CN112877070A - Eu for W-LED3+/Tb3+Doped LiSrPO4Fluorescent powder and preparation method thereof - Google Patents
Eu for W-LED3+/Tb3+Doped LiSrPO4Fluorescent powder and preparation method thereof Download PDFInfo
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- CN112877070A CN112877070A CN202110060923.6A CN202110060923A CN112877070A CN 112877070 A CN112877070 A CN 112877070A CN 202110060923 A CN202110060923 A CN 202110060923A CN 112877070 A CN112877070 A CN 112877070A
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- 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
- C09K11/7795—Phosphates
- C09K11/7796—Phosphates with alkaline earth metals
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- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
Abstract
The invention provides Eu for W-LED3+/Tb3+The LiSrPO4 doped fluorescent powder and the preparation method thereof solve the technical problems of poor color rendering index and low luminous efficiency of the single-matrix white light fluorescent powder in the prior art, and the chemical general formula of the fluorescent powder is LiSr(1‑y‑x)EuxTbyPO4Wherein x is more than or equal to 0.001 and less than or equal to 0.1, and y is more than or equal to 0.001 and less than or equal to 0.1, and the invention also discloses Eu for the W-LED3+/Tb3+The preparation method of the LiSrPO4 doped fluorescent powder can be widely applied to the technical field of LED luminescent materials.
Description
Technical Field
The invention belongs to the technical field of LED luminescent materials, and particularly relates to Eu for W-LED3+/Tb3+Doped LiSrPO4Fluorescent powder and a preparation method thereof.
Background
In recent years, with the development of the Light Emitting Diode (LED) industry, the white light LED (W-LED) lighting field has been receiving increasing attention. Compared with the traditional incandescent lamp and fluorescent lamp, the W-LED lighting source has the advantages of high luminous efficiency, environmental friendliness, high brightness, good reliability, long service life, low cost and the like, and is widely concerned by people in recent years. Near ultraviolet (n-UV) LEDs are currently used, in combination with multiple phosphors emitting in the red, green and blue regions, to produce white light by adjusting the ratio of the multiple phosphors. However, the W-LED device based on the mixing of multiple phosphors has problems of non-uniform fluorescence re-absorption and light emission, etc., and the method has new problems of complicated coating process, high production cost, color re-absorption reduction of light emission efficiency due to the mixing of multiple phosphors, poor color stability, etc. In recent years, researchers have proposed that a single-substrate white-light phosphor is used to emit white light under ultraviolet excitation, but most of the phosphors prepared by using a single substrate currently emit blue light or yellow light, and the spectrum of the phosphors under ultraviolet excitation cannot completely cover red light, green light and blue light, so that the phosphors have the problems of poor color rendering, low luminous efficiency and the like.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides Eu for W-LED3+/Tb3+Doped LiSrPO4Fluorescent powder and a preparation method thereof.
In order to solve the above technical problems, the present invention provides a Eu for W-LED3+/Tb3+Doped LiSrPO4The chemical general formula of the fluorescent powder is LiSr(1-y-x)EuxTbyPO4Wherein x is more than or equal to 0.001 and less than or equal to 0.1, and y is more than or equal to 0.001 and less than or equal to 0.1.
Preferably, x is 0.01 and y is 0.01.
Preferably, x is 0.02 and y is 0.01.
Preferably, the fluorescent powder emits white light under the excitation of ultraviolet light with the wavelength of 227 nm.
Preferably, the raw materials are respectively: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4。
Preferably, Eu3+/Tb3+The purity of the raw material adopted by the LiSrPO 4-doped fluorescent powder is higher than 99.99%.
Eu for preparing W-LED3+/Tb3+Doped LiSrPO4A method of phosphor powder comprising the steps of:
(1) according to the stoichiometric ratio of the elements Li+：Sr2-：Eu3+：Tb3+：PO4 3-Is 1: (1-y-x): x: y: 1, weighing the following compounds: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4；
(2) Dissolving the compound weighed in the step (1) in distilled water, and adding a proper amount of catalyst C6H12O6Heating and evaporating until xerogel is formed; c6H12O6Can be glucose, and can be used as a catalyst to assist in forming colloid which is changed into carbon dioxide and water in subsequent high-temperature sintering.
(3) Calcining the xerogel obtained in the step (2) in a vacuum atmosphere;
(4) and (4) cooling and grinding the calcined mixture obtained in the step (3) to obtain the fluorescent powder.
