CN104774614B - Blue fluorescent powder for white-light LED and preparation method thereof - Google Patents
Blue fluorescent powder for white-light LED and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a blue fluorescent powder for white-light LED and a preparation method thereof. The chemical formula of the powder is Sc＜4-4x＞Al6Si3O21:4xCe＜3+＞; wherein in the formula, x represents the mole doping amount of rare earth activated ions (Ce3+), which are doped on the Sc3+ positions, 0.001≤x≤0.700. The prepared fluorescent powder can be well activated by the ultraviolet lights with a wavelength of 300 to 400 nanometers. The fluorescent powder can emit blue lights having a main peak at 425 nanometers, and thus the fluorescent powder can be well matched with an ultraviolet LED. The fluorescent is prepared by mixing compounds containing the required elements through a high-temperature solid-phase method or chemical synthesis method. The technology is simple and flexible, the repeatability is good, the operation is easy, the sources of the raw materials are wide, the chemical stability and thermal stability of the obtained products are both very good, crystallizing property of the synthesized fluorescent powder is good, the morphology is regular, the particle size is uniform, the luminescent efficiency is high, and thus the fluorescent powder is suitable for the preparation of LEDs excited by ultraviolet lights or near ultraviolet lights.
Description
Technical field
The present invention relates to a kind of blue fluorescent material and preparation method thereof, particularly to a kind of white light led blue-fluorescence
Powder and preparation method thereof, belongs to fluorescent material technical field.
Background technology
In recent years, with whole world rise, white light led and the various coloured silk of the semiconductor lighting cause of light emitting diode (led)
Color led causes people as light source of new generation and greatly pays close attention to.Compared with traditional electric filament lamp, fluorescent lamp, this forth generation
The many merits such as lighting source has durable in use, pollution-free, stable performance, response time is short, efficiency is high.At present, ultraviolet led
Chip is combined with three primary colors fluorescent powder, and its color rendering properties preferably, arbitrarily mate in the range of 2500～10000k by colour temperature, and ultraviolet swashs
The photic color fluorescent material of the different glow colors lived obtains extensive research, can perform well in preparing white light led,
The fluorescent material that this allows for can effectively being inspired red, green and blue color by ultraviolet light becomes a present important topic.
Wherein, as the blue colour fluorescent powder of one of composition most important in three primary colors fluorescent powder, what research was more at present has aluminum
Hydrochlorate, silicate and borate family, such as Chinese patent cn102206488a disclose a kind of white light led blue colour fluorescent powder and its
Preparation method, chemical composition formula is: c2-m-2xx2x(b1-nmn)5o9cl:meu.Wherein c is one of ca, mg, ba or several
Kind, x is one of li, na, k or several al adding equivalent again, and m is one or several of al, ga, in；Wherein 0 ＜ x
≤ 0.1,0 ＜ m≤0.5,0 ＜ n≤0.2, through the process such as pulverizing, sieving, be centrifuged after cooling, preparation technology is loaded down with trivial details；And for example China
Patent of invention cn102286283a discloses a kind of europium ion-doped aluminium phosphate magnesium blue colour fluorescent powder and preparation method thereof, and this is glimmering
It is mg that light powder includes chemical constitution formula1-xeux(alpo4)zThe component of o, wherein x=0.001～0.1；Z=0.9～1.2, permissible
Effectively excited by ultraviolet light and blue light, launch the broadband visible fluorescence that central peak is located at 440 ran, but it goes back Primordial Qi
Body is co or h2+n2, these not only propose higher requirement to equipment, increase the danger of experiment simultaneously, and operation is more complicated.
And for example Chinese invention patent cn101735804a reports a kind of white light led blue colour fluorescent powder, and its chemical formula is: ca1- xsio3: xeu2+, wherein 0 < x < 0.2, its preparation process is related to the materials such as surfactant, flux, the work such as sucking filtration, washing
Skill step, h2+n2Deng dangerous reducing atmosphere, so these all limit its application, and its luminous efficiency has limited.
Content of the invention
The problem existing for above-mentioned prior art, it is an object of the invention to provide a kind of preparation method is simple, light effect
The high white light led blue colour fluorescent powder of rate.
