CN103450893B - A kind of white light LEDs nitrogenated silicon hydrochlorate yellow-green colour luminescent material and preparation thereof - Google Patents

A kind of white light LEDs nitrogenated silicon hydrochlorate yellow-green colour luminescent material and preparation thereof Download PDF

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CN103450893B
CN103450893B CN201310424182.0A CN201310424182A CN103450893B CN 103450893 B CN103450893 B CN 103450893B CN 201310424182 A CN201310424182 A CN 201310424182A CN 103450893 B CN103450893 B CN 103450893B
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黄维刚
齐智坚
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Sichuan University
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Abstract

The present invention relates to a kind of nitrogenated silicon hydrochlorate sosoloid based luminescent material and autoreduction preparation method thereof of novel divalent europium doping.The chemical constitution of this luminescent material can be expressed as: Ca 3si 3(O 9-xn x): Eu 2+.Preparation method adopts two-step approach, and (1) sol-gel method prepares Ca 2siO 4: Eu 3+product.(2) Ca 2siO 4: Eu 3+with the roasting under non-reducing atmosphere of silicon nitride mixture, utilize Si 3n 4autoreduction obtain final product.Raw materials used is nitrocalcite (CaN 2o 64H 2o), europium nitrate (EuN 3o 96H 2o), tetraethoxy (C 8h 20o 4and Si Si) 3n 4.This luminescent material has broadband (300 ~ 450nm) to absorb near ultraviolet to blue light, launches yellow-green light (534 ~ 544nm).Products therefrom luminous intensity is high, stable performance.Preparation process only just can need complete under nitrogen protection atmosphere, and without the need to reducing atmosphere and other reduction means, preparation method is simple, safety.