Preferably, step (1): according to the stoichiometric ratio of the elements, the compounds respectively weighed are mechanically ground and uniformly mixed to obtain a mixture. The subsequent dissolving time is shortened, and the working efficiency is improved.
Preferably, step (2): dissolving the mixture obtained in the step (1) in distilled water, and stirring by using magnetic forceStirring the solution for 30-60 minutes by a stirrer, shortening the dissolving time, and simultaneously adding a proper amount of catalyst C while stirring6H12O6The solution improves the working efficiency, and is heated for 10 to 24 hours at the temperature of 80 to 120 ℃ until xerogel is formed.
Preferably, step (3): and (3) calcining the xerogel obtained in the step (2) for 1-3 hours at 1000 ℃ in a vacuum atmosphere. The calcining apparatus may use an electric furnace.
Preferably, in the step (4), the calcined mixture obtained in the step (3) is naturally cooled and mechanically ground to obtain the fluorescent powder.
The invention has the beneficial effects that: the invention provides Eu for W-LED3+/Tb3+Doped LiSrPO4The fluorescent powder and the preparation method thereof have the following two advantages:
(1) the chemical general formula of the fluorescent powder is LiSr(1-y-x)EuxTbyPO4Wherein x is more than or equal to 0.001 and less than or equal to 0.1, and y is more than or equal to 0.001 and less than or equal to 0.1. By Eu3+、Tb3+Co-doping to realize LiSrPO4The fluorescent powder promotes the ionic hypersensitivity and the charge migration transition, and the LiSrPO is added4、Eu3+、Tb3+Energy transfer between ions. Eu (Eu)3+、Tb3+The ion concentration is adjustable. Compared with the traditional fluorescent powder, the Eu obtained by the invention3+/Tb3+Ion co-doped phosphor by adjusting Eu3+、Tb3+The doping concentration of the Eu is adjusted to realize the light color adjustment in the visible light region under the condition of single matrix, and the Eu is excited at 227nm3+/Tb3+Doped LiSrPO4The fluorescent powder is white and luminous, and has good color rendering and high luminous efficiency.
(2) The fluorescent powder is prepared by a sol-gel-high temperature solid phase synthesis method, has simple method, easy operation and good repeatability, and can effectively ensure Eu3+、Tb3+The rare earth ion doping concentration, the uniformity and the proportion and distribution of other materials, the prepared fluorescent powder has good chemical and thermal stability, and the method has the advantages of good repeatability, simple operation, low production cost, low impurity concentration and the like. Eu (Eu)3+/Tb3+Doped LiSrPO4The fluorescent powder has good application prospect in the ultraviolet W-LED.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
FIG. 1 shows fluorescence spectra measured by the phosphors prepared in examples 1 and 2 under the excitation of ultraviolet light of 227 nm.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application clearer, the present application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
The invention provides Eu for W-LED3+/Tb3+Doped LiSrPO4The chemical general formula of the fluorescent powder is LiSr(1-y-x)EuxTbyPO4Wherein x is more than or equal to 0.001 and less than or equal to 0.1, and y is more than or equal to 0.001 and less than or equal to 0.1. The raw materials are respectively LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4。
Example 1
The invention provides a preparation method of Eu3+/Tb3+ doped LiSrPO4 fluorescent powder for a W-LED, which comprises the following steps:
(1) according to the stoichiometric ratio of the elements Li+：Sr2+：Eu3+：Tb3+：PO4 3-Is 1: 0.98: 0.01: 0.01: 1, weighing the following compounds: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4Mechanically grinding and uniformly mixing to obtain a mixture;
(2) dissolving the mixture obtained in step 1) in distilled water. The solution was stirred for 30 minutes using a magnetic stirrer while adding the appropriate amount of catalyst C under stirring6H12O6The solution was heated at 100 ℃ for 24 hours until a xerogel was formed;
(3) calcining the xerogel obtained in the step 2) in an electric furnace at 1000 ℃ for 1 hour;
(4) naturally cooling the calcined mixture obtained in the step 3), and mechanically grinding to obtain the fluorescent powder.
