CN108997998A - Fluorescent powder grain of monodispersed core-shell structural and preparation method thereof - Google Patents
Fluorescent powder grain of monodispersed core-shell structural and preparation method thereof Download PDFInfo
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- CN108997998A CN108997998A CN201710417073.4A CN201710417073A CN108997998A CN 108997998 A CN108997998 A CN 108997998A CN 201710417073 A CN201710417073 A CN 201710417073A CN 108997998 A CN108997998 A CN 108997998A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- 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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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Abstract
The invention discloses fluorescent powder grains of a kind of monodispersed core-shell structural and preparation method thereof.Fluorescent powder grain includes centrally located nuclear structure and the shell structure for coating the nuclear structure, and nuclear structure is the oxidate microspheres of uniform particle diameter, and shell structure is phosphor powder layer, and the refractive index of nuclear structure is less than the refractive index of shell structure.Compared with the prior art fluorescent powder is at low cost, and good dispersion, particle diameter distribution are uniform, pattern is uniform, light extraction efficiency is high.
Description
Technical field
The invention belongs to the fluorescent powder grain of luminescent material technical field more particularly to a kind of monodispersed core-shell structural and
Preparation method.
Background technique
Phosphor material powder is widely used in the fields such as illumination, display, projection, in certain special application fields, it is desirable that
Fluorescent powder grain has micron-sized big partial size and monodispersity is good, i.e. uniform particle sizes, regular appearance, good dispersion, with full
The special light that goes out of foot requires.
However, the fluorescent powder grain that traditional high temperature solid-state method is prepared is easy to reunite, and particle diameter distribution is uneven, surface
Pattern is different, and partial size appropriate could be obtained by needing repeatedly repeatedly ball milling to be sieved, but the defect and introducing that mechanical milling process generates
Impurity can damage the luminous efficiency of fluorescent powder.Although can be made up using fluorescent powder prepared by sol-gel method, hydrothermal synthesis method
The deficiency of high temperature solid-state method synthesis can prepare monodispersed fluorescent powder, but the fluorescent powder grain prepared belongs to nanoscale, no
Suitable for preparing the big partial size fluorescent powder of micron order.
In addition, fluorescent powder is directly exposed to air when in use without encapsulation in certain specific applications
In, at this time the light emission rate of fluorescent powder be also influence its application effect an important factor for therefore, in view of the above deficiencies, it is really necessary to mention
For a kind of preparation method of monodispersed fluorescent powder micron particles, to meet the special applications demand of fluorescent powder.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of fluorescence of monodispersed core-shell structural
Powder particles and preparation method thereof, to prepare uniform particle sizes, good dispersion and the uniform big partial size fluorescent powder grain of pattern.Specific side
Case is as follows:
The present invention provides a kind of fluorescent powder grain of monodispersed core-shell structural, and the fluorescent powder grain includes being located at center
Nuclear structure and coat the shell structure of the nuclear structure, the nuclear structure is the oxidate microspheres of uniform particle diameter, the shell structure
For phosphor powder layer, the refractive index of the nuclear structure is less than the refractive index of the shell structure.
Preferably, the oxidate microspheres particle size is 5-30um.
Preferably, the phosphor powder layer with a thickness of 0.05-2um.
Preferably, the oxidate microspheres are silica, aluminum oxide, any one in magnesia.
Preferably, the phosphor powder layer is the fluorescent powder of garnet structure.
Preferably, the material of the phosphor powder layer is Y3Al5O12:Ce3+, Ca3Sc2Si3O12:Ce3+In any one.
The present invention also provides a kind of preparation methods of the fluorescent powder grain of monodispersed core-shell structural, include the following steps:
S1: preparing monodispersed oxidate microspheres suspension, and the particle size of oxidate microspheres is 5-30um；
S2: using chemical precipitation method in above-mentioned oxidate microspheres surface coating fluorescent powder layer；
S3: the fluorescence that the S2 that repeats the above steps meets the monodispersed core-shell structural of demand until obtaining phosphor powder layer thickness
Powder particles.
Wherein, step S2 includes:
S21: being added yttrium nitrate, aluminum nitrate and cerous nitrate into the oxidate microspheres suspension that step S1 is obtained, and with grass
Acid solution or ammonium bicarbonate soln mixing；
S22: it filtered, be dried to obtain desciccate, then the desciccate is obtained into monodispersed core-shell knot through calcining
The fluorescent powder of the fluorescent powder grain composition of structure.
Preferably, the step S1 further include: surface modifier is added into the oxidate microspheres suspension, obtains table
The modified oxidate microspheres suspension in face.
Preferably, the surface modifier is amino-containing organic compound.
