CN105218937A - The EVA master batch of EVA adhesive film - Google Patents

The EVA master batch of EVA adhesive film Download PDF

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CN105218937A
CN105218937A CN201510723917.9A CN201510723917A CN105218937A CN 105218937 A CN105218937 A CN 105218937A CN 201510723917 A CN201510723917 A CN 201510723917A CN 105218937 A CN105218937 A CN 105218937A
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ultrasonic vibration
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CN105218937B (en
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严梅霞
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Tianjin Shenglin Plastic Products Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C08L23/0853—Vinylacetate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • 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
    • C09K11/7794—Vanadates; Chromates; Molybdates; Tungstates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/08—Copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/04—Homopolymers or copolymers of ethene
    • C08J2423/08—Copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a kind of EVA master batch of EVA adhesive film, be prepared from by the following raw material with parts by weight: ethylene-vinyl acetate copolymer 30 ~ 50 parts, ethylene-octene copolymer 5 ~ 10 parts, polyethylene 1 ~ 5 part, initiator 0.1 ~ 1 part, tackifier 0.5 ~ 1.5 part and ruddiness fluorescent composition 5.05 ~ 9 parts; Described ruddiness fluorescent composition is YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+or YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+agSiO 2ruddiness fluorescent composition.The EVA master batch of this EVA adhesive film, avoids the shortcoming that in conventional solar photovoltaic assembly EVA adhesive film production process, additive dispersion is easily uneven, improves the quality of EVA adhesive film; The ruddiness fluorescent composition that it comprises, not only better dispersed, and there is stronger phototranstormation efficiency, luminous intensity is comparatively strong, improves the applicability of EVA master batch further.

Description

The EVA master batch of EVA adhesive film
Technical field
The present invention relates to a kind of EVA master batch of EVA adhesive film.
Background technology
EVA refers to ethylene-vinyl acetate resin, be a kind of can as the Plastic Resin of hot melt adhesive, be used in the field such as bonding of doubling glass, the encapsulation of solar photovoltaic assembly, metal sheet and plastic plate in large quantities, the application especially in photovoltaic field widely.There are Foster, Hai Youwei in domestic main EVA adhesive film supplier, forever consolidate.EVA adhesive film is the sticking glued membrane of a kind of thermoset in photovoltaic field; be used in photovoltaic module with the form of glass/EVA adhesive film/photovoltaic cell/EVA adhesive film/backboard; it serves and encapsulates and protect the effect of cell piece, is one of of paramount importance parts in assembly.
In prior art, in conventional solar photovoltaic assembly EVA adhesive film production process, additive dispersion is easily uneven, when particularly adding nanometer powder, not only easily causes powder agglomeration, and affects its luminescent properties; Therefore, the material and the preparation method that improve EVA adhesive film quality extremely have Practical significance.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, the invention provides a kind of EVA master batch of EVA adhesive film, avoiding the shortcoming that in conventional solar photovoltaic assembly EVA adhesive film production process, additive dispersion is easily uneven, improve the quality of EVA adhesive film; The ruddiness fluorescent composition that it comprises, not only better dispersed, and there is stronger phototranstormation efficiency, luminous intensity is comparatively strong, improves the applicability of EVA master batch further.
Technical problem to be solved by this invention is achieved by the following technical programs:
A kind of EVA master batch of EVA adhesive film, be prepared from by the following raw material with parts by weight: ethylene-vinyl acetate copolymer 30 ~ 50 parts, ethylene-octene copolymer 5 ~ 10 parts, polyethylene 1 ~ 5 part, initiator 0.1 ~ 1 part, tackifier 0.5 ~ 1.5 part and ruddiness fluorescent composition 5.05 ~ 9 parts; Described ruddiness fluorescent composition is YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+or YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+agSiO 2ruddiness fluorescent composition.
The present invention has following beneficial effect: the EVA master batch of EVA adhesive film of the present invention, avoids the shortcoming that in conventional solar photovoltaic assembly EVA adhesive film production process, additive dispersion is easily uneven, improves the quality of EVA adhesive film; The ruddiness fluorescent composition that it comprises, not only better dispersed, and to UV-light, there is stronger wide band absorption ability, also have stronger phototranstormation efficiency, luminous intensity is strong, improves the using value of EVA master batch further.
