CN114507064A - Novel photochromic material and preparation method thereof - Google Patents

Novel photochromic material and preparation method thereof Download PDF

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CN114507064A
CN114507064A CN202011275706.0A CN202011275706A CN114507064A CN 114507064 A CN114507064 A CN 114507064A CN 202011275706 A CN202011275706 A CN 202011275706A CN 114507064 A CN114507064 A CN 114507064A
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conversion luminescence
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陈思
毕见强
郝瀚钰
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Civil Aviation University of China
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Abstract

The invention discloses a novel photochromic effect material and a preparation method thereof. The chemical formula of the material is Ba0.7Sr0.21‑ 1.5xHoxYb0.06Nb2O6Wherein x is 0.0, 0.02, 0.04, 0.08, 0.10, 0.12 or 0.14. The preparation method is that SrCO3、BaCO3、Yb2O3、Ho2O3And Nb2O5Mixing and grinding the raw materials in proportion, and preparing Ba by a simple high-temperature solid-phase reaction method0.7Sr0.21‑1.5xHoxYb0.06Nb2O6A ceramic material. The invention has the advantages that: under near ultraviolet irradiation, the material exhibits significant discoloration. At the same time, the discoloration can be restored to the pre-irradiation state under the thermal stimulationState. The material can be used in the fields of optical switches, optical storage, safety and anti-counterfeiting in the future.

