CN113502161B - Preparation method of fluorescent material for PDP - Google Patents

Preparation method of fluorescent material for PDP Download PDF

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CN113502161B
CN113502161B CN202110672733.XA CN202110672733A CN113502161B CN 113502161 B CN113502161 B CN 113502161B CN 202110672733 A CN202110672733 A CN 202110672733A CN 113502161 B CN113502161 B CN 113502161B
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microsphere
particles
nano sio
fluorescent material
preparation
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CN113502161A (en
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解文杰
黄石
陆孝龙
李�浩
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Anhui Jianzhu University
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Anhui Jianzhu University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • 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
    • C09K11/7783—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
    • C09K11/7797—Borates

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

Abstract

The application discloses a preparation method of a fluorescent material for PDP, comprising the following steps: selecting a molecular general formula Y 0.9‑x (La，Sc，Bi) x BO 3 :Eu 3+ Wherein x is more than or equal to 0 and less than or equal to 0.1, and preparing the fluorescent material into fluorescent particles for standby; preparation of nano SiO 2 The microsphere suspension is reserved; phosphor particles and nano SiO 2 The microsphere suspension is mixed and stirred uniformly according to the mass ratio of 4:1-1:1.5, the water is removed by evaporation and drying at the low temperature of 40-60 ℃, and then the heat treatment is carried out at the temperature of 500-550 ℃ in protective atmosphere, so as to obtain the fluorescent material coated with the protective layer. The color purity and the brightness of the fluorescent material prepared by the application reach higher levels, and the use requirement of PDP can be met; the phosphor material is nano SiO 2 The microsphere particles are used as a coating protective layer, the protective layer is uniform and compact, the influence of the hydrothermal environment on the phosphor material is obviously reduced on the premise of ensuring good luminescence and light transmission performance, the maintenance of the brightness of the phosphor material is facilitated, and the display quality of the plasma flat panel display screen is prevented from being reduced.

