In this study, we evaluated the effects of acid leaching on the properties of Cr powder synthesized using self-propagating high-temperature synthesis (SHS). Cr powder was synthesized from a mixture of Cr2O3 and magnesium (Mg) powders using the SHS Process, and the byproducts after the reaction were removed using acid leaching. The properties of the recovered Cr powder were analyzed via X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), particle size analysis (PSA), and oxygen content analysis. The results show that perfect selective leaching of Cr is challenging because of various factors such as incomplete reaction, reaction kinetics, the presence of impurities, and incompatibility between the acid and metal mixture. Therefore, this study provides essential information on the properties under acidic conditions during the production of high-quality Cr powder using a self-propagating high-temperature synthesis method.

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.

In this study, an experiment is performed to recover the Li in Li₂CO₃ phase from the cathode active material NMC (LiNiCoMnO₂) in waste lithium ion batteries. Firstly, carbonation is performed to convert the LiNiO, LiCoO, and Li₂MnO₃ phases within the powder to Li₂CO₃ and NiO, CoO, and MnO. The carbonation for phase separation proceeds at a temperature range of 600°C~800°C in a CO₂ gas (300 cc/min) atmosphere. At 600~700°C, Li₂CO₃ and NiO, CoO, and MnO are not completely separated, while Li and other metallic compounds remain. At 800 °C, we can confirm that LiNiO, LiCoO, and Li₂MnO₃ phases are separated into Li₂CO₃ and NiO, CoO, and MnO phases. After completing the phase separation, by using the solubility difference of Li₂CO₃ and NiO, CoO, and MnO, we set the ratio of solution (distilled water) to powder after carbonation as 30:1. Subsequently, water leaching is carried out. Then, the Li₂CO₃ within the solution melts and concentrates, while NiO, MnO, and CoO phases remain after filtering. Thus, Li₂CO₃ can be recovered.

Citations

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• Metals Recovery from Spent Lithium-ion Batteries Cathode Via Hydrogen Reduction-water Leaching-carbothermic or Hydrogen Reduction Process
  Tahereh Rostami, Behnam Khoshandam
  Mining, Metallurgy & Exploration.2024; 41(3): 1485.     CrossRef
• Influence of Flow-Gas Composition on Reaction Products of Thermally Treated NMC Battery Black Mass
  Christin Stallmeister, Bernd Friedrich
  Metals.2023; 13(5): 923.     CrossRef
• Holistic Investigation of the Inert Thermal Treatment of Industrially Shredded NMC 622 Lithium-Ion Batteries and Its Influence on Selective Lithium Recovery by Water Leaching
  Christin Stallmeister, Bernd Friedrich
  Metals.2023; 13(12): 2000.     CrossRef
• Environmentally Friendly Recovery of Lithium from Lithium–Sulfur Batteries
  Lilian Schwich, Bernd Friedrich
  Metals.2022; 12(7): 1108.     CrossRef
• Early-Stage Recovery of Lithium from Tailored Thermal Conditioned Black Mass Part I: Mobilizing Lithium via Supercritical CO2-Carbonation
  Lilian Schwich, Tom Schubert, Bernd Friedrich
  Metals.2021; 11(2): 177.     CrossRef
• Exploring a green route for recycling spent lithium-ion batteries: Revealing and solving deep screening problem
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  Journal of Cleaner Production.2020; 255: 120269.     CrossRef

In this paper, the recovery and nanoparticle synthesis of Ag from low temperature co-fired ceramic (LTCC) by-products are studied. The effect of reaction behavior on Ag leaching conditions from the LTCC by-products is confirmed. The optimum leaching conditions are determined to be: 5 M HNO₃, a reaction temperature of 75°C, and a pulp density of 50 g/L at 60 min. For the selective recovery of Ag, the [Cl]/[Ag] equivalence ratio experiment is performed using added HCl; most of the Ag (more than 99%) is recovered. The XRD and MP-AES results confirm that the powder is AgCl and that impurities are at less than 1%. Ag nanoparticles are synthesized using a chemical reduction process for recycling, NaBH4 and PVP are used as reducing agents and dispersion stabilizers. UV-vis and FE-SEM results show that AgCl powder is precipitated and that Ag nanoparticles are synthesized. Ag nanoparticles of 100% Ag are obtained under the chemical reaction conditions.

This study focuses on the development of an alkaline leaching hydrometallurgy process for the recovery of tungsten from WC/Co hardmetal sludge, and an examination of the effect of the process parameters on tungsten recovery. The alkaline leaching hydrometallurgy process has four stages, i.e., oxidation of the sludge, leaching of tungsten by NaOH, refinement of the leaching solution, and precipitation of tungsten. The WC/Co hardmetal sludge oxide consists of WO₃ and CoWO₄. The leaching of tungsten is most affected by the leaching temperature, followed by the NaOH concentration and the leaching time. About 99% of tungsten in the WC/Co hardmetal sludge is leached at temperatures above 90°C and a NaOH concentration above 15%. For refinement of the leaching solution, pH control of the solution using HCl is more effective than the addition of Na₂S·9H₂O. The tungsten is precipitated as high-purity H₂WO₄·H₂O by pH control using HCl. With decreasing pH of the solution, the tungsten recovery rate increases and then decrease. About 93% of tungsten in the WC/Co hardmetal sludge is recovered by the alkaline leaching hydrometallurgy process.

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• Fabrication of tungsten oxide powder from WC–Co cemented carbide scraps by oxidation behaviour
  Min Soo Park, Jong-Min Gwak, Kyeong-mi Jang, Gook-Hyun Ha
  Powder Metallurgy.2023; 66(5): 688.     CrossRef

Leaching of MOCVD dust in the LED industry is an essential stage for hydro-metallurgical recovery of pure Ga and In. To recover Ga and In, the leaching behavior of MOCVD scrap of an LED, which contains significant amounts of Ga, In, Al and Fe in various phases, has been investigated. The leaching process must be performed effectively to maximize recovery of Ga and In metals using the most efficient lixiviant. Crystalline structure and metallic composition of the raw MOCVD dust were analyzed prior to digestion. Subsequently, various mineral acids were tested to comprehensively study and optimize the leaching parameters such as acidity, pulp density, temperature and time. The most effective leaching of Ga and In was observed for a boiling 4 M HCl solution vigorously stirred at 400 rpm. Phase transformation of GaN into gallium oxide by heat treatment also improved the leaching efficiency of Ga. Subsequently high purity Ga and In can be recovered by series of hydro processes.

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• Selective Solvent Extraction of In from Synthesis Solution of MOCVD Dust using D2EHPA
  Byoungyong Im, Basudev Swain, Chan Gi Lee, Jae Layng Park, Kyung-Soo Park, Jong-Gil Shim, Jeung-Jin Park
  Journal of the Korean Institute of Resources Recycling.2015; 24(5): 80.     CrossRef
• Fabrication of High Purity Ga-containing Solution using MOCVD dust
  Duk-Hee Lee, Jin-Ho Yoon, Kyung-Soo Park, Myung-Hwan Hong, Chan-Gi Lee, Jeung-Jin Park
  Journal of the Korean Institute of Resources Recycling.2015; 24(4): 50.     CrossRef
• Influence of Oxidation Temperatures on the Structure and the Microstructure of GaN MOCVD Scraps
  Hyun Seon Hong, Joong Woo Ahn
  journal of Korean Powder Metallurgy Institute.1970; 22(4): 278.     CrossRef