CN108587603A - The rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material preparation method - Google Patents

The rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material preparation method Download PDF

Info

Publication number
CN108587603A
CN108587603A CN201810547107.6A CN201810547107A CN108587603A CN 108587603 A CN108587603 A CN 108587603A CN 201810547107 A CN201810547107 A CN 201810547107A CN 108587603 A CN108587603 A CN 108587603A
Authority
CN
China
Prior art keywords
rodlike
mgsi
solution
long
ptcl
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810547107.6A
Other languages
Chinese (zh)
Inventor
海鸥
任强
武秀兰
焦叶辉
林飞
白文妮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201810547107.6A priority Critical patent/CN108587603A/en
Publication of CN108587603A publication Critical patent/CN108587603A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • C09K11/7792—Aluminates

Landscapes

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

Abstract

The invention discloses a kind of rodlike Sr2MgSi2O7 of metal platinum area load：Eu2+, Dy3+ long after glow luminous material preparation method, in rodlike Sr2MgSi2O7：Eu2+, Dy3+Material surface adsorbs one layer of H2PtCl6Solution generates under the irradiation of ultraviolet light and is carried on rodlike Sr2MgSi2O7：Eu2+, Dy3+Platinum grain, then wash away unreacted H with alcohol2PtCl6And the platinum grain that adsorption capacity is poor, obtain the rodlike Sr of platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material.Luminescent powder of the present invention afterglow property after surface metal copper deposition is remarkably reinforced, and original intensity improves 3 times or more, and slow decay process brightness improves 1.5 times.

