Preparation method of large-size two-dimensional layered metal thiophosphate crystal
A metal thiophosphate, two-dimensional layered technology, applied in crystal growth, chemical instruments and methods, self-solids, etc., to achieve the effect of simple operation
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[0028] A method for preparing large-scale two-dimensional layered metal thiophosphate crystals, comprising the following steps:
[0029] S1. Weigh indium spheres, phosphorus lumps and sulfur granules according to the stated amount and ratio, and use them as raw materials after mixing. Elemental iodine is used as a transport agent, and potassium iodide is used as a molten salt. The mass ratio of indium spheres, phosphorus blocks and sulfur granules is 2:3:9. According to the volume of the reaction vessel, the amount of elemental iodine added is 1-3 mg / mL; that is, 1-3 mg of elemental iodine needs to be added per milliliter of reaction vessel.
[0030] S2. Put the raw materials, elemental iodine and potassium iodide into the reaction vessel together, vacuum seal it under a certain pressure, and then carry out high-temperature reaction. The pressure of the reaction vessel is less than 10 -4 mbar. Place the sealed reaction vessel horizontally in a tube furnace with two temperat...
Embodiment 1
[0033] 574 mg of indium spheres, 232.5 mg of red phosphorus lumps, 720 mg of sulfur pellets, 600 mg of potassium iodide and 30 mg of iodine were vacuum sealed together in a quartz tube. The pressure in the quartz tube is less than 10 -4 mbar. React in a tube furnace with dual temperature zones for 3 days, the temperature in the high temperature zone is 700°C, and the temperature in the low temperature zone is 650°C. After the reaction is completed, wait until it drops to room temperature, wash with acetone to remove residual iodine, and wash with ultrapure water to remove potassium iodide , to obtain centimeter-sized single crystals. Such as figure 1 As shown, the size of the single crystal reaches the order of centimeters, and the crystal is yellow. Such as figure 2 As shown, the X-ray diffraction pattern shows that the obtained crystal is metal indium thiophosphate. Such as image 3 As shown, the scanning electron micrograph of the crystal shows that the obtained sing...
Embodiment 2
[0035] 574 mg of indium spheres, 232.5 mg of red phosphorus lumps, 720 mg of sulfur pellets, 600 mg of potassium iodide and 30 mg of iodine were vacuum sealed together in a quartz tube. The pressure in the quartz tube is less than 10 -4 mbar. React in a tube furnace with dual temperature zones for 3 days, the temperature in the high temperature zone is 650°C, and the temperature in the low temperature zone is 600°C. After the reaction is completed, wait until it drops to room temperature, wash with acetone to remove residual iodine, and wash with ultrapure water to remove potassium iodide , to obtain a centimeter-sized metal indium thiophosphate single crystal. Such as Figure 4 As shown, the size of the single crystal reaches the order of centimeters, and the crystal is yellow.
[0036] The metal indium thiophosphate single crystal prepared by the method described in Example 1 or Example 2 is placed on the 3M adhesive tape, and the obtained metal indium thiophosphate singl...
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