CN113913186A - A carbon dot-based room temperature phosphorescent composite material capable of stably emitting afterglow and its preparation method, application and use method - Google Patents
A carbon dot-based room temperature phosphorescent composite material capable of stably emitting afterglow and its preparation method, application and use method Download PDFInfo
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Abstract
本发明涉及新材料技术领域，特别是涉及一种能稳定发射出余辉的碳点基室温磷光复合材料及其制备方法、应用和使用方法，该碳点基室温磷光复合材料由Y(OH)xF3‑x前驱体和碳点基长余辉材料组成，使得碳点基长余辉材料发射出对应颜色的余辉，且具有性能稳定、不易淬灭的优点，该能稳定发射出余辉的碳点基室温磷光复合材料能在制造防伪产品、传感产品、信息加密产品、光电器件产品或生物成像产品中的应用。
The invention relates to the technical field of new materials, in particular to a carbon dot-based room temperature phosphorescent composite material capable of stably emitting afterglow and a preparation method, application and use method thereof. The carbon dot-based room temperature phosphorescent composite material is composed of Y(OH) x The composition of F3-x precursor and carbon dot-based long afterglow material makes the carbon dot-based long afterglow material emit the afterglow of the corresponding color, and has the advantages of stable performance and not easy to be quenched. The phosphorescent composite material can be used in the manufacture of anti-counterfeiting products, sensing products, information encryption products, optoelectronic device products or biological imaging products.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a carbon dot-based room-temperature phosphorescent composite material capable of stably emitting afterglow and a preparation method, application and a using method thereof.
Background
The carbon dots have the advantages of low preparation cost, simple preparation method, excellent physical and chemical properties and the like, can be used as long-afterglow materials, can overcome the problems of complex synthetic procedures, difficult passivation, high toxicity, high cost, low luminous efficiency and the like of the traditional afterglow materials such as semiconductor quantum dots, organic fluorescent molecules, rare earth-based fluorescent powder and the like, and are an ideal long-afterglow material.
The carbon dots have abundant functional groups on the surfaces, so the carbon dots are easy to modify and flexible to prepare, and in practical application, the carbon dot-based long afterglow material can realize multicolor luminescence, multimode luminescence and the like through design. Moreover, the designed carbon dot material also has strong adjustability. Compared with general fluorescence emission, the long afterglow can eliminate the influence of background scattered light, and has great application prospect in photoelectric devices, biosensing and information protection.
At present, most scholars have more intensive research on the characteristics, the luminescence mechanism and the application of the carbon dot-based long afterglow materials and make great progress, and more inorganic long afterglow materials such as molecular sieves, double layer hydroxides, silicon dioxide, urea, boric acid and the like are added into a large family of the carbon dot-based long afterglow materials. However, the carbon dot-based long afterglow material still has the defects as the afterglow material: (1) under the excitation of ultraviolet, only the blue light carbon dot-based long afterglow material and the green light carbon dot-based long afterglow material can emit corresponding blue light and green light, and other carbon dot-based long afterglow materials cannot emit corresponding color afterglow, so that carbon dot-based long afterglow materials of other colors cannot be fully used; (2) the current carbon dot-based long afterglow materials also have the problem of instability, which is easily photo-quenched in water or other solvents.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow, which can stably emit afterglow of corresponding colors and has the advantages of stable performance and difficult quenching.
The second purpose of the invention is to provide a preparation method of the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow.
The invention also aims to provide application of the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow.
The fourth purpose of the invention is to provide a method for using the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow.
One of the purposes of the invention is realized by the following technical scheme:
provides a carbon dot-based room temperature phosphorescent composite material which can stably emit afterglow and is prepared from Y (OH)xF3-x precursor and carbon point-based long afterglow material.
