Molybdenum, valued for its high melting point and exceptional physical and chemical properties, is studied in diverse fields such as electronics, petrochemicals, and aviation. Among molybdenum oxides, molybdenum dioxide stands out for its higher electrical conductivity than other transition metal oxides due to its structural characteristics, exhibiting metallic properties. It is applied as pellets to gas sensors, semiconductors, and secondary batteries for its properties. Thus, research on molybdenum dioxide compaction and pressureless sintering is necessary, yet research on pressureless sintering is currently insufficient. This study synthesized MoO₃ powder via solution combustion synthesis and reduced it using the 3% hydrogen/argon gas mixture to investigate the effect of reduction temperature on the powder. Additionally, the reduced powder was compacted and subjected to pressureless sintering with temperature as a variable. The density and the microstructure of brown parts were analyzed and discussed.

The structure and magnetic properties of composite powders prepared by ball milling a mixture of Fe2O3 ‧ (0.4-1.0)Fe were investigated. Hysteresis loops and differential scanning calorimetry (DSC) curves are used to characterize the materials and to examine the effect of the solid state reaction induced by ball milling. The results showed that a solid state reaction in Fe2O3 ‧ (0.4-1.0)Fe clearly proceeds after only 1 h of ball milling. The system is characterized by a positive reaction heat of +2.23 kcal/mole. The diffraction lines related to Fe2O3 and Fe disappeared after 1 h of ball milling and, instead, diffraction lines of the intermediate phase of Fe3O4 plus FeO formed. The magnetization and coercivity of the Fe2O3 ‧ 0.8Fe powders were changed by the solid state reaction process of Fe2O3 by Fe during ball milling. The coercivity of the Fe2O3 ‧ 0.8Fe powders increased with increasing milling time and reached a maximum value of 340 Oe after 5 h of ball milling. This indicates the grain size of Fe3O4 was clearly reduced during ball milling. The magnetic properties of the annealed powders depend on the amount of magnetic Fe and Fe3O4 phases.

We report the effect of plastic deformation on the thermoelectric properties of n-type Bi2Te2.5Se0.5 compounds. N-type Bi2Te2.5Se0.5 powders are synthesized by an oxide-reduction process and consolidated via sparkplasma sintering. To explore the effect of plastic deformation on the thermoelectric properties, the sintered bodies are subjected to uniaxial pressure to induce a controlled amount of compressive strains (-0.2, -0.3, and -0.4). The shaping temperature is set using a thermochemical analyzer, and the plastic deformation effect is assessed without altering the material composition through differential scanning calorimetry. This strategy is crucial because the conventional hotforging process can often lead to alterations in material composition due to the high volatility of chalcogen elements. With increasing compressive strain, the (00l) planes become aligned in the direction perpendicular to the pressure axis. Furthermore, an increase in the carrier concentration is observed upon compressive plastic deformation, i.e., the donorlike effect of the plastic deformation in n-type Bi2Te2.5Se0.5 compounds. Owing to the increased electrical conductivity through the preferred orientation and the donor-like effect, an improved ZT is achieved in n-type Bi2Te2.5Se0.5 through the compressive-forming process.

In pyroprocessing, the residual salts (LiCl containing Li and Li2O) in the metallic fuel produced by the oxide reduction (OR) process are removed by salt distillation and fed into electrorefining. This study undertook an investigation into the potential viability of employing a separate LiCl salt rinsing process as an innovative alternative to conventional salt distillation techniques. The primary objective of this novel approach was to mitigate the presence of Li and Li2O within the residual OR salt of metallic fuel, subsequently facilitating its suitability for electrorefining processes. The process of rinsing the metallic fuel involved immersing it in a LiCl salt environment at a temperature of 650°C. During this immersion process, the residual OR salt contained within the fuel underwent dissolution, thereby reducing the concentrations of Li2O and Li generated during the OR process. Furthermore, the Li and Li2O dissolved within the LiCl salt were effectively consumed through chemical reactions with ZrO2 particles present within the salt. Importantly, even after the metallic fuel had been subjected to rinsing in a conventional LiCl salt solution, the concentration of Li and Li2O within the salt remained consistent with its initial levels, due to the utilization of ZrO2. Moreover, it was observed that the Li- Li2O content within the metallic fuel was significantly diluted as a result of the rinsing process.

