CN116948644A - Preparation method of rare earth ion doped photochromic fluorescent powder - Google Patents
Preparation method of rare earth ion doped photochromic fluorescent powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 13
- 230000008859 change Effects 0.000 claims abstract description 21
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 8
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims abstract description 8
- 230000005284 excitation Effects 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000000694 effects Effects 0.000 claims description 15
- -1 rare earth ion Chemical class 0.000 claims description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 9
- 238000004020 luminiscence type Methods 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000004040 coloring Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 12
- 238000003860 storage Methods 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 description 8
- 238000000295 emission spectrum Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000005286 illumination Methods 0.000 description 4
- 230000000638 stimulation Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000001748 luminescence spectrum Methods 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
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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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
- C09K11/7769—Oxides
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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
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
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Abstract
The invention relates to the field of photochromic fluorescent powder, in particular to a preparation method of rare earth ion doped photochromic fluorescent powder, which comprises the following steps of 3 、La 2 O 3 、Nb 2 O 5 、Bi 2 O 3 、Yb 2 O 3 And Er 2 O 3 Grinding and uniformly mixing to obtain mixed powder A; sintering the mixed powder A at 1350 ℃ in air atmosphere for 6h, and grinding to obtain Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Photochromic fluorescent powder; ba (Ba) 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ The photochromic fluorescent powder can be changed from white to pink rapidly under the irradiation of a 365nm ultraviolet lamp, and correspondingly, the luminous intensity of the fluorescent powder is also reduced along with the progress of color change, so that the regulation and control of the double perovskite Ba through photochromism is realized 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Is a light emitting property of the light emitting device. Ba of the invention 2 LaNbO 6 ：Bi 3+ The photochromic material has excellent photochromic and luminous regulation performance under ultraviolet excitation. Has great application potential in the fields of optical switching, optical storage and the like.
Description
Technical Field
The invention relates to the field of photochromic fluorescent powder, in particular to a preparation method of rare earth ion doped photochromic fluorescent powder.
Background
Photochromic refers to a material that exhibits a change in optical properties upon stimulation with light of a particular wavelength, such that a change in color occurs. Among them, because of the advantages of the ease of handling and safety of the light field, the photochromic phenomenon induced by the light field has gained attention from many people. In particular, by overlapping the absorption spectrum and the luminescence spectrum, the luminescence regulation and control of lanthanide rare earth ions based on the photochromic phenomenon can be realized, and the method has wide application prospect in the fields of optical switches, information storage, anti-counterfeiting and the like.
Lead-free double perovskite halides have attracted extensive research interest in the fields of illumination, x-ray scintillators, photosensors, bioimaging, etc., due to photoluminescence quantum yield, extremely high light absorption coefficient, large defect tolerance, and extremely long carrier diffusion length. However, the relatively poor chemical and thermal stability of the halide double perovskite limits its practical application. In contrast, inorganic double perovskite oxides have not only excellent stability but also great structural variability, and are promising candidates in optics, magnetism, photovoltaics, and the like. In recent years, by changing the doping type, concentration, and the like of rare earth ions, researchers have achieved light emission regulation of inorganic double perovskite oxides, however, such regulation is not reversible and the process is complicated. Therefore, the light-emitting is regulated and controlled by the light field, which is a simpler method.
The invention develops a novel photochromic fluorescent powder through ion doping, and the fluorescent powder is irradiated by 365nm ultraviolet light, so that obvious color change effect can be generated in a short time, and Er is doped 2 O 3 As a luminescence center, the luminescence can be controlled by photochromism.
Disclosure of Invention
The invention provides a preparation method of rare earth ion doped photochromic fluorescent powder, which can generate obvious photochromic phenomenon by irradiation of 365nm ultraviolet light for 10s and can be recovered to a state before irradiation by heat treatment. After the fluorescent powder is irradiated, the color of the ceramic is changed from white to pink. By doping Er 2 O 3 Under 980nm laser stimulation, obvious green light is emitted, and the light emission can be regulated and controlled through the color change effect. Through multiplexing technologies such as color change and luminescence, the double perovskite oxide is hopeful to promote the application in the fields of optical switches, information storage, anti-counterfeiting and the like.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
a preparation method of rare earth ion doped photochromic fluorescent powder comprises the following steps:
s1: high purity BaCO 3 、La 2 O 3 、Nb 2 O 5 、Bi 2 O 3 、Yb 2 O 3 And Er 2 O 3 Grinding and uniformly mixing to obtain mixed powder A;
s2: placing the mixed powder A obtained in the step S1 into an air atmosphere at 1350 ℃ to sinter for 6h, naturally cooling to room temperature, and grinding to obtain Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Photochromic fluorescent powder;
s3: raw material BaCO 3 、La 2 O 3 、Nb 2 O 5 Weighing according to the stoichiometric ratio of 2:1:1, doping ions Bi 3+ (Bi 2 O 3 )、Yb 3+ (Yb 2 O 3 ) And Er 3+ (Er 2 O 3 ) The contents are 2mol%, 10mol% and 6mol% respectively in terms of mol%;
s4: coloring by irradiation with 365nm ultraviolet lamp for different time, changing fluorescent powder from white to pink, and realizing rare earth oxide Er based on color change effect 2 O 3 Is provided.