Example 2
(1) According to the stoichiometric ratio of the elements Li+：Sr2+：Eu3+：Tb3+：PO4 3-Is 1: 0.97: 0.02: 0.01: 1, weighing the following compounds: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4Mechanically grinding and uniformly mixing to obtain a mixture;
(2) dissolving the mixture obtained in step 1) in distilled water. The solution was stirred for 30 minutes using a magnetic stirrer while adding the appropriate amount of catalyst C under stirring6H12O6The solution was heated at 100 ℃ for 24 hours until a xerogel was formed;
(3) calcining the xerogel obtained in the step 2) in an electric furnace at 1000 ℃ for 1 hour;
(4) naturally cooling the calcined mixture obtained in the step 3), and mechanically grinding to obtain the fluorescent powder.
Example 3
(1) According to the stoichiometric ratio of the elements Li+：Sr2+：Eu3+：Tb3+：PO4 3-Is 1: 0.89: 0.1: 0.01: 1, weighing the following compounds: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4Mechanically grinding and uniformly mixing to obtain a mixture;
(2) dissolving the mixture obtained in step 1) in distilled water. The solution was stirred for 30 minutes using a magnetic stirrer while adding the appropriate amount of catalyst C under stirring6H12O6The solution was heated at 100 ℃ for 24 hours until a xerogel was formed;
(3) calcining the xerogel obtained in the step 2) in an electric furnace at 1000 ℃ for 1 hour;
(4) naturally cooling the calcined mixture obtained in the step 3), and mechanically grinding to obtain the fluorescent powder.
Example 4
(1) According to the stoichiometric ratio of the elements Li+：Sr2+：Eu3+：Tb3+：PO4 3-Is 1: 0.97: 0.01: 0.02: 1, weighing the following compounds: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4Mechanically grinding and uniformly mixing to obtain a mixture;
(2) dissolving the mixture obtained in step 1) in distilled water. The solution was stirred for 40 minutes using a magnetic stirrer while adding the appropriate amount of catalyst C under stirring6H12O6The solution was heated at 80 ℃ for 10 hours until a xerogel was formed;
(3) calcining the xerogel obtained in the step 2) in an electric furnace at 1000 ℃ for 2 hours;
(4) naturally cooling the calcined mixture obtained in the step 3), and mechanically grinding to obtain the fluorescent powder.
Example 5
(1) According to the stoichiometric ratio of the elements Li+：Sr2+：Eu3+：Tb3+：PO4 3-Is 1: 0.89: 0.01: 0.1: 1, respectively weighingA compound: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4Mechanically grinding and uniformly mixing to obtain a mixture;
(2) dissolving the mixture obtained in step 1) in distilled water. The solution was stirred for 60 minutes using a magnetic stirrer while adding the appropriate amount of catalyst C under stirring6H12O6The solution was heated at 120 ℃ for 20 hours until a xerogel was formed;
(3) calcining the xerogel obtained in the step 2) in an electric furnace at 1000 ℃ for 3 hours;
(4) naturally cooling the calcined mixture obtained in the step 3), and mechanically grinding to obtain the fluorescent powder.
As shown in fig. 1, the fluorescent powders prepared in embodiments 1 and 2 are selected, and the emission spectra of the visible light emission spectra in the wavelength range of 350nm to 750nm measured under the excitation of ultraviolet light with the wavelength of 227nm by using a xenon lamp as an excitation source have characteristic emission at the wavelengths of 440nm, 487nm, 543nm, 583nm, 618nm and the like of visible light, completely cover the specific wavelengths of red, green and blue lights, can obtain white light with high luminous intensity, and have good color rendering and high luminous efficiency.
The invention provides Eu for W-LED3+/Tb3+Doped LiSrPO4Phosphor powder with chemical general formula of LiSr(1-y-x)EuxTbyPO4Wherein x is more than or equal to 0.001 and less than or equal to 0.1, and y is more than or equal to 0.001 and less than or equal to 0.1. By Eu3+、Tb3+Co-doping to realize LiSrPO4The fluorescent powder promotes the ionic hypersensitivity and the charge migration transition, and the LiSrPO is added4、Eu3+、Tb3+Energy transfer between ions. Eu (Eu)3+、Tb3+The ion concentration is adjustable. Compared with the traditional fluorescent powder, the Eu obtained by the invention3+/Tb3+Ion co-doped phosphor by adjusting Eu3+、Tb3+The doping concentration of the Eu is adjusted to realize the light color adjustment in the visible light region under the condition of single matrix, and the Eu is excited at 227nm3+/Tb3+Doped LiSrPO4The fluorescent powder is white and luminous, and has good color rendering and high luminous efficiency.
