CN108841376A - The method that Cu deposition improves blue aluminate long-afterglow material luminescent properties - Google Patents

The method that Cu deposition improves blue aluminate long-afterglow material luminescent properties Download PDF

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CN108841376A
CN108841376A CN201810547123.5A CN201810547123A CN108841376A CN 108841376 A CN108841376 A CN 108841376A CN 201810547123 A CN201810547123 A CN 201810547123A CN 108841376 A CN108841376 A CN 108841376A
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long
sral
luminescent powder
solution
luminescent
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海鸥
曾柏林
武秀兰
任强
任宇涵
白文妮
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • 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
    • C09K11/7792—Aluminates
    • 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
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media

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

Abstract

The invention discloses Cu to deposit the method for improving blue aluminate long-afterglow material luminescent properties, by Sr4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+Luminescent powder surface Adsorption of Cu Cl2Solution, using photoreduction, in luminescent powder surface supported copper particle, to obtain the Sr of copper area load4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+Long after glow luminous material.The method increase the long-persistence luminous performances of aluminate long afterglow materials luminescent material, and the preparation method is simple, are convenient for industrialization large-scale production, the material of preparation long-persistence luminous performance with higher.

Description

The method that Cu deposition improves blue aluminate long-afterglow material luminescent properties
Technical field
The invention belongs to luminescent material technical fields, and in particular to Cu deposition improves blue aluminate long-afterglow material and shines The method of performance.
Background technique
Long after glow luminous material be can absorb the light sources such as natural light, light, and can continuous illumination energy conservation and environmental protection material. Long after glow luminous material has the absorption peak and emission peak of feature, and can store energy, to realize without electroluminescence, in spoke The fields such as monitoring, bio-medical, photocatalysis are penetrated with very strong application prospect.
The appearance of aluminate long after glow luminous material be exploitation a new generation long-afterglow luminescent powder beginning, aluminate it is glimmering Light powder MAl2O4:Eu2+(M can be Sr, Ca, Ba) has just been reported by pallila et al. early in nineteen sixty-eight, MAl2O4:Eu2+, Dy3+It is in MAl2O4:Eu2+In joined other rare earth ion Dy3+, Dy3+Trap is formed in host material, to make this Class material has afterglow property.After this kind of material is excited, persistence can reach 10h or more, have compared with previous generation good Good afterglow property, therefore cause everybody extensive concern.A large amount of scholars are prepared for such material by different preparation methods Material, has the report largely about aluminate long after glow luminous material, original intensity and persistence are also continuous every year It improves, Sr4Al14O25:Eu2+,Dy3+It is exactly one type, the exploitation of such material can further push long after glow luminous material Application, for metal deposit in addition to that can enhance local luminous performance, metal nanoparticle surface modification can also promote ultraviolet lighting The promotion of lower correlated performance has more research, such as Au, Ag, Pt, the various metals such as Cu on other basis materials such as photocatalysis Surface-modified substrates material, the explanation for obtaining approval are metal nanoparticles as electron trap, reduce answering for electron hole pair Conjunction rate is captured by more traps, and luminescent properties are greatly improved after release, but blue there is presently no being improved using surface deposition Color aluminate long after glow luminous material SrAl2O4：Eu2+, Dy3+And Sr4Al14O25:Eu2+,Dy3+The report of luminescent properties.
Summary of the invention
