A method for preparing X-ray induced color-changing and luminescent materials

Abstract

This invention designs a method for preparing X-ray induced color-changing and luminescent materials, belonging to the technical field of photochromic materials. The method involves placing raw materials in an agate mortar and grinding and mixing them uniformly to obtain a mixture; sintering the mixture at high temperature to obtain a glass melt; pouring the glass melt onto a copper plate and cooling it to room temperature with the copper plate to obtain a Tb-doped material. 3+ Borosilicate glass was prepared by cutting and polishing the sample to obtain a glass sheet. The glass underwent X-ray irradiation to induce discoloration, and then the original color was restored by heat treatment. This invention utilizes high-temperature solid-state sintering and X-ray irradiation to induce discoloration, thus preparing a colorless transparent glass with X-ray irradiation-induced discoloration. This discoloration glass has a fast response and highly distinguishable color change, and can be used as an optical switch. The material exhibits obvious discoloration and luminescence, and is reversible, controllable, and stable.

Description

Technical Field

[0001] This invention belongs to the field of photochromic materials technology, specifically relating to a method for preparing X-ray induced color-changing and luminescent materials. Technical Background

[0002] Photochromic materials have attracted attention due to their increasingly widespread applications in light energy conversion, optical lenses, automotive windshields, optical anti-counterfeiting, and decorative materials, as well as their enormous potential applications in optical information storage, optical recording, and optical switches.

[0003] Currently, the X-ray irradiation-induced photochromic materials studied have drawbacks such as long color change time, slow reaction rate, natural fading phenomenon, uncontrollable color change range, and low distinguishability, which have become a long-term bottleneck restricting the development of this material.

[0004] Therefore, it is necessary to study a photochromic material that changes color rapidly, is stable over a long period of time, has high distinguishability, and is easy to prepare, in order to solve the problems of slow color change rate, poor stability, low distinguishability, and high cost of traditional X-ray irradiation-induced photochromic materials. Summary of the Invention

[0005] To address the problems of existing technologies, such as slow color-changing rate, poor stability, low distinguishability, and high cost, X-ray irradiation-induced photochromic materials are provided. Specifically, a method for preparing X-ray induced color-changing and luminescent materials is proposed, employing high-temperature solid-state sintering and X-ray irradiation to produce a color-changing material. This material exhibits significant color changes, allows for long-term repeated adjustment of sample color, and rapidly generates a color response under X-ray induction. It possesses high color distinguishability, high stability, fast response speed, and is simple and low-cost to prepare.

[0006] A method for preparing an X-ray induced color-changing and luminescent material, the specific steps of which are as follows:

[0007] S1: Based on a total molar amount of 100% of the mixture, place the raw materials B2O3 40-70%, SiO2 20-50%, Al2O3 5-15%, K2O 10-20%, ZnO 10-20%, NaO 5-10%, AgCl 1-5%, and TbF3 1-5% into an agate mortar, grind for ten minutes, and then transfer to a ceramic crucible.

[0008] S2: Under air atmosphere, the ceramic crucible in S1 is sintered in a high-temperature furnace at 1200℃ for 1-2 hours. The molten glass is poured onto a copper plate preheated to 300℃ and held for 15 minutes. Then it is cooled to room temperature to obtain the initial glass.

[0009] S3: The glass obtained in S2 is heat-treated at 400°C for 5-10 hours in an air atmosphere and then cooled to room temperature in the furnace to obtain glass with X-ray induced color change and luminescence.

[0010] S4: The glass prepared in S2 and S3 exhibiting X-ray irradiation-induced discoloration and luminescence is placed in an irradiation dose of 3.9 × 10⁻⁶. -4 Gy / s ~ 3.5 × 10 -3 Irradiation with X-rays of Gy / s for 30s to 10min induces discoloration.

[0011] A method for preparing X-ray induced color-changing and luminescent materials, which, due to their rapid color-changing response and luminescence to X-rays, are intended for application in the field of visual X-ray radiation detection.

[0012] The basic principle of this invention is as follows: When X-rays irradiate glass, color centers are generated. The generation of color centers causes the color of the sample itself to change from colorless and transparent to brown. By heating, the defects in the glass release electrons, the color centers disappear, and the sample fades back to its original colorless and transparent state.

[0013] The beneficial effects of this invention are as follows:

[0014] (1) This invention utilizes high-temperature solid-state sintering and X-ray irradiation-induced color change to prepare colorless transparent glass with X-ray irradiation-induced color change. The color-changing glass has a fast response and a large color change with high distinguishability, and can be used as an optical switch.

[0015] (2) The present invention has a simple process, short preparation cycle, low cost and obvious color change and luminescence, and is expected to be practically applied in the field of visual X-ray detection.

[0016] (3) The X-ray irradiation-induced color-changing material of the present invention solves the problems of slow color-changing rate, poor stability, low distinguishability and high cost of traditional X-ray irradiation-induced photochromic materials. Attached Figure Description

[0017] The accompanying drawings are used to illustrate specific embodiments of this experiment and form part of the application, but do not constitute a limitation on the embodiments of the present invention.

[0018] Figure 1 These are photographs of the glass obtained in Example 1 before and after X-ray irradiation, and after fading;

[0019] Figure 2 These are photographs of the glass obtained in Example 2 before and after X-ray irradiation, and after fading;

[0020] Figure 3 Transmission spectra of glass before and after X-ray irradiation;

[0021] Figure 4 It is the emission spectrum of glass under X-ray irradiation.

[0022] Specific Implementation Cases

[0023] The present invention will be further described below with reference to specific embodiments and accompanying drawings, but the present invention is not limited to the following embodiments.

