CN109054830B - Fluorescent material of various titanium germanates for white light LED and preparation method thereof - Google Patents

Fluorescent material of various titanium germanates for white light LED and preparation method thereof Download PDF

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CN109054830B
CN109054830B CN201810780293.8A CN201810780293A CN109054830B CN 109054830 B CN109054830 B CN 109054830B CN 201810780293 A CN201810780293 A CN 201810780293A CN 109054830 B CN109054830 B CN 109054830B
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CN109054830A (en
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田莲花
付世豪
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Yanbian University
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    • 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
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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
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7775—Germanates

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Abstract

The invention discloses a fluorescent material of various titanium germanates for a white light LED, and the chemical expression of the fluorescent material is AaMbTi0.9Ge0.1O3cR, A is one or the combination of Mg, Ba, Sr and Ca; m is one or the combination of La, Gd and Y; o is oxygen element; r is one or the combination of Pr, Sm, Eu, Tb, Dy, Mn, Cr, Bi and Ce; c is more than or equal to 0.001 and less than or equal to 0.133. The invention relates to a fluorescent material which can convert ultraviolet light, near ultraviolet light and blue light into visible light with higher brightness and can be used for a white light LED. The fluorescent material can be used for white light LEDs and related display and lighting devices. The invention has the advantages of cheap and easily obtained raw materials, simple preparation method, stable chemical properties and good luminescence performance, and is an ideal candidate material of the white light LED fluorescent powder. The invention discloses a preparation method of a plurality of titanium germanate fluorescent materials for a white light LED.

Description

Fluorescent material of various titanium germanates for white light LED and preparation method thereof
Technical Field
The invention belongs to the technical field of fluorescent material science, and particularly relates to a fluorescent material which can be effectively excited by ultraviolet, near ultraviolet and blue light and is used for various titanium germanates of a white light LED and a preparation method thereof.
Background
White LEDs are fourth-generation lighting electric light sources following incandescent, fluorescent, and energy-saving lamps, and are light emitting diodes emitting light of white color, and the white light is composed of light of a plurality of wavelengths. The light source has the advantages of high efficiency, less energy consumption, strong applicability, high stability, no environmental pollution, multicolor luminescence and the like, and is called as the most valuable new light source in the 21 st century. The mainstream scheme of the current LED solid light source is a phosphor light conversion white light LED, and the core problem is to develop a high-efficiency phosphor. Since the phosphor determines important characteristics and parameters of the white LED, such as light conversion efficiency, lumen efficiency, luminous flux, correlated color temperature, chromaticity coordinate values, and color rendering index. Therefore, the development of high-efficiency luminescent materials for white LEDs is a critical step. The red fluorescent powder which can be applied to the LED at present has low conversion efficiency due to narrow absorption wavelength range, and cannot meet the requirement of high-performance devices due to poor stability. Therefore, the development of the novel red fluorescent powder for the LED has wide economic application value.
With the continuous development of LED light sources, the application of the LED light sources in the agricultural field is more and more emphasized. The spectrum of the LED light source can be controlled in a very narrow range, the spectrum energy required by plant photosynthesis and photomorphogenesis can be met to a great extent, light can be supplemented in a targeted manner according to the characteristics of chlorophyll absorption spectrum, and the photosynthesis efficiency of plants is improved. The different spectral energy distributions have different promoting effects on the growth and development of crops, the wavelength range of photosynthetically active radiation of green plants is 400-700 nm, the plants can only receive the spectral energy with specific wavelength for photosynthesis, and certain spectral energy and excessive specific wavelength have no obvious effect on the growth of the crops. The red light can promote the formation of chlorophyll and promote the decomposition of carbon dioxide and the synthesis of carbohydrate; blue-violet light can promote synthesis of proteins and the like. In modern agricultural development, the traditional light source is limited by conditions such as a light emitting mechanism and the like, and the requirement of crop illumination cannot be met. Therefore, the search for a novel high-efficiency fluorescent material suitable for agricultural illumination has certain research and practical application values.
