CN103509554B - 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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CN103509554B
CN103509554B CN201210216872.2A CN201210216872A CN103509554B CN 103509554 B CN103509554 B CN 103509554B CN 201210216872 A CN201210216872 A CN 201210216872A CN 103509554 B CN103509554 B CN 103509554B
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white light
material powder
phosphor material
fluorescent powder
white
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CN103509554A (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 the phosphor material powder and preparation method thereof of the burst of ultraviolel white light of white light LEDs
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 being applicable to the application of various White-light LED illumination 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 be expected most, and it is inestimable in the development potentiality of illumination market.Compared with incandescent osram lamp and luminescent lamp, LED have volume little (many, multiple combination), thermal value low (not having thermal radiation), current consumption little (low voltage, low current start), life-span long (more than 10,000 hours), environmental protection (shatter-proof, shock-resistant not easily broken, waste is recyclable, there is no mercury pollution), planar package, easy exploiting can become the advantages such as compact product, had an optimistic view of in coming 10 years by industry, become large potentiality commodity of alternative traditional lighting utensil.White light is different from the purple monochromatic ray of the bluish-green ultramarine of blood orange, usually obtains white light by two kinds of modes:
1, with ultraviolet or purple LED+RGB(RGB) three primary colors fluorescent powder synthesizes LED.
2, white light is formed with blue-ray LED+red green fluorescence powder or blue-ray LED+yellow fluorescent powder.
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 there is important practical significance and commercial value to the research and development of white light LEDs novel material.
Summary of the invention
For above-mentioned existing White light LED technology Problems existing, 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 381.4~83.5%
SiO 216.2%
Eu 2O 30.3~2.4%；
The mass percent sum of each component is 100%.
The present invention provides a kind of method preparing described phosphor material powder on the other hand, and described method comprises:
Bismuth silicate (Bi will be formed 4si 3o 12) precursor material and doped raw material be dissolved in alcohol water mixed solvent by proportioning, stir, dry;
In air atmosphere, under the calcined temperature of 400 ~ 600 DEG C, carry out pre-burning, after cooling, take out grinding;
In air atmosphere, calcine under the calcining temperature of 750 ~ 900 DEG C, then furnace cooling is to room temperature, and grinds to form phosphor material powder.
In a preferred embodiment, bismuth silicate (Bi is formed 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, bismuth silicate (Bi is formed 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 drying is toasted 18 ~ 24 hours at 60 ~ 90 DEG C in an oven.
In one embodiment, be warmed up to calcined temperature by the temperature rise rate of 150 ~ 200 DEG C per hour, burn-in time is 1 ~ 3 hour.
In one embodiment, be warmed up to calcining temperature by the temperature rise rate of 150 ~ 200 DEG C per hour, calcination time is 3 ~ 5 hours.
Specifically, phosphor material powder that the present invention relates to a kind of burst of ultraviolel white light for white light LEDs and preparation method thereof.Be specifically related to one and prepare rare earth doped Eu 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) composition, and the mass percent of each composition is as follows:
Bi 2O 381.4~83.5%
SiO 216.2%
Eu 2O 30.3~2.4%；
The mass percent sum of above-mentioned each composition 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 doped raw material that form bismuth silicate is dissolved in alcohol water mixed solvent by proportioning, stirs, dry; Then first carry out pre-burning in 400 ~ 800 DEG C in air atmosphere, take out grinding, calcine in 750 ~ 900 DEG C in air atmosphere more afterwards; Last furnace cooling, to room temperature, takes out grinding.
As a kind of preferred version, the precursor material forming 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 forming 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 drying refer in 60 ~ 90 DEG C of baking ovens dry 18 ~ 24 hours.
As a kind of preferred version, be warmed up to calcined temperature by the temperature rise rate of 150 ~ 200 DEG C per hour, burn-in time is 1 ~ 3 hour.
As a kind of preferred version, be warmed up to calcining temperature by the temperature rise rate of 150 ~ 200 DEG C per hour, 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+blue light is launched under burst of ultraviolel, and Eu 3+replace Bi 3+itself feature blood orange light of rear transmitting, last both are compounded to form white light.