Description

Preparation method of fluorescent material for PDP
Technical Field
The application relates to the technical field of fluorescent materials, in particular to a preparation method of a fluorescent material for PDP.
Background
The fluorescent material is prepared by mixing metal (zinc and chromium) sulfide or rare earth oxide with a trace amount of active agent and calcining. Colorless or pale white, which is visible light (400-800 nm) with various colors according to the variety and content of metals and activators in the pigment under the irradiation of ultraviolet light (200-400 nm). Along with the progress of scientific technology, the research of fluorescent materials is more and more, and the application range of fluorescent materials is wider and wider. Besides being used as dye, the fluorescent substance is widely applied to the fields of organic pigment, optical brightening agent, photooxidant, paint, chemical and biochemical analysis, solar energy collector, anti-counterfeiting mark, medicine tracing, laser and the like.
The PDP (Plasma Display Panel ) is a display technology using gas discharge, and its operation principle is very similar to that of a fluorescent lamp. The plasma tube is used as a light-emitting element, each plasma tube corresponds to a pixel on a screen, glass is used as a substrate of the screen, the substrates are separated by a certain distance, and the periphery of each substrate is hermetically sealed to form a plurality of discharge spaces. The discharge space is filled with a mixed inert gas such as neon, xenon and the like as a working medium. The inner sides of the two glass substrates are coated with metal oxide conductive films as excitation electrodes. When a voltage is applied to the electrodes, a plasma discharge phenomenon occurs in the mixed gas in the discharge space. The gas plasma discharge generates ultraviolet rays, which excite the fluorescent screen, and the fluorescent screen emits visible light, thereby displaying an image.
While the PDP has a high demand for fluorescent materials, the fluorescent materials currently used in the PDP on the market have a reduced light emission characteristic, such as a reduced brightness, when exposed to water or heat for a long period of time during operation, resulting in a reduced display quality of the PDP. The prior technical researches show that the ceramic microsphere particles (silicate and aluminosilicate) are adopted to coat and protect the fluorescent material, so that the decline trend of the luminous characteristics can be slowed down to a certain extent. However, the ceramic microsphere particles have too high viscosity and uneven thickness when forming the protective layer; in addition, the ceramic microsphere particles have poor permeability, and the overall brightness level of the fluorescent material is reduced.
Disclosure of Invention
The application aims to provide a preparation method of a fluorescent material for PDP, which solves the defect that the existing fluorescent material for PDP is easy to be influenced by water and heat environment to cause the reduction of luminous characteristics.
The application realizes the above purpose through the following technical scheme:
a preparation method of a fluorescent material for PDP comprises the following steps:
step one: selecting a molecular general formula Y 0.9-x (La，Sc，Bi) x BO 3 :Eu 3+ Wherein x is more than or equal to 0 and less than or equal to 0.1, and preparing the fluorescent material into fluorescent particles for standby;
step two: preparation of nano SiO 2 The microsphere suspension is reserved;
step three: combining the phosphor particles in the first step with the nanoparticles in the second stepSiO 2 The microsphere suspension is mixed and stirred uniformly according to the mass ratio of 4:1-1:1.5, the water is removed by evaporation and drying at the low temperature of 40-60 ℃, and then the heat treatment is carried out at the temperature of 500-550 ℃ in protective atmosphere, so as to obtain the fluorescent material coated with the protective layer.
A further improvement is that the phosphor particles have a particle diameter of 4 to 10. Mu.m.
A further improvement is that the nano SiO 2 The specific preparation steps of the microsphere suspension are as follows: mixing ethanol, ammonia water and deionized water, adding a precursor, stirring at 400-600rpm for reaction for 8-12h, separating, and washing to obtain nano SiO 2 Microsphere particles, and then nano SiO 2 Dispersing the microsphere particles in 3-8 times of water to obtain nano SiO 2 Microsphere suspensions.
The precursor is selected from one of methyl orthosilicate, tetraethyl orthosilicate, isopropyl orthosilicate or butyl orthosilicate.
The further improvement is that the ultrasonic dispersion is carried out for 20min at intervals of 1-3h in the stirring reaction process.
A further improvement is that the phosphor particles and nano SiO 2 The microsphere suspension is mixed and stirred uniformly according to the mass ratio of 2:1.
The further improvement is that the protective atmosphere is nitrogen atmosphere or argon atmosphere.
The application has the beneficial effects that: the color purity and the brightness of the fluorescent material prepared by the application reach higher levels, and the use requirement of PDP can be met; the phosphor material is nano SiO 2 The microsphere particles are used as a coating protective layer, the protective layer is uniform and compact, the influence of the hydrothermal environment on the phosphor material is obviously reduced on the premise of ensuring good luminescence and light transmission performance, the maintenance of the brightness of the phosphor material is facilitated, the service life of the phosphor material is prolonged, and the display quality of the plasma flat panel display screen is prevented from being reduced.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of the phosphor material prepared in example 2;
fig. 2 is a Scanning Electron Microscope (SEM) image of the phosphor material prepared in comparative example 1.
Detailed Description
The present application will be described in further detail with reference to the accompanying drawings, wherein it is to be understood that the following detailed description is for the purpose of further illustrating the application only and is not to be construed as limiting the scope of the application, as various insubstantial modifications and adaptations of the application to those skilled in the art can be made in light of the foregoing disclosure.
Example 1
A preparation method of a fluorescent material for PDP comprises the following steps:
