CN103450893A - Nitrogenous silicate yellow green luminescent material for white light LED (light-emitting diode) and preparation thereof - Google Patents
Nitrogenous silicate yellow green luminescent material for white light LED (light-emitting diode) and preparation thereof Download PDFInfo
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- CN103450893A CN103450893A CN2013104241820A CN201310424182A CN103450893A CN 103450893 A CN103450893 A CN 103450893A CN 2013104241820 A CN2013104241820 A CN 2013104241820A CN 201310424182 A CN201310424182 A CN 201310424182A CN 103450893 A CN103450893 A CN 103450893A
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Abstract
The invention relates to a novel divalent europium doped nitrogenous silicate solid solution base luminescent material and a self reduction preparation method. The chemical composition of the luminescent material is shown as follows: Ca3Si3 (O9-xNx):Eu<2+>. The preparation method comprises two steps of (1) preparing a Ca2SiO4:Eu<3+> product through a sol-gel method; (2) roasting the Ca2SiO4:Eu<3+> product and a silicon nitride mixture in a non reducing atmosphere, thus obtaining the final product by the self reducing action of the Si3N4, wherein the used materials comprise calcium nitrate (CaN2O6.4H2O), europium nitrate (EuN3O9.6H2O), ethyl orthosilicate (C8H20O4Si), and Si3N4. The luminescent material has broad band (300-450nm) to absorb near ultraviolet and blue light and gives out yellow green light (534-544nm). The obtained product has high light intensity and has stable properties. The preparation process can be finished only in protection atmosphere of nitrogen and needs no other reduction atmosphere and other reduction methods, so that the preparation method is simple and safe.
Description
Technical field
The invention belongs to rare earth luminescent material field.Be particularly related to a kind of nitrogenated silicon hydrochlorate sosoloid base yellow-green colour luminescent material and autoreduction preparation method thereof of the novel divalent europium doping for white light LEDs.
Background technology
LED is considered to the new high-efficiency light source of 21 century, has that the life-span is long, luminous efficiency is high, environmental protection and characteristics such as energy-conservation.The lighting fields such as city illumination, electronics, automobile have been widely used in.Wherein White-light LED illumination accounts for approximately 50% of whole LED.The development of LED light source is significant to the green energy resource of energy-conserving and environment-protective.
The approach that realizes at present the LED of white light is mainly to obtain by the fluorescent material conversion regime, the combination that common are blue-light LED chip and yellow fluorescent powder obtains white light, and another kind is to adopt the fluorescent material of ultraviolet or near ultraviolet LED chip and RGB powder mix or single-matrix to obtain.For the numerous types of LED fluorescent material, mainly concentrate on Eu at present
2+and Ce
3+the aluminate-series of ion doping, sulfide-based, molybdate series, tungstate, silicate, nitride and oxynitride etc.Nitride based and silicate luminescent material has the advantages such as physicochemical property are stable, ultraviolet resistance bombardment, pollution-free, phototranstormation efficiency height and width spectrum excites.Because the luminescent material preparation condition of nitride substrate is very harsh, synthesis temperature is very high, and generally about 1600 ℃ of left and right, this has limited its application.Wherein the silicate luminescent material comes into one's own because raw material sources are easy, cost is low, preparation condition is suitable.
The preparation method of silicate luminescent material mainly adopts solid phase method and sol-gel method etc., and doping Eu
2+fluorescent material must be by certain reduction mode in preparation process by Eu
3+be reduced into Eu
2+, as hydrogen reducing, ammonia reduction or carbon reducing agent etc.These methods are both inconvenient, also dangerous.
Summary of the invention
The purpose of this invention is to provide novel rare-earth the Eu a kind of and combination of near-ultraviolet light LED chip
2+nitrogenated silicon for the white light LEDs hydrochlorate sosoloid base yellow-green colour luminescent material of doping, significantly improved the luminous intensity of gained luminescent material by the nitrogen-atoms of solid solution in silicate substrate.
The present invention also provides a kind of autoreduction that adopts silicon nitride, under the condition of no hydrogen reductive action, obtains Eu
2+the preparation method of the nitrogenated silicon hydrochlorate sosoloid based luminescent material of doping.The method is simple, safety, and luminous intensity is high.
