The sulphate solutions came from a recycling LIBs waste cathode materials, which were done by previous research; their content is shown in Table 1 [18]. Sodium carbonate (Na2CO3) was purchased from Nihon Shiyaku Reagent, Tokyo, Japan (NaCO3, 99.8%), for the chemical precipitation. CO2 was purchased from Air Product and Chemical, Taipei, Taiwan (CO2 ≥ 99%), to carry out the hydrogenation–decomposition method. Dowex G26 was obtained from Sigma-Aldrich (St. Louis, MO, USA) and was used as a strong acidic cation exchange resin, to remove impurities. Multi-elements ICP standard solutions were acquired from AccuStandard, New Haven, Connecticut State, USA. The nitric acid (HNO3) and sulfuric acid (H2SO4) were acquired from Sigma-Aldrich (St. Louis, MO, USA) (HNO3 ≥ 65%) (H2SO4 ≥ 98%) 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), and inductively coupled plasma optical emission spectrometry (ICP-OES; Varian, Vista-MPX, PerkinElmer, Waltham, MA, USA). In order to
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control the hydrogenation temperature and heating rate, a thermostatic bath (XMtd-204;
