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1 Jurnal f the Krean Ceramic Sciety Vl. 48, N. 6, pp. 520~524, 속 보 The Prperties f the Manufactured SOFC Unit Cell using Decalcmania Methd Mi-Jai Lee, Bit-Nan Kim, Tae-Yung Lim, Sei-Ki Kim, and Byung-Hyun Chi Electrnic Materials Labratry, Krea Institute f Ceramic Engineering and Technlgy, Seul , Krea (Received Octber 11, 2011; Revised Nvember 11, 2011; Accepted Nvember 14, 2011) 전사법을이용하여제조한 SOFC 단전지의특성분석 이미재 김빛남 임태영 김세기 최병현한국세라믹기술원전자광소재센터 (2011 년 10 월 11 일접수 ; 2011 년 11 월 11 일수정 ; 2011 년 11 월 14 일채택 ) ABSTRACT The prperties f manufactured SOFC unit cell using decalcmania methd were investigated. The decalcmania methd that used in ceramics, dish, vessel and etc. was the very simple prcess. The SOFC unit cell manufacturer using decalcmania methd is very simple prcess. Especially, the decalcmania methd was the mst suitable manufacturing methd fr the segmented type SOFC. The cathde, prevent diffusin layer (PDL), ande functinal layer (AFL) and electrlyte were manufactured using decalcmania methd n prus ande supprt. The sintered electrlyte at 1450 C fr 2 h using decalcmania methd was very dense, and the thickness was abut 10 µm. The cathde, the PDL and the AFL were manufactured using decalcmania methd and was sintered at 1250 C fr 2 h, and the sintered electrdes were the prus. As a result, with humidified hydrgen used as fuel, the cell with an 15 µm-thick AFL exhibited maximum pwer densities f 0.246, 0.364, W/cm 2 at 700, 750, 800 C, respectively. Key wrds : Decalcmania methd, SOFC, Segmented type, Ande functinal layer 1. 서론 고체산화물연료전지 (Slid Oxide Fuel Cell) 는전지의모든부분이산화물로이루어져있어내구성과효율이높을뿐만아니라고가의촉매를사용하지않아도되는장점이있다. 하지만연료전지의특성상출발물질의가격이비쌀뿐만아니라세라믹으로이루어져있어형태및크기에많은제한이따르고, 복잡한형상을구현하기가어렵다는단점이있다. 이러한문제점들을해결하기위해서 cell 의구조를변화하여반응면적의극대화를통해 stack 의크기를줄이거나, 새로운물질을개발 적용하여높은효율을가지는 SOFC 의개발이활발히진행중이다. 