The object of the present invention is to provide Cu to deposit the method for improving blue aluminate long-afterglow material luminescent properties, utilizes gold Belong to copper area load in SrAl2O4：Eu2+, Dy3+Or Sr4Al14O25:Eu2+,Dy3+Improve its long-persistence luminous performance.
The technical scheme adopted by the invention is that Cu deposition improves the side of blue aluminate long-afterglow material luminescent properties Method, by Sr4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+Luminescent powder surface Adsorption of Cu Cl2Solution utilizes photo-reduction Reaction, in luminescent powder surface supported copper particle, to obtain the Sr of copper area load4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2 +, Dy3+Long after glow luminous material.
Feature of the present invention also resides in,
Further, the method is specifically implemented according to the following steps：
Step 1, by the Sr after cleaning4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+CuCl is added in luminescent powder2It is molten It in the mixed solution of liquid, acetic acid and alcohol, is stirred, ultrasonic photoreduction is carried out under ultraviolet light irradiation；
Step 2, the solution after step 1 reaction be filtered, washed, dried to get copper area load is arrived Sr4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+Long-afterglow luminescent powder.
Preferably, the Sr4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+The cleaning of luminescent powder, specially：It will Sr4Al14O25:Eu2+,Dy3+Or SrAl2O4：Eu2+, Dy3+Luminescent powder pours into absolute alcohol, and alcohol is made to flood luminescent powder, super Ultrasound 4-10 minutes in sound instrument, ultrasound are filtered after the completion, are placed in baking oven at 90-150 DEG C 15-25 minutes dry.
Preferably, the CuCl2The molar concentration of solution is 0.01-0.2mmolL-1。
Preferably, the CuCl2Solution, acetic acid and alcohol by volume ratio (1-10):(1-4):500.
Preferably, the ultrasonic photo-reduction time is 2-4 hours.
The invention has the advantages that Cu deposition of the present invention improves the side of blue aluminate long-afterglow material luminescent properties Method obtains the aluminate long after glow luminous material of copper surface load using photoreduction met hod, improves aluminate long afterglow hair The long-persistence luminous performance of luminescent material, the preparation method simple possible, while entire reaction process equipment requirement low (baking oven and purple Outer lamp), without reaction units such as expensive various processing synthesis devices and high temperature and pressure, has and be easy to high-volume synthesis etc. Advantage, strong operability, synthesis technology is simple, is convenient for industrialization large-scale production, the material of preparation long afterglow hair with higher Optical property is expected to generate good social and economic benefit.
Detailed description of the invention
Fig. 1 is the Sr of copper surface load prepared by the embodiment of the present invention 14Al14O25:Eu2+,Dy3+With it is unsupported Sr4Al14O25:Eu2+,Dy3+Absorption curve figure；
Fig. 2 is the Sr of copper surface load prepared by the embodiment of the present invention 14Al14O25:Eu2+,Dy3+With it is unsupported Sr4Al14O25:Eu2+,Dy3+Decay curve figure；
Fig. 3 is the Sr of copper surface load prepared by the embodiment of the present invention 14Al14O25:Eu2+,Dy3+Scanning electron microscope (SEM) photograph.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The method that Cu deposition of the present invention improves blue aluminate long-afterglow material luminescent properties, in Sr4Al14O25:Eu2+,Dy3 +Or SrAl2O4：Eu2+, Dy3+Luminescent powder surface adsorbs one layer of CuCl2Solution generates be carried under the irradiation of ultraviolet light Sr4Al14O25:Eu2+,Dy3+Or SrAl2O4：Eu2+, Dy3+Copper particle, then wash away unreacted CuCl with alcohol2And it inhales The poor copper particle of attached power, obtains the Sr of copper area load4Al14O25:Eu2+,Dy3+Or SrAl2O4：Eu2+, Dy3+It is long-persistence luminous Material.
It is specifically implemented according to the following steps：
Step 1, by Sr4Al14O25:Eu2+,Dy3+Or SrAl2O4：Eu2+, Dy3+Luminescent powder pours into absolute alcohol, makes alcohol Luminescent powder is flooded, ultrasound 4-10 minutes in Ultrasound Instrument, ultrasound is filtered after the completion, is placed in baking oven and is done at 90-150 DEG C It is 15-25 minutes dry；