Pyroprocessing is a promising technique for the treatment of damaged fuel debris (corium) generated by severe nuclear accidents. The debris typically consists of (U, Zr)O2 originating from the UO2 fuel and Zr alloy-based cladding. By converting the corium to a metallic form, the principal components of the fuel can be recovered through subsequent electrorefining, allowing for long-term storage or final disposal. A study investigated the reduction of zirconium oxide compounds by Li metal as a reductant in molten LiCl salt. This research explored the feasibility of treating damaged nuclear fuel debris, which mainly consists of (U, Zr)O2. The results showed that ZrO2 was successfully reduced to Zr metal by Li metal in LiCl salt at 650C without the formation of Li2ZrO3. In particular, Zr metal was produced without the formation of Li2ZrO3 when LiCl salt containing a high concentration of Li metal was used. However, Zr metal was produced with Li2ZrO3 when LiCl salt containing both Li metal and Li2O was added. This suggests that the concentration of Li metal in the LiCl salt is an important factor in determining the formation of Li2ZrO3. The study also demonstrated that Li2ZrO3 was partially reduced to Zr metal by Li metal in LiCl salt. This finding suggests that Li metal may be effective in reducing other oxide compounds in molten LiCl salt, which could be useful in the treatment of corium. Overall, the research provides valuable insights into the feasibility of using pyroprocessing for the treatment of corium. The ability to recover and store the principal components of the fuel through electrorefining could have important implications for the long-term management of nuclear waste.

In this paper, we presented a hybrid composite of graphene quantum dots (GQDs)-modified three-dimensional graphene nanoribbons (3D GNRs) composite linked by Fe3O4 and CoO nanoparticles through reflux and ultrasonic treatment with GQDs, denoted as 3D GQDs-Fe3O4/CoO@GNRs (3D GFCG). In this hybrid, the 3D GNRs framework strengthened the electrical conductivity and the synergistic effects between GQDs and 3D GFCG enhanced the oxygen reduction reaction (ORR) activity of the nanocomposite. The results imply that decorating GQDs with other electro-catalysts is an effective strategy to synergistically improve their ORR activity.

The electrochemical behavior was investigated during the electrolysis of nickel oxide in LiCl-Li2O salt mixture at 650℃ by changing several components. The focus of this work is to improve anode design and shroud design to increase current densities. The tested components were ceramic anode shroud porosity, porosity size, anode geometry, anode material, and metallic porous anode shroud. The goal of these experiments was to optimize and improve the reduction process. The highest contributors to higher current densities were anode shroud porosity and anode geometry.

As frontier materials, graphene oxide (GO) and graphene have penetrated almost all research areas and advanced numerous technologies in sensing, electronics, energy storage, catalysis, water treatment, advanced composites, biomedical, and more. However, the affordable large-scale synthesis of high-quality GO and graphene remains a significant challenge that negatively affects its commercialisation. In this article, firstly, a simple, scalable approach was demonstrated to synthesise high-quality, high yield GO by modifying the improved Hummers method. The advantages of the optimised process are reduced oxidation time, straightforward washing steps without using coagulation step, reduction in cost as eliminating the use of phosphoric acid, use of minimum chemical reagents, and increased production of GO per batch (~ 62 g). Subsequently, the produced GO was reduced to reduced graphene oxide (rGO) using three different approaches: green reduction using ascorbic acid, hydrothermal and thermal reduction techniques. The GO and rGO samples were characterised using various microscopy and spectroscopy techniques such as XRD, Raman, SEM, TEM, XPS and TGA. The rGO prepared using different methods were compared thoroughly, and it was noticed that rGO produced by ascorbic acid reduction has high quality and high yield. Furthermore, surface (surface wettability, zeta potential and surface area) and electrical properties of GO and different rGO were evaluated. The presented synthesis processes might be potentially scaled up for large-scale production of GO and rGO.

The reduced graphene oxide (rGO) has attracted more and more attention in recent years. How to choose a suitable reduction method to prepare rGO is a critical problem in the preparation of graphene composites. In this work, the differences of rGO reduced by thermal, microwave, Ultraviolet (UV) and reducing agent were studied. The reduction degree and functional groups of rGO were compared by SEM, XPS, Raman, FTIR and TGA. Thermal can remove most of the oxygen-containing groups of graphene oxide (GO) and the thermal reduction is the most effective reduction method. UV light can directly act on the unstable oxygen-containing groups, and its reduction efficiency is second only to thermal reduction. The efficiency of chemical reduction is not as good as that of UV reduction, because the reducing agent only act on the surface of GO. Microwave reduction is a mild thermal reduction with the lowest efficiency, but the residual oxygen-containing groups increase the hydrophilicity of rGO. To sum up, this work studies that rGO prepared by different reduction methods has different characteristics, which provides a reference for selecting appropriate reduction methods to prepare graphene composites with better properties.

