y的源化合物、Ge的源化合物混合,研磨成混合粉体;将混合粉体进行烧结处理,然后冷却至室温,研磨,得到所述的发光材料。
- 如权利要求4所述的发光材料制备方法,其特征在于:所述Na的源化合物为Na的碳酸盐、草酸钠、醋酸钠、氟化钠、氯化钠、溴化钠中的至少一种;所述Ln的源化合物为Ln的氧化物、硝酸盐、碳酸盐、草酸盐中的至少一种;所述Y的源化合物为Y的氧化物、硝酸盐、碳酸盐、草酸盐中的至少一种;所述Ge的源化合物为Ge的氧化物。
- 如权利要求4所述的发光材料制备方法,其特征在于:所述烧结的温度为900~1350℃,时间为2~20h。
- 如权利要求4或6所述的发光材料制备方法,其特征在于:所述烧结的温度为1100~1300℃,时间为2~10h。
- 如权利要求4所述的发光材料制备方法,其特征在于:所述Ln包含Eu、Tb、Tm、Sm、Dy、Bi中的一种。
- 如权利要求4所述的发光材料制备方法,其特征在于:所述x的取值范围为0.001≤x≤0.15。
- 如权利要求4所述的发光材料制备方法,其特征在于:所述烧结处理是在空气气氛存在条件下进行的。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2013518929A JP5667289B2 (ja) | 2010-07-19 | 2010-07-19 | 発光材料及びその製造方法、並びに電界放射デバイス |
EP10854875.1A EP2597132B1 (en) | 2010-07-19 | 2010-07-19 | Luminescent material and preparation method thereof |
CN201080066839.5A CN102906223B (zh) | 2010-07-19 | 2010-07-19 | 一种发光材料及其制备方法 |
PCT/CN2010/075254 WO2012009845A1 (zh) | 2010-07-19 | 2010-07-19 | 一种发光材料及其制备方法 |
US13/700,506 US9034205B2 (en) | 2010-07-19 | 2010-07-19 | Luminescent material and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/CN2010/075254 WO2012009845A1 (zh) | 2010-07-19 | 2010-07-19 | 一种发光材料及其制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2012009845A1 true WO2012009845A1 (zh) | 2012-01-26 |
Family
ID=45496438
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/CN2010/075254 WO2012009845A1 (zh) | 2010-07-19 | 2010-07-19 | 一种发光材料及其制备方法 |
Country Status (5)
Country | Link |
---|---|
US (1) | US9034205B2 (zh) |
EP (1) | EP2597132B1 (zh) |
JP (1) | JP5667289B2 (zh) |
CN (1) | CN102906223B (zh) |
WO (1) | WO2012009845A1 (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116103045A (zh) * | 2023-02-16 | 2023-05-12 | 华侨大学 | 一种LiSc1-xLuxGeO4:Ln3+,Eu3+光存储材料及其制备方法和应用 |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2654032C1 (ru) * | 2017-02-09 | 2018-05-15 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения академии наук | Сложный натриевый германат лантана, неодима и гольмия в качестве люминесцентного материала для преобразования монохроматического излучения лазера и способ его получения |
CN116120934A (zh) * | 2023-04-19 | 2023-05-16 | 德州学院 | 一种促植物生长的蓝-红光长余辉发光材料及制备方法和应用 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1111025A2 (en) * | 1999-12-24 | 2001-06-27 | Sumitomo Chemical Company, Limited | Phosphor for vacuum ultraviolet excited light emitting device |
JP2005298679A (ja) * | 2004-04-12 | 2005-10-27 | Fuji Photo Film Co Ltd | 希土類ホウ酸塩の製造方法 |
CN101184824A (zh) * | 2005-05-24 | 2008-05-21 | 首尔半导体株式会社 | 发光装置及其所使用的碱土金属硫化物的磷光体 |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5173611A (en) * | 1992-01-17 | 1992-12-22 | Eastman Kodak Company | Phosphor composition and X-ray intensifying screen exhibiting peak emission in the ultraviolet |
JP2001181627A (ja) * | 1999-12-24 | 2001-07-03 | Sumitomo Chem Co Ltd | 真空紫外線励起発光素子用蛍光体 |
EP1184440A3 (en) * | 2000-08-30 | 2003-11-26 | Hokushin Corporation | Electroluminescent device and oxide phosphor for use therein |
JP2004026995A (ja) * | 2002-06-25 | 2004-01-29 | Konica Minolta Holdings Inc | 真空紫外線励起発光素子用蛍光体およびそれを用いた真空紫外線励起発光素子 |
CN102337130B (zh) * | 2010-07-14 | 2014-04-02 | 海洋王照明科技股份有限公司 | 铋离子掺杂的锗硅酸盐发光材料及其制备方法 |
-
2010
- 2010-07-19 WO PCT/CN2010/075254 patent/WO2012009845A1/zh active Application Filing
