CN111892929B - X-ray activated ultra-long ultraviolet long-afterglow luminescent material and preparation method and application thereof - Google Patents
X-ray activated ultra-long ultraviolet long-afterglow luminescent material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to an X-ray activated ultra-long ultraviolet long-afterglow luminescent material and a preparation method and application thereof. The chemical composition of the ultralong ultraviolet long afterglow luminescent material is La1‑xBixGa1‑ySbyO3Wherein, 0<x is less than or equal to 0.02, and y is less than or equal to 0.01. The invention provides an X-ray activated ultra-long ultraviolet long afterglow luminescent material which is prepared from LaGaO3As a matrix, doped with ions Bi3+Co-doping of Sb for ion activation3+The afterglow performance is optimized; the obtained ultraviolet long-afterglow luminescent material can be effectively excited by X-rays to generate afterglow emission at 372nm, the afterglow time is as long as 2000 hours, and the ultraviolet long-afterglow luminescent material is expected to generate a great driving force in the research and application fields of ultraviolet afterglow materials.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to an X-ray activated ultra-long ultraviolet long-afterglow luminescent material and a preparation method and application thereof.
Background
A long persistence material is a material that can still observe persistent luminescence after being excited by an external excitation source (e.g., X-ray excitation, ultraviolet light excitation, visible light excitation, electron beam excitation, etc.) for a period of time, and the persistent luminescence in different materials varies from a few seconds to several weeks. So far, long-afterglow luminescent materials have been widely used in many fields such as security display, instrument and meter display, biological diagnosis and treatment, and information encryption.
The research on the long-afterglow luminescent materials at the present stage mainly focuses on the long-afterglow luminescent materials in visible and near-infrared bands, such as: green long afterglow SrAl2O4:Eu2+,Dy3+Application in fields of emergency lighting, night display and the like, near-infrared afterglow ZnGa2O4:Cr3+In the fields of bioimaging, biosensors, and the like. However, the band lies at 200-4 with respect to the emission bandThe ultraviolet long-afterglow luminescent material between 00nm has less reports and applications, the related research is slow in progress, but the ultraviolet long-afterglow luminescent material can continuously generate light with higher energy, can realize the applications of photocatalysis, disinfection and sterilization, medical photodynamic therapy and the like under the condition of 'excitation-free', and has important practical value and application prospect. For example, CN110028967A discloses a garnet-based ultraviolet long-afterglow luminescent material, the ultraviolet afterglow time of which is more than 1 h.
In addition, since it is required that the excitation light source has a high penetration ability in applications such as biological environments (e.g., human tissues) and catalytic environments (e.g., aqueous media), low-power X-rays are widely used as the excitation light source for the uv-afterglow luminescent material due to their extremely high penetration ability and weak radiation damage, and Cs has been reported in recent years2NaYF6:Pr、LaPO4Pr and other X-ray activated ultraviolet afterglow materials, but materials with high-efficiency ultraviolet afterglow performance are still lacked, thereby limiting the practical application of the ultraviolet afterglow materials in the fields of catalysis, biomedicine and the like.
Therefore, the development of a material with high-efficiency ultraviolet afterglow performance has important research significance and application value.
Disclosure of Invention
The invention aims to overcome the shortage of materials with high-efficiency ultraviolet afterglow performance in the prior art and provides an X-ray activated ultra-long ultraviolet long afterglow luminescent material. The ultraviolet long-afterglow luminescent material provided by the invention can be effectively excited by X-rays to generate afterglow emission at 372nm, the afterglow time is as long as 2000 hours, and the ultraviolet long-afterglow luminescent material is expected to generate a great driving force in the research and application fields of ultraviolet afterglow materials.
The invention also aims to provide a preparation method of the X-ray activated ultra-long ultraviolet long afterglow luminescent material.
The invention also aims to provide application of the X-ray activated ultra-long ultraviolet long-afterglow luminescent material in the fields of safety display, instrument and meter display, biological diagnosis and treatment or information encryption.
