CN112852403A - Ultraviolet photochromic nano system and preparation method and application thereof - Google Patents
Ultraviolet photochromic nano system and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an ultraviolet photochromic nano system and a preparation method and application thereof, wherein the preparation method comprises the following steps: adding molybdenum oxide into a mixed solvent of N-methyl pyrrolidone and water, and heating to obtain a mixed solution; carrying out centrifugal washing on the mixed solution to obtain an ultraviolet photochromic nano system; wherein the ultraviolet photochromic nano system comprises MoOxQuantum dots and the mixed solvent. According to the invention, molybdenum oxide is added into a mixed solvent of N-methylpyrrolidone and water, and the ultraviolet photochromic nano system is prepared by a hydrothermal method, so that the preparation method is simple, low in cost, fast and large-scale in production, complicated organic synthesis and purification steps are omitted, the prepared ultraviolet photochromic nano system has high sensitivity to ultraviolet light, short response time and stable cycle performance, and the color of the prepared ultraviolet photochromic nano system is increased after color changeThe plasma absorption is enhanced, the plasma regulation and control can be carried out, near infrared light can be absorbed, and the method has important significance in the fields of plasma regulation and control and energy consumption reduction.
Description
Technical Field
The invention relates to the technical field of information encryption and anti-counterfeiting, in particular to an ultraviolet photochromic nano system and a preparation method and application thereof.
Background
The phenomenon that the system color changes obviously under the action of an external excitation source is called color-changing property. In recent years, a large number of researchers are attracted by intelligent response type photoelectric materials with photoelectric properties changed remarkably under the action of external stimulation. Researchers at home and abroad successively develop a series of photochromic functional materials, and the materials are successfully applied to various optical and optoelectronic fields such as information display, safety anti-counterfeiting, information sensing, biological imaging and the like. The unique response property of the material opens up a new way for developing novel optical information storage and encryption and optical anti-counterfeiting technology.
At present, the conventional photochromic materials mostly focus on organic compound systems, such as ring-opening-ring-closing reaction, and inorganic substances combined with organic dyes to realize photochromic behavior through electron donors or acceptors. However, most photochromic molecules require complicated organic chemical synthesis and cumbersome purification processes, which make the regulation of photochromic behavior inefficient and difficult to be applied in a truly large-scale industrial manner.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide an ultraviolet photochromic nano system, a preparation method and an application thereof, aiming at solving the problems that the existing photochromic material needs complicated organic chemical synthesis and a fussy purification process, the regulation and control efficiency of photochromic behavior is low and the real large-scale industrial application is difficult.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of an ultraviolet photochromic nano system comprises the following steps:
adding molybdenum oxide into a mixed solvent of N-methyl pyrrolidone and water, and heating to obtain a mixed solution;
carrying out centrifugal washing on the mixed solution to obtain an ultraviolet photochromic nano system; wherein the ultraviolet light isThe photochromic nanosystem comprises MoOxQuantum dots and the mixed solvent.
The preparation method of the ultraviolet photochromic nano system comprises the steps of heating at the temperature of 60-180 ℃ for 0.5-42 h.
The preparation method of the ultraviolet photochromic nano system comprises the step of preparing molybdenum oxide, wherein the particle size of the molybdenum oxide is 1-300 nm.
The preparation method of the ultraviolet photochromic nano system comprises the step of mixing N-methyl pyrrolidone with water in a volume ratio of 1: 1.
The preparation method of the ultraviolet photochromic nano system comprises the step of preparing the MoOxThe particle size of the quantum dots is 2-5 nm.
The preparation method of the ultraviolet photochromic nano system comprises the step of carrying out centrifugal washing at a rotating speed of 2000-12000 rpm.
An ultraviolet photochromic nanosystem comprising: MoOxThe quantum dot-based organic light-emitting diode comprises quantum dots and a mixed solvent, wherein the mixed solvent is a mixed solvent of N-methylpyrrolidone and water.
