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 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.

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.

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.

In this study, porous Mo-5 wt% Cu with unidirectionally aligned pores is prepared by freeze drying of camphene slurry with MoO3-CuO powders. Unidirectional freezing of camphene slurry with dispersion stability is conducted at -25℃, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The green bodies are hydrogen-reduced at 750℃ and sintered at 1000℃ for 1 h. X-ray diffraction analysis reveals that MoO3- CuO composite powders are completely converted to a Mo-and-Cu phase without any reaction phases by hydrogen reduction. The sintered bodies with the Mo-Cu phase show large and aligned parallel pores to the camphene growth direction as well as small pores in the internal walls of large pores. The pore size and porosity decrease with increasing composite powder content from 5 to 10 vol%. The change of pore characteristics is explained by the degree of powder rearrangement in slurry and the accumulation behavior of powders in the interdendritic spaces of solidified camphene.

Metallic tantalum powder is manufactured by reducing tantalum oxide (Ta2O5) with magnesium gas at 1,073–1,223 K in a reactor under argon gas. The high thermodynamic stability of magnesium oxide makes the reduction reaction from tantalum oxide into tantalum powder possible. The microstructure after the reduction reaction has the form of a mixture of tantalum and magnesium oxide, and the latter could be entirely eliminated by dissolving in weak hydrochloric acid. The powder size in SEM microstructure for the tantalum powder increases after acid leaching in the range of 50–300 nm, and its internal crystallite sizes are observed to be 11.5 to 24.7 nm with increasing reduction temperatures. Moreover, the optimized reduction temperature is found to be 1,173 K as the minimum oxygen concentration is approximately 1.3 wt.%.

This study focuses on the fabrication of a WC/Co composite powder from the oxide of WC/Co hardmetal scrap using solid carbon in a hydrogen gas atmosphere for the recycling of WC/Co hardmetal. Mixed powders are manufactured by mechanically milling the oxide powder of WC-13 wt% Co hardmetal scrap and carbon black with varying powder/ball weight ratios. The oxide powder of WC-13 wt% Co hardmetal scrap consists of WO3 and CoWO4. The mixed powder mechanically milled at a lower powder/ball weight ratio (high mechanical milling energy) has a more rapid carbothermal reduction reaction in the formation of WC and Co phases compared with that mechanically milled at a higher powder/ball weight ratio (lower mechanical milling energy). The WC/Co composite powder is fabricated at 900℃ for 6 h from the oxide of WC/Co hardmetal scrap using solid carbon in a hydrogen gas atmosphere. The fabricated WC/Co composite powder has a particle size of approximately 0.25-0.5 μm.

We studied the basic properties and fabrication of reduced graphene oxide (rGO) prepared using eco-friendly reduction agents in the graphene solution process. Hydrazine is generally used to reduce graphene oxide (GO), which results in polluting emissions as well as fixed nitrogen functional groups on different defects in the graphene sheets. To replace hydrazine, we developed eco-friendly reduction agents with similar or better reducing properties, and selected of them for further analysis. In this study, GO layers were produced from graphite flakes using a modified Hummer’s method, and rGO layers were reduced using hydrazine hydrate, L-ascorbic acid, and gluconic acid. We measured the particle sizes and the dispersion stabilities in the rGO dispersed solvents for the three agents and analyzed the structural, electrical, and optical properties of the rGO films. The results showed that the degree of reduction was in the order L-ascorbic acid ≥ hydrazine > glucose. GO reduced using L-ascorbic acid had a sheet resistance of 121 kΩ/sq, while that reduced using gluconic acid showed worse electrical properties than the other two reduction agents. Therefore, L-ascorbic acid is the most suitable eco-friendly reduction agent that can be substituted for hydrazine.

A highly facile and eco-friendly green synthesis of Annona squamosa (custard apple) leaf extract reduced graphene oxide (CRG) nanosheets was achieved by the reduction of graphene oxide (GO). The as-prepared CRG was characterized with X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier-transform infrared spectroscopy (FT-IR), ultraviolet-visible (UV-Vis), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopic techniques. Removal of oxygen containing moieties from the GO was confirmed by UV-Vis, FT-IR and XPS spectroscopic data. The XRD and Raman data further confirmed the formation of the CRG. TEM images showed the sheet structure of the synthesized CRG. These results show that the phytochemicals present in custard apple leaf extract act as excellent reducing agents. The CRG showed good dispersion in water.

A black nickel oxide powder, one of the commercial nickel oxide ores, was reduced by hydrogen gas in a batchtype fluidized-bed reactor in a temperature range of 350 to 500 oC and in a residence time range of 5 to 120 min. The hydrogen reduction behavior of the black nickel oxide was found to be somewhat different from that of green nickel oxide ore. For the black nickel oxide, the maximum temperature (below which nickel oxide particles can be reduced without any agglomeration) was significantly lower than that observed for the green nickel oxide. In addition, the best curve fittings of the Avrami model were obtained at higher values of the overall rate constant “k” and at lower values of the exponent “m”, compared to those values for the green nickel oxide. It may be inferred from these results that the hydrogen reduction rate of the black nickel oxide is faster than that of the green nickel oxide in the early stages, but the situation reverses in the later stages. For the black nickel oxide ore, in spite of the low temperature sintering, it was possible to achieve a high degree fluidized-bed reduction at lower temperatures and at lower gas consumption rates than was possible for the green nickel oxide. In this regard, the use of black nickel oxide is expected to yield a benefit if its ore price is sufficiently lower than that of the green nickel oxide.

We report the preparation of sulfonated reduced graphene oxide (SRGO) by the sulfonation of graphene oxide followed by radiation-induced chemical reduction. Graphene oxide prepared by the well-known modified Hummer's method was sulfonated with the aryl diazonium salt of sulfanilic acid. Sulfonated graphene oxide (SGO) dispersed in ethanol was subsequently reduced by γ-ray irradiation at various absorbed doses to produce SRGO. The results of optical, chemical, and thermal analyses revealed that SRGO was successfully prepared by γ-ray irradiation-induced chemical reduction of the SGO suspension. Moreover, the electrical conductivity of SRGO was increased up to 2.94 S/cm with an increase of the absorbed dose.