CN112048299B - Ce3+Doped white light LED fluorescent material and preparation method thereof - Google Patents

Ce3+Doped white light LED fluorescent material and preparation method thereof Download PDF

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CN112048299B
CN112048299B CN202011057552.8A CN202011057552A CN112048299B CN 112048299 B CN112048299 B CN 112048299B CN 202011057552 A CN202011057552 A CN 202011057552A CN 112048299 B CN112048299 B CN 112048299B
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white light
light led
fluorescent material
led fluorescent
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CN112048299A (en
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田甜
刘伟
张彦
黄礼武
徐家跃
刘干
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Jiangsu Kechuang Internet Of Vehicles Industry Research Institute Co ltd
Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • 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
    • C09K11/778—Borates
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    • C01B35/00—Boron; Compounds thereof
    • C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
    • C01B35/10—Compounds containing boron and oxygen
    • C01B35/12—Borates
    • C01B35/128—Borates containing plural metal or metal and ammonium
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    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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    • C01—INORGANIC CHEMISTRY
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Abstract

The invention discloses Ce3+A doped white light LED fluorescent material and a preparation method thereof. The chemical general formula of the white light LED fluorescent material is Ca3(Tb7)1‑x(BO4)(SiO4)5O:xCe3+Wherein, 0<x is less than or equal to 0.15. The preparation method comprises the following steps: selecting compounds containing Ca, Tb, B, Si, Ce and O elements as raw materials, mixing, loading into an alumina crucible, and heating in a reducing atmosphere for presintering; then calcined in a reducing atmosphere to obtain Ce3+Doped white light LED phosphor. The invention uses borosilicate as a substrate, Ce3+An apatite structure compound as an activator. The fluorescent material emits white light when being excited by a blue light LED chip, has good color saturation and color rendering index, and is suitable for the field of warm white light LED device illumination and display.

