• 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.

• 한국진공학회:학술대회논문집
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• 한국진공학회 1999년도 제17회 학술발표회 논문개요집
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• pp.128-128
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• 1999

산소이온 전도체로 잘 알려진 Yttira-Stabilizd Ziroconia(TSZ)는 연료전지, oxygen pumps, chemical gas sensor 등 다양한 electrochemical divices에 이용되는 고체 전해질의 하나이다. 특히 YSZ는 oxygen 및 oxygen과 평형상태에 있는 gas들을 검출하는 sensor의 electrolyte로서 가장 많이 쓰이고 있다. 현재 상용화되어 있는 YSZ Sensor는 전통적인 bulk 형태의 ceramic으로 제작된 것으로 충분한 ionic conductivity를 얻기 위해서는 $600^{\circ}C$이상의 operating temperature를 필요로 하나 YSZ를 박막으로 제조시 낮은 operating temperature를 뿐만 아니라 sensor의 소형화, 낮은 ohmic loss 및 다양한 응용이 가능한 장점을 가질 수 있다. 본 실험에서는 산소 이온 전도체로서 8mol%-YSZ 고체전해질을 RF-magnetron bias sputtering 법을 이용하여 증착하였다. 제조된 YSZ 박막을 이용한 산소감응 센서셀 구조는 SiO2/Ni-NiO/Pt/YSZ/Pt-기판이다. 센서셀의 정상상태에서의 기전력(electromotive force ; EMF)을 산소분압(Po:1.013$\times$103Ta ~1.013$\times$105Pa)과 측정온도(30$0^{\circ}C$~$700^{\circ}C$)를 변화시키며 측정하였다. 이론적인 기전력과 측정값 사이의 편차는 Po:1.565$\times$104Pa 이하의 산소분압에서는 컸지만 이 이상의 분압에서는 이론치에 근접한 값을 가졌다. 증착한 YSZ와 Ni-NiO 박막의 구조는 X-ray diffractometer(XRD)를 이용하여 결정구조를 알아 보았고, TSZ 박막의 표면 morphology 관찰은 Scanning electron microscopy(SEM) 이용하였다. 박막의 조성분석은 X-ray energy dispersive analysis(EDX)을 사용하였다.

• 한국세라믹학회지
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• 제38권1호
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• pp.93-99
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• 2001

(La,Sr)MnO$_3$(LSM)-YSZ 복합체 양극에 있어서 소결온도 및 전극두께와 cathodic potential이 전극 특성에 미치는 영향을 고찰하였다. 양극의 소결은 삼상계면의 양을 결정하는 중요한 변수로 LSM 단미 양극과 YSZ가 40 wt% 포함된 LSM-YSZ 복합체 양극 모두 120$0^{\circ}C$에 소결했을 때 가장 낮은 분극저항을 나타내었다. 또한 양극 후막의 두께가 얇아지면 양극의 in-plane 저항이 증가하여 ohmic 저항이 증가하였는데, LSM-YSZ 복합체 양극의 경우 약 30$mu extrm{m}$ 정도의 전극두께가 가장 효과적인 전극 특성을 나타내었다. 한편, LSM-YSZ 복합체 양극에 -0.5 V의 cathodic potential을 인가함에 따라 양극에서 일어나는 산소환원반응의 활성이 증가하였는데, 1가 산소이온의 표면확산반응의 분극저항은 감소하였으나, 고주파수 영역에서 나타나는 산소이온전달반응의 저항은 거의 변화하지 않았다. 이것은 Mn의 환원에 의한 양극표면에 생성된 산소공공에 기인한다.