In order to achieve the purpose, the invention adopts the following technical scheme:
an X-ray activated ultra-long ultraviolet long-afterglow luminescent material, the chemical composition of which is La1-xBixGa1-ySbyO3Wherein, 0<x≤0.02，0≤y≤0.01。
The invention provides an X-ray activated ultra-long ultraviolet long afterglow luminescent material which is prepared from LaGaO3As a matrix, doped with ions Bi3+Co-doping of Sb for ion activation3+The afterglow performance is optimized; the obtained ultraviolet long-afterglow luminescent material can be effectively excited by X-rays to generate afterglow emission at 372nm, and the afterglow time is as long as 2000 hours.
Preferably, 0.0005< x.ltoreq.0.02.
Preferably, 0.005. ltoreq. y.ltoreq.0.01.
More preferably, x is 0.001.
More preferably, y is 0.005.
Preferably, the afterglow time of the ultra-long ultraviolet long afterglow luminescent material is not less than 2000 hours.
The preparation method of the X-ray activated ultra-long ultraviolet long afterglow luminescent material comprises the following steps:
s1: grinding and uniformly mixing a La-containing compound, a Bi-containing compound, a Ga-containing compound and a Sb-containing compound to obtain a mixture;
s2: and (3) performing high-temperature pre-sintering and calcining treatment on the mixture to obtain the X-ray activated ultra-long ultraviolet long-afterglow luminescent material.
Preferably, the La-containing compound in S1 is La2O3(ii) a The compound containing Bi is Bi2O3(ii) a The Ga-containing compound is Ga2O3(ii) a The Sb-containing compound is Sb2O3。
Preferably, the milling process in S1 is milling in an ethanol solvent.
Preferably, the temperature of the high-temperature pre-sintering of S2 is 900-1000 ℃, and the time is 2-5 h.
Preferably, the calcining temperature of S2 is 1250-1350 ℃, and the time is 5-10 h.
Preferably, the calcining step of S2 further comprises the steps of cooling and grinding uniformly.
The application of the X-ray activated ultra-long ultraviolet long afterglow luminescent material in the fields of safety display, instrument and meter display, biological diagnosis and treatment or information encryption is also in the protection scope of the invention.
Preferably, the application of the X-ray activated ultra-long ultraviolet long afterglow luminescent material in the preparation of photoelectric devices.
Compared with the prior art, the invention has the following beneficial effects:
the ultraviolet long-afterglow luminescent material provided by the invention can be effectively excited by X-rays to generate afterglow emission at 372nm, the afterglow time is more than 2000 hours, and the ultraviolet long-afterglow luminescent material is expected to generate a great driving force in the research and application fields of ultraviolet afterglow materials.
The preparation method provided by the invention has the advantages of simple process, low synthesis cost and convenience for large-scale industrial production.
