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1 Jurnal f the Krean Ceramic Sciety Vl. 43, N. 1, pp. 805~811, 006. Effect f Oxidatin f Ni n the Micrstructure f Ni/YSZ Ande and Crack Frmatin in YSZ Electrlyte Layer fr SOFC Jun-Sil Lim,* Jng-Hn Chi,* and Oh-Jng Kwn Department f Materials Science and Metallurgy, Kyungpk Natinal University, Daegu , Krea *LG Philips LCD C., Ltd., Gumi , Krea (Received August 14, 006; Accepted August 5, 006) Ni yƒ š y Ni/YSZ w ³ e w *Á z*á«w œw *( )LG Philips LCD ( ; ) ABSTRACT The micrstructural changes in Ni/YSZ ande substrate and crack frmatin during Ni xidatin were investigated. The cmpsitin f as-sintered andes was 56 wt% NiO+ 44 wt% YSZ and that f electrlyte was 8 ml% yttria. After cmplete reductin, specimens were xidized in N +air at 600~800 C. Oxygen partial pressure was cntrlled in between 0.05 atm and 0. atm O. When the ande was xidized, at higher than 690 C, three layers were frmed in the specimens. The first was fully xidized layer(nio/ysz), the secnd was a mixed layer and the third, near-intact layer. Under 640 C such distinctive layers were nt bserved. Cracks frmed at electrlyte layer when weight gain attained at 65~75% f the ttal gain due t cmplete xidatin despite f different xidatin temperature and xygen partial pressure. Key wrds : SOFC, Ni/YSZ ande, YSZ electrlyte, Oxidatin, Crack frmatin 1. š y (Slid Oxide Fuel Cells: SOFC) š w, œ ü w, ù yw, š q w SOFC»yw p y k. w w w» w 600~800 C j ƒ y w w š. 1-4) ¾ ƒ œ š SOFC (ande) œ Ni/YSZ p. Ni š y w»» y k. š Ni YSZ q ƒ w» p wƒ š. ƒ w SOFC w start-up shut-dwn, w, š y Crrespnding authr : Oh-Jng Kwn Tel : Fax : œ» w, Ni y w yƒ w w q. NiO y w Ni y q { x w» Ni y, y SOFC e w w ü» w. Chi 5) w, NiO/YSZƒ y 0.04% ù y 0.34% q w x. ù, Waldbillig 6) w, w r y y y ³ ùkü, w r y yƒ ù y 0.9~.5% q w. w r, Mn 7) Pechini YSZ t ù j» Ni w w, ³ wš e w j y y w x x., w y y. š, Mrales-Rdrguez 8) w y w q»œ š ƒ g j ƒ f z ƒ šw. 805

2 806 Á zá«fig. 1. Preparatin prcedure fr YSZ/Ni-YSZ bi-layer specimens. SOFC w ü œ»» ü Ni/YSZ y, yƒ w d ³ e w wš w.. x Ni/YSZ w d gq Fig. 1 œ w. 9) NiO Sumitm t, j» 0.3 µm. ü YSZ w YSZ Tsh 8ml% p (Y O 3 ) y k YSZ(Yttria Stabilized Zircnia) w. 56 wt% NiO+44 wt% YSZ. w d gq xk, 10 µm Ì YSZ w j v qw 1400 C w mm j» { w w 6 µm r p (paste) w š, q» t w 100 C 30 g. y x w NiO/YSZ y g. w š 30 N, N» z 10 C/min w. 90 C 5% H +N» y» z 750 C 5 y k ¾ þw. y r z, r d y» w, ù p r d gqw z, 100 C g šy g. SOFC 600~800 C y g. y w y y» ƒ w š, 30 N r w z, y x 600~800 C¾ 10 C w. t w w z, N œ» MFC(Mass Flw Cntrller, Mdel 1179A, MKS Inc., U.S.A.) w 0., 0.15, 0.10, 0.05» w, 00 ml/min w 1» k. t z y g, 100% N» þw. y x (SEM, Mdel S-500C, HITACHI, Japan) Ÿwx (OM, Mdel Axitech 100HD, ZEISS, Germany) w w. ¾ þw r d w z, w d ³ w» w SEM 1000 w t e w ³ w. y yd ¾ d w» w y r w š q g q Ÿw x w. š Ÿwx w q y q yw t l yd ¾ 0 d w s³ y d ¾ w.»œ x w» w œ» œ we(infiltratin) w. r œ š, œ k s (epxy) w,»œ s en g. wew z, 6 µm r p(paste) 0.05 µm ù z 500 r š, Ni y v (VISUS Fresthill Prducts, St. Petersburg, Russia) mw (pint cunting) w. t sww 100 µm / w d ¾ 11 Ni d w. 3. š 3.1. y XRD w Fig. (a) y / w NiO ZrO. š, 750 C, 5% H +N» 5 y k r Fig. (b) NiOƒ y y w. y r {, SEM y w w t ³ y w. Chi, 5) Waldbillig 6) ew. š, w wz