Sr4Al14O25:Eu2+,Dy3+Or SrAl2O4：Eu2+, Dy3+It is prepared using high temperature solid-state, granular size 10-500 Micron.In the particle size range, luminescent powder performance is best.
Step 2, by CuCl2It is dissolved in alcohol and forms homogeneous solution, wherein CuCl2The molar concentration of solution is 0.01- 0.2mmol·L-1；
Step 3, by step 2 gained CuCl2Solution, acetic acid and absolute alcohol are according to volume ratio (1-10):(1-4):500 is mixed Conjunction forms homogeneous solution；
Step 4, luminescent powder step 1 obtained pours into the resulting solution of step 3, and solution is made to flood luminescent powder, stirring It 10-25 minutes, is subsequently placed in Ultrasound Instrument, is carried out under ultraviolet light irradiation ultrasonic photo-reduction 2-4 hours；
Step 5, step 4 acquired solution is filtered, and is washed 1-3 times with absolute alcohol, is placed in baking oven in 100- 10-20 minutes are dried at 160 DEG C to get the Sr loaded to copper surface4Al14O25:Eu2+,Dy3+Or SrAl2O4：Eu2+, Dy3+ Long-afterglow luminescent powder.
In Sr4Al14O25:Eu2+,Dy3+Or SrAl2O4：Eu2+, Dy3+After blue long-afterglow luminescent powder surface deposits Cu, surface Plasma effect can also improve such composite material to the absorption intensity of light.It can promote point in light induced electron and hole simultaneously From, improve the concentration of carrier, after being captured by trap slow release realize afterglow property raising.
The present invention obtains the aluminate long after glow luminous material of copper surface load using photoreduction met hod, improves aluminic acid The long-persistence luminous performance of salt long after glow luminous material, the preparation method simple possible, while entire reaction process equipment requirement is low (baking oven and ultraviolet lamp) has without reaction units such as expensive various processing synthesis devices and high temperature and pressure and is easy to big The advantages that batch synthesizes, strong operability, synthesis technology is simple, is convenient for industrialization large-scale production, and the material of preparation has higher Long-persistence luminous performance, be expected to generate good social and economic benefit.
Embodiment 1
Step 1, by 1g Sr4Al14O25:Eu2+,Dy3+Luminescent powder pours into alcohol, ultrasound 5 minutes in Ultrasound Instrument, ultrasound It is filtered, is placed in baking oven at 150 DEG C 16 minutes dry after the completion；
Step 2, by CuCl2It is dissolved in alcohol and forms homogeneous solution, wherein CuCl2Molar concentration be 0.01mmol L-1；
Step 3, by step 2 gained CuCl2Solution, acetic acid and alcohol are according to 2:3:500 are mixed to form homogeneous solution；
Step 4, luminescent powder step 1 obtained is poured into the resulting solution of step 3 and is stirred 16 minutes, is subsequently placed in ultrasound In instrument, carried out under ultraviolet light irradiation ultrasonic photo-reduction 2 hours；
Step 5, step 4 acquired solution is filtered, and with ethanol wash 2 times, is placed in baking oven at 140 DEG C dry 15 minutes；Obtain the Sr of copper surface load4Al14O25:Eu2+,Dy3+Long-afterglow luminescent powder.
Fig. 1 is the absorption curve figure of the luminescent powder that metal surface loads in embodiment 1 and unsupported luminescent powder, from figure As can be seen that luminescent powder trap after superficial metal deposition is remarkably reinforced；
Fig. 2 is the decay curve figure of the luminescent powder that metal surface loads in embodiment 1 and unsupported luminescent powder；From figure As can be seen that luminescent powder afterglow property after superficial metal deposition is remarkably reinforced, original intensity improves 3 times or more, slow decay mistake Cheng Liangdu increases；
Fig. 3 is the scanning electron microscope (SEM) photograph of load luminescent powder in metal surface in embodiment 1, it can be seen from the figure that luminescent powder table Face loads the Cu particle of one layer of dispersion, and the area load of Cu particle both can guarantee shining for luminescent powder, and can also promote electronics and sky The generation and transfer in cave, to realize the raising of luminescent properties；
Embodiment 2
Step 1, by 1g SrAl2O4：Eu2+, Dy3+Luminescent powder pours into alcohol, ultrasound 10 minutes in Ultrasound Instrument, ultrasound It is filtered, is placed in baking oven at 135 DEG C 15 minutes dry after the completion；
