CN103468250B - Preparation method of co-doped silicate green fluorescent powder used for LEDs - Google Patents

Preparation method of co-doped silicate green fluorescent powder used for LEDs Download PDF

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CN103468250B
CN103468250B CN201310449327.2A CN201310449327A CN103468250B CN 103468250 B CN103468250 B CN 103468250B CN 201310449327 A CN201310449327 A CN 201310449327A CN 103468250 B CN103468250 B CN 103468250B
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salt
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ball milling
fluorescent powder
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CN103468250A (en
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朱达川
罗林龄
涂铭旌
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Sichuan University
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Abstract

The invention discloses a preparation method of co-doped silicate green fluorescent powder used for LEDs, and belongs to the technical field of luminescent materials. The chemical formula of the co-doped silicate green fluorescent powder is , wherein 0<=x<=0.25, 0<y<=0.02 and 0<z<=0.1. The method includes the specific steps that according to the stoichiometric ratio of all the elements in the chemical formula, barium salt, silica, europium salt, lithium salt, erbium salt and a moderate amount of surfactant are weighed; the weighed barium salt, the weighed lithium salt, the weighed silica, the weighed europium salt, the weighed erbium salt and the weighed surfactant are fully mixed with a moderated amount of ligand, ball milling is performed for a certain time at room temperature, and a moderated amount of lubricant is added in the ball milling process; drying is directly performed, and a precursor is obtained; the precursor is placed in an atmosphere furnace with reducing atmosphere and calcined at 1000-1300 DEG C for 2-7 hours, and the needed fluorescent powder is obtained. The fluorescent powder prepared with the method and used for the LEDs prepared with the method is good in crystallinity, loosened in structure, fine in particulate, uniform in distribution, good in coating performance and applicable to exciting near ultraviolet radiation InGaN tube cores.