Further, diffuse reflectance spectra of the phosphor before and after 365nm illumination were measured by a spectrophotometer (U-4100) equipped with an integrating sphere, and emission spectra before and after discoloration were measured by a fluorescence spectrometer (F7000).
Further, after the sample is irradiated by a 365nm ultraviolet lamp, the color of the sample is changed, and at the moment, the luminescence intensity of the sample can be found to be reduced compared with that before the sample is changed in color through 980nm laser excitation, which indicates that the luminescence of the sample is regulated and controlled through photochromism.
Ba prepared by the invention 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ The photochromic fluorescent powder can generate obvious color change effect after being irradiated by an ultraviolet lamp of 365nm for about 10 seconds, can be recovered to an initial state by heat treatment from white to pink, has good reversibility, and shows Er under 980nm excitation 3+ Ions typically emit spectra. When the sample changes color from white to pink, energy transfer from absorption or luminescence center to color centerFor the reasons of (1), the luminous intensity of the sample is reduced and the regulation of the luminescence is realized.
The invention has the beneficial effects that:
1. photochromic effect: photochromic refers to a material that exhibits a change in optical properties upon stimulation with light of a particular wavelength, such that a change in color occurs. According to the technical scheme, 365nm ultraviolet light irradiates the fluorescent powder to enable the fluorescent powder to generate obvious color change from white to pink. This color change effect is typically associated with vacancy-defect induced color center formation or charge transfer by valence electron hopping in the chromophore, such that upon some external field stimulus, the absorption and emission spectra of the phosphor change. The photochromic effect has wide application prospect in the fields of optical switches, information storage, anti-counterfeiting and the like.
2. And (3) light emission regulation: er doped in fluorescent powder 2 O 3 As a luminescence center, it was able to emit a clear green light under 980nm laser stimulation. This is due to Er 3+ The ions absorb 980nm laser energy and emit green light through the transition process under a specific energy level structure. The color of the sample is changed by the photochromic effect, namely 365nm ultraviolet light irradiation, and the luminous intensity of the sample is reduced by energy transfer from the absorption or luminous center to the color center. The luminous regulation and control technology can be applied to the fields of optical devices, photoelectric sensors, biological imaging and the like, and provides a new thought and method for the design and preparation of the optical devices and the photoelectric devices.
3. Reversibility of heat treatment: in the technical scheme, after the fluorescent powder is irradiated, the color of the fluorescent powder is changed from white to pink. However, by the heat treatment, the phosphor can be restored to the state before irradiation, i.e., the color is restored to white. The reversibility of heat treatment makes the fluorescent powder more convenient and reliable in practical application. The reversibility of the heat treatment may be achieved due to the release of electrons from oxygen vacancies and a decrease in color center, so that the color of the phosphor may be reversed during heating.
4. High chemical and thermal stability: compared with lead-free double perovskite halide, the technical scheme adopts inorganic double perovskite oxide as a base material. The inorganic double perovskite oxide has better chemical stability and thermal stability. Chemical stability refers to the stability of a material in different environments (e.g., acid, base, solvent, etc.), while thermal stability refers to the stability of a material at high temperatures. The material with high chemical stability and thermal stability is used as the base material, so that the stability and durability of the fluorescent powder in practical application can be improved, and the application potential of the material in various fields is expanded.
5. The simple preparation method comprises the following steps: the preparation method provided by the technical scheme is relatively simple and convenient. First, the desired material (e.g., baCO 3 、La 2 O 3 、Nb 2 O 5 、Bi 2 O 3 、Yb 2 O 3 And Er 2 O 3 ) Grinding and uniformly mixing to obtain mixed powder A; then, the mixed powder A is sintered at high temperature to obtain Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Photochromic fluorescent powder. In the preparation process, the mole percentage of various materials, the sintering temperature and the sintering time are controlled to obtain the required fluorescent powder material. The simple preparation method has good adaptability to the large-scale production of the fluorescent powder, and is helpful for promoting the practical application of the technology.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a diagram of Ba described in example 1 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Diffuse reflection spectra of the fluorescent powder after the fluorescent powder is respectively irradiated for 0s and 10s in a 365nm ultraviolet lamp;
FIG. 2 is an implementationExample 2 description of Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ The fluorescent powder irradiates the emission spectrum after 0s and 10s respectively in an ultraviolet lamp with the wavelength of 365 nm;
FIGS. 3 and 4 show the Ba of example 3 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Photographs of the fluorescent powder before and after 10 seconds of irradiation of 365nm ultraviolet lamp.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A preparation method of rare earth ion doped photochromic fluorescent powder comprises the following specific steps:
s1: high purity BaCO 3 、La 2 O 3 、Nb 2 O 5 、Bi 2 O 3 、Yb 2 O 3 And Er 2 O 3 Grinding and uniformly mixing to obtain mixed powder A;
s2: placing the mixed powder A obtained in the step S1 into an air atmosphere at 1350 ℃ to sinter for 6h, naturally cooling to room temperature, and grinding to obtain Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Photochromic fluorescent powder;
s3: raw material BaCO 3 、La 2 O 3 、Nb 2 O 5 And Bi (Bi) 2 O 3 Weighing according to stoichiometric ratio (2:1:1), doping ion Bi 3+ (Bi 2 O 3 )、Yb 3+ (Yb 2 O 3 ) And Er 3+ (Er 2 O 3 ) The contents are 2mol%, 10mol% and 6mol% respectively in terms of mol%;
s4: coloring by irradiation with 365nm ultraviolet lamp for different time, the fluorescent powder is changed from white to pink, and is based onThe color change effect can realize rare earth oxide Er 2 O 3 Is provided.
