• Advances in nano research
• /
• v.15 no.1
• /
• pp.1-13
• /
• 2023

Ti₃C₂T_x MXene, a 2D material, is known to exhibit unique characteristics that are strongly dependent on surface termination groups. Here, we developed a novel annealing approach with Ca as a reducing agent to simultaneously remove F and O groups from the surface of multilayered MXene powder. Unlike H₂ annealing that removes F effectively but has difficulty in removing O, annealing with Ca effectively removed both O and F. X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy revealed that the proposed approach effectively removed F and O from the MXene powder. The results of O/N analyses showed that the O concentration decreased by 57.5% (from 2.66 to 1.13 wt%). In addition, XPS fitting showed that the volume fraction of metal oxides (TiO₂ and Al₂O₃) decreased, while surface termination groups (-O and -OH) were enhanced, which could increase the hydrophilic and adsorption properties of the MXene. These findings suggest that when F and O are removed from the MXene powder, the interlayer spacing of its lattice structure increases. The proposed treatment also resulted in an increase in the specific surface area (from 5.17 to 10.98 m²/g), with an increase in oxidation resistance temperature in air from ~436 to ~667 ℃. The benefits of this novel technology were verified by demonstrating the significantly improved cyclic charge-discharge characteristics of a lithium-ion battery with a Ca-treated MXene electrode.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.4 no.2
• /
• pp.148-156
• /
• 1994

Three composition in the system of $YO_{1.5}-BaO-CuO$ were grown using a cold crucible (skull) melting technique with a 50 kW R.F. induction generator operating at 4 MHz as the power source. The starting materials were prepared by conventional ceramic powder processing methods, loaded into the skull, and melted at about $1200^{\circ}C$. For this study, compositions near the $YBa_2Cu_3O_X$ region were selected. The growth rates used ranged from 4 cm/hr to 0.25 cm/hr. The relation between the microstructures and the starting composition of each ingot was determined using metallograph, X-ray diffraction, and energy dispersive X-ray analysis. Both $YBa_2Cu_3O_X$ and $Y_2BaCuO_5$ needle-shaped crystals, aligned with the growth direction, were formed in the $CuO-BaCuO_2$ eutectic matrix of the $YBa_2Cu_7O_x and YBa_5Cu_{11}O_x$ ingot.

• Advances in nano research
• /
• v.13 no.4
• /
• pp.325-339
• /
• 2022

Endophytes ascertain a symbiotic relationship with plants as promoters of growth, defense mechanism etc. This study is a first report to screen the endophytic population in Waltheria indica, a tropical medicinal plant. 5 bacterial and 3 fungal strains in leaves, 3 bacterial and 1 yeast species in stems were differentiated morphologically and identified by biochemical and molecular methods. The phylogenetic tree of the isolated endophytes was constructed using MEGA X. Silver nanoparticles were biosynthesized from a rare endophytic bacterium Cupriavidus metallidurans isolated from the leaf of W. indica. The formation of silver nanoparticles was confirmed by UV-Visible spectrophotometer that evidenced a strong absorption band at 408.5 nm of UV-Visible range with crystalline nature and average particle size of 16.4 nm by Particle size analyzer. The Fourier Transform Infra-Red spectrum displayed the presence of various functional groups that stabilized the nanoparticles. X-ray diffraction peaks were conferred to face centered cubic structure. Transmission Electron Microscope and Scanning Electron Microscope revealed the spherical-shaped, polycrystalline nature with the presence of elemental silver analyzed by Energy Dispersive of X-Ray spectrum. Selected area electron diffraction also confirmed the orientation of AgNPs at 111, 200, 220, 311 planes similar to X-ray diffraction analysis. The synthesized nanoparticles are evaluated for antimicrobial activity against 7 bacterial and 3 fungal pathogens. A good zone of inhibition was observed against pathogenic bacteria than fungal pathogens. Thus the study could hold a key aspect in drug discovery research and other pharmacological conducts of human clinical conditions.

