CN114591731A - Fluorescent material and preparation method thereof - Google Patents

Fluorescent material and preparation method thereof Download PDF

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Publication number
CN114591731A
CN114591731A CN202210199574.0A CN202210199574A CN114591731A CN 114591731 A CN114591731 A CN 114591731A CN 202210199574 A CN202210199574 A CN 202210199574A CN 114591731 A CN114591731 A CN 114591731A
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fluorescent material
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preparation
nitride
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CN114591731B (en
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那日苏
朝克夫
王新然
王凤翔
马一智
胡大海
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Inner Mongolia Normal 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
    • C09K11/63—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing boron
    • C09K11/632—Halogenides
    • C09K11/634—Halogenides with alkali or alkaline earth metals
    • 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
    • C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
    • C09K11/7732—Halogenides
    • C09K11/7733—Halogenides with alkali or alkaline earth metals
    • 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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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a fluorescent material and a preparation method thereof, wherein the chemical composition general formula of the fluorescent material is MaBbNcOdDe:RfWherein M is at least one of Mg, Ca, Sr and Ba; d is Cl‑、F‑、Br‑And NH4 +At least one of; r is at least one of Eu, Nd, Dy, Ce, Er, Pr, Sm, Yb and Mn; a. b, c, d, e and f are molar coefficients, a is more than or equal to 3 and less than or equal to 9, b is more than or equal to 1 and less than or equal to 6, c is more than or equal to 4 and less than or equal to 12, d is more than or equal to 0 and less than or equal to 0.1, e is more than or equal to 0 and less than or equal to 1, f is more than or equal to 0 and less than or equal to 1, and 2b is c + d. According to the invention, through the limitation of each element and content, the prepared fluorescent material has firmer crystal structure and more stable physical and chemical properties; the excitation spectrum peak position can be adjusted by changing the type of the alkaline earth metal M, and the emission peak position can be changed at the same time, so that the output of different light-emitting wave bands is realized.

