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1 Journal of Korean Powder Metallurgy Institute Vol 18 No 011 DOI: /KPMI s WC-Co w g p w LiCoO w bá½ a* a cáv y aw» l bw» c w» l œw Synthesis of LiCoO Powders using Recycled Cobalt Precursors from Waste WC-Co Hard Metal Heeseung Yang a c Jae-Hwan Pee b and YooJin Kim a * a Engineering Ceramic Center Korea Institute of Ceramic Engineering and Technology Icheon Korea b Ceramicware Technology Center Korea Institute of Ceramic Engineering and Technology Icheon Korea c Department of Materials Science and Engineering Yonsei University 14 Shinchon-dong Seodaemun-gu Seoul Korea (Received April 8 011; Revised May 6 011; Accepted May 4 011) Abstract LiCoO a cathode material for lithium rechargeable batteries was prepared using recycled Co First the cobalt hydroxide powders were separated from waste WC-Co hard metal with acid-base chemical treatment and then the impurities were eliminated by centrifuge method Subsequently Co powders were prepared by thermal treatment of resulting Co(OH) By adding a certain amount of Li CO and LiOH ½H O the LiCoO was obtained by sintering for 10 h in air at 800 C The synthesized LiCoO particles were characterized by X-ray diffraction (XRD) and Scanning Electron Microscope (SEM) analysis Keywords : WC-Co composite powder Recycle Cobalt oxide Lithium cobalt oxide 1 x w ky l l» WC-Co w š» WC-Cow šƒ» y v ƒ [1-] s w l WC y w j ƒ ù s w š y y mw y w y NaCO k s w» NaOH NH 4 OH w g q l l w [] ù ƒ s w wœ WC wš y w w Zinc Decomposed Process(ZDP) s w š w w Co(Cobalt) k WC [1-4-5] w ZDP œ mw WC z û Co LiCoO w w LiCoO CoCl Co acetate w w w *Corresponding Author : [Tel : ; 77

2 78 Áv yá½ w w ƒ w [6-7] LiCoO ƒ j p š [8-9] s w Co w LiCoO w wš w 1 x s WCƒ š û s ü Co w Co y mw Co y g Li CoO w w Li CO LiOH H O Li w Li/Co y g LiCoO w w x 1 WC-Co l Co Co s WC-Co w ZDP œ w WC w z û s (5% HCl) w [5] s 4L 8L g w 5 M Sodium hydroxide(naoh) w ph 4 w y e w s ü w WO NaCl w 5 M NaOH w ph 7 w y g e w w š 50 o C œ» g z Co Co w w Co ù w LiCoO w Co 500 o C» 1 w w mw Co ù LiCoO w Co w Li Li CO LiOH H O ƒ w Li/Co= Co ù Li l (Vortex GENIE Scientific Industries USA) w yww yw l p w 50 MPa j xk xw x r 700 C 5 1 w o w r g j xk xw 800 C 10 o w r w w w w X-ray diffraction(xrd D/max 500v/pc Rigaku Japan) Scanning electron microscope(sem JSM-690 JEOL Japan) mw w š 1 WC-Co l Co p z s» WC- Co w xk 1-5 µm s WC w w w 10 wt% Co x s w a) mx xk w WC 1 µm j» ƒ b) y w c) XRD WCƒ š w w Co 44 o WC w» w Zinc Decomposed Process(ZDP) w s w Zn ƒw Zn o C w Zn Co ww œ w y Zn-Cow xk o C z 1000 o C ƒ w Zn { mw Co w š WC WC š s w Fig 1 Process of Co synthesis using Co precursor from waste WC-Co hardmetal Journal of Korean Powder Metallurgy Institute

3 s WC-Co w g p w LiCoO w 79 Fig (a) Photograph image of molds (b) microstructuresg and (c) XRD pattern of waste WC-Co hardmetal w ph w Co w [5] s w H S HNO HCl H S w ü Co HNO w WO Co [10] mw s WCü w Co 6 l 4 ¾ w ƒ Co ƒ 4 Co [5] HCl w WC r x l» w Co w Co ù w w Co NaOH CoOOH Co(OH) xk w Co(OH) NH NaOH w û Co y [11] ƒ w y ph ƒ ù k š w y w ù y ƒ ƒ w [1] Co y mw š Co ù» w 500 C o w w y» k 500 C 1 o mw Co XRD ql FE-SEM x a) w Co ew CoO Co O b) 0~40 nm s Co LiCoO w LiCoO w Co ù Li CO LiOHÁ H O w Li/Co yww mw LiCoO w w j» ƒƒ LiCoO w ww 1 Co ù Li Vol 18 No 011

4 양희승 피재환 김유진 80 Fig (a) X-ray diffraction pattern and (b) SEM image of CoO4 nanopowders recycled from waste WC-Co hardmetal Fig 4 X-ray diffraction patterns of synthesized LiCoO using LiCO as precursor prepared at 800 C for 10 hour (a) Li/Co=100 and (b) Li/Co=105 Fig 5 X-ray diffraction patterns of synthesized LiCoO using LiOH HO as precursor prepared at 800 C for 10 hour (a) Li/Co=100 and (b) Li/Co=105 의 열에 의한 반응에 의해 핵 생성 및 성장이 이루 어지며 차 소결을 통하여 입자 성장을 증가시킴으 입자를 합성할 수 있다 로써 균일한 크기의 그림 는 합성된 나노 입자와 를 이용하여 합성한 화합물의 패턴 결과이다 를 이용하여 몰 분율을 로혼 의 결정상 합한 경우 혼합 분율에 관계없이 이 주로 관찰되었다 와의 반응성 차이를 확인하기 위하여 두가지 종류의 전구체를 이용하였다 그림 는 를 이용하여 합성한 입자의 패턴 결과이다 몰 분율을 로 혼합한 경우 의 결정상이 관찰되었으며 불순물이 소량 존재 한다 두 가지 종류의 전구체를 이용하여 LiCoO [1] 4 CoO4 LiCO XRD LiCO Li/Co LiCoO Journal of Korean Powder Metallurgy Institute CoO4 Li HO LiCoO Li/Co 100~105 LiOH XRD LiCoO 5 Li LiCoO

