CN103509554A - Fluorescent powder material for ultraviolet exciting white light of white LED (Light Emitting Diode) and preparation method thereof - Google Patents

Fluorescent powder material for ultraviolet exciting white light of white LED (Light Emitting Diode) and preparation method thereof Download PDF

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CN103509554A
CN103509554A CN201210216872.2A CN201210216872A CN103509554A CN 103509554 A CN103509554 A CN 103509554A CN 201210216872 A CN201210216872 A CN 201210216872A CN 103509554 A CN103509554 A CN 103509554A
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white light
fluorescent powder
material powder
phosphor material
white
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CN103509554B (en
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刘茜
魏钦华
费凡
唐馥涵
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Jiangsu Institute Of Advanced Inorganic Materials
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention provides a fluorescent powder material for ultraviolet exciting white light of a white LED (Light Emitting Diode) and a preparation method thereof. The fluorescent powder is a fluorescent material doped with Eu<3+> in a bismuth silicate (Bi4Si3O12) matrix. The preparation method of the fluorescent powder material comprises the following steps: firstly, dissolving a precursor material constituting the Bi4Si3O12 and a doping raw material into an alcohol-water mixed solvent according to a proportion, stirring and drying, pre-burning the mixture at 400-800 DEG C in an air atmosphere, cooling the mixture, taking out and grinding the mixture, and then, sintering the mixture at 750-900 DEG C; and finally cooling the mixture to room temperature with the furnace. The chromaticity coordinate of light emitted by the fluorescent powder provided by the invention under excitation of ultraviolet wavelength of 260 nm is located in the white light region and is formed by overlapped intrinsic blue light of Bi4Si3O12 and characteristic orange light of Eu<3+>, emission peaks are respectively located at 472 nm, 588 nm, 593 nm and 611 nm, and the chromaticity coordinate is located in the white light region. The fluorescent powder material provided by the invention can meet the application requirements of white LED illumination field.

Description

For phosphor material powder of the burst of ultraviolel white light of white light LEDs and preparation method thereof
Technical field
The present invention relates to phosphor material powder of a kind of burst of ultraviolel white light and preparation method thereof, specifically, the present invention relates to a kind of doping Eu that is applicable to the application of various White-light LED illuminations field 3+bismuth silicate (Bi 4si 3o 12) base fluorescent powder material and preparation method thereof.
Background technology
White light LEDs is the emerging product of LED being expected most, and its development potentiality in illumination market is inestimable.Compare with incandescent osram lamp and luminescent lamp, LED have volume little (many, multiple combination), thermal value low (there is no thermal radiation), current consumption little (low voltage, low current starting), long (more than 10,000 hours), environmental protection of life-span (shatter-proof, shock-resistant be difficult for broken, waste is recyclable, there is no mercury pollution), can planar package, easy exploiting becomes the advantages such as compact product, by industry, had an optimistic view of in coming 10 years, become large potentiality commodity that substitute traditional lighting utensil.White light is different from the purple monochromatic ray of the bluish-green ultramarine of blood orange, conventionally by two kinds of modes, obtains white light:
1, with ultraviolet or purple LED+RGB(RGB) three primary colors fluorescent powder synthesizes LED.
2, with blue-ray LED+red green fluorescence powder or blue-ray LED+gold-tinted fluorescent material, form white light.
But still there are some problems in white light LEDs now: photoelectric transformation efficiency is lower, and cost is higher, and white light color developing is poor.So the research and development of white light LEDs novel material is had to great practical significance and commercial value.
Summary of the invention
The problem existing for above-mentioned existing white light LEDs technology, the object of this invention is to provide phosphor material powder of a kind of burst of ultraviolel white light and preparation method thereof.This fluorescent material color developing is good, can meet the application requiring in White-light LED illumination field.
For achieving the above object, the invention provides a kind of phosphor material powder of the burst of ultraviolel white light for white light LEDs, described phosphor material powder is doping Eu 3+bismuth silicate (the Bi of ion 4si 3o 12) sill.
