CN112251227A - Full-spectrum fluorescence conversion material with garnet structure and preparation method thereof - Google Patents
Full-spectrum fluorescence conversion material with garnet structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a full-spectrum fluorescence conversion material with a garnet structure and a preparation method thereof, wherein the chemical general formula of the fluorescence conversion material is BaaYbLucCedAleGafSigO12，0.85≤a≤1.15，0<b is less than or equal to 2.0, c is less than or equal to 0.2 and less than or equal to 2.0, d is less than or equal to 0.03 and less than or equal to 0.15, e is less than or equal to 0.5 and less than or equal to 2.5, f is less than or equal to 0.5 and less than or equal to 2.5, g is less than or equal to 1.2 and is greater than or equal to 0.8, a + b + c + d is 3, and e + f + g is; firstly, preparing Y respectively3‑dCedAl5O12And BaaLu3‑a‑dCedAl5‑f‑gGafSigO12The raw material powder is ball milled, dried, screened and calcined, and then calcined Y is added3‑ dCedAl5O12Powder and BaaLu3‑a‑dCedAl5‑f‑gGafSigO12The powder is represented by the chemical formula BaaYbLucCedAleGafSigO12Weighing the components in proportion, stirring in vacuum, drying, and calcining in a reducing atmosphere to obtain the target product. The full-spectrum fluorescence conversion material prepared by the invention has high light conversion efficiency, good chemical stability, wide excitation and emission spectrum range, simple preparation method and easy industrial production.
Description
Technical Field
The invention relates to the technical field of preparation of fluorescent conversion materials for LEDs, in particular to a full-spectrum fluorescent conversion material with a garnet structure and a preparation method thereof.
Background
Since the advent of blue LED chips, the realization of high-quality white light illumination output using low-cost LED chips has become a goal pursued by many researchers. In the world, white light LED devices that use fluorescent conversion materials to achieve high-quality white light illumination output have become the most widely used illumination lamps due to their advantages of low manufacturing cost, low energy consumption, long service life, environmental friendliness, and the like.
However, with the continuous pursuit of people for high-quality healthy life and the concern about the potential risk of blue light hazard, the white light LED lighting device needs to continuously realize breakthrough in the technical fields of color rendering index, blue light utilization rate and the like. However, for a single blue LED chip white light source, the color rendering index is much lower than that of a multi-chip three primary LED white light illumination source. The fundamental reason for this is the lack of red light component in the white light output spectrum of the excitation light source of a single blue LED chip.
Therefore, the color rendering index of the single blue LED chip lighting device is improved by domestic scholars in a mode of introducing a single red light component. Chinese patent (application No. 201910313255.6) proposes that the modification technology of silicate system red fluorescent powder realizes high-quality white light output; the Chinese patent (application No. 201610749624.2) prepares a full spectrum fluorescent powder to obtain high-efficiency white light which can meet the application requirements of different illumination fields. Although these fluorescent conversion materials achieve high-quality white light output, the white LED devices prepared in this way cannot effectively utilize blue light.
Therefore, the improvement and development of the existing fluorescent conversion material substrate to obtain the fluorescent powder matched with the blue light excitation LED chip have important significance for the development of the white light LED illuminating device of a single blue light chip.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the full-spectrum fluorescence conversion material with the garnet structure for the white light LED, which has high utilization rate of blue light, good chemical stability and temperature quenching characteristics and wide excitation and emission ranges.