Step 2, by CuCl2It is dissolved in alcohol and forms homogeneous solution, wherein CuCl2Molar concentration be 0.1mmolL-1；
Step 3, by step 2 gained CuCl2Solution, acetic acid and alcohol are according to 1:1:500 are mixed to form homogeneous solution；
Step 4, luminescent powder step 1 obtained pours into the resulting solution of step 3 and stirs 10min, is subsequently placed in ultrasound In instrument, carried out under ultraviolet light irradiation ultrasonic photo-reduction 2.5 hours；
Step 5, step 4 acquired solution is filtered, and with ethanol wash 1 time, is placed in baking oven at 150 DEG C dry 12 minutes；Obtain the SrAl of copper surface load2O4：Eu2+, Dy3+Long-afterglow luminescent powder.
Embodiment 3
Step 1, by 1g Sr4Al14O25:Eu2+,Dy3+Luminescent powder pours into alcohol, ultrasound 8 minutes in Ultrasound Instrument, ultrasound It is filtered, is placed in baking oven at 100 DEG C 20 minutes dry after the completion；
Step 2, by CuCl2It is dissolved in alcohol and forms homogeneous solution, wherein CuCl2Molar concentration be 0.15mmolL-1；
Step 3, by step 2 gained CuCl2Solution, acetic acid and alcohol are according to 4:3:500 are mixed to form homogeneous solution；
Step 4, luminescent powder step 1 obtained is poured into the resulting solution of step 3 and is stirred 19 minutes, is subsequently placed in ultrasound In instrument, carried out under ultraviolet light irradiation ultrasonic photo-reduction 4 hours；
Step 5, step 4 acquired solution is filtered, and with ethanol wash 3 times, is placed in baking oven at 115 DEG C dry 18 minutes；Obtain the Sr of copper surface load4Al14O25:Eu2+,Dy3+Long-afterglow luminescent powder.
Embodiment 4
Step 1, by 1g SrAl2O4：Eu2+, Dy3+Luminescent powder pours into alcohol, ultrasound 4 minutes in Ultrasound Instrument, and ultrasound is complete It is filtered, is placed in baking oven at 90 DEG C 25 minutes dry after；
Step 2, by CuCl2It is dissolved in alcohol and forms homogeneous solution, wherein CuCl2Molar concentration be 0.2mmolL-1；
Step 3, by step 2 gained CuCl2Solution, acetic acid and alcohol are according to 10:4:500 are mixed to form homogeneous solution；
Step 4, luminescent powder step 1 obtained is poured into the resulting solution of step 3 and is stirred 25 minutes, is subsequently placed in ultrasound In instrument, carried out under ultraviolet light irradiation ultrasonic photo-reduction 3 hours；
Step 5, step 4 acquired solution is filtered, and with ethanol wash 3 times, is placed in baking oven at 130 DEG C dry 14 minutes；Obtain the SrAl of copper surface load2O4：Eu2+, Dy3+Long-afterglow luminescent powder.
Embodiment 5
Step 1, by 1g Sr4Al14O25:Eu2+,Dy3+Luminescent powder pours into alcohol, ultrasound 9 minutes in Ultrasound Instrument, ultrasound It is filtered, is placed in baking oven at 145 DEG C 17 minutes dry after the completion；
Step 2, by CuCl2It is dissolved in alcohol and forms homogeneous solution, wherein CuCl2Molar concentration be 0.13mmolL-1；
Step 3, by step 2 gained CuCl2Solution, acetic acid and alcohol are according to 5:2:500 are mixed to form homogeneous solution；
Step 4, luminescent powder step 1 obtained is poured into the resulting solution of step 3 and is stirred 17 minutes, is subsequently placed in ultrasound In instrument, carried out under ultraviolet light irradiation ultrasonic photo-reduction 3.5 hours；
Step 5, step 4 acquired solution is filtered, and with ethanol wash 2 times, is placed in baking oven at 100 DEG C dry 20 minutes；Obtain the Sr of copper surface load4Al14O25:Eu2+,Dy3+Long-afterglow luminescent powder.
Embodiment 6
Step 1, by 1g SrAl2O4：Eu2+, Dy3+Luminescent powder pours into alcohol, ultrasound 7 minutes in Ultrasound Instrument, and ultrasound is complete It is filtered, is placed in baking oven at 125 DEG C 18 minutes dry after；
Step 2, by CuCl2It is dissolved in alcohol and forms homogeneous solution, wherein CuCl2Molar concentration be 0.015mmolL-1；
Step 3, by step 2 gained CuCl2Solution, acetic acid and alcohol are according to 3:4:500 are mixed to form homogeneous solution；
Step 4, luminescent powder step 1 obtained is poured into the resulting solution of step 3 and is stirred 15 minutes, is subsequently placed in ultrasound In instrument, carried out under ultraviolet light irradiation ultrasonic photo-reduction 2.5 hours；
Step 5, step 4 acquired solution is filtered, and with ethanol wash 3 times, is placed in baking oven at 160 DEG C dry 10 minutes；Obtain the SrAl of copper surface load2O4：Eu2+, Dy3+Long-afterglow luminescent powder.