3 Ni의 산화가 고체산화물 연료전지용 Ni/YSZ 연료극의 미세조직과 전해질의 균열에 미치는 영향 Fig.. Pwder XRD patterns f andes (a) befre and (b) after reductin. 807 Fig. 4. The cmparisn f the grwth rates f xidized layers within Ni/YSZ substrates made f different granules, after xidatin at 750C in air atmsphere (PO = 0. atm). Fig. 3. Variatin f the linear dimensin with reductin- xidatin cycling (Isthermal treatment time : reductin - h and xidatin - h). 질소 분위기에서 800 C까지 승온 후 30분 유지하고 노냉 을 시킨 후 SEM으로 전해질의 전체 표면을 조사한 결과 균열이 발생하지 않았다. 이는 가열 냉각에 의해 발생하 는 열응력만으로는 균열이 초기에 생기지 않음을 뜻한다. 산화에 따른 연료극 전해질의 변화 우선 통기도(permeability)가 다른 시료와 산화거동의 차 이를 조사하였다. 통상적인 과립법(agglmeratin)으로 만 든 과립을 사용하여 성형 제조한 연료극은 열경화성(thermsetting) 과립으로 제조한 연료극보다 기공도는 높았지만 통기도는 낮았다. 제조방법에 따라 통기도가 다른 두 시 료의 산화속도는 Fig. 4와 같이 열경화성 과립을 사용한 시료가 70 µm/min로서 통상적 과립법으로 제조한 시료의 3.. / 9) Fig. 5. Optical micrgraphs f the crss-sectin f the xidized specimens (T = 800 C, PO = 0. atm, t = 4 min). 6.3 µm/min 보다 매우 빨랐다. 산화 속도에 미치는 영향이 기공도보다는 통기도가 훨씬 크다는 것을 잘 알 수 있다. Fig. 5는 750 C에서 공기 중 산화 시킨 시편의 수직 단 면에 나타난 산화층을 보여주고 있다. 사진의 상단부가 산화층이며, 저배율 광학현미경 상에서 밝은 연두색을 띄 고 있다. 하단부는 미산화층이며 검은색으로 나타난다. 그 중간층에서는 산화가 부분적으로 진행 중임을 보이고 있 는데 남색을 띄고 있다. Fig. 6과 같이 사진 윗부분의 산화층의 두께는 시간에 따라 증가하였다. 그러나, 현미경 상에서 경계를 뚜렷하 게 구별할 수는 없었다. 연료극의 산화가 진행함에 따라 어느 시점부터 전해질 층에 균열이 발생하였으며, 연료극 산화의 영향에 의한 전해질 균열 양상은 Fig. 7과 같았다. 일정 시간 이상 산 화성 분위기에 연료극이 노출되면 전해질 층에는 Fig. 7(a) 제 43 권 제 1호(006)