Experiment proves: 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, Eu is worked as 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, and showing 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 white light by blue light and blood orange photorecombination, and emission wavelength lays respectively at 472nm, 588nm, 593nm and 611nm.Compared with usual fluorescent material, it is simple that powder body material of the present invention not only has composition, and synthesis temperature is low, and raw material is cheap and easy to get, and preparation method is simple, without the need to specific installation, is applicable to suitability for industrialized production, has practicality, can meet the application requiring of White-light LED illumination.
Accompanying drawing explanation
The different Eu of the doping of Fig. 1 (a) obtained by the embodiment of the present invention 3+the emmission spectrum of bismuth silicate fluorescent material under normal temperature 260nm excites of concentration;
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, be denoted as " green ", " blueness " in Fig. 1 (b), " purple ", " orange ", " pink colour ", " redness " and " white " be not there is obvious boundary in order to represent between each district, between the region of their displays, there is transitional region.
Known from Fig. 1 (b), " 1 ", " 2 " and the region residing for " 3 " point are white portions.Because the distance in the close surrounding look district of each point is slightly different, it is visually also slightly different, concrete as shown in Fig. 1 (c) that the white presented is put in " 1 ", " 2 " and " 3 ".
Fig. 1 (c) is different Eu 3+concentration and the photo of pure bismuth silicate powder under UV-254nm excites.
Wherein, the sample being 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.Under the prerequisite not deviating from background of the present invention and spirit, those skilled in the art can carry out equivalencing and amendment 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
By folding synthesis oxide mass ratio be 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 that deionized water and dehydrated alcohol form, wherein, the total mass of constitutive material: deionized water quality: dehydrated alcohol quality=1.9:3:1; At room temperature stir after 1 hour and put into 90 DEG C of baking ovens bakings 18 hours.
Be 150 DEG C/h by temperature rise rate and be warmed up to 400 DEG C, at air atmosphere 400 DEG C, carry out pre-burning 1 hour, take out grinding.
Then, be 150 DEG C/h by temperature rise rate and be warmed up to 750 DEG C, calcine 3 hours at air atmosphere 750 DEG C; Furnace cooling is to room temperature; Take out grinding.
As seen from Figure 1: the transmitting peak position of the phosphor material powder obtained by embodiment 1 is at 472nm, 588nm, 593nm and 611nm, chromaticity coordinates position, as shown in 1 in Fig. 1 (b), is (0.308,0.321), is positioned at white light field.
Embodiment 2
By folding synthesis oxide mass ratio be 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 that deionized water and dehydrated alcohol form, the wherein total mass of constitutive material: deionized water quality: dehydrated alcohol quality=1.9:3:1; At room temperature stir after 2 hours and put into 80 DEG C of baking ovens bakings 20 hours.
Be 160 DEG C/h by temperature rise rate and be warmed up to 500 DEG C, 500 DEG C are carried out pre-burning 2 hours in air atmosphere, take out grinding.
Then, then be 160 DEG C/h by temperature rise rate and be warmed up to 800 DEG C, in air atmosphere 800 DEG C of calcinings 4 hours; Furnace cooling is to room temperature; Take out grinding.
As seen from Figure 1: detect the transmitting peak position of the phosphor material powder learnt obtained by embodiment 2 at 472nm, 588nm, 593nm and 611nm, chromaticity coordinates position, as shown in 2 in Fig. 1 (b), is (0.333,0.326), is positioned at white light field.
Embodiment 3
By folding synthesis oxide mass ratio be 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 that deionized water and dehydrated alcohol form, the wherein total mass of constitutive material: deionized water quality: dehydrated alcohol quality=1.9:3:1; At room temperature stir after 2 hours and put into 70 DEG C of baking ovens bakings 22 hours.
Be 170 DEG C/h by temperature rise rate and be warmed up to 600 DEG C, 600 DEG C are carried out pre-burning 3 hours in air atmosphere, take out grinding.
Then, then be 170 DEG C/h by temperature rise rate and be warmed up to 800 DEG C, in air atmosphere 800 DEG C of calcinings 5 hours; Furnace cooling is to room temperature; Take out grinding.
As seen from Figure 1: detect the transmitting peak position of the phosphor material powder learnt obtained by embodiment 3 at 472nm, 588nm, 593nm and 611nm, chromaticity coordinates position, as shown in 2 in Fig. 1 (b), is (0.333,0.326), is positioned at white light field.