To achieve these goals, the technical solution used in the present invention is: a kind of white light led blue colour fluorescent powder, chemistry
Formula is sc4-4xal6si3o21:4xce3+, in formula, x is rare earth activation ion ce3+Doping sc3+Mole doping of position, its value model
Enclose: 0.001≤x≤0.700.
The preparation method of white light led blue colour fluorescent powder as above, using high temperature solid-state method, comprises the following steps:
(1) with containing scandium ion sc3+Compound, contain aluminium ion al3+Compound, contain silicon ion si4+Chemical combination
Thing, rare-earth cerium ion ce3+Compound be raw material, by molecular formula sc4-4xal6si3o21:4xce3+The chemistry meter of middle corresponding element
Amount ratio weighs each raw material, wherein 0.001≤x≤0.700；The raw material weighing is ground respectively, mix homogeneously, obtain mixture；
(2) by said mixture precalcining in air atmosphere, precalcining temperature is 100～600 DEG C, and precalcination time is
3～10 hours；
(3) after naturally cooling to room temperature, grind and mix homogeneously, in reducing atmosphere calcine, calcining heat be 800～
1300 DEG C, calcination time is 4～12 hours, after naturally cooling to room temperature, grinds and mix homogeneously, obtains fluorescent material.
In the technical scheme of high temperature solid-state method of the present invention, containing scandium ion sc3+Compound be Scia, in Scium nitrate(Sc(NO3)3)
A kind of；Containing aluminium ion al3+Compound be one of aluminium oxide, aluminum nitrate；Containing silicon ion si4+Compound be two
Silicon oxide；Containing rare-earth cerium ion ce3+Compound be one of cerium oxide, cerous nitrate；Reducing atmosphere is by activated carbon powder
Co reducing atmosphere or 95%n that burning produces2+ 5%h2Mixed gas.
One preferred version of high temperature solid-state method of the present invention is: the precalcining temperature of step (2) is 400～600 DEG C, pre-calcined
The burning time is 3～8 hours；The calcining heat of step (3) is 1200～1300 DEG C, and calcination time is 4～10 hours.
The preparation method of white light led blue colour fluorescent powder as above, using chemical synthesiss, comprises the steps:
(1) with containing scandium ion sc3+Compound, contain aluminium ion al3+Compound, contain silicon ion si4+Chemical combination
Thing, contain rare-earth cerium ion ce3+Compound be raw material, by chemical formula sc4-4xal6si3o21:4xce3+The change of middle corresponding element
Learn metering ratio and weigh each raw material, wherein 0.001≤x≤0.700；Will be containing scandium ion sc3+Compound, contain aluminium ion al3+
Compound, contain rare-earth cerium ion ce3+Compound be dissolved separately in dilute nitric acid solution, by each raw materials quality 0.5～
2.0wt% adds chelating agent respectively, stirs to its dissolving, obtain each clear solution under 60～80 DEG C of temperature conditionss；To contain
There is silicon ion si4+Compound dissolution in aqueous ethanol solution, by raw materials quality 0.5～2.0wt% add chelating agent,
Stir to dissolving under 60～80 DEG C of temperature conditionss, obtain material solution；
(2) various solution are slowly mixed together, and add the chelating agent of raw material gross mass 0.5～2.0wt%, at 60～80 DEG C
Temperature conditionss under stirring 1～2 hour after, standing, dry, obtain fluffy presoma；
(3) presoma is placed in calcining in Muffle furnace, calcines for the first time in air atmosphere, first time calcining heat is
100～500 DEG C, first time calcination time is 4～8 hours；
(4), after natural cooling, sample ground and mixed is carried out second calcining uniformly and under reducing atmosphere, forges for the second time
Burn 700～1200 DEG C of temperature, second calcination time is 5～10 hours, after natural cooling, grind and mix homogeneously, obtain glimmering
Light powder.
In the technical scheme of chemical synthesiss of the present invention, containing scandium ion sc3+Compound be Scia, in Scium nitrate(Sc(NO3)3)
A kind of；Containing aluminium ion al3+Compound be one of aluminium carbonate, aluminum nitrate；Containing rare-earth cerium ion ce3+Compound
For one of cerium oxide, cerous nitrate；Containing silicon ion si4+Compound be tetraethyl orthosilicate；Chelating agent is oxalic acid or Fructus Citri Limoniae
One of acid；Reducing atmosphere is the co reducing atmosphere or 95%n being produced by activated carbon powder burning2+ 5%h2Mixed gas.