4 임준실 최종훈 권오종 808 Fig. 8. The grwth f xidized layer thickness alng with xidatin times (Temperature = 800 C, PO = 0.15 atm). Fig. 6. Optical micrgraphs f the crss-sectins f the specimens xidized under air atmsphere at 750 C fr different times (Thickness : 1.1 mm, Sumitm NiO pwder). 와 같이 초기 균열이 한 방향으로 발생하였다. 산화성 분 위기에 노출되는 시간이 길어질수록 전해질 층의 균열은 Fig. 7(b)와 (c)에서 나타나듯이, 초기 균열이 균열의 또 다른 시작점이 되어 전해질 층에 대하여 균열이 수직 방 향으로 성장하였다. SEM 상에서 미세한 균열이 최초로 발견되는 시점을 균열 발생 시간(Crack initiatin time)으 로 정하였다. 산화온도가 690 C, 750 C, 800 C인 경우에는 산화층의 뚜렷한 경계가 나타났으며, 산화층의 두께는 시간에 대체 로 비례하여 성장하였다. Fig. 8은 산소 분압이 0.15 기압 일 때, 800 C에서 산화층이 성장하는 거동을 보여준다. 6 분이 경과한 시료에서는 미산화층이 전해질 쪽에 남아 있 음에도 불구하고 전해질에 균열이 발생하였다. 산화온도 가 690 C 이상일 때에는 모두 미산화층이 잔존하는 상태 에서 균열이 시작되었다. 그러나, 640 C, 600 C에서는 690 C 이상에서 관찰되는 NiO/YSZ의 산화층이 관찰되지 않았음에도 불구하고, 전 해질 표면에 균열이 발생하였다. 이를 자세히 알아보기 위해 산화에 의한 미세조직의 변화를 더욱 세밀하게 분 석한 결과는 다음과 같다. Fig. 9는 640 C에서, 산소분압이 0.1 기압과 0. 기압인 조건으로 산화된 시편의 단면에서 깊이방향으로의 Ni 분 율 변화를 나타낸 것이다. 미산화 Ni 분율은 연료극 표면 에서 전해질로 갈수록 증가하였다. 즉, 미산화 Ni 분율의 증가는 표면에서 전해질로 갈수록 NiO의 분율이 감소함 을 뜻한다. 또한, Ni 분율이 어느 경계를 갖고 급격하게 변화하는 양상을 보이지 않고 서서히 증가를 하였다. 이 것은 690 C 이상에서와는 달리 온도가 상대적으로 낮을 경우, 연료극의 산화는 시편 전체에서 일어나기 때문이 다. 이것은 앞서 말한 바와 같이 온도가 변화함에 따라 Fig. 7. The SEM micrgraphs f YSZ electrlyte layer re xidized under xidizing atmsphere at 800 C fr different times (PO = 0. atm). 한국세라믹학회지

5 Ni yƒ š y Ni/YSZ w ³ e w 809 Fig. 10. Cmparisn f Ni cntent prfiles fr crack frmatin at YSZ electrlyte layers alng the distance frm the surface f Ni/YSZ substrates t YSZ electrlyte layer. At higher temperature Ni cntent changed very steeply and resulted in marked xidatin layers. Fig. 9. The changes f the area fractin f metallic Ni alng with distance frm the surface f Ni/YSZ substrate at the fllwing cnditins: (a) 640 C, P O = 0. atm and (b) 640 C, P O =0.1atm.»» x., œ Ni/YSZ y w, û Ni y ƒ ü ¾ ¾ y w. w ü w š, y ü ù» š ƒ. w d ³, 640 C 0.» 10, 0.1» 14, š 600 C 0.» 1, 0.1» 0, ³ w Ni w 10%. 56 wt% NiO+44 wt% YSZ y k Ni v 40%, w Ni 75% yƒ ù, w ³ w. Fig. 10 NiO/YSZ yd ùkù 750 C yd ùkù 640 C w d ³ w Ni s w. 750 C 690 C x 3 d w Ni j ƒw», w Ni.5%., 690 C Fig. 3 TMA x NiO/YSZ yd q w w d ³ ƒ y y 56 wt% NiO+44 wt% YSZ y w, 1%. y x w r y 1% NiO ƒ Ni y y w. XRD ew. y» ƒ, z ƒw. wr 0.05~0.5» ƒ y w ƒw. Fig. 11 YSZ w d ³ w y w w š. 750 C SOFC œ»ƒ, w 5 ³. ƒ û, š û ³ 43«1y(006)

