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1 Jurnal f the Krean Ceramic Sciety Vl. 46, N. 6, pp. 648~652, DOI: /KCERS Prperties f the Electrlyte Separatrs fr Thermal Batteries Using SiOC Mat Kyung Hn Lim, Kwang Yun Ch, Dh Hyung Riu, Dng Geun Shin, Eun Ju Jin Hyun Ee Kim*, Hae Wn Cheng**, and Hng Lim lee*** Divisin f Nan materials Applicatin, KICET, Seul , Krea *Department f Materials Science and Engineering, Seul Natinal University, Seul , Krea **Agency fr Defense Develpment, Daejen , Krea ***Department f Materials Engineering, Ynsei University, Seul , Krea (Received September 24, 2009; Revised Octber 12, 2009; Accepted Octber 29, 2009) SiOC p(mat) w w q p zá Ÿ Á xá Á Á½x *Á w **Á y *** w» w * w œw ** w 4» *** w œw ( ; ; ) ABSTRACT Ceramic fiber separatr is the prmising material fr thermal battery system because it reduces the prductin cst and ffers the ptential t a new applicatin cmpared t a pellet type electrlyte. The electrlyte separatr fr thermal battery shuld be easily handled and laded a large amunt f the mlten lithium salt. Ceramic fibers were used as an electrlyte separatr and the lithium based mlten salts were infiltrated int the ceramic filters. Leakage f mlten salt (several lithium salts) leads t shrt-circuit during the thermal battery peratin. In this study, a unifrm and fine SiOC mat with fibers ranging frm 1 t 3 µm was btained by electrspinning f plycarbsilane and pyrlysis. The ptimum spinning cnditins fr btaining fine diameters f SiOC fiber were cntrlled by the slutin cmpsitin and cncentratin, applied vltage and spinning rate, release rate by prsity. The pre structures f the ceramic filter and the melting prperties f the lithium salts affected t the electrlyte lading and leakage. The imprtance f the fiber size and prsity and their cntrl was discussed and the mechanical prperties were als discussed. Key wrds : Thermal battery, Mlten salt, Ceramic filter, Electrlyte separatr, Infiltratin 1. ƒ š š xw š. w 1947 Catast research crp.(crc) p(li) ƒ sw œ w yw LiCl-KCl w w. pw œ 1-3) 352 C š k w, y ù w yw 20 ƒ w. w ý» y w ƒ w š. xw w w» w w p ƒ Crrespnding authr : Kwang Yun Ch Tel : Fax : w š, 3 p LiCl-LiF-LiBr ƒ p (Li ) ƒ š š + š. ƒ» w p w p ƒ w š k p w w. p v w œw,, w w ù kü. p ü { ƒ ƒ w» û w. š w w, p y y w» p w w. w w û w w. w w w 648

