The impact of different mixing methods and sintering temperatures on the microstructure and piezoelectric properties of PZNN-PZT ceramics is investigated. To improve the sinterability and piezoelectric properties of these ceramics, the composition of 0.13Pb((Zn_0.8Ni_0.2)_1/3Nb_2/3)O₃-0.87Pb(Zr_0.5Ti_0.5)O₃ (PZNN-PZT) containing a Pb-based relaxor component is selected. Two methods are used to create the powder for the PZNN-PZT ceramics. The first involves blending all source powders at once, followed by calcination. The second involves the preferential creation of columbite as a precursor, by reacting NiO with Nb₂O₅ powder. Subsequently, PZNN-PZT powder can be prepared by mixing the columbite powder, PbO, and other components, followed by an additional calcination step. All the PZNNPZT powder samples in this study show a nearly-pure perovskite phase. High-density PZNN-PZT ceramics can be fabricated using powders prepared by a two-step calcination process, with the addition of 0.3 wt% MnO2 at even relatively low sintering temperatures from 800°C to 1000°C. The grain size of the ceramics at sintering temperatures above 900°C is increased to approximately 3 μm. The optimized PZNN-PZT piezoelectric ceramics show a piezoelectric constant (d₃₃) of 360 pC/N, an electromechanical coupling factor (kp) of 0.61, and a quality factor (Q_m) of 275.

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Ni_1/3Co_1/3Mn_1/3(OH)₂ powders have been synthesized in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH using NH₄OH as a chelating agent. The co-precipitation temperature is varied in the range of 30-80°C. Calcination of the prepared precursors with Li₂CO₃ for 8 h at 1000°C in air results in Li Ni_1/3Co_1/3Mn_1/3O₂ powders. Two kinds of obtained powders have been characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analyzer, and tap density measurements. The co-precipitation temperature does not differentiate the XRD patterns of precursors as well as their final powders. Precursor powders are spherical and dense, consisting of numerous acicular or flaky primary particles. The precursors obtained at 70 and 80°C possess bigger primary particles having more irregular shapes than those at lower temperatures. This is related to the lower tap density measured for the former. The final powders show a similar tendency in terms of primary particle shape and tap density. Electrochemical characterization shows that the initial charge/discharge capacities and cycle life of final powders from the precursors obtained at 70 and 80°C are inferior to those at 50°C. It is concluded that the optimum co-precipitation temperature is around 50°C.

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• A kinetic descriptor to optimize Co-precipitation of Nickel-rich cathode precursors for Lithium-ion batteries
  Seon Hwa Lee, Ki Young Kwon, Byeong Kil Choi, Hyun Deog Yoo
  Journal of Electroanalytical Chemistry.2022; 924: 116828.     CrossRef

As precursors of cathode materials for lithium ion batteries, Ni_1/3Co_1/3Mn_1/3(OH)₂ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of NH4OH in air or nitrogen ambient. Calcination of the precursors with Li₂CO₃ for 8 h at 1,000°C in air produces dense spherical cathode materials. The precursors and final powders are characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analysis, tap density measurement, and thermal gravimetric analysis. The precursor powders obtained in air or nitrogen ambient show XRD patterns identified as Ni_1/3Co_1/3Mn_1/3(OH)₂. Regardless of the atmosphere, the final powders exhibit the XRD patterns of LiNi_1/3Co_1/3Mn_1/3O₂ (NCM). The precursor powders obtained in air have larger particle size and lower tap density than those obtained in nitrogen ambient. NCM powders show similar tendencies in terms of particle size and tap density. Electrochemical characterization is performed after fabricating a coin cell using NCM as the cathode and Li metal as the anode. The NCM powders from the precursors obtained in air and those from the precursors obtained in nitrogen have similar initial charge/discharge capacities and cycle life. In conclusion, the powders co-precipitated in air can be utilized as precursor materials, replacing those synthesized in the presence of nitrogen injection, which is the usual industrial practice.

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  Woonghee Choi, Chan Hyoung Kang
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Cathode materials and their precursors are prepared with transition metal solutions recycled from the the waste lithium-ion batteries containing NCM (nickel-cobalt-manganese) cathodes by a H₂ and C-reduction process. The recycled transition metal sulfate solutions are used in a co-precipitation process in a CSTR reactor to obtain the transition metal hydroxide. The NCM cathode materials (Ni:Mn:Co=5:3:2) are prepared from the transition metal hydroxide by calcining with lithium carbonate. X-ray diffraction and scanning electron microscopy analyses show that the cathode material has a layered structure and particle size of about 10 μm. The cathode materials also exhibited a capacity of about 160 mAh/g with a retention rate of 93~96% after 100 cycles.