Description

The rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material system Preparation Method
Technical field
The invention belongs to luminescent material technical fields, are related to a kind of rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+The preparation method of long after glow luminous material.
Background technology
Long after glow luminous material is a kind of after external light source irradiates, can within a very long time continuous illumination it is energy saving Environment-friendly materials.Long after glow luminous material has the absorption peak and emission peak of feature, and can store energy, Radiation monitoring, The fields such as bio-medical, photocatalysis have very strong application prospect.
Sr2MgSi2O7：Eu2+, Dy3+Long after glow luminous material emission peak is near 460nm, and turn blue coloured light, and persistence exists There is also a certain distance from large-scale application for 20h or more, good luminescence property, but its luminescent properties.Currently, luminescent properties compared with Good preparation method is high temperature solid-state method, and uses long after glow luminous material prepared by high temperature solid-state method in the preparation process of powder In, it is easy to damage the higher surface of these energy, to keep luminescent properties reduction amplitude bigger, further limit Its field applied.In Sr2MgSi2O7：Eu2+, Dy3+The centre of luminescence is Eu in long after glow luminous material2+, electron trap and hole Trap can capture the electrons and holes that generate after the excitation of centre of luminescence light, the electronics that trap captures under the action of thermal agitation with And hole returns to the compound generation long afterglow phenomenon of the centre of luminescence.Transfer light induced electron can promote light induced electron and point in hole From making more electrons and holes be captured by trap, improve its luminescent properties.
Metal deposit can also promote ultraviolet lighting in addition to that can enhance local luminous performance, metal nanoparticle surface modification 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；Metal nanoparticle surface modification simultaneously can form plasma resonance, realize the absorption of visible light.Noble metal nano Grain modification after, metallic particles activated by plasma after transfer electronics to next to matrix on, realize the transfer of electronics.
The smaller luminescent powder of grain size can directly be prepared using the method for chemical preparation, be conducive to keep luminescent powder original Luminosity, the long afterglow that different shape and size can be obtained using different preparation methods and different technologies of preparing sent out Light powder, due to the distribution of defect, using wet chemical method prepare long-afterglow luminescent powder afterglow property also need into One step improves,
To rodlike Sr2MgSi2O7：Eu2+, Dy3+Long after glow luminous material carries out surface modification, and it is solution to improve its luminescent properties A kind of certainly method of the above problem, but there is presently no about the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+More than length Brightness luminescent material improves the report of its luminescent properties.
Invention content
The object of the present invention is to provide a kind of rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+It is long-persistence luminous The preparation method of material, solves problems of the prior art.This method strong operability, synthesis technology is simple, is convenient for work Industryization mass produces.
The technical solution adopted in the present invention is the rodlike Sr of metal platinum area load of the present invention2MgSi2O7：Eu2+, Dy3+It is long The preparation method of afterglow materials, in rodlike Sr2MgSi2O7：Eu2+, Dy3+Material surface adsorbs one layer of H2PtCl6Solution, It is generated under the irradiation of ultraviolet light and is carried on rodlike Sr2MgSi2O7：Eu2+, Dy3+Platinum grain, then washed away with alcohol unreacted H2PtCl6And the platinum grain that adsorption capacity is poor, obtain the rodlike Sr of platinum area load2MgSi2O7：Eu2+, Dy3+Long-persistence luminous material Material.
It is specifically implemented according to the following steps：
Step 1, rodlike Sr is prepared2MgSi2O7：Eu2+, Dy3+Luminescent powder；
Step 2, by rodlike Sr2MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, ultrasonic in Ultrasound Instrument, and ultrasound is complete It is filtered, is placed in baking oven dry after；
Step 3, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution；
Step 4, by gained H2PtCl6Solution, acetic acid and alcohol are mixed to form homogeneous solution；
Step 5, the luminescent powder that step 2 obtains is poured into the solution obtained by step 4 and is stirred, is subsequently placed in Ultrasound Instrument, Ultrasonic photo-reduction is carried out under ultra violet lamp；
Step 6, step 5 acquired solution is filtered, ethanol wash is used in combination, be placed in baking oven lower dry to get to gold Belong to the rodlike Sr of platinum area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.
The features of the present invention also characterized in that：
Preferably, Sr in step 12MgSi2O7：Eu2+, Dy3+It is prepared using high temperature solid-state.Specific preparation method is as follows：
Step 1-1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 1-2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, and deionization is then added Water is configured to the solution of 0.02mol/L；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water The solution of 0.02mol/L is made；