One preferred version of chemical synthesiss of the present invention is: the first time calcining heat of step (3) is 300～500 DEG C,
First time calcination time is 4～6 hours；Second calcining heat of step (4) is 1100～1200 DEG C, second calcination time
For 5～9 hours.
The advantage of technical solution of the present invention is:
1st, the fluorescent material of this invention has efficient response characteristic to ultraviolet light, can preferably match with ultraviolet led, sends out
Project the blue light that main peak is located at 425 nanometers, can be advantageously used in and prepare white light led illuminating device；
2nd, the blue colour fluorescent powder that the present invention provides can preferably realize rare earth ion ce3+Filling, the good crystallinity of sample,
Reproducible, preparation process is simple, it is easy to operation, needed raw material wide material sources, can be effectively reduced cost；
3rd, the present invention prepares material and possesses good chemical stability and heat stability, granularity is tiny, particle size dispersion is uniform,
Good luminous performance, has high-luminous-efficiency simultaneously, is conducive to preparing high-power led；
4th, the fluorescent material color rendering propertiess of present invention preparation preferably, discharge by environmental friendliness, no waste water and gas, is suitable for continuous metaplasia
Produce.
Brief description
Fig. 1 is the sc by the preparation of the embodiment of the present invention 1 technical scheme3.996ce0.004al6si3o21The x-ray powder of material sample
Last diffracting spectrum；
Fig. 2 is the sc by the preparation of the embodiment of the present invention 1 technical scheme3.996ce0.004al6si3o21The scanning electricity of material sample
Mirror collection of illustrative plates；
Fig. 3 is the sc by the preparation of the embodiment of the present invention 1 technical scheme3.996ce0.004al6si3o21Material sample is at 425 nanometers
Light detection under the exciting light spectrogram that obtains；
Fig. 4 is the sc by the preparation of the embodiment of the present invention 1 technical scheme3.996ce0.004al6si3o21Material sample is at 355 nanometers
Light excite under luminescent spectrum figure；
Fig. 5 is the sc by the preparation of the embodiment of the present invention 1 technical scheme3.996ce0.004al6si3o21Material sample is in excitation wave
A length of 355 nanometers, monitoring wavelength is the decay of luminescence curve under 425 nanometers；
Fig. 6 is the sc by the preparation of the embodiment of the present invention 4 technical scheme2.8ce1.2al6si3o21The x-ray powder of material sample
Diffracting spectrum；
Fig. 7 is the sc by the preparation of the embodiment of the present invention 4 technical scheme2.8ce1.2al6si3o21Material sample is at 425 nanometers
The exciting light spectrogram obtaining under light detection；
Fig. 8 is the sc by the preparation of the embodiment of the present invention 4 technical scheme2.8ce1.2al6si3o21Material sample is at 355 nanometers
Light excite under luminescent spectrum figure；
Fig. 9 is the sc by the preparation of the embodiment of the present invention 4 technical scheme2.8ce1.2al6si3o21Material sample is in excitation wavelength
For 355 nanometers, monitoring wavelength is the decay of luminescence curve under 425 nanometers.
Specific embodiment
With reference to the accompanying drawings and examples technical solution of the present invention is further described.
Embodiment 1:
Preparation sc3.996ce0.004al6si3o21, according to chemical formula sc3.996ce0.004al6si3o21The chemistry meter of middle each element
Amount ratio weighs Scia sc respectively2o3: 2.762 grams, cerous nitrate ce (no3)3·6h2O:0.018 gram, aluminium oxide al2o3: 3.059
Gram, silicon dioxide sio2: 1.803 grams, in agate mortar grind and mix homogeneously after, select air atmosphere precalcining, pre-calcined
Burning temperature is 400 DEG C, and precalcination time 8 hours is subsequently cooled to room temperature, takes out sample, is fully ground and mix homogeneously, by
Calcine in the co reducing atmosphere that activated carbon powder burning produces, 1200 DEG C of calcining heat, calcination time 10 hours, be cooled to room temperature,
Take out sample, grind and mix homogeneously, that is, obtain fluorescent material.