Y (OH) mentioned abovexThe F3-x precursor has a unique hexagonal pore structure, Y (OH)xThe F3-x precursor plays a role in limiting the nanometer space of the carbon-point-based long afterglow material, and concretely, Y (OH)xCovalent bonds (C-F) and hydrogen bonds formed by the interaction of the F3-x precursor and the surface of the carbon point-based long afterglow material create a rigid environment for a luminescence center, thereby forming a confinement effect, effectively inhibiting the loss of molecules of the carbon point-based long afterglow material due to rotation or vibration, preventing a non-radiation inactivation approach of the carbon point-based long afterglow material, enhancing the energy transfer of ISC (interference Signal light interference) and realizing that the carbon point-based long afterglow material can stably emit corresponding afterglow under ultraviolet excitation; because of the various carbon point-based long afterglow materials in Y (OH)xThe F3-x precursor can emit the afterglow corresponding to the precursor, so that various carbon dot-based long afterglow materials can be excitedPhosphorescence, for example, orange light carbon dot-based long afterglow material can be excited to give orange phosphorescence, yellow light carbon dot-based long afterglow material can also be excited to give yellow phosphorescence, green light carbon dot-based long afterglow material can also be excited to give green phosphorescence, etc.; and, since Y (OH)xThe covalent bond (C-F) and the hydrogen bond formed by the interaction of the F3-x precursor and the surface of the carbon point-based long afterglow material also improve the stability of the carbon point-based long afterglow material, so that the carbon point-based long afterglow material is more stable, cannot generate light quenching in water or other solvents, and improves the use stability of the carbon point-based long afterglow material.
In some embodiments, the carbon dot-based long persistence material is dispersed in the Y (OH)xF3-x precursor, wherein the carbon point-based long afterglow material is dispersed in the Y (OH)xIn the F3-x precursor, the carbon point-based long afterglow material is enabled to react with Y (OH)xThe F3-x precursor was fully accessible.
In some embodiments, the Y (OH)xThe weight ratio of the F3-x precursor to the carbon-point-based long afterglow material is 1: 1-2.
The carbon dot-based room-temperature phosphorescent composite material capable of stably emitting afterglow has the beneficial effects that:
(1) y (OH) of the present inventionxThe F3-x precursor has a unique hexagonal pore structure, Y (OH)xThe F3-x precursor plays a role in limiting the nanometer space of the carbon-point-based long afterglow material, and concretely, Y (OH)xThe covalent bond (C-F) and the hydrogen bond formed by the interaction of the F3-x precursor and the surface of the carbon point-based long afterglow material create a rigid environment for a luminescence center, thereby forming a confinement effect, effectively inhibiting the loss of molecules of the carbon point-based long afterglow material due to rotation or vibration, preventing a non-radiation inactivation approach of the carbon point-based long afterglow material, enhancing the energy transfer of ISC (interference-induced chemical ionization) and realizing that the carbon point-based long afterglow material can emit corresponding afterglow under ultraviolet excitation.
(2) The invention is characterized in that various carbon point based long afterglow materials are Y (OH)xThe F3-x precursor can emit afterglow corresponding to the precursor, so that various carbon-point-based long afterglow materials can be excited to emit phosphorescence, such as orange lightThe material can be excited to emit orange phosphorescence, the yellow light carbon dot-based long afterglow material can also be excited to emit yellow phosphorescence, and the green light carbon dot-based long afterglow material can also be excited to emit green phosphorescence.
(3) The invention is due to Y (OH)xThe covalent bond (C-F) and the hydrogen bond formed by the interaction of the F3-x precursor and the surface of the carbon point-based long afterglow material also improve the stability of the carbon point-based long afterglow material, so that the carbon point-based long afterglow material is more stable, cannot generate light quenching in water or other solvents, and improves the use stability of the carbon point-based long afterglow material.
The second purpose of the invention is realized by the following technical scheme:
the preparation method of the carbon dot-based room-temperature phosphorescent composite material capable of stably emitting afterglow comprises the following steps,
s1, adding the powdered carbon dot-based long afterglow material into Y (NO)3)3Adding a NaF solution into the solution after uniformly stirring, continuously and uniformly stirring, adding a sodium hydroxide solution, and uniformly mixing to obtain a mixed material liquid;
s2, heating the mixed feed liquid prepared in the S1 at 120-150 ℃ for a certain time to obtain white precipitate, centrifuging, washing and drying the white precipitate to obtain the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow.
In the preparation steps, the carbon dot-based long afterglow material is added into Y (NO)3)3Under the solution and NaF solution, the carbon point-based long afterglow material is dispersed in Y (OH) through mixing, heating and washingxF3-x precursor.
In some embodiments, the Y (NO)3)3The adding amount of the solution is 0.084 mmol/mL-0.1 mmol/mL, the adding amount of the NaF is 0.01 mmol/mL-0.02 mmol/mLML, and the adding amount of the sodium hydroxide solution is 0.07 mmol/mL-0.09 mmol/mL.
