CN114591731B - Fluorescent material and preparation method thereof - Google Patents
Fluorescent material and preparation method thereof Download PDFInfo
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- CN114591731B CN114591731B CN202210199574.0A CN202210199574A CN114591731B CN 114591731 B CN114591731 B CN 114591731B CN 202210199574 A CN202210199574 A CN 202210199574A CN 114591731 B CN114591731 B CN 114591731B
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- 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
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- 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
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- C09K11/7733—Halogenides with alkali or alkaline earth metals
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Abstract
The invention discloses a fluorescent material and a preparation method thereof, wherein the chemical composition general formula of the fluorescent material is M a B b N c O d D e :R f Wherein M is at least one of Mg, ca, sr and Ba; d is Cl ‑ 、F ‑ 、Br ‑ And NH 4 + At least one of (a) and (b); 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 of 3.ltoreq.a.ltoreq.9, 1.ltoreq.b.ltoreq.6, 4.ltoreq.c.ltoreq.12, 0.ltoreq.d.ltoreq.0.1, 0.ltoreq.e.ltoreq.1, 0.ltoreq.f.ltoreq.1, and 2b=c+d. The invention ensures that the prepared fluorescent material has stronger crystal structure and more stable physical and chemical properties by limiting the elements and the content; 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 luminous wave bands is realized.
Description
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 LEDs are a new type of green energy-saving solid-state electric light source that has 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 saving, severe environment resistance, super long service life, simple structure, small volume, light weight, quick response, low working voltage and good safety performance. And thus are known as fourth generation illumination electric light sources following incandescent, fluorescent, and energy-saving lamps. With the rapid development of blue, violet and ultraviolet LEDs in recent years, it has become possible to realize illumination by replacing conventional incandescent lamps and fluorescent lamps with LEDs.
At present, in the prior art, the mode of realizing a white light LED is mainly two ways: 1. white light is generated by combining three LEDs of red, green and blue; 2. the corresponding fluorescent material is excited by the ultraviolet chip or the blue light chip to realize white light. The second method is superior to the first method in view of practicality and low cost commercialization. Thus, the synthesis of fluorescent materials with good luminescence properties is critical for achieving white LEDs. However, the prior art has certain limitations due to the limitations of fluorescent materials.
Nitride matrix materials are novel matrix materials with excellent physical and chemical properties and luminescent properties discovered in recent years, and most covalent bond nitrides are insulators or semiconductors and have large bandwidth. And because covalent bond nitride has stronger covalent bond, a stronger electron cloud expansion (nephelauxetic) effect can be generated, and the reduction of the excited state energy of 5d electrons of doped ions can be possibly caused. Has unique stable, firm and diverse crystal structures and proper lattice positions occupied by activator atoms, and is an ideal matrix material of luminescent materials. The nitrogen (oxygen) compound fluorescent powder has higher light conversion efficiency and light color stability, is insensitive to temperature and driving current changes, and has very small color drift of the packaged device. For example Eu 2+ 、Ce 3+ The luminescence of the doped nitrogen (oxygen) compound fluorescent powder is utilized by the rare earth activator occupying the cation position in the matrix crystal under the action of the excitation light 4 f 6 5 d→ 4 f 7 The transition achieves fluorescence emission. Due to the diversity of nitrogen (oxide) material systems and N 3- The strong covalent property and the nitrogen (oxygen) oxide system fluorescent material have good spectrum cutting performance. The crystal field structure can be changed through different ion substitutions to form rare earth ion energy level splitting with different degrees, and the adjustment of the light emitting position can be realized, so that how to provide a fluorescent material with high luminous efficiency and stable chemical property is particularly critical.
Disclosure of Invention
The invention aims to provide a fluorescent material and a preparation method thereof, wherein the excitation wavelength range of the fluorescent material is 240-450 nm, the luminous efficiency is high, the crystallization is complete, and the chemical property is stable; 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 object of the present invention, the following technical solutions are specifically adopted:
the first aspect of the invention provides a fluorescent material, wherein the chemical composition general formula of the fluorescent material is M a B b N c O d D e :R f Wherein M is at least one of Mg, ca, sr and Ba; d is Cl - 、F - 、Br - And NH 4 + At least one of (a) and (b); r is at least one of Eu, nd, dy, ce, er, pr, sm, yb and Mn; a. b, c, d, e and f are mole 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 less than or equal to 12, d is less than or equal to 0 and less than or equal to 0.1, e is less than or equal to 0 and less than or equal to 1, f is less than or equal to 0 and less than or equal to 1, and 2b=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 to 650nm.
The second aspect of the present invention provides a method for preparing the fluorescent material, which comprises the following steps:
(a) Mixing and ball milling M-containing nitride/hydride, boric acid/B-containing nitride, D-containing compound and R-containing nitride/boride uniformly according to stoichiometric composition to obtain a mixture;
(b) Calcining the mixture at high temperature in nitrogen;
(c) And cooling the calcined product, and then crushing and sieving the cooled calcined product 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 heat preservation at 1200-1500 ℃ for 6-10 h.
