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In polycrystalline compound semiconductor thin lms, structural defects such as grain boundaries as well as lateral stress can form during lm growth, which may deteriorate their electronic performance and mechanical stability. In Cu-based chalcogenide semiconductors such as Cu(In,Ga)Se2 or Cu2ZnSn(S,Se)4, temporary Cu excess during lm growth leads to improved microstructure such as a reduced grain boundary density, a strategy that has been used for decades for high-e ciency chalcopyrite thin lm solar cells. However, the mechanisms responsible for the bene cial e ect of Cu-excess are yet not fully clari ed. Here, we investigate the evolution of lateral stress, grain growth and Cu-Se segregation during Cu-Se deposition onto Cu-poor CuInSe2. Real-time x-ray di raction and uorescence analysis with a double-detector setup reveals that sudden stress relaxation occurs shortly prior to Cu-Se segregation at the surface and precisely coincides with domain growth and change of texture. Numerical reaction-di usion modeling provides an explanation for the observed delay of Cu-Se segregation. Our results show that partial recrystallization of the lm can be already reached without the necessity of an overall Cu-rich lm composition and thus suggest a new synthesis route for the fabrication of high-quality chalcopyrite absorber lms.

Sudden stress relaxation in compound semiconductor thin films triggered by secondary phase segregation