CN104152145A - Three-activator single-matrix white light phosphor and preparation method thereof - Google Patents
Three-activator single-matrix white light phosphor and preparation method thereof Download PDFInfo
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- CN104152145A CN104152145A CN201410350569.0A CN201410350569A CN104152145A CN 104152145 A CN104152145 A CN 104152145A CN 201410350569 A CN201410350569 A CN 201410350569A CN 104152145 A CN104152145 A CN 104152145A
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- white light
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Abstract
The invention relates to a three-activator single-matrix white light phosphor and a preparation method thereof, and relates to the field of luminescent materials. The chemical components of the three-activator single-matrix white light phosphor accords with M2Y8(1-x-y-z)(SiO4)6O2:xR, yG, zB, wherein M is any one of metal element Mg or Ca; R is rare earth element Eu; B is rare earth element Tm; G is one of rare earth element Tb or Dy; and x is more than or equal to 0 and less than or equal to 0.2, y is more than 0 and less than or equal to 0.2, and z is more than 0 and less than or equal to 0.2. The preparation method of the three-activator single-matrix white light phosphor adopts a high-order solid-phase method which comprises the following steps: weighing; grinding; calcining at a high temperature; and cooling. The three-activator single-matrix white light phosphor and the preparation method thereof which are provided by the invention obtain white light emission through the mixing of three activators; the three-activator single-matrix white light phosphor provided by the invention has the characteristics of stability in white light, high luminescent brightness, good chemical stability and heat stability, controllability and adjustability in quality and the like and can serve as white light luminescent powder and other luminescent materials.
Description
Technical field
The present invention relates to adjustable single matrix fluorescent material of a kind of white light quality based on three activator and preparation method thereof, belong to field of light emitting materials.
Background technology
Plurality of advantages such as that white light LEDs has is energy-efficient, environmental protection, volume is little, the life-span is long, shock resistance is good, fast response time, and be a kind of all solid state lighting installation, be considered to substitute traditional lighting device the 4th generation new light sources.Its plurality of advantages makes it have wide illumination market prospect, in industrial circle and the product for civilian use, is widely used.
Technically, white light LEDs is mainly realized by the scheme of LED chip and fluorescent material conversion, and the approach of realization mainly contains three kinds: the LED of yellow fluorescent powder, blue-ray LED collocation green and red fluorescence powder and the near-ultraviolet lights such as blue-ray LED collocation YAG excites the fluorescent material of RGB look.The white light LEDs glow color that the third approach obtains is only determined by fluorescent material proportioning, more easily obtains the stable white light of glow color, and its luminous efficiency and colour rendering index are all than two kinds of approach are well a lot of above.But owing to having mixed multiple fluorescent material, need to consider that the proportioning of various fluorescent material has increased technique fussy degree, also increase cost, and between mixture, exist energy waste, color to absorb again and the not equal problem of rate of ageing simultaneously.
If prepare single substrate fluorescent powder with multiple emission peaks, it is poor that the method both can overcome the color reducibility of the yellow fluorescent powders such as blue-ray LED collocation YAG or collocation green and red fluorescence powder, the shortcoming that colour rendering index is low, simultaneously because be single matrix, the LED that can solve again near-ultraviolet light excites that color between the mixture of fluorescent material of RGB look absorbs again, energy waste, proportioning regulation and control and the equal problem of rate of ageing, and for improving light source quality, simplify the technological process of production and have very real meaning.
Human eye is insensitive to near-ultraviolet light, and the color of synthesize white light LED is only determined by red, green, blue three primary colors fluorescent powder, therefore color stable, and reproduction power is strong, is a kind of new research tendency of white light LEDs development.For example, the patent application text of application number 200500142908 has been reported (Y
l-xgd
x) BO
3: Ce
3+, Tb
3+, Eu
3+, Y
2siO
5: Ce
3+, Tb
3+, Eu
3+fluorescent material, the single substrate fluorescent powder of LED of Here it is typical three activator.
Summary of the invention
The technical problem that the present invention solves: for the problems referred to above, the present invention aims to provide adjustable single-substrate white fluorescent powder of a kind of white light quality based on three activator and preparation method thereof.。
Technical scheme of the present invention: a kind of three activator single-substrate white fluorescent powders, the chemical composition of material is for meeting M
2y
8 (1-x-y-z)(SiO
4)
6o
2: xR, yG, zB, wherein M is any one of metallic element Mg or Ca; R is rare earth element Eu; B is rare earth element Tm; G is the one of rare earth element tb or Dy, and 0≤x≤0.2,0<y≤0.2,0<z≤0.2.
As preferably, M is metallic element Mg.
As preferably, G is rare earth element Dy.
As preferably, described three activator single-substrate white fluorescent powders use UV-light to excite as excitaton source, and ultraviolet wavelength is 340-380nm.