2 649 zá Ÿ Á xá Á Á½x Á w Á y» w. 1-5) w ƒ û» w ƒ v w. x w w w MgOƒ t š m 35% ƒ 6,7), w w ü p w x k w» (ü w ƒ) w p j w. w y w» w 0.5 mm Ì j w, w ̃ ƒw, w ü w ƒw»ƒ p j(60 mm ) w q w j p w jš w. w Ì ƒ w w. w q w j» w w ƒ sxk vl p w. s vl»œj»ƒ 1µm w p ù» we wš p ü.» (Electr-spun), ƒ š 8,9) mw SiOC»œj»ƒ s xk SiOC p w. SiOC p p»œ d w š»œ y p we wš SiOC p(mat) pwder melting 3 p (LiCl- LiF-LiBr) wew x p w q w z SiOC p s³»œj» w SiOC mat»œ v p ù we d w š 500 C p ù ù d w w. w x SiOC w q x w z d w p s ƒw. 2. x 2.1. SiOC mat sƒ s e (PCS, Nipusi Type A, Nippn Carbn c., japan) Aldrich Tluene N,N-dime thylfrmamide (DMF) yw z» w ƒ, w w s³»œ j»ƒ s š p. š Table 1. Prperties f SiOC Mat fr Impregnatin with Lithium Salt Materials Manufacture methd Thickness, in Pre size, µm Pre rate (%) SiOC Electr spun 0.5~0.8 mm 15~45 85~90 Table 2. Prperties f Lithium Salt fr Impregnatin Int SiOC Mat Cntents 3Phase Li salt Chemical Particle cmpsitin size LiCl-LiF- LiBr Melting pint Density Surface tensin 10 µm 450 C 2.17 g/cm 3 70 dyne/cm» 200 C 1 w yw z Ar» 1200 C 1 w SiOC p(table 1) w.» x scanning electrn micrscpe(sem; JSM-5800LV, JEOL) mw w š w p»œ d w. w p (LiCl-LiF-LiBr) SiOC ƒ d w t SiOCƒ gq SiC»q p (LiCl-LiF-LiBr) š p k š x (Heating Micrscpe; OKDOO, KOREA) mw w SiOC mat w w q sƒ ( ) d w 3 œ (LiCl-LiF-LiBr- 99% purity, Table 2) w pwder melting 10,11) SiOC p wew. p w w» š»( 1% w) w x ww. p s x SiOC mat s³»œj» 56 mm ü 7mm xk ƒƒ ƒœw. p w xk SiOC mat ƒ Bx Furnace š r š 500 C š 10 w p SiOC p ü we w z, p we SiOC p Éü þƒ g. SiOC p»œ v p ù we we z SiOC p d w we d w. SiOC p we k y w» w Scanning Electrn Micrscpe (SEM; JSM-5800LV, JEOL) mw t q k w. p we SiOC p d p we glass filter(watchman GF-C s³»œj» 1.2 µm w,»œ 90% ) p we SiOC p š ù v p(75 g) z, ƒ w 500 C» w wz

3 SiOC 매트(Mat)를 이용한 열전지용 전해질 격리판 제조 및 특성 Fig. 2. Fig Image f high temperature ptical micrscpe with Lithium salt(lic-lif-libr) n SiOC plate. SEM images f SiOC mat fabricated with electr spun methd. 고 30분간 유지하여 리튬염이 함침된 SiOC 매트에서 용 융되어 누액되는 리튬염을 리튬염이 함침되지 않은 glass filter(watchman사 GF-C 평균기공크기 1.2 µm 이하, 기공 률 90% 이상)가 위면과 아랫면에서 흡수하도록 하고 전 기로에서 꺼내어 상온에서 냉각 후 리튬염이 함침된 SiOC 매트만 떼어내어 소실된 리튬염의 무게를 측정하여 누액 률을 측정하였다. 리튬염이 함침된 SiOC 매트가 열전지 의 전해질분리판으로서 어느정도의 전지로서 성능을 발 현하는지를 측정하기 위해 열전지 실형상의 전해질 격리 판을 제작한 후 SiOC 전해질 분리판 양면에 전극을 대고 250 kgf로 압착하여 단전지를 구성하고 열원을 부가한 후 500 C로 가열되도록 하면서 시간에 따른 전압의 변화를 관찰하였다. 