Description

Ce3+Doped white light LED fluorescent material and preparation method thereof
Technical Field
The invention relates to Ce applied to the field of illumination and display of warm white light LED devices3+A doped white light LED luminescent material and a preparation method thereof belong to the technical field of solid luminescent materials.
Background
As a solid semiconductor light-emitting device, the white light LED has the advantages of high efficiency, energy conservation, environmental protection, small volume, light weight, less heat generation, long service life and the like compared with the traditional incandescent lamp and fluorescent lamp, and is widely applied to the fields of illumination, health care, national defense science and technology, plant illumination and the like. At present, the mainstream scheme of the commercialized white light LED is blue LED chip + yellow phosphor, but due to the lack of red light component in the spectrum, the white light LED has low luminous color rendering index, high color temperature and poor color rendering, and is difficult to meet the practical application requirement of high-performance devices. In order to solve the problems of the white light LED, researchers at home and abroad are dedicated to developing research and development of single-phase and single-doped white light LED fluorescent materials excited by a blue light LED chip, white light output is realized by exciting single-phase fluorescent powder by the blue light LED chip, the luminous color rendering index of the LED is improved, the color temperature of the LED is reduced, and therefore the warm white light LED with high color quality is obtained.
The apatite belongs to a hexagonal crystal system, the activator ions can occupy the cation positions of two nonequivalent lattice sites in the apatite structure, and the isomorphism substitution widely existing in the apatite is added, so that the apatite structure has a complex and changeable crystal field environment, and the energy level of the activator ions can be split differently in the complex and changeable crystal field environment of the apatite to generate different luminescence behaviors. The special crystal structure of apatite makes apatite an excellent matrix material doped with rare earth ions. Rare earth ion Ce3+Activated red phosphors are of increasing interest because they emit yellow-red spectra in the 590- ­ 700nm range under blue excitation.
Ca3Tb7(BO4)(SiO4)5O as a substrate, stronger green light emission exists at 530-570nm, and the green light emission is derived from rare earth ions Tb3+The blue light chip is combined, white light output is finally obtained through mixing three primary colors of light, and the fluorescent powder is a single-phase single-doped fluorescent material and has high luminous efficiency and color rendering index.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the prior white light LED has the technical problems of lower color rendering index and higher color temperature.
In order to solve the technical problems, the invention provides Ce3+The doped white light LED fluorescent material is characterized in that the chemical general formula is Ca3(Tb7)1-x(BO4)(SiO4)5O:xCe3+Wherein, 0<x is less than or equal to 0.15, and the luminescent center is rare earth ion Ce3+。
Preferably, the white light LED fluorescent material is of an apatite structure and can be effectively excited by the blue light LED chip to generate white light.
The invention also provides the Ce3+The preparation method of the doped white light LED fluorescent material is characterized by comprising the following steps of:
step 1): respectively selecting compounds containing Ca, Tb, B, Si, Ce and O elements as raw materials according to a proportion, and uniformly mixing and grinding the raw materials in an agate mortar to obtain a reaction precursor;
step 2): putting the reaction precursor into an alumina crucible, heating to 600-900 ℃ in a reducing atmosphere for presintering, and preserving heat for 3-8 h;
and step 3): taking out the pre-sintered sample obtained in the step 2), placing the sample in a mortar for grinding and uniformly mixing, then placing the sample in an alumina crucible again, and calcining the sample for 8 to 15 hours at the temperature of 1200-1350 ℃ in a reducing atmosphere to obtain Ce3+Doped white light LED phosphor.
Preferably, the compound containing Ca element in the step 1) is any one or a combination of more of calcium oxide, calcium carbonate, calcium sulfate and calcium hydroxide; the Tb element-containing compound is any one or the combination of terbium oxide and terbium hydroxide; the compound containing the B element is any one or the combination of two of boron oxide and boric acid; the compound containing Si element is any one or the combination of two of silicon oxide and silicic acid; the Ce element-containing compound is any one or combination of cerium oxide and cerium nitrate.
Preferably, the reducing atmosphere in step 2), step 3) is achieved by a reducing agent.
More preferably, the reducing agent is carbon monoxide, hydrogen or carbon powder.
Compared with the prior art, the invention has the beneficial effects that:
ce of the invention3+The doped white light fluorescent material can effectively absorb ultraviolet and blue light and is processed by a blue light chipExcitation obtains white light. The invention adopts cheap raw materials and rare earth active ions, and is prepared and obtained by adopting a high-temperature solid phase method under a reducing atmosphere. Ce of the invention3+The doped white light LED fluorescent material has the advantages of good luminous performance, good stability, easy preparation, no pollution, low cost, suitability for industrial production and the like. The raw materials and the final product do not contain harmful substances such as fluorine and the like, and no pollutant is discharged in the synthesis process.
Drawings
FIG. 1Ca3(Tb7)0.97(BO4)(SiO4)5O:0.03Ce3+XRD pattern of (a);
FIG. 2 shows Ca3(Tb7)0.97(BO4)(SiO4)5O:0.03Ce3+(ii) a diffuse reflectance spectrum of (a);
FIG. 3 shows Ca3(Tb7)0.97(BO4)(SiO4)5O:0.03Ce3+Fluorescence spectrum of (2).