The preparation method of above-mentioned three activator single-substrate white fluorescent powders provided by the invention, comprises the following steps:
(1) take respectively the oxide compound that contains Tb or Dy, Y, Eu, Tm, Si, the oxide compound of Mg or the carbonate of Ca by stoichiometric ratio;
(2) above-mentioned substance is ground, grind and add alcohol after 1 hour, then grind after 0.5 hour, dry;
(3) said mixture is packed in corundum crucible, and calcine in High Temperature Furnaces Heating Apparatus, calcining temperature is 1050～1350 DEG C, and calcination time is 3～5 hours;
(4), after calcining, naturally cooling, takes out, and makes three activator single-substrate white fluorescent powder materials.
Beneficial effect of the present invention: three activator single-substrate white fluorescent powders provided by the invention are overlapping phenomenons of utilizing the excitation spectrum of rare earth ion, obtains white light emission.Rare earth ion Tm
3+under the ultraviolet excitation of 357nm, launch the blue light that centre wavelength is 450 nm; Rare earth ion Tb
3+under the ultraviolet excitation of 377 nm, launch the green glow that centre wavelength is respectively 543 nm; Rare earth ion Dy
3+under the ultraviolet excitation of 350 nm, launch blue light that centre wavelength is 478 nm and the gold-tinted of 573 nm; Rare earth ion Eu
3+under the ultraviolet excitation of 355 nm, launch the ruddiness that centre wavelength is 613 nm.Because above-mentioned rare earth ion excitation spectrum has overlappingly, by Tm/Tb/Eu or Tm/Dy/Eu codoped, make this fluorescent material under near-ultraviolet light Same Wavelength excites, can launch the bands of a spectrum of three wave bands of red, green, blue simultaneously.By regulating Tm/Tb/Eu, the ratio of tri-kinds of ionic concns of Tm/Dy/Eu, just can regulate and control the power of several emmission spectrum, acquisition white light emission.
In the time choosing above-mentioned three kinds of rare earth ion Tm/Tb/Eu or Tm/Dy/Eu co-doped, under the exciting of 357nm light source, launch comparatively stable white light, along with the variation of dopant ion concentration, thereby three bands of a spectrum stacks have realized white light emission in single-matrix, and glow color is adjustable variation within the scope of white light.Overcome the defect of three primary colors fluorescent powder because of the irregular colour weighing apparatus of heterogeneous mixing generation simultaneously, can avoid red, green, blue three primary colors fluorescent powder to absorb again the problem that regulates and controls whole lighting efficiency is weakened with proportioning simultaneously.
Three activator single-substrate white fluorescent powders prepared in accordance with the present invention, fluorescent powder grain is even, realize the doping on fluorescent material activator molecular level, fluorescent material of the present invention can be used as white light LEDs luminescent powder, also can be used as the luminescent material of preparation ultraviolet or purple light excited display device.
Brief description of the drawings
Fig. 1 is the luminescent spectrum of three activator single-substrate white fluorescent powders under 357 nm excite that embodiment 1-5 tri-mixes Tm/Tb/Eu, and wherein M is metallic element Mg.
Fig. 2 is the luminescent spectrum of three activator single-substrate white fluorescent powders under 357 nm excite that embodiment 6-10 tri-mixes Tm/Dy/Eu, and wherein M is metallic element Mg.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1-5:
Adopt analytically pure MgO, SiO
2with 99.99% Y
2o
3, Tm
2o
3, Tb
4o
7, Eu
2o
3for main raw material, preparation three activator list substrate fluorescent powders, the chemical composition of material meets M
2y
8 (1-x-y-z)(SiO
4)
6o
2: xR, yG, zB, wherein R, G, B are respectively Eu, Tb and Tm, and the total mass of raw material is 1g, and each raw materials quality is as shown in table 1:
The quality (g) of the each feed composition of table 1 embodiment 1-5
By after above-mentioned every group of sample accurate weighing in mortar ground and mixed 1 hour, then add alcohol and grind half an hour, every group of raw material is placed in to corundum crucible, and is placed in High Temperature Furnaces Heating Apparatus, calcining temperature is 1350 DEG C, calcination time is 5 hours, naturally cooling after calcining finishes, takes out, and is crushed to powdery, obtain 5 duplicate samples, the emmission spectrum of 5 duplicate samples under exciting at 357 nm is as shown in table 2: (wherein: Tm
3+the blue light of emission of ions 450 nm, Tb
3+ion is mainly launched the green glow of 543 nm, Eu
3+ion is mainly launched the ruddiness of 615 nm.）
The luminescent properties parameter of table 2 embodiment 1-5
Fig. 1 is the luminescent spectrums of the three three activator single-substrate white fluorescent powders of mixing Tm/Tb/Eu under 357 nm excite.The existing Tm that belongs to of transmitting collection of illustrative plates of sample
3+broadband blue light transmitting, also belong to Tb
3+green emission, belong in addition Eu
3+red emission.Along with the change of activator doping content, Mg
2y
8(SiO
4)
6o
2chromaticity coordinates finally changes to (x=0.331, y=0.337) from (x=0.279, y=0.298) point-blank, and the glow color of counter sample is in white light field always.Work as Tm
3+doping content z=0.04, Tb
3+doping content y=0.10, Eu
3+doped parameterx=0.10 o'clock, Mg
2y
8(SiO
4)
6o
2chromaticity coordinates be (x=0.331, y=0.337), white light quality is best.