Accompanying drawing explanation
Fig. 1 represents the figure by the determination data of the size distribution of the different fluorescent material obtained, and wherein, 1-1 is that embodiment 1 step 3 obtains YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+the particle size distribution data figure of nucleocapsid fluorescent material; 1-2 is that embodiment 1 step 4 obtains YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+the particle size distribution data figure of ruddiness fluorescent composition;
Fig. 2 represents the excitation spectrum of fluorescent material 620nm supervisory wavelength that embodiment 1 to 5 and comparative example 1,2 obtain and the emmission spectrum of 365nm excitation wavelength; Wherein 2-1 to 2-7 represents embodiment 1 to embodiment 5 and the spectrogram corresponding to comparative example 1,2 respectively.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be described in detail.
Embodiment 1
One, YVO is prepared 4: Eu 3+, Sr 2+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) by above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir), dropwise instillation contains the Y (NO of the certain proportioning of 1.5mmol below 3) 36H 2o, Eu (NO 3) 3, Sr (NO 3) 2(0.9:0.03:0.07) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200 oinsulation reaction 1h under C, is down to 150 oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the Y of median size 10 ~ 15nm 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor; (5) to Y 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h(and is rapidly heated, and heat-treats under preferably fluorescent material being in this annealing temperature when temperature reaches 500 DEG C again), the Y of median size 20 ~ 30nm after acquisition thermal treatment 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor.
Two, YVO is prepared 4: Eu 3+, Bi 3+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) limit is dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol 3) 36H 2o, Eu (NO 3) 3, Bi (NO 3) 3(0.87:0.03:0.1) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180 oinsulation reaction 1.5h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the Y that median size is about 10nm 0.87vO 4: Eu 3+ 0.03, Bi 3+ 0.1nano-phosphor.
Three, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material
(1) pre-dispersed: to take the heat treated YVO of 0.1g 4: Eu 3+, Sr 2+nano-phosphor is placed in 10ml ethanol, and carries out ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained solution A; Take 0.008gYVO 4: Eu 3+, Bi 3+nano-phosphor is placed in 10ml ethanol, and carries out ultrasonic agitation (80KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 15min, obtained solution B; (2) limit ultrasonic agitation (60KHz ultrasonic vibration and 500r/min centrifugal speed stir) solution A, limit dropwise instills solution B; Continue ultrasonic agitation (50KHz ultrasonic vibration and 100r/min centrifugal speed stir) 5min and leave standstill 5min again, centrifugal and clean 3 times with acetone and obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the YVO of median size 40 ~ 60nm 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material.
Four, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition
(1) nucleocapsid fluorescent material ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol, obtained solution C; Add a certain proportion of (4:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90 odry 5h under C, to obtain being coated with SiO 2nucleocapsid fluorescent material; (2) this is coated with SiO 2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain fluorescent material mixture; (3) the fluorescent material mixture of step (2) is immersed in ultrasonic 1h in hydrofluoric acid, removes silicon-dioxide, centrifugal and dry, obtain the YVO of median size 60 ~ 80nm 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition.
Embodiment 2
On basis based on embodiment 1, by the YVO in step 3 4: Eu 3+, Sr 2+with YVO 4: Eu 3+, Bi 3+weight ratio change 1:0.5 into, all the other are identical with embodiment 1.
Embodiment 3
On basis based on embodiment 1, by the YVO in step 3 4: Eu 3+, Sr 2+with YVO 4: Eu 3+, Bi 3+weight ratio change 1:0.001 into, all the other are identical with embodiment 1.
Embodiment 4
One, YVO is prepared 4: Eu 3+, Sr 2+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) by above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir), dropwise instillation contains the Y (NO of the certain proportioning of 1.5mmol below 3) 36H 2o, Eu (NO 3) 3, Sr (NO 3) 2(0.9:0.03:0.07) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200 oinsulation reaction 1h under C, is down to 150 oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the Y of median size 10 ~ 15nm 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor; (5) to Y 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h(and is rapidly heated, and heat-treats under preferably fluorescent material being in this annealing temperature when temperature reaches 500 DEG C again), the Y of median size 20 ~ 30nm after acquisition thermal treatment 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor.
Two, YVO is prepared 4: Bi 3+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) limit is dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol 3) 36H 2o, Bi (NO 3) 3(0.87:0.1) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180 oinsulation reaction 1.5h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the Y that median size is about 10nm 0.87vO 4: Bi 3+ 0.1nano-phosphor.