Disclosure of Invention
The invention aims to solve the problem that the existing fluorescent material for the white light LED has a plurality of defects and cannot prepare high-performance devices, and provides a novel high-efficiency fluorescent material which can be effectively excited by ultraviolet, near ultraviolet and blue light and is used for a plurality of titanium germanates of the white light LED for meeting the agricultural illumination development.
The invention also provides a preparation method of the fluorescent materials of various titanium germanates for the white light LED.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a fluorescent material of multiple titanium germanates for white light LED has a chemical expression of AaMbTi0.9Ge0.1O3: cR，
Wherein, A is one or the combination of Mg, Ba, Sr and Ca;
m is one or the combination of La, Gd and Y;
o is oxygen element;
r is one or the combination of Pr, Sm, Eu, Tb, Dy, Mn, Cr, Bi and Ce;
c represents R and AaMbTi0.9Ge0.1O3The mass ratio of c to c is 1, and c is more than or equal to 0.001 and less than or equal to 0.133.
The fluorescent material further comprises
Ca0.8-aAaMbTi0.9Ge0.1O3cEu, wherein A = Mg, Ba, Sr or Ca, a is more than or equal to 0 and less than or equal to 0.8, and c is more than or equal to 0 and less than or equal to 0.133; ca0.8La0.133-bMbTi0.9Ge0.1O3cEu, wherein MbB is more than or equal to 0 and less than or equal to 0.133, and c is more than or equal to 0 and less than or equal to 0.133;
Ca0.8La0.133Ti0.9Ge0.1O3: cR1、R2wherein R is1，R2And c is more than or equal to 0 and less than or equal to 0.133.
The fluorescent material can realize visible light emission including red light, green white light and the like, such as Ca0.8La0.133Ti0.9Ge0.1O30.01Eu has red light emission, Ca0.8La0.133Ti0.9Ge0.1O30.01Dy has blue-white emission, etc., and the fluorescent material includes, but is not limited to:
Ca0.8La0.133Ti0.9Ge0.1O3:0.01Eu、 Ba0.8La0.133Ti0.9Ge0.1O3:0.01Eu、Mg0.8La0.133Ti0.9Ge0.1O3:0.01Eu、 Ca0.79Mg0.01La0.133Ti0.9Ge0.1O3:0.01Eu 、Ca0.7Mg0.1La0.133Ti0.9Ge0.1O3:0.01Eu、Ca0.8Gd0.133Ti0.9Ge0.1O3:0.01Eu、Ca0.8Y0.133Ti0.9Ge0.1O3:0.01Eu、 Ca0.8La0.132Gd0.001Ti0.9Ge0.1O3:0.01Eu、Ca0.8La0.132Y0.001Ti0.9Ge0.1O3:0.01Eu、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Pr、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Sm、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Dy 、Mg0.8Gd0.133Ti0.9Ge0.1O3:0.01Eu、Mg0.8Y0.133Ti0.9Ge0.1O3:0.01Eu、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Dy，Eu 、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Dy，Sm 、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Pr，Bi、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Eu，Sm。
the preparation method of the fluorescent materials of the titanium germanates for the white light LED comprises the following steps:
a. preparing materials according to any one of the chemical expression formulas of the composition of the fluorescent material according to the matrix material and the used activating agent;
b. and c, finely grinding the raw materials prepared in the step a for 30 minutes, then loading the ground raw materials into a corundum crucible with a cover, placing the corundum crucible into a calcining furnace for calcining, cooling and crushing the mixture after the calcining temperature is 1300 ℃ and the firing time is 2, and grinding the mixture again to obtain the fluorescent material.
The excitation band of the novel efficient fluorescent material provided by the invention covers the range of 200-500 nm, for example, a sample is doped with Eu3+The excitation position of the fluorescent material is 300-400 nm, and the fluorescent material for the white light LED, which has a narrow emission band and can be effectively excited by ultraviolet light, near ultraviolet light and blue light, is used. Meanwhile, the excitation position of the fluorescent material is matched with the light-emitting position of the LED chip, so that the fluorescent material is a good fluorescent material for white light LEDs. In the aspect of agriculture, because the chlorophyll has two absorption areas with the strongest light waves, one absorption area is a blue light part and a purple light part with the wavelength of 400-500 nm, and the other absorption area is a red light part with the wavelength of 600-700 nm, the red light is beneficial to the synthesis of plant carbohydrate, and can also accelerate the growth of plantsAnd (5) growing and developing. Therefore, the efficient plant supplementary lighting generally adopts 400-500 nm blue light and 600-700 nm red light. And the sample is doped with Dy3+The emission positions are located at 483nm and 574nm, and blue light is emitted; sm doped alloy3+The emission sites were located at 565nm and 601nm for red light. Meets the above conditions, so the fluorescent material is also a novel high-efficiency fluorescent material applied to agricultural illumination.