Step 1-3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measures step Rapid 1 and the solution in step 2 and tetraethyl orthosilicate, it is stirred at room temperature, precipitating reagent, ultrasound is added；
The solution of gained above is poured into the liner of reaction kettle, 24-96h is reacted at 180-240 DEG C, so by step 1-4 It is washed respectively with water and absolute ethyl alcohol afterwards, is dried to obtain presoma in an oven, obtain stick in sintering in a reducing atmosphere Shape long after glow luminous material；
Preferably, H in step 22PtCl6Molar concentration be 0.01-0.2mmol L-1.It can be right in the concentration range The effect that luminescent properties are improved, concentration is too low, very little in the particle of the Dispersion on surface of luminescent powder, do not have greatly improve it is luminous The effect of performance；Concentration is too big, and the noble metal surface particle of luminescent powder is too intensive, and the light of incident light cannot be irradiated to luminescent powder Surface, to reduce the generation of light induced electron and hole, afterglow property is greatly reduced.
Preferably, H in step 42PtCl6The volume ratio of solution, acetic acid and alcohol is (1-10):(1-4):500.
Preferably, the time of ultrasonic photo-reduction described in step 5 is 2-3 hours.Your gold is the time length of photo-reduction, decide The pattern and size for belonging to deposition, have large effect to the absorption intensity of absorption spectrum, in 2-3 hour the pattern of formation and Size is more apparent to the absorption of light, and afterglow property improves larger.
The beneficial effects of the present invention are：The rodlike Sr of metal platinum area load is obtained using photoreduction met hod2MgSi2O7： Eu2+, Dy3+, for improving its long-persistence luminous performance, which can ensure original luminescent powder pattern On the basis of improve its afterglow property, have many advantages, such as to be easy to high-volume and synthesize, strong operability, synthesis technology is simple, is convenient for work Industryization mass produces, and the material of preparation has higher long-persistence luminous performance, is expected in medical diagnosis, the necks such as radiation detection Realize application in domain.
Description of the drawings
Fig. 1 is the Sr of metal platinum area load of the present invention2MgSi2O7：Eu2+, Dy3+With unsupported Sr2MgSi2O7：Eu2+, Dy3+Absorption curve figure；
Fig. 2 is the Sr of metal platinum area load of the present invention2MgSi2O7：Eu2+, Dy3+With unsupported Sr2MgSi2O7：Eu2+, Dy3+Decay curve figure；
Fig. 3 is the Sr of metal platinum area load of the present invention2MgSi2O7：Eu2+, Dy3+Scanning electron microscope (SEM) picture.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The rodlike Sr of metal platinum area load of the present invention2MgSi2O7：Eu2+, Dy3+The preparation of long after glow luminous material is specifically pressed Implement according to following steps：
Step 1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, and deionized water is then added It is configured to the solution of 0.02mol/L；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water system At the solution of 0.02mol/L；
Step 3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measures step 1 And the solution in step 2 and tetraethyl orthosilicate, it is stirred at room temperature for 24 hours, urea is added and is used as precipitating reagent, it is ultrasonic half small When；
Step 4, the solution of gained above is poured into the liner of reaction kettle, 24-96h is reacted at 180-240 DEG C, then Washing 3-5 time is carried out with water and absolute ethyl alcohol respectively, dry 2-3h obtains presoma at 80-120 DEG C in an oven, and Primordial Qi It is being sintered 2-5h in atmosphere, sintering temperature is 900-1200 DEG C, reducing atmosphere 5%H2+95%Ar, is obtained rodlike long-persistence luminous Material；
Step 5, by the rodlike Sr obtained by 1g steps 42MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, in Ultrasound Instrument Middle ultrasound 5-10 minutes, ultrasound are filtered after the completion, are placed in baking oven at 100-150 DEG C 15-20 minutes dry；
Step 6, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution, wherein H2PtCl6Molar concentration be 0.01- 0.2mmol L-1；
Step 7, by step 6 gained H2PtCl6Solution, acetic acid and alcohol are according to (1-10):(1-4):500 are mixed to form Even solution；
Step 8, the luminescent powder that step 5 obtains is added in the solution obtained by step 7 and is stirred 10 minutes, luminescent powder is made to be flooded Not yet, it is subsequently placed in Ultrasound Instrument, ultrasonic photo-reduction 2-3 hours is carried out under ultra violet lamp；
Step 9, step 8 acquired solution is filtered, ethanol wash is used in combination 1-3 times, be placed in baking oven at 100-150 DEG C Lower dry 15-20 minutes to get to the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.
The luminescent powder of metal platinum area load of the present invention is compared with unsupported luminescent powder, it is bent by the absorption of Fig. 1 Line chart can be seen that luminescent powder trap after surface metal platinum deposition and be remarkably reinforced；It can be seen by the decay curve figure of Fig. 2 Go out, luminescent powder afterglow property after surface metal platinum deposition is remarkably reinforced, and original intensity improves 3 times or more, and slow decay process is bright Degree improves 1.5 times or more.
Fig. 3 is the scanning electron microscope (SEM) of metal platinum area load luminescent powder of the present invention, as can be seen from the figure luminescent powder table The metal platinum particles of face deposition dispersion.