Three, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Bi 3+nucleocapsid fluorescent material
(1) pre-dispersed: to take the heat treated YVO of 0.1g 4: Eu 3+, Sr 2+nano-phosphor is placed in 10ml ethanol, and carries out ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained solution A; Take 0.008gYVO 4: Bi 3+nano-phosphor is placed in 10ml ethanol, and carries out ultrasonic agitation (80KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 15min, obtained solution B1; (2) limit ultrasonic agitation (60KHz ultrasonic vibration and 500r/min centrifugal speed stir) solution A, limit dropwise instills solution B 1; Continue ultrasonic agitation (50KHz ultrasonic vibration and 100r/min centrifugal speed stir) 5min and leave standstill 5min again, centrifugal and clean 3 times with acetone and obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the YVO of median size 40 ~ 60nm 4: Eu 3+, Sr 2+yVO 4: Bi 3+nucleocapsid fluorescent material.
Four, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material
(1) by 0.05mmolEu (NO 3) 36H 2o ultrasonic disperse in 15ml ethanol solution, by YVO obtained for step 3 4: Eu 3+, Sr 2+yVO 4: Bi 3+nucleocapsid fluorescent material presoma is dispersed in above-mentioned solution; (2) (60KHz ultrasonic vibration and 500r/min centrifugal speed stir) after ultrasonic agitation 60min, reaction soln is left standstill 24h, ion exchange process is fully carried out.Wherein, Eu (NO 3) 36H 2the amount of O is according to chemical formula Y (0.9-x)vO 4: Eu 3+ (x), Bi 3+ (0.1)determine, preferably excessive a little.After reaction terminates, centrifugal, and obtain white precipitate 3 times with dehydrated alcohol and distilled water wash.Finally, 90 ounder C, dry 5h, obtains YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material.
Five, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition
(1) nucleocapsid fluorescent material ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol, obtained solution C; Add a certain proportion of (4:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90 odry 5h under C, to obtain being coated with SiO 2nucleocapsid fluorescent material; (2) this is coated with SiO 2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain fluorescent material mixture; (3) the fluorescent material mixture of step (2) is immersed in ultrasonic 1h in hydrofluoric acid, removes silicon-dioxide, centrifugal and dry, obtain the YVO of median size 60 ~ 80nm 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition.
Embodiment 5
On basis based on embodiment 1 or 4, coated one deck AgSiO again after the ruddiness fluorescent composition prepared 2nanometer film, specifically comprises the steps:
(1), under room temperature, be that the polyvinylpyrrolidone of 10000 is dissolved in 30ml ethylene glycol by 6g molecular-weight average, add 0.25gAgNO while stirring 3until formation clear solution, solution is placed in autoclave, is warming up to 130 DEG C and is incubated 30min, after being cooled to room temperature, after centrifugation, obtain quantum dot nano aluminium powder;
(2) above-mentioned for 0.15g obtained nanometer silver powder ultrasonic agitation 30min(100KHz ultrasonic vibration and 1000r/min centrifugal speed are stirred) be scattered in 30ml dehydrated alcohol and 10ml distilled water; Be that the ammoniacal liquor of 28% and the tetraethoxy TEOS of 0.15ml add in above-mentioned dispersion soln by 1.5ml massfraction, at 20 DEG C, fully stir 4h; Carry out centrifugal and with distilled water and washes of absolute alcohol 3 times, and 80 odry 3h under C, to obtain being coated with SiO 2the AgSiO of median size about 10 nanometer 2-nanometer powder;
(3) take 0.1g ruddiness fluorescent composition and be placed in 10ml ethanol, and carry out ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained solution A1; Take 0.005gAgSiO 2-nanometer powder is placed in 10ml ethanol, and carries out ultrasonic agitation (80KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 15min, obtained solution B2; Limit ultrasonic agitation (60KHz ultrasonic vibration and 500r/min centrifugal speed stir) solution A 1, limit dropwise instills solution B 2; Continue ultrasonic agitation mixing solutions 5min(50KHz ultrasonic vibration and 100r/min centrifugal speed to stir) leave standstill 5min again, centrifugal and clean 3 times with acetone, and 90 odry 4h under C, obtains the YVO of median size 70 ~ 80nm 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+agSiO 2ruddiness fluorescent composition.