[0024] Example 1

[0025] A method for preparing an X-ray induced color-changing and luminescent material, the specific steps of which are as follows:

[0026] S1: Based on a molar weight of 100%, first weigh 41.5% B2O3, 27% SiO2, 5% Al2O3, 10% K2O, 10% ZnO, 5% NaO, and 1.5% AgCl, grind them thoroughly, and then place them in a ceramic crucible.

[0027] S2: Under air atmosphere, the ceramic crucible in S1 is sintered in a high-temperature furnace at 1200℃ for 1 hour, and the molten glass is poured onto a copper plate preheated to 300℃.

[0028] S3: Place the glass in an annealing furnace at 400℃ and keep it warm for 5 hours.

[0029] S4: After grinding and polishing the glass, it is placed under X-ray irradiation to induce discoloration, and then the glass is heated to restore its original color.

[0030] This embodiment is in the case of no Tb doping. 3+ In the case of obtaining such Figure 1 The glass shown in (a) exhibits a highly colorless and transparent state. After X-ray irradiation, it undergoes X-ray irradiation-induced discoloration but does not induce luminescence. Furthermore, the X-ray-irradiated glass can be faded by heat treatment at 400°C, as shown in (a). Figure 1 As shown in (c), it has basically returned to its initial state.

[0031] Example 2

[0032] A method for preparing an X-ray induced color-changing and luminescent material, the specific steps of which are as follows:

[0033] S1: Weigh and grind 40.5% B2O3, 27% SiO2, 5% Al2O3, 10% K2O, 10% ZnO, 5% NaO, 1.5% AgCl, and 1% TbF3 in 100% molar weight, and place them in a ceramic crucible.

[0034] S2: Under air atmosphere, the ceramic crucible in S1 is sintered in a high-temperature furnace at 1200℃ for 2 hours, and the molten glass is poured onto a copper plate preheated to 300℃.

[0035] S3: Place the glass in an annealing furnace at 400℃ and keep it warm for 10 hours.

[0036] S4: After grinding and polishing the glass, it is placed under X-ray irradiation to induce discoloration, and then the glass is heated to restore its original color.

[0037] S5: The transmission and emission spectra of the glass before and after discoloration were measured using spectrometers (F7000 and U4100).

[0038] After X-ray irradiation, the glass obtained in Example 2 changed from colorless and transparent to brown and emitted green light at 548 nm. The corresponding transmittance and luminescence intensity are as follows: Figure 3 , 4 As shown. The image obtained after X-ray bleaching of the glass at 400℃ is shown below. Figure 2 As shown in (c), it has essentially returned to its initial state. Therefore, the discoloration and luminescence of this glass induced by X-ray radiation can be applied to visual X-ray radiation detection.

[0039] Example 3

[0040] like Figures 1 to 4 As shown, the glass is sintered in air and becomes colorless and transparent; under X-ray irradiation, the colorless and transparent glass turns brown and emits a relatively strong green light, which can ensure that the radiation source serves as a warning when it is activated; the glass color change can be repeated cyclically, and when used as an optical storage material, it can realize the writing and erasing of data; the degree of glass color change changes in a gradient with the change of radiation measurement; the glass color is reversible and the light emission is adjustable.

[0041] The glasses obtained in Examples 1-3 of this invention, wherein the sintering temperature is 1200℃ and the glass obtained after holding at the temperature for 5h and 10h respectively, are all glasses with X-ray irradiation-induced discoloration. Based on the displayed X-ray discoloration and luminescence phenomena, as well as the measured transmission and emission spectra, it can be seen that the glass has the characteristics of high color discrimination, strong luminescence, high stability, fast response speed and simple preparation, and has reversibility. It has broad application prospects in the fields of visual X-ray radiation detection and optical storage.

[0042] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0043] Although the main inventive examples that influence the factors of this experiment have been described and listed, those skilled in the art will understand that various changes, explorations, modifications and combinations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.

Claims

1. A method for preparing an X-ray induced color-changing and luminescent material, characterized in that, Includes the following steps: S1: Grind the raw materials B2O3, SiO2, Al2O3, K2O, ZnO, NaO, AgCl, and TbF3 evenly to obtain a mixture; S2: The mixture described in S1 is placed in a ceramic dry pot and sintered at a temperature of 1200°C for 1-2 hours under an air atmosphere. The molten mixture obtained after sintering is poured onto a copper plate and cooled to room temperature with the copper plate to obtain glass. S3: The glass obtained from S2 is heat-treated at 400℃ for 5 to 10 hours to remove residual stress in the glass. S4: Polish the glass from S3, then irradiate it under X-rays to induce discoloration and luminescence, thus preparing glass with X-ray discoloration and luminescence effects; The raw materials described in S1, in 100% molar amounts, are: 40.5% B₂O₃, 27% SiO₂, 5% Al₂O₃, 10% K₂O, 10% ZnO, 5% NaO, 1.5% AgCl, and 1% TbF₃.

2. The method for preparing an X-ray induced color-changing and luminescent material according to claim 1, characterized in that: In S4, the X-ray irradiation dose rate is 3.9 × 10⁻⁶. -4 Gy / s ~ 3.5 × 10 -3 Gy / s, time is 30s to 10min.

3. An X-ray induced color-changing and luminescent material, characterized in that: It is prepared by the preparation method according to any one of claims 1-2.

4. The application of the material prepared by the method for preparing X-ray induced color-changing and luminescent materials according to any one of claims 1-2 in visual X-ray radiation detection materials and optical storage materials.

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