CN117363354A - Tm3+ regulated dysprosium activated lanthanum calcium gallate white light fluorescent powder and preparation method and application thereof - Google Patents
Tm3+ regulated dysprosium activated lanthanum calcium gallate white light fluorescent powder and preparation method and application thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 66
- -1 dysprosium activated lanthanum calcium Chemical class 0.000 title claims abstract description 31
- 229910052692 Dysprosium Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 230000001105 regulatory effect Effects 0.000 title claims description 6
- 239000000126 substance Substances 0.000 claims abstract description 9
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 7
- ARWMTMANOCYRLU-UHFFFAOYSA-N [Ca].[La] Chemical class [Ca].[La] ARWMTMANOCYRLU-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005286 illumination Methods 0.000 claims abstract description 5
- 238000004020 luminiscence type Methods 0.000 claims abstract description 5
- 230000005284 excitation Effects 0.000 claims abstract description 4
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims description 31
- 229910052593 corundum Inorganic materials 0.000 claims description 19
- 239000010431 corundum Substances 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 14
- 239000004570 mortar (masonry) Substances 0.000 claims description 14
- 229910052775 Thulium Inorganic materials 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 11
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 5
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C09K11/7768—Chalcogenides with alkaline earth metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention discloses a Tm 3+ A dysprosium-activated calcium lanthanum gallate white light fluorescent powder and a preparation method and application thereof relate to the technical field of rare earth ion luminescence. In particular discloses a chemical formula CaDy 0.02 Tm x La 0.98‑x Ga 3 O 7 Calcium lanthanum gallate white light fluorescent powder, wherein 0<x is less than or equal to 0.03. Dy in the fluorescent powder under 355 nm near ultraviolet excitation 3+ And Tm 3+ Can be used as the light emitting center for realizing 560-600 nm yellow light and 440-470 nm blue light respectively. Further, by adjusting Tm 3+ And the ratio of the luminous intensity of yellow light to the luminous intensity of blue light is adjusted to finally realize white light emission. The fluorescent powder has the advantages of simple preparation process, high luminous efficiency and good stability, and can meet the requirements of various illumination light sources.
Description
Technical Field
The application relates to the technical field of rare earth ion luminescence, in particular to a Tm 3+ Dysprosium-activated lanthanum calcium gallate white light fluorescent powder, and preparation method and application thereof.
Background
White Light Emitting Diodes (WLEDs) are a new type of LED lighting device that has been developed to emit white light based on conventional LEDs. The LED illuminating lamp has the advantages of long service life, low consumption, low heat, high brightness, water resistance, shock resistance, light beam concentration, simplicity and convenience in maintenance and the like, is praised as a fourth-generation green illuminating light source, and has important significance on energy conservation and environmental protection.
Currently, three main methods for realizing WLED are: the first is to excite a blue LED chip to obtain yellow fluorescent powder, and the blue light emitted by the chip and the yellow light emitted by the fluorescent powder are combined to obtain white light; the second kind excites green and red fluorescent powder through blue LED chip, and white light is produced by cooperation; and thirdly, exciting blue, green and red three-primary-color fluorescent powder by using a near ultraviolet LED chip to obtain white light. Although white light can be obtained by the three methods, the defects of low color temperature, poor color rendering property of a light source, complex structure and different proportioning regulation and aging rates among various fluorescent powders still exist, so that the illumination efficiency is easily affected, and the obtained WLED can not meet the use requirement.
Based on the above analysis, the present invention intends to protect a thulium ion (Tm 3+ ) And adjusting dysprosium activated lanthanum calcium gallate white light fluorescent powder. According to the investigation, no thulium ion (Tm) exists at home and abroad at present 3+ ) And regulating the report of dysprosium activated lanthanum calcium gallate white light fluorescent powder.
Disclosure of Invention
The object of the present invention is to provide a Tm 3+ The dysprosium-activated lanthanum calcium gallate white light fluorescent powder can be adjusted to effectively absorb near ultraviolet light and efficiently emit white light. Its preparing process and application are also disclosed.