The invention also aims to provide a preparation method of the full-spectrum fluorescence conversion material with the garnet structure. The preparation method is simple, easy to operate and low in equipment cost, and enterprises can realize large-scale production on the existing production line.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a full-spectrum fluorescence conversion material with garnet structure has a chemical formula of BaaYbLucCedAleGafSigO12，
Wherein a is Ba2+Mole percent of ion, b is Y3+Mole percent of ions, c is Lu3+Mole percent of ion, d is Ce3+Mole percent of ions, e is Al3+Mole percent of ions, f is Ga3+Mole percent of ions, g is Si4+The mole percentage of the ions respectively satisfies a is more than or equal to 0.85 and less than or equal to 1.15 and 0<b is not less than 2.0, c is not less than 0.2 and not more than 2.0, d is not less than 0.03 and not more than 0.15, e is not less than 0.5 and not more than 2.5, f is not less than 0.5 and not more than 2.5, g is not less than 0.8 and not more than 1.2, and a + b + c + d is 3, and e + f + g is 5.
The invention also provides a preparation method of the full-spectrum fluorescence conversion material with the garnet structure, which comprises the following specific steps:
(1) according to the chemical formula BaaYbLucCedAleGafSigO12Selecting SiO2、Al2O3、CeO2、Lu2O3、Ga2O3And BaCO3The powder is used as raw material powder;
(2) the raw material powder prepared in the step (1) is processed according to Y3-dCedAl5O12And BaaLu3-a-dCedAl5-f- gGafSigO12The stoichiometric ratio of the elements is measured, wherein a is more than or equal to 0.85 and less than or equal to 1.15, and 0<b is less than or equal to 2.0, c is less than or equal to 2.0 and is less than or equal to 0.2, d is less than or equal to 0.15 and is less than or equal to 0.5, e is less than or equal to 2.5, f is less than or equal to 0.5, g is less than or equal to 1.2 and is less than or equal to 0.8, a + b + c + d is 3, and e + f + g is 5, the weighed raw material powder is respectively placed into two ball milling tanks, then dispersing agents are respectively added, absolute ethyl alcohol is used as a solvent to prepare slurry, and ball milling is carried out;
(3) respectively drying the slurry subjected to ball milling in the step (2), and grinding and sieving the dried powder;
(4) respectively calcining the mixed powder sieved in the step (3) at the calcining temperature of 800-1100 ℃ for 2-4 h;
(5) calcining the calcined Y in the step (4)3-dCedAl5O12Powder and BaaLu3-a-dCedAl5-f-gGafSigO12The powder is represented by the chemical formula BaaYbLucCedAleGafSigO12Weighing the mixture ratio, then placing the mixture into absolute ethyl alcohol, and stirring the mixture for 15 to 40 minutes in vacuum at the stirring speed of 1800 plus 2500 r/min; drying after stirring;
(6) placing the powder dried in the step (5) in a crucible, and calcining in a reducing atmosphere at the calcining temperature of 1200-1500 ℃ for 3-8 h; naturally cooling to room temperature to obtain the full-spectrum fluorescence conversion material Ba with the garnet structureaYbLucCedAleGafSigO12。
Preferably, the ball milling manner in the step (2) is planetary ball milling, the ball milling rotation speed is 120-.
Preferably, the dispersant in the step (2) is one or more of herring oil, fish oil, castor oil, polyetherimide and NP-10, and the addition amount of the dispersant is 0.5-1.5 wt.% of the mass of the raw material powder in the ball milling tank.
Preferably, the sieve mesh number in the step (2) is 80-200 meshes, and the sieve is used for 3-5 times.
Preferably, the reducing atmosphere in the step (6) is a reducing atmosphere with a volume ratio of 95-85: 5-15 of a mixture of nitrogen and hydrogen or a volume ratio of 95-85: 5-15 of argon and hydrogen mixture.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method is simple, easy to operate, low in equipment cost and free of pollution.
(2) The full-spectrum fluorescence conversion material with the garnet structure, prepared by the invention, has high light conversion efficiency, good chemical stability and wide excitation and emission spectrum range, can realize the absorption of blue light with the maximum content in an LED device consisting of a blue light chip, and can effectively avoid the blue light harm of a white light LED illuminating device prepared by a single blue light chip.
Drawings
FIG. 1 shows BaYLu prepared in example 10.97Ce0.03Al2Ga2SiO12XRD pattern of (a).