Description

A kind of preparation method of silicate green fluorescent powder of LED codoped
Technical field
The invention belongs to LED luminescent material preparing technical field, be specifically related to a kind of preparation method of silicate green fluorescent powder of LED codoped.
Background technology
Rare-earth ion activated alkaline-earth silicate is the important luminescent material of a class, silicates material is as luminescent ceramic matrix, luminescence center and matrix interaction energy lower, luminescent center ion can be made directly to absorb excitation energy, be conducive to improving luminous efficiency, and there is good luminosity, chemical stability and thermostability, its excitation spectrum is wider, can by ultraviolet, near ultraviolet, blue-light excited; Present higher luminous efficiency, emission wavelength covers larger scope, is the important sources of LED luminescent material.Silicate fluorescent powder is widely used in the fields such as LED, PDP, becomes the focus and emphasis of illumination field research.
Research at present for silicates fluorescent material mainly concentrates on following several respects: the 1. innovation of preparation method.As patent CN101591535A first adopts sol-gel method to prepare transparent colloid, then through microwave combustion method, finally calcining obtains fluorescent material; As patent CN102732247A first prepares matrix with high temperature solid-state method, then gained matrix to be added in presoma calcining and obtain fluorescent material, luminous intensity, thermotolerance, wet fastness obtain and improve to a certain extent.2. alkaline-earth metal proportion adjustment.As patent CN102965102A adopts the M of solid phase method three step calcining synthesis Different Ca/Ba value 2siO 4: Eu fluorescent material; Patent CN102643642A has synthesized the Ba of Sr or Ca doping 2siO 4: Eu fluorescent material.3. rare earth ion doped.Patent CN102286282A is at Sr 2siO 4: adulterate in Eu fluorescent material Lu ion; If patent CN102337122A is at Ba 2siO 4: adulterate in Eu fluorescent material Pr, Ce, Sm, Tb plasma.In these researchs, rare earth ion doped change intensity of emission spectra, alkaline-earth metal ions doping changes emission peak positions.The synthetic method adopted is mostly high temperature solid-state method, sol-gel method.High temperature solid-state method synthesis temperature is high, the sintering soak time is long, usually need repeatedly to calcine and thing mutually assorted, particle is uneven, follow-up pulverizing can make luminescent properties and use properties decline to a great extent.Sol-gel method complex process, cost is high, toxic, has pollution, harmful, is unfavorable for environment protection.
Therefore, adopt method synthetic silicate fluorescent material simple, with low cost, by ion co-doped change emmission spectrum shape, improve luminous intensity, thus it is significant to improve luminescent properties.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, there is provided a kind of synthesis cost low, save energy, the fluorescent material synthetic method that production efficiency is high, the method is, in room-temperature ball-milling process, solid state reaction occurs, utilize the mechanical force (shearing force produced in mechanical milling process, surging force) can broken solid-phase reactant, increase the specific surface area of reactant, improve reactant contact area and speed of reaction, therefore improve the ratio of nucleation rate and growth rate, can prepare fine, uniform precursor, then drying, thermolysis, obtain the target product of Uniform Doped.Improve light-emitting phosphor performance by the codoped of rare earth ion and alkalimetal ion, obtain a kind of silicate green fluorescent powder of LED codoped.
The synthetic method of the LED silicate green fluorescent powder that the present invention proposes, comprises the following steps:
(1) according to Ba in chemical formula 2-x/2-2y-zsiO 4: Eu 2+ z, Li + x+y, Er 3+ yeach element chemistry metering ratio, wherein 0≤x≤0.25,0 < y≤0.02,0 < z≤0.1 takes barium salt, lithium salts, nanometer grade silica, europium salt, erbium salt respectively.Take the tensio-active agent of the 0.2wt% ~ 1wt% of above medicine total mass again;
(2) barium salt taken, lithium salts, nanometer grade silica, europium salt, erbium salt, tensio-active agent and appropriate part are fully mixed, the mol ratio of reactant and part is 1:2 ~ 6, then ball milling 2 ~ 5h, lubricant is added during ball milling, the add-on of lubricant is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system;
(3) above-mentioned product is directly dried, obtain precursor powder;
(4) calcined under reducing atmosphere by precursor powder, calcining temperature is 1000 ~ 1300 DEG C, and calcination time is 2 ~ 7 hours, obtains target product.
In the present invention, barium salt described in step (1) is for being BaCl 22H 2o, BaCO 3in one; Described lithium salts is Li 2cO 3, one in LiCl; Described europium salt is Eu (NO 3) 36H 2o or EuCl 37H 2o; Described erbium salt is Er (NO 3) 35H 2o or ErCl 3h 2o; Described tensio-active agent is Sodium dodecylbenzene sulfonate or polyoxyethylene glycol;
In the present invention, described in step (2), part is (NH 4) 2c 2o 4, NH 4hCO 3, (NH 4) 2cO 3in one; Described lubricant is acetone or alcohol.
In the present invention, described in step (4), reducing atmosphere is hydrogen (H 2), nitrogen and hydrogen gas mixture (H 2and N 2) or provided by gac incomplete combustion.