It is the specific preparation embodiment of luminescent material of the present invention, the Sr in embodiment below2MgSi2O7：Eu2+, Dy3+It shines Powder is prepared by laboratory, and it is 10-500 microns that preparation method, which uses high temperature solid-state method, granular size,.
Embodiment 1
Step 1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, be then configured to The solution of 0.02mol/L；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water and is made The solution of 0.02mol/L；
Step 3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measures step 1 And the solution in step 2 and tetraethyl orthosilicate, it is stirred at room temperature for 24 hours, urea is added and is used as precipitating reagent, it is ultrasonic half small When；
Step 4, the solution of gained above is poured into the liner of reaction kettle, 96h is reacted at 180 DEG C, is then used respectively Water and absolute ethyl alcohol carry out washing 3 times, and dry 3h obtains presoma at 80 DEG C in an oven, in a reducing atmosphere in sintering 5h, Sintering temperature is 900 DEG C, and reducing atmosphere 5%H2+95%Ar obtains rodlike long after glow luminous material；
Step 5, by the rodlike Sr obtained by 1g steps 42MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, in Ultrasound Instrument Middle ultrasonic 5 minutes, ultrasound was filtered after the completion, was placed in baking oven at 100 DEG C 20 minutes dry；
Step 6, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution, wherein H2PtCl6Molar concentration be 0.01mmol L-1；
Step 7, by step 6 gained H2PtCl6Solution, acetic acid and alcohol are according to 1:1:500 are mixed to form homogeneous solution；
Step 8, the luminescent powder that step 5 obtains is added in the 5ml solution obtained by step 7 and is stirred 10 minutes, is subsequently placed in In Ultrasound Instrument, ultrasonic photo-reduction 2h is carried out under ultra violet lamp；
Step 9, step 8 acquired solution is filtered, ethanol wash is used in combination 1 time, be placed in baking oven at 100 DEG C dry 20 minutes to get to the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.
Embodiment 2
Step 1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, be then configured to The solution of 0.02mol/L；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water and is made The solution of 0.02mol/L；
Step 3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measures step 1 And the solution in step 2 and tetraethyl orthosilicate, it is stirred at room temperature for 24 hours, urea is added and is used as precipitating reagent, it is ultrasonic half small When；
Step 4, the solution of gained above is poured into the liner of reaction kettle, 80h is reacted at 200 DEG C, is then used respectively Water and absolute ethyl alcohol carry out washing 3 times, and dry 2h obtains presoma at 90 DEG C in an oven, in a reducing atmosphere in sintering 3h, Sintering temperature is 1000 DEG C, and reducing atmosphere 5%H2+95%Ar obtains rodlike long after glow luminous material；
Step 5, by the rodlike Sr obtained by 1g steps 42MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, in Ultrasound Instrument Middle ultrasonic 6 minutes, ultrasound was filtered after the completion, was placed in baking oven at 110 DEG C 18 minutes dry；
Step 6, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution, wherein H2PtCl6Molar concentration be 0.03mmol L-1；
Step 7, by step 6 gained H2PtCl6Solution, acetic acid and alcohol are according to 2:2:500 are mixed to form homogeneous solution；
Step 8, the luminescent powder that step 5 obtains is added in the 15ml solution obtained by step 7 and is stirred 15 minutes, is subsequently placed in In Ultrasound Instrument, ultrasonic photo-reduction 2.5 hours is carried out under ultra violet lamp；
Step 9, step 8 acquired solution is filtered, ethanol wash is used in combination 2 times, be placed in baking oven at 120 DEG C dry 15 minutes to get to the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.
Embodiment 3
Step 1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, be then configured to The solution of 0.02mol/L；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water and is made The solution of 0.02mol/L；
Step 3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measures step 1 And the solution in step 2 and tetraethyl orthosilicate, it is stirred at room temperature for 24 hours, urea is added and is used as precipitating reagent, it is ultrasonic half small When；
Step 4, the solution of gained above is poured into the liner of reaction kettle, 70h is reacted at 210 DEG C, is then used respectively Water and absolute ethyl alcohol carry out washing 4 times, and dry 2.5h obtains presoma at 100 DEG C in an oven, is being sintered in a reducing atmosphere 4h, sintering temperature are 1100 DEG C, and reducing atmosphere 5%H2+95%Ar obtains rodlike long after glow luminous material；
Step 5, by the rodlike Sr obtained by 1g steps 42MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, in Ultrasound Instrument Middle ultrasonic 7 minutes, ultrasound was filtered after the completion, was placed in baking oven at 130 DEG C 15 minutes dry；
Step 6, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution, wherein H2PtCl6Molar concentration be 0.06mmol L-1；
Step 7, by step 6 gained H2PtCl6Solution, acetic acid and alcohol are according to 1:2:500 are mixed to form homogeneous solution；
Step 8, the luminescent powder that step 5 obtains is added in the 12ml solution obtained by step 7 and is stirred 15 minutes, is subsequently placed in In Ultrasound Instrument, ultrasonic photo-reduction 2h is carried out under ultra violet lamp；
