CN104710982B - A kind of aluminosilicate novel green light fluorescent powder of rare earth ion codope and preparation method thereof - Google Patents
A kind of aluminosilicate novel green light fluorescent powder of rare earth ion codope and preparation method thereof Download PDFInfo
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Abstract
Aluminosilicate (mullite substrate) novel green light fluorescent powder that the invention provides a kind of rare earth ion codope and preparation method thereof, belongs to luminescent material technical field.Novel green light fluorescent powder chemical composition is aAl2O3BSiO2CCeO2DTb4O7, wherein a, b, c, d are molar fraction, a/b=3/2,0≤c≤2.0%, 0≤d≤5.0%, are zero when c with d is different.Preparation method is embodied as step: weighs raw material by the stoichiometric proportion of element each in chemical formula, is sufficiently mixed, and at room temperature ball milling；Sufficient for ball milling sample is put in the high temperature process furnances being connected with reducing atmosphere, calcines 2～6 hours at 1450～1550 DEG C；Treat that furnace chamber is cooled to room temperature, take out sample and carry out crushing grinding；Follow-up add H3BO3Flux, washing are or/and SiO2Claddings etc. process, and can obtain required fluorescent material.Fluorescent material prepared by the present invention, its crystallinity and particle surface pattern are good, luminous intensity high (especially having the heat stability of excellence), are suitable for use as the LED green light fluorescent powder of ultraviolet excitation.
Description
Technical field
The invention belongs to LED luminescent material preparing technical field, the aluminosilicate being specifically related to a kind of rare earth ion codope is novel
Green light fluorescent powder and preparation method thereof.
Background technology
White light emitting diode (WLED) possesses the advantages such as efficiency height, life-span length, energy-conserving and environment-protective and the most gradually replaces tradition because of it
Lighting source and become a new generation lighting source.Fluorescent material can absorb ultraviolet/near ultraviolet or blue light then sends visible ray, is
Critical material in LED solid luminescence technology.The implementation of white light mainly has three kinds at present: (1) is trichroism by red, green, blue
LED chip is packaged together, and is mixed to get white light by white light；(2) blue-light LED chip excites yellow fluorescent powder, yellow
Light and blue light obtain white light；(3) UV LED chip excites three primary colors fluorescent powder to obtain white light.Wherein, the 1st kind of mode
Not only drive circuit is complicated, and production cost is high, and heat dissipation problem is difficult to solve.Therefore, the 2nd kind of mode of commercial many employings
Synthesis white light, causes its color developing the best yet with lacking HONGGUANG.In order to meet the demand for development of LED illumination technology,
Research and develop a kind of new and effective, there is the green light fluorescent powder of superior luminescence color and thermal stability, to realize the conjunction of the 3rd kind of white light
One-tenth mode, will have broader application demand.
So far, the green emitting phosphor of exploitation both at home and abroad mainly has silicate systems, aluminates system and nitrogen oxides system
Deng, but they have the pluses and minuses of oneself.Silicate substrate fluorescent material excitation wave length and width, it is possible to be well suited for different wave length core
Exciting of sheet, can be widely used and have certain industrialized scale, such as the M of orthosilicate system2SiO4:Eu2+(M:Ca、Sr、
And Ca Ba)3Si2O7:Eu2+；But its poor heat stability (light decay when 150 DEG C is more than 50%), limits its large-scale application.Pass
System aluminates system fluorescent material can launch green glow under (closely) burst of ultraviolel, cheap, and preparation is easily；But it prepares former
Material requires of a relatively high purity, and between component, phase composition and phase transformation are complicated, and fluorescence efficiency is relatively low, such as BaMgAl10O17:Eu,
Mn.Silica-based nitrogen oxides is a kind of phosphor host that latest developments are very fast, it is possible to swashed by blue light and ultraviolet high efficiency
Send out, then coordinate the change of rare earth ion and chemical composition, the transmitting light of different wave length can be realized: such as, β-SiAlON:Eu2+It is
Applying a more class nitrogen oxide green fluorescent powder at present, it coordinates with blue chip can produce specular removal, but its shortcoming is
Preparation condition is harsh (needing High Temperature High Pressure), large-scale industrial production difficulty.
