CN105754599A - Monoclinic-system-structured superfine white nano fluorescent powder and preparation method thereof - Google Patents

Monoclinic-system-structured superfine white nano fluorescent powder and preparation method thereof Download PDF

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CN105754599A
CN105754599A CN201610135958.0A CN201610135958A CN105754599A CN 105754599 A CN105754599 A CN 105754599A CN 201610135958 A CN201610135958 A CN 201610135958A CN 105754599 A CN105754599 A CN 105754599A
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仝玉萍
王富强
符静
张存民
王清云
韩爱红
刘丽
霍洪媛
张建华
宋鹏飞
马军涛
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North China University of Water Resources and Electric Power
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    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7792—Aluminates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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Abstract

The invention relates to monoclinic-system-structured superfine white nano fluorescent powder and a preparation method thereof.The average particle size of the fluorescent powder is 65-75 nanometers, each single particle sequentially comprises four layers of fluorescent substances, the four layers of fluorescent substances have the same crystal structure and different chemical components, the chemical formula of each layer of fluorescent substances is Y2Si1-xEuxO5, x is the mole doping amount of Eu3+ doping, and 0.05</=X</=0.30.The fluorescent powder can emit light with the wavelength being 580-625 nanometers under the excitation of ultraviolet with the wavelength being 385-415 nanometers.The fluorescent powder is good in heat stability, good in chemical stability, and the like.The preparation method has the advantages that the method is simple, easy in raw material obtaining, low in synthesizing temperature, simple and controllable in process and suitable for large-scale production, and the obtained product is good in ion dispersity and even in particle size distribution.

Description

A kind of superfine white nano-phosphor of monoclinic structure and preparation method thereof
Technical field
The present invention relates to fluorescent material field, especially, relate to the superfine white nanometer of a kind of monoclinic structure Fluorescent material and preparation method thereof.
Background technology
Along with the exhaustion increasingly of earth fossil resource, the appearance of white light LEDs is with its high brightness, and the high life is gradually Substitute daily osram lamp, become the lighting system that the mankind are new.Ya chemical company takes the lead in blueness for 1993 Break through in GaN base LED technology, and quickly industrialization, developed white light LEDs in 1996, within 1998, push away Upper market, causes insider and pays close attention to greatly.Compared with conventional illumination sources, white light LEDs has many Advantage, such as: volume is little, less energy consumption, response are fast, life-span length, pollution-free etc..White light LEDs many excellent Point so that it is application in daily life is increasing, such as background illumination, traffic lights, total colouring And general lighting etc., there are huge following illumination market and notable Energy-saving Perspective.
And the fluorescent material material that to be white light LEDs the most crucial, its performance directly affect the brightness of white light LEDs, The performance indications such as chromaticity coordinates, colour temperature and colour rendering.In the evolution of fluorescent material, metal ion is utilized to mix Miscellaneous is one of method preparing colored organic pigments, and the most conventional metal ion is Cr3+, Fe3+Deng, but Containing Cr3+Pigment there is certain toxicity, therefore use and be restricted.The coloring of the transition metals such as Fe Effect is significantly affected by the change of ligancy and the impact of the character of adjacent ions, it is difficult to reliably, stably control Hair color effect.Rare earth element, because of its special electron configuration, can select to absorb visible ray and colour, and Rare earth element changes crystal phase structure as Doped ions and pigment plays a part variable color, steady look and helps look, Pigment art has important purposes.China's rare earth element unbalanced supply-demand, neodymium, praseodymium, dysprosium, terbium etc. at present Supply falls short of demand, expensive；And the fractional yield such as yttrium, lanthanum is enriched, cheap.Rare earth element substitutes certain A little heavy metal elements are doped and can solve problem of environmental pollution well, to reach friendly environment society Purpose.
A kind of rare-earth activated Y of the patent application publication of Application No. 03149639.32SiO5Fluorescent material and preparation thereof Method, obtained fluorescent material has the advantage that luminous intensity is high, powder particle size is controlled, particle surface is smooth. But in preparation process, elapsed time is long, complex operation step, if large-scale production, it is difficult to ensure that matter Amount, and synthesis temperature is high, needs to calcine at 800-1600 DEG C, is unfavorable for industrialized production.
