CN109054834A - A kind of adjustable multicolour fluorescent powder of germanate host luminescent and preparation method thereof - Google Patents
A kind of adjustable multicolour fluorescent powder of germanate host luminescent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of adjustable multicolour fluorescent powder of germanate host luminescent, chemical formula Lu2‑x‑yGeO5:xTb3+,yEu3+, wherein 0≤x≤1.50,0≤y≤1.50.The invention also discloses a kind of preparation methods of the adjustable multicolour fluorescent powder of germanate host luminescent.The present invention has the advantages that preparation method is simple, condition is easily-controllable, target product particle is uniform for (1) material；(2) sample prepared is under the excitation of UV light, Ln2GeO5:Tb3+Bright green light can be launched；Lu2GeO5:Eu3+Bright feux rouges can be launched；(3)Tb2+With Eu3+When being co-doped with, which can have full spectrum color emission peak, including blue and green light and feux rouges under ultraviolet excitation, and luminescent color may be adjusted to green light, yellow light and feux rouges etc., therefore have potential application in terms of ultraviolet LED white emitting fluorescent powder.
Description
Technical field
The present invention relates to the phosphor technical fields of luminescence generated by light more particularly to a kind of germanate host luminescent can
Multicolour fluorescent powder of tune and preparation method thereof.
Background technique
White LEDs are as a kind of novel all solid state lighting source, its brightness of W quotient, low energy consumption, the service life is long, small in size, again
Amount is light, response is fast, W and the advantages that penetrate without good fortune, is pollution-free, can planarize, is compact-sized, and is considered as the green illumination of 21 century
Light source.Currently, the implementation of white LEDs mainly has light conversion hysteria, polychromatic combination type, Multiple-quantum well-type and quantum point type
Deng.Considered based on factors such as technique, cost and the states of the art, light conversion hysteria white LEDs are constantly subjected to area research person's
Extensive concern.Currently, light conversion hysteria white LEDs pass through " blue light GaN chip excitation YAG:Ce yellow fluorescent powder " mainly to realize
White light emission.Although the cost of the skilful light powder of YAG:Ce yellow is low, luminous efficiency is higher, lack emitting red light ingredient, so that should
The colour rendering index of kind white LEDs is lower.To overcome disadvantages mentioned above, single matrix fluorescence is excited using ultraviolet/near ultraviolet chip at present
The white light LEDs that material is realized.Currently, the research hotspot that white light emission has become LED field is obtained in this way.This
Kind combination has the advantages that the LED component luminescent color of (1) this combination encapsulation depends on used fluorescence
Powder, the luminescent color of LED component also determine by the emission spectrum of fluorescent powder, therefore, the stability of the luminescent color of LED component and
Color developing than first three types than get well；(2) matrix for the fluorescent powder that this combination uses is single-phase compounds, energy
Amount loss is few, and luminous efficiency is high；(3) a variety of fluorescent powder mixing bring color imbalances can be overcome, there is no colors to reabsorb
With proportion regulation problem, the colour rendering index of LED component is helped to improve；(4) preparation cost is low.Based on above-mentioned advantage, single matrix
White emitting fluorescent powder receives the extensive concern of people, and also deepens continuously therewith to the research of single-matrix white fluorescent powder.With
The continuous development of lighting source, white light LEDs, which will certainly substitute incandescent lamp and fluorescent lamp, becomes mainstream illuminating device, and wherein,
The white light LEDs of ultraviolet/near ultraviolet excitated list substrate fluorescent powder assembling will also become necessarily becoming for semiconductor lighting industry development
Gesture.
A large amount of single-matrix white fluorescent powders have been reported that these are mostly based on the energy transmission of the centre of luminescence, such as Bi3+→
Eu3+,Eu2+→Mn2+, Ce3+→Mn2+, Eu2+→Tb3+→Mn2+And Ce3+→Tb3+→Mn2+Deng.Tb3+ is proposed in this patent
Realize that multicolour shines with Eu3+ codope, including blue and green light and feux rouges, luminescent color may be adjusted to green light, yellow light with
Feux rouges etc., therefore had potential application in terms of ultraviolet LED white emitting fluorescent powder.
