CN108277005A - A kind of multiduty fluorescent crystal material and preparation method thereof - Google Patents

A kind of multiduty fluorescent crystal material and preparation method thereof Download PDF

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Publication number
CN108277005A
CN108277005A CN201810079074.7A CN201810079074A CN108277005A CN 108277005 A CN108277005 A CN 108277005A CN 201810079074 A CN201810079074 A CN 201810079074A CN 108277005 A CN108277005 A CN 108277005A
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multiduty
fluorescent crystal
fluorescent
crystal material
morin
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向卫东
梁晓娟
邹军
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Wenzhou University
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Wenzhou University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/88Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
    • C09K11/881Chalcogenides
    • C09K11/883Chalcogenides with zinc or cadmium
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02BCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a kind of multiduty fluorescent crystal materials, including following quality proportioning:O-phenylenediamine 4 8%, m-phenylene diamine (MPD) 3 6%, zinc-cadmium sulfide 6 12%, morin 8 16%, zirconium oxide 5 10%, strontium carbonate 7 14%, silicon nitride 10 20%, solvent 7 14%.The invention also discloses a kind of preparation methods of multiduty fluorescent crystal material, include the following steps:S1:Raw material preparation;S2:Milled processed;S3:Heat treatment;S4:Final molding.Peculiar preparation method through the invention again, the fluorescent crystal material fluorescent material prepared can emit three kinds of colors of red, green, blue, three kinds of colors are three kinds of basic primary colors, primary colors is mixed in varing proportions, other new colors can be produced, a variety of demands can be met, other fluorescent material collocation can be used as white light emitting device, it also can be separately as the fluorescent paint of security pattern, easy to operate, preparation process is simple, and yield is high, the equipment for not needing complex and expensive, it is easy to accomplish industrialized production.