step one: selecting a molecular general formula Y 0.88 (La，Sc，Bi) 0.02 BO 3 :Eu 3+ Preparing fluorescent particles from the fluorescent material for standby, wherein the particle size of the fluorescent particles is 4 mu m; the preparation method of the fluorescent material is that in the prior art, for example, after mixing the oxide of the related element and boric acid, the mixture is firstly kept at 500 ℃ for 2 hours, cooled, ground and kept at 1000 ℃ for 3 hours again, and the fluorescent material is obtained (the same applies below).
Step two: preparation of nano SiO 2 The microsphere suspension is ready for use, and specifically comprises the following steps: mixing ethanol, ammonia water and deionized water, adding methyl orthosilicate, stirring at 400rpm for reaction for 12h, separating, and washing to obtain nanometer SiO 2 Microsphere particles, and then nano SiO 2 Dispersing the microsphere particles in 3 times of water to obtain nano SiO 2 Microsphere suspensions;
step three: combining the phosphor particles in the first step with the nano SiO in the second step 2 The microsphere suspension is mixed according to the mass ratio of 4:1 and is uniformly stirred, ultrasonic dispersion is carried out for 20min every 1h in the stirring reaction process, moisture is removed by low-temperature evaporation and drying at 40 ℃, and then heat treatment at 500 ℃ is carried out in nitrogen atmosphere, so that the phosphor material coated with the protective layer is obtained.
Example 2
A preparation method of a fluorescent material for PDP comprises the following steps:
step one: selecting a molecular general formula Y 0.85 (La，Sc，Bi) 0.05 BO 3 :Eu 3+ Wherein the phosphor particles are prepared for standby, and the particle size of the phosphor particles is 7 μm;
step two: preparation of nano SiO 2 The microsphere suspension is ready for use, and specifically comprises the following steps: mixing ethanol, ammonia water and deionized water, adding tetraethyl orthosilicate, stirring at 500rpm for reaction for 10h, separating, and washing to obtain nanometer SiO 2 Microsphere particles, and then nano SiO 2 Dispersing the microsphere particles in 6 times of water to obtain nano SiO 2 Microsphere suspensions;
step three: combining the phosphor particles in the first step with the nano SiO in the second step 2 The microsphere suspension is mixed according to the mass ratio of 2:1 and is uniformly stirred, ultrasonic dispersion is carried out for 20min every 2h in the stirring reaction process, moisture is removed by evaporation and drying at the low temperature of 50 ℃, and then the heat treatment at the temperature of 520 ℃ is carried out in the argon atmosphere, so that the fluorescent material coated with the protective layer is obtained.
Example 3
A preparation method of a fluorescent material for PDP comprises the following steps:
step one: selecting a molecular general formula Y 0.82 (La，Sc，Bi) 0.08 BO 3 :Eu 3+ Wherein the phosphor particles are prepared for standby, and the particle size of the phosphor particles is 10 μm;
step two: preparation of nano SiO 2 The microsphere suspension is ready for use, and specifically comprises the following steps: mixing ethanol, ammonia water and deionized water, adding isopropyl orthosilicate, stirring at 600rpm for reaction for 8h, separating, and washing to obtain nanometer SiO 2 Microsphere particles, and then nano SiO 2 Dispersing the microsphere particles in 8 times of water to obtain nano SiO 2 Microsphere suspensions;
step three: combining the phosphor particles in the first step with the nano SiO in the second step 2 The microsphere suspension is mixed according to the mass ratio of 1:1.5 and is uniformly stirred, ultrasonic dispersion is carried out for 20min every 3h in the stirring reaction process, the water is removed by evaporation and drying at the low temperature of 60 ℃, and then the heat treatment at 550 ℃ is carried out in the nitrogen atmosphere, thus obtaining the coatingA phosphor material having a protective layer.
Comparative example 1
Which is essentially the same as example 2, the only difference being that: nano SiO 2 The microsphere suspension is replaced by ceramic microsphere suspension with equal mass concentration, the ceramic microsphere suspension is prepared by dispersing ceramic microspheres in 6 times of water, and the ceramic microspheres and nano SiO 2 The particle sizes of the microsphere particles are equal.
Comparative example 2
Selecting Y 0.88 (La，Sc，Bi) 0.02 BO 3 :Eu 3+ The phosphor particles of the phosphor material are not coated and are directly used as the phosphor material.
The phosphor material obtained in example 2 was subjected to electron microscopic scanning, the scanning results are shown in fig. 1, and the phosphor material obtained in comparative example 1 was further subjected to electron microscopic scanning, the scanning results are shown in fig. 2. It can be seen that the particles of the protective layer of the phosphor material prepared in example 2 are significantly more uniformly distributed and dense, and the overall protective effect is better.
The phosphor materials prepared in examples 1 to 3 and comparative examples 1 and 2 were subjected to performance tests including initial relative brightness, relative brightness after 80% humidity environment (3000 hours), and relative brightness after 200℃environment (2000 hours). The relative luminance refers to a relative value when the initial luminance of comparative example 3 is set to 100%.
The statistics of the test results are shown in the following table:
as can be seen from the above table, the initial brightness of the phosphor materials prepared in examples 1 to 3 of the present application was consistent with the initial brightness when the protective layer was not coated, indicating that the protective layer has excellent light transmittance, so that the overall brightness level of the phosphor material was not lowered, but the comparative example 1 was lowered to some extent; in addition, examples 1-3 maintained higher brightness levels in terms of brightness performance after 80% humidity (3000 h) and after 200 ℃ environment (2000 h), with significantly less degradation compared to comparative examples 1 and 2. Therefore, the application can obviously reduce the influence of the hydrothermal environment on the phosphor material, is beneficial to the maintenance of the brightness of the phosphor material, prolongs the service life of the phosphor material and avoids the display quality degradation of the plasma flat panel display screen.
The foregoing examples illustrate only a few embodiments of the application and are described in detail herein without thereby limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application.