FIG. 2 shows BaYLu prepared in example 10.97Ce0.03Al2Ga2SiO12Photoluminescence spectrum of the fluorescence conversion material.
FIG. 3 shows BaY obtained in example 20.85LuCe0.15Al2Ga2SiO12Photoluminescence spectrum of the fluorescence conversion material.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. In the following examples, all the raw materials used were high purity raw materials.
Example 1
Garnet structureFull spectrum BaYLu0.97Ce0.03Al2Ga2SiO12The preparation method of the fluorescence conversion material comprises the following specific steps:
(1) according to the chemical formula BaLu1.97Ce0.03Al2Ga2SiO12And Y2.97Ce0.03Al5O12The types of the raw materials are prepared, and the used raw materials are respectively as follows: SiO 22、Al2O3、CeO2、Lu2O3、Ga2O3、Y2O3And BaCO3And (3) powder.
(2) Mixing the raw material powder prepared in the step (1) according to BaLu1.97Ce0.03Al2Ga2SiO12And Y2.97Ce0.03Al5O12The raw material powder is weighed according to the stoichiometric ratio, the raw material powder is respectively placed in two alumina ball milling tanks, dispersant PEI (1 wt.% of the raw material powder) is added into each ball milling tank, absolute ethyl alcohol is used as a solvent to respectively prepare slurry, planetary ball milling is carried out, the ball milling rotating speed is 120r/min, and the ball milling time is 60 min.
(3) And (3) drying the two slurries prepared in the step (2) in a 55 ℃ oven, grinding the dried powder, sieving the powder with a 80-mesh sieve, and sieving the powder for 5 times.
(4) And (4) respectively calcining the mixed powder sieved in the step (3), wherein the calcining temperature is 1100 ℃, and the heat preservation time is 4 hours.
(5) Calcining the BaLu obtained in the step (4)1.97Ce0.03Al2Ga2SiO12Powder and Y2.97Ce0.03Al5O12The powder is according to the chemical formula BaYLu0.97Ce0.03Al2Ga2SiO12Weighing the components in proportion, then placing the mixture into absolute ethyl alcohol, and stirring the mixture for 25min in vacuum at the stirring speed of 2000 r/min; then dried at 55 ℃.
(6) Putting the powder dried in the step (5) into a crucible, and reducing in a reducing atmosphere (90% N)2+10％H2) Calcining at 1200 ℃ for 5 h; after the mixture is naturally cooled to the room temperature,the full spectrum fluorescence conversion material BaYLu with the garnet structure is obtained0.97Ce0.03Al2Ga2SiO12。
FIG. 1 shows BaYLu prepared in this example0.97Ce0.03Al2Ga2SiO12The XRD pattern of the material is shown to be a garnet phase without any impurity phase.
FIG. 2 shows BaYLu prepared in this example0.97Ce0.03Al2Ga2SiO12The results of the photoluminescence spectrogram of the fluorescence conversion material show that the fluorescence conversion material with the garnet structure can realize full-spectrum luminescence.
Example 2
Garnet structure full spectrum BaY0.85LuCe0.15Al2Ga2SiO12The preparation method of the fluorescence conversion material comprises the following specific steps:
(1) according to the chemical formula BaLu1.85Ce0.15Al2Ga2SiO12And Y2.85Ce0.15Al5O12The types of the raw materials are prepared, and the used raw materials are respectively as follows: SiO 22、Al2O3、CeO2、Y2O3、Ga2O3、Lu2O3And BaCO3And (3) powder.
(2) The raw material powder prepared in the step (1) is BaLu according to the stoichiometric ratio1.85Ce0.15Al2Ga2SiO12And Y2.85Ce0.15Al5O12Weighing, respectively placing the powder in two nylon ball milling tanks, adding a dispersant PEI (polyetherimide) with the powder mass of 1 wt.%, respectively preparing slurry by taking absolute ethyl alcohol as a solvent, and carrying out planetary ball milling with the ball milling rotation speed of 150r/min and the ball milling time of 30 min.
