Polymeric Precursor Method Research Articles

Electric Properties Change during Morphological Evolution of CeO2 Nanostructures: Synergy between Bulk and Surface Defects.

CeO2 samples were synthesized via the polymeric precursor method at different calcination temperatures. Electric properties were investigated using positron annihilation lifetime spectroscopy, electron paramagnetic resonance spectroscopy, and complex impedance spectroscopy. Reduction in the specific surface area of the particles with increasing calcination temperature along with morphological changes were observed. PALS depicted doubly ionized oxygen vacancies surrounded by two Ce3+ atoms, while the EPR spectroscopy showed a singly ionized oxygen vacancy surrounded by Ce3+ and Ce4+ ions. Impedance measurements unraveled the presence of polarons, while thermal treatments led to a lower electrical conductance, as the calcination temperature increased.

TMAB modified NiFe2O4 nanoparticles for the Effective removal of Eriochrome Black-T azo dye

The Eriochrome Black-T (EBT) azo dye was removed from aqueous solution using TMAB (tetramethyl ammonium bromide) stabilised NiFe2O4 (TMAB@NFO) nanoparticles, which have been synthesized through polymeric precursor method. X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared spectra (FTIR) were used to analyse the TMAB@NFO nanoparticles. Adsorption studies were conducted under a variety of conditions, including pH, adsorbent dosage, and contact time, intraparticle diffusion, pseudo-first- and pseudo-second-order kinetic models were used to analyse the kinetic data. According to the systematic study of adsorption isotherms and kinetics models, TMAB@NFO nanoparticles will adsorb EBT dye utilising the Freundlich model and pseudo-second-order kinetics. The intraparticle diffusion model revealed a linear relationship (R2 - 0.98, 0.97, and 0.94 for TMAB@NiFe2O4 and bare NiFe2O4-NPs), demonstrating how surface modification influences the overall EBT adsorption process and the pore diffusion rate. Additionally, the manufactured nano adsorbents of NiFe2O4 were effectively regenerated and reused after the treatments up to four times following the elimination of 89% of EBT dye by TMAB@NiFe2O4-NPs. The results have demonstrated the enormous potential of TMAB @NiFe2O4-NPs to eliminate EBT in a practical way. KEY WORDS: Tetramethyl ammonium bromide, NiFe2O4, EBT, Surface capping, Adsorption, Kinetics Bull. Chem. Soc. Ethiop. 2024, 38(6), 1569-1581. DOI: https://dx.doi.org/10.4314/bcse.v38i6.6

Characterization of SnO2-based gas sensors to analyze diesel and biodiesel blends

This study analyzed biodiesel blends using sensors constituted by SnO2 pellets with gold interdigitated contacts deposited on the surface. Tin dioxide was synthesized by the polymeric precursor method with further calcination treatment at 500°C, conformed and sintered at three temperatures to form three different samples: 700°C (Sn1), 900°C (Sn2) and 1100°C (Sn3). The samples were analyzed by X-Ray Diffraction, FEG-SEM (Field Emission Gun - Scanning Electron Microscopy), Raman spectroscopy, and electrical measurements. Results confirmed the formation of rutile-type tetragonal cassiterite phase, with quasi-spherical particles a moderate degree of heterogeneity in particle size 30-90 nm). Raman vibrational modes and infrared spectrum also confirmed the presence of tin oxide in high purity rutile phase. Sensorial measurements showed high sensitivity, response, and recovery time in tests with biodiesel/ethanol mixtures, allowing to distinguish between blends with a wide range of composition and serving as a potential device to detect adulterated fuel.

Polymer precursor method for the synthesis of zinc oxide nanoparticles: A novel approach

This study presents a novel approach to synthesize zinc oxide (ZnO) nanoparticles using a polymer precursor method, offering precise control over particle size in the nanometer scale. Zinc oxide nanoparticles are of significant interest due to their wide-ranging applications in various fields such as solar cells, gas sensors, photocatalysts, and nanomedicines. The synthesized nanoparticles were thoroughly characterized using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Fourier Transform Infrared spectroscopy (FTIR). The distinct hexagonal form detected in the XRD pattern, featuring characteristic reflection planes at angles of 31.72° (100), 34.39° (002), 36.23° (101), and 47.44° (102), signifies the synthesis of ZnO possessing a hexagonal wurtzite structure. The SEM and TEM images revealed uniformly spherical particles with an average size ranging from 35 to 40 nm. Such uniform morphology and size distribution are critical for ensuring consistent performance in applications such as gas sensing and catalysis. Additionally, the FTIR spectra indicated a reduction in impurities after the synthesis process, highlighting the effectiveness of the polymer precursor method in producing high-quality ZnO nanoparticles. Heating the ZnO precursor material at 400°C for 2 hours significantly reduces impurities, suggesting conversion to ZnO nanoparticles.