Embodiment 6-10:
Adopt analytically pure MgO, SiO
2with 99.99% Y
2o
3, Tm
2o
3, Dy
2o
3, Eu
2o
3for main raw material, preparation three activator list substrate fluorescent powders, the chemical composition of material meets M
2y
8 (1-x-y-z)(SiO
4)
6o
2: xR, yG, zB, wherein R, G, B are respectively Eu, Dy and Tm, and the total mass of raw material is 1g, and each raw materials quality is as shown in table 3:
The quality (g) of the each feed composition of table 3 embodiment 6-10
By after above-mentioned every group of sample accurate weighing in mortar ground and mixed 1 hour, then add alcohol and grind half an hour, every group of raw material is placed in to corundum crucible, and is placed in High Temperature Furnaces Heating Apparatus, calcining temperature is 1350 DEG C, calcination time is 5 hours, naturally cooling after calcining finishes, takes out, and is crushed to powdery, obtain 5 duplicate samples, the emmission spectrum of 5 duplicate samples under exciting at 357 nm is as shown in table 4:
The luminescent properties parameter of table 4 embodiment 6-10
Fig. 2 is the luminescent spectrums of the three three activator single-substrate white fluorescent powders of mixing Tm/Dy/Eu under 357 nm excite.The existing Tm that belongs to of transmitting collection of illustrative plates of sample
3+broadband blue light transmitting, also belong to Dy
3+yellow green light transmitting, belong in addition Eu
3+red emission.Along with the continuous change of three kinds of activator ion concentration, Mg
2y
8(SiO
4)
6o
2chromaticity coordinates changes to (x=0.333, y=0.305) from (x=0.308, y=0.269) point-blank, and the glow color of counter sample is in white light field always.Work as Tm
3+doping content z=0.02, Dy
3+doping content y=0.02, Eu
3+doped parameterx=0.15 o'clock, Mg
2y
8(SiO
4)
6o
2: the chromaticity coordinates of Tm/Dy/Eu is (x=0.333, y=0.305), and white light quality is best.
Embodiment 11-15:
Adopt analytically pure CaCO
3, SiO
2with 99.99% Y
2o
3, Tm
2o
3, Tb
4o
7, Eu
2o
3for main raw material, preparation three activator list substrate fluorescent powders, the chemical composition of material meets M
2y
8 (1-x-y-z)(SiO
4)
6o
2: xR, yG, zB, wherein R, G, B are respectively Eu, Tb and Tm, and the total mass of raw material is 1g, and each raw materials quality is as shown in table 5:
The quality (g) of the each feed composition of table 5 embodiment 11-15
By after above-mentioned every group of sample accurate weighing in mortar ground and mixed 1 hour, then add alcohol and grind half an hour, every group of raw material is placed in to corundum crucible, and is placed in High Temperature Furnaces Heating Apparatus, calcining temperature is 1350 DEG C, calcination time is 5 hours, naturally cooling after calcining finishes, takes out, and is crushed to powdery, obtain 5 duplicate samples, the emmission spectrum of 5 duplicate samples under exciting at 357 nm is as shown in table 6:
The luminescent properties parameter of table 6 embodiment 11-15
The chromaticity coordinates of above-mentioned sample is along with the continuous change of three kinds of activator ion concentration, and the glow color of counter sample is in white light field always.Work as Tm
3+doping content z=0.02, Tb
3+doping content y=0.05, Eu
3+doped parameterx=0.12 o'clock, Mg
2y
8(SiO
4)
6o
2: the chromaticity coordinates of Tm/Tb/Eu is (x=0.314, y=0.327), and white light quality is best.