Preferably, in the step (b), the high-temperature calcination comprises heat preservation at 600 ℃ for 2 hours, and heat preservation at 1350 ℃ for 8 hours.
Compared with the prior art, the invention has the beneficial effects that at least:
the invention ensures that the prepared fluorescent material has stronger crystal structure and more stable physical and chemical properties by limiting the elements and the content; 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 luminous wave bands is realized. When no oxygen-containing compound is used in the raw material, an oxygen-free boron nitride light-emitting material can be obtained, and specific fluorescence is enhanced. The boron nitride material disclosed by the invention belongs to a high-temperature phase product, so that a luminescent material with higher crystallinity and luminescent brightness thereof can be obtained by properly adding a cosolvent (D component).
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 embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. Like elements or portions are generally identified by like reference numerals throughout the several figures. In the drawings, elements or portions thereof are not necessarily drawn to scale.
FIG. 1 is a graph showing the excitation spectrum and the emission spectrum of the fluorescent material of example 1 of the present invention.
FIG. 2 is a graph showing the excitation spectrum and the emission spectrum of the fluorescent material of example 2 of the present invention.
FIG. 3 is a graph showing the excitation spectrum and the emission spectrum of the fluorescent material of example 3 of the present invention.
FIG. 4 is a graph showing the excitation spectrum and the emission spectrum of the fluorescent material of example 4 of the present invention.
FIG. 5 is a graph showing the excitation spectrum and the emission spectrum of the fluorescent material of example 5 of the present invention.
Detailed Description
Embodiments of the technical scheme of the present invention will be described in detail below with reference to the embodiments. The following examples are only for more clearly illustrating the technical aspects of the present invention, and thus are merely examples, and are not intended to limit the scope of the present invention.
It is noted that unless otherwise indicated, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention pertains.
The starting materials used in the examples below are all commercially available as usual unless otherwise specified.
Example 1
1. Fluorescent material
The chemical composition general formula of the fluorescent material is Ca 3 B 2 N 4 (NH 4 + ) 0.02 F ﹣ 0.02 ；
2. Preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) Weighing Ca as raw material according to stoichiometric composition 3 N 2 ，BN，NH 4 F, mixing and ball milling uniformly to obtain a mixture;
(b) Placing the mixture into a boron nitride dry pot, preserving heat for 1h at 500 ℃ under nitrogen atmosphere, and then raising the temperature to 1300 ℃ and preserving heat for 6h;
(c) Cooling the calcined product, pulverizing, and sieving to obtain the fluorescent material.
Example 2
1. Fluorescent material
The chemical composition general formula of the fluorescent material is Ca 7 Mg 2 B 6 N 12 (NH 4 + ) 0.06 F ﹣ 0.06 ；
2. Preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) Weighing Ca as raw material according to stoichiometric composition 3 N 2 ，Mg 3 N 2 ，BN，NH 4 F, mixing and ball milling uniformly to obtain a mixture;
(b) Placing the mixture into a boron nitride dry pot, preserving heat for 2 hours at 600 ℃ under nitrogen atmosphere, and preserving heat for 8 hours at 1350 ℃;
(c) Cooling the calcined product, pulverizing, and sieving to obtain the fluorescent material.
Example 3
1. Fluorescent material
The chemical composition general formula of the fluorescent material is Ca 6.94 Mg 2 B 6 N 12 (NH 4 + ) 0.02 F ﹣ 0.02: Eu 0.04 ；
2. Preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) Weighing Ca as raw material according to stoichiometric composition 3 N 2 ，Mg 3 N 2 、BN，NH 4 F, mixing EuN and ball milling uniformly to obtain a mixture;
(b) Placing the mixture into a boron nitride dry pot, preserving heat for 1h at 800 ℃ under nitrogen atmosphere, and preserving heat for 8h after heating to 1400 ℃;
(c) Cooling the calcined product, pulverizing, and sieving to obtain the fluorescent material.
Example 4
1. Fluorescent material
The chemical composition general formula of the fluorescent material is Sr 3 B 2 N 4 (NH 4 + ) 0.02 F ﹣ 0.02 ；
2. Preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) Weighing various raw materials Sr according to stoichiometric composition 3 N 2 ，BN，NH 4 F, mixing and ball milling uniformly to obtain a mixture;
(b) Placing the mixture into a boron nitride dry pot, preserving heat for 1h at 500 ℃ under nitrogen atmosphere, and then raising the temperature to 1200 ℃ and preserving heat for 6h;
(c) Cooling the calcined product, pulverizing, and sieving to obtain the fluorescent material.
