CN106634999A - Square-piece-shaped dysprosium-doped bismoclite white-light fluorescent powder and preparation method thereof - Google Patents

Square-piece-shaped dysprosium-doped bismoclite white-light fluorescent powder and preparation method thereof Download PDF

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CN106634999A
CN106634999A CN201611262579.4A CN201611262579A CN106634999A CN 106634999 A CN106634999 A CN 106634999A CN 201611262579 A CN201611262579 A CN 201611262579A CN 106634999 A CN106634999 A CN 106634999A
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preparation
mixed slurry
added dropwise
white
dysprosium
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宁青菊
权博
董晨
石景俊
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7701—Chalogenides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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

Abstract

The invention discloses square-piece-shaped dysprosium-doped bismoclite white-light fluorescent powder and a preparation method thereof. The preparation method comprises the following steps: weighing the raw materials including Dy2O3 and Bi2O3 according to a stoichiometric ratio of a chemical formula BiOCl:xDy<3+>, wherein x is equal to 0.01-0.11; preparing mixed slurry from a precursor, adjusting the pH of the mixed slurry to be 3-6, transferring the mixed slurry into a polytetrafluoroethylene hydrothermal reactor liner, and filling a hydrothermal kettle with the mixed slurry in a filling ratio of 65%-80%, wherein the hydrothermal treatment temperature is 120-180 DEG C, and the hydrothermal treatment time is 6h-10h; and repeatedly washing the obtained hydrothermally treated product with distilled water until washing clear liquid is neutral, drying precipitates in a drying oven in air atmosphere of 60-80 DEG C, and finely grinding by virtue of a mortar, so as to obtain the square-piece-shaped dysprosium-doped bismoclite white-light fluorescent powder. An adopted hydrothermal synthesis method has the advantages that the synthesis temperature is low, conditions are mild, the oxygen content is low, defects are not obvious, the system is stable, the process is simple, and the like; and the method is an efficient luminescent material synthesis method. The fluorescent powder prepared by virtue of the preparation method can generate white light through compounding, has high light emitting efficiency and brightness and can be used as the fluorescent powder for a white-light LED.