In some embodiments, in S2, the heating time is 10h to 20 h.
In some embodiments, in S2, the white precipitate is centrifuged, washed no less than 1 time. The washing times are increased, and impurities can be effectively cleaned.
In some embodiments, the drying temperature in S2 is 50 ℃ to 70 ℃.
The preparation method of the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow has the beneficial effects that:
(1) the preparation method of the invention adds the carbon dot-based long afterglow material into Y (NO)3)3Under the solution and NaF solution, the carbon point-based long afterglow material is dispersed in Y (OH) through mixing, heating and washingxF3-x precursor.
(2) The preparation method can prepare the compound of Y (OH)xThe composite material composed of the F3-x precursor and the carbon dot-based long afterglow material has the advantage of easy operation and is suitable for large-scale production and application.
The invention also provides application of the carbon point-based room temperature phosphorescent composite material capable of stably emitting afterglow, and the application of the carbon point-based room temperature phosphorescent composite material capable of stably emitting afterglow in manufacturing anti-counterfeiting products, sensing products, information encryption products, photoelectric device products or biological imaging products.
The invention also provides a use method of the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow, which comprises the steps of irradiating the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow with ultraviolet laser, and removing the ultraviolet laser to ensure that the carbon-point-based room-temperature phosphorescent composite material emits afterglow.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be derived on the basis of the following drawings without inventive effort.
FIG. 1 is a transmission electron microscope image of the green carbon dot-based long afterglow phosphor (CDs-g), the yellow carbon dot-based long afterglow phosphor (CDs-y) and the orange carbon dot-based long afterglow phosphor (CDs-o) prepared in examples 1 to 3, respectively, and the corresponding particle size distribution maps thereof.
FIG. 2 is a diagram showing the UV-VIS absorption spectrum, the optimum excitation spectrum, the optimum emission spectrum and the phosphorus spectrum corresponding to CDs-g, CDs-y and CDs-o obtained in examples 1 to 3, respectively.
FIG. 3 shows Y (OH) in example 4xSEM image of F3-x.
FIG. 4 shows (a) Y (OH) obtained in examples 1 to 3xF3-x precursor composite green light carbon dot base long afterglow material (Y (OH) xF3-x @ CDs-g), (b) Y (OH)xF3-x precursor composite yellow light carbon dot base long afterglow material (Y (OH) xF3-x @ CDs-y), (c) Y (OH)xThe normalized phosphorescence emission spectra respectively corresponding to the F3-x precursor composite orange light carbon dot-based long afterglow material Y (OH) xF3-x @ CDs-o and the optimal excitation wavelengths respectively corresponding to the normalized phosphorescence emission spectra are 360nm, 376nm and 370 nm.
FIG. 5 is a graph of afterglow of (a) Y (OH) xF3-x @ CDs-g, (b) Y (OH) xF3-x @ CDs-y, and (c) Y (OH) xF3-x @ CDs-o obtained in examples 1-3, before and after the UV lamp at 365nm was turned off.
FIG. 6 is an afterglow image of (a) Y (OH) xF3-x @ CDs-g, (b) Y (OH) xF3-x @ CDs-y, and (c) Y (OH) xF3-x @ CDs-o prepared in examples 1 to 3 immersed in sodium hydroxide, acetic acid, absolute ethanol, water, DMF, DMSO, and aqueous solutions of various pH, respectively, before and after the 365nm UV lamp was turned off.
FIG. 7 shows that (a) Y (OH) xF3-x @ CDs-g, (b) Y (OH) xF3-x @ CDs-y and (c) Y (OH) xF3-x @ CDs-o obtained in example 5 in examples 1 to 4 are applied to security encrypted images under severe environmental conditions.
Detailed Description
The invention is further described with reference to the following examples and the accompanying drawings.
For convenience of describing the performance of the carbon dot-based room temperature phosphorescent composite material, the green light carbon dot-based long afterglow material, the yellow light carbon dot-based long afterglow material and the orange light carbon dot-based long afterglow material are respectively taken as examples to illustrate the performance of the carbon dot-based room temperature phosphorescent composite material, and the carbon dot-based long afterglow material is not limited to the carbon dot-based long afterglow material with three afterglow in practical application and can be used as a raw material and is also suitable for carbon dot-based long afterglow materials with other colors.