Description

A kind of white light LEDs nitrogenated silicon hydrochlorate yellow-green colour luminescent material and preparation thereof
Technical field
The invention belongs to rare earth luminescent material field.In particular 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 a feature such as energy-conservation.Be widely used in city illumination, the lighting field such as electronics, automobile.Wherein White-light LED illumination accounts for about 50% of whole LED.The green energy resource of development to energy-conserving and environment-protective of LED light source is significant.
The approach realizing the LED of white light at present is mainly obtained by fluorescent material conversion regime, the combination that common are blue-light LED chip and yellow fluorescent powder obtains white light, and another kind adopts the fluorescent material of ultraviolet or near ultraviolet LED chip and RGB powder mix or single-matrix to obtain.At present for the numerous types of LED fluorescent powder, mainly concentrate on Eu 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, generally about about 1600 DEG C, which has limited its application.Wherein silicate luminescent material is because raw material sources are easy, cost is low, preparation condition is suitable and come into one's own.
The preparation method of silicate luminescent material mainly adopts solid phase method and sol-gel method etc., and doping Eu 2+fluorescent material must by certain reduction mode by Eu in preparation process 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 object of this invention is to provide a kind of novel rare-earth Eu combined with near-ultraviolet light LED chip 2+the nitrogenated silicon hydrochlorate sosoloid base yellow-green colour luminescent material for white light LEDs of doping, significantly improves the luminous intensity of gained luminescent material by the nitrogen-atoms of solid solution in silicate substrate.
Present invention also offers a kind of autoreduction adopting silicon nitride, under the condition of no hydrogen reductive action, obtain Eu 2+the preparation method of the nitrogenated silicon hydrochlorate sosoloid based luminescent material of doping.The method is simple, and safety, 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 of white light LEDs that the present invention proposes 3si 3(O 9-xn x): Eu 2+preparation method comprise following characteristics and step:
(1) dissolve gel method and prepare 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, and wherein silicon nitride comprises the powder (micron order, submicron order and nano level) of different grain size rank.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 (volume ratio of alcohol and water is 1 ~ 3:1) in the mixed solution of a certain proportion of alcohol and water, stir and form the mixed solution of nitrocalcite and europium nitrate, then the pH value of regulator solution is to 2 ~ 4, adds C 8h 20o 4si, stirs 2 hours, forms the colloidal sol of clarification.The water-bath of colloidal sol being put into 50 ~ 80 DEG C is heated 3 ~ 6 hours, forms transparent xerogel.Xerogel drying at 100 ~ 120 DEG C, after at least 12 hours, is namely obtained required presoma.
2. put into crucible after being ground by the presoma of oven dry, in resistance furnace, in 1100 DEG C of roastings under air ambient, be incubated after 2 hours and cool with stove, obtain Ca 2siO 4: Eu 3+silicate product.
(2) Ca 3si 3(N xo 9-x): Eu 2+preparation
1. by the Ca after roasting 2siO 4: Eu 3+mix in ball mill with beta-silicon nitride powder after product grinding, Ca 2siO 4: Eu 3+be 1:y (0.4≤y≤1.2) with the mol ratio of silicon nitride, wherein y is the mole number of silicon nitride.Mixed raw material is put into tube furnace, and in 1200-1400 DEG C of calcining 2 hours under high pure nitrogen (purity >=99.99%) atmosphere that flow is 70 ~ 150ml/min, then furnace cooling is to less than 300 DEG C, takes out product.The product of acquisition is ground, namely obtains Ca 3si 3(O 9-xn x): Eu 2+fluorescent material.
Feature of the present invention and beneficial effect:
(1) the nitrogenated silicon hydrochlorate solid solution luminescent material prepared by preparation method provided by the present invention has wide band absorption near ultraviolet to blue wavelength range (300 ~ 450nm), launch yellow-green light (534 ~ 544nm), can well for 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 adopts silicon nitride to reduce trivalent Eu at a certain temperature 3+autoreduction, make Eu 3+be reduced to Eu 2+, this preparation method is simple, safety.
(3), in preparation method provided by the invention, silicon nitride is utilized 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.
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 one 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 4and europium nitrate (EuN Si) 3o 96H 2o).The volumetric ratio first nitrocalcite and europium nitrate being dissolved in dehydrated alcohol and water is in the mixed solution of 3:1, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 2.The tetraethoxy taken is added in the solution modulated, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 60 DEG C and within 4 hours, obtains dry colloid, xerogel to be put in loft drier at 120 DEG C into drying 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours after presoma 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 4mix put into tube furnace under flow is 70ml/min nitrogen atmosphere in 1200 DEG C burn 2 hours, obtain Ca after furnace cooling 3si 3(O 4.52n 4.47): Eu 2+luminescent powder material.
Implement example two and take nitrocalcite (CaN according to the ratio that the mol ratio of Ca:Si:Eu is 1.96:2:0.4 2o 64H 2o), tetraethoxy (C 8h 20o 4and europium nitrate (EuN Si) 3o 96H 2o).First nitrocalcite and europium nitrate being dissolved in volume ratio is in the dehydrated alcohol of 3:1 and the mixed solution of water, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 2.The tetraethoxy taken is added in modified good solution, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 60 DEG C the colloid obtaining for 4 hours doing, then to put in loft drier at 120 DEG C drying into 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours to after presoma grinding, 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 4mixing and putting into tube furnace is burn 2 hours in 1300 DEG C under the nitrogen atmosphere of 100ml/min at flow, obtains Ca after furnace cooling 3si 3(O 4.52n 4.47): Eu 2+luminescent powder material.
Implement example three and take nitrocalcite (CaN according to the ratio that the mol ratio of Ca:Si:Eu is 1.96:2:0.4 2o 64H 2o), tetraethoxy (C 8h 20o 4and europium nitrate (EuN Si) 3o 96H 2o).First nitrocalcite and europium nitrate being dissolved in volume ratio is in the dehydrated alcohol of 3:1 and the mixed solution of water, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 2.The tetraethoxy taken is added in modified good solution, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 60 DEG C the colloid obtaining for 4 hours doing, then to put in loft drier at 120 DEG C drying into 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours to after presoma grinding, 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 4mixing and putting into tube furnace is burn 2 hours in 1400 DEG C under the nitrogen atmosphere of 70ml/min at flow, obtains Ca after furnace cooling 3si 3(O 4.52n 4.47): Eu 2+luminescent powder material.
