The high-temperature stability of YSZ specimens fabricated by die pressure and cold isostatic press (CIP) is investigated in CaCl2-CaF2-CaO molten salt at 1,150 °C. The experimental results are as follows: green density 46.7 % and 50.9 %; sintering density 93.3 % and 99.3 % for die press and CIP, respectively. YSZ foremd by CIP exhibits higher stability than YSZ formed by die press due to denseness dependency after high-temperature stability test. YSZ shows peaks mainly attributed to CaZrO3, with a small t-ZrO2 peak, unlike the high-intensity tetragonal-ZrO2 (t-ZrO2) peak observed for the asreceived specimen. The t-ZrO2 phase of YSZ is likely stabilized by Y2O3, and the leaching of Y2O3 results in phase transformation from t-ZrO2 to m-ZrO2. CaZrO3 likely forms from the reaction between CaO and m-ZrO2. As the exposure time increases, more CaZrO3 is observed in the internal region of YSZ, which could be attributed to the inward diffusion of molten salt and outward diffusion of the stabilizer (Y2O3) through the pores. This results in greater susceptibility to phase transformation and CaZrO3 formation. To use SOM anodes for the electroreduction of various metals, YSZ stability must be improved by adjusting the high-density in the forming process.

삼불화알루미늄(AlF3)이 포함된 염화물-불화물 혼합 용융염에서 ZIRLO 튜브를 이용한 지르코늄 전해정련공정을 실증하였다. 순환 전압전류실험 결과, AlF3의 농도가 증가함에 따라 금속환원의 개시 전위가 일정하게 증가하고 지르코늄-알루미늄 합금형성과 관련된 추가적인 peak의 크기가 점차 증가하는 것으로 나타났다. 전류조절 전착법과 달리, −1.2 V의 일정전위 에서 수행한 지르코늄 전해정련에서 방사형 판 구조의 지르코늄 성장이 염의 상단 표면에서 확연하게 나타났으며, 전착물 지름의 크기는 AlF3의 농도에 따라 점차 증가하는 것으로 나타났다. 주사전자현미경(SEM)과 에너지 분산 X선 분광기(EDX) 와 X선 광전자 분광기(XPS)를 이용하여 판 구조의 지르코늄 전착물을 분석한 결과, 극미량의 알루미늄이 지르코늄-알루미늄 합금 형태로 존재하며, 전착물의 상단과 하단 간에 서로 다른 화학성분구조를 갖는 것으로 나타났다. AlF3의 첨가는 전착물 내 잔류염 양을 줄이고, 지르코늄 회수를 위한 전류효율을 향상시키는 데 효과적인 것으로 나타났다.

Li-Cd 합금을 이용한 환원추출방식을 LiCl-KCl 기반의 drawdown 공정에 적용하게 되면, LiCl-KCl 공융염의 조성이 파괴되므로 공정온도를 높여야 하며, 전해정련 및 전해제련과 같은 공정에 LiCl-KCl 용융염을 재사용할 수 없게 된다. 따라서, 본 연구에서는 공융염 조성에 적합한 Li-K-Cd 합금을 제조하였으며, 이를 이용하여 U와 Nd가 포함된 LiCl-KCl 염에 투입하여 용 융염 내 UCl3의 제거가 가능한지 평가하였다.

For diamond/metal composites it is better to use diamond particles coated with metal carbide because of improved wettability between the diamond particles and the matrix. In this study, the coating of diamond particles with a chromium carbide layer is investigated. On heating diamond and chromium powders at 800~900 oC in molten salts of LiCl, KCl, CaCl2, the diamond particles are coated with Cr7C3. The surfaces of the diamond powders are analyzed using X-ray diffraction and scanning electron microscopy. The average thickness of the Cr7C3 coating layers is calculated from the result of the particle size analysis. By using the molten salt method, the Cr7C3 coating layer is uniformly formed on the diamond particles at a relatively low temperature at which the graphitization of the diamond particles is avoided. Treatment temperatures are lower than those in the previously proposed methods. The coated layer is thickened with an increase in heating temperature up to 900 oC. The coating reaction of the diamond particles with chromium carbide is much more rapid in LiCl-KCl-CaCl2 molten salts than with the molten salts of KCl-CaCl2.