Step 9, step 8 acquired solution is filtered, ethanol wash is used in combination 3 times, be placed in baking oven at 120 DEG C dry 15 minutes to get to the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.
Embodiment 4
Step 1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, be then configured to The solution of 0.02mol/L；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water and is made The solution of 0.02mol/L；
Step 3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measures step 1 And the solution in step 2 and tetraethyl orthosilicate, it is stirred at room temperature for 24 hours, urea is added and is used as precipitating reagent, it is ultrasonic half small When；
Step 4, the solution of gained above is poured into the liner of reaction kettle, 60h is reacted at 220 DEG C, is then used respectively Water and absolute ethyl alcohol carry out washing 4 times, and dry 2h obtains presoma at 110 DEG C in an oven, in a reducing atmosphere in sintering 3h, Sintering temperature is 1100 DEG C, and reducing atmosphere 5%H2+95%Ar obtains rodlike long after glow luminous material；
Step 5, by the rodlike Sr obtained by 1g steps 42MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, in Ultrasound Instrument Middle ultrasonic 8 minutes, ultrasound was filtered after the completion, was placed in baking oven at 120 DEG C 15 minutes dry；
Step 6, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution, wherein H2PtCl6Molar concentration be 0.1mmol L-1；
Step 7, by step 6 gained H2PtCl6Solution, acetic acid and alcohol are according to 2:3:500 are mixed to form homogeneous solution；
Step 8, the luminescent powder that step 5 obtains is added in the 3ml solution obtained by step 7 and is stirred 20 minutes, is subsequently placed in In Ultrasound Instrument, ultrasonic photo-reduction 2h is carried out under ultra violet lamp；
Step 9, step 8 acquired solution is filtered, ethanol wash is used in combination 3 times, be placed in baking oven at 120 DEG C dry 15 minutes to get to the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.
Embodiment 5
Step 1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, be then configured to The solution of 0.02mol/L；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water and is made The solution of 0.02mol/L；
Step 3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measures step 1 And the solution in step 2 and tetraethyl orthosilicate, it is stirred at room temperature for 24 hours, urea is added and is used as precipitating reagent, it is ultrasonic half small When；
Step 4, the solution of gained above is poured into the liner of reaction kettle, 30h is reacted at 230 DEG C, is then used respectively Water and absolute ethyl alcohol carry out washing 4 times, and dry 2h obtains presoma at 110 DEG C in an oven, in a reducing atmosphere in sintering 3h, Sintering temperature is 1100 DEG C, and reducing atmosphere 5%H2+95%Ar obtains rodlike long after glow luminous material；
Step 5, by the rodlike Sr obtained by 1g steps 42MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, in Ultrasound Instrument Middle ultrasonic 10 minutes, ultrasound was filtered after the completion, was placed in baking oven at 150 DEG C 15 minutes dry；
Step 6, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution, wherein H2PtCl6Molar concentration be 0.15mmol L-1；
Step 7, by step 6 gained H2PtCl6Solution, acetic acid and alcohol are according to 8:3:500 are mixed to form homogeneous solution；
Step 8, the luminescent powder that step 5 obtains is added in the 6ml solution obtained by step 7 and is stirred 20 minutes, is subsequently placed in In Ultrasound Instrument, ultrasonic photo-reduction 3h is carried out under ultra violet lamp；
Step 9, step 8 acquired solution is filtered, ethanol wash is used in combination 3 times, be placed in baking oven at 150 DEG C dry 15 minutes to get to the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.
Embodiment 6
Step 1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, be then configured to The solution of 0.02mol/L；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water and is made The solution of 0.02mol/L；
Step 3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measures step 1 And the solution in step 2 and tetraethyl orthosilicate, it is stirred at room temperature for 24 hours, urea is added and is used as precipitating reagent, it is ultrasonic half small When；
Step 4, the solution of gained above is poured into the liner of reaction kettle, reacts at 240 DEG C for 24 hours, then uses respectively Water and absolute ethyl alcohol carry out washing 5 times, and dry 2h obtains presoma at 120 DEG C in an oven, in a reducing atmosphere in sintering 2h, Sintering temperature is 1200 DEG C, and reducing atmosphere 5%H2+95%Ar obtains rodlike long after glow luminous material；
Step 5, by the rodlike Sr obtained by 1g steps 42MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, in Ultrasound Instrument Middle ultrasonic 10 minutes, ultrasound was filtered after the completion, was placed in baking oven at 150 DEG C 15 minutes dry；
Step 6, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution, wherein H2PtCl6Molar concentration be 0.2mmol L-1；
Step 7, by step 6 gained H2PtCl6Solution, acetic acid and alcohol are according to 10:4:500 are mixed to form homogeneous solution；
Step 8, the luminescent powder that step 5 obtains is added in the 5ml solution obtained by step 7 and is stirred 20 minutes, is subsequently placed in In Ultrasound Instrument, ultrasonic photo-reduction 3h is carried out under ultra violet lamp；
Step 9, step 8 acquired solution is filtered, ethanol wash is used in combination 3 times, be placed in baking oven at 150 DEG C dry 15 minutes to get to the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.