1-5) 이러한연구중 segmented type SOFC 는하나의지지체에여러개의전지를형성하는방법으로, 이런구조를형성하게될경우단전지사이의거리가짧아 cmpact 한구조를가질뿐만아니라전극과 IC 에서발생하는 hmic lss 를최소화하며단위부피당전력효율이높고, 기계적강도가우수하고밀봉이간단하고열응력내구성이높다는장점을가지고있다. 6-8) 하지만 screen printing 과같은방법으로는지지체위에여러개의전지를형성할때에굴곡이있는지지체의모서리는전지를형성할수없기때문에추가로밀봉을해야한다는단점이있다. 이러한밀봉의어려움을해결하면서지지체의굴곡이있는모서리에도전지를형성함으로써반응면적을극대화하기위해전사지를이용하여전극을제조하는방법을사용하였다. 전사지법이란 Fig. 1 에나타냈듯이주변에서흔히사용하고있는그릇이나컵과같은굴곡이있는도자기에무늬를넣는방법으로원하는모양과크기로제조할수있을뿐만아니라제조공정이간단하며굴곡이있는면에도쉽게적용할수있다는장점을가지고있다. Crrespnding authr : Mi-Jai Lee Tel : Fax : Fig. 1. The decalcmania methd. 520

2 전사법을이용하여제조한 SOFC 단전지의특성분석 521 따라서본연구에서는연료극지지체를제외한공기극, 확산방지층, 연료극기능층을전사법으로제조하여연료극지지체위에적용한 SOFC 단전지를제조하고, 연료극기능층에따른전해질의미세구조특성을평가하였다. 또한최적의조건에서제조한단전지의계면및단면의미세구조를분석하고, 공기극의분극특성및출력을측정하였다. 2. 실험방법 전사지제조를위한공정은 Fig. 2 에나타내었는데, 출발물질로는연료극과연료극기능층은 YSZ (8 mle% Yttria dped Zircnia) 와 NiO 를, 전해질은 YSZ, 공기극은 (La 0.6 Sr 0.4 )(C 0.2 Fe 0.8 )O 3, 확산방지층은 GDC (10 mle% Gd dped Ceria) 를사용하여제조하였다. 전사지는전극분말과전사페이스트를 1:0.5 의비율로하여고속혼합기를이용하여혼합한뒤전사종이위에 screen print 를이용하여코팅한후 40 C 에서 2 시간동안건조한뒤다시전사오일을전면에코팅하여 40 C 에서 2 시간동안건조하여제조하였 Fig. 2. The manufacture prcess fr the decalcmania methd. 다. 이때사용한전극분말은연료극기능층의경우 NiO : TZ8Y 의비율을 60 : 40 으로하였으며, 전사지를제조할때에 binder 의함량이높기때문에바인더의 burn ut 으로인한기공형성을고려하여기공형성제는첨가하지않았다. 전해질의경우 Tsh 분말을사용하였고, 또한전해질과공기극의반응에의해생성되는 2 차상을막기위해입자크기 0.3 µm 의 GDC 를확산방지층으로사용하였으며공기극은입자크기 0.3 µm 의 LSCF 를사용하였다. 이와같은공정으로제조한전사지와전사지를이용하여제조한 unit cell 을 Fig. 3 에나타내었는데, Fig. 3(a) 는전사지를 cell 의크기에맞게원형으로제작한사진으로, 제조한전사지를이용하여연료극지지체에전극을제조한 unit cell 을 Fig. 3(b) 에나타내었다. 제조한 unit cell 에서연료극지지체의직경은 20 mm, 두께는 2.5 mm 였으며 PDL 과공기극의경우직경 15 mm 로반응면적은 mm 2 를가졌다. 연료극지지체는 NiO:TZ8Y 의비율을 60 : 40 으로하고기공형성제로활성탄을 15 wt% 첨가하여 ball mill 을이용하여 24 시간동안혼합한뒤 80 C 에서 24 시간동안건조한분말을직경 30 mm, 두께 3.5 mm 의 pellet 으로성형하였다. 성형한연료극지지체는 600 C 에서 2 시간동안 burn ut 한뒤 1250 C 에서 4 시간동안가소결하였다. 