Example 1
The true bookThe embodiment discloses a carbon dot-based room temperature phosphorescent composite material capable of stably emitting green afterglow, which is prepared from Y (OH)xF3-x precursor and green light carbon dot-based long afterglow material.
In this embodiment, the carbon dot-based long afterglow material is dispersed in the y (oh)xF3-x precursor.
In the present embodiment, the Y (OH)xThe weight ratio of the F3-x precursor to the carbon dot-based long afterglow material is 1:1.
The preparation method of the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow comprises the following steps,
s1, adding the green light carbon dot based long afterglow material into Y (NO)3)3Adding a NaF solution into the solution after uniformly stirring, continuously and uniformly stirring, adding a sodium hydroxide solution, and uniformly mixing to obtain a mixed material liquid;
s2, heating the mixed feed liquid prepared in the S1 at 120 ℃ for a certain time to obtain white precipitate, centrifuging, washing and drying the white precipitate to obtain the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting green afterglow.
In this example, the Y (NO)3)3The addition amount of the solution was 0.084mmol/mL, the addition amount of the NaF solution was 0.01mmol/mL, and the addition amount of the sodium hydroxide solution was 0.07 mmol/mL.
Specifically, the preparation method of the green carbon dot-based long afterglow material CDs-g comprises the following steps: citric acid (1.0507g) and ethylenediamine (335. mu.L) were dissolved in 10ml of deionized water. The mixture was then transferred to a polytetrafluoroethylene (teflon) -lined autoclave, 50mL, and heated at 150 f for 5 h. After the reaction is finished, the reactor is naturally cooled to room temperature. The product was brownish black, transparent, dialyzed, and then freeze-dried to obtain CDs-g.
Specifically, Y (OH)xThe preparation method of the F3-x precursor composite green light carbon dot based long afterglow material comprises the following steps: CDs-g (0.01mg/mL, 60. mu.L) was added to Y (NO)3)3(0.2M,12.64mL) solution, after vigorously stirring for 15min, a NaF (0.3M,12.64mL) solution was addedStirring was continued for 10min and finally sodium hydroxide (0.5M,4.74mL) was added. The mixture was stirred for another 10 minutes, then transferred to a stainless steel autoclave lined with Teflon (50mL), heated at 140 ℃ for 15 hours to give a white precipitate, then centrifuged, washed several times with deionized water, and dried at 60 ℃ overnight to give Y (OH)xF3-x precursor is compounded with green carbon dot-based long afterglow material.
Example 2
The embodiment discloses a carbon dot-based room temperature phosphorescent composite material capable of stably emitting green afterglow, which consists of Y (OH)xF3-x precursor and yellow light carbon point based long afterglow material.
In this embodiment, the carbon dot-based long afterglow material is dispersed in the y (oh)xF3-x precursor.
In the present embodiment, the Y (OH)xThe weight ratio of the F3-x precursor to the carbon dot-based long afterglow material is 1: 2.
The preparation method of the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow comprises the following steps,
s1, adding the yellow light carbon point-based long afterglow material into Y (NO)3)3Adding a NaF solution into the solution after uniformly stirring, continuously and uniformly stirring, adding a sodium hydroxide solution, and uniformly mixing to obtain a mixed material liquid;
s2, heating the mixed feed liquid prepared in the S1 at 150 ℃ for a certain time to obtain white precipitate, centrifuging, washing and drying the white precipitate to obtain the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow.
In this example, the Y (NO)3)3The addition amount of the solution is 0.1mmol/mL, the addition amount of the NaF solution is 0.02mmol/mL, and the addition amount of the sodium hydroxide solution is 0.09 mmol/mL.
Specifically, the preparation method of the yellow light carbon dot based long afterglow material CDs-g comprises the following steps: o-phenylenediamine (0.32442g) was added to 20mL of water and dissolved with stirring for 4 h. Subsequently, the mixed solution was transferred to a 50mL stainless steel autoclave lined with Teflon and reacted at 180 ℃ for 12 hours. After cooling to room temperature, the dark yellow solution was filtered through an S-3 microporous membrane. Finally, the solution was freeze-dried to obtain CDs-y powder.