Comparative example 1
One, YVO is prepared 4: Eu 3+, Sr 2+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) by above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir), dropwise instillation contains the Y (NO of the certain proportioning of 1.5mmol below 3) 36H 2o, Eu (NO 3) 3, Sr (NO 3) 2(0.9:0.03:0.07) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200 oinsulation reaction 1h under C, is down to 150 oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the Y of median size 10 ~ 20nm 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor; (5) to Y 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h(and is rapidly heated, and heat-treats under preferably fluorescent material being in this annealing temperature when temperature reaches 500 DEG C again), the Y of median size 20 ~ 30nm after acquisition thermal treatment 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor.
Two, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material
By the Y obtained by the first step 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07fluorescent material (1.6mmol) is dispersed in 10ml ethylene glycol solution, and according to R value (nucleocapsid mol ratio, i.e. R=YVO 4: Eu 3+, Ba 2+/ YVO 4: Eu 3+, Bi 3+) calculate, by the Y (NO of certain molar weight 3) 36H 2o, Eu (NO 3) 3, Bi (NO 3) 35H 2o(mol ratio is 0.87:0.03:0.1) add in above-mentioned solution, and ultrasonic vibration 20min; (2) 1.2mmolNa 3vO 412H 2o adds in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water, dropwise instills in (1) gained solution while stirring, add 20ml distilled water after stirring 5min after dissolving completely; (3) gained reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml (compactedness 70%), 200 ounder C, isothermal holding 2h, after reaction terminates, cools to room temperature with the furnace.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) finally this is deposited in 80 ounder C, dry 8h, obtains YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nano-phosphor.
Three, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition
(1) nucleocapsid fluorescent material ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol, obtained solution C; Add a certain proportion of (4:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90 odry 5h under C, to obtain being coated with SiO 2nucleocapsid fluorescent material; (2) this is coated with SiO 2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain fluorescent material mixture; (3) the fluorescent material mixture of step (2) is immersed in ultrasonic 1h in hydrofluoric acid, removes silicon-dioxide, centrifugal and dry, obtain ruddiness fluorescent composition.
Comparative example 2
On basis based on embodiment 1, remove step 3, and in step 4, by heat treated for 1g YVO 4: Eu 3+, Sr 2+nano-phosphor and 0.05gYVO 4: Eu 3+, Bi 3+nano-phosphor mixing ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol, obtained solution C; All the other are identical with embodiment 1.
Performance test analysis:
The ruddiness fluorescent composition that embodiment 1 is obtained carries out XRD diffraction, bragg peak positions all in diffractogram, relative intensity all with YVO 4standard card (JCPDS17-0341) is consistent, can be characterized by pure Tetragonal YVO 4crystalline structure, does not find other assorted peaks.
Average granulometry: the dispersion liquid obtained with ultrasonic homogenizer process, uses laser diffraction formula particle size distribution device (Shimadzu Seisakusho Ltd.'s system " SALD-7000 ") to measure median size.As can be seen from Figure 1, average granulometry: the dispersion liquid obtained with ultrasonic homogenizer process, uses laser diffraction formula particle size distribution device (Shimadzu Seisakusho Ltd.'s system " SALD-7000 ") to measure median size.As can be seen from Figure 1, the YVO of embodiment 1 step 3 acquisition 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material median size is 40 ~ 60nm; Embodiment 1 step 4 obtains ruddiness fluorescent composition median size 60 ~ 80nm, and nucleocapsid fluorescent material is carried out SiO 2remove again after coated annealing, can effectively prevent fluorescent material agglomeration from occurring and particle increase, the basic median size keeping ruddiness fluorescent composition.
As can be seen from Figure 2, comparative example 1 ruddiness fluorescent composition absorbs with certain broadening, and the band edge of absorption band is to long wavelength's red shift, but it is not very strong in the absorption of the ultraviolet region of short wavelength; Comparative example 2 ruddiness fluorescent composition compares ratio the last 1 in the absorption in short UV light district; Embodiment 1 to 5 ruddiness fluorescent composition absorption band has certain broadening, not only the band edge of absorption band is to long wavelength's red shift, in short UV light district, also there is good absorption at it simultaneously, particularly embodiment 5, absorbing comparatively other embodiments at ultraviolet region absorbs the strongest, is also the strongest equally at the emission peak of 620nm wavelength.