Referring to accompanying drawing 1, it is the x-ray powder diffraction spectrum of the material sample of the technical scheme preparation by the present embodiment,
Xrd test result shows, prepared material is sc3.996ce0.004al6si3o21Material, preferably, reaction is completely for crystallinity.
Referring to accompanying drawing 2, it is the scanning electron microscope collection of illustrative plates of the material sample of the technical scheme preparation by the present embodiment, from figure
It can be seen that this sc3.996ce0.004al6si3o21Fluorescent material is spheroidal particle, and mean diameter is 2 microns, even particle size distribution.
Referring to accompanying drawing 3, it be by the technology of the present invention preparation material sample under the light detection of 425 nanometers of launching light of monitoring
The exciting light spectrogram obtaining, there it can be seen that the excites scope of this material is at 300～400 nanometers, show can well by
Ultraviolet excitation.
Referring to accompanying drawing 4, it is by lighting that the material sample of the technology of the present invention preparation obtains under 355 nanometers of light excites
Spectrogram, the centre of luminescence wavelength of this material is 425 nanometers, belongs to blue region, calculates its coordinate: x simultaneously by cie
=0.150, y=0.042, are also in blue region, show to be work perfectly well as ultraviolet, near ultraviolet excitated led blueness
Fluorescent material.
Referring to accompanying drawing 5, it is to receive in excitation light wave a length of 355 by material sample prepared by the technical scheme of the present embodiment
Rice, the decay of luminescence curve of a length of 425 nanometers of light wave of monitoring, the die-away time of this blue colour fluorescent powder can be calculated from figure
For 36 nanoseconds.
Embodiment 2:
Preparation sc3.96ce0.04al6si3o21, according to chemical formula sc3.96ce0.04al6si3o21The stoichiometric proportion of middle each element
Weigh Scium nitrate(Sc(NO3)3) sc (no respectively3)3·3h2O:3.762 gram, cerium oxide ceo2: 0.023 gram, aluminium oxide al2o3: 1.020 grams, two
Silicon oxide sio2: 0.601 gram, in agate mortar grind and mix homogeneously after, select air atmosphere precalcining, precalcining temperature
It is 100 DEG C, precalcination time 10 hours, it is subsequently cooled to room temperature, takes out sample, be fully ground and mix homogeneously, consisting of
95%n2+ 5%h2Mixed gas in calcine, 800 DEG C of calcining heat, calcination time 12 hours, be cooled to room temperature, take out sample,
Grind and mix homogeneously, that is, obtain fluorescent material.
Sample manufactured in the present embodiment, its main structural behaviour, sample topography, excitation spectrum, luminescent spectrum and decay
Curve is similar to Example 1.
Embodiment 3:
Preparation sc3.4ce0.6al6si3o21, according to chemical formula sc3.4ce0.6al6si3o21The stoichiometry score of middle each element
Another name takes Scia sc2o3: 0.470 gram, cerous nitrate ce (no3)3·6h2O:0.521 gram, aluminum nitrate al (no3)3·9h2O:
4.502 grams, silicon dioxide sio2: 0.361 gram, in agate mortar grind and mix homogeneously after, select air atmosphere precalcining,
Precalcining temperature is 600 DEG C, precalcination time 3 hours, is subsequently cooled to room temperature, takes out sample；It is fully ground and mix homogeneously,
The co reducing atmosphere being produced by activated carbon powder burning is calcined, 1300 DEG C of calcining heat, calcination time 4 hours, then cool down
To room temperature, take out sample, grind and mix homogeneously, that is, obtain fluorescent material.
Sample manufactured in the present embodiment, its main structural behaviour, sample topography, excitation spectrum, luminescent spectrum and decay
Curve is similar to Example 1.