The chemical constitution of nitrogenated silicon hydrochlorate sosoloid based luminescent material of the present invention can be expressed as:
Ca
3Si
3(O
9-xN
x):Eu
2+
In formula, 3≤x≤5
The Yellow luminous material C a for white light LEDs that the present invention proposes
3si
3(O
9-xn
x): Eu
2+the preparation method comprise following characteristics and step:
(1) dissolve gel method and prepare the silicate precursor
1. with nitrocalcite (CaN
2o
64H
2o), europium nitrate (EuN
3o
96H
2o) tetraethoxy (C
8h
20o
4si), silicon nitride is raw material, wherein silicon nitride comprises other powder of different grain size level (micron order, submicron order and nano level).First according to Ca
2siO
4: Eu
3+stoichiometric ratio take corresponding raw material, by CaN
2o
64H
2o and EuN
3o
96H
2o is dissolved in the mixed solution of a certain proportion of alcohol and water (volume ratio of alcohol and water is 1 ~ 3:1), and stir and form the mixed solution of nitrocalcite and europium nitrate, then the pH value to 2 of regulator solution ~ 4, add C
8h
20o
4si, stir 2 hours, forms the colloidal sol of clarification.The water-bath that colloidal sol is put into to 50 ~ 80 ℃ is heated 3 ~ 6 hours, forms transparent xerogel.Xerogel drying under 100 ~ 120 ℃, after at least 12 hours, is obtained to required presoma.
2. after the presoma of oven dry being ground, put into crucible, in resistance furnace, in 1100 ℃ of roastings, cooling with stove after being incubated 2 hours under air ambient, obtain Ca
2siO
4: Eu
3+the silicate product.
(2) Ca
3si
3(N
xo
9-x): Eu
2+preparation
1. by the Ca after roasting
2siO
4: Eu
3+product mixes in ball mill with beta-silicon nitride powder after grinding, Ca
2siO
4: Eu
3+with the mol ratio of silicon nitride be 1:y (0.4≤y≤1.2), the mole number that wherein y is silicon nitride.Mixed raw material is put into to tube furnace, under the high pure nitrogen that is 70 ~ 150ml/min at flow (purity >=99.99%) atmosphere, in 1200-1400 ℃ of calcining 2 hours, then, below furnace cooling to 300 ℃, take out product.The product of acquisition is ground, obtained Ca
3si
3(O
9-xn
x): Eu
2+fluorescent material.
Characteristics of the present invention and beneficial effect:
(1) the prepared nitrogenated silicon hydrochlorate solid solution luminescent material of preparation method provided by the present invention has wide band absorption near ultraviolet to blue light wavelength scope (300 ~ 450nm), launch yellow-green light (534 ~ 544nm), can be well for the white light LEDs changing luminous material, luminous intensity is high.
(2) preparation method provided by the invention, without any need for reducing atmosphere, as the reductive action of hydrogen, carbon monoxide, ammonia, and adopt silicon nitride to reduce at a certain temperature trivalent Eu
3+autoreduction, make Eu
3+be reduced to Eu
2+, this preparation method is simple, safety.
(3), in preparation method provided by the invention, utilize silicon nitride to obtain nitrogenous silicate solid solution Ca at pyrogenetic decomposition
3si
3(O
9-xn
x): Eu
2+fluorescent material, and luminescent properties significantly improves.
The accompanying drawing explanation
Fig. 1 Ca
3si
3(O
9-xn
x): Eu
2+xRD figure spectrum
Fig. 2 Ca
3si
3(O
9-xn
x): Eu
2+emmission spectrum
Fig. 3 Ca
3si
3(O
9-xn
x): Eu
2+excitation spectrum
Embodiment
The ratio that embodiment mono-is 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).In the mixed solution that the volumetric ratio that first nitrocalcite and europium nitrate is dissolved in to dehydrated alcohol and water is 3:1, be stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 2 of regulator solution.The tetraethoxy taken is added in the solution modulated, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 60 ℃, put in loft drier under 120 ℃ xerogel into drying 12 hours, obtain presoma.Presoma is put into 1100 ℃ of calcinings of resistance furnace 2 hours after grinding, obtain Ca
2siO
4: Eu
3+product.Ca2SiO4:Eu in molar ratio
3+: Si
3n
4for the ratio of 1:1 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and Si
3n
4mixing and putting into tube furnace is to burn 2 hours in 1200 ℃ under the 70ml/min nitrogen atmosphere at flow, obtains Ca after furnace cooling
3si
3(O
4.52n
4.47): Eu
2+the luminescent powder material.