6 810 Á zá«fig. 11. The change f the xidatin time fr crack initiatin as a functin f temperature under varius xygen partial pressure. Fig. 1. The plt f weight gain at the crack frmatin vs. Oxidatin temperature under varius xygen partial pressure. ¼ Fig. 11 w q dw. ù, œ» w e x w z ƒ» ³ Fig. 11 ¼. œ» / w / 3d w v w., x ³. Fig. 1 Ni/YSZ y ³ w ƒ e w š. ƒ 65~75% ³ w. x 690 C w d ³ 640 C w w d ³ wš, w d ³ 65~75% yƒ û w. w d ³ w 690 C NiO/YSZd (Ni+NiO)/YSZd y 640 C w yƒ w y w w ~800 C ü 0.05» ~0.» y» š y Ni/YSZ yƒ w ³ e w w. 1. Ni y 690 C, 750 C, 800 C yd w ù, 640 C, 600 C w y w yd x š r w ƒ yƒ û.. y y ù ƒ ƒ 65~75% w d ³ w. 3. y, w yd x, yd ̃ w ƒw C yd x w yd mw w t ³ g, 640 C w w w Ni NiO y» w w t ³ w. Acknwledgment ƒ w SOFC w» w w,. w, œw š, w KIST w y Ì ¾. REFERENCES 1. G. H. Kim and H. S. Sng, Develpment Status f SOFC, Ceramist, 3 [5] 7-16 (000).. DOE/NETL, Fuel Cell Handbk (Sixth Editin), pp , EG&G Technical Services, Inc., Science Applicatins Internatinal Crpratin, N. Q. Minh and T. Takahashi, Science and Technlgy f Ceramic Fuel Cells, pp , Elsevier Science B. V. Amsterdam, Netherlands, W. Z. Zhu and S. C. Deevi, A Review n the Status f Ande Materials fr Slid Oxide Fuel Cells, Mater. Sci. w wz

7 Ni yƒ š y Ni/YSZ w ³ e w 811 and Eng., A (003). 5. J.-H., Chi, Effect f Reductin/Oxidatin f Ni and Thermal Cycling n Ni/YSZ Ande in SOFC, pp. 8-38, M. S. Thesis, Kyungpk Natinal University, Daegu, D. Waldbillig, A. Wd, and D. Ivey, Thermal Analysis f the Cyclic Reductin and Oxidatin Behavir f SOFC Andes, Slid State Inics, (005). 7. S.-D. Kim, H. Mn, S.-H. Hyun, J.-H. Mn, J.-S. Kim, and H.-W. Lee, Perfrmance and Durability f Ni-Cated YSZ Andes fr Intermediate Temperature Slid Oxide Fuel Cells, Slid State Inics, (006). 8. A. Mrales-Rdriguez, A. Brav-León, G. Richter, M. Rühle, A. Dminiguez-Rdriguez, and M. Jiménez-Melend, Influence f Oxidatin n the High-Temperature Mechanical Prperties f Zircnia/Nickel Cerments, Scripta Mater., (006). 9. D.-S. Lee, J.-H. Lee, J. Kim, H.-W. Lee, and H. S. Sng, Tuning f the Micrstructure and Electrical Prperties f SOFC Ande via Cmpactin Pressure Cntrl during Frming, Slid State Inics, (004). 43«1y(006)

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