Embodiment 4:
Preparation sc2.8ce1.2al6si3o21, according to chemical formula sc2.8ce1.2al6si3o21The stoichiometric proportion of middle each element, point
Another name takes Scium nitrate(Sc(NO3)3) sc (no3)3·3h2O:1.596 gram, cerous nitrate ce (no3)3·6h2O:1.042 gram, aluminum nitrate al (no3)3·
9h2O:4.502 gram, tetraethyl orthosilicate si (oc2h5)4: 1.250 grams.By the Scium nitrate(Sc(NO3)3) weighing sc (no3)3·3h2O, cerous nitrate ce
(no3)3·6h2O and aluminum nitrate al (no3)3·9h2O is dissolved in dilute nitric acid solution respectively, is then respectively adding each raw materials quality
The citric acid of 2.0wt%, stirs to dissolving respectively under 60 DEG C of temperature conditionss；Tetraethyl orthosilicate si (oc2h5)4It is dissolved in one
In quantitative ethanol water, and add the citric acid of raw materials quality 2.0wt%, stirring under 60 DEG C of temperature conditionss until its
Dissolving.Previously obtained various solution are mixed, adds the citric acid of raw material gross mass 2.0wt%, 60 DEG C of stirrings 2 are little
Up to being completely dissolved, stand, dry, obtain fluffy presoma；Presoma is placed in Muffle furnace in air atmosphere first
Secondary calcining, first time calcining heat is 300 DEG C, and first time calcination time is 6 hours, is cooled to room temperature, ground and mixed after taking-up
Uniformly, calcine for second in the co reducing atmosphere being produced by activated carbon powder burning, second calcining heat is 1100 DEG C, second
Secondary calcination time is 9 hours, after natural cooling, grinds and mix homogeneously, that is, obtains powder shaped fluorescent material.
Referring to accompanying drawing 6, it is the x-ray powder diffraction spectrum of the present embodiment sample, result shows that prepared material is
sc2.8ce1.2al6si3o21Material, preferably, reaction is completely for crystallinity.
Referring to accompanying drawing 7, it is to obtain in 425 nanometers of launching light of monitoring by the material sample of the present embodiment technical scheme preparation
Exciting light spectrogram, it can be seen that the excites scope of this material is based on 300～400 nanometers of ultraviolet light, with ultraviolet light
Led relatively mates.
Referring to accompanying drawing 8, it is sc2.8ce1.2al6si3o21The luminescent spectrum figure obtaining under 355 nano-ultraviolet lights excite, should
The centre of luminescence wavelength of material is 425 nanometers of blue region, calculates its coordinate: x=0.155, y=by cie simultaneously
0.031, it is also in blue region, show to be work perfectly well as ultraviolet, near ultraviolet excitated led blue colour fluorescent powder.
Referring to accompanying drawing 9, it is to be 355 nanometers by the sample of the embodiment of the present invention 4 technical scheme preparation in excitation wavelength, prison
Survey the decay of luminescence curve that wavelength is under 425 nanometers, the die-away time that can calculate fluorescent material from figure was 30 nanoseconds.
Embodiment 5:
Preparation sc2ce2al6si3o21, according to chemical formula sc2ce2al6si3o21The stoichiometric proportion of middle each element, claims respectively
Take Scia sc2o3: 0.277 gram, cerium oxide ceo2: 0.689 gram, aluminum nitrate al (no3)3·9h2O:4.502 gram, positive silicic acid second
Ester si (oc2h5)4: 1.250 grams.By the Scia weighing sc2o3, cerium oxide ceo2And aluminum nitrate al (no3)3·9h2O is respectively
It is dissolved in dilute nitric acid solution, is then respectively adding the oxalic acid of each raw materials quality 0.5wt%, stir under 80 DEG C of temperature conditionss respectively
Mix to dissolving；Tetraethyl orthosilicate si (oc2h5)4It is dissolved in a certain amount of ethanol water, and add raw materials quality 0.5wt%
Oxalic acid, stir under 80 DEG C of temperature conditionss to its dissolving.Previously obtained various solution are mixed, adds raw material
The oxalic acid of gross mass 0.5wt%, stirring under the conditions of 80 DEG C is completely dissolved for 1 hour to it, and standing is dried, obtained fluffy forerunner
Body；Presoma is placed in Muffle furnace and calcines for the first time in air atmosphere, first time calcining heat is 100 DEG C, forges for the first time
The burning time is 8 hours, is cooled to room temperature, and after taking-up, ground and mixed uniformly, is consisting of 95%n2+ 5%h2Mixed gas in
Secondary clacining, second calcining heat is 700 DEG C, and second calcination time is 10 hours, that is, obtain powder shaped fluorescent material.
Sample manufactured in the present embodiment, its main structural behaviour, sample topography, excitation spectrum, luminescent spectrum and decay
Curve is similar to Example 4.
