• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2001년도 하계학술대회 논문집
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• pp.1080-1083
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• 2001

Ultrafine NiO/YSZ composite powders were prepared by using a glycine nitrate process for anode material of solid oxide fuel cells. The specific surface areas of synthesized NiO/YSZ composite powders were examined with controlling pH of a precursor solution and the content of glycine. The characteristics of synthesized composite powders were examined with X-ray diffractometer, a BET method with N$_2$absorption, scanning and transmission electron microscopy. The strongly acid precursor solution increased the specific surface area of the synthesized composite powders. This is suggested to be caused by the increased binding of metal ions and glycine under a strong acid solution of pH=0.5 that lets glycine consist of mainly the amine group of NH$_3$$\^$+/. After sintering and reducing treatment of NiO/YSZ composite powders synthesized by GNP, the Ni/YSZ pellet showed ideal micro-structure very fine Ni parties of 3-5${\mu}$m were distributed uniformly and fine pores around Ni metal particles were formed, thes, leading to an increase of the triple phase boundary among gas Ni and YSZ.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 1999년도 춘계학술대회 논문집
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• pp.422-425
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• 1999

Ultrafine NiO/YSZ (Yttria-Stabilized Zirconic) composite powders were prepared by using a glycine nitrate process (GNP) for anode material of solid oxide fuel cells. The specific surface areas of synthesized NiO/YSZ composite powders were examined with controlling pH of a precursor solution and the content of glycine. The binding of glycine with metal ions occurring in the precursor solution was analyzed by using FTIR. The characteristics of synthesized composite powders were examined with X-ray diffractometer, a BET method with $N_2$ absorption, scanning and transmission electron microscopies. Strongly acid precursor solution increased the specific surface area of the synthesized composite powders. This is suggested to be caused by the increased binding of metal ions and glycine under a strong acid solution of pH=0.5 that lets glycine consist of mainly the amine group of NH$_3$$^{+}$ After sintering and reducing treatment of NiO/YSZ composite powders synthesized by GNP, the Ni/YSZ pellet showed ideal microstructure very fine Ni Particles of 3-5${\mu}{\textrm}{m}$ were distributed uniformly and fine pores around Ni metal particles were formed, thus, leading to an increase of the triple phase boundary among gas, Ni and YSZ.Z.

• 한국세라믹학회지
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• 제37권5호
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• pp.479-490
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• 2000

The microstructure of Ni-YSZ composite as an anode of SOFC was investigated as a function of Ni content(10-70 vol%) in order to examine the correlation between microstructural-and electrical property. Image analysis based on quantitative microscopy theory was performed to quantify the microstructural property. We could get the informations about the size and distribution, contiguity and interfacial area of each phase or between the phases from the image analysis. According to the image analysis, contiguity between the same phae was mainly dependent on the amount of the phase while the contiguity between different phases was additionally influenced by the microstructural changes, especailly by the coarsening of the Ni phase. The whole length of pores perimeter was increased as Ni content increased, which indicated the overall microstructural evolution was mostly related with the coarsening of Ni phase. Ni-Ni interfacial area was also gradually increased as Ni content increased but controlled by pore phase at low Ni content region and by YSZ phase at intermediate Ni content region. These quantified microstructural properties were used to characterize the electrical properties of Ni-YSZ composite.

• 한국결정성장학회지
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• 제20권6호
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• pp.289-294
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• 2010

SOFC용 Ni-YSZ(Yttria Stabilized Zirconia) composite powders를 glycine nitrate process를 이용하여 만들었다. $ZrO(NO_3)_2{\cdot}2H_2O$, $Y(NO_3)_3{\cdot}6H_2O$, $Ni(NO_3)_2{\cdot}6H_2O$와 glycine을 출발원료로 하였으며 Ni의 부피비를 변화시켜 각기 그들의 소결 및 환원 특성을 알아보았다. Ni과 YSZ 상들이 상호 연결된 균질하게 분포된 다공성 미세구조를 관찰 할 수 있었으며 Ni의 첨가량에 따라 가공률이 민감하게 변화함을 알 수 있었다. 35 vol% 이상의 Ni를 함유한 Ni-YSZ cermet가 SOFC용 전극재료로 사용되는데 필요한 30% 이상의 공극을 갖는 조성임을 알 수 있었다.

• 한국세라믹학회지
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• 제38권2호
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• pp.137-142
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• 2001

SOFC 음극으로 쓰이는 Ni-YSZ 복합체의 제조과정 중에 생기는 조성의 변화를 관찰하였다. XRD를 이용하여 복합체 부위별로 상분석한 결과 Ni-YSZ 복합체는 소결과정이나 환원처리시 복합체 내-외부간의 조성차가 일어나며 이로 인해 전기적 물성의 불균일성이 나타난다. 복합체 조성의 불균일성 및 전기적 물성의 불균일성은 주로 복합체를 구성하는 Ni 성분의 변화에 기인했는데 소결과정이나 환원과정시 Ni 성분이 기판으로 확산해가거나 기상으로 증발해버려 Ni 손실이 생기기 때문인 것으로 나타났다. Ni 성분의 손실은 열처리 온도와 시간에 비례하여 커졌으며 이로 인해 복합체의 전기적 물성도 악화되었다.