The ultraviolet photochromic nano system is characterized in that the volume ratio of N-methyl pyrrolidone to water in the mixed solvent is 1: 1.
The ultraviolet photochromic nano system is characterized in that the MoOxThe particle size of the quantum dots is 2-5 nm.
The application of the ultraviolet photochromic nano system in the fields of information encryption and optical anti-counterfeiting.
Has the advantages that: according to the invention, molybdenum oxide is added into a mixed solvent of N-methylpyrrolidone and water, and the ultraviolet photochromic nano system is prepared by a hydrothermal method, so that the preparation method is simple, low in cost, fast and large-scale in production, and complicated organic synthesis and purification steps are omitted, the prepared ultraviolet photochromic nano system is high in ultraviolet sensitivity, short in response time and stable in cycle performance, plasma absorption is enhanced after the ultraviolet photochromic nano system is discolored, plasma regulation and near infrared light absorption can be carried out, and the method has important significance in the fields of plasma regulation and energy consumption reduction.
Drawings
FIG. 1 is a diagram of the UV absorption spectra of the UV photochromic nano-system prepared in example 1 of the present invention obtained by irradiating the system under UV light for different periods of time;
FIG. 2 is a spectrum detection chart of the UV photochromic nano-system prepared in example 1 of the present invention under UV irradiation;
FIG. 3 is a transmission electron microscope photograph of the UV photochromic nanosystem prepared in example 1 of the present invention.
Detailed Description
The invention provides an ultraviolet photochromic nano system and a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and advantages of the invention clearer and more clear. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Photochromic refers to a compound A which undergoes a photochemical reaction when irradiated by light with a certain wavelength to obtain a product B, wherein the colors of A and B (namely, the absorption of light) are obviously different. B is irradiated by another light or heated to restore the original form A. One important criterion for photochromism is its reversible chemical reaction.
As one of the important materials for advanced photon application, photochromic molecules have been applied to information confidentiality, optical information storage, anti-counterfeiting patterns, fluorescence imaging and intelligent lenses, and the research in this field focuses on preparing new photochromic materials and precisely regulating and controlling the photochromic behavior thereof so as to meet the requirements of different photoelectric applications. At present, the conventional photochromic materials mostly focus on organic compound systems, such as ring-opening-ring-closing reaction, and inorganic substances combined with organic dyes to realize photochromic behavior through electron donors or acceptors. However, most photochromic molecules require complicated organic chemical synthesis and cumbersome purification processes, which make the regulation of photochromic behavior inefficient and difficult to be applied in a truly large-scale industrial manner.
In order to solve the above technical problems, the present invention provides a method for preparing an ultraviolet photochromic nano system, specifically, a method for preparing an ultraviolet photochromic nano system, comprising the steps of:
s1, adding molybdenum oxide into a mixed solvent of N-methyl pyrrolidone and water, and heating to obtain a mixed solution.
The molybdenum oxide is a stacked layered structure, is connected by virtue of molybdenum-oxygen bonds in the transverse direction and is tightly combined; the bonding force between the longitudinal layers is weak van der waals force, and the force can be destroyed under high-energy external conditions and is stripped to form a layered 2D nano structure. The 2D nano structure can be further destroyed under more severe conditions of proper solvent matching, hydrothermal ultrasound and the like, the connected molybdenum-oxygen bond is opened, the size is further reduced to a few nanometers, and the molybdenum oxide quantum dot with the quantum confinement effect is formed. According to the above characteristics of molybdenum oxide, in this example, molybdenum oxide is added to a mixed solvent of N-methylpyrrolidone and water, and molybdenum oxide is peeled off under heating to obtain a mixed solution. In the whole reaction process, the mixed solvent of the N-methyl pyrrolidone and the water is used as a solvent and also used as a catalyst for reaction, the added molybdenum oxide is more easily stripped to form a nano structure under the intercalation action of hydrogen ions in the water, and the nano structure formed after stripping reacts with functional groups on the N-methyl pyrrolidone to serve as a ligand to stably disperse the molybdenum oxide nano structure.
