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%.
Vanadium oxide gel was synthesized and formulated for the assembly of solid-state electrochromic cells on flexible and transparent electrodes using inkjet printing. FTIR, Raman, and X-ray diffraction spectroscopic measurements showed that the vanadium oxide gel here synthesized consisted of V(2)O(5)·6H(2)O, microstructures similar to orthorhombic V(2)O(5), while Raman spectroscopy also shows the presence of amorphous domains. Atomic force microscopy (AFM) images of the thin films printed using an inkjet shows a ribbonlike structure, which is in accordance with previous results of the vanadium oxide gels in solution. Solid-state electrochromic devices were assembled at room temperature using the inkjet printed films, without any sinterization step. The electrochemical properties of the vanadium oxide gel were characterized by cyclic voltammetry and spectroelectrochemistry by visible/NIR absorption spectroscopy (in both liquid and solid-state). Several redox steps are observed, which gives rise to a variety of color transitions as a function of the applied voltage. The different optical properties of the vanadium oxide gel are assigned to different intercalation steps of Li(+), leading to different crystalline phases of the gel. The final result is a solid-state electrochromic cell showing excellent contrast between the redox states, giving rise to colors such as yellow, green, or blue. Color space analysis was used to characterize the electrochromic transitions, and while absorption spectra showed rather long switching times (up to 100 s), in L*a*b* color space coordinates, the switching time is smaller than 30 s. These electrochromic cells also have an excellent cycling stability showing high reversibility and a cyclability up to more than 30,000 cycles with a degradation of 18%.
Conventional aerobic nitrification was adversely affected by single pulse inputs of six different classes of industrially relevant chemical toxins: an electrophilic solvent (1-chloro-2,4-dinitrobenzene, CDNB), a heavy metal (cadmium), a hydrophobic chemical (1-octanol), an uncoupling agent (2,4-dinitrophenol, DNP), alkaline pH, and cyanide in its weak metal complexed form. The concentrations of each chemical source that caused 1 5, 25, and 50% respiratory inhibition of a nitrifying mixed liquor during a short-term assay were used to shock sequencing batch reactors containing nitrifying conventional activated sludge. The reactors were monitored for recovery over a period of 30 days or less. All shock conditions inhibited nitrification, but to different degrees. The nitrate generation rate (NGR) of the shocked reactors recovered overtime to control reactor levels and showed that it was a more sensitive indicator of nitrification inhibition than both initial respirometric tests conducted on unexposed biomass and effluent nitrogen species analyses. CDNB had the most severe impact on nitrification, followed by alkaline pH 11, cadmium, cyanide, octanol, and DNP. Based on effluent data, cadmium and octanol primarily inhibited ammonia-oxidizing bacteria (AOB) while CDNB, pH 11,and cyanide inhibited both AOB and nitrite-oxidizing bacteria (NOB). DNP initially inhibited nitrification but quickly increased the NGR relative to the control and stimulated nitrification after several days in a manner reflective of oxidative uncoupling. The shocked mixed liquor showed trends toward recovery from inhibition for all chemicals tested, but in some cases this reversion was slow. These results contribute to our broader effort to identify relationships between chemical sources and the process effects they induce in activated sludge treatment systems.
The effects of shock loads of 1‐chloro‐2,4‐dinitrobenzene (CDNB); cadmium; 1‐octanol; 2,4‐dinitrophenol (DNP); weakly complexed cyanide; pH 5, 9, and 11; and high ammonia levels on activated sludge biomass growth, respiration rate, flocculation, chemical oxygen demand removal, dewaterability, and settleability were studied. For all chemical shocks, except ammonia and pH, concentrations that caused 15, 25, and 50% respiration inhibition were used to provide a single pulse shock to sequencing batch reactor systems containing a nitrifying or non‐nitrifying biomass. Cadmium and pH 11 shocks were most detrimental to all processes, followed by CDNB. The DNP and cyanide primarily affected respiration, while pH 5, pH 9, octanol, and ammonia did not affect the treatment process to a significant extent. A chemical source–process effect matrix is provided, which we believe will aid in the development of methods that prevent and/or attenuate the effects of toxic shock loads on activated sludge systems.
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