Summary of the invention
The invention proposes adjustable multicolour fluorescent powders of a kind of germanate host luminescent and preparation method thereof, on solving
State the problem of proposing in background technique.
The invention proposes a kind of adjustable multicolour fluorescent powder of germanate host luminescent, chemical formulas are as follows: Lu2-x- yGeO5:xTb3+,yEu3+, wherein 0≤x≤1.50,0≤y≤1.50.
The present invention also provides the preparation methods of the adjustable multicolour fluorescent powder of germanate host luminescent, and specific steps are such as
Under:
With Lu2-xGeO5:xTb3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Tb4O7, the corresponding molar ratio of each raw material is 2-x:1:x (0 < x≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 5-8 hours are kept the temperature in 1000-1300 degrees Celsius of lower air environment, last cooled to room temperature, regrinding obtains
Solid powdery luminescent material Lu2-xGeO5:xTb3+；
With Lu2-yGeO5:yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material is 2-y:1:y (0 < y≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 5-8 hours are kept the temperature in 1000-1300 degrees Celsius of lower air environment, last cooled to room temperature, regrinding obtains
Solid powdery luminescent material Lu2-xGeO5:yEu3+；
With Ln2-x-yGeO5:xTb3+,yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material be 2-x-y:1:x:y (0≤x≤
1.50,0≤y≤1.50)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 5-8 hours are kept the temperature in 1000-1300 degrees Celsius of lower air environment, last cooled to room temperature, regrinding obtains
Solid powdery luminescent material Lu2-x-yGeO5:xTb3+,yEu3+。
Preferably, Tb4O7And Eu2O3Purity level be analysis it is pure.
Preferably, Lu2O3And GeO2Purity level be 99.99%.
Advantages of the present invention with the utility model has the advantages that (1) material preparation method is simple, condition is easily-controllable, target product
Grain is uniformly；(2) sample prepared is under the excitation of UV light, Ln2GeO5:Tb3+Bright green light can be launched；Lu2GeO5:Eu3+It can send out
Project bright feux rouges；(3)Tb2+With Eu3+When being co-doped with, which can have full spectrum color transmitting under ultraviolet excitation
Peak, including blue and green light and feux rouges, luminescent color may be adjusted to green light, yellow light and feux rouges etc., therefore in ultraviolet LED with white
It is had potential application in terms of emitting phosphor.
Detailed description of the invention
Fig. 1 is in the present invention in Lu0.95GeO5:0.05Tb3+,Lu0.95GeO5:0.05Eu3+With Lu0.65GeO5:0.30Tb3 +,0.05Eu3+XRD spectrum.
Fig. 2 is the Lu prepared in air atmosphere in the present invention0.95GeO5:0.05Tb3+The excitation and transmitting of luminescent material
Spectrum.
Fig. 3 is the Lu prepared in air atmosphere in the present invention0.95GeO5:0.05Eu3+The emission spectrum of luminescent material.
Fig. 4 is excitation and the emission spectrum of the luminescent material prepared in air atmosphere in the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Embodiment 1
With reference to Fig. 1-4, the invention proposes a kind of adjustable multicolour fluorescent powder of germanate host luminescent, chemical formulas
Are as follows: Lu2-x-yGeO5:xTb3+,yEu3+, wherein 0≤x≤1.50,0≤y≤1.50.
The present invention also provides the preparation methods of the adjustable multicolour fluorescent powder of germanate host luminescent, and specific steps are such as
Under:
With Lu2-xGeO5:xTb3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Tb4O7, the corresponding molar ratio of each raw material is 2-x:1:x (0 < x≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 5 hours are kept the temperature in 1000 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-xGeO5:xTb3+；
With Lu2-yGeO5:yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material is 2-y:1:y (0 < y≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 5 hours are kept the temperature in 1000 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-xGeO5:yEu3+；
With Ln2-x-yGeO5:xTb3+,yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material be 2-x-y:1:x:y (0≤x≤
1.50,0≤y≤1.50)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 5 hours are kept the temperature in 1000 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-x-yGeO5:xTb3+,yEu3+。
Tb4O7And Eu2O3Purity level be analysis it is pure.