Further, the transmission spectrum of the phosphor before and after 365nm illumination was measured by a spectrophotometer (U-4100) equipped with an integrating sphere, and the emission spectrum before and after discoloration was measured by a fluorescence spectrometer (F7000).
Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ The photochromic fluorescent powder can generate obvious color change effect after being irradiated by an ultraviolet lamp of 365nm for about 10 seconds, can be recovered to an initial state by heat treatment from white to pink, and shows Er under the excitation of laser of 980nm 3+ The typical emission spectrum of ions can realize the regulation and control of luminescence.
Example 1
As shown in FIG. 1, ba was measured by a spectrophotometer (U-4100) equipped with an integrating sphere 2 La NbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Diffuse reflection spectrum of fluorescent powder before and after illumination at 365nm for 10 s; ba is added to 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ After the fluorescent powder is irradiated by a 365nm ultraviolet lamp for 10 seconds, the diffuse reflection spectrum of the sample before and after color change is measured. It can be seen that the diffuse reflection spectrum of the fluorescent powder after the ultraviolet lamp induces the color change is reduced in the range of 400nm to 800nm compared with the diffuse reflection spectrum before the color change, which proves that 365nm can effectively induce Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Photochromic phenomenon of fluorescent powder.
Example 2
As shown in FIG. 2, under excitation of 980nm laser, ba before and after 365nm light is measured by a fluorescence spectrometer (F7000) 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ And the luminescence spectrum of the fluorescent powder.
The emission spectra before and after the color change are compared, the obvious contrast is presented, the luminous intensity is reduced, and the effect of changing the color can well realize the effect of changing the color on Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ And (3) regulating and controlling photoluminescence of the fluorescent powder.
Example 3
As shown in FIG. 3, ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ The fluorescent powder is irradiated for 10s by a 365nm ultraviolet lamp, and Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ The phosphor turns from white to pink. The invention uses the photochromic effect to treat the double perovskite oxide Ba 2 LaNbO 6 The light-emitting regulation and control of obvious and quick response is realized, and the application prospect of the double perovskite oxide in the fields of optical switches, information storage, anti-counterfeiting and the like is effectively promoted.
Ba obtained by the invention 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Fluorescent powder, wherein when the sintering temperature is 1350 ℃, the sintering time is 6 hours, and Er which can be regulated and controlled by photochromism is obtained 3+ Ion-emitting photochromic phosphor Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Fluorescent powder. Description of rare earth ion doped photochromic Ba 2 LaNb 6 The fluorescent powder has wide application prospect in the aspects of optical switches, optical storage, optical detectors and the like.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (3)
1. The preparation method of the rare earth ion doped photochromic fluorescent powder is characterized by comprising the following steps of:
s1: high purity BaCO 3 、La 2 O 3 、Nb 2 O 5 、Bi 2 O 3 、Yb 2 O 3 And Er 2 O 3 Grinding and uniformly mixing to obtain mixed powder A;
s2: placing the mixed powder A obtained in the step S1 into an air atmosphere at 1350 ℃ to sinter for 6h, naturally cooling to room temperature, and grinding to obtain Ba 2 LaNbO 6 ：Yb 3+ 、Er 3+ 、Bi 3+ Photochromic fluorescent powder;
s3: raw material BaCO 3 、La 2 O 3 、Nb 2 O 5 Weighing according to the stoichiometric ratio of 2:1:1, doping ions Bi 3+ (Bi 2 O 3 )、Yb 3+ (Yb 2 O 3 ) And Er 3+ (Er 2 O 3 ) The contents are 2mol%, 10mol% and 6mol% respectively in terms of mol%;
s4: coloring by irradiation with 365nm ultraviolet lamp for different time, changing fluorescent powder from white to pink, and realizing rare earth oxide Er based on color change effect 2 O 3 Is provided.
2. The method for preparing rare earth ion doped photochromic phosphor of claim 1 wherein the phosphor in step S4 can achieve significant coloration under short irradiation of 365nm ultraviolet lamp.
3. The method for preparing rare earth ion doped photochromic fluorescent powder according to claim 2, wherein in the step S4, after the fluorescent powder is irradiated by a 365nm ultraviolet lamp, the color of the fluorescent powder is changed, and at this time, the luminous intensity of the fluorescent powder can be found to be reduced compared with that before the color change by 980nm laser excitation, which means that the luminescence of the fluorescent powder is regulated and controlled by the photochromism.
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