Tungsten oxide nanoparticles were synthesized via a sol-gel route using metallic tungsten as precursor, and were printed on a flexible electrode using inkjet printing in order to build solid-state electrochromic cells. Several spectroscopic techniques were used to characterize and compare tungsten oxide particles obtained from different origins. FTIR, Raman and X-ray diffraction spectroscopic measurements showed that the sol-gel synthesis described here produces nanoparticles mainly in an amorphous state with hexagonal crystalline domains and allowed the analysis of the hydration extent of those nanoparticles. The size was measured combining dynamic light scattering, sedimentation, and microscopic techniques (AFM), showing a consistent size of about 200 nm. The tungsten oxide nanoparticles were used to produce an ink formulation for application in inkjet printing. Solid-state electrochromic devices were assembled at room temperature, without sintering the tungsten oxide printed films, showing excellent contrast between on/off states. Electrochemical characterization of those films is described using cyclic voltammetry. The devices were then tested through spectroelectrochemistry by Visible/NIR absorption spectroscopy (400-2200 nm range), showing a dual spectroscopic response depending on the applied voltage. This phenomenon is attributed to the presence of two different crystalline states in accordance with results obtained from the spectroscopic characterization of the nanoparticles. The electrochromic cells had a good cycling stability showing high reversibility and a cyclability up to more than 50,000 cycles with a degradation of 25%.
© 2012 American Chemical Society