Description

A kind of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor and preparation method thereof
Technical field
The present invention relates to fluorescent material and preparation method thereof, and in particular to a kind of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor And preparation method thereof.
Background technology
In recent years, the inorganic compound of trivalent lanthanide ion doping is in optoelectronic device, medical diagnosis, laser material and display Important application is obtained etc. various fields, especially Dy3+Due to can absorb ultraviolet light and can while launch 460～ The blue light of 500nm and the gold-tinted of 560～600nm, after being combined white light can be produced, and it is widely studied.This emission spectrum source In 5d-4f transition and 5d states easily by crystalline field ambient influnence, therefore can by adjust Dy3+The gold-tinted of doping fluorescent powder The white light of needs is obtained with the strength ratio of blue light.
BiOCl is a kind of wide bandgap semiconductor for belonging to V-VI-VII races, with PbFCl type tetragonal phase structures, due to only Special electronic structure and the characteristics of easily replaced by rare earth ion, BiOCl becomes effective luminous host.BiOCl battery material, The aspects such as photocatalysis, dyestuff and photoelectrochemicalcell cell have potential application.Recently, the Eu of report3+The BiOCl redness of doping is glimmering Light powder has the advantages that life-span length and high quantum efficiency, but Dy3+The hydro-thermal method of the BiOCl of doping is prepared and also not ground Study carefully.
Recently, C.Shivakumara et al. is reported with regard to Dy3+The Judde-Ofelt theory analysises of the BiOCl of doping, Solid phase synthesis are which employs, but existence condition requires strict particularly requirement with relatively higher synthesis temperature.
The content of the invention
The technical problem to be solved is to provide a kind of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor and its system Preparation Method, have that low synthesis temperature, mild condition, oxygen content be little using hydrothermal synthesis method, defect not substantially, stable system, work The advantages of skill is simple, is a kind of efficient luminescent material synthetic method, and the fluorescent material of the present invention produces white light by compound, lights Efficiency high, brightness is high, can be used as phosphor for white light LED.
To achieve these goals, the technical solution used in the present invention is that a kind of square piece shape dysprosium doped chlorine oxygen bismuth white light is glimmering The preparation method of light powder, comprises the following steps：
1) with Dy2O3And Bi2O3For raw material, according to chemical formula BiOCl：xDy3+Stoichiometric proportion carry out raw material and weigh, its Middle x=0.01～0.11；
2) load weighted raw material is put into beaker, concentrated hydrochloric acid is added dropwise in beaker, and be stirred continuously until former Material is completely dissolved to form solution A；
3) ammonia spirit is added dropwise in solution A, until when no longer producing white precipitate in solution, stopping being added dropwise, is hanged Turbid liquid B；
4) suspension B is carried out being filtrated to get sediment, removes the NH in sediment4After Cl, in 60 DEG C～80 DEG C air It is dried in baking oven under atmosphere, presoma is obtained after grinding；
5) presoma is added water and is made into mixed slurry, the pH for adjusting mixed slurry is adjusted to 3～6, is then transferred to poly- four In PVF water heating kettle liner, control water heating kettle packing ratio be 65%～80% after fill kettle tighten, hydrothermal temperature be 120 DEG C～ 180 DEG C, the hydro-thermal time is 6h～10h；
6) by step 5) obtain hydro-thermal after product distilled water cyclic washing, until washing clear liquid in neutrality, subsequently Sediment is dried in an oven under 60 DEG C～80 DEG C air atmospheres, and it is finely ground with mortar, obtain the fluorescent material of the present invention.
Step 2) in concentrated hydrochloric acid mass concentration be 37.5%.
Step 3) in the concentration of ammonia spirit be 28%, rate of addition is constantly stirred to be added dropwise over during dropwise addition Mix.
Step 4) in repeatedly washing carried out to sediment using distilled water remove NH4Cl, and use AgNO3Cleaning solution is carried out Inspection, it is ensured that do not contain NH after precipitation drying4Cl。
Step 5) in by be added dropwise concentration be 28% ammoniacal liquor and concentration for 0.5mol/L citric acid adjust mixed slurry PH value.