- 2010-07-19 US US13/700,506 patent/US9034205B2/en active Active
- 2010-07-19 CN CN201080066839.5A patent/CN102906223B/zh active Active
- 2010-07-19 EP EP10854875.1A patent/EP2597132B1/en active Active
- 2010-07-19 JP JP2013518929A patent/JP5667289B2/ja active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1111025A2 (en) * | 1999-12-24 | 2001-06-27 | Sumitomo Chemical Company, Limited | Phosphor for vacuum ultraviolet excited light emitting device |
JP2005298679A (ja) * | 2004-04-12 | 2005-10-27 | Fuji Photo Film Co Ltd | 希土類ホウ酸塩の製造方法 |
CN101184824A (zh) * | 2005-05-24 | 2008-05-21 | 首尔半导体株式会社 | 发光装置及其所使用的碱土金属硫化物的磷光体 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116103045A (zh) * | 2023-02-16 | 2023-05-12 | 华侨大学 | 一种LiSc1-xLuxGeO4:Ln3+,Eu3+光存储材料及其制备方法和应用 |
CN116103045B (zh) * | 2023-02-16 | 2023-12-29 | 华侨大学 | 一种LiSc1-xLuxGeO4:Ln3+,Eu3+光存储材料及其制备方法和应用 |
Also Published As
Publication number | Publication date |
---|---|
JP5667289B2 (ja) | 2015-02-12 |
US20130069004A1 (en) | 2013-03-21 |
JP2013535528A (ja) | 2013-09-12 |
CN102906223B (zh) | 2014-07-02 |
EP2597132B1 (en) | 2016-10-19 |
CN102906223A (zh) | 2013-01-30 |
EP2597132A4 (en) | 2013-11-27 |
EP2597132A1 (en) | 2013-05-29 |
US9034205B2 (en) | 2015-05-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR20020000835A (ko) | 알루민산염 형광체의 제조 방법, 형광체, 및 형광체를함유하는 소자 | |
CN102115667B (zh) | 硼酸盐绿色发光材料及其制备方法 | |
US20130140491A1 (en) | Green to Yellow Light-Emitting Aluminate Phosphors | |
WO2012000179A1 (zh) | 含有金属颗粒的硅酸锌锰发光材料及其制备方法 | |
JP5715242B2 (ja) | 酸化物スズ酸塩発光物質の製造方法 | |
WO2012009844A1 (zh) | 硅酸盐发光材料及其制备方法 | |
WO2012009845A1 (zh) | 一种发光材料及其制备方法 | |
CN114672309A (zh) | 锰离子激活的红色荧光粉及其制备方法 | |
CN102666783A (zh) | 硼酸盐发光材料及其制造方法 | |
WO2011103721A1 (zh) | 掺铽的硼酸钆盐基绿色发光材料及其制备方法 | |
WO2011134148A1 (zh) | 硅酸盐发光材料及其制备方法 | |
US9416308B2 (en) | Core-shell structured silicate luminescent material and preparation method therefor | |
WO2014134854A1 (zh) | 一种稀土掺杂硅酸盐发光玻璃及其制备方法 | |
KR20010062527A (ko) | 진공 자외선 여기 발광 소자용 인광체 | |
CN107541211B (zh) | 适于近紫外光激发的蓝色发光荧光粉及其制备方法和应用 | |
CN1872947A (zh) | 用于等离子体显示板的蓝色磷光体及其制备方法 | |
CN109294583B (zh) | 一种白光led用铈离子掺杂钛酸钆钡蓝光荧光粉及其制备方法 | |
KR100336973B1 (ko) | 저전압용 티탄산스트론튬계 적색 형광체 및 이의 제조방법 | |
KR100285274B1 (ko) | 가돌리늄알루미네이트계 녹색 형광체와 이의 제조방법 | |
CN115261017B (zh) | 一种能够被紫光激发的蓝光发光材料及其制备方法 | |
CN101717638A (zh) | 一种场发射用荧光粉及其制备方法 | |
CN106947474B (zh) | 一种适用于近紫外至蓝光激发的铝酸盐红色荧光粉及其制备方法 | |
CN111996002A (zh) | 一种单一基质白光荧光粉、其制备方法及应用 | |
WO2003055961A1 (fr) | Luminophore rouge | |
CN113717723A (zh) | 一种Eu3+掺杂的铋酸盐红色荧光粉及其制备方法与应用 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 201080066839.5 Country of ref document: CN |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 10854875 Country of ref document: EP Kind code of ref document: A1 |
|
WWE | Wipo information: entry into national phase |
Ref document number: 13700506 Country of ref document: US |
|
REEP | Request for entry into the european phase |
Ref document number: 2010854875 Country of ref document: EP |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2010854875 Country of ref document: EP |
|
ENP | Entry into the national phase |
Ref document number: 2013518929 Country of ref document: JP Kind code of ref document: A |
|
NENP | Non-entry into the national phase |
Ref country code: DE |