The capacity of high nickel Li(NixCoyMn1-x-y)O2 (NCM, x ≥ 0.8) cathodes is known to rapidly decline, a serious problem that needs to be solved in a timely manner. It was reported that cathode materials with the {010} plane exposed toward the outside, i.e., a radial structure, can provide facile Li+ diffusion paths and stress buffer during repeated cycles. In addition, cathodes with a core-shell composition gradient are of great interest. For example, a stable surface structure can be achieved using relatively low nickel content on the surface. In this study, precursors of the high-nickel NCM were synthesized by coprecipitation in ambient atmosphere. Then, a transition metal solution for coprecipitation was replaced with a low nickel content and the coprecipitation reaction proceeded for the desired time. The electrochemical analysis of the core-shell cathode showed a capacity retention of 94 % after 100 cycles, compared to the initial discharge capacity of 184.74 mA h/g. The rate capability test also confirmed that the core-shell cathode had enhanced kinetics during charging and discharging at 1 A/g.

Extensive research is being carried out on Ni-rich Li(NixCoyMn1-x-y)O2 (NCM) due to the growing demand for electric vehicles and reduced cost. In particular, Ni-rich Li(NixCoyMn1-x-y-zAlz)O2 (NCMA) is attracting great attention as a promising candidate for the rapid development of Co-free but electrochemically more stable cathodes. Al, an inactive element in the structure, helps to improve structural stability and is also used as a doping element to improve cycle capability in Ni-rich NCM. In this study, NCMA was successfully synthesized with the desired composition by direct coprecipitation. Boron and tin were also used as dopants to improve the battery performance. Macro- and microstructures in the cathodes were examined by microscopy and X-ray diffraction. While Sn was not successfully doped into NCMA, boron could be doped into NCMA, leading to changes in its physicochemical properties. NCMA doped with boron revealed substantially improved electrochemical properties in terms of capacity retention and rate capability compared to the undoped NCMA.

Magnetite particles were synthesized by co-precipitation of water-soluble 밀 스케일-derived precursor by various concentrations of (0.5, 0.67, 1, 2 N) NaOH and (0.6, 0.8, 1.2, 2.4 N) NH4OH. It is theoretically known that as the concentration of the alkaline additive used in iron oxide synthesis increases, the particle size distribution of that iron oxide decreases. This trend was observed in both kind of alkaline additive used, NaOH and NH4OH. In addition, the magnetite synthesized in NaOH showed a relatively smaller particle size distribution than magnetite synthesized in NH4OH. Crystalline phase of the synthesized magnetite were determined by X-ray diffraction spectroscopy(XRD). The particles were then used as an adsorbent for phosphate(P) removal. Phosphorus adsorption was found to be more efficient in NaOH-based synthesized magnetite than the NH4OH-based magnetite.

Ni1/3Co1/3Mn1/3(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 30-80oC. Calcination of the prepared precursors with Li2CO3 for 8 h at 1000oC in air results in Li Ni1/3Co1/3Mn1/3O2 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 80oC 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 80oC are inferior to those at 50oC. It is concluded that the optimum co-precipitation temperature is around 50oC.

As precursors of cathode materials for lithium ion batteries, Ni1/3Co1/3Mn1/3(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 Ni1/3Co1/3Mn1/3(OH)2. Regardless of the atmosphere, the final powders exhibit the XRD patterns of LiNi1/3Co1/3Mn1/3O2 (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.

This study was carried out for characterization of MIO synthesized in our laboratory by co-precipitation method and applied isotherm and kinetic models for adsorption properties. XRD analysis were conducted to find crystal structure of synthesized MIO. Further SEM and XPS analysis was performed before and after phosphate adsorption, and BET analysis for surface characterization. Phosphate stock solution was prepared by KH2PO4 for characterization of phosphate adsorption, and batch experiment was conducted using 50 ml conical tube. Langmuir and Freundlich models were applied based on adsorption equilibrium test of MIO by initial phosphate solution. Pseudo first order and pseudo second order models were applied for interpretation of kinetic model by temperature. Surface area and pore size of MIO were found 89.6 m2/g and 16 nm respectively. And, the determination coefficient (R2) value of Langmuir model was 0.9779, which was comparatively higher than that of Freundlich isotherm model 0.9340.