Lu2O3And GeO2Purity level be 99.99%.
Embodiment 2
With reference to Fig. 1-4, the invention proposes a kind of adjustable multicolour fluorescent powder of germanate host luminescent, chemical formulas
Are as follows: Lu2-x-yGeO5:xTb3+,yEu3+, wherein 0≤x≤1.50,0≤y≤1.50.
The present invention also provides the preparation methods of the adjustable multicolour fluorescent powder of germanate host luminescent, and specific steps are such as
Under:
With Lu2-xGeO5:xTb3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Tb4O7, the corresponding molar ratio of each raw material is 2-x:1:x (0 < x≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 6 hours are kept the temperature in air environment at 1100 degrees celsius, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-xGeO5:xTb3+；
With Lu2-yGeO5:yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material is 2-y:1:y (0 < y≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 6 hours are kept the temperature in air environment at 1100 degrees celsius, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-xGeO5:yEu3+；
With Ln2-x-yGeO5:xTb3+,yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material be 2-x-y:1:x:y (0≤x≤
1.50,0≤y≤1.50)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 6 hours are kept the temperature in air environment at 1100 degrees celsius, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-x-yGeO5:xTb3+,yEu3+。
Tb4O7And Eu2O3Purity level be analysis it is pure.
Lu2O3And GeO2Purity level be 99.99%.
Embodiment 3
With reference to Fig. 1-4, the invention proposes a kind of adjustable multicolour fluorescent powder of germanate host luminescent, chemical formulas
Are as follows: Lu2-x-yGeO5:xTb3+,yEu3+, wherein 0≤x≤1.50,0≤y≤1.50.
The present invention also provides the preparation methods of the adjustable multicolour fluorescent powder of germanate host luminescent, and specific steps are such as
Under:
With Lu2-xGeO5:xTb3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Tb4O7, the corresponding molar ratio of each raw material is 2-x:1:x (0 < x≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 7 hours are kept the temperature in 1200 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-xGeO5:xTb3+；
With Lu2-yGeO5:yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material is 2-y:1:y (0 < y≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 7 hours are kept the temperature in 1200 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-xGeO5:yEu3+；
With Ln2-x-yGeO5:xTb3+,yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material be 2-x-y:1:x:y (0≤x≤
1.50,0≤y≤1.50)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 7 hours are kept the temperature in 1200 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-x-yGeO5:xTb3+,yEu3+。
Tb4O7And Eu2O3Purity level be analysis it is pure.
Lu2O3And GeO2Purity level be 99.99%.
Embodiment 4
With reference to Fig. 1-4, the invention proposes a kind of adjustable multicolour fluorescent powder of germanate host luminescent, chemical formulas
Are as follows: Lu2-x-yGeO5:xTb3+,yEu3+, wherein 0≤x≤1.50,0≤y≤1.50.
The present invention also provides the preparation methods of the adjustable multicolour fluorescent powder of germanate host luminescent, and specific steps are such as
Under:
With Lu2-xGeO5:xTb3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Tb4O7, the corresponding molar ratio of each raw material is 2-x:1:x (0 < x≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 8 hours are kept the temperature in 1300 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-xGeO5:xTb3+；
With Lu2-yGeO5:yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material is 2-y:1:y (0 < y≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 8 hours are kept the temperature in 1300 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-xGeO5:yEu3+；
With Ln2-x-yGeO5:xTb3+,yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material be 2-x-y:1:x:y (0≤x≤
1.50,0≤y≤1.50)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, in air environment
5 hours are kept the temperature under 500 degrees Celsius, cooled to room temperature, products therefrom regrinding uniformly, then puts high temperature process furnances into
In, 8 hours are kept the temperature in 1300 degrees Celsius of lower air environments, last cooled to room temperature, regrinding obtains solid powder
Last shape luminescent material Lu2-x-yGeO5:xTb3+,yEu3+。
Tb4O7And Eu2O3Purity level be analysis it is pure.