Description

Novel photochromic material and preparation method thereof
Technical Field
The invention belongs to the technical field of inorganic non-metallic functional materials, and particularly relates to a novel photochromic material and a preparation method thereof.
Background
Photochromic materials have many important applications in data storage, optical switching, rewritable paper and multicolor displays and the like. For many years, researchers have conducted extensive research on photochromic materials. However, the past studies have been mainly focused on organic substances such as stilbene derivatives, sulfoxides, stanhaus compounds, hydrazone compounds, o-nitrobenzyl derivatives, and the like. However, most organic materials are poor in thermal stability and toxic to the environment, thus limiting their applications.
Compared with organic materials, inorganic photochromic materials have many advantages, such as good chemical stability, high mechanical strength, strong oxidation resistance, etc. It is noted that relatively few inorganic photochromic materials exist and that the performance is not as desirable. In order to meet the requirements of future photoelectric devices, researchers are required to develop novel inorganic photochromic materials.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a novel photochromic material and a method for preparing the same.
In order to achieve the purpose, the up-conversion luminescence reversible regulation material based on the photochromic effect provided by the invention has a chemical formula of Ba0.7Sr0.21-1.5xHoxYb0.06Nb2O6Wherein x is 0.0, 0.02, 0.04, 0.08, 0.10, 0.12 or 0.14.
The preparation method of the material is to use SrCO3、BaCO3、Yb2O3、Ho2O3And Nb2O5Mixing the raw materials in proportion, grinding the mixture into uniformly mixed powder in a ball mill by using ethanol as a solvent, drying the powder, and pre-sintering at 1300 ℃; grinding the pre-sintered powder again, adding a binder, granulating, tabletting, sintering at 1350 ℃, cooling to room temperature, polishing and thinning the surface of the silicon carbide to obtain Ba with photochromic effect0.7Sr0.21-1.5xHoxYb0.06Nb2O6A ceramic material.
The material with photochromic effect and the preparation method thereof provided by the invention have the following characteristics:
1. with SrCO3、BaCO3、Yb2O3、Ho2O3And Nb2O5As raw material, and Ba is prepared by simple high-temperature solid-phase reaction method0.7Sr0.21-1.5xHoxYb0.06Nb2O6A ceramic material.
2. The study shows that Ba0.7Sr0.21-1.5xHoxYb0.06Nb2O6After the ceramic material is irradiated by near ultraviolet light for a certain time, the diffuse reflection spectrum intensity of the material is obviously reduced.
3. Research shows that Ba is generated after ultraviolet light irradiation for a certain time0.7Sr0.21-1.5xHoxYb0.06Nb2O6The ceramic sample changes color and exhibits a significant photochromic effect.
Drawings
FIG. 1 shows Ba provided by an embodiment of the present invention0.7Sr0.21-1.5xHoxYb0.06Nb2O6(X ═ 0.0, 0.02, 0.04, 0.08, 0.10, 0.12, or 0.14) the X-ray diffraction pattern of the ceramic material.
FIG. 2 shows Ba provided in an embodiment of the present invention0.7Sr0.21-1.5xHoxYb0.06Nb2O6(x ═ 0.0, 0.02, 0.04, 0.08, 0.10, 0.12, or 0.14) the diffuse reflectance spectrum of the ceramic material before and after irradiation with near ultraviolet light.
FIG. 3 shows Ba provided by an embodiment of the present invention0.7Sr0.21-1.5xHoxYb0.06Nb2O6(x ═ 0.12) photograph of the surface of the ceramic material, the color of the portion of the center irradiated with near ultraviolet light changed from yellowish brown to grayish black.
FIG. 4 shows Ba provided by an embodiment of the present invention0.7Sr0.21-1.5xHoxYb0.06Nb2O6(x ═ 0.12) photographs of the surfaces of the ceramic materials after heat treatment at 200 ℃ for 1 minute, the color of the samples returning to the initial state.
Detailed Description
The invention will now be further described with reference to specific embodiments:
example 1:
the up-conversion luminescence reversible control material provided by the embodiment is Ba0.7Sr0.21-1.5xHoxYb0.06Nb2O6The ceramic material, wherein x is 0.02, is prepared by the following steps:
2.7907 g of BaCO were weighed out3(99%), 0.5368 g SrCO3(99%), 0.0756 g Ho2O3(99.9%), 0.2367 g Yb2O3(99.9%) and 5.3167 g Nb2O5(99.99%) was placed in a clean agate jar and ground on a planetary ball mill for 24 hours using absolute ethanol (99.7%) as a solvent to make a uniformly mixed powder. And then drying the powder by using an oven, then placing the powder into a corundum crucible, placing the corundum crucible into a box-type furnace, continuously heating to 1300 ℃, presintering for 3 hours, and cooling to 550 ℃. And grinding the product obtained after furnace cooling by using an agate mortar, adding a bonding agent PVB (the weight ratio of the PVB to the product is 0.5%), fully grinding, uniformly mixing and granulating. Ceramic green sheets having a diameter of 13mm were prepared under a pressure of 10 MPa. Placing the ceramic green sheet in a high-temperature furnace, continuously heating, keeping the temperature at 700 ℃ for 120 minutes for plastic removal, then continuously heating, sintering at 1350 ℃ for 3 hours, cooling to 550 ℃, and naturally cooling to obtain Ba with x being 0.020.7Sr0.3-1.5xErxNb2O6A ceramic material.
Example 2:
the up-conversion luminescence reversible control material provided by the embodiment is Ba0.7Sr0.21-1.5xHoxYb0.06Nb2O6The ceramic material, wherein x is 0.08, is prepared by the following steps:
2.7907 g of BaCO were weighed out3(99%), 0.2684 g SrCO3(99%), 0.3026 g Ho2O3(99.9%), 0.2367 g Yb2O3(99.9%) and 5.3167 g Nb2O5(99.99%) was placed in a clean agate jar and ground on a planetary ball mill for 24 hours using absolute ethanol (99.7%) as a solvent to make a uniformly mixed powder. And then drying the powder by using an oven, then placing the powder into a corundum crucible, placing the corundum crucible into a box-type furnace, continuously heating to 1300 ℃, presintering for 3 hours, and cooling to 550 ℃. Grinding the product with agate mortar, adding adhesive PVB (0.5 wt% of product), grinding, and mixingAnd (4) homogenizing and granulating. Ceramic green sheets having a diameter of 13mm were prepared under a pressure of 10 MPa. Placing the ceramic green sheet in a high-temperature furnace, continuously heating, keeping the temperature at 700 ℃ for 120 minutes for plastic removal, then continuously heating, sintering at 1350 ℃ for 3 hours, cooling to 550 ℃, and naturally cooling to obtain Ba with x being 0.040.7Sr0.3-1.5xErxNb2O6A ceramic material.
Example 3:
the up-conversion luminescence reversible control material provided by the embodiment is Ba0.7Sr0.21-1.5xHoxYb0.06Nb2O6The ceramic material, wherein x is 0.12, is prepared by the following steps:
2.7907 g of BaCO were weighed out3(99%), 0.0895 g SrCO3(99%), 0.4539 g Ho2O3(99.9%), 0.2367 g Yb2O3(99.9%) and 5.3167 g Nb2O5(99.99%) was placed in a clean agate jar and ground on a planetary ball mill for 24 hours using absolute ethanol (99.7%) as a solvent to make a uniformly mixed powder. And then drying the powder by using an oven, then placing the powder into a corundum crucible, placing the corundum crucible into a box-type furnace, continuously heating to 1300 ℃, presintering for 3 hours, and cooling to 550 ℃. And grinding the product obtained after furnace cooling by using an agate mortar, adding a bonding agent PVB (the weight ratio of the PVB to the product is 0.5%), fully grinding, uniformly mixing and granulating. Ceramic green sheets having a diameter of 13mm were prepared under a pressure of 10 MPa. Placing the ceramic green sheet in a high-temperature furnace, continuously heating, keeping the temperature at 700 ℃ for 120 minutes for plastic removal, then continuously heating, sintering at 1350 ℃ for 3 hours, cooling to 550 ℃, and naturally cooling to obtain Ba with x being 0.120.7Sr0.3-1.5xErxNb2O6A ceramic material.

