[논문]Recovery of Gallium and Indium from Waste Light Emitting Diodes

Chen, Wei-Sheng; Chung, Yi-Fan; Tien, Ko-Wei

doi:10.7844/kirr.2020.29.1.81

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발광다이오드는 많은 양의 갈륨과 인듐을 함유하고 있어, 폐발광다이오드로부터 이들 원소의 회수는 최근 많은 관심을 받은 연구 분야이다. 본 연구에서는 폐발광다이오드에 포함된 질화갈륨으로부터 갈륨과 인듐을 회수하고자 시도하였다. 전체 공정은 물성분석, 알칼리배소, 침출의 세 단계로 구성되었다. 화학성분 분석결과 폐발광다이오드의 경우, 70.32% 갈륨, 5.31% 규소, 2.27% 알루미늄 및 2.07% 인듐이 함유됨을 확인하였다. 두 번째 단계인 알칼리배소 공정은 탄산나트륨과 함께, 900℃하에서 3시간의 반응이 최적 조건인 것으로 확인되었고, 이 공정을 통해 질화갈륨이 질화산화물로 변화되었다. 마지막은 침출 단계로서, 산의 종류 및 농도, 고액비, 반응시간에 따른 변화를 조사하여, 최적조건을 확립하였다. 최적조건은 반응온도 25℃ 및 2.0 M의 염산 환경에서 30 ml/g의 고액비와 반응시간 32분으로 나타났으며, 그 때의 침출 효율은 갈륨 96.88%와 인듐 96.61%로 나타났다.

Abstract ▼ AI-Helper

Recovery of gallium and indium from waste light emitting diodes has been emphasized gradually owing to high content of gallium and indium. This study was established the recovery of gallium (Ga3+) and indium (In3+) from waste gallium nitride was contained in waste light-emitting diodes. The procedur...

Recovery of gallium and indium from waste light emitting diodes has been emphasized gradually owing to high content of gallium and indium. This study was established the recovery of gallium (Ga3+) and indium (In3+) from waste gallium nitride was contained in waste light-emitting diodes. The procedure was divided into the following steps; characteristic analysis, alkaline roasting, and leaching. In characteristic analysis part, the results were used as a theoretical basis for the acid leaching part, and the chemical composition of waste light emitting diodes is 70.32% Ga, 5.31% Si, 2.27% Al and 2.07% In. Secondly, with reduction of non-metallic components by alkaline roasting, gallium nitride was reacted into sodium gallium oxide, in this section, the optimal condition of alkaline roasting is that the furnace was soaked at 900℃ for 3 hours with mixing Na2CO3. Next, leaching of waste light emitting diodes was extremely important in the process of recovery of gallium and indium. The result of leaching efficiency was investigated on the optimal condition accounting for the acid agent, concentration of acid, the ratio of liquid and solid, and reaction time. The optimal condition of leaching procedures was carried out for 2.0M of HCl liquid-solid mass ratio of 30 ml/g in 32minutes at 25℃ and about 96.88% Ga and 96.61% In were leached.

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그림 Fig. 1. (a) Microstructure analysis of waste light emitting diodes by scanning electron microscope (SEM).
그림 Fig. 1. (b) Characteristic analysis of waste gallium nitride by energy dispersive X-ray spectrometry (EDS).
표 Table 1. The content of waste light emitting diodes
그림 Fig. 2. XRD pattern of waste light emitting diodes.
그림 Fig. 3. XRD pattern of alkaline roasting at 800℃ for 3 hours.
그림 Fig. 4. XRD pattern of alkaline roasting at 900℃ for 3 hours.
그림 Fig. 5. XRD pattern of alkaline roasting at 1000℃ for 3 hours.
그림 Fig. 6. XRD pattern of alkaline roasting at 1100℃ for 3 hours.
그림 Fig. 7. XRD pattern of alkaline roasting at 900℃ for 2 hours.
그림 Fig. 8. XRD pattern of alkaline roasting at 900℃ for 3 hours.
표 Table 2. The leaching efficiency of pretreated LED dust by H₂SO₄, HCl, HNO₃, C₂H₂O₄ and NaOH with concentration of 5M at liquid-solid ratio 50 at 25℃
그림 Fig. 9. Leaching efficiency by various concentration of HCl [HCl] = 2.0M, L/S=50 with 500 rpm for 2 hours at 25℃.
그림 Fig. 10. Leaching efficiency by various liquid-solid ratio [HCl] = 2.0M, with 500 rpm for 2 hours at 25℃.
그림 Fig. 11. Leaching efficiency by various leaching time [HCl] = 2.0M, L/S=30 with 500 rpm at 25℃.