가소결된연료극지지체위에연료극기능층전사지를코팅하여 600 C 에서 2 시간동안 burn ut 한뒤 1250 C 에서 4 시간동안가소결하였다. 전해질의경우코팅된연료극기능층위에전해질전사지를 2 회코팅한뒤 600 C 에서 2 시간동안 burn ut 하여 1450 C 에서 4 시간동안소결하였는데, 이때 dense 한전해질층을얻기위해 100 C/h 로천천히냉각하였다. 공기극과전해질층사이에는확산방지층으로써 GDC 를사용하였으며 GDC 는 1 회코팅하고 LSCF 를 2 회코팅하여 600 C 에서 2 시간동안 burn ut 한뒤 1250 C 에서 4 시간동안소결하여완성된 cell 을얻었다. 기공율의경우전사지제조와동일한혼합조성으로시편을제조한후단전지제조와같은조건에서열처리하여, 수은압입법을이용한 Prsimeter (Micrmerics 사, Autpre IV) 를이용하여측정하였다. 교류임피던스의경우전사지로제조한각전극을 YSZ 전해질지지체위에형성하여, 800 C 에서 Frequency Respnse Analyzer (Slatrn, SI1260) 와 Ptentistat/Galvanstat (Slatrn, SI1287) 을사 Fig.3. The shape f the manufacturing decalcmania paper and the manufacture unit cell using it. 제 48 권제 6 호 (2011)

3 이미재 김빛남 임태영 김세기 최병현 522 용하여 측정하였다. 측정 시 주파수 범위는 0.1 Hz~100 khz 이고 amplitude는 10 mv였다. 이때 H2 gas의 유량은 200 ml/min으로 하였으며 각각 800C에서 2시간동안 환원 시킨 뒤 800, 750, 700 C로 온도를 내리면서 측정하였다. 또 한 전사지를 이용하여 제조한 단전지는 700, 750, 800C에서 출력을 측정하였다. 3. 결과 및 고찰 제조한 전사지의 열처리 조건 확립 및 열처리 시 전지 내부에 존재하는 il의 잔류 회분량을 확인하기 위해 측 정한 전사 il의 TG-DSC 측정 결과를 Fig. 4에 나타내었다. 그림의 TG를 살펴보면, 약 400C에서 전사 il의 질량이 모두 감소하는 것을 확인할 수 있는데 이는 400C에서 전사 il이 모두 burn ut 된다는 것을 알 수 있다. 또한 DSC 그래 프에서 흡열 피크가 나타나고 C에서 모든 반응이 끝 나는 것으로 보아 전사 il에 함유되어 있는 유기용매 및 Fig. 4. TG-DSC f decalcmania il. Fig. 6. SEM phtgraphs f the unit cell cmpnents. 한국세라믹학회지 바인더가 약 550 C에서 열에 의해 모두 burn ut 된다는 것을 알 수 있었다. Fig. 5에 다공성인 연료극 지지체 표면 위에 치밀한 전해 질을 형성하기 위해 연료극 기능층을 전사지를 이용하여 0회부터 3회까지 처리하였을 때 전해질 표면의 미세구조를 나타내었다. 연료극 기능층 처리 횟수를 증가시킴에 따라 점차 치밀한 전해질 층을 형성할 수 있었는데, 0회와 1회 처리한 경우 연료극 지지체의 기공으로 인해 전해질의 표면 에 크랙 또는 기공이 형성되어 있는 것을 확인할 수 있 었다. 이에 반해 연료극 기능층을 2회 처리한 경우와 3회 처리한 경우 치밀한 전해질 층을 형성하였는데, 3회 형성한 경우는 도리어 두꺼운 연료극 기능층으로 인해 전해질 표 면이 고르지 않게 형성되는 경향을 나타내었다. Fig. 6과 Fig. 7에는 연료극 기능층을 전사지로 2회 처리 하여 제조한 단전지의 미세구조와 계면 사진을 나타내었 Fig. 5. SEM phtgraphs f the electrlyte accrding t the number f decalcmania treatment.

