Inorganic compound crystal CsSb5S8 and preparation method and application thereof
A technology of inorganic compounds and crystals, applied in chemical instruments and methods, crystal growth, self-solid, etc., to achieve the effect of simple process, good application value, and high crystallinity
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Embodiment 1
[0062] Example 1 Sample CsSb 5 S 8 Synthesis
[0063] After Ba (28.8mg), Sb (127.8mg), S (60.6mg) and CsCl (282.8mg) were mixed evenly, they were put into a quartz tube and evacuated to 1×10 -4 Seal the tube with Pa, put it into the muffle furnace and heat it to 800°C at a rate of 32°C / h. ℃), the chemical formula is CsSb 5 S 8 crimson crystals. Take it out and grind it to get powdered CsSb 5 S 8 compound.
[0064] The sample numbers, types and amounts of raw materials, reaction temperature and holding time, and cooling rate are shown in Table 1.
[0065] Table 1
[0066]
Embodiment 2
[0067] The structural analysis of embodiment 2 crystal
[0068] Using single crystal X-ray diffraction and powder X-ray diffraction methods, sample 1 # ~5 # Perform structural analysis.
[0069] The instrument used for single crystal X-ray diffraction: Rigaku FR-X microfocus diffractometer, test condition: 293K, and SHELXTL crystallographic software for structure analysis.
[0070] The instrument used for powder X-ray diffraction: Rigaku Flex600 X-ray diffractometer, test condition: 293K.
[0071] Among them, the results of single crystal X-ray diffraction showed that sample 1 # ~5 # The chemical formula is CsSb 5 S 8 , is a centrosymmetric structure, belongs to the monoclinic crystal system, and the space group is P2 1 / n, the unit cell parameter is Z=4. The inorganic compound crystal CsSb 5 S 8 The crystal structure of figure 1 shown. Inorganic compound free crystal CsSb 5 S 8 is a one-dimensional infinite band structure 1 ∞ [Sb 5 S 8 ], consisting of mu...
Embodiment 3
[0075] Embodiment 3 Differential scanning calorimetry experiment and result
[0076] Take sample 1 # represented by the inorganic compound crystal CsSb 5 S 8 Differential scanning calorimetry tests were performed. The test instrument is a Mettler Toledo thermal analyzer, and the test method is to mix CsSb 5 S 8 The polycrystalline sample is placed in a quartz tube and then pumped to about 10 -4 Pa and sealed. Then, two heating / cooling cycles were performed at a rate of 30°C / min.
[0077] image 3 for its test results, where image 3 (a) represents CsSb 5 S 8 The first differential scanning calorimetry (DSC) cycle of the image 3 (b) means CsSb 5 S 8 of the second DSC cycle. show that CsSb 5 S 8 Its glass transition temperature is 202°C, and it has a crystalline-glass phase transition behavior.
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