CN110498878A - A kind of preparation method of fluorescent microsphere - Google Patents
A kind of preparation method of fluorescent microsphere Download PDFInfo
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- CN110498878A CN110498878A CN201910843153.5A CN201910843153A CN110498878A CN 110498878 A CN110498878 A CN 110498878A CN 201910843153 A CN201910843153 A CN 201910843153A CN 110498878 A CN110498878 A CN 110498878A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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Abstract
The invention discloses a kind of preparation methods of fluorescent microsphere, the preparation method of the fluorescent microsphere is the following steps are included: being added polymer seeds and initiator in the aqueous solution containing dispersing agent, it stirs evenly, form seed suspension liquid, wherein, by weight percentage, the polymer seeds account for 50% or less institute's seed suspension liquid weight；Fluorescent monomer and polymerized monomer are mixed, stirring forms uniform monomer suspension；Under 70-80 DEG C of constant temperature, the monomer suspension is dispersed into the seed suspension liquid by nozzle with drop form, after the completion of the monomer suspension addition, the reaction was continued obtains fluorescent microsphere.The size tunable of fluorescent microsphere prepared by the present invention is higher, and fluorescence intensity is high, has in field of biological detection and is widely applied.
Description
Technical field
The present invention relates to polymer material field, in particular to a kind of preparation method of fluorescent microsphere.
Background technique
Fluorescent microsphere is a kind of functional microsphere for being loaded with fluorescent molecule, in immune detection, the fields such as isolates and purifies and has
It is widely applied.About fluorescent microsphere preparation method there are many, be generally divided into physisorphtion, self-assembly method, embedding hair, chemistry
Bonding method, copolymerization method etc., current preparation method at least have the following deficiencies: that uncontrollable factor is more in production process, Yi Sheng
At little particle impurity, cause fluorescent microsphere particle size distribution range wide, low yield, poor controllability.Moreover, reaction time is long, it is unfavorable
In large-scale production.
Summary of the invention
In order to solve the above technical problems, the embodiment of the invention provides a kind of preparation methods of fluorescent microsphere.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
The embodiment of the invention provides a kind of preparation method of fluorescent microsphere, the preparation method of the fluorescent microsphere include with
Lower step:
S10, polymer seeds and initiator are added in the aqueous solution containing dispersing agent, are stirred evenly, form seed
Suspension, wherein by weight percentage, the polymer seeds account for 50% or less institute's seed suspension liquid weight；
S20, fluorescent monomer and polymerized monomer are mixed, stirring forms monomer suspension, wherein by weight percentage,
The fluorescent monomer accounts for 50% or more of the monomer suspension；
S30, under 70-80 DEG C of constant temperature, the monomer suspension is dispersed by nozzle with drop form
In the seed suspension liquid, after the completion of monomer suspension addition, the reaction was continued 60min obtains fluorescent microsphere suspension, washes
Fluorescent microsphere is obtained after washing, drying.
Further, step S30 is further comprising the steps of:
S31, the seed suspension liquid is put into the first container, the monomer suspension is put into second container, institute
Nozzle is stated to be mounted on the second container；
S32, preset pressure is applied to the second container, under the preset pressure, described in the monomer suspension warp
Nozzle is dispersed into the seed suspension liquid with drop form.
Further, the preset pressure is 0.1~10Mpa.
Further, the dispersing agent is hydroxymethyl cellulose, oleic acid, oleyl alcohol, polyethylene glycol, at least one in dextrin
Kind.
Further, the fluorescent monomer is dansyl chloride allylamine fluorescent monomer, N acrylamide ethyl -2- (1-
Pyrenyl amide-based small) hydrocinnamamide fluorescent monomer, N- allyl anthranilamide fluorescent monomer or 2- allyloxy naphthalene-
6,8- disulfonic acid potassium fluorescent monomers.
Further, the polymer seeds are as follows: by the poly- of emulsion polymerization, dispersion copolymerization method or suspension polymerization preparation
Styrene seed or styrene-divinylbenzene seed.
Further, the average grain diameter of the fluorescent microsphere is 100nm~1000 μm.
Further, the initiator is azo water soluble starter.
Further, the initiator is two isobutyl imidazoline hydrochloride of azo or azo diisobutyl amidine hydrochloride.
Further, the polymerized monomer is styrene, divinylbenzene, 2,4- dichlorostyrene, acrylic acid, metering system
At least one of amino acid methyl esters, ethyl acrylate, vinylacetate, glycidyl methacrylate.