Compared with existing result of study, the present invention has following beneficial effect:
1, the fluorescent material that prepared by the present invention has once calcined matrix generation, ion doping and reduction process, and compared with high temperature solid-state method, calcining temperature is low, the time is short, production efficiency is high.
2, the fluorescent material that prepared by the present invention generates presoma in mechanical milling process, and due to the effect of mechanical force (shearing force, surging force), the presoma prepared is tiny, even, calcine the fluorescent material good crystallinity obtained, short texture, particle is tiny, be evenly distributed, there is good coating property.
3, the fluorescent material prepared of the present invention is due to Li +and Er 3+codoped, strengthen matrix to the absorption of light, reduce calcining temperature, luminous intensity is significantly improved.
4, the fluorescent material prepared of the present invention due to Li +and Er 3+codoped, works as Er 3+increase time, there is the emission peak being positioned at 488nm and 530nm place.
5, the fluorescent material excitation wavelength range prepared of the present invention is wide, and luminous intensity is high, and stability is high, effectively can be excited, invent bright green glow by near ultraviolet LED chip.
Four, accompanying drawing explanation
Fig. 1 is green emitting phosphor Ba 2-x/2-2y-zsiO 4: Eu 2+ z, Li + x+y, Er 3+ ypreparation technology's schema
Fig. 2 is green emitting phosphor Ba 2-x/2-2y-zsiO 4: Eu 2+ z, Li + x+y, Er 3+ yx ray diffracting spectrum
Fig. 3 is green emitting phosphor Ba 1.97siO 4: Eu 2+ 0.01, Li + 0.01, Er 3+ 0.01excite and launch collection of illustrative plates
Fig. 4 is green emitting phosphor Ba 1.87siO 4: Eu 2+ 0.05, Li + 0.1, Er 3+ 0.02excite and launch collection of illustrative plates
Five, concrete case study on implementation
Case study on implementation 1:
According to chemical formula Ba 1.97siO 4: Eu 2+ 0.01, Li + 0.01, Er 3+ 0.01take BaCO respectively 3(A.R.) 1.97mol, nano level SiO 21mol, Eu (NO 3) 36H 2o (A.R.) 0.01mol, Li 2cO 3(A.R.) 0.005mol and Er (NO 3) 35H 2o (A.R.) 0.01mol, then the surfactant sodium dodecyl base benzene sulfonic acid sodium salt taking above medicine total mass 0.8wt%; By the BaCO taken 3(A.R.), nano level SiO 2, Eu (NO 3) 36H 2o (A.R.), Li 2cO 3(A.R.), Er (NO 3) 35H 2o (A.R.), Sodium dodecylbenzene sulfonate and appropriate part NH 4hCO 3(reactant and part ratio are 1:6) fully mixes, and then carries out ball milling (Ball-milling Time is 2h), adds lubricant ethanol during ball milling, and the add-on of ethanol is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcined in nitrogen and hydrogen gas mixture by precursor powder, calcining temperature is 1150 DEG C, and calcination time is 4h, obtains target product.Its excitation-emission spectrum as shown in Figure 3.
Case study on implementation 2:
According to chemical formula Ba 1.87siO 4: Eu 2+ 0.05, Li + 0.1, Er 3+ 0.02take BaCl respectively 22H 2o (A.R.) 1.87mol, nano level SiO 21mol, EuCl 37H 2o (A.R.) 0.05mol, LiCl (A.R.) 0.1mol and ErCl 3h 2o (A.R.) 0.02mol, then the surfactant polyethylene taking above medicine total mass 0.6wt%; By the BaCl taken 22H 2o (A.R.), nano level SiO 2, EuCl 37H 2o (A.R.), LiCl (A.R.), ErCl 3h 2o (A.R.), polyoxyethylene glycol and appropriate part (NH 4) 2c 2o 4(reactant and part ratio are 1:2) fully mixes, and then carries out ball milling (Ball-milling Time is 5h), adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcined in reducing atmosphere hydrogen by precursor powder, calcining temperature is 1200 DEG C, and calcination time is 3h, obtains target product.Its excitation-emission spectrum as shown in Figure 4.
Case study on implementation 3:
According to chemical formula Ba 1.91siO 4: Eu 2+ 0.08, Li + 0.005, Er 3+ 0.005take BaCO respectively 3(A.R.) 1.91mol, nano level SiO 21mol, Eu(NO 3) 36H 2o (A.R.) 0.08mol, Li 2cO 3(A.R.) 0.0025mol and Er (NO 3) 35H 2o (A.R.) 0.005mol, then the surfactant polyethylene taking above medicine total mass 0.4wt%; By the BaCO taken 3(A.R.), nano level SiO 2, Eu(NO 3) 36H 2o (A.R.), Li 2cO 3(A.R.), Er (NO 3) 35H 2o (A.R.), polyoxyethylene glycol and appropriate part (NH 4) 2c 2o 4(reactant and part ratio are 1:2) fully mixes, and then carries out ball milling (Ball-milling Time is 3h), adds lubricant ethanol during ball milling, and the add-on of ethanol is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcined in nitrogen and hydrogen gas mixture by precursor powder, calcining temperature is 1150 DEG C, and calcination time is 5h, obtains target product.
Case study on implementation 4:
According to chemical formula Ba 1.83siO 4: Eu 2+ 0.03, Li + 0.25, Er 3+ 0.01take BaCl respectively 22H 2o (A.R.) 1.83mol, nano level SiO 21mol, EuCl 37H 2o (A.R.) 0.03mol, LiCl (A.R.) 0.25mol and ErCl 3h 2o (A.R.) 0.01mol, then the surfactant sodium dodecyl base benzene sulfonic acid sodium salt taking above medicine total mass 0.2wt%; By the BaCl taken 22H 2o (A.R.), nano level SiO 2, EuCl 37H 2o (A.R.), LiCl (A.R.), ErCl 3h 2o (A.R.), Sodium dodecylbenzene sulfonate and appropriate part NH 4hCO 3(reactant and part ratio are 1:4) fully mixes, and then carries out ball milling (Ball-milling Time is 5h), adds lubricant ethanol during ball milling, and the add-on of ethanol is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcine in the reducing atmosphere provided at gac incomplete combustion by precursor powder, calcining temperature is 1200 DEG C, and calcination time is 3.5h, obtains target product.