Influence of cobalt doping on structural, optical, and electrical properties of zinc oxide nanoparticles prepared by polymeric precursor method

Cobalt-doped ZnO nanoparticles at different compositions have been obtained by the polymeric precursor method. The nanoparticles were obtained at the working pH from 8.3 to 8.5 and synthesized at 550 °C. The properties were studied using X-ray diffraction (XRD), vibrational spectroscopy (FTIR/Raman), diffuse reflectance absorbance spectroscopy (DR UV–Vis), photoluminescence spectroscopy (PL), scanning electron microscopy (SEM/EDS), and impedance spectroscopy. The lattice parameters were determined at room temperature by Rietveld refinement, confirming single-phase composition with a hexagonal wurtzite structure. FTIR and Raman analyzes identified the characteristic vibrations of the synthesized system and the typical deformations of the wurtzite-type hexagonal structure, corroborating the results obtained from XRD. A redshift in the optical energy band gap (Egopt) was observed with increasing cobalt content compared to the ZnO sample. Considering the doping percentage, Egopt value varied between 3.13 eV and 3.04 eV for pure ZnO and Co-doped ZnO with 5 at. %., indicating that the optical properties of the nanoparticles were affected by dopant concentration. PL and SEM/EDS characterization were used to determine the associated defects for each sample and the morphology and composition of the nanoparticles. PL results showed a strong blue emission at around 439 nm (2.83 eV), which is redshift with cobalt content (ΔE between 0.05 eV and 0.01 eV), attributed to the surface defects present in the doped samples. Conductivity analysis to temperature revealed a semiconductor behavior for all samples, and their respective activation energies determined. The results provide an easy method to obtain Co-doped ZnO nanoparticles with interesting properties for optoelectronics devices.

Unveiling the magnetic and optical properties of barium bismuthate thin films with distinct Ba/Bi ratios

This research aims to investigate the optical and magnetic properties of BaBiO3 (80:20), BaBiO3 (50:50), and BaBiO3 (30:70) thin films obtained by the polymeric precursor method. For better sample designations, the following codes were employed: (80:20) (BBO82), (50:50) (BBO55), and (30:70) (BBO37). The observed properties for barium bismuthates thin films were elucidated in terms of bismuth and oxygen vacancies as well as grain morphology, which can be controlled by stoichiometric changes (Ba/Bi ratios). According to the x-ray results the films crystallize in a rhombohedral BaBiO3 structure with an R-3R space group without any secondary phase as confirmed by Rietveld analyses. According to the photoluminescence results, x-ray photoelectron spectroscopy measurements as well as the law of approach to saturation (LAS), there are a significant presence of oxygen vacancies and vacancy clusters [BiO5.Vo.] in the films with high proportion of bismuth. The optical and magnetic properties developed by these films are originated from the following factors: tilting of BiO6 clusters which changes the length and angle of Bi–O–Bi bonds, creating a magnetic field responsible for the distinct Mr/Ms ratios, the formation of bipolarons caused by charge transfer between [BiO6] and [BiO5. Vo⋅] due to the oxygen vacancies formation, plate-like morphology which makes the domains easier to be switched under an applied external field resulting in a superparamagnetic behavior, charge disproportionation of various valence states (Bi+3 and Bi+5). Based on these results, new potential devices can emerge as possible tools to be applied in switches, actuators, spintronics, magnetic field sensors, etc.