The experimental scheme of the invention is briefly described as follows:
1. preparation of the Material
The raw materials of the fluorescent material are all inorganic salts of various elements, including but not limited to oxides, carbonates and nitrates, and are all obtained by a high-temperature solid-phase method. The specific dosage is calculated by the chemical formula of the fluorescent material, and according to the difference of the fluorescent powder basic material and the activating agent, the invention selects and calcines for 10 minutes at the melting point of each raw material, the firing temperature is 1300 ℃, the preparation time is 2 hours, the process comprises weighing, grinding and calcining, and then the formed crystal is cooled, crushed and carefully ground to obtain the fluorescent material.
2. Evaluation of Performance
Optical absorption emission Properties of the phosphor samples obtained in the present invention were measured for ultraviolet-visible absorption emission spectra in an F-7000 FL Spectrophotometer of Hitachi, Japan. In summary, the invention relates to a fluorescent material which can convert ultraviolet light, near ultraviolet light and blue light into visible light with higher brightness and can be used for white light LED. The fluorescent material can be used for white light LEDs and related display and lighting devices. The invention has the advantages of simple and easily obtained raw materials and simple preparation method, and is an ideal candidate material of the white light LED fluorescent powder.
The titanate luminescent material is a novel functional material, has stable physical and chemical properties, has lower phonon energy and high vibration frequency, and is suitable to be used as a luminescent matrix material. Meanwhile, the germanate has excellent physical and chemical stability, low synthesis temperature and larger band gap width; therefore, titanium germanate is selected as the matrix light reflecting material. The excitation band of the sample covers the range of 200-500 nm, wherein the Eu-doped excitation position of the sample is located in the range of 300-400 nm, the Eu-doped excitation position of the sample is matched with the light-emitting excitation position of the LED chip, the emission band is narrow, namely the half-height width is narrow, the Eu-doped excitation position can emit visible light after being excited by ultraviolet light, near ultraviolet light and blue light, and the Eu-doped excitation band can be combined with other appropriate fluorescent materials of various colors to manufacture a white light-emitting device and related display and lighting. The invention has the advantages of cheap raw materials, simple process, easy preparation, stable chemical property and good luminescence property, and is an ideal candidate fluorescent material for white light LEDs.
Drawings
FIG. 1 shows Ca in example 1 of the present invention0.8La0.133Ti0.9Ge0.1O3 Excitation spectrum (lambda) of 0.01Eu materialem= 614 nm) and emission spectrum (λ)ex = 396nm）。
FIG. 2 shows Ca in example 2 of the present invention0.8La0.133Ti0.9Ge0.1O3Excitation spectrum (lambda) of 0.01Sm materialem = 565 nm；λem= 601 nm) and emission spectrum (λ)ex = 408 nm）。
FIG. 3 shows Ca in example 3 of the present invention0.8La0.133Ti0.9Ge0.1O3Excitation spectrum (lambda) of 0.01Dy materialem = 482nm；λem= 574 nm) and emission spectrum (λex = 388 nm）。
FIG. 4 shows Ca in example 4 of the present invention0.8La0.133Ti0.9Ge0.1O3Excitation spectrum (lambda) of 0.01Pr materialem= 614 nm) and emission spectrum (λ)ex = 330nm）。
FIG. 5 shows Ca in example 5 of the present invention0.8La0.133Ti0.9Ge0.1O3 0.01Pr, excitation spectrum (lambda) of Bi materialem= 614 nm) and emission spectrum (λ)ex = 360nm）。
FIG. 6 shows Ca in example 6 of the present invention0.8Gd0.133Ti0.9Ge0.1O3 Excitation spectrum (lambda) of 0.01Eu materialem= 616 nm) and emission spectrum (λex = 396nm）。
FIG. 7 shows Mg in example 7 of the present invention0.8La0.133Ti0.9Ge0.1O3 Excitation spectrum (lambda) of 0.01Eu materialem= 614 nm) and emission spectrum (λ)ex = 324nm；λex = 394nm）。
Detailed Description
The embodiments of the present invention will be described below, but the present invention is by no means limited to the embodiments.