Description

Fluorescent material and preparation method thereof
Technical Field
The invention relates to the technical field of fluorescent materials, in particular to a fluorescent material and a preparation method thereof.
Background
White light LED is a new green energy-saving solid-state electric light source which is rapidly developed in recent years. Compared with the traditional incandescent lamp and fluorescent lamp, the white light LED has the characteristics of environmental protection, high efficiency, energy conservation, severe environment resistance, overlong service life, simple structure, small volume, light weight, quick response, low working voltage and good safety performance. And thus is known as a fourth generation lighting electric light source following incandescent, fluorescent, and energy saving lamps. With the rapid development of blue, purple and ultraviolet LEDs in recent years, it is possible to replace traditional incandescent lamps and fluorescent lamps with LEDs for illumination.
At present, in the prior art, the way of implementing white light LED is mainly two ways: firstly, combining three LEDs of red, green and blue to generate white light; and secondly, exciting a corresponding fluorescent material through an ultraviolet chip or a blue light chip to realize white light. The second method is superior to the first method in view of practicality and low cost commercialization. Therefore, the synthesis of fluorescent materials with good luminescent properties is the key to the realization of white LEDs. However, the prior art has certain limitations due to the limitation of fluorescent materials.
Nitride matrix materials are a novel matrix material with excellent physicochemical properties and light-emitting properties discovered in recent years, and most covalent bond nitrides are insulators or semiconductors and have larger bandwidth. Further, covalent bonding of the covalent-bond nitride is strong, and thus a strong electron cloud expansion (nephelacytic) effect may be generated, which may result in a decrease in excited-state energy of the 5d electron of the dopant ion. Has unique stable, firm and diversified crystal structures and has proper lattice positions occupied by activator atoms, so that the material is an ideal host material of a luminescent material. The nitrogen (oxide) compound fluorescent powder has high light conversion efficiency and light color stability, is insensitive to the change of temperature and driving current, and the color drift of the packaged device is very small. For example, Eu2+、Ce3+Luminescence of doped nitrogen (oxide) phosphorIs made up by using rare earth activator occupying cation position in matrix crystal under the action of exciting light4f6 5d→4f7The transition effects fluorescence emission. Due to the diversity of the nitrogen (oxide) material system and N3-The fluorescent material has stronger covalency and good spectrum cutting performance. The crystal field structure can be changed by replacing different ions, rare earth ion energy level splitting with different degrees is formed, and the adjustment of the position of emitted light can be realized, so that the key is how to provide the fluorescent material with high luminous efficiency and stable chemical performance.
Disclosure of Invention
The invention aims to provide a fluorescent material and a preparation method thereof, and the fluorescent material has the excitation wavelength range of 240-450 nm, high luminous efficiency, complete crystallization and stable chemical performance; in addition, the preparation method of the fluorescent material is simple, pollution-free, easy to operate and low in cost.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a fluorescent material in a first aspect, wherein the chemical composition general formula of the fluorescent material is MaBbNcOdDe:RfWherein M is at least one of Mg, Ca, Sr and Ba; d is Cl-、F-、Br-And NH4 +At least one of (a); r is at least one of Eu, Nd, Dy, Ce, Er, Pr, Sm, Yb and Mn; a. b, c, d, e and f are molar coefficients, a is more than or equal to 3 and less than or equal to 9, b is more than or equal to 1 and less than or equal to 6, and 4<c is not more than 12, d is not less than 0 and not more than 0.1, e is not less than 0 and not more than 1, f is not less than 0 and not more than 1, and 2b is c + d.
Preferably, M is Ca and Mg, and the molar ratio of Ca to Mg is 7: 2.
Preferably, M is Sr and Mg, and the molar ratio of Sr to Mg is 8: 1.
Preferably, the wavelength range of the excitation light of the fluorescent material is 240-450 nm.
Preferably, the wavelength range of the emitted light of the fluorescent material is 450-650 nm.
The second aspect of the present invention provides a method for preparing the above fluorescent material, wherein the method comprises the following steps:
(a) according to stoichiometric composition, mixing nitride/hydride containing M, boric acid/nitride containing B, compound containing D and nitride/boride containing R, and performing ball milling uniformly to obtain a mixture;
(b) calcining the mixed mixture at high temperature in nitrogen;
(c) and cooling the calcined product, crushing and sieving to obtain the fluorescent material.
Preferably, in the step (b), the high-temperature calcination specifically comprises heat preservation at 500-800 ℃ for 1-2 h, and then heating to 1200-1500 ℃ for 6-10 h.
Preferably, in the step (b), the high-temperature calcination comprises keeping the temperature at 600 ℃ for 2 hours, and then raising the temperature to 1350 ℃ for 8 hours.
Compared with the prior art, the invention has the beneficial effects that at least:
according to the invention, through the limitation of each element and content, the prepared fluorescent material has firmer crystal structure and more stable physical and chemical properties; the excitation spectrum peak position can be adjusted by changing the type of the alkaline earth metal M, and the emission peak position can be changed at the same time, so that the output of different light-emitting wave bands is realized. When the raw materials do not adopt oxygen-containing compounds, oxygen-free boron nitride luminescent materials can be obtained, and specific fluorescence is enhanced. The boron nitride material belongs to a high-temperature phase product, so that a luminescent material with higher crystallinity and the luminescent brightness thereof can be obtained by properly adding a cosolvent (component D).
Compared with silicon nitride and boron nitride matrix materials, the fluorescent material provided by the invention has the advantages of simple preparation process and low cost.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1 shows the excitation spectrum and the emission spectrum of the fluorescent material of example 1 of the present invention.
FIG. 2 shows the excitation spectrum and the emission spectrum of the fluorescent material of example 2 of the present invention.
FIG. 3 shows the excitation spectrum and the emission spectrum of the fluorescent material of example 3 of the present invention.
FIG. 4 shows the excitation spectrum and the emission spectrum of the fluorescent material of example 4 of the present invention.
FIG. 5 shows the excitation spectrum and the emission spectrum of the fluorescent material of example 5 of the present invention.