Case study on implementation 5:
According to chemical formula Ba 1.7775siO 4: Eu 2+ 0.1, Li + 0.2, Er 3+ 0.015take BaCO respectively 3(A.R.) 1.7775mol, nano level SiO 21mol, EuCl 37H 2o (A.R.) 0.1mol, Li 2cO 3(A.R.) 0.1mol and ErCl 3h 2o (A.R.) 0.015mol, then the surfactant sodium dodecyl base benzene sulfonic acid sodium salt taking above medicine total mass 1 wt%; By the BaCO taken 3(A.R.), nano level SiO 2, EuCl 37H 2o (A.R.), Li 2cO 3(A.R.), ErCl 3h 2o (A.R.), Sodium dodecylbenzene sulfonate and appropriate part (NH 4) 2c 2o 4(reactant and part ratio are 1:3) fully mixes, and then carries out ball milling (Ball-milling Time is 4h), adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcine in the reducing atmosphere provided at gac incomplete combustion by precursor powder, calcining temperature is 1250 DEG C, and calcination time is 2.5h, obtains target product.
Case study on implementation 6:
According to chemical formula Ba 1.9225siO 4: Eu 2+ 0.02, Li + 0.1, Er 3+ 0.005take BaCl respectively 22H 2o (A.R.) 1.9225mol, nano level SiO 21mol, EuCl 37H 2o (A.R.) 0.02mol, LiCl (A.R.) 0.1mol and ErCl 3h 2o (A.R.) 0.005mol, then the surfactant polyethylene taking above medicine total mass 0.2 wt%; By the BaCl taken 22H 2o (A.R.), nano level SiO 2, EuCl 37H 2o (A.R.), LiCl (A.R.), ErCl 3h 2o (A.R.), polyoxyethylene glycol and appropriate part (NH 4) 2cO 3(reactant and part ratio are 1:3) fully mixes, and then carries out ball milling (Ball-milling Time is 4h), adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcined in nitrogen and hydrogen gas mixture by precursor powder, calcining temperature is 1250 DEG C, and calcination time is 2.5h, obtains target product.
Case study on implementation 7:
According to chemical formula Ba 1.87siO 4: Eu 2+ 0.09, Li + 0.02, Er 3+ 0.02take BaCO respectively 3(A.R.) 1.87mol, nano level SiO 21mol, EuCl 37H 2o (A.R.) 0.09mol, Li 2cO 3(A.R.) 0.01mol and Er (NO 3) 35H 2o (A.R.) 0.02mol, then the surfactant sodium dodecyl base benzene sulfonic acid sodium salt taking above medicine total mass 0.3 wt%; By the BaCO taken 3(A.R.), nano level SiO 2, EuCl 37H 2o (A.R.), Li 2cO 3(A.R.), Er (NO 3) 35H 2o (A.R.), Sodium dodecylbenzene sulfonate and appropriate part (NH 4) 2c 2o 4(reactant and part ratio are 1:2) fully mixes, and then carries out ball milling (Ball-milling Time is 5h), adds lubricant ethanol during ball milling, and the add-on of ethanol is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcined in nitrogen and hydrogen gas mixture by precursor powder, calcining temperature is 1300 DEG C, and calcination time is 2h, obtains target product.
Case study on implementation 8:
According to chemical formula Ba 1.905siO 4: Eu 2+ 0.04, Li + 0.05, Er 3+ 0.02take BaCl respectively 22H 2o (A.R.) 1.905mol, nano level SiO 21mol, EuCl 37H 2o (A.R.) 0.04mol, LiCl (A.R.) 0.05mol and ErCl 3h 2o (A.R.) 0.02mol, then the surfactant polyethylene taking above medicine total mass 0.5 wt%; By the BaCl taken 22H 2o (A.R.), nano level SiO 2, EuCl 37H 2o6H 2o (A.R.), LiCl (A.R.), ErCl 3h 2o (A.R.), polyoxyethylene glycol and appropriate part NH 4hCO 3(reactant and part ratio are 1:5) fully mixes, and then carries out ball milling (Ball-milling Time is 3h), adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcine in the reducing atmosphere provided at gac incomplete combustion by precursor powder, calcining temperature is 1000 DEG C, and calcination time is 7h, obtains target product.
Case study on implementation 9:
According to chemical formula Ba 1.8325siO 4: Eu 2+ 0.07, Li + 0.15, Er 3+ 0.015take BaCl respectively 22H 2o (A.R.) 1.8325mol, nano level SiO 21mol, EuCl 37H 2o (A.R.) 0.07mol, LiCl (A.R.) 0.15mol and ErCl 3h 2o (A.R.) 0.015mol, then the surfactant sodium dodecyl base benzene sulfonic acid sodium salt taking above medicine total mass 0.7 wt%; By the BaCl taken 22H 2o (A.R.), nano level SiO 2, EuCl 37H 2o (A.R.), LiCl (A.R.), ErCl 3h 2o (A.R.), Sodium dodecylbenzene sulfonate and appropriate part (NH 4) 2c 2o 4(reactant and part ratio are 1:4) fully mixes, and then carries out ball milling (Ball-milling Time is 4h), adds lubricant ethanol during ball milling, and the add-on of ethanol is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcine in the reducing atmosphere provided at gac incomplete combustion by precursor powder, calcining temperature is 1100 DEG C, and calcination time is 6h, obtains target product.
Case study on implementation 10:
According to chemical formula Ba 1.91siO 4: Eu 2+ 0.06, Li + 0.015, Er 3+ 0.015take BaCO respectively 3(A.R.) 1.91mol, nano level SiO 21mol, Eu (NO 3) 36H 2o (A.R.) 0.06mol, Li 2cO 3(A.R.) 0.0075mol and ErCl 3h 2o (A.R.) 0.015mol, then the surfactant polyethylene taking above medicine total mass 0.9 wt%; By the BaCO taken 3(A.R.), nano level SiO 2, Eu (NO 3) 36H 2o (A.R.), Li 2cO 3(A.R.), ErCl 3h 2o (A.R.), polyoxyethylene glycol and appropriate part NH 4hCO 3(reactant and part ratio are 1:4) fully mixes, and then carries out ball milling (Ball-milling Time is 2h), adds lubricant acetone during ball milling, and the add-on of acetone is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; The product obtained directly is dried, obtains precursor powder; Calcined in reducing atmosphere hydrogen by precursor powder, calcining temperature is 1300 DEG C, and calcination time is 2h, obtains target product.