In order to achieve the above object, the present invention provides a Tm 3+ Dysprosium-activated lanthanum calcium gallate white light fluorescent powder material with chemical expression CaDy 0.02 Tm x La 0.98-x Ga 3 O 7 Wherein 0 is<x≤0.03。
After experimental preference, thulium ions (Tm) with optimal luminescence properties are obtained 3+ ) The dysprosium-activated lanthanum calcium gallate white light fluorescent powder material is CaDy 0.02 Tm x La 0.98-x Ga 3 O 7 Wherein x=0.01. To facilitate the preparation and implementation of the phosphor, a thulium ion (Tm 3+ ) The preparation method of the dysprosium-activated lanthanum calcium gallate white light fluorescent powder material comprises the following specific steps of:
s1: caDy according to chemical expression with analytical balance 0.02 Tm x La 0.98-x Ga 3 O 7 The stoichiometric ratio of each element accurately weighs CaCO 3 、La 2 O 3 、Ga 2 O 3 、Dy 2 O 3 And Tm 2 O 3 The raw materials are put into agate grinding, after being uniformly mixed, the raw materials are pressed into round slices by a tablet press, and the round block materials are put into a corundum crucible;
s2: and (3) placing the corundum crucible in the step (S1) in a muffle furnace, calcining for one time in an air atmosphere at the primary calcining temperature of 1100-1200 ℃ for 24-36 hours, and naturally cooling to room temperature to obtain a primary calcined product. Grinding the calcined product into powder by an agate mortar, pressing the powder into a round sheet by a tablet press again, placing the round block material in a corundum crucible and placing the corundum crucible in a muffle furnace, carrying out secondary calcination under the air atmosphere, wherein the secondary calcination temperature is 1200-1300 ℃, the secondary calcination time is 36-48 hours, and naturally cooling to room temperature to obtain a secondary calcination product; s3: grinding the secondary calcined product in the step S2 into powder by an agate mortar to obtain thulium ions (Tm) 3+ ) And adjusting dysprosium activated lanthanum calcium gallate white light fluorescent powder product. Preferably, the calcium source is CaCO with purity of 99.98 percent 3 The method comprises the steps of carrying out a first treatment on the surface of the The lanthanum source is La of 5N grade 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The gallium source is Ga of 4N grade 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The dysprosium source is Dy of 5N grade 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The thulium source is Tm of 5N-stage 2 O 3 。
Further, in order to facilitate application, implementation and popularization of the phosphor, thulium ions (Tm 3+ ) The application of the dysprosium activated lanthanum calcium gallate white light fluorescent powder is regulated, and the dysprosium activated lanthanum calcium gallate white light fluorescent powder is applied to the field of WLED illumination.
Benefits of the present application include, but are not limited to:
(1) The invention is whiteThe fluorescent powder is Dy 3+ : CaLaGa 3 O 7 Incorporation of Tm 3+ By adjusting Tm 3+ The ratio of the luminous intensity of yellow/blue light is adjusted, thereby realizing white light emission;
(2) CaDy of the invention 0.02 Tm x La 0.98-x Ga 3 O 7 The white light fluorescent powder can effectively absorb near ultraviolet light and efficiently emit white light, so that the fluorescent powder becomes a WLED fluorescent powder;
(3) The method adopts the high-temperature solid-phase sintering method to prepare CaDy 0.02 Tm x La 0.98-x Ga 3 O 7 The white light fluorescent powder has the advantages of simplified process, short production period, high production efficiency and environmental friendliness, is beneficial to realizing the integrated design of material devices, and has the potential of industrialization and mass production;
(4) The product of the invention has the advantages of no toxicity, no pollution and high physical and chemical stability, releases stronger white light under the excitation of near ultraviolet light, and greatly widens the application field of the ion doped lanthanum calcium gallate based multifunctional material.
