Cobalt (Co) is mainly used to prepare cathode materials for lithium-ion batteries (LIBs) and binder metals for WC-Co hard metals. Developing an effective method for recovering Co from WC-Co waste sludge is of immense significance. In this study, Co is extracted from waste cemented carbide soft scrap via mechanochemical milling. The leaching ratio of Co reaches approximately 93%, and the leached solution, from which impurities except nickel are removed by pH titration, exhibits a purity of approximately 97%. The titrated aqueous Co salts are precipitated using oxalic acid and hydroxide precipitation, and the effects of the precipitating agent (oxalic acid and hydroxide) on the cobalt microstructure are investigated. It is confirmed that the type of Co compound and the crystal growth direction change according to the precipitation method, both of which affect the microstructure of the cobalt powders. This novel mechanochemical process is of significant importance for the recovery of Co from waste WC-Co hard metal. The recycled Co can be applied as a cemented carbide binder or a cathode material for lithium secondary batteries.
고리 1호기는 원전해체 계획에 따라 영구정지 이후 가능한 한 빠른 시일 내에 원자로냉각재계통의 화학제염을 수행할 계획으로, 계통제염 기술 확보를 위해 한수원에서는 2014년부터‘원전 해체설계를 위한 냉각재계통 및 기기제염 상용기술 개발’연구과제를 통해 화학제염기술을 개발하고 있다. 본 연구를 위해 Lab. 규모 계통제염 공정장치를 제작하였으며, 계통제염 대상의 주요재료인 STS304, 316, 410, Alloy600, SA508을 사용하여 화학제염 공정실험을 수행하였다. 화학제염 공정실험의 목적은 산화-환원공정의 최적시간, 최적제염제 및 공정횟수를 도출하기 위함이다. 화학제염 공정실험은 과망간산-옥살산 기반의 단위공정 및 연속공정 실험, 과망간산+질산-옥살산 기반의 연속공정 실험으로 나누어 수행하였다. 그 결과 단위공정실험을 통해 최적공정 시간인 산화공정 5시간, 환원공정 4시간을 도출하였으며, 연속공정실험을 통해 최적제 염제와 공정횟수를 도출하였다. 최적제염제는 산화제의 경우 200 mg·L-1 과망간산 + 200 mg·L-1 질산이고, 환원제는 2000 mg·L-1 옥살산이며, 공정횟수는 STS304와 SA508의 경우 2 cycle, Alloy600의 경우 3 cycle 이상 수행하는 것이 적절할 것 으로 평가되었다.
Nano-sized Y2O3 powders were prepared via a sol-gel method starting with Y(NO3)3·6H2O (Yttrium(III) nitrate hexahydrate) and water with ethanol as a cosolvent. Y2O3 is an important rare earth oxide and has been considered for use in nuclear applications, such as ceramic materials, due to its excellent optical and refractory characteristics. It has been used as a chemically stable substrate, a crucible material for melting reactive metals, and a nozzle material for jet casting molten rare earth-iron magnetic alloys. Oxalic acid (C2H2O4) has been adopted as a chelating agent in order to control the rate of hydrolysis and polycondensation, and ammonia was added in order to adjust the base condition. The synthesized Y2O3 powder was characterized using TG/DTA, XRD, FE-SEM, BET and Impedance Analyzer analyses. The powder changed its properties in accordance with the pH conditions of the catalyst. As the pH increases according to the FE-SEM, the grain grew and it showed that the pore size decreased while confirming the effect of the grain size. The nano-material Y2O3 powders demonstrated that the surface area was improved with the addition of oxalic acid with ammonium hydroxide.