Lu2O3And GeO2Purity level be 99.99%.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (4)
1. a kind of adjustable multicolour fluorescent powder of germanate host luminescent, which is characterized in that its chemical formula are as follows: Lu2-x-yGeO5:
xTb3+,yEu3+, wherein 0≤x≤1.50,0≤y≤1.50.
2. a kind of preparation method of the adjustable multicolour fluorescent powder of germanate host luminescent according to claim 1, special
Sign is, the specific steps are as follows:
With Lu2-xGeO5:xTb3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Tb4O7, the corresponding molar ratio of each raw material is 2-x:1:x (0 < x≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, 500 take the photograph in air environment
5 hours are kept the temperature under family name's degree, cooled to room temperature, products therefrom regrinding uniformly, is then put into high temperature process furnances,
5-8 hours are kept the temperature in 1000-1300 degrees Celsius of lower air environment, last cooled to room temperature, regrinding obtains solid
Powdered luminescent materials Lu2-xGeO5:xTb3+；
With Lu2-yGeO5:yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material is 2-y:1:y (0 < y≤1.5)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, 500 take the photograph in air environment
5 hours are kept the temperature under family name's degree, cooled to room temperature, products therefrom regrinding uniformly, is then put into high temperature process furnances,
5-8 hours are kept the temperature in 1000-1300 degrees Celsius of lower air environment, last cooled to room temperature, regrinding obtains solid
Powdered luminescent materials Lu2-xGeO5:yEu3+；
With Ln2-x-yGeO5:xTb3+,yEu3+For basis material inorganic fluorescent substances the preparation method is as follows:
1) raw material: Lu, is weighed2O3, GeO2With Eu2O3, the corresponding molar ratio of each raw material be 2-x-y:1:x:y (0≤x≤1.50,0
≤y≤1.50)；
2), synthetic sample: each raw material in 1) is accurately weighed, is put into Muffle furnace after grinding uniformly, 500 take the photograph in air environment
5 hours are kept the temperature under family name's degree, cooled to room temperature, products therefrom regrinding uniformly, is then put into high temperature process furnances,
5-8 hours are kept the temperature in 1000-1300 degrees Celsius of lower air environment, last cooled to room temperature, regrinding obtains solid
Powdered luminescent materials Lu2-x-yGeO5:xTb3+,yEu3+。
3. the adjustable multicolour fluorescent powder of germanate host luminescent according to claim 2, which is characterized in that Tb4O7And
Eu2O3Purity level be analysis it is pure.
4. the adjustable multicolour fluorescent powder of germanate host luminescent according to claim 2, which is characterized in that Lu2O3And
GeO2Purity level be 99.99%.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120199791A1 (en) * | 2009-10-12 | 2012-08-09 | Mingjie Zhou | Bismuth ion sensitized rare earth germanate luminescence materials and preparation methods thereof |
-
2018
- 2018-09-26 CN CN201811123225.0A patent/CN109054834A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120199791A1 (en) * | 2009-10-12 | 2012-08-09 | Mingjie Zhou | Bismuth ion sensitized rare earth germanate luminescence materials and preparation methods thereof |
Non-Patent Citations (3)
| Title |
|---|
| PEIMIN GUO等: "Novel phosphors of Eu3þ; Tb3þ or Bi3þ activated Gd2GeO5", 《JOURNAL OF LUMINESCENCE》 * |
| WENBO MA等: "Luminescence properties of full-color single-phased phosphors for white LEDs", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| ZHOU, JUN等: "Multi-color emission evolution and energy transfer behavior of La3GaGe5O16:Tb3+,Eu3+ phosphors", 《JOURNAL OF MATERIALS CHEMISTRY C》 * |
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