Drawings
FIG. 1 is CaDy obtained according to examples 1-3 0.02 Tm x La x0.98- Ga 3 O 7 （xAn XRD pattern of =0.005, 0.01, 0.03);
FIG. 2 is CaDy obtained according to examples 1-3 0.02 Tm x La x0.98- Ga 3 O 7 （xEmission spectrum of =0.005, 0.01, 0.03);
FIG. 3 is CaDy obtained according to examples 1-3 0.02 Tm x La x0.98- Ga 3 O 7 （xRatio graph of emission intensity of blue-yellow light of=0.005, 0.01, 0.03);
FIG. 4 is CaDy obtained according to examples 1-3 0.02 Tm x La x0.98- Ga 3 O 7 （x=0.005, 0.01, 0.03).
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
Unless otherwise indicated, all materials and reagents used in this application were purchased commercially, used as received, and the equipment and apparatus used employed the protocols and parameters recommended by the manufacturer.
In the examples, the starting material used was CaCO having a purity of 99.98% 3 La of 5N grade 2 O 3 Dy of 5N level 2 O 3 Tm of 5N-order 2 O 3 And 5N-grade Ga 2 O 3 。
Example 1
S1: taking x=0.005, and according to the chemical formula CaDy 0.02 Tm 0.005 La 0.975 Ga 3 O 7 Is used for accurately weighing CaCO by an electronic balance 3 、La 2 O 3 、Ga 2 O 3 、Dy 2 O 3 And Tm 2 O 3 Raw materials. Placing the raw materials into an agate mortar for full grinding to obtain raw material mixture powder, pressing the raw material mixture powder into a round sheet shape by a tablet press, and placing the round block material into a corundum crucible;
s2: and (3) placing the corundum crucible obtained in the step (S1) in a muffle furnace, calcining for one time in an air atmosphere, wherein the primary calcining temperature is 1200 ℃, the pre-calcining time is 24 hours, and naturally cooling to room temperature to obtain a primary calcining product. Grinding the calcined product into powder by an agate mortar, pressing the powder into a round sheet by a tablet press again, placing the round block material in a corundum crucible and placing the corundum crucible in a muffle furnace, and carrying out secondary calcination at 1250 ℃ for 36 hours in an air atmosphere, and naturally cooling to room temperature to obtain a secondary calcined product; s3: grinding the secondary calcination product in the step S2 into powder by an agate mortar to obtain CaDy 0.02 Tm 0.005 La 0.975 Ga 3 O 7 A phosphor product.
Example 2
S1: taking x=0.01, and according to the chemical formula CaDy 0.02 Tm 0.01 La 0.97 Ga 3 O 7 Is prepared by an electronic balanceAccurately weigh CaCO 3 、La 2 O 3 、Ga 2 O 3 、Dy 2 O 3 And Tm 2 O 3 Raw materials. Placing the raw materials into an agate mortar for full grinding to obtain raw material mixture powder, pressing the raw material mixture powder into a round sheet shape by a tablet press, and placing the round block material into a corundum crucible;
s2: placing the corundum crucible obtained in the step S1 in a muffle furnace, calcining for one time in an air atmosphere, wherein the primary calcining temperature is 1200 ℃, the pre-calcining time is 24 hours, and naturally cooling to room temperature to obtain a primary calcining product; grinding the calcined product into powder by an agate mortar, pressing the powder into a round sheet by a tablet press again, placing the round block material in a corundum crucible, placing the corundum crucible in a muffle furnace, and carrying out secondary calcination at 1250 ℃ for 36 hours in an air atmosphere to obtain a secondary calcined product, and naturally cooling to room temperature; s3: grinding the secondary calcination product in the step S2 into powder by an agate mortar to obtain CaDy 0.02 Tm 0.01 La 0.97 Ga 3 O 7 A phosphor product.