The ratio that to implement example two be 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).First nitrocalcite and europium nitrate are dissolved in the mixed solution of dehydrated alcohol that volume ratio is 3:1 and water, are stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 2 of regulator solution.The tetraethoxy taken is added in modified good solution, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 60 ℃, then put in loft drier under 120 ℃ drying into 12 hours, obtain presoma.Put into 1100 ℃ of calcinings of resistance furnace 2 hours after presoma is ground, obtain Ca
2siO
4: Eu
3+powder.Ca in molar ratio
2siO
4: Eu
3+: Si
3n
4for the ratio of 1:1 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and Si
3n
4mix to put under the nitrogen atmosphere that tube furnace is 100ml/min at flow in 1300 ℃ and burn 2 hours, obtain Ca after furnace cooling
3si
3(O
4.52n
4.47): Eu
2+the luminescent powder material.
The ratio that to implement example three be 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).First nitrocalcite and europium nitrate are dissolved in the mixed solution of dehydrated alcohol that volume ratio is 3:1 and water, are stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 2 of regulator solution.The tetraethoxy taken is added in modified good solution, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 60 ℃, then put in loft drier under 120 ℃ drying into 12 hours, obtain presoma.Put into 1100 ℃ of calcinings of resistance furnace 2 hours after presoma is ground, obtain Ca
2siO
4: Eu
3+powder.Ca in molar ratio
2siO
4: Eu
3+: Si
3n
4for the ratio of 1:1 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and Si
3n
4mix to put under the nitrogen atmosphere that tube furnace is 70ml/min at flow in 1400 ℃ and burn 2 hours, obtain Ca after furnace cooling
3si
3(O
4.52n
4.47): Eu
2+the luminescent powder material.
The ratio that to implement example four be 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).First nitrocalcite and europium nitrate are dissolved in the mixed solution of dehydrated alcohol that volume ratio is 3:1 and water, are stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 2 of regulator solution.The tetraethoxy taken is added in modified good solution, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 60 ℃, then put in loft drier under 120 ℃ drying into 12 hours, obtain presoma.Put into 1100 ℃ of calcinings of resistance furnace 2 hours after presoma is ground, obtain Ca
2siO
4: Eu
3+powder.Ca in molar ratio
2siO
4: Eu
3+: Si
3n
4for the ratio of 1:0.4 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and Si
3n
4mix to put under the nitrogen atmosphere that tube furnace is 100ml/min at flow in 1400 ℃ and burn 2 hours, obtain Ca after furnace cooling
3si
3(O
6n
3): Eu
2+the luminescent powder material.
The ratio that to implement example five be 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).First nitrocalcite and europium nitrate are dissolved in the mixed solution of dehydrated alcohol that volume ratio is 4:1 and water, are stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 2 of regulator solution.The tetraethoxy taken is added in modified good solution, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 60 ℃, then put in loft drier under 120 ℃ drying into 12 hours, obtain presoma.Put into 1100 ℃ of calcinings of resistance furnace 2 hours after presoma is ground, obtain Ca
2siO
4: Eu
3+powder.Ca in molar ratio
2siO
4: Eu
3+: Si
3n
4for the ratio of 1:0.6 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and Si
3n
4mix to put under the nitrogen atmosphere that tube furnace is 130ml/min at flow in 1400 ℃ and burn 2 hours, obtain Ca after furnace cooling
3si
3(O
5.51n
3.49): Eu
2+the luminescent powder material.