A kind of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor, its chemical formula is BiOCl：xDy3+, wherein x=0.01～ 0.11。
Compared with prior art, the present invention has following beneficial technique effect：The present invention provides one kind and prepares efficiently BiOCl:Dy3+The method of fluorescent material, i.e. hydrothermal synthesis method, the present invention has reaction temperature low, the morphology microstructure rule for obtaining, and is in Square piece shape, the square piece length of side is 300nm～500nm, and thickness is 20nm～30nm.Fluorescent material prepared by the method, excitation spectrum Wide ranges, the blue light of its emission spectrum main peak 476nm and the gold-tinted of 574nm, by compound white light is produced, and luminous efficiency is high, bright Degree is high, can be used as phosphor for white light LED.
Description of the drawings
Fig. 1 is the SEM figures that embodiment 3 prepares fluorescent material.
Fig. 2 is the XRD that embodiment 3 prepares fluorescent material.
Fig. 3 is the exciting light spectrogram that embodiment 2 prepares fluorescent material.
Fig. 4 is the launching light spectrogram that embodiment 2 prepares fluorescent material.
Specific embodiment
Presently in connection with specific embodiment, the present invention is further elaborated：
Embodiment 1：
1) according to chemical formula BiOCl：xDy3+Stoichiometric proportion weigh Bi respectively2O3And Dy2O3Burning is put into as raw material Cup, wherein x=0.05；The concentrated hydrochloric acid that concentration is 37.5% is added dropwise in beaker again, and is stirred continuously, until by raw material Till being just completely dissolved, solution A is formed；
2) ammonia spirit that concentration is 28% is added dropwise in solution A, it should be noted that the speed that ammoniacal liquor is added dropwise should not mistake Hurry up, constantly stir during dropwise addition, until when just no longer producing white precipitate in solution, stopping that ammoniacal liquor is added dropwise, hanged Turbid liquid B；
3) suspension B is carried out being filtrated to get sediment, then sediment is repeatedly washed, AgNO is used afterwards3To washing Wash liquid to test, it is ensured that do not contain NH after precipitation drying4Cl, is dried under 60 DEG C of air atmospheres in baking oven, obtains after grinding Presoma；
4) presoma is added water and is made into mixed slurry, be 0.5mol/L by ammoniacal liquor and concentration that dropwise addition concentration is 28% Citric acid, adjusts the pH of mixed slurry to 4, and in being transferred to polytetrafluoroethylene (PTFE) water heating kettle liner, the packing ratio for controlling water heating kettle is Fill kettle after 70% to tighten, hydro-thermal 8h at 120 DEG C；
5) by step 4) product distilled water cyclic washing after the hydro-thermal that obtained, until washing clear liquid is in neutrality, with The drying under 70 DEG C of air atmospheres in an oven afterwards, and it is finely ground with mortar, obtain required BiOCl:0.05Dy3+Fluorescent material.
Embodiment 2：
1) according to chemical formula BiOCl：xDy3+Stoichiometric proportion weigh Bi respectively2O3And Dy2O3Burning is put into as raw material Cup, wherein x=0.01；The concentrated hydrochloric acid that concentration is 37.5% is added dropwise in beaker again, and is stirred continuously, until by raw material Till being just completely dissolved, solution A is formed；
2) ammonia spirit that concentration is 28% is added dropwise in solution A, it should be noted that the speed that ammoniacal liquor is added dropwise should not mistake Hurry up, constantly stir during dropwise addition, until when just no longer producing white precipitate in solution, stopping that ammoniacal liquor is added dropwise, hanged Turbid liquid B；
3) suspension B is carried out being filtrated to get sediment, then sediment is repeatedly washed, AgNO is used afterwards3To washing Wash liquid to test, it is ensured that do not contain NH after precipitation drying4Cl, is dried under 70 DEG C of air atmospheres in baking oven, obtains after grinding Presoma；
4) presoma is added water and is made into mixed slurry, be 0.5mol/L by ammoniacal liquor and concentration that dropwise addition concentration is 28% Citric acid, adjusts the pH of mixed slurry to 6, and in being transferred to polytetrafluoroethylene (PTFE) water heating kettle liner, the packing ratio for controlling water heating kettle is Fill kettle after 65% to tighten, hydro-thermal 10h at 180 DEG C；
5) by step 4) product distilled water cyclic washing after the hydro-thermal that obtained, until washing clear liquid is in neutrality, with The drying under 60 DEG C of air atmospheres in an oven afterwards, and it is finely ground with mortar, obtain required BiOCl:0.01Dy3+Fluorescent material.