Embodiment 4
By folding synthesis oxide mass ratio be 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 that deionized water and dehydrated alcohol form, the wherein total mass of constitutive material: deionized water quality: dehydrated alcohol quality=1.9:3:1; At room temperature stir after 2 hours and put into 60 DEG C of baking ovens bakings 24 hours.
Be 200 DEG C/h by temperature rise rate and be warmed up to 800 DEG C, 800 DEG C are carried out pre-burning 2 hours in air atmosphere, take out grinding.
Then, then be 200 DEG C/h by temperature rise rate and be warmed up to 900 DEG C, in air atmosphere 900 DEG C of calcinings 3 hours; Furnace cooling is to room temperature; Take out grinding.
As seen from Figure 1: detect the transmitting peak position of the phosphor material powder learnt obtained by embodiment 4 at 472nm, 588nm, 593nm and 611nm, chromaticity coordinates position, as shown in 3 in Fig. 1 (b), is (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 (9)

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+the bismuth silicate Bi of ion 4si 3o 12sill; 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;
Wherein, the preparation method of the phosphor material powder of the described burst of ultraviolel white light for white light LEDs comprises:
(1) bismuth silicate Bi will be formed 4si 3o 12precursor material and doped raw material be dissolved in alcohol water mixed solvent by proportioning, stir, dry;
(2) under the calcined temperature of 400 ~ 600 DEG C, carry out pre-burning in air atmosphere, after cooling, take out grinding;
(3) calcine under the calcining temperature of 750 ~ 900 DEG C in air atmosphere, then furnace cooling is to room temperature, and grinds to form phosphor material powder.
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 phosphor material powder is by bismuth oxide (Bi 2o 3), silicon-dioxide (SiO 2) and europium sesquioxide (Eu 2o 3) composition, wherein, the mass percent of each component is as follows:
Bi 2O 381.4～83.5％
SiO 216.2％
Eu 2O 30.3～2.4％；
The mass percent sum of each component is 100%.
3. prepare a method for phosphor material powder described in any one of claim 1-2, described phosphor material powder is doping Eu 3+the bismuth silicate Bi of ion 4si 3o 12sill; 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; Described method comprises:
Bismuth silicate Bi will be formed 4si 3o 12precursor material and doped raw material be dissolved in alcohol water mixed solvent by proportioning, stir, dry;
Under the calcined temperature of 400 ~ 600 DEG C, carry out pre-burning in air atmosphere, after cooling, take out grinding;
Calcine under the calcining temperature of 750 ~ 900 DEG C in air atmosphere, then furnace cooling is to room temperature, and grinds to form phosphor material powder.
4. method according to claim 3, is characterized in that: form bismuth silicate Bi 4si 3o 12precursor material be Bismuth trinitrate and tetraethoxy, described doped raw material is europium nitrate.
5. method according to claim 3, is characterized in that: described alcohol water mixed solvent is (4 ~ 6) by deionized water and dehydrated alcohol in mass ratio: 2 form.
6. method according to claim 3, is characterized in that: form bismuth silicate Bi 4si 3o 12precursor material and the total mass of doped raw material and the mass ratio of alcohol water mixed solvent be 6:(10 ~ 14).
7. method according to claim 3, is characterized in that: described drying is toasted 18 ~ 24 hours at 60 ~ 90 DEG C in an oven.
8. method according to claim 3, is characterized in that: be warmed up to calcined temperature by the temperature rise rate of 150 ~ 200 DEG C per hour, and burn-in time is 1 ~ 3 hour.
9. method according to claim 3, is characterized in that: be warmed up to calcining temperature by the temperature rise rate of 150 ~ 200 DEG C per hour, 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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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
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* Cited by examiner, † Cited by third party
Title
Synthesis and Luminescence Properties of Eu3+-doped Bi4Si3O12;ZHANG Yan et al.;《Journal of Inorganic Materials》;20111231;1341-1344 *
稀土元素( Ce 、Nd 和Eu) 掺杂Bi4Si3O12晶体的生长与性能;费一汀等;《人工晶体学报》;19990228;37-41 *

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