Summary of the invention
For solving the problems referred to above, the invention provides the superfine white nano-phosphor of a kind of monoclinic structure And preparation method thereof, this nano-phosphor is that Eu is doped into Y2SiO5In lattice, synthesize at a lower temperature The environment friendly inorganic pigment of high brightness, is suitable to large-scale production.Meanwhile, its preparation method technique is simple, instead Answering temperature low, preparation time is the shortest.
The present invention solves that above-mentioned technical problem be employed technical scheme comprise that the ultra-fine of a kind of monoclinic structure White nano-phosphor, its average grain diameter is 65～75nm, and individual particle is the most successively by crystal structure The fluorescent material composition of four layers that identical and chemical constituent is different, in the fluorescent material of described four layers, each layer is glimmering The chemical formula of stimulative substance is Y2Si1-xEuxO5, wherein x is Eu3+Mole doping of doping, and 0.05≤X ≤0.30；This fluorescent material is under the ultraviolet excitation that wavelength is 385～415nm, and sending wavelength is 580～62 The light of 5nm.
Preferably, described chemical formula is Y2Si1-xEuxO5, wherein 0.10≤X≤0.20.
In any of the above-described scheme preferably, described chemical formula is Y2Si1-xEuxO5Structure, wherein 0.10 ≤X≤0.15。
Additionally, present invention also offers the preparation method of the superfine white nano-phosphor of this monoclinic structure, Comprise the following steps:
(1) according to Y2Si1-xEuxO5In the stoichiometric proportion of each element, take corresponding Na respectively2SiO3·5H2O、 Eu(NO3)3·6H2O、Y(NO3)3·6H2O is dissolved in 100mL water and obtains mixed solution；
(2) mixed solution obtained in above-mentioned steps (1) is joined going of the glycine that dissolved in advance In the aqueous solution of ion, maintain the temperature at 60 DEG C, stir at least 1 hour；
(3) mixed solution of above-mentioned steps (2) is concentrated 120 DEG C of burnings, add lubricant, lubricant Addition with by ball milling system keep dispersion be limited, grind afterwards, be dried, obtain precursor powder；
(4) precursor powder that above-mentioned steps (3) obtains is directly placed in graphite crucible calcining, calcining Temperature is 700～900 DEG C, calcines 2～4 hours, sieves, obtain the fluorescent powder of semi-finished product；
(5) choose the fluorescent powder of the semi-finished product prepared by step (4) of 40% weight, wherein add hard Baton round mixes, and with the rotating speed batch mixings 2 of 10～20 revs/min～4 hours, adds 20% weight the most wherein The fluorescent powder of the semi-finished product prepared by step (4), continue with rigid plastic balls batch mixing 2～4 hours, Stop mixing being grown 2～4 hours at a temperature of 1200 DEG C～1300 DEG C by mixture；Then it is further continued for adding The fluorescent powder of the semi-finished product prepared by step (4) of 20% weight, with rigid plastic balls batch mixing 2～4 hours, Stop mixing being grown 2～4 hours at a temperature of 1200 DEG C～1300 DEG C by mixture；Finally, add The fluorescent powder of the semi-finished product prepared by step (4) of 20% weight, with rigid plastic balls batch mixing 1～3 hours, Stop mixing being grown 1～3 hour at a temperature of 1200 DEG C～1300 DEG C by mixture, final prepared four layers of knot The superfine white nano-phosphor of the monoclinic structure of structure.
Preferably, described step (1) being Y:(Si+Eu according to mol ratio)=2:1 to be to mix above-mentioned unit Element；
In any of the above-described scheme preferably, in described step (2), mixing speed is 80 revs/min～100 Rev/min, mixing time is 1.5～2h.
In any of the above-described scheme preferably, in described step (3), lubricant is acetone or alcohol.
In any of the above-described scheme preferably, the calcining heat in described step (4) is 750～850 DEG C.
In any of the above-described scheme preferably, for every 200 kilograms of material add 10 in described step (5) Baton round, each baton round a diameter of 8～10cm.
