Novel organic–inorganic layer-by-layer (LbL) multilayers for visible-light phototropy, comprised of polyvinylpyrrolidone (PVP) and phosphomolybdic acid (PMoA), were fabricated via layer-by-layer (LbL) assembly with ultrasonic pretreatment. The characterizations revealed that the Keggin spatial geometry of the PMoA was still maintained in the final ultrasonic-assisted LbL thin films, which promoted halogenesis between the PVP and PMoA. Intriguingly, instead of destroying the PVP thin film, the ultrasonic pretreatment process successfully dispersed the PMoA in the PVP thin film with a median size of approximately 3.6 nm. Thanks to the dispersion of the PMoA particles, the photochromic capabilities of the ultrasonic-assisted PVP/PMoA LbL thin films gained remarkable improvement. Moreover, decreasing the size of the PMoA particles to quantum dots (10–3.4 nm) induces an up-conversion and dielectric confinement effect, which increases the intensity of the absorption peak (0.235 increased to 0.45) while narrowing the emission energy (2.51 eV narrowed to 2.23 eV). At the same time, the size reduction also extended the range of the absorption wavelength, increases the characteristic absorption intensity, and accelerates the coloration rate over the same illumination period.
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