(3) And (3) drying the slurry prepared in the step (2) in a 55 ℃ oven, grinding the dried powder, sieving with a 100-mesh sieve, and sieving for 3 times.
(4) And (4) respectively calcining the mixed powder sieved in the step (3), wherein the calcining temperature is 900 ℃, and the heat preservation time is 4 hours.
(5) Calcining the BaLu obtained in the step (4)1.85Ce0.15Al2Ga2SiO12Powder and Y2.85Ce0.15Al5O12The powder is represented by the chemical formula BaY0.85LuCe0.15Al2Ga2SiO12Weighing the components in proportion, then placing the mixture into absolute ethyl alcohol, and stirring the mixture for 25min in vacuum at the stirring speed of 2000 r/min; then dried at 55 ℃.
(6) Placing the powder dried in the step (5) in a crucible and reducing in a reducing atmosphere (95% N)2+5％H2) Then, the calcining temperature is 1500 ℃, and the heat preservation time is 5 hours; naturally cooling to room temperature to obtain the full-spectrum fluorescence conversion material BaY with the garnet structure0.85LuCe0.15Al2Ga2SiO12。
FIG. 3 shows BaY obtained in this example0.85LuCe0.15Al2Ga2SiO12The results of the photoluminescence spectrogram of the fluorescence conversion material show that the fluorescence conversion material with the garnet structure can realize full-spectrum luminescence.
The phosphor and the 5W blue light COB chip were packaged together, and the light efficiency results are shown in table 1 by an integrating sphere test (I350 mA, U14V, model: SIS-3_1.0m _ R98, hangzhou remote optoelectronic information corporation, room temperature).
TABLE 1
| Type (B) | Light effect (lm/W) |
| Commercial Ce: YAG phosphor | 297 |
| Commercial Ce: LuAG fluorescent powder | 319 |
| BaYLu0.97Ce0.03Al2Ga2SiO12 | 343 |
| BaY0.85LuCe0.15Al2Ga2SiO12 | 338 |
The raw material powder is respectively prepared according to the stoichiometric ratio of the YAG-based fluorescent material to the LuAG-based fluorescent material, the YAG-based fluorescent conversion material and the LuAG-based fluorescent conversion material can be in phase at the same sintering temperature, and single doping of rare earth ion Ce can be realized3+The garnet crystal structure emits full spectrum light, and the light conversion efficiency is far higher than that of a single matrix material.
Claims (6)
1. The full-spectrum fluorescence conversion material with the garnet structure is characterized in that the chemical general formula is BaaYbLucCedAleGafSigO12，
Wherein a is Ba2+Mole percent of ion, b is Y3+Mole percent of ions, c is Lu3+Mole percent of ion, d is Ce3+Mole percent of ions, e is Al3+Mole percent of ions, f is Ga3+Mole percent of ions, g is Si4+The mole percentage of the ions respectively satisfies a is more than or equal to 0.85 and less than or equal to 1.15 and 0<b is not less than 2.0, c is not less than 0.2 and not more than 2.0, d is not less than 0.03 and not more than 0.15, e is not less than 0.5 and not more than 2.5, f is not less than 0.5 and not more than 2.5, g is not less than 0.8 and not more than 1.2, and a + b + c + d is 3, and e + f + g is 5.
