• 한국분말재료학회지
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• 제23권2호
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• pp.136-142
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• 2016

As precursors of cathode materials for lithium ion batteries, $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of $NH_4OH$ in air or nitrogen ambient. Calcination of the precursors with $Li_2CO_3$ for 8 h at $1,000^{\circ}C$ 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 $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$. Regardless of the atmosphere, the final powders exhibit the XRD patterns of $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ (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.

• 한국재료학회지
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• 제34권10호
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• pp.475-481
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• 2024

Lithium-ion batteries are widely used in various advanced devices, including electric vehicles and energy storage devices. As the application range of lithium-ion batteries expands, it will be increasingly important to improve their gravimetric and volumetric energy density. Layer-structured oxide materials have been widely adopted as cathode materials in Li-ion batteries. Among them, LiNiO₂ has attracted interest because of its high theoretical capacity, ~274 mAh g^-1, assuming reversible one Li⁺-(de)intercalation from the structure. Presently, such layered structure cathode materials are prepared by calcination of precursors. The precursors are typically hydroxides synthesized by coprecipitation reaction. Precursors synthesized by coprecipitation reaction have a spherical morphology with a size larger than 10 ㎛. Spherical precursors in the several micrometer range are difficult to obtain due to the limited coprecipitation reaction time, and can lead to vigorous collisions between the precursor particles. In this study, spherical and small-sized Ni(OH)₂ precursors were synthesized using a new synthesis method instead of the conventional precipitation method. The highest capacity, 170 mAh g^-1, could be achieved in the temperature range of 730~760 ℃. The improved capacity was confirmed to be due to the higher quality of the layered structure.

• 한국세라믹학회지
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• 제43권7호
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• pp.402-407
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• 2006

NiO/YSZ(70 wt%NiO) composite powders were prepared by ball-milling of 8YSZ and NiO precursors, dried and then followed by calcination. The approach was to combine acidic $Ni(NO_3)_2{\cdot}6H_2O$ and basic $2NiCO_3{\cdot}3Ni(OH)_2{\cdot}4H_2O$ via acid-base reaction as a mixed NiO precursor. Their effects were studied in the aspects of DSC, microstructure, porosity, and electrical conductivity. Ni/YSZ composite of 1N9C (1 mole NiO from the nitrate and 9 moles of NiO from the carbonate) was prepared by consolidation at $1400^{\circ}C$ for 3 h, and then followed by reduction at $1000^{\circ}C$ for 3 h under flowing of 6% $H_2/N_2$. It showed a homogeneous microstructure with ${\sim}20%$ porosity and 1880 S/cm at $1000^{\circ}C$.

• 한국분말재료학회지
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• 제23권4호
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• pp.287-296
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• 2016

$Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders have been synthesized in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH using $NH_4OH$ as a chelating agent. The co-precipitation temperature is varied in the range of $30-80^{\circ}C$. Calcination of the prepared precursors with $Li_2CO_3$ for 8 h at $1000^{\circ}C$ in air results in Li $Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ 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 $80^{\circ}C$ 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 $80^{\circ}C$ are inferior to those at $50^{\circ}C$. It is concluded that the optimum co-precipitation temperature is around $50^{\circ}C$.

• 전기화학회지
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• 제16권4호
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• pp.191-197
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• 2013

리튬2차전지용 양극소재인 $Li(Ni_{0.5}Co_{0.2}Mn_{0.3})O_2$를 공침법을 이용해 $Ni_{0.5}Co_{0.2}Mn_{0.3}(OH)_2$ 전구체로부터 합성하였고, 공침조건을 조절하여 전구체의 1차 입자 형상을 Flake형상과 Needle형상으로 제어하였다. 동일한 공정으로 리튬과 혼합하고 열처리하여, 입도, 탭밀도, 화학적 성분 등이 동일한 분체물성의 양극 소재를 합성하였다. 전구체의 1차입자 형상에 따른 $Li(Ni_{0.5}Co_{0.2}Mn_{0.3})O_2$의 전기화학적 특성을 평가하고, 이 특성의 변화를 SEM, XRD, EELS로 이용하여 분석하여 연관성을 고찰하였다. Needle형상 전구체로 합성한 $Li(Ni_{0.5}Co_{0.2}Mn_{0.3})O_2$ 양극의 1차입자는 Flake형상 전구체로 합성한 경우보다 작고, EELS결과로는 입자표면의 Li농도가 내부보다 상대적으로 높았다. 전기화학적인 수명과 출력특성에서 Needle형상 전구체로 합성한 양극이 Flake형상 전구체의 경우보다 우수한 특성을 보였는데, 임피던스 측정으로부터 낮은 전하이동저항에 연관되어 있을 것으로 생각된다.

• 센서학회지
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• 제23권3호
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• pp.211-215
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• 2014

The Pt-, Ni- and Cr-decorated tubular $SnO_2$ nanofibers for gas sensors were prepared by the electrospinning of polyvinylpyrrolidone (PVP) nanofibers containing Pt, Ni, and Cr precursors, the sputtering of $SnO_2$ on the electrospun PVP nanofibers, and the removal of sacrificial PVP parts by heat treatment at $600^{\circ}C$ for 2 h. Pt-decorated tubular $SnO_2$ nanofibers showed high response ($R_a/R_g=210.5$, $R_g$: resistance in gas, $R_a$: resistance in air) to 5 ppm $C_2H_5OH$ at $350^{\circ}C$ with negligible cross-responses to other interference gases (5 ppm trimethylamine, $NH_3$, HCHO, p-xylene, toluene and benzene). Cr-decorated tubular $SnO_2$nanofibers showed the selective detection of p-xylene at $400^{\circ}C$. In contrast, no significant selectivity to a specific gas was found in Ni-decorated tubular $SnO_2$ nanofibers. The selective and sensitive detection of gases using Pt-decorated and Cr-decorated tubular $SnO_2$ nanofibers were discussed in relation to the catalytic promotion of gas sensing reaction.

