Manganese-doped Cs2ZnCl4 metal halide and preparation method thereof
By controlling the molar ratio of cesium chloride, zinc chloride and manganese chloride and temperature treatment, the problems of uniformity and reaction sufficiency of manganese-doped Cs2ZnCl4 crystals were solved, and efficient preparation of high-uniformity crystals was achieved, which is suitable for large-scale production and property research.
Patent Information
- Application Number
- CN202410309867.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-19
- Publication Date
- 2025-09-23
AI Technical Summary
The existing preparation method of manganese-doped Cs2ZnCl4 results in poor crystal size uniformity and insufficient reaction of reactants, which affects the research of optical properties.
Cesium chloride, zinc chloride and manganese chloride in a specific molar ratio are dissolved in deionized water, and after being treated in an oven, they are transferred to a petri dish for slow crystallization. The temperature and time are controlled to ensure that the reaction proceeds fully.
The uniformity of manganese-doped Cs2ZnCl4 crystals and the utilization rate of reactants are improved, making it suitable for large-scale preparation and conducive to property research.
Abstract
Description
Technical Field
[0001] The present disclosure relates to the field of metal halide preparation, and in particular to a manganese-doped Cs2ZnCl4 metal halide and a preparation method thereof. Background Art
[0002] Cs2ZnCl4 is a zero-dimensional metal halide with simple synthesis, excellent chemical stability, and a wide band gap. Under X-ray irradiation, Cs2ZnCl4 exhibits strong ultraviolet emission at 310 nm, with two emission bands at 260 nm and 410 nm. Due to its rapid Auger-free luminescence in the ultraviolet spectral region, this compound is commonly used as a scintillator for high-energy X-ray detection. Its high temporal resolution and detection efficiency have attracted the attention of researchers. To further investigate its optical properties after doping, manganese ion doping experiments have been conducted. However, current methods for preparing manganese-doped Cs2ZnCl4 result in poor crystal size uniformity, hindering the study of the compound's optical properties and also causing issues with insufficient reactant reaction. Summary of the Invention
[0003] The embodiments of the present disclosure provide a manganese-doped Cs2ZnCl4 metal halide and a preparation method thereof, which can at least synthesize crystals with high uniformity, and the reactants react fully when prepared using the preparation method.
[0004] According to some embodiments of the present disclosure, on the one hand, an embodiment of the present disclosure provides a manganese-doped Cs2ZnCl4 metal halide, comprising: placing cesium chloride, zinc chloride and manganese chloride in a beaker according to a certain molar ratio; then adding deionized water to the beaker, stirring the deionized water to dissolve the cesium chloride, the zinc chloride and the manganese chloride in the deionized water, and obtaining a precursor solution; transferring the precursor solution to a reactor, placing the reactor in an oven, the program of the oven being configured to specific conditions, obtaining a reactant solution after the program of the oven is completed, and taking out the reactor when the oven is close to room temperature; transferring the reactant solution in the reactor to a culture dish, placing the culture dish in a constant temperature chamber, and slowly crystallizing the reactant solution to finally obtain the manganese-doped Cs2ZnCl4 metal halide.
[0005] In some embodiments, the molar ratio of the cesium chloride, the zinc chloride and the manganese chloride is 10:(5-10x):10x, where x represents Mn 2+ Doping concentration.
[0006] In some embodiments, 1%≤x≤15%.
[0007] In some embodiments, the specific conditions are: maximum temperature is 120°C-200°C, and insulation time is 15h-30h.
[0008] In some embodiments, the specific conditions are: the maximum temperature is 160° C., and the insulation time is 24 hours.
[0009] In some embodiments, the operating temperature of the constant temperature chamber is 30°C-50°C.
[0010] In some embodiments, the operating temperature of the constant temperature chamber is 35°C.
[0011] According to some embodiments of the present disclosure, on the other hand, embodiments of the present disclosure further provide a manganese-doped Cs2ZnCl4 metal halide, which is prepared using the preparation method of manganese-doped Cs2ZnCl4 described in any of the above embodiments.