Beneficial effects of the present invention:
1. the fluorescent material of the present invention has the strongest fluorescence activity, and bright in colour, and Doped ions enters monocline In crystal structure, form the solid solution of single stable, it is difficult to dissolution, and luminous intensity is high, has thermally-stabilised Get well, chemical stability is good, bright in colour, the non-discoloring advantage of high temperature；
2. the toxic element such as the most leaded chromium, environmental protection in the product of the present invention；
Preparation method the most of the present invention is simple, and raw material is easy to get, products therefrom particle good dispersion, granularity Being evenly distributed, colour generation is good, and synthesis temperature is low, and technique is the most controlled, is suitable to large-scale production.
Brief Description Of Drawings
The present invention will be further described in detail with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is the superfine white nano-phosphor Y of the monoclinic structure of the present invention2Si1-xEuxO5X penetrate Ray diffraction diagram is composed, wherein x=0,0.05,0.10,0.15,0.20,0.30, and abscissa is the angle of diffraction, vertical seat It is designated as diffracted intensity；
Fig. 2 is the superfine white nano-phosphor of the monoclinic structure of the present invention under different temperatures Y2Si0.9Eu0.1O5The XRD of powder；
Fig. 3 is the superfine white nano-phosphor of the monoclinic structure of the present invention at 800 DEG C Y2Si0.9Eu0.1O5The scanning electron microscope (SEM) photograph of powder different amplification；30,000 times the most successively, 50,000 times, 80000 times, 100,000 times；
Fig. 4 is the superfine white nano-phosphor Y of the monoclinic structure of the present invention2Si0.9Eu0.1O5Powder exists EDS figure at 800 DEG C.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is further described, but claimed model Enclose and be not limited thereto.
The superfine white nano-phosphor of a kind of monoclinic structure, its average grain diameter is 65～75nm, single Particle the most successively by crystal structure is identical and chemical constituent is different that the fluorescent material of four layers forms, institute State the chemical formula of each layer of fluorescent material in the fluorescent material of four layers and be Y2Si1-xEuxO5, wherein x is Eu3+Mix Miscellaneous mole doping, and 0.05≤X≤0.30；This fluorescent material is at the ultraviolet light that wavelength is 385～415nm Excite down, send the light that wavelength is 580～625nm.
Wherein 0.10≤X≤0.20, is further 0.10≤X≤0.15.
Additionally, the preparation method of the superfine white nano-phosphor of this monoclinic structure, comprise the following steps:
(1) according to Y2Si1-xEuxO5In the stoichiometric proportion of each element, take corresponding Na respectively2SiO3·5H2O、 Eu(NO3)3·6H2O、Y(NO3)3·6H2O is dissolved in 100mL water and obtains mixed solution；
(2) mixed solution obtained in above-mentioned steps (1) is joined going of the glycine that dissolved in advance In the aqueous solution of ion, maintain the temperature at 60 DEG C, stir at least 1 hour；
(3) mixed solution of above-mentioned steps (2) is concentrated 120 DEG C of burnings, add lubricant, lubricant Addition with by ball milling system keep dispersion be limited, grind afterwards, be dried, obtain precursor powder；
(4) precursor powder that above-mentioned steps (3) obtains is directly placed in graphite crucible calcining, calcining Temperature is 700～900 DEG C, calcines 2～4 hours, sieves, obtain the fluorescent powder of semi-finished product；
(5) choose the fluorescent powder of the semi-finished product prepared by step (4) of 40% weight, wherein add hard Baton round mixes, and with the rotating speed batch mixings 2 of 10～20 revs/min～4 hours, adds 20% weight the most wherein The fluorescent powder of the semi-finished product prepared by step (4), continue with rigid plastic balls batch mixing 2～4 hours, Stop mixing being grown 2～4 hours at a temperature of 1200 DEG C～1300 DEG C by mixture；Then it is further continued for adding The fluorescent powder of the semi-finished product prepared by step (4) of 20% weight, with rigid plastic balls batch mixing 2～4 hours, Stop mixing being grown 2～4 hours at a temperature of 1200 DEG C～1300 DEG C by mixture；Finally, add The fluorescent powder of the semi-finished product prepared by step (4) of 20% weight, with rigid plastic balls batch mixing 1～3 hours, Stop mixing being grown 1～3 hour at a temperature of 1200 DEG C～1300 DEG C by mixture, final prepared four layers of knot The superfine white nano-phosphor of the monoclinic structure of structure.