Embodiment 16-20:
Adopt analytically pure CaCO
3, SiO
2with 99.99% Y
2o
3, Tm
2o
3, Dy
2o
3, Eu
2o
3for main raw material, preparation three activator list substrate fluorescent powders, the chemical composition of material meets M
2y
8 (1-x-y-z)(SiO
4)
6o
2: xR, yG, zB, wherein R, G, B are respectively Eu, Dy and Tm, and the total mass of raw material is 1g, and each raw materials quality is as shown in table 7:
The quality (g) of the each feed composition of table 7 embodiment 16-20
By after above-mentioned every group of sample accurate weighing in mortar ground and mixed 1 hour, then add alcohol and grind half an hour, every group of raw material is placed in to corundum crucible, and is placed in High Temperature Furnaces Heating Apparatus, calcining temperature is 1350 DEG C, calcination time is 5 hours, naturally cooling after calcining finishes, takes out, and is crushed to powdery, obtain 5 duplicate samples, the emmission spectrum of 5 duplicate samples under exciting at 357 nm is as shown in table 8:
The luminescent properties parameter of table 8 embodiment 16-20
The chromaticity coordinates of above-mentioned sample is along with the continuous change of three kinds of activator ion concentration, and the glow color of counter sample is in white light field always.Work as Tm
3+doping content z=0.04, Dy
3+doping content y=0.02, Eu
3+doped parameterx=0.15 o'clock, Mg
2y
8(SiO
4)
6o
2: the chromaticity coordinates of Tm/Dy/Eu is (x=0.329, y=0.311), and white light quality is best.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (5)
1. three activator single-substrate white fluorescent powders, is characterized in that: the chemical composition of material is for meeting M
2y
8 (1-x-y-z)(SiO
4)
6o
2: xR, yG, zB, wherein M is any one of metallic element Mg or Ca; R is rare earth element Eu; B is rare earth element Tm; G is the one of rare earth element tb or Dy, and 0≤x≤0.2,0<y≤0.2,0<z≤0.2.
2. three activator single-substrate white fluorescent powders according to claim 1, is characterized in that: M is metallic element Mg.
3. three activator single-substrate white fluorescent powders according to claim 1, is characterized in that: G is rare earth element Dy.
4. three activator single-substrate white fluorescent powders according to claim 1, is characterized in that: described three activator single-substrate white fluorescent powders use UV-light to excite as excitaton source, and ultraviolet wavelength is 340-380nm.
5. a preparation method for three activator single-substrate white fluorescent powders claimed in claim 1, is characterized in that, comprises the following steps:
(1) take respectively the oxide compound that contains Tb or Dy, Y, Eu, Tm, Si, the oxide compound of Mg or the carbonate of Ca by stoichiometric ratio;
(2) above-mentioned substance is ground, grind and add alcohol after 1 hour, then grind after 0.5 hour, dry;
(3) said mixture is packed in corundum crucible, and calcine in High Temperature Furnaces Heating Apparatus, calcining temperature is 1050～1350 DEG C, and calcination time is 3～5 hours;
(4), after calcining, naturally cooling, takes out, and makes three activator single-substrate white fluorescent powder materials.
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Cited By (6)
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| CN104877680A (en) * | 2015-04-22 | 2015-09-02 | 南方科技大学 | White light fluorescent powder and preparation method thereof and white light emitting device |
| CN107033902A (en) * | 2017-05-27 | 2017-08-11 | 西安交通大学 | A kind of single matrix three primary colours are used for silicate fluorescent material of LED white lights and preparation method thereof |
| WO2020220669A1 (en) * | 2019-04-29 | 2020-11-05 | 佛山市国星光电股份有限公司 | Novel light emitting lamp bead and lamp |
| CN112779009A (en) * | 2021-02-05 | 2021-05-11 | 淮阴师范学院 | High-sensitivity optical temperature sensing luminescent material and preparation method thereof |
| CN115820255A (en) * | 2022-12-21 | 2023-03-21 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
| CN116814263A (en) * | 2023-06-07 | 2023-09-29 | 云南大学 | Single-phase white light fluorescent material and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877680A (en) * | 2015-04-22 | 2015-09-02 | 南方科技大学 | White light fluorescent powder and preparation method thereof and white light emitting device |
| CN107033902A (en) * | 2017-05-27 | 2017-08-11 | 西安交通大学 | A kind of single matrix three primary colours are used for silicate fluorescent material of LED white lights and preparation method thereof |
| WO2020220669A1 (en) * | 2019-04-29 | 2020-11-05 | 佛山市国星光电股份有限公司 | Novel light emitting lamp bead and lamp |
| CN112779009A (en) * | 2021-02-05 | 2021-05-11 | 淮阴师范学院 | High-sensitivity optical temperature sensing luminescent material and preparation method thereof |
| CN115820255A (en) * | 2022-12-21 | 2023-03-21 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
| CN115820255B (en) * | 2022-12-21 | 2023-09-26 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
| CN116814263A (en) * | 2023-06-07 | 2023-09-29 | 云南大学 | Single-phase white light fluorescent material and preparation method and application thereof |
| CN116814263B (en) * | 2023-06-07 | 2024-05-28 | 云南大学 | Single-phase white light fluorescent material and preparation method and application thereof |
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Application publication date: 20141119 |