2. The preparation method of the full-spectrum fluorescence conversion material with the garnet structure of claim 1, which is characterized by comprising the following steps:
(1) according to the chemical formula BaaYbLucCedAleGafSigO12Selecting SiO2、Al2O3、CeO2、Lu2O3、Ga2O3And BaCO3The powder is used as raw material powder;
(2) the raw material powder prepared in the step (1) is processed according to Y3-dCedAl5O12And BaaLu3-a-dCedAl5-f-gGafSigO12The stoichiometric ratio of the elements is measured, wherein a is more than or equal to 0.85 and less than or equal to 1.15, and 0<b is less than or equal to 2.0, c is less than or equal to 2.0 and is less than or equal to 0.2, d is less than or equal to 0.15 and is less than or equal to 0.5, e is less than or equal to 2.5, f is less than or equal to 0.5, g is less than or equal to 1.2 and is less than or equal to 0.8, a + b + c + d is 3, and e + f + g is 5, the weighed raw material powder is respectively placed into two ball milling tanks, then dispersing agents are respectively added, absolute ethyl alcohol is used as a solvent to prepare slurry, and ball milling is carried out;
(3) respectively drying the slurry subjected to ball milling in the step (2), and grinding and sieving the dried powder;
(4) respectively calcining the mixed powder sieved in the step (3) at the calcining temperature of 800-1100 ℃ for 2-4 h;
(5) calcining the calcined Y in the step (4)3-dCedAl5O12Powder and BaaLu3-a-dCedAl5-f-gGafSigO12The powder is represented by the chemical formula BaaYbLucCedAleGafSigO12Weighing the mixture ratio, then placing the mixture into absolute ethyl alcohol, and stirring the mixture for 15 to 40 minutes in vacuum at the stirring speed of 1800 plus 2500 r/min; drying after stirring;
(6) placing the powder dried in the step (5) in a crucible, and calcining in a reducing atmosphere at the calcining temperature of 1200-1500 ℃ for 3-8 h; naturally cooling to room temperature to obtain the full-spectrum fluorescence conversion material Ba with the garnet structureaYbLucCedAleGafSigO12。
3. The method for preparing a full-spectrum fluorescence conversion material with a garnet structure as claimed in claim 2, wherein the ball milling in step (2) is planetary ball milling, the ball milling speed is 120-150r/min, and the ball milling time is 30-60 min.
4. The method for preparing a full spectrum fluorescence conversion material with a garnet structure according to claim 2, wherein the dispersant in the step (2) is one or more of herring oil, fish oil, castor oil, polyetherimide and NP-10, and the amount of the dispersant is 0.5-1.5 wt.% of the mass of the raw powder in the ball mill pot.
5. The method for preparing a full-spectrum fluorescence conversion material of garnet structure according to claim 2, wherein the sieving mesh number in the step (2) is 80-200 meshes, and the sieving is performed 3-5 times.
6. The method of claim 2, wherein the reducing atmosphere in step (6) is a mixture of 95-85 vol.%: 5-15 of a mixture of nitrogen and hydrogen or a volume ratio of 95-85: 5-15 of argon and hydrogen mixture.
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| CN113150783A (en) * | 2021-04-27 | 2021-07-23 | 中国科学院长春应用化学研究所 | Color-adjustable afterglow luminescent material, preparation method thereof and lighting product |
| CN115305088A (en) * | 2022-08-22 | 2022-11-08 | 杭州爱视芙健康科技有限公司 | Garnet structure-derived fluorescent powder material and preparation method and application thereof |
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| CN115678557B (en) * | 2022-11-04 | 2023-10-03 | 昆明理工大学 | Thermal quenching-resistant up-conversion luminescence thermal enhancement material and preparation method and application thereof |
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| CN113150783A (en) * | 2021-04-27 | 2021-07-23 | 中国科学院长春应用化学研究所 | Color-adjustable afterglow luminescent material, preparation method thereof and lighting product |
| CN113150783B (en) * | 2021-04-27 | 2022-11-01 | 中国科学院长春应用化学研究所 | Color-adjustable afterglow luminescent material, preparation method thereof and lighting product |
| CN115305088A (en) * | 2022-08-22 | 2022-11-08 | 杭州爱视芙健康科技有限公司 | Garnet structure-derived fluorescent powder material and preparation method and application thereof |
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Application publication date: 20210122 |