가압 경수형 원자로 (pressurized light water reactor) 냉각재 계통 내의 주된 분식 생성물로 알려져 있는 nickel ferrite의 거동에 대해 고찰하기 위해 모의 nickel ferrite(Ni0.75Fe2.25O4)를 공침법으로 제조하였다. 수용액-pH-조절로는 am-monia 또는 potassium carbonate를, 공침물-세척제는 ammonia 수용액이나 potassium carbonate 수용액 또는 2차 증류수를 사용하였다. Nickel ferrite의 생성 및 수용액-pH-조절제와 공치물-세척제가 최종 생성물의 Ni-Fe 몰 비에 따른 수율 및 특성에 미치는 영향은 EDX, XPS, XRD 및 SEM으로 고찰하였다. 반응 전.후 Ni/Fe 몰 비에 따른 수율은, pH를 potassium carbon-ate로 조절한 후 2차 증류수로 공침물을 세척한 경우가 0.994로 가장 높이 나왔으며, pH-조절제로 potassium carbonate를 사용한 경우가 ammonia를 사용한 경우에 비해 높은 수율을 나타냈다. 이러한 차이는 공침 시에 수용액 내에서 ammonia가 보여주는 상대적으로 큰 Na2+←NH3 착화 효과와 더불어 공침물-세척제의 pH에 기인하는 것으로 해석하였다.

공침법을 이용하여 In2O3가 0-10 wt.% 첨가된 SnO2 계 미세 분말을 합성한 후, 스크린 인쇄법(screen printing)으로 후막형 가스센서를 제조하고 탄화수소(C3h8, C4h10) 가스에 대하여 가스 감응 특성을 조사하였다. In2O3는 SnO2의 입자 성장을 억제시키기 위하여 첨가해 주었는데, 600˚C에서 하소한 후에도 수 nm 크기의 미세한 입자를 얻을 수 있었다. 공침시 pH 값은 SnO2 의 입자 크기에 영향을 거의 미치지 않은 반면, In2O3 첨가량은 입자 크기와 미세 구조에 큰 영향을 주었다. In2O3 첨가량이 증가할수록 입자 크기는 감소하고 비표면적은 증가하였으며, 센세의 동작 온도를 약 500˚C로 하여 측정한 가스 감응 특성은 3wt.% 첨가했을 때 최대 감도를 나타내고 그 이상의 첨가량에서는 오히려 저하되었다. 3wt.%의 In2O3첨가시 SnO2의 입자 크기와 비표면적은 각각 9.5nm, 38m2/g이었다. 임피던스 측정으로부터 얻은 단일 반원의 Nyquist curve와 선형의 전류-전압(1-V)특성 곡선으로부터, In2O3를 첨가하여 수nm로 입자 크기를 억제한 SnO2 계 가스센서는 미세 입자들끼리 형성한 치밀한 응집체와 이들 간의 계면(boundary)에 의해서 가스 감응 특성이 영향을 받음을 알 수 있었다.

공침법으로 제조된 비정질 PbTiO3전구체의 결정화거동과 구조적 변화를 XRD, 라만스펙트럼, TEM, RDF등으로 조사하였다. 전구체는 이온안정제로 H2O2혹은 NH4NO3를 사용하여 제조된 질산납과 사염화티탄의 혼합수용액으로부터 45˚C, pH 9에서 제조되었다. 이온안정제로 H2O2를 사용한 경우보다 NH4NO3를 사용하여 제조된 공침물이 더 낮은 온도에서 결정화가 시작되며 결정화의 활성화에너지도 더 작은 값을 가진다. 비정질의 공침물은 transient phase를 거쳐 결정 PbTiO3로 변태된다. 비정질 상태의 평균 원자거리는 열처리온도의 증가에 따라 감소한다.

[ ZrO2+Y2O3 ] 계 분말결정을 ZrOCl2·8HO-YCl33·6H2O를 출발물질로 하여 공침법으로 합성하였다. 출발물질의 농도, 용액의 pH, 부분안정화제로 사용된 Y2O3의 양, 합성 후 소결온도 등 합성에 요구되는 실험변수에 따른 상 변이에 대한 연구결과를 바탕으로 실험조건을 고정시켜 3 mole% Y2O3를 포함하는 부분안정화 지르코니아 3YSZ를 합성할 수 있었다. 합성된 3YSZ의 소결특성에 따른 ZrO2 상전이에 대한 연구를 위하여 XRD, Raman, DTA 및 SEM을 사용하였다. 순수한 ZrO2에 비하여 합성된 3YSZ는 ZrO2+Y2O3 계에서 Y2O3의 함량 면화에 따라 순수한 ZrO2고온상의 단사정상에서 정방정상으로 상전이가 일어나게 되고 이때 Raman 스팩트럼이 낮은 파수쪽에서 현저하게 나타나는 것으로 쉽게 구분이 되었다.