Description

A kind of multiduty fluorescent crystal material and preparation method thereof
Technical field
Invention is related to fluorescent crystal technical field, specially a kind of multiduty fluorescent crystal material and preparation method thereof.
Background technology
Fluorescent material has a wide range of applications in daily life, industrial production and scientific research, as people are to glimmering The research of light is more and more, and application range is also more and more extensive.Fluorescent material serves not only as fluorescent pigment, for advertisement, packet Dress making, dangerous warning and traffic signals etc. are also widely used for fluorescence analysis, show that illuminating device, solar energy, medicine are examined The multiple fields such as disconnected, anti-fake mark.But existing fluorescent material shine above for, existing fluorescent powder absorbs part Yellow light can be sent out after the blue light that LED is sent out, unabsorbed blue light then mixes with this yellow light and sends out white light, existing yttrium aluminium Garnet fluorescent powder causes blue light caused by LED that can not be used effectively since its quantum efficiency is still relatively low, therefore derivative The problem of going out luminance shortage, and usage is extremely dull.
Invention content
Invention is designed to provide a kind of multiduty fluorescent crystal material and preparation method thereof, to solve above-mentioned background The problem of being proposed in technology.
To achieve the above object, invention provides the following technical solutions:A kind of multiduty fluorescent crystal material, including it is following Quality proportioning:O-phenylenediamine 4-8%, m-phenylene diamine (MPD) 3-6%, zinc-cadmium sulfide 6-12%, morin 8-16%, zirconium oxide 5-10%, carbonic acid Strontium 7-14%, silicon nitride 10-20%, solvent 7-14%.
Preferably, including following quality proportioning, o-phenylenediamine 4%, m-phenylene diamine (MPD) 3%, zinc-cadmium sulfide 6%, morin 8%, oxygen Change zirconium 5%, strontium carbonate 7%, silicon nitride 10%, solvent 7%.
Preferably, including following quality proportioning, o-phenylenediamine 5.5%, m-phenylene diamine (MPD) 4%, zinc-cadmium sulfide 8%, morin 11%, Zirconium oxide 7%, strontium carbonate 9%, silicon nitride 13%, solvent 9%.
Preferably, including following quality proportioning, o-phenylenediamine 7%, m-phenylene diamine (MPD) 5%, zinc-cadmium sulfide 10%, morin 14%, Zirconium oxide 8.7%, strontium carbonate 11%, silicon nitride 17%, solvent 11%.
Preferably, including following quality proportioning, o-phenylenediamine 8%, m-phenylene diamine (MPD) 6%, zinc-cadmium sulfide 12%, morin 16%, Zirconium oxide 10%, strontium carbonate 14%, silicon nitride 20%, solvent 14%.
Preferably, the solvent includes following quality proportioning, formamide 13-26%, ethylene glycol 10-20%, light stabilizer 7- 14%, distilled water 20-40%.
A kind of preparation method of multiduty fluorescent crystal material, includes the following steps:
S1:Raw material preparation, by o-phenylenediamine, m-phenylene diamine (MPD), zinc-cadmium sulfide, morin, zirconium oxide, strontium carbonate and silicon nitride according to Set ratio, weighing are taken, and are placed in same container, are sufficiently stirred;
S2:Milled processed, will carry out more the raw mixture that is sufficiently stirred be ground by planetary ball mill, milling time It it is 20-60 minutes, final grinding finally obtains raw material hybrid particles at the particle of 100-400 mesh;
S3:Raw material hybrid particles are put into heating container, and are added load weighted molten according to both certainty ratios by heat treatment Then agent is sealed processing, puts into muffle furnace later, temperature, and the control in 4-7 hours are controlled with temperature controller Temperature rise is to 340 degree, quiet to put 4-7 days and in 340 degree, is then taking out, quiet to let cool but, obtains the thick embryo of fluorescent crystal;
S4:The thick embryo of fluorescent crystal is cut into the fluorescent crystal of the sizes such as uniform by final molding by cutter device.
Compared with prior art, advantageous effect of the invention is:The preparation method of the multiduty fluorescent crystal material, passes through Cooperation effect of o-phenylenediamine, m-phenylene diamine (MPD), zinc-cadmium sulfide, morin, zirconium oxide, strontium carbonate and silicon nitride adds formyl The auxiliary booster action of amine, ethylene glycol and light stabilizer, then peculiar preparation method through the invention, the fluorescence prepared are brilliant Body material fluorescent material can emit three kinds of colors of red, green, blue, which is three kinds of basic primary colors, in varing proportions will Primary colors mixes, and can produce other new colors, can meet a variety of demands, and other fluorescent material collocation can be used as white light hair Electro-optical device, also can be separately as the fluorescent paint of security pattern, and easy to operate, preparation process is simple, and yield is high, does not need complexity Expensive equipment, it is easy to accomplish industrialized production.
Specific implementation mode
Below in conjunction with inventive embodiments, the technical solution in inventive embodiments is clearly and completely described, is shown So, described embodiment is only invention a part of the embodiment, instead of all the embodiments.Based on the implementation in invention Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to Invent the range of protection.
Embodiment one
Invention provides a kind of technical solution:A kind of multiduty fluorescent crystal material, including following quality proportioning:O-phenylenediamine 4%, m-phenylene diamine (MPD) 3%, zinc-cadmium sulfide 6%, morin 8%, zirconium oxide 5%, strontium carbonate 7%, silicon nitride 10%, solvent 7%.
The solvent includes following quality proportioning, formamide 13%, ethylene glycol 10%, light stabilizer 7%, distilled water 20%.
A kind of preparation method of multiduty fluorescent crystal material, includes the following steps:
S1:Raw material preparation, by o-phenylenediamine, m-phenylene diamine (MPD), zinc-cadmium sulfide, morin, zirconium oxide, strontium carbonate and silicon nitride according to Set ratio, weighing are taken, and are placed in same container, are sufficiently stirred;
S2:Milled processed, will carry out more the raw mixture that is sufficiently stirred be ground by planetary ball mill, milling time It it is 20 minutes, final grinding finally obtains raw material hybrid particles at the particle of 100 mesh;