[0012] The technical solution provided by the embodiments of the present disclosure has at least the following advantages: An embodiment of the present disclosure provides a manganese-doped Cs2ZnCl4 metal halide, comprising: placing cesium chloride, zinc chloride, and manganese chloride in a beaker at a certain molar ratio; adding deionized water to the beaker, stirring the deionized water to dissolve the cesium chloride, zinc chloride, and manganese chloride in the deionized water, and obtaining a precursor solution; transferring the precursor solution to a reactor, placing the reactor in an oven, wherein the oven program is configured to specific conditions, obtaining a reactant solution after the oven program is completed, and taking out the reactor when the oven is close to room temperature; transferring the reactant solution in the reactor to a culture dish, placing the culture dish in a constant temperature chamber, and allowing the reactant solution to slowly crystallize to ultimately obtain the manganese-doped Cs2ZnCl4 metal halide. The preparation method provided by the disclosed embodiments can ensure that the cesium chloride, zinc chloride, and manganese chloride reactants fully react in the reactor, thereby improving the utilization rate of the reactants and the efficiency of the manganese-doped Cs2ZnCl4 synthesis. The prepared manganese-doped Cs2ZnCl4 crystals have high uniformity in size, which is conducive to studying the properties of manganese-doped Cs2ZnCl4 metal halides. In addition, the preparation method is simple and can be applied to the large-scale preparation of manganese-doped Cs2ZnCl4. DETAILED DESCRIPTION
[0013] As can be seen from the background technology, the crystal size uniformity of the current preparation method of manganese-doped Cs2ZnCl4 is poor, which is not conducive to the study of the optical properties of the compound, and there is a problem of insufficient reaction of the reactants.
[0014] The following describes various embodiments of the present disclosure in detail. However, those skilled in the art will appreciate that many technical details are provided in the various embodiments of the present disclosure to facilitate a better understanding of the present disclosure. However, even without these technical details and the various variations and modifications based on the following embodiments, the technical solutions claimed in the present disclosure can still be implemented.
[0015] A method for preparing manganese-doped Cs2ZnCl4 metal halide comprises: placing cesium chloride, zinc chloride and manganese chloride in a beaker at a certain molar ratio; adding deionized water to the beaker, stirring the deionized water to dissolve the cesium chloride, zinc chloride and manganese chloride in the deionized water, and obtaining a precursor solution; transferring the precursor solution to a reactor, placing the reactor in an oven, wherein a program of the oven is configured to specific conditions, obtaining a reactant solution after the oven program is completed, and taking out the reactor when the oven is close to room temperature; transferring the reactant solution in the reactor to a culture dish, placing the culture dish in a constant temperature chamber, and allowing the reactant solution to slowly crystallize to finally obtain manganese-doped Cs2ZnCl4 metal halide.
[0016] In some embodiments, the molar ratio of cesium chloride, zinc chloride and manganese chloride is 10: (5-10x): 10x, where x represents Mn 2+ Doping concentration.
[0017] In some embodiments, 1%≤x≤15%. Within this range, it can be ensured that manganese ions are incorporated into Cs2ZnCl4 without changing the Cs2ZnCl4 matrix crystal structure.
[0018] It is understandable that in other examples, x may be greater than 15%.
[0019] In some embodiments, the specific conditions are: the maximum temperature is 120° C. to 200° C., for example, 120° C., 130° C., 140° C., 150° C., 160° C., 170° C., 180° C., 190° C., and 200° C. The holding time is 15 h to 30 h, for example, 15 h, 17 h, 19 h, 21 h, 23 h, 25 h, 27 h, 29 h, and 30 h.
[0020] In some embodiments, the operating temperature of the constant temperature chamber is 30°C-50°C, for example, 30°C, 32°C, 34°C, 36°C, 38°C, 40°C, 42°C, 44°C, 46°C, 48°C and 50°C.
[0021] To make the objectives, technical solutions, and advantages of the present invention more clearly apparent, various embodiments of the present invention will be described in detail below. However, those skilled in the art will appreciate that, in various embodiments of the present invention, many technical details are provided to help readers better understand the present application. However, even without these technical details and various variations and modifications based on the following embodiments, the technical solutions claimed in the present application can still be implemented. Example
[0022] Cesium chloride, zinc chloride and manganese chloride are placed in a beaker at a molar ratio of 10:4.9:0.1; deionized water is added to the beaker, and the deionized water is stirred to dissolve the cesium chloride, zinc chloride and manganese chloride in the deionized water to obtain a precursor solution; the precursor solution is transferred to a reactor, and the reactor is placed in an oven, and the oven program is configured to be 120°C for 15 hours. After the oven program is completed, a reactant solution is obtained, and the reactor is taken out when the oven is close to room temperature; the reactant solution in the reactor is transferred to a culture dish, and the culture dish is placed in a constant temperature chamber with the temperature set to 30°C. The reactant solution slowly crystallizes and finally obtains manganese-doped Cs2ZnCl4 metal halide. Example