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Starting materials used in examples 1 to 6: h3BO3(purity 99.9%, Shanghai chemical Co., Ltd., China pharmaceutical group), CaCO3(purity 99.9%, Shanghai chemical Co., Ltd., China pharmaceutical group), SiO2(purity 99.9%, Shanghai chemical reagent Co., China pharmaceutical group), CeO2(purity 99.9%, Shanghai chemical Co., Ltd., China pharmaceutical group), Tb4O7(purity 99.9%, Shanghai chemical Co., Ltd., China pharmaceutical group).
Example 1
This example synthesizes a Ce3+The chemical structural formula of the doped white light LED fluorescent material is Ca3(Tb7)0.99(BO4)(SiO4)5O:0.01Ce3+；
The preparation method comprises the following steps:
the method comprises the following steps: according to the formula Ca3(Tb7)0.99(BO4)(SiO4)5O:0.01Ce3+Weighing raw materials according to a stoichiometric ratio, and fully mixing and grinding the raw materials in a mortar to obtain mixed powder;
step two: pre-sintering, namely placing the mixed powder in the step one in an alumina crucible, then heating to 900 ℃ in a carbon powder reducing atmosphere, and preserving heat for 3 hours at 900 ℃; (ii) a
Step three: and (5) taking out the sample obtained in the step two, grinding, heating to 1300 ℃, preserving heat for 12 hours at 1300 ℃, and cooling along with the furnace to obtain the product.
Example 2
This example synthesizes a Ce3+The chemical structural formula of the doped white light LED fluorescent material is Ca3(Tb7)0.98(BO4)(SiO4)5O:0.02Ce3+；
The preparation method comprises the following steps:
the method comprises the following steps: according to the formula Ca3(Tb7)0.98(BO4)(SiO4)5O:0.02Ce3+Weighing raw materials according to a stoichiometric ratio, fully mixing in a mortar, and grinding to obtain mixed powder;
step two: placing the mixed powder in the first step into an alumina crucible, then sintering in a hydrogen atmosphere, heating to 850 ℃ at a temperature of 100 ℃/h, and keeping the temperature at 850 ℃ for 5 h;
step three: and (4) mixing and grinding the samples cooled in the step two, placing the samples in an alumina crucible, heating to 1250 ℃ in a hydrogen atmosphere, preserving heat for 24 hours at 1250 ℃, and cooling along with the furnace to obtain the product.
Example 3
This example synthesizes a Ce3+The chemical structural formula of the doped white light LED fluorescent material is Ca3(Tb7)0.97(BO4)(SiO4)5O:0.03Ce3+；
The preparation method comprises the following steps:
the method comprises the following steps: according to the formula Ca3(Tb7)0.97(BO4)(SiO4)5O:0.03Ce3+Weighing raw materials according to a stoichiometric ratio, fully grinding and mixing in a mortar to obtain mixed powder;
step two: placing the mixed powder in the step one in an alumina crucible, then heating to 900 ℃ in a carbon monoxide atmosphere, and preserving heat for 5 hours at 900 ℃;
step three: and pouring the sample cooled in the step two into a mortar for grinding and mixing, placing the powder into an alumina crucible, then heating to 1350 ℃ in a carbon monoxide atmosphere, preserving the heat for 10 hours at 1350 ℃, and cooling along with the furnace to obtain the product.
For the obtained product Ca3(Tb7)0.97(BO4)(SiO4)5O:0.03Ce3+Phase analysis was performed by x-ray powder diffraction and compared to a standard card of other apatite phases, the powder diffraction pattern was free of peaks and other phases, and the resulting compound was pure phase, as shown in fig. 1. Fig. 2 is a diffuse reflection diagram of the sample in the uv-visible region, from which it can be seen that the sample has strong absorption in the uv and blue regions, which can match commercial uv and blue LED chips. FIG. 3 is a fluorescence spectrum of a sample excited at 450nm, wherein the fluorescence spectrum has fluorescence peaks at 488nm, 543nm, 585nm and 622nm when the sample is excited at 450nm, and the fluorescence peaks correspond to Tb respectively3+And Ce3 +Luminescence of the ions.
Example 4
This example synthesizes a Ce3+The chemical structural formula of the doped white light LED fluorescent material is Ca3(Tb7)0.96(BO4)(SiO4)5O:0.04Ce3+；
The preparation method comprises the following steps:
the method comprises the following steps: according to the formula Ca3(Tb7)0.96(BO4)(SiO4)5O:0.04Ce3+Weighing raw materials according to a stoichiometric ratio, fully grinding and mixing in a mortar to obtain mixed powder;
step two: placing the mixed powder in the step one in an alumina crucible, then heating to 900 ℃ in a carbon powder environment, and preserving heat for 8 hours at 900 ℃;
step three: and pouring the sample cooled in the step two into a mortar for grinding and mixing, placing the mixed powder into an alumina crucible, heating to 1350 ℃ in a carbon powder atmosphere, preserving heat for 10 hours at 1350 ℃, and cooling along with the furnace to obtain the product.
Example 5
This example synthesizes a Ce3+The chemical structural formula of the doped white light LED fluorescent material is Ca3(Tb7)0.95(BO4)(SiO4)5O:0.05Ce3+；
The preparation method comprises the following steps:
the method comprises the following steps: according to the formula Ca3(Tb7)0.95(BO4)(SiO4)5O:0.05Ce3+Weighing raw materials according to a stoichiometric ratio, fully grinding and mixing in a mortar to obtain mixed powder;
step two: placing the mixed powder in the step one in an alumina crucible, then heating to 900 ℃ in a carbon powder atmosphere, and preserving heat for 8 hours at 900 ℃;
step three: and pouring the sample cooled in the step two into a mortar for grinding and mixing, placing the mixed powder into an alumina crucible, then heating to 1350 ℃ in a carbon powder atmosphere, preserving the heat for 15h at 1350 ℃, and cooling along with the furnace to obtain the product.
Example 6
This example synthesizes a Ce3+The chemical structural formula of the doped novel white light LED fluorescent material is Ca3(Tb7)0.94(BO4)(SiO4)5O:0.06Ce3+；
The preparation method comprises the following steps:
the method comprises the following steps: is represented by the chemical formula Ca3(Tb7)0.94(BO4)(SiO4)5O:0.06Ce3+Weighing raw materials according to a stoichiometric ratio, fully grinding and mixing in a mortar to obtain mixed powder;
step two: placing the mixed powder in the first step into an alumina crucible, then heating to 900 ℃ in a hydrogen atmosphere, and preserving heat for 8 hours at 900 ℃;
step three: and (4) pouring the sample cooled in the step two into a mortar for grinding and mixing, heating to 1250 ℃ in the atmosphere of carbon monoxide, preserving heat for 36 hours at 1250 ℃, and cooling along with the furnace to obtain the product.