Embodiment 6:
Preparation sc1.2ce2.8al6si3o21, according to chemical formula sc1.2ce2.8al6si3o21The stoichiometric proportion of middle each element, point
Another name takes Scium nitrate(Sc(NO3)3) sc (no3)3·3h2O:0.684 gram, cerous nitrate ce (no3)3·6h2O:2.431 gram, aluminium carbonate al2(co3)3:
1.404 grams, tetraethyl orthosilicate si (oc2h5)4: 1.250 grams.By the Scium nitrate(Sc(NO3)3) weighing sc (no3)3·3h2O, cerous nitrate ce
(no3)3·6h2O and aluminium carbonate al2(co3)3It is dissolved in respectively in dilute nitric acid solution, be then respectively adding each raw materials quality
The oxalic acid of 1.5wt%, stirs to dissolving respectively under 70 DEG C of temperature conditionss；Tetraethyl orthosilicate si (oc2h5)4It is dissolved in certain
In the ethanol water of amount, and add the oxalic acid of raw materials quality 1.5wt%, stirring under 70 DEG C of temperature conditionss is until it is molten
Solution.Previously obtained various solution are mixed, adds the oxalic acid of raw material gross mass 1.5wt%, 70 DEG C are stirred 1.5 hours
To being completely dissolved, stand, dry, obtain fluffy presoma；Presoma is placed in Muffle furnace in air atmosphere for the first time
Calcining, first time calcining heat is 500 DEG C, and first time calcination time is 4 hours, is cooled to room temperature, after taking-up, ground and mixed is equal
Even, calcine for second in the co reducing atmosphere being produced by activated carbon powder burning, second calcining heat is 1200 DEG C, second
Calcination time is 5 hours, after natural cooling, grinds and mix homogeneously, that is, obtains powder shaped fluorescent material.
Sample manufactured in the present embodiment, its main structural behaviour, sample topography, excitation spectrum, luminescent spectrum and decay
Curve is similar to Example 4.
Claims (7)
1. a kind of white light led blue colour fluorescent powder it is characterised in that: chemical formula be sc4-4xal6si3o21:4xce3+, in formula, x is
Rare earth activation ion ce3+Doping sc3+Mole doping of position, its span: 0.001≤x≤0.700.
2. a kind of preparation method of white light led blue colour fluorescent powder as claimed in claim 1 is it is characterised in that adopt high temperature solid
Xiang Fa, comprises the following steps:
(1) with containing scandium ion sc3+Compound, contain aluminium ion al3+Compound, contain silicon ion si4+Compound,
Rare-earth cerium ion ce3+Compound be raw material, by molecular formula sc4-4xal6si3o21:4xce3+The stoichiometric proportion of middle corresponding element
Weigh each raw material, wherein 0.001≤x≤0.700；The raw material weighing is ground respectively, mix homogeneously, obtain mixture；
(2) by said mixture precalcining in air atmosphere, precalcining temperature be 100～600 DEG C, precalcination time be 3～
10 hours；
(3) after naturally cooling to room temperature, grind and mix homogeneously, calcine in reducing atmosphere, calcining heat is 800～1300
DEG C, calcination time is 4～12 hours, after naturally cooling to room temperature, grinds and mix homogeneously, obtains fluorescent material.
3. white light led blue colour fluorescent powder according to claim 2 preparation method it is characterised in that: described contains
Scandium ion sc3+Compound be one of Scia, Scium nitrate(Sc(NO3)3)；Described containing aluminium ion al3+Compound be oxidation
One of aluminum, aluminum nitrate；Described containing silicon ion si4+Compound be silicon dioxide；Described contains rare-earth cerium ion
ce3+Compound be one of cerium oxide, cerous nitrate；Described reducing atmosphere is the co also Primordial Qi being produced by activated carbon powder burning
Atmosphere or 95%n2+ 5%h2Mixed gas.
4. white light led blue colour fluorescent powder according to claim 2 preparation method it is characterised in that: described step (2)
Precalcining temperature be 400～600 DEG C, precalcination time be 3～8 hours；The calcining heat of step (3) is 1200～1300
DEG C, calcination time is 4～10 hours.