[0023] Cesium chloride, zinc chloride and manganese chloride are placed in a beaker at a molar ratio of 10:4.5:0.5; deionized water is added to the beaker, and the deionized water is stirred to dissolve the cesium chloride, zinc chloride and manganese chloride in the deionized water to obtain a precursor solution; the precursor solution is transferred to a reactor, and the reactor is placed in an oven, and the oven program is configured to be 160°C for 15 hours. After the oven program is completed, a reactant solution is obtained, and the reactor is taken out when the oven is close to room temperature; the reactant solution in the reactor is transferred to a culture dish, and the culture dish is placed in a constant temperature chamber set at 40°C. The reactant solution slowly crystallizes and finally obtains manganese-doped Cs2ZnCl4 metal halide. Example
[0024] Cesium chloride, zinc chloride and manganese chloride are placed in a beaker at a molar ratio of 10:4:1; deionized water is added to the beaker, and the deionized water is stirred to dissolve the cesium chloride, zinc chloride and manganese chloride in the deionized water to obtain a precursor solution; the precursor solution is transferred to a reactor, and the reactor is placed in an oven, and the oven program is configured to be 200°C for 30 hours. After the oven program is completed, a reactant solution is obtained, and the reactor is taken out when the oven is close to room temperature; the reactant solution in the reactor is transferred to a culture dish, and the culture dish is placed in a constant temperature chamber with the temperature set at 50°C. The reactant solution slowly crystallizes and finally obtains manganese-doped Cs2ZnCl4 metal halide. The above-mentioned method for preparing manganese-doped Cs2ZnCl4 metal halide ensures that the cesium chloride, zinc chloride, and manganese chloride reactants fully react in the reactor, thereby improving the utilization rate of the reactants and the efficiency of the manganese-doped Cs2ZnCl4 synthesis. Furthermore, the prepared manganese-doped Cs2ZnCl4 crystals have high uniformity in size, which is beneficial for studying the properties of manganese-doped Cs2ZnCl4 metal halide. Furthermore, the preparation method is simple and suitable for large-scale preparation of manganese-doped Cs2ZnCl4.
[0025] Accordingly, another embodiment of the present disclosure further provides a manganese-doped Cs2ZnCl4 metal halide, which is prepared using the method for preparing the manganese-doped Cs2ZnCl4 metal halide described in any of the above embodiments. The preparation method of the adhesive remover provided in another embodiment of the present disclosure is described in detail below. For portions identical or corresponding to the previous embodiment, reference may be made to the corresponding description of the previous embodiment and will not be repeated in detail below.
[0026] Manganese-doped Cs2ZnCl4 metal halide is a lead-free zero-dimensional metal halide.
[0027] The above embodiments are intended only to illustrate the technical concepts and features of the present invention. Their purpose is to enable those skilled in the art to understand the contents of the present invention and implement them accordingly. They are not intended to limit the scope of protection of the present invention. Any equivalent changes or modifications made based on the spirit of the present invention are intended to be covered by the scope of protection of the present invention.
Claims
1. A method for preparing manganese-doped Cs2ZnCl4 metal halide, characterized in that: include: Place cesium chloride, zinc chloride and manganese chloride in a beaker according to a certain molar ratio; Adding deionized water into the beaker, stirring the deionized water to dissolve the cesium chloride, the zinc chloride, and the manganese chloride in the deionized water, and obtaining a precursor solution; The precursor solution is transferred to a reactor, and the reactor is placed in an oven. The oven program is configured to specific conditions. After the oven program is completed, a reactant solution is obtained. When the oven is close to room temperature, the reactor is taken out. The reactant solution in the reactor is transferred to a culture dish, and the culture dish is placed in a constant temperature chamber. The reactant solution is slowly crystallized to finally obtain the manganese-doped Cs2ZnCl4 metal halide.
2. The method for preparing manganese-doped Cs2ZnCl4 metal halide according to claim 1, characterized in that: The molar ratio of the cesium chloride, the zinc chloride and the manganese chloride is 10:(5-10x):10x, where x represents Mn 2+ Doping concentration.
3. The method for preparing manganese-doped Cs2ZnCl4 metal halide according to claim 2, characterized in that: 1%≤x≤15%。 4. The method for preparing manganese-doped Cs2ZnCl4 according to claim 1, characterized in that: The specific conditions are: maximum temperature of 120° C.-200° C., and insulation time of 15 h-30 h.
5. The method for preparing manganese-doped Cs2ZnCl4 metal halide according to claim 4, characterized in that: The specific conditions are: the maximum temperature is 160° C. and the insulation time is 24 hours.
6. The method for preparing manganese-doped Cs2ZnCl4 metal halide according to claim 1, characterized in that: The operating temperature of the constant temperature chamber is 30°C-50°C.
7. The method for preparing manganese-doped Cs2ZnCl4 metal halide according to claim 6, characterized in that: The operating temperature of the constant temperature chamber is 35°C.
8. A manganese-doped Cs2ZnCl4 metal halide, characterized in that The method for preparing manganese-doped Cs2ZnCl4 is used as described in any one of claims 1 to 7.