Preparing conductive polymer-based adsorbent with better cupric ion adsorption efficiency by monomer precursor cross-linking method

Abstract Conductive polymer-based adsorbents have showed excellent heavy metal ion removing capabilities. Crosslinking modification is one of the feasible methods to further improve their properties. To make use of the advantages of monomer precursor method over the polymer precursor method in forming dense interpenetrating networks, and then optimizing the surface structure of materials and providing more adsorption sites, the mesoporous cross-linked poly-o-phenylenediamine (M-CR-PoPD) prepared by using the former one and used in removing Cu2+ from aqueous solution. The FTIR results showed that the monomer was successfully crosslinked and polymerized. The loosely packed target product with a hierarchical pore structure distribution was successfully formed. The maximum adsorption capacity of 105.18 mg g−1 was obtained at 25 °C after 3 h of adsorption when M-CR-PoPD prepared at the reaction time of 6 h using anhydrous ethanol as solvent and trimethylolpropane-tris(3-aziridinyl) propionate as crosslinking agent. This value reached the optimum Cu2+ removal capability of reported PoPD-based adsorbents. According to EDX, FTIR, and XPS data before and after adsorption, the possible adsorption mechanism based on the cation-π interaction and the formation of Cu–N bonds was proposed. These results could help develop more effective conductive polymer-based adsorbents to remove Cu2+ from wastewater.

Improved relaxor ferroelectrics and energy storage performance of polycrystalline Ba0.95Sr0.05Ti2O5 ceramics modified with La dopants

Lead-free relaxor ferroelectrics are useful in energy storage applications. In particular, BaTi2O5-based dielectric materials may have great potential for such applications. In this study, polycrystalline Ba0.95Sr0.05Ti2O5-xLa (BST2-xLa) ceramics were synthesized using a standard solid-state reaction method with as-prepared nanoparticles prepared via a modified Pechini polymeric precursor method. The structural and electrical properties of the BST2-xLa ceramics were systematically investigated using a series of measurements. The phase analysis results confirm that La3+ is a donor dopant that replaced Ba2+ sites in the structure, which results in a decrease in oxygen vacancies to maintain charge neutrality. The intrinsic electronic conduction mechanism for electrical conductivity was evaluated from the fitted activation energy based on the Arrhenius equation. The relaxor ferroelectric behaviour and energy storage density and efficiency are improved by the addition of a small amount of lanthanum (<3.6 mol%) because of the charge and ionic radius mismatch in the structure. These results suggest that lanthanum can effectively optimise the relaxor ferroelectrics of BST2-xLa ceramics, which have promising potential as energy storage materials.

Deciphering fast lithium storage kinetics via R-based self-derivation effects in siloxanes

Silicon oxycarbide (SiOC) is regarded as a promising anode material for lithium-ion batteries. However, the effect of SiOC's structural composition on lithium-ion storage behaviors, especially the controllable introduction of free carbon (Cfree) and its influence on electrochemical performance, remains a critical challenge that needs to be solved. In this study, based on our finding that the R-based functional group (composed exclusively of carbon and hydrogen atoms) in R-based triethoxysilane can be derived to carbon radicals through thermal decomposition, and then generates Cfree phases into SiOC, we propose a novel concept of R-based self-derivation effects in siloxanes to achieve controlled Cfree introduction for the SiOC anode material. SiOC spheres with tailored structural compositions and Cfree contents are subsequently prepared using a facile and scalable polymeric precursor method, and the effect of Cfree of SiOC spheres on lithium-ion storage performance is studied in combination with density functional theory calculations, revealing that higher Cfree content significantly enhances the lithium-ion storage kinetics of SiOC anode via constructing ion/electron migration “highways”. Notably, SiOC with a high Cfree content up to 37.5 wt% displays excellent lithium-ion storage capability, with a theoretical storage capacity of up to 1004 mAh g−1 and achieving a high reversible capacity of 453 mAh g−1 after 200 cycles at 0.5 A g−1.

Engineering Er-doped ZnO nanocrystals for As-removal: Targeting water remediation

Erbium-doped zinc oxide nanocrystals (Zn1−xErxO) produced by the polymeric precursor method are the subject of a comprehensive study in this report. Our results indicate that only the wurtzite ZnO phase is produced up to x = 0.050. After that (x > 0.050), a mixed system with a secondary phase (Er2O3) is found. The lower solubility limit of erbium in the ZnO crystal lattice is correlated with the higher ionic radii of Er3+-ions compared to Zn2+-ions, impacting remarkably the solid solution limit. Magnetic measurements show the coexistence of the two phases: paramagnetism (PM) related to Zn1−xErxO nanocrystals (free and short-range coupled Er3+-ions) and a weak ferromagnetic (FM) contribution assigned to the presence of bound magnetic polarons. UV–vis spectra show a transition from one to two excitonic peaks as the Er-content increases; the second peak related to the nucleation process of the secondary Er2O3 phase, which was successfully acknowledged using the Elliott’s model. Fourier transform infrared (FTIR) spectroscopy was used to characterize vibrational properties and the results are in agreement with the x-ray diffraction data analysis. To assess the efficiency of using the Zn1−xErxO samples to remove As(V) from contaminated water, a reference water solution containing 500 ppb As(V), at a neutral (pH = 7), was prepared to simulate drinking water. Our results show the effectiveness of As-removal. It was determined that the effectiveness is improved with the Er-content, reaching the limit imposed by World Health Organization. According to the linearity achieved while applying the pseudo-second-order-adsorption model, our findings strongly suggest that a chemisorption mechanism takes place between the Zn1−xErxO nanoparticle surface and As(V) in solution.