Drawings
FIG. 1 is an excitation emission spectrum of the ultraviolet long afterglow luminescent materials provided in examples 1, 2, 3 and 4;
FIG. 2 is a comparison of XRD spectra of materials provided in examples 1-7 with standard diffraction cards;
FIG. 3 is the steady state emission spectrum of the ultraviolet long afterglow luminescent materials provided by examples 2 and 5 under the excitation of an X ray source;
FIG. 4 is a comparison graph of the long-afterglow decay curves obtained after the ultraviolet long-afterglow luminescent materials provided by the embodiments 2 and 5 are irradiated by X-rays for 15 minutes, and the testing time is within 1000 seconds;
FIG. 5 is a long-afterglow decay curve obtained after the ultraviolet long-afterglow luminescent material provided in embodiment 5 is irradiated by X-rays for 15 minutes, wherein the testing time is within 100 hours;
FIG. 6 is an afterglow emission spectrum of the UV long afterglow luminescent material provided in example 5 at different time points with decay time within 2000 hours after 15 minutes of X-ray irradiation;
FIG. 7 is a comparison graph of the long-afterglow decay curves obtained after the ultraviolet long-afterglow luminescent materials provided by examples 3, 4, 6 and 7 are irradiated by X-rays for 15 minutes, and the test range is within 1000 seconds.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specific conditions noted in the examples below, generally according to conditions conventional in the art or as suggested by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Example 1
This example provides a long-afterglow UV-luminescent material La0.9995Bi0.0005GaO3(doping with Sb3+The amount of (b) is 0), and the preparation method thereof is as follows: according to the composition design of the materials, the matrix is LaGaO3Doping with ions Bi3+The doping amount of the lanthanum oxide (La) is 0.05 mol%, and the lanthanum oxide (La) is accurately weighed2O3) Gallium oxide (Ga)2O3) And bismuth oxide (Bi)2O3) Respectively weighing three compound raw materials according to the stoichiometric proportion of each component element, wherein the molar ratio of La to Ga to O to Bi is 0.9995 to 1 to 3 to 0.0005, and the corresponding product is LaGaO3:0.05％Bi3+。
The raw materials are put into an agate mortar, then a small amount of ethanol is added for grinding for about 1 hour, the raw materials are fully mixed and then are moved into a corundum crucible, and the raw materials are presintered for 5 hours at 900 ℃. And (3) regrinding the pre-sintered powder, then burning at 1350 ℃ for 10 hours again, naturally cooling to room temperature, taking out the sample, and grinding to obtain the afterglow luminescent sample.
Example 2
This example provides a long-afterglow UV-luminescent material La0.999Bi0.001GaO3(doping with Sb3+The amount of (b) is 0), and the preparation method thereof is as follows: according to the composition design of the materials, the matrix is LaGaO3Doping with ions Bi3+Amount of dopingThe lanthanum oxide (La) was accurately weighed at 0.1 mol%2O3) Gallium oxide (Ga)2O3) And bismuth oxide (Bi)2O3) Respectively weighing three compound raw materials according to the stoichiometric proportion of each component element, wherein the molar ratio of La to Ga to O to Bi is 0.999 to 1 to 3 to 0.001, and the corresponding product is LaGaO3:0.1％Bi3+。
The raw materials are put into an agate mortar, then a small amount of ethanol is added for grinding for about 1 hour, the raw materials are fully mixed and then are moved into a corundum crucible, and the raw materials are presintered for 5 hours at 1000 ℃. And (3) regrinding the pre-sintered powder, then burning at 1350 ℃ for 8 hours again, naturally cooling to room temperature, taking out the sample, and grinding to obtain the afterglow luminescent sample.
Example 3
This example provides a long-afterglow UV-luminescent material La0.99Bi0.01GaO3(doping with Sb3+The amount of (b) is 0), and the preparation method thereof is as follows: according to the composition design of the materials, the matrix is LaGaO3Doping with ions Bi3+The doping amount of the lanthanum oxide (La) is 1mol percent, and the lanthanum oxide (La) is accurately weighed2O3) Gallium oxide (Ga)2O3) And bismuth oxide (Bi)2O3) Respectively weighing three compound raw materials according to the stoichiometric proportion of each component element, wherein the molar ratio of La to Ga to O to Bi is 0.99 to 1 to 3 to 0.01, and the corresponding product is LaGaO3:1％Bi3+。
The raw materials are put into an agate mortar, then a small amount of ethanol is added for grinding for about 1 hour, the raw materials are fully mixed and then are moved into a corundum crucible, and the raw materials are presintered for 5 hours at 900 ℃. And (3) regrinding the pre-sintered powder, then burning at the high temperature of 1300 ℃ for 10 hours again, naturally cooling to room temperature, taking out the sample, and grinding to obtain the afterglow luminescent sample.