Preferably, the amino-containing organic compound is polyethyleneimine, N, N- diethyl trimethylsilyl amine, 3-
Any one in aminopropyl trimethoxysilane
Preferably, the step S22 further include: washing, the technique of the washing is between the filtering and the drying
Between technique, the technique of the washing is that the filter residue generated using technique of the deionized water to the filtering is washed.
Preferably, the calcination temperature is 800-1400 DEG C.
Preferably, the calcination time is 2-6h.
Preferably, the molar ratio of the yttrium nitrate and the aluminum nitrate is 3:5.
Preferably, the additive amount of the cerous nitrate meets cerium ion in the yttrium nitrate, the aluminum nitrate and the nitric acid
Molar content in material solution composed by cerium is 0.01%~1%.
Compared with the existing technology, beneficial effects of the present invention are as follows:
On the one hand the fluorescent powder of core-shell structure prepared by the present invention utilizes polymolecularity and the uniform oxide of particle diameter distribution
Kernel prepares dispersed preferable, the uniform core-shell structure of particle diameter distribution fluorescent powder grain, on the other hand utilizes low-refraction
Oxide kernel, high refractive index fluorescent powder outer layer make light the two interface occur total reflection make its light extraction efficiency improve.Especially
It directlys adopt commercial oxide microsphere surface coating fluorescent powder, can obtain the splendid spherical fluorescent grain of particle size uniformity.
The present invention, as nuclear structure, compares solid fluorescent powder grain, Neng Gouyou using lower-cost oxidate microspheres
Effect reduces the cost of fluorescent powder grain；Due to the uniform particle sizes of oxide kernel, good dispersion, can prepare dispersibility compared with
The fluorescent powder of good core-shell structure；Since the phosphor powder layer thickness of cladding is controllable, the more uniform core of partial size can be prepared
The fluorescent powder of shell structure；Since the refractive index of nuclear structure is less than the refractive index of the shell structure, the corpuscular emission of phosphor powder layer goes out
Wide-angle luminous energy can be totally reflected in the interface of core-shell structure, and for the fluorescent powder grain of uniform composition, this portion
The light divided is to be absorbed and lose, thus keep the light extraction efficiency of the fluorescent powder with core-shell structure higher.In conclusion the present invention compares
The fluorescent powder of the prior art is at low cost, and good dispersion, particle diameter distribution are uniform, pattern is uniform, light extraction efficiency is high.
Present invention will be further explained below with reference to the attached drawings and examples.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the fluorescent powder with core-shell structure particle of the first embodiment of the invention；
Fig. 2 is the light reflection signal of the fluorescent powder grain of the monodispersed core-shell structural of the first embodiment of the invention
Figure；
Fig. 3 is the structural schematic diagram of the fluorescent powder grain of the monodispersed core-shell structural of second of embodiment of the invention.
Specific embodiment
The present invention provides a kind of fluorescent powder grain and preparation method thereof of monodispersed core-shell structural, to solve existing fluorescence
Powder particles are easy to reunite, and particle diameter distribution is uneven, and surface topography is different, are difficult to prepare uniform particle sizes, good dispersion and pattern
Single big partial size fluorescent powder.
Embodiment one
Shown in referring to Fig.1, the fluorescent powder grain of monodispersed core-shell structural provided by the invention includes centrally located core
Structure 11 and the shell structure 12 for coating the nuclear structure, wherein the oxide that nuclear structure 11 is uniform particle diameter, size is 5-30um
Microballoon, shell structure 12 are the phosphor powder layer with a thickness of 0.05-2um.
Specifically in the present embodiment, oxidate microspheres are Al2O3 (aluminum oxide) microballoon, and phosphor powder layer uses YAG
Y in (yttrium aluminium garnet) fluorescent powder3Al5O12:Ce3+Fluorescent powder.Since Al2O3 microballoon is uniform spherical shape, cladding Al2O3 is micro-
The phosphor powder layer thickness of ball is uniform, i.e. the pattern of the fluorescent powder grain of monodispersed core-shell structural is also uniform spherical shape, so that
The light of the fluorescent powder exciting light own transmission is consistent in all angles；
In addition, the refractive index of Al2O3 is 1.76, Y3Al5O12:Ce3+The refractive index of fluorescent powder is 1.81, so that nuclear structure
The refractive index of Al2O3 is less than shell structure Y3Al5O12:Ce3+Refractive index, can when exciting light and stimulated light both are radiated at interface
It can be totally reflected, keep its light extraction efficiency higher.Referring to shown in Fig. 2, according to angle of total reflection formula(ncFor core
The refractive index of structure, nsFor the refractive index of shell structure) it is found that when exciting light and stimulated light are on nucleocapsid interface in the present embodiment
Incident angle can be totally reflected when being greater than 76.5 °.