The ratio that to implement example six be 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).First nitrocalcite and europium nitrate are dissolved in the mixed solution of dehydrated alcohol that volume ratio is 3:1 and water, are stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 2 of regulator solution.The tetraethoxy taken is added in modified good solution, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 60 ℃, then put in loft drier under 120 ℃ drying into 12 hours, obtain presoma.Put into 1100 ℃ of calcinings of resistance furnace 2 hours after presoma is ground, obtain Ca
2siO
4: Eu
3+powder.Get x=3.98, in molar ratio Ca
2siO
4: Eu
3+: Si
3n
4for the ratio of 1:0.8 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and Si
3n
4mix to put under the nitrogen atmosphere that tube furnace is 150ml/min at flow in 1400 ℃ and burn 2 hours, obtain Ca after furnace cooling
3si
3(O
5.02n
3.98): Eu
2+the luminescent powder material.
The ratio that to implement example seven be 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).First nitrocalcite and europium nitrate are dissolved in the mixed solution of dehydrated alcohol that volume ratio is 4:1 and water, are stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 2 of regulator solution.The tetraethoxy taken is added in modified good solution, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 80 ℃, then put in loft drier under 120 ℃ drying into 12 hours, obtain presoma.Put into 1100 ℃ of calcinings of resistance furnace 2 hours after presoma is ground, obtain Ca
2siO
4: Eu
3+powder.Ca in molar ratio
2siO
4: Eu
3+: Si
3n
4for the ratio of 1:1.2 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and Si
3n
4mix to put under the nitrogen atmosphere that tube furnace is 150ml/min at flow in 1400 ℃ and burn 2 hours, obtain Ca after furnace cooling
3si
3(O
4.04n
4.96): Eu
2+the luminescent powder material.
The ratio that to implement example eight be 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).First nitrocalcite and europium nitrate are dissolved in the mixed solution of dehydrated alcohol that volume ratio is 2:1 and water, are stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 2.5 of regulator solution.The tetraethoxy taken is added in modified good solution, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 60 ℃, then put in loft drier under 120 ℃ drying into 12 hours, obtain presoma.Put into 1100 ℃ of calcinings of resistance furnace 2 hours after presoma is ground, obtain Ca
2siO
4: Eu
3+powder.Get x=4.47, in molar ratio Ca
2siO
4: Eu
3+: Si
3n
4for the ratio of 1:1 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and α-Si
3n
4mix to put under the nitrogen atmosphere that tube furnace is 100ml/min at flow in 1400 ℃ and burn 2 hours, obtain Ca after furnace cooling
3si
3(O
4.53n
4.47): Eu
2+the luminescent powder material.
The ratio that to implement example nine be 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes nitrocalcite (CaN
2o
64H
2o), tetraethoxy (C
8h
20o
4si) and europium nitrate (EuN
3o
96H
2o).First nitrocalcite and europium nitrate are dissolved in the mixed solution of dehydrated alcohol that volume ratio is 1:1 and water, are stirred to nitrocalcite and europium nitrate is uniformly dissolved, then the pH value to 3 of regulator solution.The tetraethoxy taken is added in modified good solution, stirred the colloidal sol that obtains clarification in 2 hours, colloidal sol heat and within 4 hours, obtains dry colloid in the water-bath of 80 ℃, then put in loft drier under 120 ℃ drying into 12 hours, obtain presoma.Put into 1100 ℃ of calcinings of resistance furnace 2 hours after presoma is ground, obtain Ca
2siO
4: Eu
3+powder.Ca in molar ratio
2siO
4: Eu
3+: Si
3n
4for the ratio of 1:1 takes Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and α-Si
3n
4mix to put under the nitrogen atmosphere that tube furnace is 150ml/min at flow in 1400 ℃ and burn 2 hours, obtain Ca after furnace cooling
3si
3(O
4.53n
4.47): Eu
2+the luminescent powder material.
Claims (2)
1. a rear-earth-doped nitrogenated silicon hydrochlorate sosoloid base yellow-green colour luminescent material, its chemical constitution can be expressed as:
Ca
3Si
3(O
9-xN
x):Eu
2+
3≤x in formula≤5.
2. luminescent material according to claim 1 adopts two step process of preparings, its processing step:
(1) sol-gel method prepares Ca
2siO
4: Eu
3+product.(2) Ca
2siO
4: Eu
3+with the roasting of silicon nitride mixture, under non-reduced atmosphere, utilize Si
3n
4autoreduction, obtain Ca
3si
3(O
9-xn
x): Eu
2+.The concrete technology method is as follows:
(A) Ca
2siO
4: Eu
3+the preparation of fluorescent material
1. with nitrocalcite (CaN
2o
64H
2o), europium nitrate (EuN
3o
96H
2o), tetraethoxy (C
8h
20o
4si) be raw material.The ratio that is 1.96:2:0.4 according to the mol ratio of Ca:Si:Eu takes corresponding raw material.