• 한국재료학회지
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• 제26권11호
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• pp.649-655
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• 2016

Ni nanoparticles (NPs)-graphitic carbon nanofiber (GCNF) composites were fabricated using an electrospinning method. The amounts of Ni precursor used as catalyst for the catalytic graphitization were controlled at 0, 2, 5, and 8 wt% to improve the photovoltaic performances of the nanoparticles and make them suitable for use as counter electrodes for dye-sensitized solar cells (DSSCs). As a result, Ni NPs-GCNF composites that were fabricated with 8 wt% Ni precursors showed a high circuit voltage (0.73 V), high photocurrent density ($14.26mA/cm^2$), and superb power-conversion efficiency (6.72%) when compared to those characteristics of other samples. These performance improvements can be attributed to the reduced charge transport resistance that results from the synergetic effect of the superior catalytic activity of Ni NPs and the efficient charge transfer due to the formation of GCNF with high electrical conductivity. Thus, Ni NPs-GCNF composites may be used as promising counter electrodes in DSSCs.

• 마이크로전자및패키징학회지
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• 제22권3호
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• pp.45-50
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• 2015

Glycine-nitrate와 citric acid를 이용하여 단상의 Ni-Zn ferrite, Ba-ferrite 나노입자와 두 나노복합체 ferrite의 전구체를 제조하고 이를 열처리하여 XRD 및 FT-IR로 각각의 상 분석을, SEM으로 분말의 형상과 크기를, VSM으로 자기적 특성과 합성된 나노복합체 ferrite에서의 exchange-coupling 상호작용을 확인하였다. XRD 분석 결과, 자전 연소법으로 얻은 전구체로 단상의 Ni-Zn ferrite와 Ba-ferrite 나노 입자 및 $BaFe_{12}O_{19}/Ni_{0.5}Zn_{0.5}Fe_2O_4$ 나노복합체 페라이트가 합성되었으며, 나노복합체에는 $BaFe_{12}O_{19}$와 $Ni_{0.5}Zn_{0.5}Fe_2O_4$가 잘 분포되어 있어 경자성과 연자성이 공존하고 있음을 확인하였고, 나노복합체 페라이트의 히스테리시스 곡선의 형상을 통해 경자성과 연자성 사이에 exchange-copuling이 잘 이루어졌음을 확인할 수 있었다. VSM으로 측정한 나노복합체의 경우. GNP로 제조한 precursor를 $900^{\circ}C$에서 하소한 $BaFe_{12}O_{19}/Ni_{0.5}Zn_{0.5}Fe_2O_4$ 나노복합체는 포화자화 81.69 emu/g, 잔류자화 38 emu/g, 보자력 2598.48G를 나타내었다. $Ni_{0.5}Zn_{0.5}Fe_2O_4/BaFe_{12}O_{19}$ 복합체에서 $BaFe_{12}O_{19}$의 무게비가 증가 할수록 보자력은 증가하였고, 포화자화값과 잔류자화 값은 감소하였다.

• 전기화학회지
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• 제8권1호
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• pp.42-46
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• 2005

It has been known that the synthesis of the cathode materials for the lithium rechargeable batteries by the sol-gel process has many advantages over the conventional solid-state method. It has been, however, a continuing issue that new additional steps should be introduced to commercialize this process. In this work, spray drying was introduced to the existing sol-gel process as a continuous mass production method of the pre-heat treatment precursor materials. The precursors of $LiCoO_2$ and $LiNi_{0.8}Co_{0.2}O_2$ were continuously produced through spray drying from the solution containing stoichiometric amount of lithium, cobalt, and nickel sources as well as a chelating agent. The process variables, such as pH of the starting solution, spray drying conditions, and calcination conditions were optimized. The XRD pattern for the synthesized material indicated a good crystallinity with a layered structure.

• 자원리싸이클링
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• 제28권5호
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• pp.60-67
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• 2019

금속 폐기물로부터의 유가금속 회수는 관련 원료의 수입 혹은 안정적 원료 수급을 위해서 매우 중요하다. 특히 폐리튬이차전지(LIBs)로부터 회수가 가능한 금속(Li, Co, Ni, Mn 등)의 재사용뿐만 아니라 폐리튬이차전지의 재활용 연구가 필수적이다. 폐리튬이차전지에서 회수된 수산화리튬($LiOH{\cdot}xH_2O$)은 촉매, 이산화탄소 흡수제 및 양극재의 전구체로 재사용이 가능하다. 본 연구에서는 폐리튬이차전지로부터 회수된 탄산리튬 전구체를 사용하였으며, 침전공정을 이용한 선택적인 리튬 분리를 통해 고순도 수산화리튬 분말의 제조 및 최적화 연구를 진행하였다. 수산화리튬 제조 조건으로는 교반을 기반으로 반응온도 $90^{\circ}C$, 반응시간 3 시간, 탄산리튬과 수산화칼슘의 비율 1:1의 조건에서 수행하였으며, 순도 향상을 위해 2-step 수산화리튬 제조 공정을 추가적으로 진행하여 최종적으로 고순도의 수산화리튬 제일수화물($LiOH{\cdot}xH_2O$)을 제조하였다.