Claims (1)

1. A preparation method of a fluorescent material for PDP comprises the following steps:
step one: selecting a molecular general formula Y 0.85 (La，Sc，Bi) 0.05 BO 3 :Eu 3+ Wherein the phosphor particles are prepared for standby, and the particle size of the phosphor particles is 7 μm;
step two: preparation of nano SiO 2 The microsphere suspension is ready for use, and specifically comprises the following steps: mixing ethanol, ammonia water and deionized water, adding tetraethyl orthosilicate, stirring at 500rpm for reaction for 10h, separating, and washing to obtain nanometer SiO 2 Microsphere particles, and then nano SiO 2 Dispersing the microsphere particles in 6 times of water to obtain nano SiO 2 Microsphere suspensions;
step three: combining the phosphor particles in the first step with the nano SiO in the second step 2 Mixing microsphere suspension according to the mass ratio of 2:1, stirring uniformly, performing ultrasonic dispersion for 20min every 2h in the stirring reaction process, removing water by low-temperature evaporation and drying at 50 ℃, and performing heat treatment at 520 ℃ in argon atmosphere to obtain a fluorescent material coated with a protective layer;
by adopting nano SiO 2 The microsphere particles are used as a coating protective layer, so that the influence of the hydrothermal environment on the fluorescent material is reduced.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101298557A (en) * 2008-06-06 2008-11-05 浙江理工大学 Preparation of europium-doped yttrium borate spherical luminescent material
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
CN102660281A (en) * 2012-05-28 2012-09-12 北京晶创达科技有限公司 Silica-coated orange-red phosphor and preparation method thereof
CN104017558A (en) * 2014-04-14 2014-09-03 江苏嘉娜泰有机硅有限公司 Method for improving sedimentation performance of fluorescent powder for LED (Light Emitting Diode) packaging

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101298557A (en) * 2008-06-06 2008-11-05 浙江理工大学 Preparation of europium-doped yttrium borate spherical luminescent material
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
CN102660281A (en) * 2012-05-28 2012-09-12 北京晶创达科技有限公司 Silica-coated orange-red phosphor and preparation method thereof
CN104017558A (en) * 2014-04-14 2014-09-03 江苏嘉娜泰有机硅有限公司 Method for improving sedimentation performance of fluorescent powder for LED (Light Emitting Diode) packaging

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Luminescence optimization with superior asymmetric ratio (red/orange) and color purity of MBO3:Eu3+@SiO2 (M = Y, Gd and Al) nano down-conversion phosphors;U. Rambabu 等;《RSC Advances》;20121121;第3卷;第1368-1379页 *

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