Claims (7)

1. A novel photochromic material is characterized in that: the material has a chemical formula of Ba0.7Sr0.21- 1.5xHoxYb0.06Nb2O6Wherein x is 0.0, 0.02, 0.04. 0.08, 0.10, 0.12 or 0.14.
2. A novel photochromic material is characterized in that: ba0.7Sr0.21-1.5xHoxYb0.06Nb2O6(x ═ 0.0, 0.02, 0.04, 0.08, 0.10, 0.12, or 0.14) ceramic materials have a pronounced color change effect under near ultraviolet radiation.
3. A method for preparing the reversible regulating material for up-conversion luminescence according to claim 1, wherein the method comprises the following steps: the preparation method is to use BaCO3、SrCO3、Yb2O3、Ho2O3And Nb2O5Mixing the raw materials in proportion, grinding the mixture into uniformly mixed powder in a ball mill by using ethanol as a solvent, drying the powder, and pre-sintering at 1300 ℃; then grinding the pre-sintered powder again, adding an adhesive and granulating, sintering at 1350 ℃ after tabletting, cooling to room temperature, and obtaining Ba belonging to the up-conversion luminescence reversible regulation material after polishing and thinning the surface of silicon carbide0.7Sr0.21-1.5xHoxYb0.06Nb2O6A ceramic material.
4. The method for preparing the up-conversion luminescence reversible modulation material according to claim 3, wherein: the ball mill adopts a planetary ball mill.
5. The method for preparing the up-conversion luminescence reversible modulation material according to claim 3, wherein: the grinding time in the ball mill is 24 h.
6. The method for preparing the up-conversion luminescence reversible modulation material according to claim 3, wherein: the pre-sintering time is 3 hours.
7. The method for preparing the up-conversion luminescence reversible modulation material according to claim 3, wherein: the sintering time is 3 hours.
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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN116925765A (en) * 2023-07-18 2023-10-24 西华大学 Scandium aluminate photochromic reversible up-conversion luminescent fluorescent powder material and modulation method thereof

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Publication number Priority date Publication date Assignee Title
CN116925765A (en) * 2023-07-18 2023-10-24 西华大学 Scandium aluminate photochromic reversible up-conversion luminescent fluorescent powder material and modulation method thereof
CN116925765B (en) * 2023-07-18 2024-05-07 西华大学 Scandium aluminate photochromic reversible up-conversion luminescent fluorescent powder material and modulation method thereof

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