CN112708422A - High-temperature red fluorescent material and preparation method thereof - Google Patents
High-temperature red fluorescent material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 33
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000006104 solid solution Substances 0.000 claims abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 4
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 4
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 16
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 16
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 2
- 230000005284 excitation Effects 0.000 abstract description 13
- 238000004020 luminiscence type Methods 0.000 abstract description 3
- 238000010791 quenching Methods 0.000 abstract description 3
- 230000000171 quenching effect Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000000295 emission spectrum Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 3
- 238000009877 rendering Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910003443 lutetium oxide Inorganic materials 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
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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
- C09K11/7776—Vanadates; Chromates; Molybdates; Tungstates
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- H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
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- H10H20/85—Packages
- H10H20/851—Wavelength conversion means
- H10H20/8511—Wavelength conversion means characterised by their material, e.g. binder
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Abstract
本发明公开了一种高温红色荧光材料及其制备方法，属于稀土发光材料技术领域。本发明所述红色荧光材料是Cr3+激活的荧光粉为固溶体，其化学通式为La3‑yMyGa5GeO14:xA，其中A为Cr3+，M为Gd3+，Y3+，Lu3+中的至少一种，0＜x≤0.2，0≤y≤1.5；所述红色荧光材料的制备方法是：按化学通式中的配比称取各种材料并研磨混合均匀，在1100‑1450℃煅烧4‑8h，冷却后研碎后得到。所述荧光粉发光性能优异，学稳定性好，激发效率高，制备过程简单，易于工业化生产，随着温度的升高无热猝灭现象，并随着温度的升高至200摄氏度，红色发光强度相比于常温可增加30％‑60％，热稳定性好。可与蓝光LED匹配，是一种新型的白光LED用高温红色荧光粉。可适用于高温环境下或者大功率LED器件，具有巨大的应用前景。
The invention discloses a high-temperature red fluorescent material and a preparation method thereof, belonging to the technical field of rare earth luminescent materials. The red fluorescent material of the present invention is a Cr 3+ activated fluorescent powder as a solid solution, and its general chemical formula is La 3-y My Ga 5 GeO 14 :xA, wherein A is Cr 3+ , M is Gd 3+ , and Y 3+ , at least one of Lu 3+ , 0<x≤0.2, 0≤y≤1.5; the preparation method of the red fluorescent material is: weighing various materials according to the proportion in the general chemical formula, grinding and mixing Homogeneous, calcined at 1100-1450°C for 4-8h, cooled and ground. The fluorescent powder has excellent luminescence performance, good chemical stability, high excitation efficiency, simple preparation process, easy industrial production, no thermal quenching phenomenon as the temperature rises, and red luminescence as the temperature rises to 200 degrees Celsius Compared with normal temperature, the strength can be increased by 30%-60%, and the thermal stability is good. Compatible with blue LEDs, it is a new type of high temperature red phosphor for white LEDs. It can be applied to high temperature environment or high-power LED devices, and has huge application prospects.
Description
Technical Field
The invention relates to a high-temperature red fluorescent material and a preparation method thereof, belonging to the technical field of rare earth luminescent materials.
Background
The advent of high efficiency blue light chips (LEDs) has made white LEDs an important way to obtain white light and has evolved into fourth generation illumination sources. In 1996, Japan first develops yellow light garnet (YAG) fluorescent powder, cooperates with blue light LED to obtain high-efficiency white light source. The blue light excites the YAG fluorescent powder, part of the blue light is absorbed by the fluorescent powder to excite yellow light, and the rest part of the blue light is mixed with the yellow light to form white light. The white light realization mode has lower cost and is a mode widely adopted at present, however, the fluorescent powder lacks red light components, so the color rendering index is poor, the color temperature is higher, the adjustment is difficult, and warm white light cannot be obtained. Another way of generating white light with the assistance of phosphor is to use a near ultraviolet LED to excite the mixture of red, green and blue phosphors to realize white light, where the ultraviolet LED has stronger excitation intensity and higher conversion efficiency, however, the red phosphor has lower luminous efficiency than the blue-green phosphor, such as Y2O 2S: eu (Eu)3+The phosphor has low energy conversion efficiency and poor thermal stability. So far, blue chip LEDs are relatively widely used, but the emitted white light lacks long-wavelength light components, and the color of the device changes with the thickness of the phosphor coating, the color repeatability of each LED is poor, the color rendering index is low, and the luminous intensity gradually decreases with the temperature, resulting in performance degradation.