Tin Oxide Nanoparticles: A Review

Abstract: The aim of this review article is an overview of the tin oxide (SnO2) nanoparticles, and the literature addresses the existing research related to the various modifications and characterization of SnO2 nanoparticles with their physicochemical investigations. Among various metal-oxide nanoparticles, SnO2 nanoparticles are considered one of the potential candidates for electronic and electrical device fabrication, sensors, display devices, gas sensing, photovoltaic devices, LIBs (Lithium-ion batteries), photocatalysis and optoelectronic devices, supercapacitors, SnO2 nanowires would provide electrolyte channels for effective transport, catalyst, and anode materials. Apart from their technological supremacy, SnO2 nanoparticles have demonstrated their compatibility with human cervical cancer cells and have successfully achieved hyperthermia temperature when subjected to an alternating current magnetic field. Doping with some of the potential rare-earth dopants via various synthesis methods such as Chemical co-precipitation, sol-gel, polymeric precursor method, and nebulizer spray pyrolysis method is the major highlight of this review article. As per the requirement of the system, SnO2 nanoparticles can be tuned by size, shape, and functionality.

Nanoparticles of the Perovskite-Structure CaTiO3 System: The Synthesis, Characterization, and Evaluation of Its Photocatalytic Capacity to Degrade Emerging Pollutants.

In this research work, the photocatalytic capacity shown by the nanoparticles of the CaTiO3 system was evaluated to degrade two pollutants of emerging concern, namely methyl orange (MO)-considered an organic contaminating substance of the textile industry that is non-biodegradable when dissolved in water-and levofloxacin (LVF), an antibiotic widely used in the treatment of infectious diseases that is released mostly to the environment in its original chemical form. The synthesis process used to obtain these powders was the polymeric precursor method (Pechini), at a temperature of 700 °C for 6 h. The characterization of the obtained oxide nanoparticles of interest revealed the presence of a majority perovskite-type phase with an orthorhombic Pbnm structure and a minority rutile-type TiO2 phase, with a P42/mnm structure and a primary particle size <100nm. The adsorption-desorption isotherms of the synthesized solids had H3-type hysteresis loops, characteristic of mesoporous solids, with a BET surface area of 10.01m2/g. The Raman and FTIR spectroscopy results made it possible to identify the characteristic vibrations of the synthesized system and the characteristic deformations of the perovskite structure, reiterating the results obtained from the XRD analysis. Furthermore, a bandgap energy of ~3.4eV and characteristic emissions in the violet (437 nm/2.8 eV) and orange (611 nm/2.03 eV) were determined for excitation lengths of 250 nm and 325 nm, respectively, showing that these systems have a strong emission in the visible light region and allowing their use in photocatalytic activity to be potentialized. The powders obtained were studied for their photocatalytic capacity to degrade methyl orange (MO) and levofloxacin (LVF), dissolved in water. To quantify the coloring concentration, UV-visible spectroscopy was used considering the variation in the intensity of the characteristic of the greatest absorption, which correlated with the change in the concentration of the contaminant in the solution. The results showed that after irradiation with ultraviolet light, the degradation of the contaminants MO and LVF was 79.4% and 98.1% with concentrations of 5 g/L and 10 g/L, respectively.