Present invention also offers a kind of EVA master batch of EVA adhesive film, it is filled with YVO of the present invention 4: Eu 3+, Ba 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition or YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+agSiO 2-ruddiness fluorescent composition.This EVA master batch is prepared from by the following raw material with parts by weight: ethylene-vinyl acetate copolymer 30 ~ 50 parts, ethylene-octene copolymer 5 ~ 10 parts, polyethylene 1 ~ 5 part, initiator 0.1 ~ 1 part, tackifier 0.5 ~ 1.5 part and ruddiness fluorescent composition 5.05 ~ 9 parts, this ruddiness fluorescent composition accounts for 15% of ethylene-vinyl acetate copolymer and ethylene-octene copolymer total mass.
The weight content of the vinyl acetate between to for plastic in described ethylene-vinyl acetate copolymer is 10 ~ 40%, and melting means is 15 ~ 45g/10min.In described ethylene-octene copolymer, the molar content of octene is 15 ~ 60%, and the fusing point of ethylene-octene copolymer is 40 ~ 120 DEG C.
Embodiment 6 ~ 10, comparative example 3 ~ 7, specifically fills a prescription in table 1.
The preparation method of the EVA master batch of this EVA adhesive film of embodiment 6 to 9, comparative example 3 to 7, specifically comprises the steps:
(1) ruddiness fluorescent composition is joined in 50ml deionized water, solution D is formed after ultrasonic agitation (80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stir) dispersion 20min, take 1g stearic acid to add in 100ml propyl carbinol and form E solution, after being mixed by D, E solution, ultrasonic agitation (80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stir) disperses 20min again, put into 120 DEG C of oil bath return stirrings, cool to room temperature after reaction 1h, obtains oil loving ruddiness fluorescent composition after centrifugation, deionized water wash, 90 DEG C of dryings;
(2) mix by the ruddiness fluorescent composition of table 1 weight ratio by ethylene-vinyl acetate copolymer, ethylene-octene copolymer, polyethylene, initiator, tackifier and oleophylic process;
(3) mixture step (2) prepared carries out grafting pretreatment reaction (150 DEG C) by forcing machine and extrudes, and extrudate becomes particle masterbatch through overcooling, traction, pelletizing.
Wherein, the ruddiness fluorescent composition of the ruddiness fluorescent composition of embodiment 6 to 8 obtained by embodiment 1 to 3; The ruddiness fluorescent composition of ruddiness fluorescent composition obtained by embodiment 4 of embodiment 9; The ruddiness fluorescent composition of oleophylic process in comparative example 3 accounts for 20% of ethylene-vinyl acetate copolymer and ethylene-octene copolymer total mass; The ruddiness fluorescent composition of oleophylic process in comparative example 4 accounts for 10% of ethylene-vinyl acetate copolymer and ethylene-octene copolymer total mass; The ruddiness fluorescent composition of ruddiness fluorescent composition obtained by embodiment 1 of comparative example 3,4; Ruddiness fluorescent composition in comparative example 5,6 is the ruddiness fluorescent composition of comparative example 1 and comparative example 2 respectively.
The preparation method of the EVA master batch of the EVA adhesive film of embodiment 10: ethylene-vinyl acetate copolymer, ethylene-octene copolymer, polyethylene, initiator, tackifier and ruddiness fluorescent composition mix by table 1 weight ratio by (1); (2) mixture step (1) prepared carries out grafting pretreatment reaction (150 DEG C) by forcing machine and extrudes, and extrudate becomes particle masterbatch through overcooling, traction, pelletizing.Wherein, the ruddiness fluorescent composition of ruddiness fluorescent composition obtained by embodiment 5.
The EVA master batch being used for EVA adhesive film of the various embodiments described above and comparative example is applied in EVA adhesive film, mix with EVA resin by the ratio of EVA master batch in 40:58, add other auxiliary agents (oxidation inhibitor, photostabilizer) of 2 parts again, by this mixture heating and melting film extrusion at 60 DEG C ~ 120 DEG C, obtain EVA adhesive film.Comparative example 7 does not make EVA master batch, directly carries out heating and melting and film extrusion by after formula rate and EVA resin, oxidation inhibitor, photostabilizer mixing, obtain EVA adhesive film.The property indices of EVA adhesive film is measured by the following method:
1, resistance to ultraviolet(ray) radiation energy
Test sample book is the glued membrane multi-disc of 0.5mm.Uv-radiation ageing testing method is International Electrotechnical Commission IEC61345 standard, and test condition is: temperature 60 ± 5 DEG C, wavelength 200 ~ 400nm, irradiation intensity 15KWh/m2.Determination of light transmittance presses GB/T2410 standard, its printing opacity conservation rate=(sample mean transmittance after irradiation/pre-irradiation sample mean transmittance) × 100%.Yellowness index is analyzed according to GB2409-80.Test result is as shown in table 1.