In one embodiment of the present invention, described Eu 3+the doping of ion is 0.5 ~ 3mol%, with Eu in described fluorescent material 3+and Bi 3+total mole number meter.
In one embodiment of the present invention, described phosphor material powder is by bismuth oxide (Bi 2o 3), silicon-dioxide (SiO 2) and europium sesquioxide (Eu 2o 3) make, wherein, the mass percent of each component is as follows:
Bi 2O 3 81.4~83.5%
SiO 2 16.2%
Eu 2O 3 0.3~2.4%；
The mass percent sum of each component is 100%.
The present invention provides a kind of method of preparing described phosphor material powder on the other hand, and described method comprises:
To form bismuth silicate (Bi 4si 3o 12) precursor material and doped raw material by proportioning, be dissolved in alcohol water mixed solvent, stir, dry;
Under air atmosphere, under the calcined temperature of 400 ~ 600 ℃, carry out pre-burning, cooling rear taking-up is ground;
Under air atmosphere, under the calcining temperature of 750 ~ 900 ℃, calcine, then furnace cooling arrives room temperature, and grinds to form phosphor material powder.
In a preferred embodiment, form bismuth silicate (Bi 4si 3o 12) precursor material be Bismuth trinitrate and tetraethoxy, described doped raw material is europium nitrate.
In an embodiment of the invention, described alcohol water mixed solvent is (4 ~ 6) by deionized water and dehydrated alcohol in mass ratio: 2 form.
In one embodiment, form bismuth silicate (Bi 4si 3o 12) precursor material and the total mass of doped raw material and the mass ratio of alcohol water mixed solvent be 6:(10 ~ 14).
In one embodiment, described being dried is at 60 ~ 90 ℃, to toast 18 ~ 24 hours in baking oven.
In one embodiment, by the temperature rise rates of 150 ~ 200 ℃ per hour, be warmed up to calcined temperature, the pre-burning time is 1 ~ 3 hour.
In one embodiment, by the temperature rise rates of 150 ~ 200 ℃ per hour, be warmed up to calcining temperature, calcination time is 3 ~ 5 hours.
Specifically, the present invention relates to a kind of phosphor material powder and preparation method thereof of the burst of ultraviolel white light for white light LEDs.Be specifically related to a kind of rare earth doped Eu for preparing 3+bismuth silicate (Bi 4si 3o 12) method of sill.
As a kind of preferred version, described Eu 3+doping in described powder body material, account for 0.5 ~ 3mol%.
As further prioritization scheme, described powder body material is by bismuth oxide (Bi 2o 3), silicon-dioxide (SiO 2) and europium sesquioxide (Eu 2o 3) form, and each mass percent forming is as follows:
Bi 2O 3 81.4~83.5%
SiO 2 16.2%
Eu 2O 3 0.3~2.4%；
The above-mentioned mass percent sum that each forms is 100%.
Phosphor material powder of a kind of burst of ultraviolel white light for white light LEDs and preparation method thereof is provided in the present invention, first the precursor material and the doped raw material that form bismuth silicate is dissolved in alcohol water mixed solvent by proportioning, stir, dry; Then first under air atmosphere, carry out pre-burning in 400 ~ 800 ℃, take out and grind, under air atmosphere, in 750 ~ 900 ℃, calcine again afterwards; Last furnace cooling, to room temperature, takes out and grinds.
As a kind of preferred version, the precursor material that forms bismuth silicate is Bismuth trinitrate and tetraethoxy, and described doped raw material is europium nitrate.
As a kind of preferred version, described alcohol water mixed solvent is (4 ~ 6) by deionized water and dehydrated alcohol in mass ratio: 2 form.
As a kind of preferred version, the mass ratio that forms the precursor material of bismuth silicate and the total mass of doped raw material and alcohol water mixed solvent is 6:(10 ~ 14).
As a kind of preferred version, described dry referring in 60 ~ 90 ℃ of baking ovens dried 18 ~ 24 hours.
As a kind of preferred version, by the temperature rise rates of 150 ~ 200 ℃ per hour, be warmed up to calcined temperature, the pre-burning time is 1 ~ 3 hour.
