The corrosion behavior of the Inconel X-750 alloy was investigated for its potential application under a Cl2-O2 mixed gas flow in an Ar atmosphere. The corrosion rate was found to be negligible at temperatures up to 400℃ under a flow rate of 30 mL·min-1 Cl2 + 170 mL·min-1 Ar, whereas an exponential increase was observed in the corrosion rate at temperatures greater than 500℃. The suppression of the corrosion reaction due to the presence of O2 was verified experimentally at flow rates of 30 mL·min-1 Cl2 (4.96 g·m-2·h-1), 20 mL·min-1 Cl2 + 10 mL·min-1 O2 (2.02 g·m-2·h-1), and 10 mL·min-1 Cl2 + 20 mL·min-1 O2 (1.34 g·m-2·h-1) under a constant Ar flow rate of 170 mL·min-1 at 600℃ for 8 h. The surface morphology analysis results revealed that porous surfaces with tunnel-type holes were produced under the Cl2-O2 mixed-gas condition. Furthermore, the effects of the Cl2 flow rate on the corrosion rate were investigated, indicating that its impact was negligible within the range of 5–30 mL·min-1 Cl2 at 600℃.

Here, the stability of stainless steel 316 (SS-316) was investigated to identify its applicability in the oxide reduction process, as a component in related equipment, to produce a complicated gas mixture composed of O2 and Cl2 under an argon (Ar) atmosphere. The effects of the mixed gas composition were investigated at flow rates of 30 mL/min O2, 20 mL/min O2 + 10 mL/min Cl2, 10 mL/min O2 + 20 mL/ min Cl2, and 30 mL/min Cl2, each at 600℃, during a constant argon flow rate of 170 mL/min. It was found that the corrosion of SS-316 by the chlorine gas was suppressed by the presence of oxygen, while the reaction proceeded linearly with the reaction time regardless of gas composition. Surface observation results revealed an uneven surface with circular pits in the samples that were fed mixed gases. Thermodynamic calculations proposed the combination of Fe and Ni chlorination reactions as an explanation for this pit formation phenomenon. An exponential increase in the corrosion rate was observed with an increase in the reaction temperature in a range of 300 ~ 600℃ under a flow of 30 mL/min Cl2 + 170 mL/min Ar.

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.%.

파이로 공정에서는 사용후핵연료 관리 공정 개발의 일환으로 산화 우라늄을 고온 용융염 전해질계에서 전기화학적 방법으로 환원시키기 위한 전해환원 공정이 개발되고 있다. 이에 따른 전해환원 공정의 반응기 설계를 위해서는 전기화학적 이론에 기초한 모델이 요구되고 있다. 본 연구에서는 상 분리를 설명하는 phase-field 이론에 기초하여 우라늄 산화물의 전해환원 모사를 위한 1차원 모델이 개발되었다. 모델은 우라늄 산화물 내 산소 원소의 확산과 펠렛 표면에서 전기화학 반응 속도를 나타내는 매개변수를 사용하여 외부로부터 내부로 진행되는 전해환원을 잘 모사하고 있으며 계산 결과 전체 전류는 산소 원소의 내부 확산에 크게 의존하는 것으로 나타났다. 전해환원 반응에 대한 모델은 대용량 장치 설계에 최적화된 조건 도출에 활용될 것으로 예상되며 장치 설계가 완료되면 공정 연계 모사에 직접 사용될 것으로 기대된다.

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.

Electrochemical reduction has previously been reported for uranium oxide and mixed oxide nuclear fuel (uranium oxide, plutonium oxide). The laboratory scale electrochemical reduction of plutonium oxide powder is demonstrated in CaCl2- 1wt%CaO. The plutonium oxide contained within a permeable steel basket cathode is sacrificed during the process. A graphite anode is also employed during the reduction, leading to a significant contamination of the product.

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.

In this study, the reduction kinetics and behaviors of oxides in the water-atomized iron powder have been evaluated as a function of temperature ranging 850-1000˚C in hydrogen environment, and compared to the reduction behaviors of individual iron oxides including Fe2O3, Fe3O4 and FeO. The water-atomized iron powder contained a significant amount of iron oxides, mainly Fe3O4 and FeO, which were formed as a partially-continuous surface layer and an inner inclusion. During hydrogen reduction, a significant weight loss in the iron powder occurred in the initial stage of 10 min by the reduction of surface oxides, and then further reduction underwent slowly with increasing time. A higher temperature in the hydrogen reduction promoted a high purity of iron powder, but no significant change in the reduction occurred above 950˚C. Sequence reduction process by an alternating environment of hydrogen and inert gases effectively removed the oxide scale in the iron powder, which lowered reduction temperature and/or shortened reduction time.

Freeze drying of a porous Cu-Sn alloy with unidirectionally aligned pore channels was accomplished by using a composite powder of CuO-SnO2 and camphene. Camphene slurries with CuO-SnO2 content of 3, 5 and 10 vol% were prepared by mixing with a small amount of dispersant at 50˚C. Freezing of a slurry was done at -25˚C while the growth direction of the camphene was unidirectionally controlled. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green bodies were hydrogen-reduced at 650˚C and then were sintered at 650˚C and 750˚C for 1 h. XRD analysis revealed that the CuO-SnO2 powder was completely converted to Cu-Sn alloy without any reaction phases. The sintered samples showed large pores with an average size of above 100μm which were aligned parallel to the camphene growth direction. Also, the internal walls of the large pores had relatively small pores. The size of the large pores decreased with increasing CuO-SnO2 content due to the change of the degree of powder rearrangement in the slurry. The size of the small pores decreased with increase of the sintering temperature from 650˚C to 750˚C, while that of the large pores was unchanged. These results suggest that a porous alloy body with aligned large pores can be fabricated by a freeze-drying and hydrogen reduction process using oxide powders.

The study on the fabrication of iron powder from forging scales using hydrogen gas has been conducted on the effect of hydrogen partial pressure, temperature, and reactive time. The mechanism for the reduction of iron oxides was proposed with various steps, and it was found that reduction pattern might be different depending on tem- perature. The iron content in the scale and reduction ratio of oxygen were both increased with increasing reactive time at 0.1atm of hydrogen partial pressure. On the other hand, for over 30 minutes at 0.5 atm of hydrogen partial pressure, the values were found to be almost same. In the long run, iron metallic powder was obtained with over 90% of iron content and an average size of its powder was observed to be about 100 µm.