5. a kind of preparation method of white light led blue colour fluorescent powder as claimed in claim 1 is it is characterised in that closed using chemistry
Cheng Fa, comprises the steps:
(1) with containing scandium ion sc3+Compound, contain aluminium ion al3+Compound, contain silicon ion si4+Compound,
Containing rare-earth cerium ion ce3+Compound be raw material, by chemical formula sc4-4xal6si3o21:4xce3+The chemistry meter of middle corresponding element
Amount ratio weighs each raw material, wherein 0.001≤x≤0.700；Will be containing scandium ion sc3+Compound, contain aluminium ion al3+Change
Compound, contain rare-earth cerium ion ce3+Compound be dissolved separately in dilute nitric acid solution, by each raw materials quality 0.5～
2.0wt% adds chelating agent respectively, stirs to its dissolving, obtain each clear solution under 60～80 DEG C of temperature conditionss；To contain
There is silicon ion si4+Compound dissolution in aqueous ethanol solution, by raw materials quality 0.5～2.0wt% add chelating agent,
Stir to dissolving under 60～80 DEG C of temperature conditionss, obtain material solution；
(2) various solution are slowly mixed together, and add the chelating agent of raw material gross mass 0.5～2.0wt%, in 60～80 DEG C of temperature
After stirring 1～2 hour under the conditions of degree, standing, dry, obtain fluffy presoma；
(3) presoma being placed in Muffle furnace calcining, calcine for the first time in air atmosphere, first time calcining heat is 100～
500 DEG C, first time calcination time is 4～8 hours；
(4) after natural cooling, sample ground and mixed is carried out second calcining uniformly and under reducing atmosphere, calcine temperature second
700～1200 DEG C of degree, second calcination time is 5～10 hours, after natural cooling, grinds and mix homogeneously, obtains fluorescent material.
6. the white light led blue colour fluorescent powder according to claims 5 preparation method it is characterised in that: described contains
There is scandium ion sc3+Compound be one of Scia, Scium nitrate(Sc(NO3)3)；Described containing aluminium ion al3+Compound be carbonic acid
One of aluminum, aluminum nitrate；Described containing rare-earth cerium ion ce3+Compound be one of cerium oxide, cerous nitrate；Described
Containing silicon ion si4+Compound be tetraethyl orthosilicate；Described chelating agent is one of oxalic acid or citric acid；Described reduction
Atmosphere is the co reducing atmosphere or 95%n being produced by activated carbon powder burning2+ 5%h2Mixed gas.
7. white light led blue colour fluorescent powder according to claim 5 preparation method it is characterised in that: described step (3)
First time calcining heat be 300～500 DEG C, first time calcination time be 4～6 hours；Second calcining heat of step (4)
For 1100～1200 DEG C, second calcination time is 5～9 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510126697.1A CN104774614B (en) | 2015-03-20 | 2015-03-20 | Blue fluorescent powder for white-light LED and preparation method thereof |
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| CN201510126697.1A CN104774614B (en) | 2015-03-20 | 2015-03-20 | Blue fluorescent powder for white-light LED and preparation method thereof |
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| CN104774614A CN104774614A (en) | 2015-07-15 |
| CN104774614B true CN104774614B (en) | 2017-01-18 |
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| WO2004082032A2 (en) * | 2003-03-13 | 2004-09-23 | Osram Opto Semiconductors Gmbh | Luminescence conversion of led with phosphorescence effect and use thereof |
| JP2005330348A (en) * | 2004-05-19 | 2005-12-02 | Shin Etsu Chem Co Ltd | Cerium-containing oxide |
| CN104250555A (en) * | 2013-06-27 | 2014-12-31 | 宁波升谱光电半导体有限公司 | Yellow fluorescent powder and preparation method thereof and light emitting device using fluorescent powder |
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| WO2004082032A2 (en) * | 2003-03-13 | 2004-09-23 | Osram Opto Semiconductors Gmbh | Luminescence conversion of led with phosphorescence effect and use thereof |
| JP2005330348A (en) * | 2004-05-19 | 2005-12-02 | Shin Etsu Chem Co Ltd | Cerium-containing oxide |
| CN104250555A (en) * | 2013-06-27 | 2014-12-31 | 宁波升谱光电半导体有限公司 | Yellow fluorescent powder and preparation method thereof and light emitting device using fluorescent powder |
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