Example 1
Mixing raw material Ca2CO3、La2O3、TiO2、GeO2、Eu2O3According to Ca0.8La0.133Ti0.9Ge0.1O30.01Eu in a stoichiometric ratio, and the mixture is weighed and uniformly mixed in a mortar for 30 minutes, and the obtained components are loaded into a corundum crucible with a cover and then placed into a calcining furnace for calcination at 825 ℃ (CaCO) respectively3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and finely grinding to obtain Ca0.8La0.133Ti0.9Ge0.1O30.01Eu fluorescent material. The test results are shown in FIG. 1.
Example 2
Mixing raw material Ca2CO3、La2O3、TiO2、GeO2、Sm2O3According to Ca0.8La0.133Ti0.9ge0.1o3: weighing 0.01Sm stoichiometric ratio, mixing in mortar for 30 min, loading into corundum crucible with cover, calcining in calciner at 825 deg.C (CaCO)3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and finely grinding to obtain Ca0.8La0.133Ti0.9Ge0.1O30.01Sm fluorescent material. The test results are shown in FIG. 2.
Example 3
Mixing raw material Ca2CO3、La2O3、TiO2、GeO2、Dy2O3According to Ca0.8La0.133Ti0.9Ge0.1O30.01Dy in a stoichiometric ratio, uniformly mixed in a mortar for 30 minutes, and the obtained mixture was loaded into a corundum crucible with a lid and then calcined in a calciner at 825 ℃ (CaCO) respectively3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and finely grinding to obtain Ca0.8La0.133Ti0.9Ge0.1O30.01Dy fluorescent material. The test results are shown in FIG. 3.
Example 4
Mixing raw material Ca2CO3、La2O3、TiO2、GeO2、Pr2O3According to Ca0.8La0.133Ti0.9ge0.1o3: pr is weighed according to the stoichiometric ratio, evenly mixed in a mortar for 30 minutes, and the obtained split body is put into a corundum crucible with a cover and then put into a calcining furnace for calcining at 825 ℃ (CaCO)3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and finely grinding to obtain Ca0.8La0.133Ti0.9Ge0.1O30.01Pr fluorescent material. The test results are shown in FIG. 4.
Example 5
Mixing raw material Ca2CO3、La2O3、TiO2、GeO2、Pr2O3、Bi2O3According to Ca0.8La0.133Ti0.9Ge0.1O3: pr and Bi are weighed according to the stoichiometric ratio, evenly mixed in a mortar for 30 minutes, and the obtained components are loaded into a corundum crucible with a cover and then are placed into a calcining furnace for calcining at 825 ℃ (CaCO)3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and finely grinding to obtain Ca0.8La0.133Ti0.9Ge0.1O30.01Pr and Bi fluorescent materials. The test results are shown in FIG. 5.
Example 6
Mixing raw material Ca2CO3、Gd2O3、TiO2、GeO2、Eu2O3According to Ca0.8Gd0.133Ti0.9Ge0.1O3: eu is weighed according to the stoichiometric ratio, the Eu is evenly mixed in a mortar for 30 minutes, the obtained split body is put into a corundum crucible with a cover and then put into a calcining furnace to be calcined at 825 ℃ (CaCO)3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and finely grinding to obtain Ca0.8Gd0.133Ti0.9Ge0.1O30.01Eu fluorescent material. The test results are shown in FIG. 6.
Example 7
Mixing raw material Mg2CO3、La2O3、TiO2、GeO2、Eu2O3According to Mg0.8La0.133Ti0.9Ge0.1O3: eu is weighed according to the stoichiometric ratio, the Eu is evenly mixed in a mortar for 30 minutes, the obtained split body is put into a corundum crucible with a cover and then put into a calcining furnace to be calcined at 700 ℃ (MgCO)3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and fine grinding to obtain Mg0.8La0.133Ti0.9Ge0.1O30.01Eu fluorescent material. The test results are shown in FIG. 7.
