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1 Jurnal f the Krean Ceramic Sciety Vl. 44, N. 8, pp. 424~429, Dual Phase Cnductive CO 2 Membranes: Mechanism, Micrstructure, and Electrical Cnductivity Shiw Lee, Ji Haeng Yu, and Sang Kuk W Energy Materials Research Center, Krea Institute f Energy Research, Daejen , Krea (Received May 19, 2007; Accepted August 22, 2007) Dual Phase CO 2 : f,» Á wá w» l ( ; ) ABSTRACT Nvel cnductive CO 2 membranes cmpsed f dual phases, mlten carbnates and electrnic cnducting ceramics, were investigated. As the micrstructure cntrl f electrnic cnducting ceramic supprts is extremely imprtant t keep the mlten carbnates stable in the membranes by a capillary frce applied by the pre structure f the supprts, we have scrutinized the micrstructure f the electrnic cnducting supprts utilizing micrscpic images and gas permeability measurement. Frm the evaluatin f the electrical cnductivities f the mlten carbnates and the electrnic cnducting ceramic supprts, we fund that the inic cnductivity f the mlten carbnates culd determine CO 2 flux thrugh the dual phase membranes if the surface exchange rate were relatively high enugh. Key wrds : Carbn dixide, Membrane, Dual phase, Mlten carbnate 1. CO 2 z w» w œ þ,, w e œ w d z. 1) p, yw ü d š w. ù»œ w» yw l CO 2 w 100 C k x w, š»ƒ l CO 2 w» w ƒ œ. 2) š CO 2 w k ( 2 ) p w, j ƒ w.,» k (mlten carbnate fuel cell, MCFC) w Fig. 1(a) ùk ü. 3) feed-side(cathde ) CO 2 sww yw» ƒ CO 2 O 2 w mw ww k Crrespnding authr : Shiw Lee Tel : Fax : x wš»yw w k w mw permeate-side(ande ) w. ande k ü š xk CO 2 O 2. MCFC w CO 2 cncentratr» w CO 2 w» J. Winnick w š 4) z w z ƒ w. k p w CO 2 w k dual phase yw w. 5) ƒ w wù, Fig. 1(b) ùkü, w v w» w w CO 2 ƒ ƒ w. dual phase CO 2»œ w xk» leakƒ w k, MCFC w CO 2 cncentratr w z v w œ e ƒ š. dual phase CO 2 w ww Chung 25~40%»œ stainless steel(mtt metallurgy, grade 0.5, 2, 5, 10) w. d 6) CO 2 permeance ml/m 2 s Pa 424

2 Dual Phase CO 2 : f,» 425 Fig. 2. Phase diagram f Li 2 -Na 2 -K 2 system.» n d w,» p sƒ mw CO 2 p y w v w. y dual phase CO 2 p w x w w. 2. x Fig. 1. Schematic diagram f (a) a CO 2 cncentratr and (b) a CO 2 membrane. w w ù k CO 2 /N 2 =3.5, CO 2 +O 2 /N 2 =16.27 f w» w k. w CO 2 x z t» w j, lithium ferritesƒ š šwš. x ¾ š, k k w (yw) w dual phase w š w. p ƒ»œ w k w w w» w w, CO 2 œ xk» leak w» w k»œ we» v w. y w dual phase CO 2 wš, sƒ» Fig. 2 k Li 2 - Na 2 -K 2 ywk k. 7) w ywk 390 C 720 C¾ w, l k w. 488 C ƒ, k w ƒ š 62%Li 2-38%K 2 k w, k ³ w yww x xk w. y w, sƒ ³ w La 0.6 Sr 0.4 -δ( w LSC) (Seimi Chemicals, Japan) 2 w kg f /cm 21 mm j xk xw 900 ~ 1200 C 2 w w. œ s ƒ w» n d w. d w w» n p sƒ e Fig. 3 ùk 44«8y(2007)