Claims (6)

1. Ce3+The doped white light LED fluorescent material is characterized in that the chemical general formula is Ca3(Tb7)1-x(BO4)(SiO4)5O:xCe3+Wherein, 0<x is less than or equal to 0.15, and the luminescent center is rare earth ion Ce3+。
2. Ce of claim 13+The doped white light LED fluorescent material is characterized in that the white light LED fluorescent material is of an apatite structure and can be effectively excited by a blue light LED chip to generate white light.
3. Ce as claimed in claim 1 or 23+The preparation method of the doped white light LED fluorescent material is characterized by comprising the following steps of:
step 1): respectively selecting compounds containing Ca, Tb, B, Si, Ce and O elements as raw materials according to a proportion, and uniformly mixing and grinding the raw materials in an agate mortar to obtain a reaction precursor;
step 2): putting the reaction precursor into an alumina crucible, heating to 600-900 ℃ in a reducing atmosphere for presintering, and preserving heat for 3-8 h;
step 3): taking out the pre-sintered sample obtained in the step 2), placing the sample in a mortar for grinding and uniformly mixing, then placing the sample in an alumina crucible again, and calcining the sample for 8 to 15 hours at the temperature of 1200-1350 ℃ in a reducing atmosphere to obtain Ce3+Doped white light LED phosphor.
4. The Ce of claim 33+The preparation method of the doped white light LED fluorescent material is characterized in that the Ca element-containing compound in the step 1) is calcium oxide, calcium carbonate, calcium sulfate and oxyhydrogenAny one or combination of more of calcium compounds; the Tb element-containing compound is any one or combination of terbium oxide and terbium hydroxide; the compound containing the B element is any one or the combination of two of boron oxide and boric acid; the compound containing Si element is any one or the combination of two of silicon oxide and silicic acid; the compound containing Ce element is any one or the combination of two of cerium oxide and cerium nitrate.
5. The Ce of claim 33+The preparation method of the doped white light LED fluorescent material is characterized in that the reducing atmosphere in the step 2) and the step 3) is realized by a reducing agent.
6. Ce of claim 53+The preparation method of the doped white light LED fluorescent material is characterized in that the reducing agent is carbon monoxide, hydrogen or carbon powder.
CN202011057552.8A 2020-09-30 2020-09-30 Ce3+Doped white light LED fluorescent material and preparation method thereof Active CN112048299B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW201226530A (en) * 2010-12-20 2012-07-01 Univ Nat Chiao Tung Yellow phosphor having oxyapatite structure, preparation method and white light-emitting diode thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Sr4Y6(AlO4)x(SiO4)6-xOδ:Eu2+: A novel apatite structure blue-green emitting phosphor;Shan Yan et al.;《Ceramics International》;20190729;第44卷;第19900–19906页 *
可调白光发射的Ce-Tb-Eu 共掺钙硼硅酸盐发光玻璃;冯永安等;《发光学报》;20130331;第34卷(第3期);第303-307页 *

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