| Summary: | Nanoscale tungsten bronze can convert near-infrared light into thermal energy. For a chemical synthesis, intermediate products and processes are potentially positive or negative to an end product. In this study, (NH<sub>4</sub>)<sub>2</sub>SO<sub>4</sub> was added into the hydrothermal system of WO<sub>3</sub>, CsCl, CH<sub>3</sub>CH<sub>2</sub>CHO, and NH<sub>3</sub>·H<sub>2</sub>O to increase the Cs/W ratio in solution. An intermediate, Cs<sub>1.1</sub>W<sub>1.65</sub>O<sub>5.5</sub>, was isolated. Subsequently, it was confirmed via a kinetics experiment conducted for different times. The results of the NH<sub>3</sub>·H<sub>2</sub>O and NH<sub>4</sub>COOCH<sub>3</sub> system indicate there are two influence factors that influence the formation of Cs<sub>1.1</sub>W<sub>1.65</sub>O<sub>5.5</sub>: the leaching out of W and imine reactions. A low leaching out rate induces a high Cs/W ratio and low-concentration W in solution, leading to the formation of Cs<sub>1.1</sub>W<sub>1.65</sub>O<sub>5.5</sub>. The imine reaction decreasing CH<sub>3</sub>CH<sub>2</sub>CHO restrains the reduction in Cs<sub>1.1</sub>W<sub>1.65</sub>O<sub>5.5</sub>. The increase in CH<sub>3</sub>CH<sub>2</sub>COO<sup>−</sup> with the reduction reaction results in both the micron-size sticks and nano-size equiaxial particles in powder.
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