3 이시우 유지행 우상국 426 Fig. 3. Schematic diagram f gas permeatin measuring system. Fig. 4. Prsity variatin f the membrane supprts with sintering temperatures. 내었다. 분리막의 feed-side에 가해지는 압력의 함수로써 permeate-side로 투과되는 기체의 유속을 측정하였으며, permeance로 환산된 결과를 이용하여 지지체의 소결온도 에 따른 기공 크기의 변화를 평가하였다. 투과 기체는 N2 를 사용하였으며, dial 밸브를 이용하여 분리막 지지체의 feed side에 가해지는 압력을 조절하였고 투과되는 기체의 유량은 digital bubble flwmeter로 측정하였다. 용융탄산염과 전자전도성 지지체의 온도에 따른 전기 전도도는 D.C. 4-prbe법으로 측정하였다. 용융탄산염의 전기전도도 측정을 위해 기공율을 알고 있는 다공성 8YSZ (8 ml%-y O stabilized ZrO ) 지지체에 용융된 탄산염을 함침시켜 측정용 시편을 제조하였으며, 전자전도성 지지 체의 경우에는 기공율 3% 미만의 치밀질 소결체를 이용 하였다 결과 및 고찰 다공구조 전자전도성 지지체의 미세구조 Dual phase 분리막의 지지체는 용융상태의 탄산염을 담 지할 수 있도록 다공성 구조를 가져야 하는 동시에, 전자 전도체로서의 역할을 위해서는 분리막 전체에 걸쳐 연결 성이 양호해야한다. 또한 분리막 외부로의 기체 leak를 방 지하는 sealant 역할이 요구되며 전체 분리막의 구조를 유 지하기 위해 적절한 기계적 강도를 갖추어야 한다. 한편, 안정성 측면에서 전자전도성 지지체는 탄산염과 반응기 체에 대해 화학적 반응성이 적어야 하며, 작동온도에서 기공율이나 기공 크기의 변화가 작아야한다. Fig. 4는 다공구조 전자전도성 지지체의 소결온도에 따 른 기공율 변화를 나타내는 도표이다. 소결온도의 증가에 3.1. 한국세라믹학회지 Fig. 5. SEM images f the membrane supprts sintered at (a) 900C, (b) 950C, and (c) 1000C, respectively. 따라 기공율은 감소하는 경향을 나타내는데, 1050 C 이상 에서는 24% 미만의 기공율을 가지며 1200 C에서는 완전 히 치밀화된다. 따라서 perclatin 이론에 의할 경우, 전 자전도성 지지체의 기공에 담지되는 혼합탄산염이 탄산 염이온의 경로로서 역할을 하기 위해서는 기공율이 30% 이상이 되는 900~1000 C에서 지지체가 소결되어야 함을 알 수 있다. 각 온도에서 소결하여 제조된 전자전도성 지지체의 미 세구조를 Fig. 5에 나타내었다. 900~1000 C의 범위에서 소결된 시편의 경우, 소결온도의 증가에 따라 결정립의 크기가 약간씩 증가하고 기공의 크기는 점차 감소함을 관 찰할 수 있다.

4 Dual Phase CO 2 : f,» 427 Fig. 6. Permeated gas flw rate as a functin f the applied pressure f membrane supprts sintered at 900 ~ 1000 C. 3.2.» n w sƒ 900 ~ 1000 C œ, feed-side permeate-side,» n Fig. 6 ùkü. ƒ r»œ»œj»ƒ w w» ƒ n» w v w ƒw. œ»œ sƒw» w ù» n p w w. œ mw» 8) f»œ j» p ƒ, š w»œ j» œ r Knudsen (viscus flw) f w w. Kundsen» s³y (mean free path) ƒ»œ j» { f» z ƒ»»œ wall z y», w s ³y ƒ»œ j» {. ƒ» n ƒƒ û Fig. 6 mw, Knuden y w Fig. 7. Gas permeance as a functin f the average pressure f membrane supprts sintered at 900 ~ 1000 C. š w.» n d s³ (P av =(P high P lw )/2) w permeance w Fig. 7. s³ (P av ) w permeance y ùkù, x fitting mw»» β y r α w.», α β ƒƒ Knudsen diffusin viscus flw» w w, tx. 8) α = 1.06 ε - τ β = ε τ r p L M ω RT 2 r p LηRT», ε»œ (prsity), τ trtusity, r p s³» œ, L Ì, η n» (N 2 ) (= pise, 20 C) M ω n» w.» ƒ w w, s³»œ r p w, Table 1 w ùkü. ƒ œ»œ j» w». d» n l»œ (1) (2) Table 1. Linear Fitting Data, Y-axis Intercept (α) and Slpe (β), f the Permeance Presented in Fig. 7 and Grain Radius (r p ) Calculated frm the Data Heat-treatment temperature ( C) α (10 6 ml/m 2 secpa) β (10 12 ml/m 2 secpa 2 ) β/α (10 6 Pa 1 ) r (µm) «8y(2007)