• 한국수소및신에너지학회논문집
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• 제28권6호
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• pp.663-668
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• 2017

SOFC anode fabricated core-shell using machano-fusion method using core with submicron size Ni, nano size YSZ for shell. Using prepared core-shell, depending on the thickness of the shell, we studied how the characteristics of sintering and SOFC cell change by sintering the anode. The Ni-YSZ core-shell has a Ni core of 0.5 to $1.2{\mu}m$ over 2 to 7 YSZ of 15 to 20 nm is, and as the high speed mixing time increases, the YSZ number increases and the shell thickness becomes uniform increased. When the fuel electrode is manufactured with core-shell, it has superior sintering property, has grain of uniform size compared with the one synthesized by general mixing, the falling path is short, the conductors (electrons and ions) connection is excellent, the electrical conductivity has become excellent. The thicker the shell, the lower the electrical conductivity. When the thickness of shell ranged from 46 to 139 nm and 61 to 81 nm, the performance was the highest and the ASR was the smallest.

• 한국세라믹학회지
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• 제43권12호
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• pp.805-811
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• 2006

The microstructural changes in Ni/YSZ anode substrate and crack formation during Ni oxidation were investigated. The composition of as-sintered anodes was 56 wt% NiO+44 wt% YSZ and that of electrolyte was 8 mol% yttria. After complete reduction, specimens were oxidized in $N_2$ + air at $600\sim800^{\circ}C$. Oxygen partial pressure was controlled in between 0.05 atm and 0.2 atm $O_2$. When the anode was oxidized, at higher than $690^{\circ}C$, three layers were formed in the specimens. The first was fully oxidized layer(NiO/YSZ), the second was a mixed layer and the third, near-intact layer. Under $640^{\circ}C$ such distinctive layers were not observed. Cracks formed at electrolyte layer when weight gain attained at $65\sim75%$ of the total gain due to complete oxidation despite of different oxidation temperature and oxygen partial pressure.

• 한국수소및신에너지학회논문집
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• 제28권1호
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• pp.40-46
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• 2017

We reviewed the electrical properties of SOFC anode manufactured using spherical Ni and nano YSZ powder. When core-shell is fabricated by using submicron Ni as core and nano-sized YSZ as shell for SOFC anode, the electrical conductivity of the $0.2{\mu}m$ Ni-YSZ core-shell was 3 times higher than that of $1.0{\mu}m$ NiO or $1.0{\mu}m$ Ni-YSZ. Hydrogen selectivity was similar at $800^{\circ}C$, but hydrogen selectivity and methane conversion rate under $750^{\circ}C$ was 10~25% higher, Power density was more than 2 times, ASR was about 1/3, when exposed to $H_2$ atmosphere at $750^{\circ}C$ for a long time, Ni particles did not have any growth or cut off conduction path.

• 한국세라믹학회지
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• 제41권3호
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• pp.229-234
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• 2004

수계슬러리의 동결건조 공정을 이용하여 배향성 기공을 갖는 NiO-YSZ 지지체를 제조하였다. 슬러리의 동결과정에서 형성된 얼음 결정은 진공건조 과정을 거치면서 승화되어 그 자리에 기공을 형성하였으며. 열전달 방향과 속도를 조절함으로써 얼음결정의 성장을 제어할 수 있음을 알 수 있었다. 제조된 NiO-YSZ 지지체는 배향성을 가진 거대(macro) 기공과 함께 표면에는 미세기공이 존재하는 독특한 기공구조를 형성하였다. 이것은 동결과정에 있어서 성형체의 위치에 따라 얼음의 성장속도가 다르기 때문에 발생하는 현상으로 생각된다. 얻어진 다공체 표면에 YSZ 슬러리를 dip 코팅하여 막을 형성한 후 140$0^{\circ}C$에서 동시소성(co-firing)하여 다공성 NiO-YSZ 지지체의 표면에 치밀한 YSZ 막이 코팅된 bilayer 제조에 성공하였다.