Unveiling the polar properties on barium bismuthate perovskite thin films with distinct Ba/Bi ratios

This research aims to investigate the domain structure of BaBiO3 (80:20), BaBiO3 (50:50), and BaBiO3 (30:70) thin films obtained by the polymeric precursor method. For better sample designations, the following codes were employed: (80:20) (BBO82), (50:50) (BBO55), and (30:70) (BBO37). The piezo-ferroelectric coupled behavior observed for barium bismuthates thin films was elucidated in terms of bismuth and oxygen vacancies as well as grain morphology, which can be controlled by stoichiometric changes (Ba/Bi ratios). The films crystallize in a rhombohedral BaBiO3 structure with an R-3R space group without any deleterious secondary phase. Additionally, the hysteretic strain, dielectric, ferroelectric, and piezoelectric properties of BaBiO3 thin films are strongly dependent on the film texture. Sample BBO55 showed a distinguished preferred orientation along the (341) plane with a low associated coercive field (66.87 kV/cm), free of imprint and with no polarizations gap compared to samples BBO37 and BBO82. Sample BBO55 presented the highest piezoelectric (d33-eff ≈ 45.7 pm/V) and ferroelectric (Pr≈19.87 μC/cm2) responses. This behavior can be ascribed to a highly textured film, which generates less strain throughout the crystal lattice, facilitating the polarization switching mechanism and improving piezo/ferroelectricity. These findings are significant for developing novel, high-performance, lead-free piezoelectric materials to be applied in different electronic components such as magnetic field sensors, switches, actuators, and other types of memory devices.

Investigating laser sintering in Y3Al5O12 ceramics

This study investigates the experimental parameters of the laser sintering process of Y3Al5O12 ceramics. Ceramic powders were produced using the polymeric precursor method and sintered using a CO2 laser as the heating source. The samples were characterized using differential thermal analysis, thermogravimetric analysis, X-ray diffraction, and scanning electron microscopy techniques. The results showed that parameters such as powder calcination temperature, dwell time, and laser power density rate are crucial in obtaining dense ceramic bodies. Furthermore, developing and using a sample holder made of the same material composition to be sintered showed significant advances in the laser sintering process.

Structure, optical, colorimetric, and supercapacitor properties of anode α-CuWO4 crystals

In this work, alpha-copper tungstate (α-CuWO4) crystals were prepared by polymeric precursor method. The structural and optical data were performed by X-ray diffraction (XRD), Rietveld refinement, Fourier-transform infrared (FTIR), and ultraviolet–visible (UV–Vis) diffuse reflectance spectroscopies. Moreover, their colorimetric and supercapacitor properties were investigated. Pristine α-CuWO4 crystals present a triclinic structure, symmetric and antisymmetric stretch vibrations in the O–Cu–O and O–W–O bonds corresponding to IR-active modes and an optical bandgap value of 2.24 eV. Colorimetric results showed that the α-CuWO4 crystals exhibit a brown color to be employed in pigments coating floors. The α-CuWO4 crystals present a specific capacitance of 275.68F/g at 5 mV/s to be applied as a stable anodic electrode. These results suggest that α-CuWO4 is an excellent candidate as an electrode for energy storage devices in the next generation of batteries.

Magnetic heterostructures of NiFe2O4 and TiO2: Pechini synthesis, characterization and photocatalytic performance in arsenite oxidation

In this work, the aim was to synthesize photocatalysts containing NiFe2O4 and TiO2, forming heterostructures applied in the decontamination of As (III) in an aqueous medium. The photocatalysts were prepared using the polymeric precursor method and calcined at three temperatures (500, 700 and 900 °C). The synthesized samples presented different crystalline phases: NiFe2O4, α-Fe2O3, NiO, and the allotropic forms of TiO2 anatase and rutile. The band gap values for all the samples were lower than those reported in the literature for TiO2. The sample calcined at 700 °C showed the best performance in the photocatalytic removal of As (III), resulting in the removal of 97.5 % of its concentration after 80 min. Additionally, it was possible to achieve a magnetic recovery of the catalyst after each cycle, with a recovery rate exceeding 80 %. This can be associated with a higher nickel ferrite content in relation to α-Fe2O3 and NiO simple oxides, the presence of both TiO2 polymorphs (anatase and rutile) in considerable amounts, and a lower band gap energy value.