Example 3
S1: taking x=0.03, according to the chemical formula CaDy 0.02 Tm 0.03 La 0.95 Ga 3 O 7 Is used for accurately weighing CaCO by an electronic balance 3 、La 2 O 3 、Ga 2 O 3 、Dy 2 O 3 And Tm 2 O 3 Raw materials. Placing the raw materials into an agate mortar for full grinding to obtain raw material mixture powder, pressing the raw material mixture powder into a round sheet shape by a tablet press, and placing the round block material into a corundum crucible;
s2: and (3) calcining, namely placing the corundum crucible obtained in the step (S1) in a muffle furnace, calcining for one time in an air atmosphere, wherein the primary calcining temperature is 1200 ℃, the pre-calcining time is 24 hours, and naturally cooling to room temperature to obtain a primary calcining product. Grinding the calcined product into powder with agate mortar, pressing into round sheet again with tablet press, placing the round block material in corundum crucible, placing in muffle furnace, and air-treatingSecondary calcination is carried out, the secondary calcination temperature is 1250 ℃, the secondary calcination time is 36 hours, and the secondary calcination product is obtained after natural cooling to room temperature; s3: grinding the secondary calcined product in the step S2 into powder by an agate mortar to obtain CaDy 0.02 Tm 0.03 La 0.95 Ga 3 O 7 A phosphor product.
Experimental detection and data
In the examples, the powder diffraction pattern of the phosphor sample was measured on an X-ray diffractometer SmartLab manufactured by japan physics corporation; the emission spectra were measured on an FLS980 fluorescence spectrometer manufactured by Edinburgh, UK.
Referring to FIG. 1, caDy prepared according to the technical scheme of examples 1-3 0.02 Tm x La x0.98- Ga 3 O 7 （x=0.005, 0.01, 0.03). As can be seen from the graph, the diffraction peak positions of XRD patterns of the adjustable fluorescent powder prepared in each embodiment of the invention basically correspond to the diffraction peak positions of pure phases of XRD patterns of standard samples, and the peak types of the adjustable fluorescent powder have no obvious change, which shows that the embodiment 1,2 and 3 successfully synthesizes pure-phase CaDy with good crystallization 0.02 Tm x La x0.98- Ga 3 O 7 （x=0.005, 0.01, 0.03).
Referring to FIG. 2, caDy prepared according to the technical scheme of examples 1-3 0.02 Tm x La x0.98- Ga 3 O 7 （x=0.005, 0.01, 0.03) emission spectrum at excitation wavelength 355 nm. As can be seen from the figure, the different Tm 3+ The fluorescent powder with doping concentration can emit blue light and yellow light with peak wavelengths near 454 nm and 574 nm, which respectively correspond to Tm 3+ : 1 D 2 → 3 F 4 And Dy 3+ : 4 F 9/2 → 6 H 13/2 And the luminescence intensity of blue light and yellow light is also due to Tm 3+ The doping concentration varies. Therefore, the fluorescent powder can be effectively excited by near ultraviolet light and can emit light in an adjustable state.
Referring to FIG. 3, pressCaDy prepared according to the technical scheme of examples 1-3 0.02 Tm x La x0.98- Ga 3 O 7 （xRatio of blue-yellow light emission intensity of =0.005, 0.01, 0.03) phosphor. As can be seen from the graph, with Tm 3+ The ratio of the luminous intensity of blue and yellow light is also enhanced by the enhancement of the doping concentration. Thus by varying Tm 3+ The relative intensity of the blue-yellow light emission intensity can be adjusted by doping concentration, so that white light is obtained.
Referring to FIG. 4, caDy prepared according to the technical scheme of examples 1-3 0.02 Tm x La x0.98- Ga 3 O 7 （x=0.005, 0.01, 0.03). As can be seen from the figure, whenxWhen=0.01, the color coordinates of the phosphor prepared in example 2 were located in the white light region (x= 0.3321, y= 0.3231), indicating that the phosphor prepared according to the invention was the best experimental color, caDy 0.02 Tm x La x0.98- Ga 3 O 7 （x=0.01) phosphor is a white light phosphor excellent in light emission performance.
In conclusion, the invention successfully prepares the thulium ion and dysprosium ion double doped calcium lanthanum gallate white light fluorescent powder by using a high temperature solid phase sintering method, and Dy in the fluorescent powder is excited by 355 nm near ultraviolet light 3+ And Tm 3+ Can be used as the light emitting center for realizing 560-600 nm yellow light and 440-470 nm blue light respectively. Further, by adjusting Tm 3+ And the ratio of the luminous intensity of yellow light to the luminous intensity of blue light is adjusted to finally realize white light emission. Thulium ion (Tm) of the present invention 3+ ) The dysprosium-activated lanthanum calcium gallate white light fluorescent powder can meet the requirements of various illumination light sources, and has wide application prospects.