4 전사법을이용하여제조한 SOFC 단전지의특성분석 523 Fig. 7. SEM phtgraphs f the unit cell. 다. Fig.6 에서살펴보면, 연료극지지체, 연료극기능층, 공기극및확산방지층모두다공성구조를나타내고있으며, 전해질의경우는치밀한조직을나타내고있었다. 각구성요소의기공율을측정한결과연료극지지체의경우약 32%, 연료극기능층의경우는약 28%, 확산방지층은약 23%, 공기극은 39% 의기공을가지고있었으며, 전해질의경우는 0.8% 정도를나타내었다. Fig. 7 의 (a) 는연료극기능층을적용하지않은사진이고, (b) 는연료극기능층을 2 층적용한계면사진을나타낸것으로연료극기능층을형성하지않은 (a) 의경우치밀한전해질이 10 µm 두께로형성되어있고, 연료극기능층을 2 층적층한 (b) 의경우다공성연료극지지체위에약 10 µm 정도두께를갖는다공성의연료극기능층이형성되어있고, 그위에치밀한 10 µm 정도의전해질층이형성되어있는것을확인할수있었다. 치밀한전해질층위에는약 15 µm 내외의공기극과확산방지층이형성되어단전지를형성하고있는것을볼수있었다. Fig. 8 은전사지를이용하여제조한단전지의 800 C 에서측정한교류임피던스특성을 cle-cle plt 한결과이다. 일반적으로 SOFC 단전지의경우 cle-cle plt 에서좌측반원의좌측실수부시작점을단전지스택의 IR (hmic) 저항으로, 여기에좌측반원의끝지점혹은우측반원의시작지점을 IR 저항과분극 (plarizatin) 저항의합에의한저항으로, 우측반원의끝지점을 IR 저항, 분극저항, 물질전달 (mass transfer) 저항의합에의한저항으로분해하여분석한다고보고되어있다. 본실험에서측정한결과를살펴보면먼저 IR 저항에있어서약 0.1 Ω 이며, 분극저항을나타내는우측반원의경우약 0.06 Ω 정도를나타내고있어전체저항의합은약 0.16 Ω 을나타내었다. 일반적으로공기극의산화환원반응기구를두단계반응으로나누어생각해볼수있는데, 산소이온의확산반응과산소이온의표면확산이다. 이러한반응은전극 / 전해질 / 기상이만나는삼상계면의양에따라달라지는데, 산화환원반응의활성점인삼상계면의양이많으면전극의분극저항이감소하고, 삼상계면의양이적으면분극저항이증가한다고알려져있다. 9) 또한, 보통 IR 저항은 gas 농도에따라변하지않으나, mass transprt 와 kinetics 와관계된 impedance 부분은전극의공극에따라변화한다고보고되고있으며, 고주파수영역반원은가스 Fig. 8. AC impedance spectra f the unit cell (800 C). Fig. 9. Perfrmance f the unit cell with hydrgen at different temperature. 분압에대한의존성이거의없으나다른반원은가스분압에따라변화한다고보고되고있다 ) 본연구에서전사법으로제조한 SOFC 단전지에있어서분극저항에가장큰영향을미치는것은기공에의한영향으로, 약 3mm 두께로제조된연료극지지체와 15 µm 내외로제조된공기극의두께와기공률차이에의해발생되는삼상계면의차이에의해발생하는것으로생각되어지는데, 제조한공기극은비교적낮은기공율가지고있으며, 이로인해산화환원반응의활성점인삼상계면이적어져비교적높은저항을갖는것으로보인다. 또한, 측정한 impedance 의경우오른쪽반원이 0 에교차하지않고있는것을볼수있는데, 이는 mass transfer 저항이큰것으로보여지며, 이는비교적낮은기공을갖는공기극으로인한삼상계면의감소하고, 이로인해 mass transprt prcess 가 electrchemical prcess 에비해상대적으로느리게진행되기때문이라고생각되어진다. Fig. 9 에는연료극기능층을 2 회처리하였을때가장치밀한전해질구조를형성한단전지의출력특성을나타내었다. 출력특성을살펴보면 700 C 에서 W/cm 2, 750 C 에서 W/cm 2, 800 C 에서 W/cm 2 의출력을나타내었다. 따라서, 전사지를이용한단전지제조에있어비교적기공 제 48 권제 6 호 (2011)

5 524 이미재 김빛남 임태영 김세기 최병현 의양이많은전극을형성하여활성점인삼상계면의양이많아지면전극의분극저항이감소하여좀더양호한특성을갖는전지를제조할수있을것으로생각되어진다. 4. 결론 전사법을이용하여제조한단전지의특성분석연구에서복잡한형상에적용이가능한방법인전사법을이용하여단전지를제조하였다. 제조한단전지는전해질층의경우연료극기능층을전사지로 2 회처리하여치밀한미세조직을형성하였으며, 공기극, 확산방지층및연료극기능층을전사지로제조하여다공층을형성할수있었다. 또한전사법으로제조한연료극지지체단전지는약 0.16 Ω 의분극저항을나타내었으며, 출력의경우 700 C 에서 W/cm 2, 750 C 에서 W/cm 2, 800 C 에서 W/cm 2 을나타내었다. 