Claims (6)

  1. The method that 1.Cu deposition improves blue aluminate long-afterglow material luminescent properties, which is characterized in that by Sr4Al14O25： Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+Luminescent powder surface Adsorption of Cu Cl2Solution, it is negative in luminescent powder surface using photoreduction Copper-loaded particle, to obtain the Sr of copper area load4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+Long-persistence luminous material Material.
  2. 2. the method that Cu deposition according to claim 1 improves blue aluminate long-afterglow material luminescent properties, feature It is, is specifically implemented according to the following steps：
    Step 1, by the Sr after cleaning4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+CuCl is added in luminescent powder2Solution, acetic acid And in the mixed solution of alcohol, be stirred, ultrasonic photoreduction is carried out under ultraviolet light irradiation；
    Step 2, the solution after step 1 reaction be filtered, washed, dried to get the Sr of copper area load is arrived4Al14O25： Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+Long-afterglow luminescent powder.
  3. 3. the method that Cu deposition according to claim 2 improves blue aluminate long-afterglow material luminescent properties, feature It is, the Sr4Al14O25：Eu2+, Dy3+Or SrAl2O4：Eu2+, Dy3+The cleaning of luminescent powder, specially：By Sr4Al14O25:Eu2 +,Dy3+Or SrAl2O4：Eu2+, Dy3+Luminescent powder pours into absolute alcohol, and alcohol is made to flood luminescent powder, the ultrasound 4- in Ultrasound Instrument 10 minutes, ultrasound was filtered after the completion, was placed in baking oven at 90-150 DEG C 15-25 minutes dry.
  4. 4. the method that Cu deposition according to claim 2 improves blue aluminate long-afterglow material luminescent properties, feature It is, the CuCl2The molar concentration of solution is 0.01-0.2mmolL-1。
  5. 5. the method that Cu deposition according to claim 4 improves blue aluminate long-afterglow material luminescent properties, feature It is, the CuCl2Solution, acetic acid and alcohol by volume ratio (1-10):(1-4):500.
  6. 6. the method that Cu deposition according to claim 2 improves blue aluminate long-afterglow material luminescent properties, feature It is, the ultrasound photo-reduction time is 2-4 hours.
CN201810547123.5A 2018-05-31 2018-05-31 The method that Cu deposition improves blue aluminate long-afterglow material luminescent properties Pending CN108841376A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116640570A (en) * 2023-05-29 2023-08-25 江苏师范大学 Super-long afterglow red fluorescent powder material and preparation method thereof

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CN102373059A (en) * 2010-08-13 2012-03-14 海洋王照明科技股份有限公司 Silicate fluorescent material and manufacturing method thereof

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ZHENG TONG ET AL.: "Surface Modification of SrAl2O4: Eu2+, Dy3+ and Sr4Al14O25: Eu2+, Dy3+ Long Lasting Phosphors and Their Application in Water-borne Paint", 《J CHIN CERAM SOC (ENG)》 *
覃欣欣等: "银颗粒包覆CaTiO3:Eu3+荧光粉的制备及其光学性能的研究", 《硅酸盐通报》 *

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Application publication date: 20181120