Example 5
1. Fluorescent material
The chemical composition general formula of the fluorescent material is Sr 8 Mg 1 B 6 N 12 (NH 4 + ) 0.02 F ﹣ 0.02 ；
2. Preparation method
The preparation method of the fluorescent material comprises the following steps:
(a) Weighing various raw materials Sr according to stoichiometric composition 3 N 2 ，Mg 3 N 2 ，BN，NH 4 F, mixing and ball milling uniformly to obtain a mixture;
(b) Placing the mixture into a boron nitride dry pot, preserving heat for 2 hours at 500 ℃ under nitrogen atmosphere, and then raising the temperature to 1200 ℃ and preserving heat for 8 hours;
(c) Cooling the calcined product, pulverizing, and sieving to obtain the fluorescent material.
Experimental example
1. A fluorescent material was prepared according to the method of example 1, and the excitation spectrum and the emission spectrum of the fluorescent material were tested, and the test results are shown in fig. 1;
as can be seen from FIG. 1, ca 3 B 2 N 4 The matrix material can realize luminescence, the most effective excitation wavelength is 276nm, the emission maximum peak position 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 the emission spectrum of the fluorescent material were tested, and the test results are shown in fig. 2; as can be seen from FIG. 2, ca 7 Mg 2 B 6 N 12 The matrix material can realize luminescence, the most effective excitation wavelength is 248nm, the emission maximum peak position is about 579nm, and orange light is emitted. In comparative examples 1 and 2, the excitation wavelength and the emission wavelength can be controlled by controlling the contents of Ca and Mg by controlling the alkaline earth metal ions, the excitation wavelength is shifted to a short wavelength, and the emission wavelength is shifted to a long wavelength.
3. A fluorescent material was prepared in the same manner as in example 3, and the excitation spectrum and the emission spectrum of the fluorescent material were measured, and the measurement results are shown in fig. 3; as can be seen from FIG. 3, when the rare earth ions are doped with Ca 7 Mg 2 B 6 N 12 After that, a result quite different from that of example 1 and example 2 was achieved. Eu formation 2+ Is the most effective excitation waveThe length is 400nm, the maximum intensity peak position is about 618nm, and the red light is emitted. Comparative example 1 and example 2, in Ca 7 Mg 2 B 6 N 12 Eu is obtained in the matrix structure of (a) 2+ Is a wideband transmission of (a). The matrix material with the priority of the patent can provide effective lattice sites for rare earth luminescent ions to realize the luminescence of the rare earth ions.
4. A fluorescent material was prepared in the same manner as in example 4, and the excitation spectrum and the emission spectrum of the fluorescent material were measured, and the measurement results are shown in fig. 4; as can be seen from FIG. 4, sr 3 B 2 N 4 The matrix material can realize luminescence, the most effective excitation wavelength is 361nm, the emission maximum peak position is about 545nm, and yellow light is emitted.
5. Fluorescent materials were prepared according to the method of example 5, and the excitation spectrum and the emission spectrum of the fluorescent materials were tested, and the test results are shown in fig. 5; as can be seen from FIG. 5, sr 8 Mg 1 B 6 N 12 The matrix material can realize luminescence, the most effective excitation wavelength is 251nm, the emission maximum peak position is about 545nm, and yellow-green light is emitted. Compared with the above 4 embodiments, the excitation wavelength and the emission wavelength can be regulated and controlled by regulating and controlling alkaline earth metal ions and regulating the dosage of Sr and Mg, and the excitation wavelength moves to a short wave and the emission wavelength moves to a long wave.
6. Fluorescent materials were prepared in the same manner as in examples 1 to 5, respectively; and detecting the emission spectrum intensity of the obtained fluorescent material under 420nm excitation, wherein the detection result is shown in table 1:
TABLE 1
| Group of | Light intensity (relative values) |
| Example 1 | 7248 |
| Example 2 | 14560 |
| Example 3 | 17550 |
| Example 4 | 6041 |
| Example 5 | 7038 |
As can be seen from table 1: by substituting Ca or Sr for part of Mg in the material, not only the spectrum can be regulated, but also the fluorescence intensity can be improved.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention, and are intended to be included within the scope of the appended claims and description.
Claims (2)
1. A fluorescent material, characterized in that the chemical composition general formula of the fluorescent material is Ca 6.94 Mg 2 B 6 N 12 (NH 4 + ) 0.02 F ﹣ 0.02: Eu 0.04 。
2. The method for preparing a fluorescent material according to claim 1, comprising the steps of:
(a) In stoichiometric groupsWeighing Ca as various raw materials 3 N 2 ，Mg 3 N 2 、BN，NH 4 F, mixing EuN and ball milling uniformly to obtain a mixture;
(b) Placing the mixture into a boron nitride dry pot, preserving heat for 1h at 800 ℃ under nitrogen atmosphere, and preserving heat for 8h after heating to 1400 ℃;
(c) Cooling the calcined product, pulverizing, and sieving to obtain the fluorescent material.
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