CN111057549A - Novel low-cost single-matrix fluorescent powder for white light LED - Google Patents

Novel low-cost single-matrix fluorescent powder for white light LED Download PDF

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Publication number
CN111057549A
CN111057549A CN201911354434.0A CN201911354434A CN111057549A CN 111057549 A CN111057549 A CN 111057549A CN 201911354434 A CN201911354434 A CN 201911354434A CN 111057549 A CN111057549 A CN 111057549A
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China
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fluorescent powder
white light
light led
matrix
mixture
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CN201911354434.0A
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徐德康
谢飞燕
封科军
刘国聪
陈晓慧
刘燕蕊
彭晓彤
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Huizhou University
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Huizhou University
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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
    • C09K11/7795—Phosphates
    • C09K11/7796—Phosphates 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention belongs to the field of fluorescent materials. A novel cheap single-matrix fluorescent powder for white light LED has a chemical formula of Ca8MgLu(0.6‑x)Alx(PO4)7:0.4Eu3+(ii) a X is more than or equal to 0 and less than or equal to 0.6. The fluorescent powder has stable property structure and fluorescent property, and the preparation method is simple and has low cost.

Description

Novel low-cost single-matrix fluorescent powder for white light LED
Technical Field
The invention belongs to the field of fluorescent materials, and relates to novel low-cost single-matrix fluorescent powder for a white light LED.
Background
The white light LED is a novel solid cold light source, has the advantages of high brightness, low energy consumption, low pollution and the like, and is called as a fourth generation light source following incandescent light, fluorescent light and high-pressure gas discharge lamps. White lightThe main approach is phosphor conversion, and the main performance and indexes of the light source such as luminous efficiency, color rendering index, light color temperature and the like of the white light LED product are directly influenced by the luminous performance of the phosphor. Currently, there are four white LED approaches: the LED chip comprises a yellow fluorescent powder, a blue LED chip, a red-green-blue semiconductor chip, a red-green-blue fluorescent powder and a white fluorescent powder, wherein the yellow fluorescent powder and the blue LED chip are coated on the near-ultraviolet LED chip, and the white fluorescent powder is coated on the near-ultraviolet LED chip. The combination of the white light fluorescent powder and the near ultraviolet LED chip is a scheme with simple preparation process and high energy utilization rate, so that the method is a popular research direction in the current LED research field. The choice of the single-matrix white phosphor has a great influence on the properties of the emission, in particular the luminous efficiency, the emission color and the brightness. The rare earth doped calcium phosphate luminescent material is a good luminescent substrate, however, at present, the rare earth doped calcium phosphate luminescent material is mostly focused on the substrate taking rare earth elements as main components, such as Ca8MgLa(PO4)7、Ca8MgY(PO4)7、Ca8MgGd(PO4)7、Ca8MgLu(PO4)7Although these single substrates can achieve better white light performance, the rare earth is expensive, and the cost for reaching pilot scale and mass production is high, so it is important to find a single-substrate phosphor with lower price.
The doping modification of the rare earth-based fluorescent powder is generally carried out by doping the same group of elements, namely rare earth ions are used for replacing the rare earth ions, and the physicochemical properties of the fluorescent powder can be effectively maintained mainly due to the similarity of the element properties. Nevertheless, the rare earth elements have high preparation cost, and thus a metal element with low price and excellent properties is demanded as a substitute.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel low-cost single-matrix fluorescent powder for a white light LED, wherein the fluorescent powder has stable property structure and fluorescent property, and the preparation method is simple and has low cost.
The technical scheme of the invention is as follows:
novel cheap white light LThe single-matrix fluorescent powder for ED has a chemical formula of Ca8MgLu(0.6-x)Alx(PO4)7:0.4Eu3 +；0≤x≤0.6。
A preparation method of novel cheap single-matrix fluorescent powder for a white light LED comprises the following steps: by NH4H2PO4、CaCO3、(MgCO3)4·Mg(OH)2·5H2O、Eu2O3、Al2O3And Lu2O3Is prepared by adopting a high-temperature solid phase method as a raw material.
Further, the preparation method comprises the following steps: reacting NH4H2PO4、CaCO3、(MgCO3)4·Mg(OH)2·5H2O、Eu2O3、Al2O3And Lu2O3Weighing according to the stoichiometric ratio of the chemical formula, fully grinding until the mixture is uniformly mixed, transferring the mixture into a corundum crucible, calcining the mixture for 3 to 5 hours at the temperature of 1100-1300 ℃ by adopting a high-temperature box furnace, and cooling the mixture to room temperature to obtain the single-matrix fluorescent powder.
The invention has the following beneficial effects:
the aluminum ions and the rare earth ions are equivalent, the ionic radius of the aluminum ions is smaller than that of the rare earth ions, the aluminum ions are used as a light element to replace heavy rare earth elements, the rare earth ions can well replace the rare earth ion lattice sites in the fluorescent powder matrix, and the lattice structure of the fluorescent powder is not changed. By substitution of equivalent aluminium ions for Ca8MgLu(PO4)7The lutetium ions in the fluorescent powder have stable fluorescent effect, and the preparation cost of the fluorescent powder is greatly reduced on the basis of not changing the crystal structure and the fluorescent property of the fluorescent powder.
Drawings
FIG. 1 is an XRD spectrum of phosphors of examples 1-7 of the present invention;
FIG. 2 is a fluorescent image of the phosphors of examples 1-7 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention.
Example 1
A novel cheap single-matrix fluorescent powder for white light LED has a chemical formula of Ca8MgLu0.6(PO4)7:0.4Eu3+。
Example 2
A novel cheap single-matrix fluorescent powder for white light LED has a chemical formula of Ca8MgLu0.5Al0.1(PO4)7:0.4Eu3+。
Example 3
A novel cheap single-matrix fluorescent powder for white light LED has a chemical formula of Ca8MgLu0.4Al0.2(PO4)7:0.4Eu3+。
Example 4
A novel cheap single-matrix fluorescent powder for white light LED has a chemical formula of Ca8MgLu0.3Al0.3(PO4)7:0.4Eu3+。
Example 5
A novel cheap single-matrix fluorescent powder for white light LED has a chemical formula of Ca8MgLu0.2Al0.4(PO4)7:0.4Eu3+。
Example 6
A novel cheap single-matrix fluorescent powder for white light LED has a chemical formula of Ca8MgLu0.1Al0.5(PO4)7:0.4Eu3+。
Example 7
A novel cheap single-matrix fluorescent powder for white light LED has a chemical formula of Ca8MgAl0.6(PO4)7:0.4Eu3+。
The preparation method of the novel cheap single-matrix fluorescent powder for the white light LED comprises the following steps: reacting NH4H2PO4、CaCO3、(MgCO3)4·Mg(OH)2·5H2O、Eu2O3、Al2O3And Lu2O3Weighing according to the stoichiometric ratio of the chemical formula, fully grinding until the mixture is uniformly mixed, transferring the mixture into a corundum crucible, calcining the mixture for 3 hours at the temperature of 1200 ℃ by adopting a high-temperature box furnace, and cooling the mixture to room temperature to obtain the single-matrix fluorescent powder.
The experimental results of the novel cheap single-matrix fluorescent powder for the white light LED of the invention in the embodiments 1 to 7 are as follows:
FIG. 1 shows examples 1 to 7 with different Al3+Ca prepared at ionic concentration8MgLu x0.6-Al x (PO4)7:0.4Eu3+XRD spectrogram of the phosphor powder shows that Al is visible3+Doping and Al3+The change of the concentration does not affect the crystal structure of the fluorescent powder, only the crystal lattices of the fluorescent powder slightly expand, and the fluorescence performance of the fluorescent powder is not affected.
FIG. 2 shows examples 1 to 7 with different Al3+Ca prepared at ionic concentration8MgLu x0.6-Al x (PO4)7:0.4Eu3+The fluorescence patterns of the phosphors, 1-7 in FIG. 2 correspond to the phosphor samples of examples 1-7, respectively, and the fluorescence intensity of different samples has no obvious change by visual observation, so that Al can be seen3+The doping of the fluorescent powder has no influence on the fluorescent effect of the fluorescent powder, and the fluorescent powder has stable fluorescent performance.
The novel cheap single-matrix fluorescent powder for the white light LED has stable property structure and fluorescent property, the preparation method is simple, and the cost is low.