Example 4
This example provides a long-afterglow UV-luminescent material La0.98Bi0.02GaO3(doping with Sb3+The amount of (b) is 0), and the preparation method thereof is as follows: according to the composition design of the materials, the matrix is LaGaO3Doping with ions Bi3+The doping amount of the lanthanum oxide (La) is 2mol percent, and the lanthanum oxide (La) is accurately weighed2O3) Gallium oxide (Ga)2O3) And bismuth oxide (Bi)2O3) Respectively weighing three compound raw materials according to the stoichiometric proportion of each component element, wherein the molar ratio of La to Ga to O to Bi is 0.98 to 1 to 3 to 0.02, and the corresponding product is LaGaO3:2％Bi3+。
The raw materials are put into an agate mortar, then a small amount of ethanol is added for grinding for about 1 hour, the raw materials are fully mixed and then are moved into a corundum crucible, and the raw materials are presintered for 2 hours at 900 ℃. And (3) regrinding the pre-sintered powder, then burning at 1250 ℃ for 10 hours, naturally cooling to room temperature, taking out the sample, and grinding to obtain the afterglow luminescent sample.
Example 5
This example provides a long-afterglow UV-luminescent material La0.999Bi0.001Ga0.9995Sb0.0005O3The preparation method comprises the following steps: according to the composition design of the materials, the matrix is LaGaO3Doping with ions Bi3+The doping amount of (2) is 0.1 mol%, and Sb is codoped3+The amount of lanthanum oxide (La) was accurately weighed at 0.05 mol%2O3) Gallium oxide (Ga)2O3) Bismuth oxide (Bi)2O3) And antimony oxide (Sb)2O3) Respectively weighing four compound raw materials according to the stoichiometric proportion of each component element, wherein the molar ratio of La, Ga, O, Bi and Sb is 0.999:0.9995:3:0.001:0.0005, and the corresponding product is LaGaO3:0.1％Bi3+,0.05％Sb3+。
The raw materials are put into an agate mortar, then a small amount of ethanol is added for grinding for about 1 hour, the raw materials are fully mixed and then are moved into a corundum crucible, and the raw materials are presintered for 5 hours at 1000 ℃. And (3) regrinding the pre-sintered powder, then burning the powder at the high temperature of 1300 ℃ for 5 hours again, naturally cooling the powder to the room temperature, taking out the sample, and grinding the sample to obtain the afterglow luminescent sample.
Example 6
This example provides a long-afterglow UV-luminescent material La0.99Bi0.01Ga0.995Sb0.005O3The preparation method comprises the following steps: according to the composition design of the materials, the matrix is LaGaO3Doping with ions Bi3+Doped in an amount of 1 mol%, co-doping with Sb3+The amount of lanthanum oxide (La) was accurately weighed at 0.5 mol%2O3) Gallium oxide (Ga)2O3) Bismuth oxide (Bi)2O3) And antimony oxide (Sb)2O3) Respectively weighing four compound raw materials according to the stoichiometric proportion of each component element, wherein the molar ratio of La, Ga, O, Bi and Sb is 0.99:0.995:3:0.01:0.005, and the corresponding product is LaGaO3:1％Bi3+,0.5％Sb3+。
Placing the raw materials in an agate mortar, adding a small amount of ethanol, grinding for about 1 hour, fully mixing the raw materials, transferring the mixture to a corundum crucible, and presintering for 2 hours at 950 ℃. And (3) regrinding the pre-sintered powder, then burning for 5 hours at the high temperature of 1350 ℃, naturally cooling to the room temperature, taking out the sample, and grinding to obtain the afterglow luminescent sample.
