Controllable preparation method of Cu3SbS4 nanocrystalline material
A nanocrystalline material and temperature control technology, applied in the nanomaterials and nano fields, to achieve the effect of simple process, good reproducibility and low cost
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Embodiment 1
[0019] Cu 3 Sb 4 The controllable preparation method of nanocrystalline material comprises the following steps:
[0020] (1) Add 3mmol cuprous iodide and 1mmol antimony chloride to 10mL oleylamine, pass through argon protection gas, control the temperature at 100°C, and stir rapidly for 20 minutes to make cuprous iodide and antimony chloride Completely dissolve to obtain a complex solution of metal salt;
[0021] (2) Add 11mL, 1mol / L diphenylthiourea diphenyl ether solution to the above metal salt solution, heat to the set temperature of 180°C and react for 120 minutes;
[0022] (3) After the reaction, cool to room temperature, add a large amount of methanol to react the Cu 3 Sb 4 Nanocrystals are cleaned to obtain Cu 3 Sb 4 nanocrystalline material.
[0023] This embodiment prepares Cu 3 Sb 4 The particle size of the nanocrystalline material is 5.95nm, and its TEM image is shown in figure 2 in a.
Embodiment 2
[0025] Cu 3 Sb 4 The controllable preparation method of nanocrystalline material comprises the following steps:
[0026] (1) Add 3mmol cuprous iodide and 1mmol antimony chloride to 10mL oleylamine, pass through argon protection gas, control the temperature at 80°C, and stir rapidly for 10 minutes to make cuprous iodide and antimony chloride Completely dissolve to obtain a complex solution of metal salt;
[0027] (2) Add 9mL, 1mol / L diphenylthiourea diphenyl ether solution to the above metal salt solution, heat to the set temperature of 120°C and react for 60 minutes;
[0028] (3) After the reaction, cool to room temperature, add a large amount of methanol to react the Cu 3 Sb 4 Nanocrystals are cleaned to obtain Cu 3 Sb 4 nanocrystalline material.
[0029] This embodiment prepares Cu 3 Sb 4 The particle size of the nanocrystalline material is 4.81nm, and its TEM image is shown in image 3 in a.
Embodiment 3
[0031] Cu 3 Sb 4 The controllable preparation method of nanocrystalline material comprises the following steps:
[0032] (1) Add 3mmol cuprous iodide and 1mmol antimony chloride to 10mL oleylamine, pass through argon protection gas, control the temperature at 60°C, and stir rapidly for 5 minutes to make cuprous iodide and antimony chloride Completely dissolve to obtain a complex solution of metal salt;
[0033] (2) Add 7mL, 1mol / L diphenylthiourea solution in diphenyl ether to the above metal salt solution, heat to the set temperature of 60°C and react for 1 minute;
[0034] (3) After the reaction, cool to room temperature, add a large amount of methanol to react the Cu 3 Sb 4 Nanocrystals are cleaned to obtain Cu 3 Sb 4 nanocrystalline material.
[0035] This embodiment prepares Cu 3 Sb 4 The particle size of the nanocrystalline material is 3.37nm, and its TEM image is shown in Figure 4 in a.
[0036] Cu prepared by the present invention 3 Sb 4 For the XRD spect...
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