The embodiment of the invention provides a kind of preparation method of fluorescent microsphere, using eruption mode by monomer suspension jet flow
Uniform drop is formed, and is dispersed in seed suspension liquid, polymer seeds rapidly absorb drop and grow, and obtain after reaction
Fluorescent microsphere.Because monomer suspension size droplet diameter of the invention is uniform, it is easier to be fully absorbed, reduce by polymer seeds
The time required to whole preparation process, production efficiency is improved.In addition, uniform monomer suspension drop is more easily complete by seed
It absorbs, reduces the little particle impurity content in the fluorescent microsphere of generation, improve the yield of fluorescent microsphere, be suitable for extensive raw
It produces.
Detailed description of the invention
Fig. 1 is blue-fluorescence microballoon photo in the embodiment of the present invention one.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright a part of the embodiment, rather than whole embodiments.Based on described the embodiment of the present invention, those skilled in the art institute
The every other embodiment obtained, belongs to the scope of the present invention.
The embodiment of the invention provides a kind of preparation method of fluorescent microsphere, the preparation method of fluorescent microsphere includes following step
It is rapid:
S10, polymer seeds and initiator are added in the aqueous solution containing dispersing agent, are stirred evenly, form seed
Suspension, wherein by weight percentage, polymer seeds account for 50% or less institute's seed suspension liquid weight；
S20, fluorescent monomer and polymerized monomer are mixed, stirring forms monomer suspension, wherein by weight percentage,
Hexamethylene accounts for the 3~10% of monomer suspension, and fluorescent monomer accounts for 50% of monomer suspension or more；
S30, under 70-80 DEG C of constant temperature, monomer suspension is dispersed into seed by nozzle with drop form
In suspension, after the completion of monomer suspension addition, the reaction was continued 60min obtains fluorescent microsphere suspension, washing, it is dry after it is glimmering
Light microballoon.
In the embodiment of the present invention, fluorescent monomer grows polymer seeds, and after reaching preset microspherulite diameter, washing is dry
It is dry, fluorescent microsphere is obtained, therefore, the preparation method of the embodiment of the present invention is constantly grown using seed, real by adjusting reaction condition
The purpose of size tunable is showed.
Specifically, monomer suspension jet flow is formed using eruption mode by uniform drop, and is dispersed in seed suspension liquid
In, one-step polymerization makes polymer seeds fast-growth, obtains fluorescent microsphere after reaction.Because of monomer suspension drop of the invention
Uniform particle diameter, it is easier to be fully absorbed by polymer seeds, the time required to reducing whole preparation process, improve production effect
Rate.In addition, uniform monomer suspension drop is easier to be fully absorbed by seed, small in the fluorescent microsphere of generation is reduced
Grain impurity content, improves the yield of fluorescent microsphere, is suitable for large-scale production.
Further, polymerized monomer is styrene, divinylbenzene, 2,4- dichlorostyrene, acrylic acid, metering system amino acid
At least one of methyl esters, ethyl acrylate, vinylacetate, glycidyl methacrylate.
In some embodiments of the invention, step S30 is further comprising the steps of:
S31, seed suspension liquid is put into the first container, monomer suspension is put into second container, nozzle is mounted on
On second container；
S32, preset pressure is applied to second container, under preset pressure, monomer suspension is through nozzle with drop form point
It dissipates and enters in seed suspension liquid.
Preferably, the aperture of nozzle can be 50nm~5000 μm, it is further preferred that the aperture of nozzle be 10 μm~
200μm。
Further, preset pressure is 0.1~10Mpa.
Further, dispersing agent is at least one of hydroxymethyl cellulose, oleic acid, oleyl alcohol, polyethylene glycol, dextrin.
In other embodiments of the invention, fluorescent monomer is dansyl chloride allylamine fluorescent monomer, N- acryloyl
Amine ethyl -2- (1- pyrenyl amide-based small) hydrocinnamamide fluorescent monomer, N- allyl anthranilamide fluorescent monomer or 2-
Allyloxy naphthalene -6,8- disulfonic acid potassium fluorescent monomer.
Further, polymer seeds are as follows: the polyphenyl second prepared by emulsion polymerization, dispersion copolymerization method or suspension polymerization
Alkene seed or styrene-divinylbenzene seed.
Further, initiator is azo water soluble starter.
Further, initiator is two isobutyl imidazoline hydrochloride of azo or azo diisobutyl amidine hydrochloride.
In some other embodiment of the invention, the average grain diameter of fluorescent microsphere is 100nm~1000 μm.Of the invention
The preparation method further expansion particle size range of fluorescent microsphere.