Claims (3)

1. A novel cheap single-matrix fluorescent powder for white light LED is characterized in that the chemical formula of the fluorescent powder is Ca8MgLu(0.6-x)Alx(PO4)7:0.4Eu3+；0≤x≤0.6。
2. The method for preparing the novel cheap single-matrix fluorescent powder for the white light LED as claimed in claim 1, wherein NH is used4H2PO4、CaCO3、(MgCO3)4·Mg(OH)2·5H2O、Eu2O3、Al2O3And Lu2O3Is prepared by adopting a high-temperature solid phase method as a raw material.
3. The method for preparing the novel cheap single-matrix fluorescent powder for the white light LED according to claim 2, is characterized in that: reacting NH4H2PO4、CaCO3、(MgCO3)4·Mg(OH)2·5H2O、Eu2O3、Al2O3And Lu2O3Weighing according to the stoichiometric ratio of the chemical formula, fully grinding until the mixture is uniformly mixed, transferring the mixture into a corundum crucible, calcining the mixture for 3 to 5 hours at the temperature of 1100-1300 ℃ by adopting a high-temperature box furnace, and cooling the mixture to room temperature to obtain the single-matrix fluorescent powder.
CN201911354434.0A 2019-12-25 2019-12-25 Novel low-cost single-matrix fluorescent powder for white light LED Pending CN111057549A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW201113352A (en) * 2009-10-12 2011-04-16 Ind Tech Res Inst Phosphors, fabricating method thereof, and light emitting device employing the same
CN102051176A (en) * 2009-10-27 2011-05-11 财团法人工业技术研究院 Fluorescent material, manufacture method thereof and light-emitting device comprising fluorescent material
CN108192615A (en) * 2018-01-11 2018-06-22 青海大学 White phosphorus ore deposit type Sr9Al(PO4)7:Eu2+Phosphate base fluorescent material and its preparation method and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW201113352A (en) * 2009-10-12 2011-04-16 Ind Tech Res Inst Phosphors, fabricating method thereof, and light emitting device employing the same
CN102051176A (en) * 2009-10-27 2011-05-11 财团法人工业技术研究院 Fluorescent material, manufacture method thereof and light-emitting device comprising fluorescent material
CN108192615A (en) * 2018-01-11 2018-06-22 青海大学 White phosphorus ore deposit type Sr9Al(PO4)7:Eu2+Phosphate base fluorescent material and its preparation method and application

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
FEIYAN XIE ET AL.,: ""A novel pure red phosphor Ca8MgLu(PO4)7:Eu3+ for near ultraviolet white li"A novel pure red phosphor Ca8MgLu(PO4)7:Eu3+ for near ultraviolet white light-emitting diodes"ght-emitting diodes"", 《CERAMICS INTERNATIONAL》 *
SHIQI LIU ET AL.,: ""The exploration of structure evolution and photoluminescence property in Ca9Al1-xYx(PO4)7:Eu2+ solid solution phosphors via the construction of bi-directional relationships"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
斋藤胜裕: "《漫画元素118》", 30 April 2015, 上海交通大学出版社 *
杜福平: ""Eu3+掺杂具有白磷钙矿结构碱土金属多磷酸盐的发光和结构研究"", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》 *
洪广言 等: "《稀土发光材料》", 31 May 2016, 冶金工业出版社 *
范红俊 等: "《化学基础》", 31 July 2017, 中国矿业大学出版社 *

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Application publication date: 20200424