Detailed Description
The following describes embodiments of the present invention in detail with reference to the following embodiments. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
The starting materials used in the following examples are all commercially available in a usual manner unless otherwise specified.
Example 1
Fluorescent material
The chemical composition general formula of the fluorescent material is Ca3B2N4(NH4 +)0.02F﹣ 0.02；
Second, preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) weighing various raw materials Ca according to stoichiometric composition3N2，BN，NH4F, mixing and ball-milling uniformly to obtain a mixture;
(b) placing the mixture in a boron nitride dry pot, preserving heat for 1h at 500 ℃ under the nitrogen atmosphere, and then heating to 1300 ℃ and preserving heat for 6 h;
(c) and cooling the calcined product, crushing and sieving to obtain the fluorescent material.
Example 2
Fluorescent material
The chemical composition general formula of the fluorescent material is Ca7Mg2B6N12(NH4 +)0.06F﹣ 0.06；
Second, preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) weighing various raw materials Ca according to stoichiometric composition3N2，Mg3N2，BN，NH4F, mixing and ball-milling uniformly to obtain a mixture;
(b) placing the mixture in a boron nitride dry pot, preserving heat for 2h at 600 ℃ under the nitrogen atmosphere, and then heating to 1350 ℃ and preserving heat for 8 h;
(c) and cooling the calcined product, crushing and sieving to obtain the fluorescent material.
Example 3
Fluorescent material
The chemical composition general formula of the fluorescent material is Ca6.94Mg2B6N12(NH4 +)0.02F﹣ 0.02:Eu0.04；
Second, preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) weighing various raw materials Ca according to stoichiometric composition3N2，Mg3N2、BN，NH4F, mixing EuN, and performing ball milling uniformly to obtain a mixture;
(b) placing the mixture in a boron nitride dry pot, preserving heat for 1h at 800 ℃ under the nitrogen atmosphere, and then heating to 1400 ℃ and preserving heat for 8 h;
(c) and cooling the calcined product, crushing and sieving to obtain the fluorescent material.
Example 4
Fluorescent material
The chemical composition general formula of the fluorescent material is Sr3B2N4(NH4 +)0.02F﹣ 0.02；
Second, preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) weighing various raw materials Sr according to stoichiometric composition3N2，BN，NH4F, mixing and ball-milling uniformly to obtain a mixture;
(b) placing the mixture in a boron nitride dry pot, preserving heat for 1h at 500 ℃ under the nitrogen atmosphere, and then raising the temperature to 1200 ℃ and preserving heat for 6 h;
(c) and cooling the calcined product, crushing and sieving to obtain the fluorescent material.
Example 5
Fluorescent material
The chemical composition general formula of the fluorescent material is Sr8Mg1B6N12(NH4 +)0.02F﹣ 0.02；
Second, preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) weighing various raw materials Sr according to stoichiometric composition3N2，Mg3N2，BN，NH4F, mixing and ball-milling uniformly to obtain a mixture;
(b) placing the mixture in a boron nitride dry pot, preserving heat for 2h at 500 ℃ under the nitrogen atmosphere, and then raising the temperature to 1200 ℃ and preserving heat for 8 h;
(c) and cooling the calcined product, crushing and sieving to obtain the fluorescent material.
Examples of the experiments
1. A fluorescent material was prepared according to the method of example 1, and the excitation spectrum and emission spectrum of the fluorescent material were measured, and the results of the measurement are shown in fig. 1;
as shown in FIG. 1, Ca3B2N4The host material can realize luminescence, the most effective excitation wavelength is 276nm, the strongest peak position of the emission is about 530nm, and green light is emitted. 2. A fluorescent material was prepared according to the method of example 2, and the excitation spectrum and emission spectrum of the fluorescent material were measured, and the results of the measurement are shown in fig. 2; as can be seen from FIG. 2, Ca7Mg2B6N12The matrix material can realize luminescence, the most effective excitation wavelength is 248nm, the strongest peak position of emission is about 579nm, and orange yellow light is emitted. In comparative example 1 and example 2, the excitation wavelength and the emission wavelength can be controlled by controlling the content of Ca and Mg through the regulation of alkaline earth metal ions, the excitation wavelength is shifted to the short wavelength, and the emission wavelength is shifted to the long wavelength.
3. A fluorescent material was prepared according to the method of example 3, and the excitation spectrum and emission spectrum of the fluorescent material were measured, and the results of the measurement are shown in fig. 3; as can be seen from FIG. 3, when the rare earth ions are doped with Ca7Mg2B6N12Thereafter, results distinctly different from those of example 1 and example 2 were achieved. Formation of Eu2+The most effective excitation wavelength is 400nm, the strongest peak position is about 618nm, and red light is emitted. Comparative example 1 and example 2, at Ca7Mg2B6N12Obtaining Eu in the matrix structure2+Broadband transmission of (2). The preferential host material of the patent can provide effective lattice sites for the rare earth luminescent ions to realize the luminescence of the rare earth ions.
4. A fluorescent material was prepared according to the method of example 4, and the excitation spectrum and emission spectrum of the fluorescent material were measured, and the results of the measurement are shown in fig. 4; as can be seen from FIG. 4, Sr3B2N4The host material can realize luminescence, the most effective excitation wavelength is 361nm, the strongest peak position of emission is about 545nm, and yellow light is emitted.
5. A fluorescent material was prepared according to the method of example 5, and the excitation spectrum and emission spectrum of the fluorescent material were measured, and the results of the measurement are shown in fig. 5; as can be seen from FIG. 5, Sr8Mg1B6N12The host material can realize luminescence, the most effective excitation wavelength is 251nm, and the emission is the mostThe strong peak position is about 545nm, and yellow green light is emitted. Compared with the 4 embodiments, the excitation wavelength and the emission wavelength can be regulated and controlled by regulating the dosage of Sr and Mg through regulating and controlling the alkaline earth metal ions, the excitation wavelength moves towards short wave, and the emission wavelength moves towards long wave.
6. Respectively preparing fluorescent materials according to the methods of the embodiments 1 to 5; and detecting the emission spectrum intensity of the obtained fluorescent material under 420nm excitation, wherein the detection results are shown in table 1:
TABLE 1
Group of Light intensity (relative value)
Example 1 7248
Example 2 14560
Example 3 17550
Example 4 6041
Example 5 7038
As can be seen from Table 1: the light spectrum can be regulated and controlled by partially substituting Ca or Sr in Mg in the material, and the intensity of fluorescence can be improved.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.