5 이시우 유지행 우상국 428 Fig. 9. Fig. 8. Electrical cnductivity f the specimens cmpsed f mlten carbnate and YSZ matrix sintered at 1200C and 1300C. 0.47~0.91 µm로서, Fig. 5의 SEM 미세구조 사진으로부터 관찰되는 기공의 크기와 유사한 것을 알 수 있으며, 기체 투과도 측정으로부터 다공성 세라믹스의 기공 크기를 계 산하는 방법이 유용한 것으로 판단된다. 분리막 구성 상의 전기전도도 Fig. 8은 1200 C 및 1300 C에서 소결한 8YSZ를 지지체 로 하여 탄산염을 함침시킨 dual phase 복합체의 전기전 도도 측정 결과이며, 소결된 후 및 탄산염을 함침시킨 후 상온에서 관찰한 8YSZ 지지체의 미세구조를 Fig. 9에 나 타내었다 C에서 소결한 8YSZ를 지지체로 하는 dual phase 시편의 경우, 460~600 C의 범위에서는 0.11~0.25 S/cm의 전기전도도를 나타낸다. 이러한 값은 일반적인 8YSZ의 전기전도도(600에서 약 S/cm)보다 훨씬 높 은 값이므로, dual phase 시편의 전기전도도는 8YSZ의 개 기공(pen pre)을 채우고 있는 높은 전도도의 용융 탄산 염에 의해 결정된다고 할 수 있다. 따라서 8YSZ 지지체 의 기공(약 35%)이 모두 용융탄산염에 의해 채워졌다고 가정하면, 본 연구에서 사용된 용융탄산염의 600 C에서의 실제 전기전도도는 측정된 값(0.25 S/cm)을 부피분율(0.35) 로 나누어 약 0.71 S/cm 로 추산된다. 한편, 450 C 부근에 서부터 온도가 낮아짐에 따라 전기전도도의 급격한 감소 가 관찰되는데, 이러한 현상은 Li-K계 혼합탄산염이 냉각 됨에 따라 녹는점(488 C) 부근에서 용융상태로부터 고화 됨에 따라 발생하는 것으로 보인다. 한편, 1300 C에서 소결된 8YSZ 지지체에 혼합탄산염을 함침시켜 제조한 dual phase 시편의 경우에는 600 C에서 3.3. SEM images f 8YSZ supprts sintered at (a) 1200C and (b) 1300C. (c) and (d) are the images f 8YSZ supprts infiltrated with mlten carbnates fr the specimens (a) and (b) respectively. 의 전기전도도가 S/cm에 해당하였다. 전도도는 Arrhenius plt에서 온도에 따라 선형적으로 감소하는데, 측정된 값은 8YSZ의 온도에 따른 전기전도도와 근사한 값을 나타내었다. Fig. 9(b)의 미세구조에서도 관찰할 수 있는 바와 같이, 1300 C에서 소결한 8YSZ는 결정립이 조 대하며 기공 분율은 perclatin threshld 이하에 해당하 여 기공이 고립된 구조를 갖고 있다. 따라서 Fig. 9(d)에 나타낸 것과 같이, 용융된 탄산염이 폐기공을 충분히 채 우기 어렵고, 담지된 용융탄산염도 연결성이 양호하지 않 기 때문에 측정된 전기전도도는 8YSZ의 이온전도도에 의 해 결정되는 것으로 판단된다. 한편, 450 C 이하에서는 두 3 한국세라믹학회지 Fig. 10. Temperature dependence f the electrical cnductivity f LSC supprt sintered at 1200C.

6 Dual Phase CO 2 : f,» 429 r w» ùküš, š k 8YSZ w û. Fig. 10 LSC» y. ƒ ƒ w w ù kü, 650 C» 2 10 S/cm d 3. LSC y w w w, ƒ w rder ƒ y x. dual phase k y (bulk diffusin) w (3) Wagner xk tx. 6) J CO2 P'' 3RT t σ el σ in 8F dlnp t P' L t σ el + σ in = », L Ì, P' t P" t ƒƒ feed-side permeate-side (P CO2 + P O2 ), σ in σ el ƒƒ k. w CO 2 w, j y k û w., d k LSC w j û», t y ƒ, k mw k ƒ CO 2 w. ywk dual phase CO 2 p w j» w yw k w w. 4. w CO 2 /N 2 k ùký», k dual phase w., (3) k w w sƒwš w w,» n d mw»œ w š, w. k» d w CO 2 j y ƒ k w. Anknwledgment y w,. REFERENCES 1. D. Shekhawat, D. R. Luebke, and H. W. Pennline, A Review f Carbn Dixide Selective Membranes, A Tpical Reprt, DOE/NETL-2003/1200S R. Bredesen, K. Jrdal, and O. Blland, High-Temperature Membranes in Pwer Generatin with CO 2 Capture, Chem. Eng. & Prc., (2004). 3. K. Sugiura, K. Takei, K. Tanimt, and Y. Miyazaki, The Carbn Dixide Cncentratr by using MCFC, J. Pwer Surce, (2003). 4. J. L. Weaver and J. Winnick, The Mlten Carbnate Carbn Dixide Cncentratr: Cathde Perfrmance at High CO 2 Utilizatin, J. Electrchem. Sc., (1983). 5. S. J. Chung, D. Li, J. H. Park, J. I. Ida, I. Kumakiri, and J. Y. S. Lin, Dual-Phase Inrganic Metal-Carbnate Membrane fr High Temperature Carbn Dixide Separatin, Ind. Eng. Chem. Res., (2005). 6. S. J. Chung, Dual-Phase Inrganic Membrane fr High- Temperature Carbn Dixide Separatin, pp , M.S. thesis, Univ. f Cincinnati, Cincinnati, G. Mamantv and J. Braunstein, Advances in Mlten Salt Chemistry, Vl. 4, pp , Plenum Press, New Yrk, Y. S. Lin and A. J. Burggraaf, Experimental Studies n Pre Size Change f Prus Ceramic Membranes after Mdificatin, J. Membrane Sci., (1993). 44«8y(2007)

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