Described step (1) is Y:(Si+Eu according to mol ratio)=2:1 to be to mix above-mentioned element；
In described step (2), mixing speed is 80 revs/min～100 revs/min, and mixing time is 1.5～2h.
In described step (3), lubricant is acetone or alcohol.
Calcining heat in described step (4) is 750～850 DEG C.
For every 200 kilograms of material add 10 baton rounds in described step (5), each baton round a diameter of 8～ 10cm。
Described step (4) is to calcine in reducing environment；Wherein, this reducing environment is for strictly controlling volume ratio H2∶N2=1: 5, ratio is excessive or the too small superfine white nano-phosphor that all can affect this monoclinic structure Illumination effect.
Embodiment 1
0.22g europium nitrate, 7.66g yttrium nitrate and 2.70g sodium metasilicate are added in 100ml water stirring obtain Solution 1.Glycine 3.08g is added in 50ml water obtain solution 2, solution 1 is poured in solution 2, At 60 DEG C, stir to clarify solution 3, utilize supersonic oscillations to stir with the speed of 80 revs/min～100 revs/min 1.5 hours, then condensed combustion at 120 DEG C, obtained precursor powder.And by precursor powder at 800 DEG C Calcining 4 hours, the rate of heat addition is 15 DEG C/min, then grind 1 hour, more as stated above in residue Concrete steps obtain monoclinic structure Y2Si0.9Eu0.1O5Inorganic fluorescent powder.
Embodiment 2
0.45g europium nitrate, 7.66g yttrium nitrate and 2.56g sodium metasilicate are added in 100ml water stirring obtain Solution 1.Glycine 3.15g is added in 50ml water obtain solution 2, solution 1 is poured in solution 2, At 60 DEG C, stir to clarify solution 3, utilize supersonic oscillations to stir with the speed of 80 revs/min～100 revs/min 1.5 hours, then condensed combustion at 120 DEG C, obtained precursor powder.And by precursor powder at 800 DEG C Calcining 4 hours, the rate of heat addition is 15 DEG C/min, then grind 1 hour, more as stated above in residue Concrete steps obtain monoclinic structure Y2Si0.9Eu0.1O5Inorganic fluorescent powder.
Embodiment 3
0.67g europium nitrate, 7.66g yttrium nitrate and 2.42g sodium metasilicate are added in 100ml water stirring obtain Solution 1.Glycine 3.23g is added in 50ml water obtain solution 2, solution 1 is poured in solution 2, At 60 DEG C, stir to clarify solution 3, utilize supersonic oscillations to stir with the speed of 80 revs/min～100 revs/min 1.5 hours, then condensed combustion at 120 DEG C, obtained precursor powder.And by precursor powder at 800 DEG C Calcining 4 hours, the rate of heat addition is 15 DEG C/min, then grind 1 hour, more as stated above in residue Concrete steps obtain monoclinic structure Y2Si0.85Eu0.15O5Inorganic fluorescent powder.
Embodiment 4
0.89g europium nitrate, 7.66g yttrium nitrate and 2.27g sodium metasilicate are added in 100ml water stirring obtain Solution 1.Glycine 3.30g is added in 50ml water obtain solution 2, solution 1 is poured in solution 2, At 60 DEG C, stir to clarify solution 3, utilize supersonic oscillations to stir with the speed of 80 revs/min～100 revs/min 1.5 hours, then condensed combustion at 120 DEG C, obtained precursor powder.And by precursor powder at 800 DEG C Calcining 4 hours, the rate of heat addition is 15 DEG C/min, then grind 1 hour, more as stated above in residue Concrete steps obtain monoclinic structure Y2Si0.8Eu0.2O5Inorganic fluorescent powder.
Embodiment 5
1.34g europium nitrate, 7.66g yttrium nitrate and 2.84g sodium metasilicate are added in 100ml water stirring obtain Solution 1.Glycine 3.45g is added in 50ml water obtain solution 2, solution 1 is poured in solution 2, At 60 DEG C, stir to clarify solution 3, utilize supersonic oscillations to stir with the speed of 80 revs/min～100 revs/min 1.5 hours, then condensed combustion at 120 DEG C, obtained precursor powder.And by precursor powder at 800 DEG C Calcining 4 hours, the rate of heat addition is 15 DEG C/min, then grind 1 hour, more as stated above in residue Concrete steps obtain monoclinic structure Y2Si0.7Eu0.3O5Inorganic fluorescent powder.