Fig. 3 is the excitation spectrum of the present embodiment, and under the detection of 574nm launching lights, the main excitation light wave of gained is a length of 389nm, excitation spectrum wide ranges.
Fig. 4 is the emission spectrum of the present embodiment, under the exciting of 389nm light, most strong emission peak for 476nm blue light and The gold-tinted of 574nm, by compound white light can be produced, and luminosity is high, can be used as a kind of phosphor for white light LED.
Embodiment 3：
1) according to chemical formula BiOCl：xDy3+Stoichiometric proportion weigh Bi respectively2O3And Dy2O3Burning is put into as raw material Cup, wherein x=0.09；The concentrated hydrochloric acid that concentration is 37.5% is added dropwise in beaker again, and is stirred continuously, until by raw material Till being just completely dissolved, solution A is formed；
2) ammonia spirit that concentration is 28% is added dropwise in solution A, it should be noted that the speed that ammoniacal liquor is added dropwise should not mistake Hurry up, constantly stir during dropwise addition, until when just no longer producing white precipitate in solution, stopping that ammoniacal liquor is added dropwise, hanged Turbid liquid B；
3) suspension B is carried out being filtrated to get sediment, then sediment is repeatedly washed, AgNO is used afterwards3To washing Wash liquid to test, it is ensured that do not contain NH after precipitation drying4Cl, is dried under 70 DEG C of air atmospheres in baking oven, obtains after grinding Presoma；
4) presoma is added water and is made into mixed slurry, be 0.5mol/L by ammoniacal liquor and concentration that dropwise addition concentration is 28% Citric acid, adjusts the pH of mixed slurry to 4, and in being transferred to polytetrafluoroethylene (PTFE) water heating kettle liner, the packing ratio for controlling water heating kettle is Fill kettle after 70% to tighten, hydro-thermal 8h at 120 DEG C；
5) by step 4) product distilled water cyclic washing after the hydro-thermal that obtained, until washing clear liquid is in neutrality, with The drying under 70 DEG C of air atmospheres in an oven afterwards, and it is finely ground with mortar, obtain required BiOCl:0.09Dy3+Fluorescent material.
Fig. 1 is the SEM figures of the present embodiment, and using the ESEM of Hitachi-S4800, electron accelerating voltage is 3kV, work Distance is 8.5mm, and multiplication factor is 30,000 times.Surveyed sample topography morphology microstructure rule, in square piece shape, the square piece length of side is 300nm ～500nm, thickness is 20nm～30nm.
Fig. 2 is the XRD of the present embodiment, and abscissa is 2 θ values, and ordinate is relative intensity value, and its diffracting spectrum is corresponded to The thing phase collection of illustrative plates of BiOCl (JCPDS No.02-0429), good crystallinity, thing phase purity is high.
Embodiment 4：
1) according to chemical formula BiOCl：xDy3+Stoichiometric proportion weigh Bi respectively2O3And Dy2O3Burning is put into as raw material Cup, wherein x=0.11；The concentrated hydrochloric acid that concentration is 37.5% is added dropwise in beaker again, and is stirred continuously, until by raw material Till being just completely dissolved, solution A is formed；
2) ammonia spirit that concentration is 28% is added dropwise in solution A, it should be noted that the speed that ammoniacal liquor is added dropwise should not mistake Hurry up, constantly stir during dropwise addition, until when just no longer producing white precipitate in solution, stopping that ammoniacal liquor is added dropwise, hanged Turbid liquid B；
3) suspension B is carried out being filtrated to get sediment, then sediment is repeatedly washed, AgNO is used afterwards3To washing Wash liquid to test, it is ensured that do not contain NH after precipitation drying4Cl, is dried under 80 DEG C of air atmospheres in baking oven, obtains after grinding Presoma；
4) presoma is added water and is made into mixed slurry, be 0.5mol/L by ammoniacal liquor and concentration that dropwise addition concentration is 28% Citric acid, adjusts the pH of mixed slurry to 3, and in being transferred to polytetrafluoroethylene (PTFE) water heating kettle liner, the packing ratio for controlling water heating kettle is Fill kettle after 80% to tighten, hydro-thermal 6h at 150 DEG C；
5) by step 4) product distilled water cyclic washing after the hydro-thermal that obtained, until washing clear liquid is in neutrality, with The drying under 80 DEG C of air atmospheres in an oven afterwards, and it is finely ground with mortar, obtain required BiOCl:0.11Dy3+Fluorescent material.

