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1 Jurnal f the Krean Magnetics Sciety, Vlume 19, Number 6, December 2009 DOI: /JKMS œe w w r p(bam) x» e ph w Áû k w œw, z w¼1, ( , , y ) M-type r p(bafe 12 ) œe w w w. Fe :Ba 8 š wš Fe Ba w. ph w», x y XRD(X- Ray Diffractmeter), FESEM(Field Emissin Scanning Electrn Micrscpe), VSM(Vibrating Sample Magnetmeter) w w. phƒ 8 š Fe :Ba ƒ 12:1.5 ƒ j. phƒ 8 Fe Ba sy y yƒ j ùkû. r p ƒ α-fe 2 O 3. phƒ 10 Fe Ba M-type r p w y ùkü. Fe Ba ƒ 13.6 : 1.7 ƒ j y (55.7 emu/g),» z þw y ùkü. FESEM j» 50~200 nm. : M-type r p, œe,, ph, I. M-type r p(bafe 12 ) r y y w w w w š. Magnetplumbitetype(hexagnal) r p ƒ q c y w j» w (6700 Oe) j sy y(72 emu/g), j (450 C) [1]. w r p»» š [2] j q»q w [3]. w p ƒ» w w w.» w w ƒ». BaFe 12» w ƒ w š, œew, y, w, w w [4-12]. w w BaFe 12, j» xk, j. w w» š wš w» w œ v t vw ƒ.» wwš *Tel: (033) , ƒ ³ wš ƒ w û w w œe w w w [13, 14]. û BaFe 12 x w» w Fe :Ba ƒ w š š [15, 16], p Fe :Ba ƒ 8 ƒ w» ùkü š š [17, 18]. w phƒ w» ƒ w w w e» w w e š š [19, 20]. Fe :Ba ƒ 8 w» ùkü Fe Ba w. w Fe Ba ƒ w w» ùkü ph w. II. BaFe 12 œe w w w. Ba(NO 3 ) 2 Fe(NO 3 ) 3Á9H 2 O w š Fe : Ba 8 š wš Fe Ba w (13.6 : 1.7, 12 : 1.5, 10.4 : 1.3, 8 : 1). k yw w z 3 NaOH w e jš e decanting w z ƒƒ phƒ 8 10 w. ph z w w e 100 C 6 w. x 209

2 한국자기학회지 제19권 6호, 2009년 12월 210 Fig. 1. Experimental prcedure. Fig. 2. 모르타르를 이용해 분쇄한 후 상자형로를 이용하여 공기 분 위기에서 열처리 하거나 관상로를 이용하여 산소분위기에서 열처리 하였다. 서로 다른 분위기(공기, 산소)에서 열처리 온 도는 800 C로, 유지 시간은 2시간으로 하였다. 열처리 온도 는 M-type이 생성되는 온도이면서 결정립 성장에 의해 자기 적 성질이 저하되는 것을 고려하였다. 분말을 로에 장입한 후 분당 5도씩 승온 하여 800 C에서 2시간 동안 유지하거나 800 C로 승온이 된 로에 분말을 장입한 후 2시간 동안 유지 하여 열처리 하였으며 열처리가 끝난 후 노냉을 하거나 공기 중에서 냉각하였다. 실험과정과 열처리 조건은 Fig. 1과 Fig. 2에 나타내었다. 제조된 분말의 결정성은 Philips사의 X pert PRO X선회절분석기를 이용하여 조사하였고, 자기적 특성은 Lake Shre 7300 mdel의 진동시료형 자력계(VSM)로 최대 Heat treatment cnditins. 10 koe를 인가하여 상온에서 측정하였다. 표면분석은 HITACHI사(S-4300)의 전계방사형 주사전자현미경(FESEM) 을 이용하였다. Fig. 3. III. 실험 결과 및 고찰 제조된 분말의 결정구조를 조사하기 위하여 XRD회절 분 석을 행하였으며 그 결과를 Fig. 3과 Fig. 4에 나타내었다. Fig. 3은 Fe : Ba 의 비가 12 : 1.5이며 ph를 8과 10으로 하여 제조한 분말의 열처리 조건에 따른 회절 패턴이다. 그 림에서 알 수 있듯이 같은 Fe : Ba 에서도 ph에 따라서 다른 회절 패턴을 나타내고 생성된 상의 비율이 다름을 알 수 있다. ph 8인 경우에는 적용한 모든 열처리 조건에서 단 XRD patterns f BaM pwder heat treated under varius cn- ditins (Fe : Ba = 12 : 1.5, 800 C, 2 hrs). (a) ph 8, (b) ph 10.