Claims (6)

1. the rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+The preparation method of long after glow luminous material, which is characterized in that In rodlike Sr2MgSi2O7：Eu2+, Dy3+Material surface adsorbs one layer of H2PtCl6Solution is generated under the irradiation of ultraviolet light and is carried on Rodlike Sr2MgSi2O7：Eu2+, Dy3+Platinum grain, then wash away unreacted H with alcohol2PtCl6And the platinum that adsorption capacity is poor Grain, obtains the rodlike Sr of platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material.
2. the rodlike Sr of metal platinum area load according to claim 12MgSi2O7：Eu2+, Dy3+Long after glow luminous material Preparation method, which is characterized in that include the following steps：
Step 1, rodlike Sr is prepared2MgSi2O7：Eu2+, Dy3+Luminescent powder；
Step 2, by rodlike Sr2MgSi2O7：Eu2+, Dy3+Luminescent powder pours into alcohol, ultrasonic in Ultrasound Instrument, and ultrasound is completed laggard Row filtering is placed in baking oven dry；
Step 3, by H2PtCl6It is dissolved in deionized water and forms homogeneous solution；
Step 4, by gained H2PtCl6Solution, acetic acid and alcohol are mixed to form homogeneous solution；
Step 5, the luminescent powder that step 2 obtains is poured into the solution obtained by step 4 and is stirred, is subsequently placed in Ultrasound Instrument, in purple Ultrasonic photo-reduction is carried out under outer light irradiation；
Step 6, step 5 acquired solution is filtered, ethanol wash is used in combination, be placed in baking oven lower dry to get to metal platinum The rodlike Sr of area load2MgSi2O7：Eu2+, Dy3+Long-afterglow luminescent powder.
3. the rodlike Sr of metal platinum area load according to claim 22MgSi2O7：Eu2+, Dy3+Long after glow luminous material Preparation method, which is characterized in that Sr described in step 12MgSi2O7：Eu2+, Dy3+It is prepared using high temperature solid-state：
Step 1-1, respectively by Sr (NO3)2With Mg (NO3)2It is dissolved in deionized water, prepares the Sr (NO of 0.2mol/L3)2With Mg (the NO of 0.1mol/L3)2Solution；
Step 1-2, by Eu2O3Clear solution can be formed by being dissolved in stirring half an hour in concentrated nitric acid, and deionized water is then added and matches The solution of 0.02mol/L is made；By Dy2O3It is dissolved in concentrated nitric acid, stirring 12h forms clear solution, is eventually adding deionized water and is made The solution of 0.02mol/L；
Step 1-3, according to chemical expression Sr1.96MgSi2O7:0.02Eu2+,0.02Dy3+Required component ratio measure step 1 and Solution in step 2 and tetraethyl orthosilicate, are stirred at room temperature, and precipitating reagent, ultrasound is added；
The solution of gained above is poured into the liner of reaction kettle, 24-96h is reacted at 180-240 DEG C, is then divided by step 1-4 It is not washed with water and absolute ethyl alcohol, is dried to obtain presoma in an oven, obtain rodlike length in sintering in a reducing atmosphere Afterglow materials.
4. the rodlike Sr of metal platinum area load according to claim 22MgSi2O7：Eu2+, Dy3+Long after glow luminous material Preparation method, which is characterized in that H described in step 22PtCl6Molar concentration be 0.01-0.2mmol L-1。
5. the rodlike Sr of metal platinum area load according to claim 22MgSi2O7：Eu2+, Dy3+Long after glow luminous material Preparation method, which is characterized in that H described in step 42PtCl6The volume ratio of solution, acetic acid and alcohol is (1-10):(1-4): 500。
6. the rodlike Sr of metal platinum area load according to claim 22MgSi2O7：Eu2+, Dy3+Long after glow luminous material Preparation method, which is characterized in that the time of ultrasonic photo-reduction described in step 5 is 2-3 hours.
CN201810547107.6A 2018-05-31 2018-05-31 The rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material preparation method Pending CN108587603A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810547107.6A CN108587603A (en) 2018-05-31 2018-05-31 The rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810547107.6A CN108587603A (en) 2018-05-31 2018-05-31 The rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material preparation method