Considering that the particle size of molybdenum oxide, the heating temperature and heating time during the reaction affect the stripping of molybdenum oxide and MoO formed by the reactionxThe size of the quantum dots further influences the photochromic property of the obtained ultraviolet photochromic nano system, the particle size of the molybdenum oxide used in the embodiment is 1-300 nm, the heating temperature during the reaction is 60-180 ℃, the heating time is 0.5-42 h, and the ultraviolet photochromic nano system obtained under the condition has better ultraviolet photochromic property. In the embodiment, the ultraviolet photochromic nano system is synthesized by a solvothermal one-pot method, the synthesis time is only several hours, the preparation method is simple, the cost is low, the preparation method is quick, large-scale production can be realized, and the method has important scientific and engineering significance for preparing a large amount of photochromic molecular materials.
Specifically, the mixed solvent of N-methyl pyrrolidone and water is mentioned in the foregoing steps as a solvent and a catalyst for the reaction in the reaction process, wherein the intercalation of hydrogen ions in water can accelerate the stripping of molybdenum oxide to form a nanostructure, and N-methyl pyrrolidone as a ligand can stably disperse the molybdenum oxide nanostructure, that is, the ratio of N-methyl pyrrolidone to water in the mixed solvent can affect the formation and stability of the molybdenum oxide nanostructure. In this embodiment, a mixed solution of N-methylpyrrolidone and water at a volume ratio of 1:1 is selected as a mixed solvent for the reaction, so that rapid stripping of molybdenum oxide and stable dispersion of the formed molybdenum oxide nanostructure are realized. In a specific embodiment, the mass of the molybdenum oxide is 0.01g to 0.3g, and the volumes of the N-methylpyrrolidone and the water in the mixed solvent are respectively 5 mL to 10 mL.
S2, carrying out centrifugal washing on the mixed solution to obtain an ultraviolet photochromic nano system; wherein the ultraviolet photochromic nano system comprises MoOxQuantum dots and the mixed solvent.
In consideration of the presence of some larger particles or unreacted components in the mixed solution obtained by the reaction, in this example, after the mixed solution is obtained, the mixed solution is subjected to centrifugal washing, and the centrifuged product is dissolved in the mixed solvent to obtain the ultraviolet photochromic system. Wherein the ultraviolet photochromic nano system comprises MoOxThe volume ratio of N-methyl pyrrolidone to water in the mixed solvent is 1:1, and the MoO isxThe particle size of the quantum dots is 2-5 nm. MoOxThe quantum dots exist in an oxidation state and a dispersion system in a mixed solvent of N-methylpyrrolidone and water, and MoO exists after ultraviolet irradiationxOxygen vacancies are formed and are agglomerated, and then a color change effect is generated after the agglomeration through plasma absorption, wherein the main peak value of the color change is 700-900 nm; agglomerated MoO when the UV light was stoppedxThe structure will slowly recover dispersion, the plasma absorption will begin to decrease, and the slow color will begin to recover, thereby achieving ultraviolet photochromism. Compared with molybdenum oxide quantum prepared by other methodsThe method has the characteristics that the system does not have illumination discoloration or can be quickly recovered after illumination discoloration, in the embodiment, because the mixed solvent of N-methyl pyrrolidone and water is used as the solvent and the catalyst for reaction, the prepared ultraviolet photochromic nano system has higher sensitivity to ultraviolet light, the response time to the ultraviolet light is less than one minute, and the system can be quickly recovered after illumination is finished.