Claims (8)

1. The fluorescent material is characterized in that the chemical composition general formula of the fluorescent material is MaBbNcOdDe:RfWherein M is at least one of Mg, Ca, Sr and Ba; d is Cl-、F-、Br-And NH4 +At least one of; r is at least one of Eu, Nd, Dy, Ce, Er, Pr, Sm, Yb and Mn; a. b, c, d, e and f are molar coefficients, a is more than or equal to 3 and less than or equal to 9, b is more than or equal to 1 and less than or equal to 6, c is more than or equal to 4 and less than or equal to 12, d is more than or equal to 0 and less than or equal to 0.1, e is more than or equal to 0 and less than or equal to 1, f is more than or equal to 0 and less than or equal to 1, and 2b is c + d.
2. The phosphor of claim 1, wherein M is Ca and Mg at a 7: 2 molar ratio.
3. The phosphor of claim 1, wherein M is Sr and Mg at a molar ratio of 8: 1.
4. The fluorescent material according to claim 1, wherein the wavelength of excitation light of the fluorescent material is in the range of 240 to 450 nm.
5. The fluorescent material according to claim 1, wherein the wavelength of the emitted light is 450 to 650 nm.
6. A method for preparing a fluorescent material according to any one of claims 1 to 5, characterized by comprising the steps of:
(a) according to stoichiometric composition, mixing nitride/hydride containing M, boric acid/nitride containing B, compound containing D and nitride/boride containing R, and performing ball milling uniformly to obtain a mixture;
(b) calcining the mixture in nitrogen at high temperature;
(c) and cooling the calcined product, and then crushing and sieving to obtain the fluorescent material.
7. The method of claim 6, wherein: in the step (b), the high-temperature calcination comprises heat preservation at 500-800 ℃ for 1-2 h, and then heating to 1200-1500 ℃ for 6-10 h.
8. The method of claim 7, wherein: in the step (b), the high-temperature calcination comprises heat preservation at 600 ℃ for 2h, and then heating to 1350 ℃ and heat preservation for 8 h.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4810479A (en) * 1986-04-15 1989-03-07 Centre National De La Recherche Scientifique (Cnrs) Preparation of cubic boron nitride using as a flux a fluoronitride
CN104781369A (en) * 2012-05-22 2015-07-15 皇家飞利浦有限公司 New phosphors, such as new narrow-band red emitting phosphors, for solid state lighting
US20190309222A1 (en) * 2018-04-10 2019-10-10 Nichia Corporation Boron nitride fluorescent material, and method for producing the same
JP2019183146A (en) * 2018-04-10 2019-10-24 日亜化学工業株式会社 Boron nitride phosphor and method for manufacturing the same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4810479A (en) * 1986-04-15 1989-03-07 Centre National De La Recherche Scientifique (Cnrs) Preparation of cubic boron nitride using as a flux a fluoronitride
CN104781369A (en) * 2012-05-22 2015-07-15 皇家飞利浦有限公司 New phosphors, such as new narrow-band red emitting phosphors, for solid state lighting
US20190309222A1 (en) * 2018-04-10 2019-10-10 Nichia Corporation Boron nitride fluorescent material, and method for producing the same
JP2019183146A (en) * 2018-04-10 2019-10-24 日亜化学工業株式会社 Boron nitride phosphor and method for manufacturing the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
RYOTA YAMANASHI, ET AL.: "Photoluminescence property of red light excitable Ca3B2N4:Eu2+ phosphor" *

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