Publications (1)

Publication Number Publication Date
CN108587603A true CN108587603A (en) 2018-09-28

Family

ID=63629947

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810547107.6A Pending CN108587603A (en) 2018-05-31 2018-05-31 The rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material preparation method

Country Status (1)

Country Link
CN (1) CN108587603A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112662201A (en) * 2020-12-21 2021-04-16 江西善纳新材料科技有限公司 Preparation method of mica-based fluorescent pearlescent pigment
CN113262773A (en) * 2021-05-28 2021-08-17 杭州电子科技大学 Long afterglow light catalytic material rich in oxygen vacancy for photocatalysis of CO all day long2Application to reduction

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102373059B (en) * 2010-08-13 2013-10-02 海洋王照明科技股份有限公司 Silicate fluorescent material and manufacturing method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102373059B (en) * 2010-08-13 2013-10-02 海洋王照明科技股份有限公司 Silicate fluorescent material and manufacturing method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张浩然等，: ""亚微米Sr2MgSi2O7：Eu2+，Dy3+的水热共沉淀制备及发光性能研究"", 《发光学报》 *
洪祖培: "《化学魔术师-催化剂》", 31 January 1989, 上海教育出版社 *
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》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112662201A (en) * 2020-12-21 2021-04-16 江西善纳新材料科技有限公司 Preparation method of mica-based fluorescent pearlescent pigment
CN113262773A (en) * 2021-05-28 2021-08-17 杭州电子科技大学 Long afterglow light catalytic material rich in oxygen vacancy for photocatalysis of CO all day long2Application to reduction

Similar Documents

Publication Publication Date Title
Liu et al. A gC 3 N 4@ Au@ SrAl 2 O 4: Eu 2+, Dy 3+ composite as an efficient plasmonic photocatalyst for round-the-clock environmental purification and hydrogen evolution
CN108841375A (en) A method of improving aluminate long after glow luminous material luminescent properties
Guo et al. A potential red‐emitting phosphor BaGd2 (MoO4) 4: Eu3+ for near‐UV white LED
CN113637476B (en) Rare earth ion co-doped near infrared long afterglow luminescent nano material, preparation method and application thereof
CN108587603A (en) The rodlike Sr of metal platinum area load2MgSi2O7：Eu2+, Dy3+Long after glow luminous material preparation method
CN101298337B (en) Preparation of Y2O3: Eu3+ nanosphere powder
CN105062484A (en) Rare earth oxysulfide upconversion nanotube and preparation method thereof
CN101368101A (en) Process for producing LaPO4-LnPO4 core-shell structured fluorescence granular material
CN108559495A (en) A kind of preparation method of high luminescence energy aluminate long after glow luminous material
Zhang et al. CaAl2O4: Eu2+, Nd3+ anti-corrosive coating and its afterglow-Catalytic process
Hai et al. Ag nanoparticles significantly improve the slow decay brightness of SrAl 2 O 4: Eu 2+, Dy 3+ by the surface plasmon effect
CN108559489A (en) The Ca of surface modification2MgSi2O7：Eu2+, Dy3+Long after glow luminous material and preparation method
Liu et al. Deposition of GdVO4: Eu3+ nanoparticles on silica nanospheres by a simple sol–gel method
CN103204538A (en) Preparation method of porous ZnO and ZnO/Ag nanometer free-standing film
CN103013519A (en) Rare-earth luminescent nanoparticle and application of rare-earth luminescent nanoparticle in Fe<3+> detection
CN102827193B (en) Rare-earth complex nano luminescent material
CN102337116B (en) Metal nano particle-coated oxide core-shell luminescent material and preparation method thereof
Xia et al. Long-distance transfer of plasmonic hot electrons across the Au–Pt porous interface for the hydrogen evolution reaction
Zhong et al. Enhancement of emission intensity of Sr 2 Si 5 N 8: Eu 2+ red-emitting phosphor by localized surface plasmon resonance of Ag nanoparticles with different morphologies
CN101428854B (en) Process for producing calcium doped mesoporous zirconium oxide powder
CN108410454A (en) A method of improving aluminate long afterglow materials luminescent properties using platinum
CN108841376A (en) The method that Cu deposition improves blue aluminate long-afterglow material luminescent properties
CN107195462B (en) A kind of preparation method and applications of photosensitizer nanocomposite
CN108841380A (en) Metal silver surface loads M2MgSi2O7：Eu2+, Dy3+The preparation method of long after glow luminous material
JP5599942B2 (en) Yttrium oxide phosphor and method for producing the same

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20180928