Background
The photochromic phenomenon means that a certain compound A undergoes a specific reaction when being irradiated by light with a certain wavelength and intensity to obtain another product B, and the absorption/diffuse reflection spectrum of the product B is obviously changed (the color of the product B is changed) due to the difference of the structure, the valence state, the concentration of a color center and the like of the product B. And under the irradiation of light with another wavelength or under the action of heat, the product B can be restored to the form of the compound A. Such compounds, which undergo a reversible colour change under the action of light, are known as photochromic materials. Photochromic materials can be broadly classified into organic photochromic materials and inorganic photochromic materials according to their components, and among them, inorganic photochromic materials have more excellent thermal stability, longer life span of use cycle number, and coloring property by multiple cycles than organic photochromic materials and are receiving much attention. The photochromic material has potential application in a plurality of fields such as information storage, information encryption, safety anti-counterfeiting, luminous regulation and control, architectural decoration and the like.
However, since inorganic photochromic materials have been reported to have few multi-color changes, they mainly focus on the change of the shade of color, and only the change of the absorption intensity is present without significant change of the position of the characteristic absorption peak in the absorption/diffuse reflection spectrum, which greatly limits the application of the inorganic photochromic materials. Therefore, it is important to broaden the variety of photochromic color changes.
Disclosure of Invention
In order to solve the technical problems, the invention designs molybdate reversible multicolor photochromic up-conversion phosphor and a preparation method thereof, and the reversible photochromic up-conversion phosphor is light yellow, blue gray and pink under the stimulation of light with different wavelengths. The up-conversion spectrum of the fluorescent powder is changed along with the change of the color, so that the up-conversion luminescence regulation and control are realized.
In order to achieve the technical effects, the invention is realized by the following technical scheme: the molybdate reversible multicolor photochromic upconversion fluorescent powder has the following chemical formula:
Pb1-xYb0.005ErxW0.05Mo0.95O4wherein x is 0.01-0.05.
The invention also provides a preparation method of the molybdate reversible multicolor photochromic up-conversion phosphor, which comprises the following steps:
step 1: according to the chemical formula, Pb1-xYb0.005ErxW0.05Mo0.95O4Wherein, MoO3, WO3, yellow PbO, Yb2O3 and Er2O3 are weighed according to the mol ratio of 0.01-0.05, and absolute ethyl alcohol is added to be mixed and ground uniformly until the mixture is dried to obtain the mixed material.
Step 2: and (3) uniformly heating the dried mixed material to 520 ℃ in a muffle furnace for 2 hours in the air atmosphere, keeping the temperature for 2-4 hours at constant temperature, and cooling to room temperature along with the furnace to obtain the light yellow molybdate reversible multicolor photochromic upconversion fluorescent powder.
A molybdate up-conversion phosphor reversible multicolor photochromic method comprises the following steps:
1. the original light yellow molybdate up-conversion fluorescent powder is placed under light with wavelength of 405 nanometers at the concentration of 400mW/cm2The power density of (a) was irradiated for 21 minutes, and the phosphor changed from pale yellow to blue-gray. Then the fluorescent powder which has changed into blue gray is treated by 808 nanometer laser at the speed of 2.5W/cm2Is irradiated for 60 seconds to return to the original light yellow state.
2. Putting original light yellow or blue-gray molybdate up-conversion fluorescent powder under 473 nm wavelength laser at 3W/cm2Light yellow or blue-gray phosphor turns pink when irradiated for 50 seconds. Then the fluorescent powder which has changed into pink is treated by 808 nanometer laser at the speed of 2.5W/cm2Is irradiated for 60 seconds to return to the original light yellow state.
The color of the fluorescent powder is changed to reflect the change of a diffuse reflection spectrum, and the multi-mode reversible regulation and control of up-conversion luminescence is realized through the self-absorption effect of the material.
The invention has the beneficial effects that:
the invention provides molybdate reversible multicolor photochromic up-conversion phosphor and a preparation method thereof, which realize multicolor reversible photochromism of light yellow, blue gray and pink of the phosphor under the stimulation of light with different wavelengths. The up-conversion spectrum of the fluorescent powder is changed along with the change of the color, so that up-conversion luminescence regulation and control are realized; the photochromic color change variety is broadened.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
Example 1
Pb1-xYb0.005ErxW0.05Mo0.95O4Preparing fluorescent powder:
step 1, weighing MoO according to a chemical formula and a molar ratio3,WO3Yellow PbO, Yb2O3,Er2O3And adding absolute ethyl alcohol, mixing and grinding uniformly until the mixture is dried to obtain a mixed material.