As a kind of preferred version, by the temperature rise rates of 150 ~ 200 ℃ per hour, be warmed up to calcining temperature, calcination time is 3 ~ 5 hours.
Design philosophy of the present invention is by the Eu that adulterates in bismuth silicate 3+, make Eu 3+part replaces the Bi in bismuth silicate 3+.Due to Bi in bismuth silicate 3+under burst of ultraviolel, launch blue light, and Eu 3+replace Bi 3+itself feature blood orange light of rear transmitting, finally both are compounded to form white light.
Experimental results show that: singly mix Eu 3+after, along with Eu 3+the increase gradually of concentration, emmission spectrum is from single blue light peak to blue light and the bimodal transformation of blood orange light.Wherein, work as Eu 3+when concentration is positioned at 0.5 ~ 3mol%, the chromaticity coordinates of phosphor material powder of the present invention is positioned at white light field, shows that final synthetic product is a kind of potential fluorescent material that can be used for white light LEDs.
Compared with prior art, phosphor material powder prepared by the present invention a kind of rare earth ion that only need adulterate can obtain the white light being formed by blue light and blood orange photorecombination, and emission wavelength lays respectively at 472nm, 588nm, 593nm and 611nm.Compare with common fluorescent material, powder body material of the present invention not only has that composition is simple, and synthesis temperature is low, and raw material is cheap and easy to get, and preparation method is simple, without specific installation, is applicable to suitability for industrialized production, has practicality, can meet the application requiring of White-light LED illumination.
Accompanying drawing explanation
Fig. 1 (a) is the different Eu of the prepared doping of the embodiment of the present invention 3+the emmission spectrum of the bismuth silicate fluorescent material of concentration under normal temperature 260nm excites;
Fig. 1 (b) is the different Eu of doping 3+the chromaticity coordinates position of the bismuth silicate fluorescent material of concentration;
It should be noted that, in Fig. 1 (b), be denoted as " green ", " blueness ", " purple ", " orange ", " pink colour ", " redness " and " white " is not between each district, to have obvious boundary in order to represent, between the region that their show, has transitional region.
Known from Fig. 1 (b), it is white portion that residing region is put in " 1 ", " 2 " and " 3 ".Because the distance near look district around of each point is slightly different, the white that " 1 ", " 2 " and " 3 " point present is also slightly different vision, specifically as shown in Fig. 1 (c).
Fig. 1 (c) is different Eu 3+concentration and the pure bismuth silicate powder photo under UV-254nm excites.
Wherein, the sample that is designated as " pure " is shown as blue cast, and " 1 " number sample is candoluminescence tone, and " 2 " number sample is ordinary white, and " 3 " number sample is white warm photochromic tune.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail.It should be noted that content of the present invention is not limited to these concrete embodiments.Do not deviating under the prerequisite of background of the present invention and spirit, those skilled in the art can carry out substitutions and modifications of equal value on the basis of reading content of the present invention, and its content is also included within the scope of protection of present invention.
Embodiment 1
Mass ratio by folding synthesis oxide is Bi 2o 3: SiO 2: Eu 2o 3=263.4:51.2:1(is equivalent to Eu 3+doping is 0.5mol%) take Bismuth trinitrate (Bi (NO 3) 35H 2o), tetraethoxy (TEOS) and europium nitrate (Eu (NO 3) 36H 2o) each raw material; Above-mentioned all constitutive materials are dissolved in the mixed solvent of deionized water and dehydrated alcohol composition, wherein, the total mass of constitutive material: deionized water quality: dehydrated alcohol quality=1.9:3:1; At room temperature stir and after 1 hour, put into 90 ℃ of baking ovens and dry 18 hours.
By temperature rise rate, be 150 ℃/h and be warmed up to 400 ℃, at 400 ℃ of air atmospheres, carry out pre-burning 1 hour, take out and grind.
Then, by temperature rise rate, be 150 ℃/h and be warmed up to 750 ℃, at 750 ℃ of air atmospheres, calcine 3 hours; Furnace cooling is to room temperature; Take out and grind.