The preparation method of the fluorescent powder grain of monodispersed core-shell structural of the present invention includes the following steps:
S1: using particle size to prepare oxidate microspheres suspension for the oxidate microspheres of 5-30um, and the specific steps are will
Monodispersed, morphological rules, particle size is that the Al2O3 microballoon of 5-30um is distributed in deionized water, obtains Al2O3 microballoon
Suspension.
S2: using chemical precipitation method by oxidate microspheres surface coating fluorescent powder layer in suspension, stoichiometrically to
Yttrium nitrate, aluminum nitrate and cerous nitrate are added in above-mentioned oxidate microspheres suspension, ammonium bicarbonate soln is added under agitation,
Filtering, drying, obtain desciccate after reacting sufficiently, and monodispersed core-shell structural can be obtained through calcining in desciccate
The fluorescent powder of fluorescent powder grain composition.
Specifically, being dried in the temperature environment that drying condition is 60 DEG C in the present embodiment.
Specifically, calcination condition is to calcine 2-6h at 800-1400 DEG C in the present embodiment.
S3: the fluorescence that the S2 that repeats the above steps meets the monodispersed core-shell structural of demand until obtaining phosphor powder layer thickness
Powder particles.
It should be noted that, for the quality for improving desciccate, filtered after reacting sufficiently in above-mentioned steps S2, then
Filter residue is washed using deionized water, is then dried, the desciccate of high-quality is obtained.
In above-mentioned steps S2, as long as it is 3:5, cerous nitrate addition that chemical dosage ratio, which meets yttrium nitrate and the molar ratio of aluminum nitrate,
It is 0.01%~1% that amount, which meets molar content of the cerium ion in the material solution composed by yttrium nitrate, aluminum nitrate and cerous nitrate,
, specific mass component determines according to the thickness of required shell structure.
The preparation method of present embodiment, using monodispersed micron order oxidate microspheres as nuclear structure, reaction is lived
Property it is very low, need could chemically react at a higher temperature, and the fluorescent powder of shell structure be aluminium oxide, yttrium oxide and oxidation
Cerium, reactivity is higher, can chemically react between each other at a lower temperature, therefore can prepare core-shell structure
Fluorescent powder, and solid fluorescent powder grain is compared, it can be effectively reduced the cost of fluorescent powder grain；Secondly as can basis
Need to be repeated several times step S2 to obtain the controllable phosphor powder layer of thickness, and then can be big by adjusting the particle of oxidate microspheres
The granular size of small and phosphor powder layer thickness control nucleocapsid fluorescent powder, therefore the more uniform nucleocapsid knot of partial size can be prepared
The fluorescent powder of structure.Further, since the uniform particle sizes of oxide kernel, good dispersion, therefore the monodispersed core-shell knot prepared
The fluorescent powder grain of structure is also spherical and uniform particle sizes, good dispersion.
Embodiment two:
As shown in figure 3, present embodiment and the first embodiment are essentially identical, the fluorescent powder of monodispersed core-shell structural
Particle includes centrally located nuclear structure 21 and the shell structure 22 for coating the nuclear structure, wherein nuclear structure 21 is particle size
For the oxidate microspheres of 5-30um, shell structure 22 is the phosphor powder layer with a thickness of 0.05-2um.
Difference is that in the present embodiment, the oxidate microspheres of nuclear structure 21 use SiO2 (silica) microballoon, glimmering
Light bisque is Y3Al5O12:Ce3+.Wherein, the refractive index of SiO2 is 1.46, Y3Al5O12:Ce3+The refractive index of fluorescent powder is 1.81.
Since the refractive index of SiO2 is less than the refractive index of Al2O3, in the present embodiment, the specific refractivity of nuclear structure and shell structure compared with
Greatly, according to angle of total reflection formula
(nc is the refractive index of nuclear structure, nsFor the refractive index of shell structure) it is found that when exciting light and being excited in the present embodiment
Light can be totally reflected when the incident angle on nucleocapsid interface is greater than 53.77 °.Compare the first embodiment, this implementation
In mode, the angle of total reflection is smaller, and more light shine between nucleocapsid and are totally reflected, and light extraction efficiency is higher., light extraction efficiency is higher.
The preparation method of present embodiment and the first embodiment are essentially identical, and difference is, being in step S1 will be single
Dispersing, morphological rules, particle size is that the SiO2 microballoon of 5~30um is distributed in deionized water, and it is outstanding to obtain SiO2 microballoon
Supernatant liquid.