• 한국분말재료학회지
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• 제18권5호
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• pp.430-436
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• 2011

Joining of NiO-YSZ to 316 stainless steel was carried out with B-Ni2 brazing alloy (3 wt% Fe, 4.5 wt% Si, 3.2 wt% B, 7 wt% Cr, Ni-balance, m.p. 971-$999^{\circ}C$) to seal the NiO-YSZ anode/316 stainless steel interconnect structure in a SOFC. In the present research, interfacial (chemical) reactions during brazing at the NiO-YSZ/316 stainless steel interconnect were enhanced by the two processing methods, a) addition of an electroless nickel plate to NiO-YSZ as a coating or b) deposition of titanium layer onto NiO-YSZ by magnetron plasma sputtering method, with process variables and procedures optimized during the pre-processing. Brazing was performed in a cold-wall vacuum furnace at $1080^{\circ}C$. Post-brazing interfacial morphologies between NiO-YSZ and 316 stainless steel were examined by SEM and EDS methods. The results indicate that B-Ni2 brazing filler alloy was fused fully during brazing and continuous interfacial layer formation depended on the method of pre-coating NiO-YSZ. The inter-diffusion of elements was promoted by titanium-deposition: the diffusion reaction thickness of the interfacial area was reduced to less than 5 ${\mu}m$ compared to 100 ${\mu}m$ for electroless nickel-deposited NiO-YSZ cermet.

• 한국세라믹학회지
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• 제36권4호
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• pp.391-402
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• 1999

Characteristics of composite electrolytes which were prepared by coating a thin film of YSZ (yttria sta-bilized zirconia : (ZrO2)0.92 (Y2O3)0.08) on YDC (yttria doped ceria : Ce0.8Y0.2O1.9) with mixed conductivity have been investigated in order to develop the low-temperature solid oxide fuel cell. The thickness (t) of spin-coated YSZ thin films after the heat-treatment at 600$^{\circ}C$ was increased proportionally to the sol con-centrations (C) while the decrease in its thickness with the spin rate ($\omega$) could be expressed in the e-quation of ln t=9.49-0.53 ln $\omega$(0.99mol//s sol conc.) When the sol concentration and the spin rate being less than 0.99 mol/l and higher than 1000 rpm respectively reliable YSZ/YDC composite electrolytes could be obtained by multi-coating although several micro-cracks were observed in singly coated YSZ film surfaces. The dense YSZ film with a 1$\mu\textrm{m}$ thickness was prepared by coating of 0.99 mol/l YSZ sol five-times at 2000 rpm followed by heat-treatment at 1400$^{\circ}C$ for 2h, The adhesion between YSZ film and YDC substrate was found to be very good. The open circuit voltages of H2/O2 single cell with YSZ/YDC composite electrolytes were 0.79∼0.82 V at 800$^{\circ}C$ and 0.75∼0.77V at 900$^{\circ}C$ The open circuit voltage was inversely proportioned to the thickness ratio of YSZ thin film (1$\mu\textrm{m}$) to YDC substrate(0.28-2.22 mm)

• 한국결정성장학회지
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• 제21권1호
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• pp.21-26
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• 2011

Ni-YSZ(Yttria Stabilized Zirconia) composite powders를 glycine nitrate process으로 만들었다. 합성된 분말은 $1300{\sim}1400^{\circ}C$ 4시간 동안 소성하였으며 $1000^{\circ}C$에서 2시간 동안 질소 및 수소 분위기에서 환원 소성하여 Ni-YSZ cermet을 제조하였다. Ni의 부피비를 변화 시켜 각기 그들의 미세구조, 전기전도도, 열팽창 및 강도 특성을 알아보았다. Ni과 YSZ 상 사이에 상호 연결된 균질하게 분포된 다공성 미세구조를 얻을 수 있었다. 기공률, 전기전도도, 열팽창계수 및 곡강도 모두 Ni의 양에 민감하게 영향 받는 것을 알 수 있으며 40 vol%의 Ni를 함유한 Ni-YSZ cermet가 전극재료로 가장 적당하였다. $1350^{\circ}C$에서 소성한 40 vol% Ni-YSZ 시편의 경우 30 %의 기공율, 65.5 Mpa의 강도, 917.4 S/cm의 전기 전도도($1000^{\circ}C$)및 $12.6{\times}10^{-6}^{\circ}C^{-1}$의 열팽창계수($1000^{\circ}C$)를 가져 YSZ 전해질의 음극재료로 가장 적합하였다.