Embodiment 6
0.45g europium nitrate, 7.66g yttrium nitrate and 2.56g sodium metasilicate are added in 100ml water stirring obtain Solution 1.Glycine 3.15g is added in 50ml water obtain solution 2, solution 1 is poured in solution 2, At 60 DEG C, stir to clarify solution 3, utilize supersonic oscillations to stir with the speed of 80 revs/min～100 revs/min 1.5 hours, then condensed combustion at 120 DEG C, obtained precursor powder.And by precursor powder at 800 DEG C Calcining 4 hours, the rate of heat addition is 15 DEG C/min, then grind 1 hour, more as stated above in residue Concrete steps obtain monoclinic structure Y2Si0.9Eu0.1O5Inorganic fluorescent powder.
Eu is used in the above embodiment of the present invention3+Ion doping, Eu3+The radius of ion is 0.092nm.
Its structure of white fluorescent powder synthesized in the above embodiment of the present invention is monoclinic system type.
According to the present invention stoichiometric monoclinic system superfine fluorescent powder powder, when 0.05≤x≤0.30, pigment Color be white, if x is less than 0.05, then its color is the lightest, and colourity is too low, it is impossible to as fluorescent material Use.Whereas if x is more than 0.3, then colourity and the brightness of pigment is not significantly increased, and on the contrary can Slightly reduce.Understanding in conjunction with XRD, after exceeding certain doping, product is no longer single solid solution, But other crystalline phases occur.
Test example
XRD tests
Product prepared by different addition quantity is carried out XRD analysis, as shown in Figure 1.Result understands: when The volume x of Eu is when 0.10～0.15, and the diffracted intensity at peak persistently rises.Products therefrom structure is complete with matrix Unanimously, for the monoclinic structure of single-phase.As the volume x > 0.2 of Eu, begin with impurity peaks and occur, And along with the increase of volume, the diffracted intensity of product the most significantly strengthens.
When other conditions are the most identical, Y under different calcining heats2Si0.9Eu0.1O5The XRD of products therefrom As shown in Figure 2.Can be seen that equal energy success synthetic product at four temperature, along with the knot of the increase product of temperature Crystalline substance is become better and better, and it is preferable calcining heat that overall economic efficiency selects 800 DEG C.
SEM tests
By ESEM, product being carried out micro-structural test, it is Y that Fig. 3 show2Si0.9Eu0.1O5SEM Photo, the explanation of this photo is good by the material scatter synthesized by this doping method, even particle size distribution.Right For fluorescent material, granularity is the least, and particle specific surface is the biggest, and specific surface energy is the highest, in addition material scatter Good, in use it is easily formed uniform coating, and adhesive force is strong, evenness.
EDS analyzes
By energy disperse spectroscopy, product is carried out face constituent to be tested, as shown in Figure 4.This figure explanation Product after doping is made up of tri-kinds of elements of element Y, Eu, Si, O and surface distributed is visibly homogeneous, does not has Chemistry segregation phenomena occurs.From figure, we can also become apparent from: atomic ratio Y:(Eu+Si) about For 2:1, meet stoichiometric proportion.
The fluorescent material of the present invention has the strongest fluorescence activity, and bright in colour, and Doped ions enters monoclinic crystal In architecture, form the solid solution of single stable, it is difficult to dissolution, and luminous intensity be high, have thermally-stabilised good, Chemical stability is good, bright in colour, the non-discoloring advantage of high temperature.Additionally, it is the most leaded in the product of the present invention The toxic element such as chromium, environmental protection.
Preparation method of the present invention is simple, and raw material is easy to get, and products therefrom particle good dispersion, granularity are divided Cloth is uniform, and colour generation is good, and synthesis temperature is low, and technique is the most controlled, is suitable to large-scale production.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees other form Limiting, any those skilled in the art are changed possibly also with the technology contents of the disclosure above or are changed Type is the Equivalent embodiments of equivalent variations.But it is every without departing from technical solution of the present invention content, according to this Any simple modification, equivalent variations and the remodeling that above example is made by bright technical spirit, still falls within this The protection domain of inventive technique scheme.

