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We studied the surface reaction between metallic In and a single-crystal GaAs substrate at 400–600 °C induced by the improved sessile drop method. Studying the surface morphology and microstructure using scanning electron microscopy, we found that many large particles had formed on the GaAs substrate, indicating a violent reaction between the In and GaAs. This reaction became more violent with increasing temperature. Characterizing the generated phases by X-ray diffraction and transmission electron microscopy, we identified the particles as InxGa1−xAs compounds. Our results show that indium (In) reacted with single-crystal GaAs through this method to form InxGa1−xAs compounds. Moreover, during the synthesis of InxGa1−xAs by the sessile drop method, the molten In and GaAs exhibited wettability at 400–600 °C. This experiment lays the foundation for synthesizing InxGa1−xAs compounds only using the metal In and GaAs substrate by a simple method.