3. 결과 및 고찰 Fig. 1은 Plycarbsilane(PCS)을 전구체로 사용하여 Electrspun 방법으로 섬유형상으로 방사한 후 아르곤분위기에서 1200 C로 열처리한 SiOC 매트(mat)의 전자현미경 사진이 다. 전자현미경사진에서 보면 SiOC 매트(mat)가 부직포형 상으로 구성된 것을 볼 수 있다. 그리고 섬유 한가닥의 형상은 매끈하지 않고 불규칙한 형상을 띠고 있으며 표 면은 패인 것 같은 기공들이 상당량 포함하고 있으며 단 면에서도 표면의 기공들이 섬유경 바깥쪽으로 존재하고 있음을 관찰하였다. Electr-spun 방법에 의한 방사는 전 구체인 PCS를 극성용매에 녹여서 원료와 전극사이에 자 장 차이를 유도하여 전구체 PCS 용액이 연신되면서 섬유 형상을 갖도록 하는 방사방법이다. 이때 연신이 되면서 방사되는 섬유가 공기중에 노출되면 극성용매가 섬유에 서 휘발하게 되는데 동시에 방사되는 섬유가 경화되면서 표면에 휘발된 부분이 기공으로 남게 되는 것이다. Fig. 2는 3성분계 리튬염(LiC-LiF-LiBr )의 젖음각을 측 Fig. 3. SEM phtgraphs f SiOC mat impregnated with lithium salt(lic-lif-libr). 정을 위한 고온현미경 관찰을 실시한 사진이다. 456 C에 서 용융이 되기 시작하여 465 C에서는 완전히 용융이 된 것을 볼 수 있다. 완전히 용융된 상태에서 젖음각은 거의 2 정도로 매우 작았다. 이는 D.G.SHIN 등이 glass 소재 를 리튬염의 지지체로 사용한 연구결과 에 의하면 glass 소재와 용융된 3성분계 리튬염(LiC-LiF-LiBr)간의 젖음각 이 완전히 용융된 상태에서 4~7 정도를 나타낸다는 결 과와 비교했을 때 용융된 3성분계 리튬염(LiC-LiF-LiBr) 이 glass 소재보다 상대적으로 젖음이 좋음을 알 수 있다. 이는 Fig. 1에서 관찰한 바와 같이 다공성 표면은 열전지 가 500 C 부근의 온도에서 구동시 SiOC 섬유로 구성된 매트(mat)가 용융된 리튬염을 효과적으로 잡아주어 리튬 염이 누액되지 않도록 해주는 특성으로 판단된다. Fig. 3은 3성분계 리튬염(LiC-LiF-LiBr)을 pwder melting 법에 의해 SiOC 매트(mat)에 담지한 후 표면과 파단면의 SEM 사진이다. 리튬염이 SiOC 매트(mat)의 표면에 치밀 하게 함침되어 있음을 확인하였다. 또한 파단면에서도 SiOC 매트(mat)에 리튬염이 균일하고 치밀하게 함침되어 있음을 확인하였다. 이는 융용된 리튬염과 SiOC 소재간의 낮은젖 음각과 SiOC 섬유 표면에 존재하는 다량의 기공들로 인 해 용융된 리튬염이 효과적으로 함침된 것으로 판단된다. Fig. 4는 전기방사에 의해 제조한 SiOC 매트(mat)의 기 공크기에 따른 분포를 나타낸 그래프이다. 전기방사시 전 구체 PCS의 주입량이나 농도, 그리고 전극간의 전압차 등 의 변수를 조절하여 평균기공크기가 각각 15, 21, 30, 45 µm를 갖는 SiOC 매트(mat)를 제조하였다. D.G.SHIN 등 이 유리필터를 사용한 연구에서 보면 매트(mat)의 평균기 공 크기가 크면 용융된 리튬염의 담지량이 증가하지만 열 12) 제 46 권 제 6호(2009)

4 651 zá Ÿ Á xá Á Á½x Á w Á y Fig. 4. Pre vlume distributin f SiOC mat as a functin f average pre size. Fig. 6. Discharge test f SiOC separatr separatr impregnated with Lit salt(licl-lif-libr). Fig. 5. Lithium salt lading rate and lithium salt release rate f ceramic filter separatr with average pre size. 500 C p ƒw š šwš. SiOC p(mat) s³» œj»ƒ ùküš 3 p (LiC- LiF- LiBr) ý q. Fig. 5 SiOC p(mat) s³»œj» 3 p ùkü. p s³»œj»ƒ ƒw w ƒw ƒ 30 µm s³»œj» w w. D.G.SHIN vl w š 13) w s³»œj»ƒ ƒw ƒw ew x s³»œj»ƒ 30 µm f 3 p û w we»œ» wš ü» q. wr x, s³»œj»ƒ j p ƒw. p ü x»œ j m ƒ x p û ƒ w SiOC p(mat) ùƒ x w ƒw q. w 3 LiCl-LiF- LiBr œ t 70 dyne/cm ƒ û y ƒ ƒ p SiOC p(mat) ùƒ q, s³»œj»ƒ p(mat) p p(mat) t š p šw» q. Fig. 6 p w SiOC p w q x ƒœw z ƒ 500 C ƒ w k w q š 250 kgf w y ù kü. 500 C ƒ p š p p w p xw» w.» x j» w ù û s³»œj» 45µm j»œ ƒ SiOC p w q w. s³» œj»ƒ SiOC p q ùkü. Fig. 5 s³»œj»ƒ j SiOC p f k w w p ùƒ»»p q. s³»œj»ƒ SiOC p w p q. 4. Electr-spun w SiOC p sx š x ñw š ³ew x š t q»œ w wz