• 한국세라믹학회지
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• 제43권12호
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• pp.764-767
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• 2006

Ni/YSZ $(Y_2O_3-stabilized\;ZrO_2)$ composite as an electrode component for High Temperature Electrolysis (HTE) was fabricated by mechanical alloying method using Ni and YSZ powders. Characterization of the synthesized composite was investigated with various analysis tools, including XRD, SEM and PSA, and a self-supporting planar unit cell prepared with the Ni/YSZ composite was prepared to study the electrochemical reactions for the production of hydrogen. The Ni/YSZ cermet is composed of crystalline Ni and YSZ, in a sub-micro scale, and has an even distribution without aggregated particles. In addition, under an electrochemical reaction, the unit cell showed an $H_2$ evolution rate from steam of 14 Nml/min and $600mA/cm^2$ of current density at the electrode.

• 한국수소및신에너지학회논문집
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• 제15권2호
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• pp.98-107
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• 2004

Modified Ni/YSZ cermets for high temperature electrolysis were synthesized by dry or wet mechanical alloying methods. The Ni/YSZ composit particle was directly fabricated from the ball milling of Ni and YSZ powder or obtained from the reduction of NiO/YSZ particle after the ball milling of NiO and YSZ. In the case of the NiO/YSZ composite particle, the dry milling increased the average particle size whereas the wet milling decreased the size. The dry milling showed that fine YSZ particles were distributed over large Ni surfaces while Ni and YSZ particles similar in size were well mixed in the wet milling method. These features were the same in the Ni/YSZ composite particle prepared from Ni and YSZ powders. The electrical conductivity of the wet-milled Ni/YSZ cermet showed the highest value of $2{\times}10^2S/cm$ among the specimens and this value was increased to $1.4\times10^4S/cm$ after the sintering at $900^\circ{C}$ for 1 h.

• 한국세라믹학회지
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• 제38권5호
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• pp.466-473
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• 2001

Ni-YSZ 음극의 미세구조와 임피던스특성에 미치는 YSZ 입자크기 및 소결온도의 영향을 고찰하였다. 0.3~0.6$\mu\textrm{m}$의 미세한 NiO 분말을 사용할 경우에는 NiO 분말과 크기가 비슷한 미세한 YSZ 분말(TZ8Y, 0.3$\mu\textrm{m}$)을 첨가했을 때 NiO의 입성장을 억제하는 효과가 가장 크고 환원후 Ni의 입자크기를 미세하게 유지할 수 있는 미세구조를 형성하였다. 또한 미세한 YSZ 분말 (TZ8Y, 0.3$\mu\textrm{m}$)과 조대한 YSZ 분말(FYT13.0, 2$\mu\textrm{m}$)의 혼합비를 달리하여 후막을 제조하였을 때에 TZ8Y 분말만 첨가한 조성이 가장 낮은 분극 저항을 나타내었다. 한편 소결온도는 삼상계면의 양과 분극저항에 영향을 주었으며, 140$0^{\circ}C$에서 소결한 시편의 분극저항이 가장 낮은 값을 나타내었다.

• 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 $1000^{\circ}C$.

• 한국세라믹학회지
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• 제37권12호
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• pp.1140-1145
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• 2000

Ni의 함량이 서로 다른 Ni-YSZ 복합체를 100$0^{\circ}C$ 환원 분위기 하에서 열처리하며 시간에 따른 미세구조의 변화를 관찰하였다. Quantitative microscopy 이론을 응용한 화상분석 결과 Ni-YSZ 복합체의 미세구조는 열처리시 나타나는 Ni상의 미세구조 변화에 가장 큰 영향을 받고 있었다. 특히 Ni의 양이 많은 조성에서는 Ni 상간의 접촉이 많아 고상반응에 의한 미세구조의 변화가 심하였는데 이로 인해 복합체 미세구조의 안정화가 느리게 진행되었다. Ni-YSZ 복합체의 전기 전도도 역시 Ni상의 미세구조 변화에 큰 영향을 받았는데 복합체 전체 미세구조의 경시변화와는 달리 Ni상의 많은 조성보다는 Ni상의 percolation이 일어나는 조성 부근에서 더 큰 영향을 받았다. 이로 인해 Ni-YSZ의 전기 전도도는 Ni의 percolation threshold 부근 조성에서 안정화되는데 더 많은 시간을 요하였다.