Meanwhile, with mullite as substrate, the phosphor material powder of doping different rare earth ions, excellent luminescent properties can be obtained,
Start to attract many research to pay close attention to: such as, use water heat transfer Eu2+The mullite fluorescent material of doping, uses sol-gel
Method prepares Tb3+The mullite fluorescent material of doping, additionally prepares Ce also by sol-gel3+, Tb3+The mullite being co-doped with
Eu prepared by fluorescent material and high temperature solid-state method2+, Tb3+The 3/2 mullite fluorescent material being co-doped with.But, add boric acid for fluxing
Agent, uses high temperature solid-state method to prepare Ce3+,Tb3+The mullite fluorescent material being co-doped with not yet occurs.
Summary of the invention
It is an object of the invention to develop the novel green light fluorescent powder of aluminosilicate of a kind of rare earth ion codope, i.e. can be by ultraviolet
LED chip excites and launches high intensity, the fluorescent material of stable green glow.
The technical problem to be solved is to provide one, and technique is simple, product quality is high, low cost, can extensively apply
Novel green light fluorescent powder of aluminosilicate of a kind of rare earth ion codope in luminescent material manufactures and preparation method thereof.
The novel green light fluorescent powder of aluminosilicate of the present invention a kind of rare earth ion codope, its primary chemical consists of:
aAl2O3BSiO2CCeO2DTb4O7
Wherein a, b, c, d are molar fraction, a/b=3/2,0≤c≤2.0%, 0≤d≤5.0%；And be zero during c, d difference.
According to experimental result, the preferred value of c Yu d is respectively 1.3% and 2%, along with Ce3+、Tb3+Ion doping concentration is opened from zero
Beginning to increase, the excitation peak of fluorescent material and the intensity of emission peak gradually strengthen, and light intensity is as the same；When reaching preferred concentration value, swash
Send out peak and emission peak intensity and light intensity reaches the strongest；After exceeding optium concentration, concentration quenching under high doping occur, light intensity is gradually
Reduce.
It addition, for promoting high temperature solid state reaction, reacting fully is carried out, and can add a certain amount of flux in being co-doped with fluorescent material,
With H3BO3Preferable for flux effect, its optimum addition is 5wt%.Along with H3BO3Interpolation, flux was reacting
Journey melts, it is provided that a semifluid environment, be conducive to improving reaction rate and the crystallinity of product；But work as H3BO3
When addition is more than 5wt%, the H of excess3BO3Al can be caused20B4O36The generation of cenotype.
3Al of the present invention2O32SiO2Refer to 3/2 mullite.
The Tb of doping in mullite substrate3+It is to provide the centre of luminescence as activator, utilizes Tb3+Special level structure, passes through
Electronics transition absorption between different energy levels and transmitting photon, show the transmitting of different colours light.The Ce of doping in substrate3+
It is to improve the activator ion absorption to light as sensitizer, i.e. utilizes Ce-Tb energy to transmit, by non-radiative energy transition
Luminous energy is passed to activator ion from sensitizer ion, then luminous by activator ion energy level transition.
The Ce of the mullite that the present invention relates to3+、Tb3+Ion doping belongs to structural vacancy doping, the advantage of this doping way
It is more weak to be that the centre of luminescence is affected by lattice environment, has excellent stability.Rare earth ion Ce3+And Tb3+The model that properly adulterates
Enclosing respectively 0～2.0% and 0～20.0%, wherein optimum doping concentration is that 1.3mol% and 8.0mol% is (i.e. with aforementioned respectively
0≤c≤2.0%, 0≤d≤5.0%, it is consistent that the preferred value of c with d is respectively 1.3% and 2% effect)；Now Tb3+And Ce3+Between deposit
Energy in greater efficiency transmits, and fluorescent material shows good green emission, and has good thermal stability: at environment
When temperature is 260 DEG C, fluorescent material sample luminous intensity is 91% under room temperature, hence it is evident that be better than general commercial fluorescent material.
For improving Al further6Si2O13: the crystallinity of Ce, Tb fluorescent material and luminescent properties, add H3BO3As flux, and
Carry out certain post processing.In the case of content is less than 5wt%, flux H3BO3High temperature solid state reaction can be promoted, make reaction
Fully carry out smoothly, and be unlikely to damage the luminescent properties of fluorescent material.
In the present invention, the preparation method of aforementioned fluorescent powder, comprises the steps:
(1) aAl is pressed2O3BSiO2CCeO2DTb4O7The stoichiometric proportion of each element in chemical formula, weigh aluminium oxide,
Silicon dioxide, cerium oxide and terbia. Diterbium trioxide raw material；
(2) raw material weighed is sufficiently mixed, and at room temperature ball milling；
(3) pour the sample after abundant ball milling into boron nitride crucible, put in the high temperature process furnances being connected with reducing atmosphere,
Calcine 2～6 hours at 1450～1550 DEG C；
(4) treat that furnace chamber is cooled to room temperature, take out sample and carry out crushing grinding；
(5) follow-up employing adds flux, and deionized water carries out ultrasonic wave water washing or/and carry out SiO2Claddings etc. process.