Example 8
Raw material CaCO3、Y2O3、TiO2、GeO2、Eu2O3According to Ca0.8Y0.133Ti0.9Ge0.1O3: eu is weighed according to the stoichiometric ratio, the Eu is evenly mixed in a mortar for 30 minutes, the obtained split body is put into a corundum crucible with a cover and then put into a calcining furnace to be calcined at 825 ℃ (CaCO respectively3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling, and fine grinding to obtain Ca0.8Y0.133Ti0.9Ge0.1O30.01Eu fluorescent material. It can effectively emit red light under the excitation of ultraviolet.
Example 9
The raw material MgCO is mixed3、Gd2O3、TiO2、GeO2、Eu2O3According to Mg0.8Gd0.133Ti0.9Ge0.1O3: eu is weighed according to the stoichiometric ratio, the Eu is evenly mixed in a mortar for 30 minutes, the obtained split body is put into a corundum crucible with a cover and then is put into a calcining furnace to be calcined at 700 ℃ (MgCO) respectively3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and fine grinding to obtain Mg0.8Gd0.133Ti0.9Ge0.1O30.01Eu fluorescent material. It can effectively emit red light under the excitation of ultraviolet.
Example 10
The raw material MgCO is mixed3、Y2O3、TiO2、GeO2、Eu2O3According to Mg0.8Y0.133Ti0.9Ge0.1O3: eu is weighed according to the stoichiometric ratio, the Eu is evenly mixed in a mortar for 30 minutes, the obtained split body is put into a corundum crucible with a cover and then is put into a calcining furnace to be calcined at 700 ℃ (MgCO) respectively3Melting point), 1115 ℃ (GeO2Melting point) for 10 minutes and at 1300 ℃ for 2 hours. Cooling and fine grinding to obtain Mg0.8Y0.133Ti0.9Ge0.1O30.01Eu fluorescent material. It can effectively emit red light under the excitation of ultraviolet.

Claims (2)

1. A fluorescent material of multiple titanium germanates for white light LED has chemical expression of Ca0.8La0.133Ti0.9Ge0.1O3:0.01Eu、 Ba0.8La0.133Ti0.9Ge0.1O3:0.01Eu、Mg0.8La0.133Ti0.9Ge0.1O3:0.01Eu、 Ca0.79Mg0.01La0.133Ti0.9Ge0.1O3:0.01Eu 、Ca0.7Mg0.1La0.133Ti0.9Ge0.1O3:0.01Eu、Ca0.8Gd0.133Ti0.9Ge0.1O3:0.01Eu、Ca0.8Y0.133Ti0.9Ge0.1O3:0.01Eu、 Ca0.8La0.132Gd0.001Ti0.9Ge0.1O3:0.01Eu、Ca0.8La0.132Y0.001Ti0.9Ge0.1O3:0.01Eu、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Pr、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Sm、Ca0.8La0.133Ti0.9Ge0.1O3:0.01Dy 、Mg0.8Gd0.133Ti0.9Ge0.1O3:0.01Eu、Mg0.8Y0.133Ti0.9Ge0.1O3:0.01Eu、
Ca0.8La0.133Ti0.9Ge0.1O3:0.01（Dy，Eu） 、Ca0.8La0.133Ti0.9Ge0.1O3:0.01（Dy，Sm） 、Ca0.8La0.133Ti0.9Ge0.1O3:0.01（Pr，Bi）、Ca0.8La0.133Ti0.9Ge0.1O30.01 (Eu, Sm).
2. A method of preparing the multiple titanium germanate phosphors of claim 1 for a white LED, comprising the steps of:
a. preparing materials according to the chemical expression of the fluorescent material;
b. and c, finely grinding the raw materials prepared in the step a for 30 minutes, then loading the ground raw materials into a corundum crucible with a cover, placing the corundum crucible into a calcining furnace for calcining, cooling and crushing the mixture after calcining for 2 hours at 1300 ℃, and grinding the mixture again to obtain the fluorescent material.
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