As seen from Figure 1: the transmitting peak position of embodiment 1 prepared phosphor material powder is at 472nm, 588nm, 593nm and 611nm, chromaticity coordinates position, as shown in 1 in Fig. 1 (b), for (0.308,0.321), is positioned at white light field.
Embodiment 2
Mass ratio by folding synthesis oxide is Bi 2o 3: SiO 2: Eu 2o 3=131:25.6:1(is equivalent to Eu 3+doping is 1mol%) take Bismuth trinitrate (Bi (NO 3) 35H 2o), tetraethoxy (TEOS) and europium nitrate (Eu (NO 3) 36H 2o) each raw material; Above-mentioned all constitutive materials are dissolved in the mixed solvent of deionized water and dehydrated alcohol composition, wherein the total mass of constitutive material: deionized water quality: dehydrated alcohol quality=1.9:3:1; At room temperature stir and after 2 hours, put into 80 ℃ of baking ovens and dry 20 hours.
By temperature rise rate, be 160 ℃/h and be warmed up to 500 ℃, under air atmosphere, 500 ℃ are carried out pre-burning 2 hours, take out and grind.
Then, then by temperature rise rate, be 160 ℃/h and be warmed up to 800 ℃, under air atmosphere, 800 ℃ of calcinings are 4 hours; Furnace cooling is to room temperature; Take out and grind.
As seen from Figure 1: detect learn embodiment 2 prepared phosphor material powders transmitting peak position at 472nm, 588nm, 593nm and 611nm, chromaticity coordinates position, as shown in 2 in Fig. 1 (b), for (0.333,0.326), is positioned at white light field.
Embodiment 3
Mass ratio by folding synthesis oxide is Bi 2o 3: SiO 2: Eu 2o 3=131:25.6:1(is equivalent to Eu 3+doping is 1mol%) take Bismuth trinitrate (Bi (NO 3) 35H 2o), tetraethoxy (TEOS) and europium nitrate (Eu (NO 3) 36H 2o) each raw material; Above-mentioned all constitutive materials are dissolved in the mixed solvent of deionized water and dehydrated alcohol composition, wherein the total mass of constitutive material: deionized water quality: dehydrated alcohol quality=1.9:3:1; At room temperature stir and after 2 hours, put into 70 ℃ of baking ovens and dry 22 hours.
By temperature rise rate, be 170 ℃/h and be warmed up to 600 ℃, under air atmosphere, 600 ℃ are carried out pre-burning 3 hours, take out and grind.
Then, then by temperature rise rate, be 170 ℃/h and be warmed up to 800 ℃, under air atmosphere, 800 ℃ of calcinings are 5 hours; Furnace cooling is to room temperature; Take out and grind.
As seen from Figure 1: detect learn embodiment 3 prepared phosphor material powders transmitting peak position at 472nm, 588nm, 593nm and 611nm, chromaticity coordinates position, as shown in 2 in Fig. 1 (b), for (0.333,0.326), is positioned at white light field.
Embodiment 4
Mass ratio by folding synthesis oxide is Bi 2o 3: SiO 2: Eu 2o 3=45:9:1(is equivalent to Eu 3+doping 3mol%) take Bismuth trinitrate (Bi (NO 3) 35H 2o), tetraethoxy (TEOS) and europium nitrate (Eu (NO 3) 36H 2o) each raw material; Above-mentioned all constitutive materials are dissolved in the mixed solvent of deionized water and dehydrated alcohol composition, wherein the total mass of constitutive material: deionized water quality: dehydrated alcohol quality=1.9:3:1; At room temperature stir and after 2 hours, put into 60 ℃ of baking ovens and dry 24 hours.
By temperature rise rate, be 200 ℃/h and be warmed up to 800 ℃, under air atmosphere, 800 ℃ are carried out pre-burning 2 hours, take out and grind.
Then, then by temperature rise rate, be 200 ℃/h and be warmed up to 900 ℃, under air atmosphere, 900 ℃ of calcinings are 3 hours; Furnace cooling is to room temperature; Take out and grind.