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문제 정의

However, the chemical stability of gallium nitride is stable, and the acid and alkali resistance make gallium difficult to recover⁵⁾. This research aims to conquer this tough problem and to recover gallium with high purity.
Compared with other reports, in this study, the research would focus on finding the most suitable acid concentration, reaction temperature, liquid-solid mass ratio and apposite oxidant added in the solution. The goal of this study was focus on the most suitable leaching condition on waste light emitting diodes.

제안 방법

In our current study, treatment of gallium nitride through oxidative roasting¹⁰⁾ followed by recovery of gallium through leaching from waste light emitting diodes. In this report would discuss the alkaline roasting with and Na₂CO₃ and query the optimize condition including roasting temperature, roasting time and solubilizer.
To acquire the optimal condition of alkaline roasting, the waste light emitting diodes samples were treated at 800, 900, 1000, 1100 and 1200°C for 3h/air with the ratio of waste LED dust over alkaline 1:1 and then characterized analysis by XRD.
This study proposed an operative method to leach gallium and indium effectively, and it was based on conducive to environmental technology and issues. Besides, the content of waste light emitting diodes was analyzed 70.

대상 데이터

The sample of gallium nitride used in the experiment was provided from a technology materials company. The original waste light emitting diodes were crushed and were adsorbed by powdered activated carbon.
The materials were analyzed by energy-dispersive X-ray spectroscopy (EDS; XFlash6110, Bruker, Billerica, MA, USA), X-ray diffraction (XRD; DX-2700, Dangdong City, Liaoning, China), scanning electron microscopy (SEM; S-3000N, Hitachi, Tokyo, Japan), X-ray fluorescence analyser (XRF, Spectro XEPOS), and inductively coupled plasma optical emission spectrometry (ICP-OES; Varian, Vista-MPX, PerkinElmer, Waltham, MA, USA).

후속연구

Nowadays, there are few relevant reports to deal with waste light emitting diodes, and the leaching agent such as oxalic acid, sulfuric acid¹¹⁾, nitrous acid, hydrochloric acid, and alkaline fusion-leaching are whole mentioned in this study. Compared with other reports, in this study, the research would focus on finding the most suitable acid concentration, reaction temperature, liquid-solid mass ratio and apposite oxidant added in the solution. The goal of this study was focus on the most suitable leaching condition on waste light emitting diodes.

참고문헌 (12)

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상세보기
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상세보기
Zhan, L., Xia, F., Ye, Q., et al., 2015 : Novel recycle technology for recovering rare metals (Ga, In) from waste light-emitting diodes, J. Hazard. Mater., 299, pp.388-394.

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Wang, Q., Yang, L., Chen, Y., et al., 2013 : Method for Recycling Germanium, Gallium, Indium and Selenium in Waste Diodes, CN102951618 A, China.
Chen, W.T., Tsai, L.C., Tsai, F.C., et al., 2012 : Recovery of gallium and arsenic from gallium arsenide waste in the electronics industry, Clean-Soil Air Water, 40, pp.531-537.

상세보기
Swain, B., Mishra, C., Kang, L., et al., 2015 : Recycling of metal-organic chemical vapor deposition waste of GaN based power device and LED industry by acidic leaching: Process optimization and kinetics study, J. Power Sources, 281, pp.265-271.

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Xu, K., Deng, T., Liu, J., et al., 2007 : Study on the recovery of gallium from phosphorus flue dust by leaching with spent sulfuric acid solution and precipitation. Hydrometallurgy, 86, pp.172-177.

상세보기
Li, L., Dunn, J.B., Zhang, X.X., et al., 2013 : Recovery of metals from spent lithium-ion batteries with organic acids as leaching reagents and environmental assessment, J. Power Sources, 233, pp.180-189.

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