The current applications are mainly sulfide phosphor (Sr, Ca) S: eu (Eu)2+. However, the instability of sulfide in the using process and environmental pollution lead people to continuously develop red phosphor powder capable of replacing the existing sulfide. Fluorescent materials based on strong absorption of 420-470nm red light are very few, and when the temperature of a blue chip risesWhen the vibrational energy of the atoms is higher than a certain value, electrons exchange energy with lattice atoms (or ions) when they transition from an excited state to a ground state, and nonradiative transition occurs. After the temperature rises to a certain degree, the emission intensity decreases. At present, high-stability red fluorescent powder which has excellent performance and can avoid the thermal quenching problem caused by the long-time working and heating of a blue light chip is not available in the market, and the three-primary-color fluorescent powder for the white light illumination LED based on a near ultraviolet or blue light diode, in particular to high-temperature-resistant red fluorescent powder which can be excited by blue light.
Disclosure of Invention
The invention aims to provide a high-temperature red fluorescent material and a preparation method thereof, which solve the problems that in the prior art, the red light component of an emission spectrum is less, the color rendering index is lower, and single white light cannot be synthesized, and the problems of thermal quenching caused by overheating of the red fluorescent powder under the condition of long-time work at the present stage, and the like, and the luminous intensity of the material at high temperature (about 200 ℃) can be increased by 30-60% compared with the luminous intensity at normal temperature. The high-temperature red fluorescent material capable of being excited by the blue light chip is realized. The method can be suitable for high-temperature environments or high-power LED devices, and has a huge application prospect.
A high-temperature red fluorescent material and a preparation method thereof belong to the technical field of rare earth luminescent materials. The red fluorescent material is Cr3+The activated fluorescent powder is solid solution and has a chemical general formula of La3-yMyGa5GeO14: x A, wherein A is Cr3+M is Gd3+，Y3+，Lu3+X is more than 0 and less than or equal to 0.2, and y is more than or equal to 0 and less than or equal to 1.5;
the preparation method of the red fluorescent powder comprises the following steps:
(1) the raw material La is added2O3、Ga2O3、GeO2、Cr2O3、M2O3Mixing the ingredients according to the general formula of the finally prepared fluorescent powder, adding alcohol, grinding and uniformly mixing;
(2) grinding and uniformly mixing the raw materials weighed in the step (1);
(3) then the mixed raw materials are put into a crucible and are kept at the temperature of 1100-1450 ℃ in the atmospheric environment for 4-8 hours; cooling to room temperature, sintering into block solid solution, grinding into powder to obtain La3-yMyGa5GeO14: x A Single phase powder.
The invention has the beneficial effects that:
the red fluorescent powder has good chemical thermal stability and high excitation efficiency, can obtain red luminescence about 700nm under the excitation of blue light (466nm), can be matched with a blue LED, can improve the luminous intensity by 30-60 percent compared with the luminous intensity at normal temperature within the temperature range of 50-200 ℃, and is novel high-temperature red fluorescent powder. The method can be suitable for high-temperature environments or high-power LED devices, and has a huge application prospect.
Drawings
FIG. 1 shows excitation spectra of the phosphor of embodiment 1 of the present invention;
FIG. 2 shows an emission spectrum of the phosphor of embodiment 1 of the present invention;
FIG. 3 is a graph showing the change in emission intensity with an increase in temperature of the phosphor according to embodiment 1 of the present invention;
Detailed Description
The invention will be described in more detail with reference to the following figures and embodiments, but the scope of the invention is not limited thereto.