Preparation method of the invention is described further combined with specific embodiments below, it is to be understood that the present invention
It is not limited to following embodiment:
Embodiment one
In ice-water bath, using the acetone of 1:1 volume ratio/methylene chloride mixed solution as solvent, with dansyl Cl and allyl
Base amine synthesizes dansyl chloride allylamine fluorescent monomer, spare.
Polymer seeds suspension is prepared in the first container: by 82g polystyrene seed, (its granularity is 4.6 microns, CV
=3%) it is added in the aqueous solution containing 3g dextrin, stirs evenly with two isobutyl imidazoline hydrochloride of 1.5g azo, form kind
Sub- suspension, wherein by weight percentage, polystyrene seed accounts for the 48% of institute's seed suspension liquid weight；
Monomer suspension is prepared in second container, wherein nozzle is installed, the aperture of nozzle is 10 μ on second container
m.110g dansyl chloride allylamine fluorescent monomer and 50g styrene are mixed, stirring forms monomer suspension.Then, to
Two containers apply the pressure of 0.5Mpa, keep the pressure, monomer suspension is dispersed into seed suspension through nozzle with drop form
In liquid.Finally, under 70 DEG C of constant temperature, the reaction was continued 60min obtains fluorescent microsphere suspension, washing, it is dry after fluorescence
Microballoon.
Use that Beckman Counter measures its partial size and particle diameter distribution obtains: partial size is 10 μm, CV (coefficient
Of variation) it is 2.9%, the fluorescent emission peak position of microballoon is in 510nm, after fluorescent microsphere is placed 6 months, 13 months,
It was found that microballoon dispersibility and fluorescence property are showed no significant change.The yield of fluorescent microsphere is 99.6%.As shown in Figure 1, this reality
It applies example and obtains the fluorescent microsphere of blue.
Illustrate: above-mentioned material amounts being expanded into 2 times, 10 times, 50 times, 100 times, 500 times of productions respectively in proportion, per secondary
Cheng Jun is repeated 3 times, and having obtained partial size is 10 microns, and CV's (Coefficient of Variation)=2.9~3.0% is glimmering
Light microballoon.And generated without little particle, particle size is uniform.The yield of fluorescent microsphere is 99.3~99.7%.
Embodiment two
In ice-water bath, using the acetone of 1:1 volume ratio/methylene chloride mixed solution as solvent, with dansyl Cl and allyl
Base amine synthesizes dansyl chloride allylamine fluorescent monomer, spare.
Polymer seeds suspension is prepared in the first container: by 82g polystyrene seed, (its granularity is 1.5 microns, CV
=3%) it is added in the aqueous solution containing 3g dextrin, stirs evenly with two isobutyl imidazoline hydrochloride of 1.5g azo, form kind
Sub- suspension, wherein by weight percentage, polystyrene seed accounts for the 48% of institute's seed suspension liquid weight；
Monomer suspension is prepared in second container, wherein nozzle is installed, the aperture of nozzle is 10 μ on second container
m.110g dansyl chloride allylamine fluorescent monomer and 60g acrylic acid are mixed, stirring forms monomer suspension.Then, to
Two containers apply the pressure of 0.5Mpa, keep the pressure, monomer suspension is dispersed into seed suspension through nozzle with drop form
In liquid.Finally, reaction 60min obtains fluorescent microsphere suspension under 70 DEG C of constant temperature, fluorescent microsphere is obtained after washing, drying.
Use that Beckman Counter measures its partial size and particle diameter distribution obtains: partial size is 5 micron, CV (coefficient
Of variation) it is 2.5%, the fluorescent emission peak position of microballoon is in 510nm, after fluorescent microsphere is placed 6 months, 13 months,
It was found that microballoon dispersibility and fluorescence property are showed no significant change.
Illustrate: above-mentioned material amounts being expanded into 2 times, 10 times, 50 times, 100 times, 500 times of productions respectively in proportion, per secondary
Cheng Jun is repeated 3 times, and having obtained partial size is 10 microns, and CV's (Coefficient of Variation)=2.5~2.6% is glimmering
Light microballoon.The yield of fluorescent microsphere is 99.5~99.7%.And generated without little particle, particle size is uniform, and the quality of production is stablized.