Specifically, Y (OH)xThe preparation method of the F3-x precursor composite yellow light carbon dot-based long afterglow material comprises the following steps: CDs-Y (0.01mg/mL, 60. mu.L) was added to Y (NO)3)3(0.2M,12.64mL) solution, after vigorous stirring for 15min, a further NaF (0.3M,12.64mL) solution was added, stirring continued for 10min, and finally sodium hydroxide (0.5M,4.74mL) was added. The mixture was stirred for another 10 minutes, then transferred to a stainless steel autoclave lined with Teflon (50mL), heated at 140 ℃ for 15 hours to give a white precipitate, then centrifuged, washed several times with deionized water, and dried at 60 ℃ overnight to give Y (OH)xF3-x precursor composite yellow light carbon point-based long afterglow material.
Example 3
The embodiment discloses a carbon dot-based room temperature phosphorescent composite material capable of stably emitting green afterglow, which consists of Y (OH)xF3-x precursor and carbon point-based long afterglow material capable of emitting orange light.
In this embodiment, the carbon dot-based long afterglow material is dispersed in the y (oh)xF3-x precursor.
In the present embodiment, the Y (OH)xThe weight ratio of the F3-x precursor to the carbon dot-based long afterglow material is 1: 1.5.
The preparation method of the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow comprises the following steps,
s1, adding the orange light carbon dot-based long afterglow material into Y (NO)3)3Adding a NaF solution into the solution after uniformly stirring, continuously and uniformly stirring, adding a sodium hydroxide solution, and uniformly mixing to obtain a mixed material liquid;
s2, heating the mixed feed liquid prepared in the S1 at 130 ℃ for a certain time to obtain white precipitate, centrifuging, washing and drying the white precipitate to obtain the carbon-point-based room-temperature phosphorescent composite material capable of stably emitting afterglow.
In this example, the Y (NO)3)3Solutions ofThe addition amount of (2) is 0.9mmol/mL, the addition amount of the NaF solution is 0.15mmol/mL, and the addition amount of the sodium hydroxide solution is 0.08 mmol/mL.
Specifically, the preparation method of the orange light carbon dot-based long afterglow material CDs-g comprises the following steps: pyrene (2g, TCl, 98% purity) was in 160mL HNO3Nitrated to trinitropyrene in nitric acid, refluxed and stirred for 12h at 80 ℃, cooled to room temperature, diluted with 1L of deionized water, filtered by a 0.22 μm microporous filter, and washed with double distilled water for 4 times. Dispersing the filter cake (1, 3, 6-trinitropyrene) into a sodium hydroxide solution, and then carrying out ultrasonic treatment. The resulting suspension was transferred to a polytetrafluoroethylene (teflon) -lined autoclave and heated to 200 ℃ for 10 h. After cooling, the product was filtered in a dialysis bag and dialyzed for 2 days (retained molecular weight: 3500 Da). Finally freeze drying to obtain CDs-o powder
Specifically, Y (OH)xThe preparation method of the F3-x precursor composite orange light carbon dot-based long afterglow material comprises the following steps: CDs-o (0.01mg/mL, 60. mu.L) was added to Y (NO)3)3(0.2M,12.64mL) solution, after vigorous stirring for 15min, a further NaF (0.3M,12.64mL) solution was added, stirring continued for 10min, and finally sodium hydroxide (0.5M,4.74mL) was added. The mixture was stirred for another 10 minutes, then transferred to a stainless steel autoclave lined with Teflon (50mL), heated at 140 ℃ for 15 hours to give a white precipitate, then centrifuged, washed several times with deionized water, and dried at 60 ℃ overnight to give Y (OH)xF3-x precursor composite orange light carbon point-based long afterglow material.
Example 4
The embodiment discloses a preparation method of Y (OH) xF 3-x: add NaF (0.3M,12.64mL) in water to Y (NO)3)3(0.2M,12.64mL) solution under vigorous stirring then aqueous sodium hydroxide (0.5M,4.74mL) was added carefully. The mixture was stirred for an additional 10 minutes and then transferred to a teflon lined stainless steel autoclave (50mL) and heated at 140 ℃ for 15h, and the white precipitate was centrifuged and washed several times with deionized water and then dried overnight at 60 ℃ to produce y (oh) xF3-x powder.
Example 5
Y(OH)xF3-x precursor composite carbonThe point-based long afterglow material (Y (OH) xF3-x @ CDs) is used for encryption application in a severe environment, and the application method comprises the following steps:
1) y (OH) xF3-x @ CDs powder is prepared into a specific pattern, placed in air for 6 months, and the afterglow pattern after excitation is stopped can be captured by naked eyes or a mobile phone under the excitation of an ultraviolet lamp.