• Restorative Dentistry and Endodontics
• /
• v.47 no.4
• /
• pp.36.1-36.17
• /
• 2022

Objectives: This study aimed to evaluate the effect of aging on the marginal quality of glass hybrid (GH) material used to elevate dentin gingival margins, and to analyze the consistency of the results obtained by 3 in vitro methods. Materials and Methods: Ten teeth received compound class II cavities with subgingival margins. The dentin gingival margins were elevated with GH, followed by resin composite. The GH/gingival dentin interfaces were examined through digital microscopy, scanning electron microscopy (SEM) using resin replicas, and according to the World Dental Federation (FDI) criteria. After initial evaluations, all teeth were subjected to 10,000 thermal cycles, followed by repeating the same marginal evaluations and energy dispersive spectroscopy (EDS) analysis for the interfacial zone of 2 specimens. Marginal quality was expressed as the percentage of continuous margin at ×200 for microscopic techniques and as the frequency of each score for FDI ranking. Data were analyzed using the paired sample t-test, Wilcoxon signed-rank test, and Pearson and Spearmen correlation coefficients. Results: None of the testing techniques proved the significance of the aging factor. Moderate and strong significant correlations were found between the testing techniques. The EDS results suggested the presence of an ion-exchange layer along the GH/gingival dentin interface of aged specimens. Conclusions: The marginal quality of the GH/dentin gingival interface defied aging by thermocycling. The replica SEM and FDI ranking results had stronger correlations with each other than either showed with the digital microscopy results.

• Restorative Dentistry and Endodontics
• /
• v.47 no.3
• /
• pp.32.1-32.11
• /
• 2022

Objectives: This study aimed to evaluate the influence of inorganic composition and filler particle morphology on the mechanical properties of different self-adhesive resin cements (SARCs). Materials and Methods: Three SARCs including RelyX Unicem-2 (RUN), Maxcem Elite (MAX), and Calibra Universal (CAL) were tested. Rectangular bar-shaped specimens were prepared for flexural strength (FS) and flexural modulus (FM) and determined by a 3-point bending test. The Knoop microhardness (KHN) and top/bottom microhardness ratio (%KHN) were conducted on the top and bottom faces of disc-shaped samples. Sorption (Wsp) and solubility (Wsl) were evaluated after 24 hours of water immersion. Filler morphology was analyzed by scanning electron microscopy and X-ray energy dispersive spectroscopy (EDS). FS, FM, %KHN, Wsp, Wsl, and EDS results were submitted to 1-way analysis of variance and Tukey's post-hoc test, and KHN also to paired t-test (α = 0.05). Results: SARC-CAL presented the highest FS value, and SARC-RUN presented the highest FM. SARC-MAX and RUN showed the lowest Wsp and Wsl values. KHN values decreased from top to bottom and the SARCs did not differ statistically. Also, all resin cements presented carbon, aluminum, and silica in their composition. SARC-MAX and RUN showed irregular and splintered particles while CAL presented small and regular size particles. Conclusions: A higher mechanical strength can be achieved by a reduced spread in grit size and the filler morphology can influence the KHN, as well as photoinitiators in the composition. Wsp and Wsl can be correlated with ions diffusion of inorganic particles.

• Journal of Electrochemical Science and Technology
• /
• v.14 no.4
• /
• pp.361-368
• /
• 2023

In lithium-sulfur (Li-S) batteries, encapsulation of sulfur in activated carbon (AC) materials is a promising strategy for preventing the dissolution of lithium polysulfide into electrolytes and enhancing cycle life, because instead of solid-liquid-solid reactions, quasi-solid-state (QSS) reactions occur in the AC micropores. While a high weight fraction of sulfur in S/AC composites is essential for achieving a high energy density of Li-S cells, the deterioration mechanisms under such conditions are still unclear. In this study, we report the deterioration mechanisms during charge-discharge cycling when the discharge products overflow from the AC. Analysis using scanning electron microscopy and energy-dispersive X-ray spectrometry confirms that the sulfur in the S/AC composites migrates outside the AC as cycling progresses, and it is barely present in the AC after 20 cycles, which corresponds to the capacity decay of the cell. Impedance analysis clearly shows that the electrical resistance of the S/AC composite and the charge-transfer resistance of QSS reactions significantly increase as a result of sulfur migration. On the other hand, the charge-discharge cycling performance under limited-capacity conditions, where the discharge products are encapsulated inside the AC, is extremely stable. These results reveal the degradation mechanism of a Li-S cell with micro-porous carbon and provide crucial insights into the design of a S/AC composite cathode and its operating conditions needed to achieve stable cycling performance.

• Journal of Surface Science and Engineering
• /
• v.56 no.5
• /
• pp.299-308
• /
• 2023

In this study, phosphorus (P)-doped nickel cobaltite (P-NiCo₂O₄) and nickel-cobalt layered double hydroxide (P-NiCo-LDH) were synthesized on nickel (Ni) foam as a conductive support using hydrothermal synthesis. The thermal properties, crystal structure, microscopic surface morphology, chemical distribution, electronic state of the constituent elements on the sample surface, and electrical properties of the synthesized P-NiCo₂O₄ and P-NiCo-LDH samples were analyzed using thermogravimetric analysis-differential scanning calorimetry (TGA-DSC), X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS). The P-NiCo₂O₄ electrode exhibited a specific capacitance of 1,129 Fg^-1 at a current density of 1 Ag^-1, while the P-NiCo-LDH electrode displayed a specific capacitance of 1,012 Fg^-1 at a current density of 1 Ag-1. When assessing capacity changes for 3,000 cycles, the P-NiCo₂O₄ electrode exhibited a capacity retention rate of 54%, whereas the P-NiCo-LDH electrode showed a capacity retention rate of 57%.