The foregoing description is only a few examples of the present application and is not intended to limit the present application in any way, and although the present application is disclosed in the preferred examples, it is not intended to limit the present application, and any person skilled in the art may make some changes or modifications to the disclosed technology without departing from the scope of the technical solution of the present application, and the technical solution is equivalent to the equivalent embodiments.
Claims (6)
1. Tm (Tm) 3+ The dysprosium activated lanthanum calcium gallate white light fluorescent powder is characterized in that: the chemical formula of the fluorescent powder is as follows:
CaDy 0.02 Tm x La 0.98-x Ga 3 O 7 ，
wherein x is 0< 0.03;
in which the ion Dy is doped 3+ And Tm 3+ Occupying Ca 2+ /La 3+ Lattice site of (C), ca 2+ 、Dy 3+ 、Tm 3+ And La (La) 3+ Randomly distributed in the space formed by GaO 4 In the layered electronegative skeleton structure formed by tetrahedra, the crystal structure with multi-lattice regulation and local disorder is realized by regulating Tm 3+ The relative intensity of the yellow/blue light luminous intensity can be changed, and the white light emission is realized.
2. A Tm according to claim 1 3+ The dysprosium activated lanthanum calcium gallate white light fluorescent powder is characterized in that: under 355 nm near ultraviolet excitation, dysprosium and thulium are taken as luminescence centers, and yellow light and blue light with peak center wavelengths of 574 nm and 454 nm are emitted respectively.
3. A Tm according to any one of claims 1-2 3+ The preparation method of the dysprosium activated calcium lanthanum gallate white light fluorescent powder is characterized by at least comprising the following steps: and preparing the white light fluorescent powder from raw materials containing a calcium source, a lanthanum source, a gallium source, a dysprosium source and a thulium source by a high-temperature solid-phase sintering method.
4. A Tm according to claim 3 3+ The preparation method of the dysprosium activated lanthanum calcium gallate white light fluorescent powder is characterized by comprising the following specific steps:
s1: caDy according to chemical expression with analytical balance 0.02 Tm x La 0.98-x Ga 3 O 7 The stoichiometric ratio of each element in the raw materials is accurately weighed, wherein,0<x is less than or equal to 0.03; putting the raw materials into an agate mortar, uniformly mixing to obtain raw material mixture powder, pressing the raw material mixture powder into a round sheet shape by a tablet press, and placing the round block material into a corundum crucible;
s2: placing the corundum crucible in the step S1 in a muffle furnace, calcining for one time in an air atmosphere at the primary calcining temperature of 1100-1200 ℃ for 24-36 hours, and naturally cooling to room temperature to obtain a primary calcining product; grinding the calcined product into powder by an agate mortar, pressing the powder into a round sheet by a tablet press again, placing the round block material in a corundum crucible, and placing the corundum crucible in a muffle furnace for secondary calcination at 1200-1300 ℃ for 36-48 hours under the air atmosphere, and naturally cooling to room temperature to obtain a secondary calcined product; s3: grinding the secondary calcined product in step S2 into powder with agate mortar to obtain thulium ion (Tm) 3+ ) And adjusting dysprosium activated lanthanum calcium gallate white light fluorescent powder material.
5. A Tm according to claim 3 3+ The preparation method of the dysprosium activated lanthanum calcium gallate white light fluorescent powder is characterized by comprising the following steps of: the calcium source is CaCO with the purity of 99.98 percent 3 The method comprises the steps of carrying out a first treatment on the surface of the The lanthanum source is La of 5N grade 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The gallium source is Ga of 4N grade 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The dysprosium source is Dy of 5N grade 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The thulium source is Tm of 5N-stage 2 O 3。
6. A Tm according to claims 1 to 2 3+ Application of dysprosium activated lanthanum calcium gallate white light fluorescent powder is regulated, which is characterized in that Tm 3+ The dysprosium-activated lanthanum calcium gallate white light fluorescent powder is used for the field of LED illumination.
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