Example 7
This example provides a long-afterglow UV-luminescent material La0.98Bi0.02Ga0.99Sb0.01O3The preparation method comprises the following steps: according to the composition design of the materials, the matrix is LaGaO3Doping with ions Bi3+The doping amount of (2%) co-doped with Sb3+The amount of lanthanum oxide (La) is 1 mol%, accurately weighing lanthanum oxide (La)2O3) Gallium oxide (Ga)2O3) Bismuth oxide (Bi)2O3) And antimony oxide (Sb)2O3) Respectively weighing four compound raw materials according to the stoichiometric proportion of each component element, wherein the molar ratio of La, Ga, O, Bi and Sb is 0.98, 0.99, 3, 0.02 and 0.01, and the corresponding product is LaGaO3:2％Bi3+,1％Sb3+。
The raw materials are put into an agate mortar, then a small amount of ethanol is added for grinding for about 1 hour, the raw materials are fully mixed and then are moved into a corundum crucible, and the raw materials are presintered for 2 hours at 1000 ℃. And (3) regrinding the pre-sintered powder, then burning at 1250 ℃ for 8 hours, naturally cooling to room temperature, taking out the sample, and grinding to obtain the afterglow luminescent sample.
Comparative example 1
This comparative example provides a material LaGaO not doped with Bi ions3The preparation method comprises the following steps: according to the composition design of the materials, lanthanum oxide (La) is accurately weighed2O3) And gallium oxide (Ga)2O3) Respectively weighing two compound raw materials according to the stoichiometric proportion of each component element, wherein the molar ratio of the elements is La, Ga and O is 1:1:3, and the corresponding product is LaGaO3。
The raw materials are put into an agate mortar, then a small amount of ethanol is added for grinding for about 1 hour, the raw materials are fully mixed and then are moved into a corundum crucible, and the raw materials are presintered for 5 hours at 1000 ℃. And (4) regrinding the pre-sintered powder, then burning the powder at the high temperature of 1300 ℃ for 10 hours again, naturally cooling the powder to the room temperature, taking out the sample, and grinding the sample to obtain a comparative sample.
Performance testing
The afterglow performance of the ultraviolet long afterglow luminescent materials provided in the examples and comparative example 1 were measured.
FIG. 1 shows the UV long-afterglow luminescent materials (samples) provided in examples 1-4 and the LaGaO material provided in comparative example 13The excitation emission spectrum of the sample is measured by a steady-state instant fluorescence spectrometer FLS1000 model Edinburgh, UK, and a xenon lamp of 500W is used as an excitation light source. It can be seen that all of the Bi-doped samples can emit uv light centered at 372nm under 306nm uv excitation, and the samples of the examples show similar emission peak shapes with only relative intensity difference. Among them, the sample provided in example 2 has the strongest relative intensity and the most excellent afterglow performance. In addition, comparative example 1 did not detect any fluorescence signal in this band.
FIG. 2 is an X-ray powder diffraction pattern of the samples provided in examples 1-7. The X-ray powder diffraction pattern and LaGaO of the doped sample provided in all examples are determined by an X-ray powder diffractometer of Bruker D8ADVANCE model3Standard card (ICSD 50388) was identical, indicating no other phases or impurities were introduced.
FIG. 3 is a steady state emission spectrum of the samples provided in examples 2 and 5 under X-ray excitation. The test was carried out using an Edinburgh FLS1000 model steady-state instant fluorescence spectrometer, Edinburgh, UK, with an X-ray light tube (mini-X X-ray, hereinafter the same type of X-ray source is used) from Amptek, the operating voltage and operating current of the X-ray excitation light source being set to 50kV and 79 μ A, respectively. As can be seen from comparison of FIG. 1, the samples provided in examples 2 and 5 (single-doped Bi and co-doped Sb/Bi samples) have identical emission peak shapes under X-ray and ultraviolet excitation, and the emission wavelengths are 372 nm. The ultraviolet long persistence luminescent materials provided in the other embodiments (examples 1, 3 to 4, 6 to 7) also have similar luminescence peak shapes.