이러한결과를통해복잡한형상의스택, 특히 segmented type SOFC 에전사법을적용하여스택을제조할수있을것으로예상되어진다. Acknwledgments 본연구는지식경제부기술혁신사업인신재생에너지기술개발사업 - 원천기술 (2010T ) 의지원으로수행되었음을밝힙니다. REFERENCES 1. T. Tsai and S. A Barnett, Effect f LSM-YSZ Cathde n Thin-Electrlyte Slid Oxide Fuel Cell Perfrmance, Slid State Inics, (1997). 2. J. Kng, K. Sun, D. Zhu, N. Zhang, J. Mu, and J. Qia, N- YSZ Gradient Ande fr Ande-supprted SOFCs, J. Pwer. Surces, (2007). 3. Z. Wang, N. Zhang, J. Qia, K. Sun, and P. Xu, Imprved SOFC Perfrmance with Cntinuusly Graded Ande Functinal Layer, Electrchemistry Cmmunicatins, (2009). 4. K. Chen, X. Chen, Z. Lu, N. Ai, X. Huang, and W. Su, Perfrmance f an Ande-supprted SOFC with Ande Functinal Layers, Electrchimcal Acta, (2008). 5. N. Ai, Z. Lu, J. Tang, K. Chen, X. Huang, and W. Su, Imprvement f Output Perfrmance f Slid Oxide Fuel Cell by Optimizing Ni/samaria-dped Ceria Ande Functinal Layer, J. Pwer, Surces, (2008). 6. Y. Bai, J. Liu, and C. Wang, Perfrmance f Cne-shaped Tubular Ande-supprted Segmented-in-series Slid Oxide Fuel Cell Stack Fabricated by Dip Cating Technique, Int. J. Hydr. Energy, (2009). 7. T. Lai and S. Barnett, Effect f Cathde Sheet Resistance n Segmented-in-series SOFC Pwer Density, J. Pwer Surces, (2007). 8. J. Ding and J. Liu, A Nvel Design and Perfrmance f Cneshaped Tubular Ande-supprted Segmented-in Series Slid Oxide Fuel Cell Stack, J. Pwer Surces, (2009). 9. N. U. Ch, S. C. Hwang, and I. S. Lee, Single Cell Stacked Planar Type SOFC Assembled using a Ag-current Cllectr, J. Kr. Ceram. Sc., 44 [12] (2007). 10. P. V. Hendriksen, S. Kch, M. Mgensen, Y. L. Liu, and P. H. Larsen, in Slid Oxide Fuel Cells VIII, eds S. C. Singhal and M. Dkiya, The Electrchemical Sciety Prceedings, Penningtn, NJ, PV (2003). 11. J. D. Kim, G. D. Kim, and K. T. Lee, Oxygen Reductin Mechanism and Electrde Prperties f (La,Sr)MnO 3 -YSZ Cmpsite Cathde fr Slid Oxide Fuel Cell (Part : Oxygen Reductin Mechanism), J. Kr. Ceram. Sc., 38 [1] (2001). 12. J. D. Kim, G. D. Kim, and K. T. Lee, Oxygen Reductin Mechanism and Electrde Prperties f (La,Sr)MnO 3 -YSZ Cmpsite Cathde fr Slid Oxide Fuel Cell (Part : Oxygen Reductin Mechanism), J. Kr. Ceram. Sc., 38 [1] 93-9 (2001). 한국세라믹학회지

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