Investigation of supercapacitor properties using iron tungsten porous electrode in neutral aqueous electrolyte

Porous supercapacitors (SCs) materials are great interesting for energy storage systems. Electrolyte contributes to the enhancement of supercapacitor performance. In this paper, iron tungstate mixed oxides electrode was prepared by polymeric precursor method. The material was deposited onto conductor substrate by drop casting and annealed at 500 ºC for 2 h. The thermal, structural, and morphological characterizations were realized by differential scanning calorimetry (DSC), X-ray diffraction (XRD), micro-Raman, emission–scanning electron microscopy (FE-SEM), and atomic force microscopy (AFM), respectively. The crystallization process of polymeric resin occurred at 454 °C. The synergistic effect of monoclinic FeWO4 and monoclinic Fe2W3O12 phases was confirmed with Fe2+|Fe3+ of iron tungstate mixed oxides. An irregular shape of condensed spherical-like particles aggregated with rough and porous nanostructures was observed. Neutral electrolytes were employed in electrochemical measurement as lithium nitrate (LiNO3) and sodium sulfate (Na2SO4). SC electrochemical analyses of FeWO4|Fe2W3O12 electrode accomplishes a capacitance of 75 F g–1 at 5 mV s–1, energy density of 3.73 Wh kg–1, power density of 582.1 W kg−1and long-term electrochemical cycling with a capacity retention of 94.04% after 6000 cycles in 1.0 mol L−1 Na2SO4. Therefore, an iron tungstate-based electrode demonstrates a potential supercapacitor device with excellent stability in a nontoxic aqueous electrolyte.

LSF films formed on YSZ electrolytes via polymeric precursor deposition for solid oxide fuel cell anode applications

AbstractDifferent materials have been applied as anode in solid oxide fuel cell (SOFC). Perovskite structured materials are promising as an alternative electrode material to Ni. Here, we investigated perovskite‐structured mixed ionic and electronic conducting material, lanthanum strontium ferrite (LSF), which has typically been used as a cathode material. LSF has also shown potential for an anode in SOFC. LSF films with two different compositions, La0.6Sr0.4FeO3 (6LSF) and La0.8Sr0.2FeO3 (8LSF) were fabricated by a polymeric precursor method. The effects of the phase content, surface chemistry, and microstructure on the anode performance were investigated. It was found that a mixture of the Ruddlesden–Popper phase, SrCO3 phases, and rhombohedral perovskite exists in both cell structures. Both cells had Ruddlesden–Popper and SrCO3 phases at their surface, in addition to the rhombohedral perovskite. Symmetrical half‐cell measurements showed that the polarization resistance of 6LSF (0.34 Ω cm2) is lower than that of 8LSF (0.47 Ω cm2), mostly because of its highly porous microstructure as a result of slower A‐site diffusion rates induced by higher Sr content.The symmetrical 6LSF fuel and air electrodes exhibited ASRelectrode values of 0.34 and 0.14 Ω cm2, respectively, at 800 ˚C.

Surface modification of T-Nb2O5 with low-crystallinity Nb2O5 to enhance photocatalytic degradation of rhodamine B

This work demonstrates the obtainment of an orthorhombic Nb2O5 (T) heterostructure synthesized by the polymeric precursor method coated with low-crystallinity Nb2O5 synthesized by the microwave-assisted hydrothermal method. The sample was submitted to the photocatalytic degradation test using Rhodamine B (RhB) dye decolorization under UVC irradiation for 60 min. The heterostructure sample demonstrated a significant enhancement in photocatalytic performance as compared to orthorhombic Nb2O5, achieving complete degradation of RhB within 60 min. In contrast, the orthorhombic Nb2O5 sample only discolored 26% in the same duration.

Intrinsic defects generated by iodine during TiO2 crystallization and its relationship with electrical conductivity and photoactivity

AbstractDefect formation during synthesis is one of the strategies used to improve the photoactivity of polycrystalline semiconductors such as titanium dioxide (TiO2). Defects can modify the electronic structure of TiO2 and change the surface of the interaction between the photocatalyst and the reactants. In this study, TiO2 relationship between processing in the presence of iodine and the consequent formation of intrinsic defects were explored. TiO2 nanoparticles were synthesized using the polymeric precursor method and exposed to iodine ions at concentrations up to 5 mol%. After calcination at 350°C, detailed chemical analyses revealed that iodine was absent in the samples. However, the TiO2 properties, such as specific surface area, crystallite sizes, and specific grain boundary area, were affected. Further experiments, such as electron paramagnetic resonance, diffuse reflectance, optical measurements, and electrochemical impedance spectroscopy indicated the presence of defects in the iodine‐processed samples. These defects directly influenced the electrical properties of the material, which affected the photoactivity, measured by the degradation of acetaminophen.