The ultraviolet photochromic nano system provided by the embodiment of the invention can be quickly changed into blue-green from almost transparent color within seconds under ultraviolet light, can be changed into color under sunlight even within minutes in cloudy days, and can be recovered within hours (changed from blue to colorless) when placed under indoor illumination. At the same time, some external stimuli may accelerate their recovery process, such as temperature increase, increase of oxygen concentration or ultrasound operation. Compared with the existing preparation method, the preparation method in the embodiment is fast and can be used for mass production, and complicated organic synthesis and purification steps are omitted. The ultraviolet photochromic nano system can be synthesized by a solvothermal one-pot method, the synthesis time is only a few hours, and MoOxThe quantum dots can be stably dispersed in a liquid phase, and meanwhile, the ultraviolet photochromic nano system can be recycled for more than 10 times, so that the circulating performance is good, the repeatability is high, and a foundation is laid for the subsequent large-scale industrialization.
The invention also provides an ultraviolet photochromic nano system, which is prepared by adopting the preparation method of the ultraviolet photochromic nano system. The ultraviolet photochromic nano system comprises MoOxThe quantum dot-based organic light-emitting diode comprises quantum dots and a mixed solvent, wherein the mixed solvent is a mixed solvent of N-methyl pyrrolidone and water, the volume ratio of the N-methyl pyrrolidone to the water in the mixed solvent is 1:1, and the MoOxThe particle size of the quantum dots is 2-5 nm. The MoO in the ultraviolet photochromic nano system provided by the inventionxThe quantum dots exist in an oxidation state and a dispersion system in a mixed solvent of N-methylpyrrolidone and water, oxygen vacancies are formed and begin to agglomerate after ultraviolet irradiation, a color change effect is generated after plasma absorption after agglomeration, and the main peak value of color change is in the range of 700-900 nm; when the ultraviolet irradiation is finished, the clustersPoly MoOxThe structure will slowly recover dispersion, the plasma absorption will begin to decrease, and the slow color will begin to recover, thereby achieving ultraviolet photochromism. The ultraviolet photochromic nano system can be synthesized by a solvothermal one-pot method, the synthesis time is only a few hours, and MoOxThe quantum dots can be stably dispersed in a liquid phase, and simultaneously the ultraviolet photochromic nano system can be cycled for more than 10 times, and has good cycle performance and high repeatability
The invention also provides an application of the ultraviolet photochromic nano system in the fields of information encryption and optical anti-counterfeiting. In addition, the ultraviolet photochromic nano system provided by the invention can also be applied to modified buildings, for example, the glass surface of the modified building is used as intelligent glass, when sunlight is strong in the daytime, the ultraviolet photochromic nano system starts to absorb light with the wave band of 700-800 nm in the sunlight after changing color, the sunlight incidence and the heat transfer are effectively reduced, the energy consumption can be reduced, and the ultraviolet photochromic nano system can be quickly restored to be transparent so as to transmit the moonlight in the evening. Because the ultraviolet photochromic nano system changes color under ultraviolet light, the system can keep stable and can not change color under indoor illumination.
The invention is further illustrated by the following specific examples.
Example 1
(1) Preparing a mixed solvent from 8mL of N-methylpyrrolidone and 8mL of water;
(2) adding 0.1g of molybdenum oxide into the mixed solution, and heating at 80 ℃ for 15 hours to obtain a mixed solution;
(3) and (3) centrifuging and washing the mixed solution at 10000rpm, and dissolving a centrifuged product in a mixed solvent of N-methylpyrrolidone and water in a volume ratio of 1:1 to obtain the ultraviolet photochromic nano system.
As shown in fig. 1, the ultraviolet absorption spectrum is obtained by irradiating the ultraviolet photochromic nano system prepared in example 1 of the present invention with an ultraviolet light source having a power of 365nm of 5w for 0s, 5s, 10s, 15s, 20s, 25s, 35s, 50s, 70s, 100s, 120s, and 180 s. As can be seen from fig. 1, the ultraviolet photochromic nano system prepared in this embodiment can complete the color change in several minutes even under the sun in the shade, and the absorption intensity increases as the illumination time increases.