Implement example four and take nitrocalcite (CaN according to the ratio that the mol ratio of Ca:Si:Eu is 1.96:2:0.4 2o 64H 2o), tetraethoxy (C 8h 20o 4and europium nitrate (EuN Si) 3o 96H 2o).First nitrocalcite and europium nitrate being dissolved in volume ratio is in the dehydrated alcohol of 3:1 and the mixed solution of water, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 2.The tetraethoxy taken is added in modified good solution, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 60 DEG C the colloid obtaining for 4 hours doing, then to put in loft drier at 120 DEG C drying into 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours to after presoma grinding, 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 4mixing and putting into tube furnace is burn 2 hours in 1400 DEG C under the nitrogen atmosphere of 100ml/min at flow, obtains Ca after furnace cooling 3si 3(O 6n 3): Eu 2+luminescent powder material.
Implement example five and take nitrocalcite (CaN according to the ratio that the mol ratio of Ca:Si:Eu is 1.96:2:0.4 2o 64H 2o), tetraethoxy (C 8h 20o 4and europium nitrate (EuN Si) 3o 96H 2o).First nitrocalcite and europium nitrate being dissolved in volume ratio is in the dehydrated alcohol of 4:1 and the mixed solution of water, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 2.The tetraethoxy taken is added in modified good solution, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 60 DEG C the colloid obtaining for 4 hours doing, then to put in loft drier at 120 DEG C drying into 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours to after presoma grinding, 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 4mixing and putting into tube furnace is burn 2 hours in 1400 DEG C under the nitrogen atmosphere of 130ml/min at flow, obtains Ca after furnace cooling 3si 3(O 5.51n 3.49): Eu 2+luminescent powder material.
Implement example six and take nitrocalcite (CaN according to the ratio that the mol ratio of Ca:Si:Eu is 1.96:2:0.4 2o 64H 2o), tetraethoxy (C 8h 20o 4and europium nitrate (EuN Si) 3o 96H 2o).First nitrocalcite and europium nitrate being dissolved in volume ratio is in the dehydrated alcohol of 3:1 and the mixed solution of water, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 2.The tetraethoxy taken is added in modified good solution, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 60 DEG C the colloid obtaining for 4 hours doing, then to put in loft drier at 120 DEG C drying into 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours to after presoma grinding, 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 4mixing and putting into tube furnace is burn 2 hours in 1400 DEG C under the nitrogen atmosphere of 150ml/min at flow, obtains Ca after furnace cooling 3si 3(O 5.02n 3.98): Eu 2+luminescent powder material.
Implement example seven and take nitrocalcite (CaN according to the ratio that the mol ratio of Ca:Si:Eu is 1.96:2:0.4 2o 64H 2o), tetraethoxy (C 8h 20o 4and europium nitrate (EuN Si) 3o 96H 2o).First nitrocalcite and europium nitrate being dissolved in volume ratio is in the dehydrated alcohol of 4:1 and the mixed solution of water, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 2.The tetraethoxy taken is added in modified good solution, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 80 DEG C the colloid obtaining for 4 hours doing, then to put in loft drier at 120 DEG C drying into 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours to after presoma grinding, 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 4mixing and putting into tube furnace is burn 2 hours in 1400 DEG C under the nitrogen atmosphere of 150ml/min at flow, obtains Ca after furnace cooling 3si 3(O 4.04n 4.96): Eu 2+luminescent powder material.
Implement example eight and take nitrocalcite (CaN according to the ratio that the mol ratio of Ca:Si:Eu is 1.96:2:0.4 2o 64H 2o), tetraethoxy (C 8h 20o 4and europium nitrate (EuN Si) 3o 96H 2o).First nitrocalcite and europium nitrate being dissolved in volume ratio is in the dehydrated alcohol of 2:1 and the mixed solution of water, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 2.5.The tetraethoxy taken is added in modified good solution, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 60 DEG C the colloid obtaining for 4 hours doing, then to put in loft drier at 120 DEG C drying into 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours to after presoma grinding, 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+with α-Si 3n 4mixing and putting into tube furnace is burn 2 hours in 1400 DEG C under the nitrogen atmosphere of 100ml/min at flow, obtains Ca after furnace cooling 3si 3(O 4.53n 4.47): Eu 2+luminescent powder material.
Implement example nine and take nitrocalcite (CaN according to the ratio that the mol ratio of Ca:Si:Eu is 1.96:2:0.4 2o 64H 2o), tetraethoxy (C 8h 20o 4and europium nitrate (EuN Si) 3o 96H 2o).First nitrocalcite and europium nitrate being dissolved in volume ratio is in the dehydrated alcohol of 1:1 and the mixed solution of water, is stirred to nitrocalcite and europium nitrate is uniformly dissolved, and then the pH value of regulator solution is to 3.The tetraethoxy taken is added in modified good solution, stir the colloidal sol obtaining for 2 hours clarifying, colloidal sol heat in the water-bath of 80 DEG C the colloid obtaining for 4 hours doing, then to put in loft drier at 120 DEG C drying into 12 hours, obtain presoma.Put into resistance furnace 1100 DEG C calcining 2 hours to after presoma grinding, 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+with α-Si 3n 4mixing and putting into tube furnace is burn 2 hours in 1400 DEG C under the nitrogen atmosphere of 150ml/min at flow, obtains Ca after furnace cooling 3si 3(O 4.53n 4.47): Eu 2+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+, wherein 3≤x≤5.
2. a method for the luminescent material described in manufacturing claims 1, is characterized in that, processing step is:
(1) by chemical formula Ca 2siO 4: Eu 3+take the nitrocalcite of aequum, europium nitrate, tetraethoxy; Nitrocalcite and europium nitrate are dissolved in alcohol and water volume ratio is in the mixed solution of 3 ~ 1:1, stir formation mixed solution, the pH value of regulator solution is to 2 ~ 4, add tetraethoxy, stir 2 hours, form the colloidal sol of clarification, gained colloidal sol heats 3 ~ 6 hours in the water-bath of 50 ~ 80 DEG C, form xerogel, then xerogel to be put at the temperature of 100 ~ 120 DEG C, loft drier inherence drying at least 12 hours, after drying, obtain presoma; By presoma 1100 DEG C little roastings 2 hours, obtain Ca 2siO 4: Eu 3+product; (2) by Ca 2siO 4: Eu 3+: Si 3n 4mol ratio be that the ratio of 1:y takes Ca 2siO 4: Eu 3+and Si 3n 4, wherein y value scope is 0.4≤y≤1.2; By Ca 2siO 4: Eu 3+and Si 3n 4put into tube furnace after mixing in ball mill, in nitrogen atmosphere, in 1200 ~ 1400 DEG C of roastings 2 hours, then furnace cooling was to less than 300 DEG C, obtains Ca 3si 3(O 9-xn x): Eu 2+fluorescent material.
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CN105038779B (en) * 2015-07-24 2017-09-26 南昌大学 A kind of Eu3+/Eu2+The aluminate multicolor fluorescence material and preparation method of doping
CN105802616B (en) * 2016-04-15 2018-07-03 江苏博睿光电有限公司 A kind of preparation method of silicate yellowish green fluorescent powder

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