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Enhanced chlorine evolution from dimensionally stable anode by heterojunction with Ti and Bi based mixed metal oxide layers prepared from nanoparticle slurry before final annealing at 525 °C for 1 h. For preparation of outer heterojunction layers, three different types of precursor were prepared as follows. A) P90 TiO2 (Evonik Industries) and Bi2O3 particles separately ball- milled (Ultra Apex mill) in ethanol to have particle size range of 80–100 nm and 1–2 μm, respectively. The TiO2 nanoparticles (3.8 wt%) were dispersed in ethanol/terpineol (16:19 wt%) solution with added ethyl cellulose binder (2.2 wt%). Bi2O3 micro-particles were added with variable Bi to Ti ratios (0:10, 1:9, and 3:7). B) 6 mL titanium butoxide was added to 150 mL ethylene glycol to be stirred for 8 h in room temperature. The mixture was poured into 510 mL acetone and 8 mL of deionized (DI) water was added before vigorous stirring for 1 h. Resulting precipitate was collected using a centrifuge (6000 rpm for 4 min), washed with ethanol 5 times, and re-dispersed in ethanol with a given concentration of bismuth citrate. C) titanium tetraisopropoxide (1.25 mL) in ethanol (25 mL) was added to 8 mM Bi(NO3)3 solution (pH 1.5 adjusted by acetic acid) by dropwise and the mixture was stirred overnight. Resulting precipitate was collected (11000 rpm for 10 min), washed with DI water 5 times, and re-dispersed in DI water. These precursors were sprayed on the IrTaOy layer and annealed at 450 °C for 30 min and the coating procedure was performed for 3 times. In this study, heterojunction anodes from precursor A were denoted as (Bi2O3)x(TiO2)1−x (x = 0, 0.1, and 0.3), while the outer layers with low mass loading (L) were prepared without repetition to compare the performance with analogues with high mass loading (H). The anodes from precursor B and C with nominal Bi to Ti ratio of 3:7 were named as Bi3Ti7Ox-1 and Bi3Ti7Ox-2, respectively, to describe greater mixing level of Bi. The surface morphologies were observed by using a ZEISS 1550VP field emission scanning electron microscope (SEM) and elemental compositions were estimated using an Oxford X-Max SDD X-ray energy- dispersive spectrometer (EDS) system. The EDS analysis was performed either in a point-and-identification mode for 10 arbitrary sites or in mapping mode. The surface crystallography was assessed by X-ray diffraction (XRD) using an X’pert MD (Panalytical) diffractometer with Cu−K radiation. 2.2. Electroanalysis. The electrochemical activities of (Bi2O3)x(TiO2)1−x and Bi3Ti7Ox-1/2 heterojunction anodes were assessed using linear sweep voltammetry (LSV) and cyclic voltammetry (CV). In a single compartment cell (working volume = 60 mL), each anode was parallel matched with AISI 304 stainless steel cathode (distance = 5 mm) with active geometric surface area of 3 × 2 cm2. Ag/AgCl/sat. KCl reference electrode (BASI Inc.) was located 3 mm away from the anode center. The three electrodes configuration was connected to a potentiostat (SP-50, Bio-Logic) to control anodic potential (Ea) in normal hydrogen electrode (NHE) scale (Ea (NHE) = Ea (Ag/AgCl) + 0.197 V). The CV and LSV data were recorded with Ea ranges of 0.2–1.0 V NHE (scan rate of 20 mV s−1) and of 0.8–2.0 V NHE (scan rate of 5 mV s−1), respectively. Before all electrochemical experiments, open circuit potentials were measured for 30 min and ohmic resistances were measured by current interruption method at 200 mA current bias. 2.3. Potentiostatic Electrolysis. The efficiency of RCS generation was evaluated during potentiostatic electrolysis of 50 mM NaCl solutions at variable Ea values (2.0, 2.5, and 3.0 V NHE). The evolution of [RCS] was measured by DPD (N, N- diethyl-p-phenylenediamine) reagents 3 times at 2 min intervals and, during this period, further oxidation of RCS to ClO3− or ClO4− could be negligible [15]. The specific rate (SR), current (CE) and energy efficiency (EE) of the RCS generation were estimated by the following equations (Eqs. (7)–(9)). https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7539370/?report=printable[10/12/2020 8:49:16 AM]PDF Image | Enhanced chlorine evolution
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