1：Experimental Design and Method Selection:

The study involved synthesizing Cu3SbSe4 nanocrystals via hot injection methods (single and double injection) to achieve phase purity and monodispersity. Thin films were deposited using a dip-coating technique with ligand exchange to improve electronic properties. The experimental design focused on controlling synthetic conditions, surface modification, and film deposition to study material properties under ambient conditions.

2：Sample Selection and Data Sources:

Nanocrystals were synthesized from precursors including CuCl2, SbCl3, Se powder, oleylamine (OLA), and dodecanethiol (DDT). Thin films were deposited on glass substrates. Data sources included characterization techniques like XRD, TEM, XPS, and Hall measurements.

3：List of Experimental Equipment and Materials:

Equipment included Bruker D8 X-ray diffractometer, JEOL JEM 1400 and JEM2100F TEM, Ecopia HMS-3000 Hall Effect Measurement System, Bruker DektakXT contact profilometer, JEOL JSM-6500F SEM, Nicolet 380 FTIR spectrometer, and Physical Electronics ESCA 5800 XPS system. Materials included chemicals from Sigma-Aldrich, Strem Chemical, and Fisher Scientific.

4：Experimental Procedures and Operational Workflow:

Synthesis involved degassing precursors under vacuum, heating under N2, and injecting reactants to form nanocrystals. Ligand exchange was performed by dipping films in solutions of exchanging ligands (e.g., Na2S, EDA) and acetonitrile. Films were characterized immediately after deposition and over time under ambient conditions. Hall measurements were conducted at regular intervals to monitor electronic properties.

5：Data Analysis Methods:

XRD data were analyzed with Rietveld refinements using GSAS/EXPGUI. XPS data were fitted using the Shirley method and shifted to adventitious carbon. Hall data were corrected for film thickness. Statistical analysis included monitoring conductivity, carrier concentration, and mobility over time.