Embodiment three
Present embodiment is the improvement made on the basis of first two embodiment, and difference is, in present embodiment
Preparation method in, further include surface modifier being added into oxidate microspheres suspension to carry out surface modified in step S1, from
And obtain the modified oxidate microspheres suspension in surface.
The preferably amino-containing organic compound of the surface modifier can be polyethyleneimine, N, N- diethyl front three
At least one of base silane base amine, 3- aminopropyl trimethoxysilane.
In step S2, yttrium nitrate, aluminum nitrate and cerous nitrate are added into oxidate microspheres suspension, under agitation plus
Enter oxalic acid solution, ruthenium ion, aluminium ion, cerium ion is made to invest oxidate microspheres surface, high temperature sintering by acid amide condensation reaction
More fine and close phosphor powder layer shell is obtained afterwards.
It is illustrated for being improved for second of embodiment below:
The SiO2 microballoon that monodispersed, morphological rules, particle size is 5~30um is distributed in deionized water,
Surface modifier polyethyleneimine or N, N- diethyl trimethylsilyl amine or 3- aminopropyl front three are added under conditions of stirring
Oxysilane, then 2~4h of magnetic agitation, obtains the modified SiO2 microsphere suspension liquid in surface.
Yttrium nitrate, aluminum nitrate and cerous nitrate are stoichiometrically added into above-mentioned oxidate microspheres suspension, is stirring
Under the conditions of oxalic acid solution is added, so that ruthenium ion, aluminium ion, cerium ion is invested oxidate microspheres surface by acid amide condensation reaction,
Ammonium hydroxide is added after reacting sufficiently and adjusts pH, is filtered, washed, dries, desciccate is calcined into 2~6h at 800~1400 DEG C,
Obtain the fluorescent powder of the fluorescent powder grain composition of monodispersed core-shell structural.
In the present embodiment, after being modified processing to SiO2 microsphere surface, phosphor powder layer coated Si O2 can be made
It is more easier and fluorescent powder clad is finer and close, structure is more ideal.
Stoichiometric ratio can refer to embodiment one in present embodiment.
In selectable other embodiments, oxidate microspheres can also be magnesia, and phosphor powder layer can also use
Ca3Sc2Si3O12:Ce3+, correspondingly, the raw material of fluorescent powder shell be calcium nitrate, scandium nitrate, ethyl orthosilicate, structure and system
Preparation Method is essentially identical, and belongs to present inventive concept and can be realized the object of the invention, is not limited in above-mentioned several realities
Apply enumerating for mode.
The present invention uses lower-cost micron order oxidate microspheres as inner core, by chemical precipitation method described
Micron order oxidate microspheres surface coating fluorescent powder layer forms shell structure.Solid fluorescent powder grain is compared, can be effectively reduced
The cost of fluorescent powder grain；Due to the uniform particle sizes of oxide kernel, good dispersion, the fluorescent powder point for the core-shell structure prepared
Scattered property is also preferable；And since the phosphor powder layer thickness of cladding is controllable, the fluorescent powder partial size of core-shell structure is also more uniform；
Since the refractive index of nuclear structure is less than the refractive index of the shell structure, the corpuscular emission of phosphor powder layer goes out wide-angle luminous energy in nucleocapsid
The interface of structure can be totally reflected, and for the fluorescent powder grain of uniform composition, the light of this part be absorbed and
Loss, thus keep the light extraction efficiency of the fluorescent powder with core-shell structure higher.In conclusion the fluorescent powder of the present invention compared with the prior art
At low cost, good dispersion, particle diameter distribution are uniform, pattern is uniform, light extraction efficiency is high.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (16)
1. a kind of fluorescent powder grain of monodispersed core-shell structural, which is characterized in that the fluorescent powder grain includes being located at center
Nuclear structure and coat the shell structure of the nuclear structure, the nuclear structure is the oxidate microspheres of uniform particle diameter, the shell structure
For phosphor powder layer, the refractive index of the nuclear structure is less than the refractive index of the shell structure.
2. the fluorescent powder grain of monodispersed core-shell structural according to claim 1, which is characterized in that the oxide is micro-
Ball particle size is 5-30um.
3. the fluorescent powder grain of monodispersed core-shell structural according to claim 1, which is characterized in that the phosphor powder layer
With a thickness of 0.05-2um.
4. the fluorescent powder grain of monodispersed core-shell structural according to claim 3, which is characterized in that the oxide is micro-
Ball is silica, aluminum oxide, any one in magnesia.
5. the fluorescent powder grain of monodispersed core-shell structural according to claim 3, which is characterized in that the phosphor powder layer
Material be garnet structure fluorescent powder.