2, wet and heat ageing resistant performance
Wet and heat ageing resistant testing method presses GB/T2423.3 standard, and test condition is: temperature 85 DEG C, relative humidity 85%, time 2000h.Determination of light transmittance presses GB/T2410 standard, its printing opacity conservation rate=(sample mean transmittance after irradiation/pre-irradiation sample mean transmittance) × 100%.Yellowness index is analyzed according to GB2409-80.Test result is as shown in table 1.
The formula of each embodiment of table 1 and comparative example and make the test-results of EVA adhesive film
As can be seen from Table 1, the stripping strength result of the printing opacity conservation rate of gained embodiment 4 to 10, photoelectric conversion rate and glass thereof is obviously better than comparative example, shows the superiority of formula.
The above embodiment only have expressed embodiments of the present invention; it describes comparatively concrete and detailed; but therefore can not be interpreted as the restriction to the scope of the claims of the present invention; in every case the technical scheme adopting the form of equivalent replacement or equivalent transformation to obtain, all should drop within protection scope of the present invention.

Claims (5)

1. the EVA master batch of an EVA adhesive film, be prepared from by the following raw material with parts by weight: ethylene-vinyl acetate copolymer 30 ~ 50 parts, ethylene-octene copolymer 5 ~ 10 parts, polyethylene 1 ~ 5 part, initiator 0.1 ~ 1 part, tackifier 0.5 ~ 1.5 part and ruddiness fluorescent composition 5.05 ~ 9 parts; Described ruddiness fluorescent composition is YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+or YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+agSiO 2ruddiness fluorescent composition.
2. the EVA master batch of EVA adhesive film according to claim 1, is characterized in that, described ruddiness fluorescent composition accounts for 15% of ethylene-vinyl acetate copolymer and ethylene-octene copolymer total mass.
3. the EVA master batch of EVA adhesive film according to claim 1, is characterized in that, described YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition carries out oleophylic process in advance.
4. the EVA master batch of EVA adhesive film according to claim 1, is characterized in that, described YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition is obtained by following methods:
One, YVO is prepared 4: Eu 3+, Sr 2+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed are stirred below the dropwise Y (NO of instillation containing the certain proportioning of 1.5mmol 3) 36H 2o, Eu (NO 3) 3, Sr (NO 3) 28ml ethylene glycol solution in, more simultaneously 80KHz ultrasonic vibration and 300r/min centrifugal speed stir 5 ~ 10min and clarify to solution, add 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200 oinsulation reaction 1h under C, is down to 150 oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature; Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 ounder C, dry 5h, obtains Y 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor; (5) to Y 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h, and after acquisition thermal treatment, median size is 20 ~ 30nmY 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor;
Two, YVO is prepared 4: Eu 3+, Bi 3+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stirring limit are dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol 3) 36H 2o, Eu (NO 3) 3, Bi (NO 3) 38ml ethylene glycol solution in, more simultaneously 80KHz ultrasonic vibration and 300r/min centrifugal speed stir 5 ~ 10min and clarify to solution, add 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180 oinsulation reaction 1.5h under C, after reaction terminates, is cooled to room temperature; Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtaining median size is 10nmY 0.87vO 4: Eu 3+ 0.03, Bi 3+ 0.1nano-phosphor;
Three, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material
(1) pre-dispersed: to take the heat treated YVO of 1g 4: Eu 3+, Sr 2+nano-phosphor is placed in 10ml ethanol, and disperses 30min, obtained solution A under carrying out 100KHz ultrasonic vibration and the stirring of 1000r/min centrifugal speed; Take 0.05gYVO 4: Eu 3+, Bi 3+nano-phosphor is placed in 10ml ethanol, and disperses 15min, obtained solution B under carrying out 80KHz ultrasonic vibration and the stirring of 1000r/min centrifugal speed; (2) limit 60KHz ultrasonic vibration and 500r/min centrifugal speed stirred solution A, limit dropwise instills solution B; Continue 50KHz ultrasonic vibration and 100r/min centrifugal speed to stir 5min and leave standstill 5min again, centrifugal and clean 3 times with acetone and obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtaining median size is 40 ~ 60nmYVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material;
Four, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition
(1) nucleocapsid fluorescent material is scattered in ethanol under 100KHz ultrasonic vibration and 1000r/min centrifugal speed stir, obtained solution C; Additional proportion is water and the ammoniacal liquor of 4:1 afterwards, and the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90 odry 5h under C, to obtain being coated with SiO 2nucleocapsid fluorescent material; (2) this is coated with SiO 2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain fluorescent material mixture; (3) the fluorescent material mixture of step (2) is immersed in ultrasonic 1h in hydrofluoric acid, removes silicon-dioxide, centrifugal and dry, obtain median size 60 ~ 80nm ruddiness fluorescent composition.