2) The fully ground Y (OH) xF3-x @ CDs white powder was prepared in the desired numerical pattern, and the remainder of the number "8" was then supplemented with the same Y (OH) xF3-x white powder, and the afterglow numerical pattern after cessation of excitation was likewise captured by the naked eye or cell phone under UV lamp excitation.
3) Prepared Y (OH) xF3-x @ CDs were coated with the letters "c", "o", "M", "e", "o", "n" on the surface of the quartz glass wafer and immersed in various environmental liquids prepared beforehand, including NaOH (2M), Acetic Acid (2M), DMF (AR, 99.5%), DMSO (AR, 99%), Ethanol (AR), H2O. Under uv lamp excitation, the afterglow letters after excitation had ceased were observed.
Performance detection
FIG. 1 is a transmission electron microscope image and a corresponding particle size distribution diagram of the green carbon dot-based long afterglow phosphors (CDs-g), the yellowish carbon dot-based long afterglow phosphors (CDs-y) and the orange carbon dot-based long afterglow phosphors (CDs-o) respectively prepared in examples 1 to 3, wherein it can be seen that the CDPMs contained therein show spherical particles having a uniform and good dispersibility, and the average particle sizes are respectively: 3.1nm, 3.6nm and 3.5nm, and the interplanar spacings are respectively 0.21nm, 0.23nm and 0.22 nm.
FIG. 2 is a diagram of the UV-visible absorption spectrum, the optimum excitation spectrum, the optimum emission spectrum and the phosphorescence spectrum corresponding to CDs-g, CDs-y and CDs-o respectively prepared in examples 1-3, wherein it can be seen that CDs-g, CDs-y and CDs-o have strong absorption in the UV and blue regions, and the emission peaks are respectively at 440nm, 570nm and 537 nm. Phosphorescence spectra indicate that they are carbon dots that do not have afterglow emission themselves.
FIG. 3 shows Y (OH) in example 4xSEM image of F3-x, from which it can be seen that the substance is porous and ellipsoidal and is uniformly distributed.
FIG. 4 shows (a) Y (OH) obtained in examples 1 to 3xF3-x precursor composite green light carbon dot base long afterglow material (Y (OH) xF3-x @ CDs-g), (b) Y (OH)xF3-x precursor composite yellow light carbon dot base long afterglow material (Y (OH) xF3-x @ CDs-y), (c) Y (OH)xThe F3-x precursor composite orange light carbon dot-based long afterglow material Y (OH) xF3-x @ CDs-o has normalized phosphorescence emission spectra, and the optimal excitation wavelengths corresponding to the three materials are 360nm, 376nm and 370nm respectively.
FIG. 5 is an afterglow plot of (a) Y (OH) xF3-x @ CDs-g, (b) Y (OH) xF3-x @ CDs-Y and (c) Y (OH) xF3-x @ CDs-o before and after the 365nm UV lamp is turned off, as shown in examples 1-3, wherein Y (OH) xF3-x @ CDs-g, Y (OH) xF3-x @ CDs-Y and Y (OH) xF3-x @ CDs-o all emit phosphorescence after the lamp 3s is turned off.
FIG. 6 shows afterglow images of (a) Y (OH) xF3-x @ CDs-g, (b) Y (OH) xF3-x @ CDs-y and (c) Y (OH) xF3-x @ CDs-o prepared in examples 1 to 3 after being immersed in aqueous solutions of sodium hydroxide, acetic acid, absolute ethanol, water, DMF, DMSO and different pH values and before and after the UV lamp is turned off at 365nm, and it can be seen that phosphorescence can still be emitted after treatment with corrosive solvents such as alkali and acid, and thus the composite material of the present invention has good stability.
FIG. 7 shows that (a) Y (OH) xF3-x @ CDs-g, (b) Y (OH) xF3-x @ CDs-y and (c) Y (OH) xF3-x @ CDs-o obtained in example 5 in examples 1 to 4 are applied to security encrypted images under severe environmental conditions, and it can be seen that images of samples under sunlight and after overlooking, front-looking and magnification after 365nm ultraviolet light excitation stops exhibit bright afterglow, so that Y (OH) xF3-x @ CDs can be applied to encryption in severe environments.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
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