Chan Gi Lee

Recycling process for recovery of gallium from GaN an e-waste of LED industry through ball milling, annealing and leaching

Waste dust generated during manufacturing of LED contains significant amounts of gallium and indium, needs suitable treatment and can be an important resource for recovery. The LED industry waste dust contains primarily gallium as GaN. Leaching followed by purification technology is the green and clean technology. To develop treatment and recycling technology of these GaN bearing e-waste, leaching is the primary stage. In our current investigation possible process for treatment and quantitative leaching of gallium and indium from the GaN bearing e-waste or waste of LED industry dust has been developed. To recycle the waste and quantitative leaching of gallium, two different process flow sheets have been proposed. In one, process first the GaN of the waste the LED industry dust was leached at the optimum condition. Subsequently, the leach residue was mixed with Na2CO3, ball milled followed by annealing, again leached to recover gallium. In the second process, the waste LED industry dust was mixed with Na2CO3, after ball milling and annealing, followed acidic leaching. Without pretreatment, the gallium leaching was only 4.91 w/w % using 4M HCl, 100°C and pulp density of 20g/L. After mechano-chemical processing, both these processes achieved 73.68 w/w % of gallium leaching at their optimum condition. The developed process can treat and recycle any e-waste containing GaN through ball milling, annealing and leaching.

Valorization of GaN based metal-organic chemical vapor deposition dust a semiconductor power device industry waste through mechanochemical oxidation and leaching: A sustainable green process

Dust generated during metal organic vapor deposition (MOCVD) process of GaN based semiconductor power device industry contains significant amounts of gallium and indium. These semiconductor power device industry wastes contain gallium as GaN and Ga0.97N0.9O0.09 is a concern for the environment which can add value through recycling. In the present study, this waste is recycled through mechanochemical oxidation and leaching. For quantitative recovery of gallium, two different mechanochemical oxidation leaching process flow sheets are proposed. In one process, first the Ga0.97N0.9O0.09 of the MOCVD dust is leached at the optimum condition. Subsequently, the leach residue is mechanochemically treated, followed by oxidative annealing and finally re-leached. In the second process, the MOCVD waste dust is mechanochemically treated, followed by oxidative annealing and finally leached. Both of these treatment processes are competitive with each other, appropriate for gallium leaching and treatment of the waste MOCVD dust. Without mechanochemical oxidation, 40.11 and 1.86 w/w% of gallium and Indium are leached using 4M HCl, 100°C and pulp density of 100 kg/m(3,) respectively. After mechanochemical oxidation, both these processes achieved 90 w/w% of gallium and 1.86 w/w% of indium leaching at their optimum condition.

Leaching behavior of Ga and In from MOCVD dust

【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.】

Synthesis of Cu3(MoO4)2(OH)2 nanostructures by simple aqueous precipitation: understanding the fundamental chemistry and growth mechanism

Lindgrenite (Cu3(MoO4)2(OH)2) nanoflowers were synthesized through the simplest possible route by an aqueous chemical precipitation technique at room temperature without using any surfactants, template, expensive chemicals, complex instrumentation or tedious multistage synthesis process. Their morphology, structure, thermal properties, surface area, synthesis chemistry, and structural and growth mechanisms involved in the synthesis process were analyzed. Using XRD, FE-SEM, HR-TEM and FT-IR spectroscopy, their structure and morphology were analyzed. The thermal stability, surface area and porosity of the Cu3(MoO4)2(OH)2 nanoflowers were analyzed by TGA and BET. XRD analysis showed that the Cu3(MoO4)2(OH)2 nanoflowers have a pure monoclinic structure. The morphological analysis showed that the Cu3(MoO4)2(OH)2 nanoflowers are ∼10 μm in size, which are formed from self-assembly of thin nanosheets with a thickness of ∼20 nm. TGA indicated that the Cu3(MoO4)2(OH)2 nanoflowers are stable materials up to 328 °C and the isotherm from BET analysis indicated that the Cu3(MoO4)2(OH)2 nanoflowers are non-porous materials. The BET surface area of the synthesized Cu3(MoO4)2(OH)2 nanoflowers was found to be 21.357 m2 g−1. Moreover, the effects of the pH value and reaction time on the morphology of the Cu3(MoO4)2(OH)2 nanoflowers were studied and their optimization was performed. The results of the optimization study indicated that the reaction time and pH are two important parameters influencing the nucleation, growth, morphology, and synthesis mechanism. These flower-shaped Cu3(MoO4)2(OH)2 nanostructures are promising precursors for preparing molybdenum oxide materials which have various applications and can be synthesized in a very simple one-pot reaction system using commonly available chemicals without using a complex route.

Recycling of waste automotive laminated glass and valorization of polyvinyl butyral through mechanochemical separation.

Due to strong binding, optical clarity, adhesion to many surfaces, toughness and flexibility polyvinyl butyral (PVB) resin films are commonly used in the automotive and architectural application as a protective interlayer in the laminated glass. Worldwide million tons of PVB waste generated from end-of-life automotive associated with various environmental issues. Stringent environmental directive, higher land cost eliminates land filling option, needs a study, we have developed a mechanochemical separation process to separate PVB resins from glass and characterized the separated PVB through various techniques, i.e., scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), infrared spectroscopy (IR) and nuclear magnetic resonance spectroscopy (NMR). Commercial nonionic surfactants D201 used for the mechanochemical separation purpose. Through parameter optimization following conditions are considered to be the optimum condition; 30v ol% D201, stirring speed of 400 rpm, 35 °C temperature, operation time 1h, and dilute D201 volume to waste automotive laminated glass weight ratio of ≈25. The technology developed in our laboratory is sustainable, environmentally friendly, techno-economical feasible process, capable of mass production (recycling).