Detailed description of the preferred embodiment 1
1. The general chemical formula of the red fluorescent material prepared in this example is La2GdGa4.99GeO14：0.01Cr3+. The average particle size of the phosphor is 15-20 μm, and the main phase structure of the phosphor belongs to a trigonal system. The preparation method comprises the following steps:
(1) according to La2O3(99.99％)∶Ga2O3(99.99％)∶GeO2(99.99％)∶Cr2O3(99.99％)∶ Gd2O3(99.99%) in a molar ratio of 2: 4.99: 1: 0.01: 1, and La was accurately weighed2O3(99.99％)，Ga2O3(99.99％)， GeO2(99.99％)，Cr2O3(99.99％)，Gd2O3(99.99%) in an agate mortar, adding 120% alcohol by volume fraction, grinding for 0.7h, and mixing uniformly.
(2) Placing the mixture obtained in the step (1) in a corundum crucible, sintering for 6 hours at 1250 ℃ in air atmosphere, cooling to room temperature, and grinding to obtain the high-temperature red fluorescent powder La2GdGa4.99GeO14：0.01Cr3+。
The excitation spectrum of the obtained fluorescent powder is shown in figure 1, and it can be seen from figure 1 that the excitation peak has stronger excitation at 466nm, the excitation wavelength of the fluorescent powder is just positioned at the blue light position and matched with the excitation wavelength of the LED blue light chip, and the fluorescent powder is suitable for the excitation of a blue light LED. The excitation spectrum of the obtained phosphor is shown in FIG. 2, and the emission spectrum of the phosphor has a main emission peak at 718nm and emits bright red light. The thermal stability of the obtained phosphor is shown in FIG. 3, and its thermal stability is that the luminous intensity at 150 deg.C is increased with the temperature, and compared with the luminous intensity at room temperature, the luminous intensity can be increased by 40%
Detailed description of the preferred embodiment 2
The general chemical formula of the red fluorescent material prepared in this example is La2YGa4.99GeO14∶0.01Cr3+. The average particle size of the phosphor is 15-20 μm, and the main phase structure of the phosphor belongs to a trigonal system. The preparation method comprises the following steps:
(1) according to La2O3(99.99％)∶Ga2O3(99.99％)∶GeO2(99.99％)∶Cr2O3(99.99％)∶ Y2O3(99.99%) in a molar ratio of 2: 4.99: 1: 0.01: 1, and La was accurately weighed2O3(99.99％)，Ga2O3(99.99％)， GeO2(99.99％)，Cr2O3(99.99％)，Y2O3(99.99%) in an agate mortar, adding 140% volume fraction alcohol, grinding for 0.5h, and mixing well.
(2) Placing the mixture obtained in the step (1) in a corundum crucible, sintering for 5 hours at 1230 ℃ in air atmosphere, cooling to room temperature, and grinding to obtain the high-temperature red fluorescent powder La2YGa4.99GeO14：0.01Cr3+。
The obtained fluorescent powder is matched with the excitation wavelength of the LED blue light chip and is suitable for excitation of the blue light LED. The emission spectrum of the obtained phosphor has a main emission peak at 718nm and emits bright red light. The luminous intensity of the obtained fluorescent powder can be improved by 30-50% compared with the luminous intensity at normal temperature within the range of about 170 ℃.
Detailed description of the preferred embodiment 3
The general chemical formula of the red fluorescent material prepared in this example is La2 LuGa4.99GeO14：0.01Cr3+. The average particle size of the phosphor is 15-20 μm, and the main phase structure of the phosphor belongs to a trigonal system. The preparation method comprises the following steps:
(1) according to La2O3(99.99％)∶Ga2O3(99.99％)∶GeO2(99.99％)∶Cr2O3(99.99％)∶ Lu2O3(99.99%) in a molar ratio of 2: 4.99: 1: 0.01: 1, and La was accurately weighed2O3(99.99％)，Ga2O3(99.99％)， GeO2(99.99％)，Cr2O3(99.99％)，Lu2O3(99.99%) in an agate mortar, adding 140% volume fraction alcohol, grinding for 0.5h, and mixing well.