Embodiment three
Polymer seeds suspension is prepared in the first container: by 153g polystyrene seed, (its granularity is 100nm, CV
=2.8%) it is added in the aqueous solution containing 5g polyethylene glycol, stirs evenly with two isobutyl imidazoline hydrochloride of 1.8g azo,
Form seed suspension liquid, wherein by weight percentage, polystyrene seed accounts for the 50% of institute's seed suspension liquid weight；
Monomer suspension is prepared in second container, wherein nozzle is installed, the aperture of nozzle is 50 μ on second container
m.By 230gN- acrylamide ethyl -2- (1- pyrenyl amide-based small) hydrocinnamamide fluorescent monomer and 160g metering system acid-mixed
It closes, stirring forms monomer suspension.Then, the pressure for applying 0.5Mpa to second container, keeps the pressure, monomer suspension
It is dispersed into seed suspension liquid through nozzle with drop form.Finally, under 70 DEG C of constant temperature, the reaction was continued 60min is obtained
Fluorescent microsphere suspension obtains fluorescent microsphere after washing, drying.
Use that Beckman Counter measures its partial size and particle diameter distribution obtains: partial size 500nm, CV (coefficient
Of variation) it is 2.8%, the fluorescent emission peak position of microballoon is in 510nm, after fluorescent microsphere is placed 6 months, 13 months,
It was found that microballoon dispersibility and fluorescence property are showed no significant change.The yield of fluorescent microsphere is 99.5%.
Example IV
In ice-water bath, using the acetone of 1:1 volume ratio/methylene chloride mixed solution as solvent, with dansyl Cl and allyl
Base amine synthesizes dansyl chloride allylamine fluorescent monomer, spare.
In the first container prepare polymer seeds suspension: by 82g polystyrene seed (its granularity be 0.55 micron,
CV=3% it) is added in the aqueous solution containing 3g dextrin, stirs evenly with two isobutyl imidazoline hydrochloride of 1.5g azo, formed
Seed suspension liquid, wherein by weight percentage, polystyrene seed accounts for the 48% of institute's seed suspension liquid weight；
Monomer suspension is prepared in second container, wherein nozzle is installed, the aperture of nozzle is 10 μ on second container
m.By 110g dansyl chloride allylamine fluorescent monomer and 90g glycidyl methacrylate, stirring forms monomer and suspends
Liquid.Then, the pressure for applying 0.5Mpa to second container, keeps the pressure, monomer suspension is dispersed through nozzle with drop form
Into in seed suspension liquid.Finally, under 70 DEG C of constant temperature, the reaction was continued 60min obtains fluorescent microsphere suspension, washing,
Fluorescent microsphere is obtained after drying.
Use that Beckman Counter measures its partial size and particle diameter distribution obtains: partial size is 1.3 μm, CV (coefficient
Of variation) it is 2.9%, the fluorescent emission peak position of microballoon is in 510nm, after fluorescent microsphere is placed 6 months, 13 months,
It was found that microballoon dispersibility and fluorescence property are showed no significant change.The yield of fluorescent microsphere is 99.5%.
Embodiment five
In ice-water bath, using the acetone of 1:1 volume ratio/methylene chloride mixed solution as solvent, with dansyl Cl and allyl
Base amine synthesizes dansyl chloride allylamine fluorescent monomer, spare.
In the first container prepare polymer seeds suspension: by 82g polystyrene seed (its granularity be 0.55 micron,
CV=3% it) is added in the aqueous solution containing 3g dextrin, stirs evenly with two isobutyl imidazoline hydrochloride of 1.5g azo, formed
Seed suspension liquid, wherein by weight percentage, polystyrene seed accounts for the 48% of institute's seed suspension liquid weight；
Monomer suspension is prepared in second container, wherein nozzle is installed, the aperture of nozzle is 10 μ on second container
m.By 210g dansyl chloride allylamine fluorescent monomer and 90g hydroxyethyl methacrylate, stirring forms monomer suspension.So
Afterwards, the pressure for applying 0.5Mpa to second container, keeps the pressure, monomer suspension is dispersed into kind through nozzle with drop form
In sub- suspension.Finally, under 70 DEG C of constant temperature, the reaction was continued 60min obtains fluorescent microsphere suspension, washing, it is dry after
Obtain fluorescent microsphere.
Use that Beckman Counter measures its partial size and particle diameter distribution obtains: partial size is 3.2 μm, CV (coefficient
Of variation) it is 2.8%, the fluorescent emission peak position of microballoon is in 510nm, after fluorescent microsphere is placed 6 months, 13 months,
It was found that microballoon dispersibility and fluorescence property are showed no significant change.The yield of fluorescent microsphere is 99.6%.