5 SiOC p(mat) w w q p 652 swwš. p k SiOC t x w ƒ 2. SiOC œ t ƒ 500 C p z w p q. Pwder melting w SiOC p (mat) w z t q SEM mw p SiOC p(mat) t q e w w e y w. p SiOC û ƒ SiOC t w»œ w p z we q. p s³»œj»ƒ ƒw w ƒw ƒ 30 µm s³»œj» w. p s³»œj»ƒ j p ƒw. 3 LiCl-LiF-LiBr œ t 70 dyne/cm ƒ û ƒ ƒ p q, s³»œj»ƒ p(mat) p p(mat) t p šw wš» q. p w SiOC p w q x ƒœw z p w,» x j» w ù û s³»œj»ƒ j SiOC p w q w. s³»œj»ƒ SiOC p q ùkü. s ³»œj»ƒ j SiOC p f p ùƒ»»p q. REFERENCES 1. P. Masset, Thermal Activated (Thermal) Battery Technlgy, Part II. Mlten Salt Electrlytes, J. Pw. Sur., (2007). 2. R. A. Guidtti, Thermally Activated ( Thermal ) Battery Technlgy Part I: An Overview, J. Pw. Sur., (2006). 3. P. Butler, Lng-Life, Multi-Tap Thermal Battery Develpment, J. Pw. Sur., (2004). 4. S. S. Zhang, A Review n the Separatrs f Liquid Electrlyte Li-In Batteries, J. Pw. Sur., (2007). 5. P. Masset, Retained Mlten Salt Electrlytes in Thermal Batteries, J. Pw. Sur., (2005). 6. R. Pnnappan, Cntact Thermal Resistance f Li-In Cell Electrde Stack, J. Pw. Sur., (2004). 7. B. Culpin, Thermal Runaway in Valve-Regulated Lead- Acid Cells and the Effect f Separatr Structure, J. Pw. Sur., (2004). 8. J. M. Deitzel, The Effect f Prcessing Variables n the Mrphlgy f Electrspun Nanfibers and Textiles, J. Pl., (2001). 9. S. H. Tan and R. Inai, Systematic Parameter Study fr Ultra-Fine Fiber Fabricatin via Electrspinning Prcess, J. Pl., (2005). 10. J. Saunier, Plasticized Micrprus Ply(Vinylidene Fluride) Separatrs fr Lithium-In Batteries. III. Gel Prperties and Irreversible Mdificatins f Ply(Viny lidene Fluride) Membranes under Swelling in Liquid Electrlytes, J. Pw. Sur., (2004). 11. P. Masset, Idide-Based Electrlytes: A Prmising Alternative fr Thermal Batteries, J. Pw. Sur., (2006). 12. D. G. Shin, Web-Type Silicn Carbide Fibers Prepared by the Electrspinning f Plycarbsilanes, J. Ceram. Prces. Res., (2008). Acknwledgment w» y w,. 46«6y(2009)

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