Claims (9)

1. the superfine white nano-phosphor of a monoclinic structure, it is characterized in that, its average grain diameter is 65～75nm, individual particle the most successively by crystal structure is identical and chemical constituent is different that the fluorescent material of four layers forms, in the fluorescent material of described four layers, the chemical formula of each layer of fluorescent material is Y2Si1-xEuxO5, wherein x is Eu3+Mole doping of doping, and 0.05≤X≤0.30；This fluorescent material, under the ultraviolet excitation that wavelength is 385～415nm, sends the light that wavelength is 580～625nm.
The superfine white nano-phosphor of monoclinic structure the most according to claim 1, it is characterised in that described chemical formula is Y2Si1-xEuxO5, wherein 0.10≤X≤0.20.
The superfine white nano-phosphor of monoclinic structure the most according to claim 1, it is characterised in that described chemical formula is Y2Si1-xEuxO5Structure, wherein 0.10≤X≤0.15.
4. the preparation method according to the superfine white nano-phosphor of the monoclinic structure described in claim 1-3, it is characterised in that comprise the following steps:
(1) according to Y2Si1-xEuxO5In the stoichiometric proportion of each element, take corresponding Na respectively2SiO3·5H2O、Eu(NO3)3·6H2O、Y(NO3)3·6H2O is dissolved in 100mL water and obtains mixed solution；
(2) mixed solution obtained in above-mentioned steps (1) is joined in the deionized aqueous solution of the glycine dissolved in advance, maintain the temperature at 60 DEG C, stir at least 1 hour；
(3) being concentrated 120 DEG C of burnings by the mixed solution of above-mentioned steps (2), add lubricant, the addition of lubricant, to be kept dispersion to be limited by ball milling system, is ground afterwards, is dried, obtain precursor powder；
(4) precursor powder that above-mentioned steps (3) obtains being directly placed in graphite crucible calcining, calcining heat is 700～900 DEG C, calcines 2～4 hours, sieves, obtain the fluorescent powder of semi-finished product；
(5) fluorescent powder of the semi-finished product prepared by step (4) of 40% weight is chosen, wherein add rigid plastic balls mixing, with the rotating speed batch mixings 2 of 10～20 revs/min～4 hours, add the fluorescent powder of the semi-finished product prepared by step (4) of 20% weight the most wherein, continue, with rigid plastic balls batch mixing 2～4 hours, to stop mixing and grown 2～4 hours at a temperature of 1200 DEG C～1300 DEG C by mixture；Then it is further continued for adding the fluorescent powder of the semi-finished product prepared by step (4) of 20% weight, with rigid plastic balls batch mixing 2～4 hours, stops mixing and mixture is grown 2～4 hours at a temperature of 1200 DEG C～1300 DEG C；Finally, add the fluorescent powder of the semi-finished product prepared by step (4) of 20% weight, with rigid plastic balls batch mixing 1～3 hours, stop mixing being grown 1～3 hour at a temperature of 1200 DEG C～1300 DEG C by mixture, the superfine white nano-phosphor of the final monoclinic structure preparing four-layer structure.
Preparation method the most according to claim 4, it is characterised in that be Y:(Si+Eu according to mol ratio in described step (1))=2:1 to be to mix above-mentioned element.
6. according to the preparation method described in claim 4 or 5, it is characterised in that in described step (2), mixing speed is 80 revs/min～100 revs/min, and mixing time is 1.5～2h.
7. according to the preparation method described in claim 4 or 5 or 6, it is characterised in that in described step (3), lubricant is acetone or alcohol.
8. according to the preparation method described in claim 4 or 5 or 6 or 7, it is characterised in that the calcining heat in described step (4) is 750～850 DEG C.
9. according to the preparation method described in claim 4 or 5 or 6 or 7 or 8, it is characterised in that for every 200 kilograms of material add 10 baton rounds, each baton round a diameter of 8～10cm in described step (5).
CN201610135958.0A 2016-03-10 2016-03-10 Monoclinic-system-structured superfine white nano fluorescent powder and preparation method thereof Pending CN105754599A (en)

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