(2) Placing the mixture obtained in the step (1) in a corundum crucible, sintering for 7 hours at 1300 ℃ in air atmosphere, cooling to room temperature, and grinding to obtain the high-temperature red fluorescent powder La2LuGa4.99GeO14：0.01Cr3+。
The obtained fluorescent powder is matched with the excitation wavelength of the LED blue light chip and is suitable for excitation of the blue light LED. The emission spectrum of the obtained phosphor has a main emission peak at 718nm and emits bright red light. The luminous intensity of the obtained fluorescent powder can be improved by about 60 percent compared with the luminous intensity at normal temperature within the range of about 200 ℃ in thermal stability.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (6)
1. A high-temperature red fluorescent material and a preparation method thereof belong to the technical field of rare earth luminescent materials. The red fluorescent material is Cr3+The activated fluorescent powder is solid solution and has a chemical general formula of La3-yMyGa5GeO14: xA, wherein A is Cr3 +M is Gd3+，Y3+，Lu3+X is more than 0 and less than or equal to 0.2, and y is more than or equal to 0 and less than or equal to 1.5.
2. The high temperature red fluorescent material according to claim 1, wherein: the average particle size of the phosphor is 15-20 μm, and the main phase structure of the phosphor belongs to a trigonal system.
3. The method for preparing a high-temperature red fluorescent material according to claim 1, wherein the method comprises the following steps:
(1) the raw material La is added2O3、Ga2O3、GeO2、Cr2O3、M2O3Mixing the ingredients according to the general formula of the finally prepared fluorescent powder, adding alcohol, grinding and uniformly mixing;
(2) then the mixed raw materials are put into a crucible and are kept at the temperature of 1100-1450 ℃ in the atmospheric environment for 4-8 hours; cooling to room temperature, sintering into block solid solution, grinding into powder to obtain La3-yMyGa5GeO14: single-phase powder of xA.
4. The method for preparing a high-temperature red fluorescent material according to claim 3, wherein: the purity of the alcohol is more than 98 wt%, and the adding amount of the alcohol is 80-120% of the volume of the mixture.
5. The high temperature red fluorescent material according to claim 1, wherein: in the temperature range of 25-200 ℃, the red luminous intensity can be increased by 30-60% compared with the normal temperature along with the temperature rise to 200 ℃, and the thermal stability is good. Is suitable for high-temperature red high-brightness fluorescence emission.
6. The high temperature red fluorescent material according to claim 1, wherein: can be matched with a blue LED, and is a novel high-temperature red fluorescent powder material for a white LED.
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Cited By (3)
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|---|---|---|---|---|
| CN113690359A (en) * | 2021-08-24 | 2021-11-23 | 昆明理工大学 | High-stability near-infrared LED plant lamp light-emitting chip and preparation method thereof |
| CN114409252A (en) * | 2022-01-18 | 2022-04-29 | 中国计量大学 | Boron-free high-density gadolinium lutetium germanate glass and preparation method thereof |
| CN117025220A (en) * | 2023-08-10 | 2023-11-10 | 昆明理工大学 | Ultra-wideband shortwave near infrared fluorescent powder and preparation method thereof |
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2020
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113690359A (en) * | 2021-08-24 | 2021-11-23 | 昆明理工大学 | High-stability near-infrared LED plant lamp light-emitting chip and preparation method thereof |
| CN114409252A (en) * | 2022-01-18 | 2022-04-29 | 中国计量大学 | Boron-free high-density gadolinium lutetium germanate glass and preparation method thereof |
| CN114409252B (en) * | 2022-01-18 | 2022-12-20 | 中国计量大学 | A kind of boron-free high density gadolinium lutetium germanate glass and preparation method thereof |
| CN117025220A (en) * | 2023-08-10 | 2023-11-10 | 昆明理工大学 | Ultra-wideband shortwave near infrared fluorescent powder and preparation method thereof |
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