As an approach for estimation of the droplet size in the molten salt-liquid metal extraction process, a droplet formation experiment at room temperature was conducted to evaluate the applicability of the Scheele-Meister model with water-mercury system as a surrogate that is similar to the molten salt-liquid metal system. In the experiment, droplets were formed through the nozzle and the droplet size was measured using a digital camera and image analysis software. As nozzles, commercially available needles with inner diameters (ID) of 0.018 cm and 0.025 cm and self-fabricated nozzles with 3-holes (ID: 0.0135 cm), 4-holes (ID: 0.0135 cm), and 2-holes (ID: 0.0148 cm) were used. The mercury penetration lengths in the nozzles were 1.3 cm for the needles and 0.5 cm for the self-fabricated nozzles. The droplets formed from each nozzle maintained stable spherical shape up to 20 cm below the nozzle. The droplet size measurements were within a 10% error range when compared to the Scheele-Meister model estimates. The experimental results show th

LiCl-KCl 용융염에서 광학적으로 투명한 텅스텐 망으로 제작된 작업전극에 대해 사마륨의 전기화학적 거동을 Cyclic voltammetry와 Potential step chronoabsorptometry의 전기화학적 및 분광전기화학적 방법으로 조사하였다. Cyclic voltammogram 으로 결정된 Sm3+/Sm2+의 산화환원 반응의 가역성을 기반으로 형식전위와 확산계수를 계산하여 각각 –1.99 V vs. Cl2/Cl- 와 2.53×10-6 cm2·s-1를 얻었다. 작업 전극에 –1.5 V vs. Ag/AgCl (wt%)로 전압을 인가하여 측정한 Chronoabsorptometry 를 통해 사마륨 이온의 특성 파장으로 Sm3+에 대해 408.08 nm, Sm2+에 대해 545.62 nm를 확인하였다. Voltammogram에서 얻은 환원 피크 전압과 산화 피크 전압을 이용하여 Potential step chronoabsorptometry를 수행하였다. 545.63 nm의 흡광 피크 값을 분석하여 2.15×10-6 cm2·s-1의 확산계수를 얻었으며 이 값은 동일한 온도에서 Cyclic voltammtry 분석으로 얻은 값과 큰 차이를 보이지 않았다. 실험결과로부터 고온 용융염에서 광학적으로 투명한 작업전극을 이용한 분광전기화학적 방 법이 용융염에 용해된 이온의 종류를 확인하며 전기화학적 거동을 조사하는데 유용한 도구로 활용될 수 있음을 확인하였다.

Zirconium(Zr) nuclear fuel cladding tubes are made using a three-time pilgering and annealing process. In order to remove the oxidized layer and impurities on the surface of the tube, a pickling process is required. Zr is dissolved in HF and HNO3 mixed acid during the process and pickling waste acid, including dissolved Zr, is totally discarded after being neutralized. In this study, the waste acid was recycled by adding BaF2, which reacted with the Zr ion involved in the waste acid; Ba2ZrF8 was subsequently precipitated due to its low solubility in water. It is very difficult to extract zirconium from the as-recovered Ba2ZrF8 because its melting temperature is 1031 oC. Hence, we tried to recover Zr using an electrowinning process with a low temperature molten salt compound that was fabricated by adding ZrF4 to Ba2ZrF8 to decrease the melting point. Change of the Zr redox potential was observed using cyclic voltammetry; the voltage change of the cell was observed by polarization and chronopotentiometry. The structure of the electrodeposited Zr was analyzed and the electrodeposition characteristics were also evaluated.

Nd-Fe-B permanent magnets have been used in a wide variety of applications because of their high magnetic flux density. So, demand for neodymium has been increasing in worldwide. In this study, an electrowinning process was performed in LiF-NdF3-Nd2O3 high temperature molten salts. However, a corrosion resistant material for use in the molten salt must be found for stable operation because of the harsh corrosion environment of the electrowinning process. Therefore, for this paper, boron nitride(BN), aluminum nitride(AlN), and silicon nitride(Si3N4) were selected as protective and structural materials in the high temperature electrolyte. To investigate the characteristics of BN, AlN, and Si3N4, in molten salts, materials were immersed in the molten salts for 24, 72, 120, and 192 hours. Also, surface condition and stability were investigated by SEM and EDS and corrosion products were calculated by HSC chemistry. As a result, among BN, AlN, and Si3N4, AlN was found to show the best protective material properties.