Claims (6)

1. a kind of preparation method of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor, it is characterised in that comprise the following steps：
1) with Dy2O3And Bi2O3For raw material, according to chemical formula BiOCl：xDy3+Stoichiometric proportion carry out raw material and weigh, wherein x =0.01～0.11；
2) load weighted raw material is put into beaker, concentrated hydrochloric acid is added dropwise in beaker, and be stirred continuously until raw material is complete CL forms solution A；
3) ammonia spirit is added dropwise in solution A, until when no longer producing white precipitate in solution, stopping being added dropwise, obtains suspension B；
4) suspension B is carried out being filtrated to get sediment, removes the NH in sediment4After Cl, under 60 DEG C～80 DEG C air atmospheres It is dried in baking oven, presoma is obtained after grinding；
5) presoma is added water and is made into mixed slurry, the pH for adjusting mixed slurry is adjusted to 3～6, is then transferred to polytetrafluoroethyl-ne In alkene water heating kettle liner, control water heating kettle packing ratio be 65%～80% after fill kettle tighten, hydrothermal temperature be 120 DEG C～180 DEG C, the hydro-thermal time is 6h～10h；
6) by step 5) product distilled water cyclic washing after the hydro-thermal that obtains, until washing clear liquid is in neutrality, subsequently will be heavy Starch is dried in an oven under 60 DEG C～80 DEG C air atmospheres, and finely ground with mortar, obtains the fluorescent material of the present invention.
2. a kind of preparation method of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor according to claim 1, its feature exists In step 2) in concentrated hydrochloric acid mass concentration be 37.5%.
3. a kind of preparation method of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor according to claim 1, its feature exists In step 3) in the concentration of ammonia spirit be 28%, rate of addition is stirred continuously to be added dropwise over during dropwise addition.
4. a kind of preparation method of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor according to claim 1, its feature exists In step 4) in repeatedly washing carried out to sediment using distilled water remove NH4Cl, and use AgNO3Cleaning solution is tested, Ensure not containing NH after precipitation drying4Cl。
5. a kind of preparation method of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor according to claim 1, its feature exists In step 5) in by be added dropwise concentration be 28% ammoniacal liquor and concentration for 0.5mol/L citric acid adjust mixed slurry pH Value.
6. a kind of square piece shape dysprosium doped chlorine oxygen bismuth white emitting phosphor, it is characterised in that its chemical formula is BiOCl：xDy3+, wherein x =0.01～0.11.
CN201611262579.4A 2016-12-30 2016-12-30 Square-piece-shaped dysprosium-doped bismoclite white-light fluorescent powder and preparation method thereof Pending CN106634999A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108735873A (en) * 2018-04-25 2018-11-02 广州市欧玛灯光设备有限公司 A kind of LED light emitting sources preparation process
CN115246653A (en) * 2022-07-12 2022-10-28 中南大学 Nanometer dysprosium oxide and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
JPH06128564A (en) * 1992-10-14 1994-05-10 Fuji Photo Film Co Ltd Bismuth oxyhalide phosphor and radiation-sensitized screen
CN1513943A (en) * 2003-07-02 2004-07-21 中国科学院上海硅酸盐研究所 Preparation method of nano-level yttrium oxide base luminous powder doped with rare earth
CN103421511A (en) * 2013-08-30 2013-12-04 昆明理工大学 Bismuth oxyhalide light-emitting material with doped rare earth ions and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JPH06128564A (en) * 1992-10-14 1994-05-10 Fuji Photo Film Co Ltd Bismuth oxyhalide phosphor and radiation-sensitized screen
CN1513943A (en) * 2003-07-02 2004-07-21 中国科学院上海硅酸盐研究所 Preparation method of nano-level yttrium oxide base luminous powder doped with rare earth
CN103421511A (en) * 2013-08-30 2013-12-04 昆明理工大学 Bismuth oxyhalide light-emitting material with doped rare earth ions and preparation method thereof

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邝庆亮,等: "近紫外激发BiOCl∶Dy3+白光LED荧光粉的制备及发光性能研究", 《光谱学与光谱分析》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108735873A (en) * 2018-04-25 2018-11-02 广州市欧玛灯光设备有限公司 A kind of LED light emitting sources preparation process
CN115246653A (en) * 2022-07-12 2022-10-28 中南大学 Nanometer dysprosium oxide and preparation method and application thereof
CN115246653B (en) * 2022-07-12 2023-10-17 中南大学 Nanometer dysprosium oxide and preparation method and application thereof

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Application publication date: 20170510