S3:Raw material hybrid particles are put into heating container, and are added load weighted molten according to both certainty ratios by heat treatment Then agent is sealed processing, puts into muffle furnace later, control temperature with temperature controller, and temperature is controlled in 4 hours Degree rises to 340 degree, and in 340 degree, quiet to put 4 days, is then taking out, quiet to let cool but, obtains the thick embryo of fluorescent crystal;
S4:The thick embryo of fluorescent crystal is cut into the fluorescent crystal of the sizes such as uniform by final molding by cutter device.
Embodiment two
Invention provides a kind of technical solution:A kind of multiduty fluorescent crystal material, including following quality proportioning:O-phenylenediamine 5.5%, m-phenylene diamine (MPD) 4%, zinc-cadmium sulfide 8%, morin 11%, zirconium oxide 7%, strontium carbonate 9%, silicon nitride 13%, solvent 9%.
The solvent includes following quality proportioning, formamide 17%, ethylene glycol 13%, light stabilizer 9%, distilled water 27%.
A kind of preparation method of multiduty fluorescent crystal material, includes the following steps:
S1:Raw material preparation, by o-phenylenediamine, m-phenylene diamine (MPD), zinc-cadmium sulfide, morin, zirconium oxide, strontium carbonate and silicon nitride according to Set ratio, weighing are taken, and are placed in same container, are sufficiently stirred;
S2:Milled processed, will carry out more the raw mixture that is sufficiently stirred be ground by planetary ball mill, milling time It it is 35 minutes, final grinding finally obtains raw material hybrid particles at the particle of 200 mesh;
S3:Raw material hybrid particles are put into heating container, and are added load weighted molten according to both certainty ratios by heat treatment Then agent is sealed processing, puts into muffle furnace later, control temperature with temperature controller, and temperature is controlled in 5 hours Degree rises to 340 degree, and in 340 degree, quiet to put 5 days, is then taking out, quiet to let cool but, obtains the thick embryo of fluorescent crystal;
S4:The thick embryo of fluorescent crystal is cut into the fluorescent crystal of the sizes such as uniform by final molding by cutter device.
Embodiment three
Invention provides a kind of technical solution:A kind of multiduty fluorescent crystal material, including following quality proportioning:O-phenylenediamine 7%, m-phenylene diamine (MPD) 5%, zinc-cadmium sulfide 10%, morin 14%, zirconium oxide 8.7%, strontium carbonate 11%, silicon nitride 17%, solvent 11%.
The solvent includes following quality proportioning, formamide 22%, ethylene glycol 17%, light stabilizer 11%, distilled water 33%.
A kind of preparation method of multiduty fluorescent crystal material, includes the following steps:
S1:Raw material preparation, by o-phenylenediamine, m-phenylene diamine (MPD), zinc-cadmium sulfide, morin, zirconium oxide, strontium carbonate and silicon nitride according to Set ratio, weighing are taken, and are placed in same container, are sufficiently stirred;
S2:Milled processed, will carry out more the raw mixture that is sufficiently stirred be ground by planetary ball mill, milling time It it is 45 minutes, final grinding finally obtains raw material hybrid particles at the particle of 300 mesh;
S3:Raw material hybrid particles are put into heating container, and are added load weighted molten according to both certainty ratios by heat treatment Then agent is sealed processing, puts into muffle furnace later, control temperature with temperature controller, and temperature is controlled in 6 hours Degree rises to 340 degree, and in 340 degree, quiet to put 6 days, is then taking out, quiet to let cool but, obtains the thick embryo of fluorescent crystal;
S4:The thick embryo of fluorescent crystal is cut into the fluorescent crystal of the sizes such as uniform by final molding by cutter device.
Example IV
Invention provides a kind of technical solution:A kind of multiduty fluorescent crystal material, including following quality proportioning:O-phenylenediamine 8%, m-phenylene diamine (MPD) 6%, zinc-cadmium sulfide 12%, morin 16%, zirconium oxide 10%, strontium carbonate 14%, silicon nitride 20%, solvent 14%.
The solvent includes following quality proportioning, formamide 26%, ethylene glycol 20%, light stabilizer 14%, distilled water 40%.
A kind of preparation method of multiduty fluorescent crystal material, includes the following steps:
S1:Raw material preparation, by o-phenylenediamine, m-phenylene diamine (MPD), zinc-cadmium sulfide, morin, zirconium oxide, strontium carbonate and silicon nitride according to Set ratio, weighing are taken, and are placed in same container, are sufficiently stirred;
S2:Milled processed, will carry out more the raw mixture that is sufficiently stirred be ground by planetary ball mill, milling time It it is 60 minutes, final grinding finally obtains raw material hybrid particles at the particle of 400 mesh;
S3:Raw material hybrid particles are put into heating container, and are added load weighted molten according to both certainty ratios by heat treatment Then agent is sealed processing, puts into muffle furnace later, control temperature with temperature controller, and temperature is controlled in 7 hours Degree rises to 340 degree, and in 340 degree, quiet to put 7 days, is then taking out, quiet to let cool but, obtains the thick embryo of fluorescent crystal;
S4:The thick embryo of fluorescent crystal is cut into the fluorescent crystal of the sizes such as uniform by final molding by cutter device.
By comparing above four groups of embodiments, we are it can be found that pass through above four groups different proportioning embodiments To obtain our required multiduty fluorescent crystal materials, and the fluorescent crystal material prepared by o-phenylenediamine, Cooperation effect of m-phenylene diamine (MPD), zinc-cadmium sulfide, morin, zirconium oxide, strontium carbonate and silicon nitride, along with formamide, ethylene glycol With the auxiliary booster action of light stabilizer, then peculiar preparation method through the invention, the fluorescent crystal material prepared is glimmering Luminescent material can emit three kinds of colors of red, green, blue, which is three kinds of basic primary colors, in varing proportions mixes primary colors It closes, other new colors can be produced, a variety of demands can be met, other fluorescent material collocation can be used as white-light emitting dress It sets, also can be separately as the fluorescent paint of security pattern, easy to operate, preparation process is simple, and yield is high, does not need complex and expensive Equipment, it is easy to accomplish industrialized production.
While there has been shown and described that the embodiment invented, for the ordinary skill in the art, Ke Yili Solution can carry out these embodiments in the case where not departing from the principle and spirit of invention a variety of variations, modification, replace and become The range of type, invention is defined by the appended claims and the equivalents thereof.