Claims (1)

1. a synthetic method for the silicate green fluorescent powder of LED codoped, is characterized in that concrete steps are as follows:
(1) according to Ba in chemical formula 2-x/2-2y-zsiO 4: Eu 2+ z, Li + x+y, Er 3+ yeach element chemistry metering ratio, wherein 0≤x≤0.25,0 < y≤0.02,0 < z≤0.1 takes barium salt, nanometer grade silica, europium salt, lithium salts, erbium salt respectively; Take the tensio-active agent of the 0.2wt% ~ 1wt% of above medicine total mass again; Described barium salt is BaCl 22H 2o, BaCO 3in one; Described lithium salts is Li 2cO 3, one in LiCl; Described europium salt is Eu (NO 3) 36H 2o or EuCl 37H 2o; Described erbium salt is Er (NO 3) 35H 2o or ErCl 3h 2o; Described tensio-active agent is Sodium dodecylbenzene sulfonate or polyoxyethylene glycol;
(2) barium salt taken, nanometer grade silica, europium salt, lithium salts, erbium salt, tensio-active agent and appropriate part are fully mixed, the mol ratio of reactant and part is 1:2 ~ 6, then ball milling 2 ~ 5h, lubricant is added during ball milling, the add-on of lubricant is to be kept dispersion to be limited, till reactant and part complete reaction by ball milling system; Described part is (NH 4) 2c 2o 4, NH 4hCO 3, (NH 4) 2cO 3in one; Described lubricant is acetone or alcohol;
(3) above-mentioned product is directly dried, obtain precursor powder;
(4) calcined under reducing atmosphere by precursor powder, calcining temperature is 1000 ~ 1300 DEG C, and calcination time is 2 ~ 7 hours, obtains target product; Described reducing atmosphere is hydrogen (H 2), nitrogen and hydrogen gas mixture (H 2and N 2) or provided by gac incomplete combustion.
CN201310449327.2A 2013-04-26 2013-09-29 Preparation method of co-doped silicate green fluorescent powder used for LEDs Expired - Fee Related CN103468250B (en)

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CN110564408A (en) * 2019-08-26 2019-12-13 昆明理工大学 Samarium-doped silicate luminescent material and preparation method thereof

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