Described ball milling is carried out in agate mortar, and the time is 30～40min, until the color of raw material is substantially uniform unanimously.
Described reducing atmosphere is 95%N2+ 5%H2Mixed gas.
The described crushing grinding time is about 30min, makes the sample broke of caking and is ground to small grains, and particle diameter is distributed in
Below 30 μm.
Described flux is H3BO3, best results when addition is 5wt%, beneficially reactant granule tiny and uniform.
When deionized water carries out ultrasonic wave water washing, the Al that 1.5g is prepared6Si2O13: 100ml beaker poured into by Ce, Tb fluorescent material,
Adding 70ml deionized water, carry out ultrasonic disperse washing, the time is 2h, after having cleaned, mixed liquor is carried out sucking filtration and drying
Processing, make particle dispersion good, particle diameter is distributed in 5～10 μm.
Described SiO2It is to utilize tetraethyl orthosilicate (TEOS) hydrolysis in an acidic solution to produce Si (OH) that cladding processes4,
Then at 600 DEG C, carry out heat treatment, be incubated 2h, make the Si (OH) on fluorescent powder grain surface4It is converted into the finest and close nothing fixed
Type amorphous Si O2Film, now fluorescent powder grain size does not changes much.SiO2Optimal covering amount is 15wt%.
Last handling process includes washing and cladding.Use ultra-sonic dispersion method to carry out washing and can reduce fluorescent powder grain reunion degree,
Improve dispersibility and specific surface area, so that the luminous intensity of fluorescent material improves.Utilize chemical method that fluorescent powder grain is carried out SiO2
Cladding, especially works as SiO2When content is 15wt%, the surface topography of fluorescent powder grain be improved significantly, and heat stability obtains
Bigger lifting.
Compared with existing result of study, there is advantages that
1. the present invention uses high temperature solid-state method to prepare fluorescent material, have that yield is big, production cost is low and can the advantage of industrialized production,
And it is simple to prepare fluorescent material flow process, powder surface defect is few.
2. the fluorescent material that prepared by the present invention is by rare earth ion Ce3+And Tb3+It is co-doped with, Ce3+As sensitizer ion, passed by energy
Passing and can effectively strengthen the activator ion absorption to light, luminous intensity is significantly improved.
3. the present invention with the addition of flux in preparation process and carried out washing and the post processing of cladding, can significantly improve reaction bar
Part, obtains granule fine uniform, and surface topography is good, the fluorescent material of good heat stability.
4. the fluorescent material excitation wavelength range width that prepared by the present invention, luminous intensity is high, has good heat stability, can be by ultraviolet
Light effectively excites and generates bright green glow.
5. this fluorescent material can exciting by the emission spectrum light-emitting component in 200～300nm regions, main absorbing wavelength is 300
Light near nm, produces in the range of 420～620nm, main emission peak is at the emission spectrum of about 540nm, and has
It is better than the good thermal stability energy of general commercial fluorescent material.
Accompanying drawing explanation
Fig. 1 is excitation spectrum and the emission spectrum of embodiment 1；
Fig. 2 is excitation spectrum and the emission spectrum of embodiment 2；
Fig. 3 be embodiment 4 with the addition of H3BO3Fluorescent material XRD figure spectrum；
Fig. 4 is that embodiment 2 is adding H with example 43BO3Fluorescence emission spectrum comparison diagram front and back.
Fluorometric investigation condition is: 150W xenon lamp, and PMT voltage is 400V, sweeps speed for 1200nm/min, light inlet and go out light
Mouth slit is 5nm, step-length 1nm.
Embodiment
Explain the present invention with accompanying drawing with the following Examples, but technical solution of the present invention is not limited to act specific embodiment party set forth below
Formula, also includes the combination in any between each detailed description of the invention.