• Journal of Surface Science and Engineering
• /
• v.56 no.6
• /
• pp.437-442
• /
• 2023

This research aims to enhance the efficiency of Pt/C catalysts due to the limited availability and high cost of platinum in contemporary fuel cell catalysts. Nano-sized platinum particles were distributed onto a carbon-based support via the polyol process, utilizing the metal precursor H₂PtCl₆·6H₂O. Key parameters such as pH, temperature, and RPM were carefully regulated. The findings revealed variations in the particle size, distribution, and dispersion of nano-sized Pt particles, influenced by temperature and pH. Following sodium hydroxide treatment, heat treatment procedures were systematically executed at diverse temperatures, specifically 120, 140, and 160 ℃. Notably, the thermal treatment at 140 ℃ facilitated the production of Pt/C catalysts characterized by the smallest platinum particle size, measuring at 1.49 nm. Comparative evaluations between the commercially available Pt/C catalysts and those synthesized in this study were meticulously conducted through cyclic voltammetry, X-ray diffraction (XRD), and field-emission scanning electron microscopy-energy dispersive X-ray spectroscopy (FE-SEM EDS) methodologies. The catalyst synthesized at 160 ℃ demonstrated superior electrochemical performance; however, it is imperative to underscore the necessity for further optimization studies to refine its efficacy.

• Journal of Surface Science and Engineering
• /
• v.56 no.6
• /
• pp.420-426
• /
• 2023

We prepared a highly sensitive hydrogen (H₂) sensor based on Indium oxides (In₂O₃) porous nanoparticles (NPs) loaded with Platinum (Pt) nanoparticle in the range of 1.6~5.7 at.%. In₂O₃ NPs were fabricated by microwave irradiation method, and decorations of Pt nanoparticles were performed by electroless plating on In₂O₃ NPs. Crystal structures, morphologies, and chemical information on Pt-loaded In₂O₃ NPs were characterized by grazing-incident X-ray diffraction, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, respectively. The effect of the Pt nanoparticles on the H₂-sensing performance of In₂O₃ NPs was investigated over a low concentration range of 5 ppm of H₂ at 150-300 ℃ working temperatures. The results showed that the H₂ response greatly increased with decreasing sensing temperature. The H₂ response of Pt loaded porous In₂O₃ NPs is higher than that of pristine In₂O₃ NPs. H₂ gas selectivity and high sensitivity was explained by the extension of the electron depletion layer and catalytic effect. Pt loaded porous In₂O₃ NPs sensor can be a robust manner for achieving enhanced gas selectivity and sensitivity for the detection of H₂.

• Korean Journal of Materials Research
• /
• v.34 no.5
• /
• pp.254-260
• /
• 2024

This study is to manufacture a titanium dioxide (TiO₂) photocatalyst by recycling sludge generated using titanium tetrachloride (TiCl₄) as a coagulant. Compared to general sewage, a TiCl₄ coagulant was applied to dyeing wastewater containing a large amount of non-degradable organic compounds to evaluate its performance. Then the generated sludge was dried and fired to prepare a photocatalyst (TFS). Scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), and nitrogen oxide reduction experiments were conducted to analyze the surface properties and evaluate the photoactive ability of the prepared TFS. After using titanium tetrachloride (TiCl₄) as a coagulant in the dyeing wastewater, the water quality characteristics were measured at 84 mg/L of chemical oxygen demand (COD), 10 mg/L of T-N, and 0.9 mg/L of T-P to satisfy the discharge water quality standards. The surface properties of the TFS were investigated and the anatase crystal structure was observed. It was confirmed that the ratio of Ti and O, the main components of TiO₂, accounted for more than 90 %. As a result of the nitric oxide (NO) reduction experiment, 1.56 uMol of NO was reduced to confirm a removal rate of 20.60 %. This is judged to be a photocatalytic performance similar to that of the existing P-25. Therefore, by applying TiCl₄ to the dyeing wastewater, it is possible to solve the problems of the existing coagulant and to reduce the amount of carbon dioxide generated, using an eco-friendly sludge treatment method. In addition, it is believed that environmental and economic advantages can be obtained by manufacturing TiO₂ at an eco-friendly and lower cost than before.