6. the fluorescent powder grain of monodispersed core-shell structural according to claim 5, which is characterized in that the phosphor powder layer
Material be Y3Al5O12:Ce3+, Ca3Sc2Si3O12:Ce3+In any one.
7. a kind of preparation method of the fluorescent powder grain of monodispersed core-shell structural, which comprises the steps of:
S1: preparing monodispersed oxidate microspheres suspension, and the particle size of oxidate microspheres is 5-30um；
S2: using chemical precipitation method in the oxidate microspheres surface coating fluorescent powder layer；
S3: the S2 that repeats the above steps is until the phosphor powder layer thickness of acquisition meets the fluorescent powder of the monodispersed core-shell structural of demand
Particle.
8. wherein, step S2 includes:
S21: yttrium nitrate, aluminum nitrate and cerous nitrate are added into the oxidate microspheres suspension that step S1 is obtained, and molten with oxalic acid
Liquid or ammonium bicarbonate soln mixing；
S22: it filtered, be dried to obtain desciccate, then the desciccate is calcined to obtain the glimmering of monodispersed core-shell structural
The fluorescent powder of light powder particles composition.
9. the preparation method of the fluorescent powder grain of monodispersed core-shell structural according to claim 7, which is characterized in that institute
State step S1 further include: surface modifier is added into the oxidate microspheres suspension, it is micro- to obtain the modified oxide in surface
Ball suspension.
10. the preparation method of the fluorescent powder grain of monodispersed core-shell structural according to claim 8, which is characterized in that
The surface modifier is amino-containing organic compound.
11. the preparation method of the fluorescent powder grain of monodispersed core-shell structural according to claim 9, which is characterized in that
The amino-containing organic compound is polyethyleneimine, N, N- diethyl trimethylsilyl amine, 3- aminopropyl trimethoxy
Any one in silane.
12. the preparation method of the fluorescent powder grain of monodispersed core-shell structural according to claim 7, which is characterized in that
The step S22 further include: washing, the technique of the washing are described to wash between the filtering and the technique of the drying
The technique washed is that the filter residue generated using technique of the deionized water to the filtering is washed.
13. the preparation method of the fluorescent powder grain of monodispersed core-shell structural according to claim 7, which is characterized in that
The calcination temperature is 800-1400 DEG C.
14. the preparation method of the fluorescent powder grain of monodispersed core-shell structural according to claim 12, which is characterized in that
The calcination time is 2-6h.
15. the preparation method of the fluorescent powder grain of monodispersed core-shell structural according to claim 7, which is characterized in that
The molar ratio of the yttrium nitrate and the aluminum nitrate is 3:5.
16. the preparation method of the fluorescent powder grain of the monodispersed core-shell structural according to claim 7 or 14, feature exist
In the additive amount of the cerous nitrate meets cerium ion original composed by the yttrium nitrate, the aluminum nitrate and the cerous nitrate
Expect that the molar content in solution is 0.01% ~ 1%.
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| CN201710417073.4A CN108997998A (en) | 2017-06-06 | 2017-06-06 | Fluorescent powder grain of monodispersed core-shell structural and preparation method thereof |
| PCT/CN2017/114710 WO2018223632A1 (en) | 2017-06-06 | 2017-12-06 | Fluorescent powder particle with monodispersed core-shell structure, and manufacturing method therefor |
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| CN107805056A (en) * | 2016-09-09 | 2018-03-16 | 深圳市光峰光电技术有限公司 | The preparation method and ceramic composite of ceramic composite, light supply apparatus |
| CN113025305A (en) * | 2019-12-09 | 2021-06-25 | 上海航空电器有限公司 | High-refractive-index edge-covered wide-spectrum emission composite phosphor and preparation method thereof |
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| KR101579457B1 (en) * | 2014-12-22 | 2015-12-22 | 코닝정밀소재 주식회사 | Method of fabricating light extraction substrate, light extraction substrate for oled and oled including the same |
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| CN102191033A (en) * | 2010-03-11 | 2011-09-21 | 海洋王照明科技股份有限公司 | Fluorescent material with core-shell structure and preparation method thereof |
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| CN107805056A (en) * | 2016-09-09 | 2018-03-16 | 深圳市光峰光电技术有限公司 | The preparation method and ceramic composite of ceramic composite, light supply apparatus |
| CN113025305A (en) * | 2019-12-09 | 2021-06-25 | 上海航空电器有限公司 | High-refractive-index edge-covered wide-spectrum emission composite phosphor and preparation method thereof |
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| WO2018223632A1 (en) | 2018-12-13 |
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