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<p>Nanoparticle-derived Cu<sub>2</sub>ZnSn(S, Se)<sub>4</sub> (CZTSSe) thin films provide a scalable non-vacuum route for kesterite absorber fabrication, but converting a porous colloidal compact into a dense, large-grained absorber remains a coupled reaction–sintering challenge. In this study, Cu<sub>2</sub>ZnSnS<sub>4</sub> (CZTS) nanoparticle green films prepared by a direct heating-up colloidal route were converted into CZTSSe films by confined Se-vapor selenization. Rather than treating N<sub>2</sub> rapid thermal annealing as a rigorous one-variable control for pressure, this work focuses on clarifying the time-dependent conversion mechanism of a constrained nanoparticle compact under Se-containing conditions. SEM, XRD, Raman spectroscopy, EDS, HR-TEM, and SAED analyses reveal that selenization proceeds through spatially non-uniform Se transport, recrystallization, and grain growth, producing a characteristic bilayer microstructure composed of a large-grained upper layer and a fine-grained lower layer. Short selenization times lead to rapid Se uptake but incomplete phase development and secondary/intermediate phases, whereas selenization at 500&#xa0;°C for 25&#xa0;min provides the most balanced phase formation, crystallinity, and surface compactness among the examined conditions. Based on the time-dependent structural and microstructural evolution, a three-stage chalcogenization–sintering mechanism is proposed: Se-assisted CZTSSe recrystallization, transient liquid-phase-assisted sintering, and final solid-state coarsening. Optical and electrical measurements are discussed as supporting indicators of Se incorporation and microstructure-dependent transport, rather than as independent proof of a pressure effect. These results establish a mechanistic framework for understanding vapor transport, reaction, bilayer formation, and sintering in nanoparticle-derived kesterite absorber films.</p>

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Confined Se-vapor selenization of nanoparticle-derived CZTS thin films: coupled chalcogenization–sintering and bilayer microstructure evolution

  • 期刊论文

  • 发表日期：

    2026年7月30日

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  • Hsiang-Hua Pan,
  • Hsing-I. Hsiang

摘要

Nanoparticle-derived Cu2ZnSn(S, Se)4 (CZTSSe) thin films provide a scalable non-vacuum route for kesterite absorber fabrication, but converting a porous colloidal compact into a dense, large-grained absorber remains a coupled reaction–sintering challenge. In this study, Cu2ZnSnS4 (CZTS) nanoparticle green films prepared by a direct heating-up colloidal route were converted into CZTSSe films by confined Se-vapor selenization. Rather than treating N2 rapid thermal annealing as a rigorous one-variable control for pressure, this work focuses on clarifying the time-dependent conversion mechanism of a constrained nanoparticle compact under Se-containing conditions. SEM, XRD, Raman spectroscopy, EDS, HR-TEM, and SAED analyses reveal that selenization proceeds through spatially non-uniform Se transport, recrystallization, and grain growth, producing a characteristic bilayer microstructure composed of a large-grained upper layer and a fine-grained lower layer. Short selenization times lead to rapid Se uptake but incomplete phase development and secondary/intermediate phases, whereas selenization at 500 °C for 25 min provides the most balanced phase formation, crystallinity, and surface compactness among the examined conditions. Based on the time-dependent structural and microstructural evolution, a three-stage chalcogenization–sintering mechanism is proposed: Se-assisted CZTSSe recrystallization, transient liquid-phase-assisted sintering, and final solid-state coarsening. Optical and electrical measurements are discussed as supporting indicators of Se incorporation and microstructure-dependent transport, rather than as independent proof of a pressure effect. These results establish a mechanistic framework for understanding vapor transport, reaction, bilayer formation, and sintering in nanoparticle-derived kesterite absorber films.