Selective recovery of silver from waste low-temperature co-fired ceramic and valorization through silver nanoparticle synthesis

Considering the value of silver metal and silver nanoparticles, the waste generated during manufacturing of low temperature co-fired ceramic (LTCC) were recycled through the simple yet cost effective process by chemical-metallurgy. Followed by leaching optimization, silver was selectively recovered through precipitation. The precipitated silver chloride was valorized though silver nanoparticle synthesis by a simple one-pot greener synthesis route. Through leaching-precipitation optimization, quantitative selective recovery of silver chloride was achieved, followed by homogeneous pure silver nanoparticle about 100nm size were synthesized. The reported recycling process is a simple process, versatile, easy to implement, requires minimum facilities and no specialty chemicals, through which semiconductor manufacturing industry can treat the waste generated during manufacturing of LTCC and reutilize the valorized silver nanoparticles in manufacturing in a close loop process. Our reported process can address issues like; (i) waste disposal, as well as value-added silver recovery, (ii) brings back the material to production stream and address the circular economy, and (iii) can be part of lower the futuristic carbon economy and cradle-to-cradle technology management, simultaneously.

A validation experiment on indium recovery by electrowinning of aqueous electrolytes: Optimization of electrolyte composition

Abstract A batch-type and lab-scale indium recovery method was developed via electrowinning (EW) to prove mass production-capability and economic recovery of indium from InCl3 crystals precipitated from the solvent extraction using a suitable phosphoric acid-based extractant. More precisely, the InCl3 crystals thus precipitated were further dissolved in three different aqueous electrolyte mixtures for subsequent electrowinning experiments: 0.05 M InCl3 – 0.7 M LiCl; 0.05M InCl3; 0.05 M InCl3 – 0.7 M NaCl. The effect of adding LiCl and NaCl supporting electrolytes to InCl3 on overall EW efficiency was thus comprehensibly investigated. Direct electroreduction of InCl3 using 0.05 M InCl3 aqueous electrolyte resulted in the highest indium metal purity of 99.996 % deposited on the copper cathode. Thus, metallic contents obtained from the validation experiments were further characterized using various analytical tools such as inductively coupled plasma/atomic emission spectroscopy (ICP/AES), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) and X-ray fluorescence (XRF).

Synthesis of cosmetic grade TiO2-SiO2 core-shell powder from mechanically milled TiO2 nanopowder for commercial mass production

TiO2 nanoparticles as an active sunscreen ingredient generate reactive oxygen species (ROS) upon UVA irradiation which is cytotoxic, genotoxic and potential to damage the DNA. The health concern and potential risks from TiO2 can be mitigated by shielding the particles through the suitable coating. Considering the advantages of SiO2, SiO2 coated TiO2 nanoparticles can be a potential material which can replace TiO2 for thickening, whitening, lubricating, and sunscreen ingredient in cosmetics. This article reports the synthesis of cosmetic grade TiO2-SiO2 core-shell nanopowder from mechanically milled TiO2 nanopowder for commercial mass production. From commercial TiO2 nanopowder was fabricated through size reduction by nanoset milling. Followed by the fabricated TiO2 nanopowder coated with SiO2 through sol-gel technique. A suitable optimum condition was explored for cosmetic grade TiO2-SiO2 core-shell nanopowder. Various physical properties and optical properties were analyzed. Synthesized of cosmetic grade TiO2-SiO2 core-shell nanopowder found to be at 100 nm size, with a homogeneous SiO2 coating having UVA protection factor 39 and sun protection factor (SPF) is 42. From the size, safety, and SPF perspective it can be an excellent cosmetic grade powder and from process simplicity perspective it can be commercially viable.

An investigation into the effective surface passivation of quantum dots by a photo-assisted chemical method

In this study, we have developed an effective amino passivation process for quantum dots (QDs) at room temperature and have investigated a passivation mechanism using a photo-assisted chemical method. As a result of the reverse reaction of the H2O molecules, the etching kinetics of the photo-assisted chemical method increased upon increasing the 3-amino-1-propanol (APOL)/H2O ratio of the etching solution. Photon-excited electron-hole pairs lead to strong bonding between the organic and surface atoms of the QDs, and results in an increase of the quantum yield (QY%). This passivation method is also applicable to CdSe/ZnSe core/shell structures of QDs, due to the passivation of mid-gap defects states at the interface. The QY% of the as-synthesized CdSe QDs is dramatically enhanced by the amino passivation from 37% to 75% and the QY% of the CdSe/ZnSe core/shell QDs is also improved by ∼28%.

Synthesis and analysis CdSe Quantum dot with a Microfluidic Reactor Using a Combinatorial Synthesis System

A microfluidic reactor with computer-controlled programmable isocratic pumps and online detectors is employed as a combinatorial synthesis system to synthesize and analyze materials for fabricating CdSe quantum dots for various applications. Four reaction condition parameters, namely, the reaction temperature, reaction time, Cd/Se compositional ratio, and precursor concentration, are combined in synthesis condition sets, and the size of the synthesized CdSe quantum dots is determined for each condition. The average time corresponding to each reaction condition for obtaining the ultraviolet-visible absorbance and photoluminescence spectra is approximately 10 min. Using the data from the combinatorial synthesis system, the effects of the reaction conditions on the synthesized CdSe quantum dots are determined. Further, the data is used to determine the relationships between the reaction conditions and the CdSe particle size. This method should aid in determining and selecting the optimal conditions for synthesizing nanoparticles for diverse applications.