Embodiment six
Polymer seeds suspension is prepared in the first container: by 82g polystyrene seed, (its granularity is 10 microns, CV
=3%) it is added in the aqueous solution containing 3g dextrin, stirs evenly with two isobutyl imidazoline hydrochloride of 1.5g azo, form kind
Sub- suspension, wherein by weight percentage, polystyrene seed accounts for the 48% of institute's seed suspension liquid weight；
Monomer suspension is prepared in second container, wherein nozzle is installed, the aperture of nozzle is 10 μ on second container
m.110g dansyl chloride allylamine fluorescent monomer and 90g acrylic acid are mixed, stirring forms monomer suspension.Then, to
Two containers apply the pressure of 0.5Mpa, keep the pressure, monomer suspension is dispersed into seed suspension through nozzle with drop form
In liquid.Finally, under 70 DEG C of constant temperature, the reaction was continued 60min obtains fluorescent microsphere suspension, washing, it is dry after fluorescence
Microballoon.
Use that Beckman Counter measures its partial size and particle diameter distribution obtains: partial size is 30 micron, CV (coefficient
Of variation) it is 3.0%, the fluorescent emission peak position of microballoon is in 510nm, after fluorescent microsphere is placed 6 months, 13 months,
It was found that microballoon dispersibility and fluorescence property are showed no significant change.The yield of fluorescent microsphere is 99.6%.
Other operations of fluorescent microsphere preparation method according to an embodiment of the present invention are to those skilled in the art all
It is to be understood that and easy to accomplish, therefore is not described in detail.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (10)
1. a kind of preparation method of fluorescent microsphere, which is characterized in that the preparation method of the fluorescent microsphere the following steps are included:
S10, polymer seeds and initiator are added in the aqueous solution containing dispersing agent, are stirred evenly, form seed suspension
Liquid, wherein by weight percentage, the polymer seeds account for 50% or less institute's seed suspension liquid weight；
S20, fluorescent monomer and polymerized monomer are mixed, stirring forms uniform monomer suspension, wherein by weight percentage
Meter, the fluorescent monomer account for 50% or more of the monomer suspension；
S30, under 70-80 DEG C of constant temperature, the monomer suspension is dispersed into drop form by nozzle described
In seed suspension liquid, after the completion of monomer suspension addition, the reaction was continued 60min obtains fluorescent microsphere suspension, washs glimmering
Light microballoon.
2. preparation method according to claim 1, which is characterized in that step S30 is further comprising the steps of:
S31, the seed suspension liquid is put into the first container, the monomer suspension is put into second container, the spray
Mouth is mounted on the second container；
S32, preset pressure is applied to the second container, under the preset pressure, the monomer suspension is through the nozzle
It is dispersed into the seed suspension liquid with drop form.
3. preparation method according to claim 2, which is characterized in that the preset pressure is 0.1~10Mpa.
4. preparation method according to claim 1, which is characterized in that the dispersing agent is hydroxymethyl cellulose, oleic acid, oil
At least one of alcohol, polyethylene glycol, dextrin.
5. preparation method according to claim 1, which is characterized in that the fluorescent monomer is that dansyl chloride allylamine is glimmering
Light monomer, N acrylamide ethyl -2- (1- pyrenyl amide-based small) hydrocinnamamide fluorescent monomer, N- allyl anthraniloyl
Amine fluorescent monomer or 2- allyloxy naphthalene -6,8- disulfonic acid potassium fluorescent monomer.
6. preparation method according to claim 1, which is characterized in that the polymer seeds are as follows: by emulsion polymerization, divide
Dissipate the polystyrene seed or styrene-divinylbenzene seed of polymerization or suspension polymerization preparation.
7. preparation method according to claim 1, which is characterized in that the average grain diameter of the fluorescent microsphere be 100nm~
1000μm。
8. preparation method according to claim 1, which is characterized in that the initiator is azo water soluble starter.
9. preparation method according to claim 8, which is characterized in that the initiator is two isobutyl imidazoline hydrochloric acid of azo
Salt or azo diisobutyl amidine hydrochloride.
10. preparation method according to claim 1, which is characterized in that the polymerized monomer be styrene, divinylbenzene,
2,4- dichlorostyrenes, acrylic acid, metering system amino acid methyl esters, ethyl acrylate, vinylacetate, Glycidyl methacrylate are sweet
At least one of grease.
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| CN111498900A (en) * | 2020-04-28 | 2020-08-07 | 无锡迈科为生物科技有限公司 | Preparation method of zirconium dioxide microspheres |
| CN113861324A (en) * | 2021-10-08 | 2021-12-31 | 无锡瑞格生物科技有限责任公司 | Monodisperse fluorescent microsphere particles and preparation method thereof |
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