Claims (7)

1. a kind of multiduty fluorescent crystal material, which is characterized in that including following quality proportioning:O-phenylenediamine 4-8%, isophthalic Diamines 3-6%, zinc-cadmium sulfide 6-12%, morin 8-16%, zirconium oxide 5-10%, strontium carbonate 7-14%, silicon nitride 10-20%, solvent 7-14%。
2. a kind of multiduty fluorescent crystal material according to claim 1, it is characterised in that:Match including following quality Than o-phenylenediamine 4%, m-phenylene diamine (MPD) 3%, zinc-cadmium sulfide 6%, morin 8%, zirconium oxide 5%, strontium carbonate 7%, silicon nitride 10%, solvent 7%。
3. a kind of multiduty fluorescent crystal material according to claim 1, it is characterised in that:Match including following quality Than, o-phenylenediamine 5.5%, m-phenylene diamine (MPD) 4%, zinc-cadmium sulfide 8%, morin 11%, zirconium oxide 7%, strontium carbonate 9%, silicon nitride 13%, Solvent 9%.
4. a kind of multiduty fluorescent crystal material according to claim 1, it is characterised in that:Match including following quality Than o-phenylenediamine 7%, m-phenylene diamine (MPD) 5%, zinc-cadmium sulfide 10%, morin 14%, zirconium oxide 8.7%, strontium carbonate 11%, silicon nitride 17%, solvent 11%.
5. a kind of multiduty fluorescent crystal material according to claim 1, it is characterised in that:Match including following quality Than, o-phenylenediamine 8%, m-phenylene diamine (MPD) 6%, zinc-cadmium sulfide 12%, morin 16%, zirconium oxide 10%, strontium carbonate 14%, silicon nitride 20%, Solvent 14%.
6. a kind of multiduty fluorescent crystal material according to claim 1, it is characterised in that:The solvent includes following Quality proportioning, formamide 13-26%, ethylene glycol 10-20%, light stabilizer 7-14%, distilled water 20-40%.
7. a kind of preparation method of multiduty fluorescent crystal material as described in claim 1-6, it is characterised in that:Including with Lower step:
S1:Raw material preparation, by o-phenylenediamine, m-phenylene diamine (MPD), zinc-cadmium sulfide, morin, zirconium oxide, strontium carbonate and silicon nitride according to Set ratio, weighing are taken, and are placed in same container, are sufficiently stirred;
S2:Milled processed, will carry out more the raw mixture that is sufficiently stirred be ground by planetary ball mill, milling time It it is 20-60 minutes, final grinding finally obtains raw material hybrid particles at the particle of 100-400 mesh;
S3:Raw material hybrid particles are put into heating container, and are added load weighted molten according to both certainty ratios by heat treatment Then agent is sealed processing, puts into muffle furnace later, temperature, and the control in 4-7 hours are controlled with temperature controller Temperature rise is to 340 degree, quiet to put 4-7 days and in 340 degree, is then taking out, quiet to let cool but, obtains the thick embryo of fluorescent crystal;
S4:The thick embryo of fluorescent crystal is cut into the fluorescent crystal of the sizes such as uniform by final molding by cutter device.
CN201810079074.7A 2018-01-26 2018-01-26 A kind of multiduty fluorescent crystal material and preparation method thereof Pending CN108277005A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1789373A (en) * 2005-11-15 2006-06-21 中国地质科学院矿产综合利用研究所 Preparation method of fluorescent grade strontium carbonate
CN103074063A (en) * 2012-12-19 2013-05-01 青岛盛瀚色谱技术有限公司 Fluorescent material
CN103525402A (en) * 2013-09-18 2014-01-22 中国科学院宁波材料技术与工程研究所 Fluorescent material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1789373A (en) * 2005-11-15 2006-06-21 中国地质科学院矿产综合利用研究所 Preparation method of fluorescent grade strontium carbonate
CN103074063A (en) * 2012-12-19 2013-05-01 青岛盛瀚色谱技术有限公司 Fluorescent material
CN103525402A (en) * 2013-09-18 2014-01-22 中国科学院宁波材料技术与工程研究所 Fluorescent material and preparation method thereof

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Application publication date: 20180713