5. the EVA master batch of EVA adhesive film according to claim 1, is characterized in that, described YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition is obtained by following methods:
One, YVO is prepared 4: Eu 3+, Sr 2+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit 80 ~ 100KHz ultrasonic vibration and 300r/min are dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol below 3) 36H 2o, Eu (NO 3) 3, Sr (NO 3) 28ml ethylene glycol solution in, then 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stir 10min and clarify to solution, add 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200 oinsulation reaction 1h under C, is down to 150 oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature; Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the Y of median size 10 ~ 15nm 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor; (5) to Y 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h, the Y of median size 20 ~ 30nm after acquisition thermal treatment 0.9vO 4: Eu 3+ 0.03, Sr 2+ 0.07nano-phosphor;
Two, YVO is prepared 4: Bi 3+nano-phosphor
(1) by 1.2mmolNa 3vO 412H 2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stirring limit are dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol 3) 36H 2o, Bi (NO 3) 38ml ethylene glycol solution in, then 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stir 10min and clarify to solution, add 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180 oinsulation reaction 1.5h under C, after reaction terminates, is cooled to room temperature; Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the Y that median size is about 10nm 0.87vO 4: Bi 3+ 0.1nano-phosphor;
Three, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Bi 3+nucleocapsid fluorescent material
(1) pre-dispersed: to take the heat treated YVO of 0.1g 4: Eu 3+, Sr 2+nano-phosphor is placed in 10ml ethanol, and carries out 100KHz ultrasonic vibration and 1000r/min centrifugal speed dispersed with stirring 30min, obtained solution A; Take 0.008gYVO 4: Bi 3+nano-phosphor is placed in 10ml ethanol, and carries out 80KHz ultrasonic vibration and 1000r/min centrifugal speed dispersed with stirring 15min, obtained solution B1; (2) limit 60KHz ultrasonic vibration and 500r/min centrifugal speed stirred solution A, limit dropwise instills solution B 1; Continue ultrasonic agitation 50KHz ultrasonic vibration and 100r/min centrifugal speed to stir 5min and leave standstill 5min again, centrifugal and clean 3 times with acetone and obtain white precipitates; (4) this is deposited in 90 odry 5h under C, obtains the YVO of median size 40 ~ 60nm 4: Eu 3+, Sr 2+yVO 4: Bi 3+nucleocapsid fluorescent material;
Four, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material
(1) by 0.05mmolEu (NO 3) 36H 2o ultrasonic disperse in 15ml ethanol solution, by YVO obtained for step 3 4: Eu 3+, Sr 2+yVO 4: Bi 3+nucleocapsid fluorescent material presoma is dispersed in above-mentioned solution; (2), after 60KHz ultrasonic vibration and 500r/min centrifugal speed stir 60min, reaction soln is left standstill 24h; After reaction terminates, centrifugal, and obtain white precipitate 3 times with dehydrated alcohol and distilled water wash; 90 ounder C, dry 5h, obtains YVO 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+nucleocapsid fluorescent material;
Five, YVO is prepared 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition
(1) by nucleocapsid fluorescent material 100KHz ultrasonic vibration and 1000r/min centrifugal speed dispersed with stirring in ethanol, obtained solution C; Additional proportion is water and the ammoniacal liquor of 4:1 afterwards, and the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90 odry 5h under C, to obtain being coated with SiO 2nucleocapsid fluorescent material; (2) this is coated with SiO 2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain fluorescent material mixture; (3) the fluorescent material mixture of step (2) is immersed in ultrasonic 1h in hydrofluoric acid, removes silicon-dioxide, centrifugal and dry, obtain the YVO of median size 60 ~ 80nm 4: Eu 3+, Sr 2+yVO 4: Eu 3+, Bi 3+ruddiness fluorescent composition.
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