Highly (001)‐oriented thin films of 4‐(N,N‐dimethylamino)‐3‐acetamidonitrobenzene were prepared on a thermally oxidized silicon substrate using vapor deposition. The degree of (001) orientation depends considerably on the substrate temperature (Ts) and deposition rate (R), which determines the kinetic energy (Ek) of the molecules in a flux. Under the optimized experimental parameters of Ts=30 °C and R=600 nm/min, we fabricated the (001)‐oriented thin film showing the full width at half‐maximum of x‐ray rocking curve of 1.6°. Surface flatness was also improved as the deposition rate increased. It became clear that kinetic energy (Ek) of the molecules in an evaporating flux strongly promoted (001) preferred orientation as could be seen by observing the surface morphology and a cross‐sectional view of the samples at their initial stage of growth.

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