The invention also provides Eu for the W-LED3+/Tb3+Doped LiSrPO4The preparation method of the fluorescent powder is prepared by a sol-gel-high temperature solid phase synthesis method, has simple method, easy operation and good repeatability, and can effectively ensure Eu3+、Tb3+The rare earth ion doping concentration, the uniformity and the proportion and distribution of other materials, the prepared fluorescent powder has good chemical and thermal stability, and the method has the advantages of good repeatability, simple operation, low production cost, low impurity concentration and the like. Eu (Eu)3+/Tb3+Doped LiSrPO4The fluorescent powder has good application prospect in the ultraviolet W-LED.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. Eu for W-LED3+/Tb3+Doped LiSrPO4The fluorescent powder is characterized in that the chemical general formula of the fluorescent powder is LiSr(1-y-x)EuxTbyPO4Wherein x is more than or equal to 0.001 and less than or equal to 0.1, and y is more than or equal to 0.001 and less than or equal to 0.1.
2. Eu for W-LED according to claim 13+/Tb3+Doped LiSrPO4The fluorescent powder is characterized in that the value of x is 0.01, and the value of y is 0.01.
3. Eu for W-LED according to claim 13+/Tb3+Doped LiSrPO4The fluorescent powder is characterized in that the value of x is 0.02, and the value of y is 0.01.
4. Eu for W-LED according to claim 13+/Tb3+Doped LiSrPO4The fluorescent powder is characterized in that the fluorescent powder emits white light under the excitation of ultraviolet light with the wavelength of 227 nm.
5. Eu for W-LED according to any one of claims 1 to 33+/Tb3+Doped LiSrPO4The fluorescent powder is characterized in that the raw materials are respectively as follows: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4。
6. Eu for preparing W-LED3+/Tb3+Doped LiSrPO4The method of the fluorescent powder is characterized by comprising the following steps:
(1) according to the stoichiometric ratio of the elements Li+：Sr2-：Eu3+：Tb3+：PO4 3-Is 1: (1-y-x): x: y: 1, weighing the following compounds: LiNO3、Sr(NO3)2、Eu(NO3)3·5H2O、Tb(NO3)3·5H2O、(NH4)2HPO4；
(2) Dissolving the compound weighed in the step (1) in distilled water, and adding a proper amount of catalyst C6H12O6Heating and evaporating until xerogel is formed;
(3) calcining the xerogel obtained in the step (2) in a vacuum atmosphere;
(4) and (4) cooling and grinding the calcined mixture obtained in the step (3) to obtain the fluorescent powder.
7. The method according to claim 6, wherein the step (1): according to the stoichiometric ratio of the elements, the compounds respectively weighed are mechanically ground and uniformly mixed to obtain a mixture.
8. The method of claim 6,the step (2): dissolving the mixture obtained in the step (1) in distilled water, stirring the solution for 30-60 minutes by using a magnetic stirrer, and simultaneously adding a proper amount of catalyst C while stirring6H12O6And heating the solution at 80-120 ℃ for 10-24 hours until a dry gel is formed.
9. The method of claim 6, wherein the step (3): and (3) calcining the xerogel obtained in the step (2) for 1-3 hours at 1000 ℃ in a vacuum atmosphere.
10. The method according to claim 6, wherein the calcined mixture obtained in the step (3) is naturally cooled in the step (4), and the phosphor is obtained after mechanical grinding.
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Citations (3)
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| CN101872741A (en) * | 2009-04-24 | 2010-10-27 | 晶元光电股份有限公司 | Dominant wavelength distribution convergent light emitting element and manufacturing method thereof |
| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
| CN105199729A (en) * | 2015-10-20 | 2015-12-30 | 陕西科技大学 | NaSrPO4:xEu<3+> red phosphor powder for LED (Light Emitting Diode) and preparation method thereof |
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- 2021-01-18 CN CN202110060923.6A patent/CN112877070A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101872741A (en) * | 2009-04-24 | 2010-10-27 | 晶元光电股份有限公司 | Dominant wavelength distribution convergent light emitting element and manufacturing method thereof |
| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
| CN105199729A (en) * | 2015-10-20 | 2015-12-30 | 陕西科技大学 | NaSrPO4:xEu<3+> red phosphor powder for LED (Light Emitting Diode) and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| PATRESIO A.M.NASCIMENTO等: "Luminescence varied by selective excitation in Eu3+,Tb3+-doped LiSrPO4phosphors for W-LEDs applications", 《OPTICAL MATERIALS》 * |
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