As seen from Figure 1: detect learn embodiment 4 prepared phosphor material powders transmitting peak position at 472nm, 588nm, 593nm and 611nm, chromaticity coordinates position, as shown in 3 in Fig. 1 (b), for (0.404,0.334), is positioned at white light field.
Finally be necessary described herein: above embodiment is only for being described in further detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.

Claims (10)

1. for a phosphor material powder for the burst of ultraviolel white light of white light LEDs, described phosphor material powder is doping Eu 3+bismuth silicate (the Bi of ion 4si 3o 12) sill.
2. the phosphor material powder of the burst of ultraviolel white light for white light LEDs according to claim 1, is characterized in that: described Eu 3+the doping of ion is 0.5 ~ 3mol%, with Eu in described fluorescent material 3+and Bi 3+total mole number meter.
3. the phosphor material powder of the burst of ultraviolel white light for white light LEDs according to claim 2, is characterized in that: described phosphor material powder is by bismuth oxide (Bi 2o 3), silicon-dioxide (SiO 2) and europium sesquioxide (Eu 2o 3) make, wherein, the mass percent of each component is as follows:
Bi 2O 3 81.4~83.5%
SiO 2 16.2%
Eu 2O 3 0.3~2.4%；
The mass percent sum of each component is 100%.
4. a method of preparing phosphor material powder described in claim 1-3 any one, described method comprises:
To form bismuth silicate (Bi 4si 3o 12) precursor material and doped raw material by proportioning, be dissolved in alcohol water mixed solvent, stir, dry;
Under air atmosphere, under the calcined temperature of 400 ~ 600 ℃, carry out pre-burning, cooling rear taking-up is ground;
Under air atmosphere, under the calcining temperature of 750 ~ 900 ℃, calcine, then furnace cooling arrives room temperature, and grinds to form phosphor material powder.
5. method according to claim 4, is characterized in that: form bismuth silicate (Bi 4si 3o 12) precursor material be Bismuth trinitrate and tetraethoxy, described doped raw material is europium nitrate.
6. method according to claim 4, is characterized in that: described alcohol water mixed solvent is (4 ~ 6) by deionized water and dehydrated alcohol in mass ratio: 2 form.
7. method according to claim 4, is characterized in that: form bismuth silicate (Bi 4si 3o 12) precursor material and the total mass of doped raw material and the mass ratio of alcohol water mixed solvent be 6:(10 ~ 14).
8. method according to claim 4, is characterized in that: described being dried is at 60 ~ 90 ℃, to toast 18 ~ 24 hours in baking oven.
9. method according to claim 4, is characterized in that: the temperature rise rate by 150 ~ 200 ℃ per hour is warmed up to calcined temperature, and the pre-burning time is 1 ~ 3 hour.
10. method according to claim 4, is characterized in that: the temperature rise rate by 150 ~ 200 ℃ per hour is warmed up to calcining temperature, and calcination time is 3 ~ 5 hours.
CN201210216872.2A 2012-06-27 2012-06-27 Fluorescent powder material for ultraviolet exciting white light of white LED (Light Emitting Diode) and preparation method thereof Active CN103509554B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104342103A (en) * 2013-08-01 2015-02-11 中国石油化工股份有限公司 A foam gelling acid, and preparation, a using method and applications thereof
CN107256920A (en) * 2017-08-15 2017-10-17 苏州轻光材料科技有限公司 A kind of high luminous intensity burst of ultraviolel white light LEDs and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ZHANG YAN ET AL.: "Synthesis and Luminescence Properties of Eu3+-doped Bi4Si3O12", 《JOURNAL OF INORGANIC MATERIALS》 *
费一汀等: "稀土元素( Ce 、Nd 和Eu) 掺杂Bi4Si3O12晶体的生长与性能", 《人工晶体学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104342103A (en) * 2013-08-01 2015-02-11 中国石油化工股份有限公司 A foam gelling acid, and preparation, a using method and applications thereof
CN107256920A (en) * 2017-08-15 2017-10-17 苏州轻光材料科技有限公司 A kind of high luminous intensity burst of ultraviolel white light LEDs and preparation method thereof

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