5 폐 계 초경합금에서 추출된 코발트 재생 원료를 이용한 WC-Co LiCoO 입자 합성 연구 81 Fig 6 SEM images of particles using LiCO as precursor (a) Li/Co=100 and (b) Li/Co=105 Fig 7 SEM images of particles synthesized with LiOH HO (a) Li/Co=100 and (b) Li/Co=105 분말 합성 결과 LiCoO 와 Li CO 의 혼합물의 형태 가 관찰되었다 Li 전구체의 양이 증가하게 되면 반 응에 참여하는 Li 이온의 농도가 증가하고 결정성이 증가되는 것을 확인 할 수 있다 불순물은 Li CO 의 결정상으로 LiOH H O가 800 C의 저온 반응에 의해 Co O 로의 확산이 완전히 이루어지지 않아 생긴 것 으로 판단된다 반응온도 및 반응시간을 증가에 의해 고순도의 LiCoO 를 얻을 수 있을 것이다 그림 6은 Li CO 를 사용하여 얻어진 LiCoO 입 자의 미세구조 결과이다 그림 6a)은 Li/Co= 100의 몰 분율로 합성된 LiCoO 입자이며 각 입자의 크기 는 약 5-6 µm의 분포를 나타내는 반면 그림 6b)의 Li/Co=105의 몰 분율로 합성된 LiCoO 는 8-9 µm 의 분포를 갖고 있었다 그림 7은 LiOH H O를 전구 체로 사용하여 합성된 LiCoO 의 미세구조 결과이다 그림 6과 마찬가지로 Li/Co=100 Li/Co=105(그림 7a b)의 몰 분율을 갖는 LiCoO 입자의 합성 결과 o 4 이다 각각 6 µm 8 µm의 분포로 Li CO 를 사용했 을 때와 유사한 크기의 입자가 합성되었으며 LiOH H O의 양이 증가함에 따라 입자의 크기가 증가되는 것을 확인하였다 즉 Li 전구체의 양이 증가되면 LiCoO 입자의 열처리 과정에서 LiCoO 의 표면에서 내부로의 Li 이온 확산이 증가됨에 따라 성장속도가 증가되어 입자의 크기가 커지는 것으로 판단된다[11] 과량의 Li 전구체를 함유할 경우 소결 과정 중 형성되는 H O CO 등이 증가되어 많은 양의 Li 이온 이 손실될 수 있다[1-15] 4 결 론 이차전지의 재료로서 높은 에너지 밀도 및 충 방 전 사이클을 갖는 LiCoO 입자를 합성하기 위하여 산업 현장에서 버려지는 폐산 수용액으로부터 Co 전 구체를 추출하였다 얻어진 Co 전구체를 이용하여 소 Vol 18 No 011

6 8 Áv yá½ mw LiCoO w w w j» ƒƒ 6-7 µm(li/co=100) 8-9 µm (Li/Co=105) s ùkü š w Li j»ƒ w s» l w y z w d w w w» w s w l Co y w w w ƒ w y» w š x [1] T J Chung S Y Ahn and Y K Paek: J Kor Ceram Soc 4 (005) 171 [] S Venkateswaran W D Schubert B Lux M Ostermann and B Kieffer: Int J Refract Met Hard Mater 14 (1996) 6 [] T Madhavi Latha and S Venkata chalam: Hydrometallurgy (1989) 5 [4] S Hairummisha G K Sendil J Prabhakar Rethinaraj G N Srinivasan P Adaikkalam and S Kulandaisamy: Hydrometallurgy 85 (007) 67 [5] J H Pee Y J Kim N E Sung K T Hwang W S Cho and K J Kim: J Kor Ceram Soc 48 (011) 17 [6] J N Reimers and J R Dahn: J Electrochem Soc 19 (199) 091 [7] M Tabuchi K Ado H Kobayashi H Sakaebe H Kageyama C Masquelier M Yonemura A Hirano and R Kanno: J Mater Chem 9 (1999) 199 [8] J M Tarascon and M Armand: Nature 414 (001) 59 [9] L Li W H Meyer G Wagner and M Wohlfahrt- Mehrens: Adv Mater 17 (005) 984 [10] C Adorjan A Bock S Myllymaki W D Schubert and K Kontturi: Int J Refract Met Hard Mater 6 (008) 569 [11] T N Ramesh: J Solid State Chem 18 (010) 14 [1] T Kojima T Shimizu R Sasai and H Itoh: J Mater Sci 40 (005) 5167 [1] T Nakamura and A Kajiyama: Solid State Ionics 1 (1999) 95 [14] T Ohzuku A Ueda and Nagayama: J Electrochem Soc 140 (199) 186 [15] W Li J N Reimers and J R Dahn: Solid State Ionics 67 (199) 1 Journal of Korean Powder Metallurgy Institute

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