2. by CaN
2o
64H
2o and EuN
3o
96H
2o is dissolved in the mixed solution of alcohol and water (volume ratio of alcohol and water is 3 ~ 1:1), stirs and forms the mixed solution of nitrocalcite and europium nitrate.
3. the 2. pH value to 2 of gained mixing solutions ~ 4 of control method, add C
8h
20o
4si, stir 2 hours, forms the colloidal sol of clarification.
4. gained colloidal sol heats 3 ~ 6 hours in the water-bath of 50 ℃ ~ 80 ℃, forms xerogel, then xerogel is put at inherent 100 ℃ ~ 120 ℃ temperature of loft drier to drying at least 12 hours, obtains presoma after dry.
5. by presoma 1100 ℃ little roastings 2 hours, obtain Ca
2siO
4: Eu
3+product.
(B) utilize the silicon nitride autoreduction, preparation Ca
3si
3(O
9-xn
x): Eu
2+fluorescent material
Press Ca
2siO
4: Eu
3+: Si
3n
4mol ratio, 1:y (0.4≤y≤1.2), the molar fraction that y is silicon nitride, ratio take Ca
2siO
4: Eu
3+and Si
3n
4, by Ca
2siO
4: Eu
3+and Si
3n
4put into tube furnace after mixing in ball mill, in the nitrogen atmosphere of certain flow, burn 2 hours in 1200 ~ 1400 ℃, then, below furnace cooling to 300 ℃, obtain Ca
3si
3(O
9-xn
x): Eu
2+fluorescent material.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103865529A (en) * | 2014-03-07 | 2014-06-18 | 四川大学 | Nitrogen-containing silicate green luminescent material for white LED (light-emitting diode) and preparation method |
CN103964691A (en) * | 2014-05-15 | 2014-08-06 | 天津理工大学 | Fluorescent glass ceramic material and preparation method thereof |
CN105038779A (en) * | 2015-07-24 | 2015-11-11 | 南昌大学 | Eu3+/Eu2 doped aluminate multicolor fluorescent material and preparing method thereof |
CN105802616A (en) * | 2016-04-15 | 2016-07-27 | 江苏博睿光电有限公司 | Preparation method of yellow green silicate phosphor |
-
2013
- 2013-09-18 CN CN201310424182.0A patent/CN103450893B/en not_active Expired - Fee Related
Non-Patent Citations (2)
Title |
---|
BONG-GOO YUN ET. AL.: "Preparation and Luminescence Properties of SrSi2O2N2: Eu2+ Phosphors for White LEDs", 《JOURNAL OF THE CERAMIC SOCIETY OF JAPAN》 * |
YI-CHEN CHIU ET. AL.: "Eu2+-activated silicon-oxynitride Ca3Si2O4N2: a green-emitting phosphor for white LEDs", 《OPTICS EXPRESS》 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103865529A (en) * | 2014-03-07 | 2014-06-18 | 四川大学 | Nitrogen-containing silicate green luminescent material for white LED (light-emitting diode) and preparation method |
CN103865529B (en) * | 2014-03-07 | 2015-06-10 | 四川大学 | Nitrogen-containing silicate green luminescent material for white LED (light-emitting diode) and preparation method |
CN103964691A (en) * | 2014-05-15 | 2014-08-06 | 天津理工大学 | Fluorescent glass ceramic material and preparation method thereof |
CN103964691B (en) * | 2014-05-15 | 2016-01-06 | 天津理工大学 | A kind of fluorescent glass stupalith and preparation method thereof |
CN105038779A (en) * | 2015-07-24 | 2015-11-11 | 南昌大学 | Eu3+/Eu2 doped aluminate multicolor fluorescent material and preparing method thereof |
CN105802616A (en) * | 2016-04-15 | 2016-07-27 | 江苏博睿光电有限公司 | Preparation method of yellow green silicate phosphor |
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