FIG. 4 is a graph showing the UV long afterglow attenuation curves of the samples provided in examples 2 and 5, wherein the attenuation curve at 372nm is monitored after 15 minutes of X-ray source excitation (wherein the X-ray tube operating voltage and operating current are 50kV and 79 μ A, respectively), and the afterglow emission peak at 372nm is shown. The afterglow intensity of the sample provided by the example 2 is about 1/5 of the sample prepared in the example 5, and the co-doping of Sb further improves the afterglow intensity of the ultraviolet long afterglow luminescent material. The UV long persistence decay curves for the samples of examples 1 and 3-4 are similar to example 2; the UV long persistence decay curves for the samples provided in examples 6-7 are similar to those of example 5.
FIG. 5 is an afterglow decay curve obtained by continuously testing 100 hours after the sample provided in example 5 is excited by an X-ray source for 15 minutes, wherein the afterglow emission peak is located at 372nm and has the best afterglow performance, and the afterglow emission peak still has a signal-to-noise ratio of about 3 orders of magnitude after being attenuated for 100 hours. Wherein the X-ray tube operating voltage and operating current were 50kV and 79 mua, respectively, and the monitored afterglow emission wavelength was 372 nm.
FIG. 6 is the ultraviolet afterglow emission spectra of the sample provided in example 5 at different attenuation moments, and the afterglow emission spectra of the sample measured within 2000 hours after the X-ray excitation is stopped show that the afterglow emission peak is 372nm in the attenuation process, and the afterglow time exceeds 2000 hours. Wherein the X-ray tube operating voltage and current were 50kV and 79 mua, respectively, and the excitation time was 15 minutes.
FIG. 7 is an afterglow decay curve of the samples provided in examples 3, 4, 6 and 7, the afterglow emission peak being at 372 nm. Wherein, the afterglow performance of the sample provided by the embodiment 6 is better than that of the sample singly doped with Bi provided by the embodiment 3; the afterglow performance of the sample provided in example 7 is better than that of the sample singly doped with Bi prepared in example 4.
Furthermore, examples 5, 6 and 7 provide samples with similar structural and luminescent properties, with only relative intensity differences.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The X-ray activated ultra-long ultraviolet long-afterglow luminescent material is characterized in that the chemical composition of the ultra-long ultraviolet long-afterglow luminescent material is La1-xBixGa1-ySbyO3Wherein, 0<x≤0.02，0.005≤y≤0.01。
2. The X-ray activated ultra-long ultraviolet long persistence luminescent material of claim 1, wherein 0.0005< X ≦ 0.02.
3. The X-ray activated ultra-long ultraviolet long afterglow luminescent material of claim 1, wherein X is 0.001; y is 0.005.
4. The preparation method of the X-ray activated ultra-long ultraviolet long afterglow luminescent material as claimed in any one of claims 1 to 3, characterized by comprising the following steps:
s1: grinding and uniformly mixing a La-containing compound, a Bi-containing compound, a Ga-containing compound and a Sb-containing compound to obtain a mixture;
s2: and (3) performing high-temperature pre-sintering and calcining treatment on the mixture to obtain the X-ray activated ultra-long ultraviolet long-afterglow luminescent material.
5. The method according to claim 4, wherein the La-containing compound in S1 is La2O3(ii) a The compound containing Bi is Bi2O3(ii) a The Ga-containing compound is Ga2O3(ii) a The Sb-containing compound is Sb2O3。
6. The method according to claim 4, wherein the milling in S1 is performed in an ethanol solvent.
7. The preparation method according to claim 4, wherein the high-temperature pre-sintering temperature of S2 is 900-1000 ℃ and the time is 2-5 h.
8. The preparation method according to claim 4, wherein the calcining temperature of S2 is 1250-1350 ℃ and the time is 5-10 h.
9. The method of claim 4, wherein the step of cooling and grinding the calcined S2 to uniformity is further included.
10. The use of the X-ray activated ultra-long ultraviolet long afterglow luminescent material of any one of claims 1 to 3 in the preparation of safety display, instrument and meter display, biological diagnosis and treatment or information encryption products.
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