Fig. 2 is a spectrum detection diagram obtained by performing spectrum detection on the ultraviolet photochromic nano system prepared in embodiment 1 of the present invention under ultraviolet irradiation by using a fiber optic spectrometer. As can be seen from fig. 2, under the irradiation of ultraviolet light, the ultraviolet photochromic nano system prepared in the embodiment can strongly absorb light between 700 nm and 800nm, i.e., change color.
FIG. 3 is a transmission electron microscope image of the UV photochromic nanosystem prepared in example 1 of the present invention. As can be seen from FIG. 3, the MoO in the ultraviolet photochromic nano system prepared by the embodiment of the inventionxThe quantum dots are uniform in size and have the particle size of 2-5 nm.
In summary, the present invention discloses an ultraviolet photochromic nano system, a preparation method and an application thereof, comprising: adding molybdenum oxide into a mixed solvent of N-methyl pyrrolidone and water, and heating to obtain a mixed solution; carrying out centrifugal washing on the mixed solution to obtain an ultraviolet photochromic nano system; the preparation method is simple, low in cost, fast and capable of realizing large-scale production, complex organic synthesis and purification steps are omitted, the prepared ultraviolet photochromic nano system is high in ultraviolet sensitivity, short in response time and stable in cycle performance, plasma absorption is enhanced after the ultraviolet photochromic nano system changes color, plasma regulation and near infrared light absorption can be carried out, and the preparation method has important significance in the fields of plasma regulation and energy consumption reduction.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of an ultraviolet photochromic nano system is characterized by comprising the following steps:
adding molybdenum oxide into a mixed solvent of N-methyl pyrrolidone and water, and heating to obtain a mixed solution;
carrying out centrifugal washing on the mixed solution to obtain an ultraviolet photochromic nano system; wherein the ultraviolet photochromic nano system comprises MoOxQuantum dots and the mixed solvent.
2. The method for preparing the ultraviolet photochromic nano-system according to claim 1, wherein the heating temperature is 60 ℃ to 180 ℃, and the heating time is 0.5h to 42 h.
3. The method for preparing the ultraviolet photochromic nano system according to claim 1, wherein the particle size of the molybdenum oxide is 1-300 nm.
4. The method for preparing the ultraviolet photochromic nano system according to claim 1, wherein the volume ratio of the N-methyl pyrrolidone to the water in the mixed solvent is 1: 1.
5. The method of claim 1, wherein the MoO is a polymer of the ultraviolet photochromic nanosystemxThe particle size of the quantum dots is 2-5 nm.
6. The method for preparing the ultraviolet photochromic nano system according to claim 1, wherein the rotation speed of the centrifugal washing is 2000-12000 rpm.
7. An ultraviolet photochromic nanosystem, comprising: MoOxThe quantum dot-based organic light-emitting diode comprises quantum dots and a mixed solvent, wherein the mixed solvent is a mixed solvent of N-methylpyrrolidone and water.
8. The ultraviolet photochromic nanosystem of claim 7, wherein the volume ratio of the N-methylpyrrolidone to the water in the mixed solvent is 1: 1.
9. The ultraviolet photochromic nanosystem of claim 7, wherein the MoO isxThe particle size of the quantum dots is 2-5 nm.
10. An application of the ultraviolet photochromic nano system as claimed in any one of claims 7 to 9 in the fields of information encryption and optical anti-counterfeiting.
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| CN115472705A (en) * | 2022-09-05 | 2022-12-13 | 深圳技术大学 | Photoresistance material and preparation method thereof |
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| CN114620767A (en) * | 2022-03-15 | 2022-06-14 | 宁波磁性材料应用技术创新中心有限公司 | Sensitization processing method of molybdenum oxide nanosheet and resistance type hydrogen sulfide gas sensor |
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| CN115472705B (en) * | 2022-09-05 | 2024-05-17 | 深圳技术大学 | Photoresistor material and preparation method thereof |
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