Lately, Raman spectroscopy has become powerful tool for quality assessment of graphene analogues with identification of intensity ratio of Raman active D-band and G-band ( ID/IG ratio) as a vital parameter for quantification of defects. However, during chemical reduction of graphitic oxide (GrO) to reduced GrO (RGrO), the increased ID/ IG ratio is often wrongly recognized as defect augmentation, with “formation of more numerous yet smaller size sp2 domains” as its explanation. Herein, by giving due attention to normalized peak height, full-width half-maxima and integrated peak area of Raman D- and G-bands, and compliment the findings by XRD data, we have shown that in-plane size of sp2 domains actually increases upon chemical reduction. Particularly, contrary to increased ID/ IG ratio, the calculated decrease in integrated peak area ratio ( AD/AG ratio) in conjunction with narrowing of D-band and broadening of G-band, evinced the decrease in in-plane defects. Finally, as duly supported by reduction induced broadening of interlayer-spacing characteristic XRD peak and narrowing of ~ 43° centered XRD hump, we have also shown that the sp2 domains actually expands in size and the observed increase in ID/ IG ratio is indeed due to increase in across-plane defects, formed via along-the-layer slicing of graphitic domains.

Thermal reduction of graphite oxide (GO) is considered as a prospective method for the preparation of high-performance graphene-based materials. However, this method has certain limitations, and the major is that this exothermic process is difficult to control. In this research, we focused on the kinetic studies of the reduction of graphite oxide using non-isothermal differential calorimetry (DSC) method. Six GO nanocomposites with dyes were tested to study the shift in kinetic parameters. The apparent reaction order is determined to be ca 0.7 for the thermal decomposition of pure GO, while in the presence of dye molecules it increases sometimes reaching a value of 2.0 for higher dye concentrations. Decisively, the thermal decomposition of pure GO can be presented as an intermediate between a zero- and first-order reaction, while the introduction of dye molecules turns a certain part of the energy consumption via the bimolecular pathway. Our research revealed that the process of GO thermal decomposition can be operated and properties of the final product (reduced graphene oxide (rGO) and its derivatives) can be adjusted more precisely using additive molecules, which interact with GO sheets.

Solid-state mechanochemical reduction combined with subsequent melting consolidation was suggested as a technical option for the oxide reduction in pyroprocessing. Ni ingot was produced from NiO as a starting material through this technique while Li metal was used as a reducing agent. To determine the technical feasibility of this approach for pyroprocessing, which handles spent nuclear fuels, thermodynamic calculations of the phase stabilities of various metal oxides of U and other fission elements were made when several alkaline and alkali-earth metals were used as reducing agents. This technique is expected to be beneficial, not only for oxide reduction but also for other unit processes involved in pyroprocessing.

The reaction between Li2CO3 and Cl2 was investigated to verify its occurrence during a carbon-anode-based oxide reduction (OR) process. The reaction temperature was identified as a key factor that determines the reaction rate and maximum conversion ratio. It was found that the reaction should be conducted at or above 500℃ to convert more than 90% of the Li2CO3 to LiCl. Experiments conducted at various total flow rate (Q) / initial sample weight (W i) ratios revealed that the reaction rate was controlled by the Cl2 mass transfer under the experimental conditions adopted in this work. A linear increase in the progress of reaction with an increase in Cl2 partial pressure (pCl2) was observed in the pCl2 region of 2.03–10.1 kPa for a constant Q of 100 mL∙min−1 and W i of 1.00 g. The results of this study indicate that the reaction between Li2CO3 and Cl2 is fast at 650℃ and the reaction is feasible during the OR process.

PURPOSES : The purpose of this study was to analyze the effect of reducing nitrogen oxide concentration in a photocatalyst (titanium dioxide) using statistical methods such as the Anderson-Darling test. METHODS : To compare and analyze the effect of reducing the nitrogen oxide concentrations in titanium dioxide, titanium dioxide was applied to the public road, and data acquisition in terms of nitrogen oxide concentration was conducted from roads with/without applying titanium dioxide (test section and reference section, respectively). Then, the probabilities of occurrence of nitrogen oxide concentrations in the test and reference sections were estimated and compared using the Anderson-Darling test. RESULTS : According to the comparison and analysis of probabilities in the nitrogen oxide concentration of the test and reference sections, the probabilities of nitrogen oxide concentration on December 4th were estimated as ‘High’ (17.5%, 37.9%), ‘Moderate’ (30.5%, 40.8%), and ‘Low’ (52.0%, 21.3%), respectively, and on December 5th, as ‘High’ (20.6%, 39.1%), ‘Moderate’ (26.2%, 33.0%), and ‘Low’ (53.2%, 27.9%), respectively. In addition, the probabilities of nitrogen oxide concentration in the test and reference sections were analyzed on December 6th as ‘High’ (16.5%, 36.8%), ‘Moderate’ (27.9%, 38.5%), and ‘Low’ (55.6%, 24.8%), respectively. CONCLUSIONS : Based on the results of this study, in the test section with application of titanium dioxide, the nitrogen oxide concentration was found to have a low probability, and in the reference section, the nitrogen oxide concentration was found to be higher than that in the test section. Therefore, it can be concluded that titanium dioxide applied to road facilities has a nitrogen oxide reduction effect.