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采用水热法,以CuCl·22H2O、Zn(Ac)·22H2O、SnCl·45H2O作金属源,硫脲作硫源,在乙二胺和去离子水混合溶液中合成亚稳态正交相CZTS颗粒。利用XRD、Raman、SEM、TEM、EDS、UV-Vis吸收光谱探讨了乙二胺与去离子水比例对产物相结构、形貌、原子比以及光学性能的影响。结果表明:随着体系中乙二胺与去离子水比例的增加,所得CZTS颗粒相结构由锌黄锡矿逐渐转变为亚稳态正交相;颗粒形貌、化学计量比、光学性能也发生明显变化;当体系中乙二胺与去离子水比例为1∶1时,合成的颗粒为纯相亚稳态正交相结构、结晶性较好、颗粒形貌为不规则立方体、原子比1.7∶1.1∶1∶4、光学带隙1.53eV,与太阳能电池所需的最佳带隙接近。最后,还发现在充满S气氛中,450℃条件下退火处理1h,可实现亚稳态正交相向锌黄锡矿结构转变。
Hydrothermal method was used to synthesize metastable phase CZTS particles with CuCl · 22H2O, Zn (Ac) · 22H2O and SnCl · 45H2O as metal sources and thiourea as sulfur source in a mixed solution of ethylenediamine and deionized water . The effects of the ratio of ethylenediamine to deionized water on the phase structure, morphology, atomic ratio and optical properties were investigated by XRD, Raman, SEM, TEM, EDS and UV-Vis absorption spectra. The results show that with the increase of the ratio of ethylenediamine to deionized water, the phase structure of the obtained CZTS particles gradually changes from zinc yellow tin ore to metastable quadrature phase. The particle morphology, stoichiometry and optical properties also occur When the ratio of ethylenediamine to deionized water is 1: 1, the synthesized particles are pure phase metastable phase with good crystallinity and irregular particle morphology with the atomic ratio of 1.7 : 1.1: 1: 4, optical bandgap 1.53 eV, which is close to the best bandgap required for solar cells. Finally, it was found that the transformation of the metastable orthorhombic phase to the kesterite structure can be achieved by annealing at 450 ℃ for 1h in an atmosphere full of S.