And 2, uniformly heating the dried mixed material in a muffle furnace for 2 hours to 520 ℃ in an air atmosphere, keeping the temperature for 2-4 hours at a constant temperature, and cooling the mixture to room temperature along with the furnace to obtain the light yellow molybdate reversible multicolor photochromic upconversion fluorescent powder.
The molybdate up-conversion phosphor reversible light yellow-blue gray photochromic method comprises the following steps:
the original light yellow molybdate up-conversion fluorescent powder is placed under light with wavelength of 405 nanometers at the concentration of 400mW/cm2The power density of (a) was irradiated for 21 minutes, and the phosphor changed from pale yellow to blue-gray. Then the fluorescent powder which has changed into blue gray is treated by 808 nanometer laser at the speed of 2.5W/cm2Is irradiated for 60 seconds to return to the original light yellow state. The light yellow and blue gray diffuse reflectance spectra are shown in FIG. 2.
The molybdate up-conversion phosphor can regulate up-conversion luminescence by reversible light yellow-blue gray photochromism:
the light yellow and blue gray colors, respectively, of the molybdate upconverted fluorescence were excited with a 980 nm laser and the change in the upconverted luminescence spectrum was measured as shown in fig. 3.
Example 2
Pb1-xYb0.005ErxW0.05Mo0.9504Preparing fluorescent powder:
step 1, weighing MoO according to a chemical formula and a molar ratio3,WO3Yellow PbO, Yb2O3,Er2O3And adding absolute ethyl alcohol, mixing and grinding uniformly until the mixture is dried to obtain a mixed material.
And 2, uniformly heating the dried mixed material in a muffle furnace for 2 hours to 520 ℃ in an air atmosphere, keeping the temperature for 2-4 hours at a constant temperature, and cooling the mixture to room temperature along with the furnace to obtain the light yellow molybdate reversible multicolor photochromic upconversion fluorescent powder.
The molybdate up-conversion phosphor reversible light yellow/blue gray-pink-light yellow photochromic method comprises the following steps:
putting original light yellow or blue-gray molybdate up-conversion fluorescent powder under 473 nm wavelength laser at 3W/cm2Light yellow or blue-gray phosphor turns pink when irradiated for 50 seconds. Then the fluorescent powder which has changed into pink is treated by 808 nanometer laser at the speed of 2.5W/cm2Is irradiated for 60 seconds to return to the original light yellow state. The light yellow, blue-gray and pink diffuse reflectance spectra are shown in FIG. 2.
The molybdate up-conversion phosphor can regulate up-conversion luminescence by reversible light yellow-pink photochromism:
the molybdate up-converted fluorescence was excited with a 980 nm laser and the up-converted luminescence spectrum was measured as shown in fig. 3 for light yellow/blue gray and pink, respectively.
Example 3
Pb1-xYb0.005ErxW0.05Mo0.95O4Preparing fluorescent powder:
step 1, weighing MoO according to a chemical formula and a molar ratio3,WO3Yellow PbO, Yb2O3,Er2O3And adding absolute ethyl alcohol, mixing and grinding uniformly until the mixture is dried to obtain a mixed material.
And 2, uniformly heating the dried mixed material in a muffle furnace for 2 hours to 520 ℃ in an air atmosphere, keeping the temperature for 2-4 hours at a constant temperature, and cooling the mixture to room temperature along with the furnace to obtain the light yellow molybdate reversible multicolor photochromic upconversion fluorescent powder.
The molybdate up-conversion phosphor reversible light yellow-blue gray-pink-light yellow photochromic method comprises the following steps:
the original light yellow molybdate up-conversion fluorescent powder is placed under light with wavelength of 405 nanometers at the concentration of 400mW/cm2The power density of (a) was irradiated for 21 minutes, and the phosphor changed from pale yellow to blue-gray. Placing the blue-gray fluorescent powder under 473 nm wavelength laser at 3W/cm2The blue-gray phosphor changed to pink after being irradiated for 50 seconds. Then the fluorescent powder which has changed into pink is treated by 808 nanometer laser at the speed of 2.5W/cm2Is irradiated for 60 seconds to return to the original light yellow state. The light yellow, blue gray and pink diffuse reflection spectrum is shown in figure 2.
The molybdate up-conversion phosphor can regulate up-conversion luminescence by reversible light yellow-blue gray-pink-light yellow photochromism:
the molybdate up-conversion phosphor was excited with 980 nm laser and measured for up-conversion luminescence spectrum change for light yellow, blue gray and pink colors, respectively, as shown in fig. 3.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments 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 utilize the invention. The invention is limited only by the claims and their full scope and equivalents.