Embodiment 1
Weighing aluminium oxide 5.998g (0.588mol), silicon dioxide 2.352g (0.392mol), terbia. Diterbium trioxide 1.496g (0.02mol),
It is mixed, agate mortar grinds 30min.The raw material of full and uniform mixing is poured in boron nitride crucible, under crucible
Corundum sheet put by pad, puts in high temperature process furnances and is sintered, is passed through reducing atmosphere 95%N2+ 5%H2, arranging sintering temperature is
1470 DEG C, temperature retention time is 5h.Treat that furnace chamber is cooled to room temperature, take out sample and carry out crushing grinding about 30min, can obtain
Al6Si2O13: Tb fluorescent material.Now Tb3+Doping content be 8mol%, excitation and emission spectra is as shown in Figure 1.
Embodiment 2
Weighing aluminium oxide 5.918g (0.5802mol), silicon dioxide 2.321g (0.3868mol), terbia. Diterbium trioxide 1.496g (0.02mol),
Cerium oxide 0.2236g (0.013mol), is mixed, and grinds 30min in agate mortar.Raw material by full and uniform mixing
Pour in boron nitride crucible, put corundum sheet at crucible underlay, put in high temperature process furnances and be sintered, be passed through reducing atmosphere
95%N2+ 5%H2, sintering temperature is 1470 DEG C, and temperature retention time is 5h.Treat that furnace chamber is cooled to room temperature, take out sample and crush
Grind about 30min, Al can be obtained6Si2O13: Tb, Ce green light fluorescent powder.Now Ce3+And Tb3+Doping content be respectively
1.3mol% and 8.0mol%, excitation and emission spectra is as shown in Figure 2.With 297nm as excitation wavelength, the luminous quantity of fluorescent material
Sub-efficiency is 24.21%, has a good heat stability simultaneously: the luminous intensity of fluorescent material when 260 DEG C, for luminous under room temperature
The 91% of intensity.
Embodiment 3
Weighing aluminium oxide 5.918g (0.5802mol), silicon dioxide 2.321g (0.3868mol), terbia. Diterbium trioxide 1.496g (0.02mol),
Cerium oxide 0.2236g (0.013mol), is mixed, and grinds 30min in agate mortar.Raw material by full and uniform mixing
Pour in boron nitride crucible, put corundum sheet at crucible underlay, put in high temperature process furnances and be sintered, be passed through reducing atmosphere
95%N2+ 5%H2, sintering temperature is 1470 DEG C, and temperature retention time is 5h.Treat that furnace chamber is cooled to room temperature, take out sample and crush
Grind about 30min, Al can be obtained6Si2O13: Tb, Ce green light fluorescent powder；Follow-up carry out 15wt%SiO again2Cladding processes: tool
Body utilizes tetraethyl orthosilicate (TEOS) hydrolysis in an acidic solution to produce Si (OH)4, at 600 DEG C, then carry out heat
Process, be incubated 2h, make the Si (OH) on fluorescent powder grain surface4It is converted into the finest and close unformed amorphous Si O2Film.Now
Fluorescent material Ce3+And Tb3+Doping content be respectively 1.3mol% and 8.0mol%, when with 297nm as excitation wavelength, luminous quantity
Sub-efficiency is 18.33%；But there is better heat stability: the light-emitting phosphor intensity when 260 DEG C, for lower light intensity of room temperature
The 98.8% of degree.
Embodiment 4
Weighing aluminium oxide 5.918g (0.5802mol), silicon dioxide 2.321g (0.3868mol), terbia. Diterbium trioxide 1.496g (0.02mol),
Cerium oxide 0.2236g (0.013mol), boric acid 0.524g (0.0085mol), be mixed, and grinds 30min in agate mortar.
Again the raw material of full and uniform mixing is poured in boron nitride crucible, put corundum sheet at crucible underlay, put in high temperature process furnances and carry out
Sintering, is passed through reducing atmosphere 95%N2+ 5%H2, arranging sintering temperature is 1470 DEG C, and temperature retention time is 5h.Treat that furnace chamber cools down
To room temperature, take out sample and carry out crushing grinding about 30min, the Al of B element doping can be obtained6Si2O13: Tb, Ce green-emitting fluorescent
Powder.Add the fluorescent material XRD figure after different content boric acid to compose as shown in Figure 3.When with 297nm as excitation wavelength, luminous quantity
Sub-efficiency is 21.96%；Its luminous intensity when 260 DEG C is about 76% under room temperature.
Embodiment 5
Weighing aluminium oxide 5.918g (0.5802mol), silicon dioxide 2.321g (0.3868mol), terbia. Diterbium trioxide 1.496g (0.02mol),
Cerium oxide 0.2236g (0.013mol), boric acid 0.524g (0.0085mol), be mixed, and grinds 30min in agate mortar.
The raw material of full and uniform mixing is poured in boron nitride crucible, puts corundum sheet at crucible underlay, put in high temperature process furnances and burn
Knot, is passed through reducing atmosphere 95%N2+ 5%H2, arranging sintering temperature is 1470 DEG C, and temperature retention time is 5h.Treat that furnace chamber is cooled to
Room temperature, takes out sample and carries out crushing grinding about 30min, can obtain the Al of B element doping6Si2O13: Tb, Ce green light fluorescent powder.
Weigh the fluorescent material sample that 1.5g has prepared, pour in 100ml beaker, add the deionized water of 70ml, at certain power
Under carry out ultrasonic disperse cleaning, the time is 2h, after cleaning, mixed liquor is carried out sucking filtration, dry, milled processed.When with 297
Nm is excitation wavelength, and its luminescent spectrum is as shown in Figure 4；Compared with the fluorescent material that example 2 is not added with boric acid flux, luminous strong
Degree is significantly improved.
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert the present invention
Be embodied as be confined to these explanations.For general technical staff of the technical field of the invention, without departing from this
On the premise of inventive concept, it is also possible to make some simple inferences or replacement, all should be considered as belonging to protection scope of the present invention.
Claims (9)
1. the novel green light fluorescent powder of the aluminosilicate of a rare earth ion codope, it is characterised in that new phosphors chemical composition is
aAl2O3·bSiO2·cCeO2·dTb4O7, wherein a, b, c, d are molar fraction, and a/b=3/2, c are 1.3%, 0≤d≤5.0%.
The novel green light fluorescent powder of aluminosilicate of a kind of rare earth ion codope the most according to claim 1, it is characterised in that
Tb4O7It is 2%.
3. according to the novel green-emitting fluorescent of aluminosilicate of a kind of rare earth ion codope described in claim 12 any claim
Powder, it is characterised in that on the basis of described fluorescent material, the flux H of interpolation3BO3, H3BO3Quality for fluorescent material is divided
Number is 5wt%.
4. the aluminosilicate of a rare earth ion codope novel green-emitting fluorescent powder, preparation method thereof, it is characterised in that such as claim 1
The novel green light fluorescent powder of aluminosilicate of the rare earth ion codope described in 3 any claim, comprises the steps:
(1) aAl is pressed2O3·bSiO2·cCeO2·dTb4O7The stoichiometric proportion of each element in chemical formula, weighs aluminium oxide, dioxy
SiClx, cerium oxide and terbia. Diterbium trioxide raw material；
(2) raw material weighed is sufficiently mixed, and at room temperature ball milling；
(3) sample after abundant ball milling is put in the high temperature process furnances being connected with reducing atmosphere, at 1450～1550 DEG C calcine 2～
6 hours；
(4) treat that furnace chamber is cooled to room temperature, take out sample and carry out crushing grinding；
(5) follow-up employing adds flux, and deionized water carries out ultrasonic wave water washing or/and carry out SiO2Claddings etc. process.
Preparation method the most according to claim 4, it is characterised in that: under described room temperature, ball milling is carried out in agate mortar, time
Between be 30～40 minutes.
Preparation method the most according to claim 4, it is characterised in that: described reducing atmosphere is volume ratio 95%N2+ 5%H2
Mixed gas.
Preparation method the most according to claim 4, it is characterised in that: the described crushing grinding time is about 30 minutes, makes knot
The sample broke of block is also ground to small grains, and particle diameter is distributed in below 30 μm.
Preparation method the most according to claim 4, it is characterised in that: described for flux H3BO3, H3BO3For fluorescent material
Mass fraction be 5wt%.
Preparation method the most according to claim 5, it is characterised in that: when described employing deionized water carries out ultrasonic wave water washing,
The fluorescent material of 1.5g being poured into 100ml beaker, adds 70ml deionized water, then carry out ultrasonic disperse washing, the time is 2h；
Cleaning carries out sucking filtration and drying and processing to mixed liquor after completing, and makes particle dispersion good, and particle diameter is distributed in 5～10 μm；Or
SiO described in person2When cladding processes, it is to utilize tetraethyl orthosilicate hydrolysis in an acidic solution to produce Si (OH)4, so
After carry out at 600 DEG C heat treatment insulation 2h, make the Si (OH) on fluorescent powder grain surface4It is converted into the unformed of densification continuously
Amorphous Si O2Film, SiO2Optimal covering amount is 15wt%.
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