3 œe w w r p (BaM) x» e Áû k 211 Fig. 4. XRD pattern f BaM pwder prepared with different Fe :Ba (800 C, 2 hrs, ph 10). (a) HT.1: Furnace cling after heat treatment in air (b) HT.4: Furnace cling after heat treatment in O 2. M-type š α-fe 2 O 3 wì w ùkü ph 10 α-fe 2 O 3. r p š w α-fe 2 O 3 l w š [21]. ph 8 α-fe 2 O 3ƒ r p w š wš. û ph w e yw ù 800 C α-fe 2 O 3ƒ M-type r p ƒ ù w š q. ph 10 r pƒ š, Fe Ba (HT.1 and HT.2) Feƒ w. Fe Ba Fe y w» w XRD ql Fig. 4 ùkü. œ» z þw(ht.1) Fe :Ba ƒ 10.4 : 1.3,» z þw(ht.4) 12 : 1.5 Fe vjƒ ùkù. ph 10 w. α- Fe 2 O 3 ùkù. ph 10 w Fe :Ba w š Feƒ w w š û. Fevjƒ ùkù» Fe :Ba» x w Fe Ba š w. l Fe :Ba w š. w ¾ š û 800 C M-type ùkü. Fe :Ba 12 : 1.5, ph 10 š wš w t x FESEM micrgraph w Fig. 5 ùkü. x j 800 C j ù. ph ƒƒ 8 10 wš Fe :Ba 12 : 1.5 w œew» 800 C 2 w z þ(ht.4)w FESEM micrgraph Fig. 6 ùkü. Fig. 6 ph x j ù ph 10 e wš š j» ƒ š. Fig. 5 Fig. 6 q w FESEM w M-type r p j»ƒ š w š wš ³ew q x ùkü. ƒq» w û ƒ q. Fe :Ba 12 : 1.5 ph» š y Fig. 7 ùkü. ph 8 y ph 10 ùkûš XRD ew α-fe 2 O 3» q. ph 8

4 한국자기학회지 제19권 6호, 2009년 12월 212 FESEM micrgraph f BaM pwder btained at different Heat treatment cnditins (Fe : Ba = 12 : 1.5, 800 C, 2 hrs, ph 10). (a) HT.1 (b) HT.2 (c) HT.3 (d) HT.4 (e) HT.5 (f) HT.6. Fig. 5. 에는 특히 800 C로 유지된 노에 장입 하여 공기 중에서 냉 각한 분말의 자화 값이 다른 열처리 조건보다 작게 나타났고 이 경우에는 공기 중에서 열처리한 경우와 산소분위기에서 열 처리한 경우가 같은 경향을 보였다(HT.3, HT.6). 그러나 ph 10일 때에는 자화 값과 보자력 값 모두 대부분 고르게 나타났으며 공기 중이나 산소분위기에서 열처리 후 노냉하여 얻은 분말이 자화 값과 보자력 값이 가장 높은 값을 나타냈 다(HT.1 and HT.4). 산소 분위기에서 800 C로 열처리한 후 노냉(HT.4)한 분말의 조사한 모든 Fe : Ba 와 ph에 따른 자기이력 곡선을 Fig. 8에 나타내었다. 그림에서 나타난 바와 같이 ph 8인 경우에는 α-fe O 상의 존재로 인해서 ph 10 일 때보다 상대적으로 작은 자화 값과 큰 보자력 값을 나타 내었으며 Fe : Ba 의 상대적인 양에 따라서 큰 자기적인 성 질의 변화를 보였다. 또한 Fe 와 Ba 의 양이 증가함에 따라 자화 값이 증가하였고 보자력 값은 감소하였으며, 산소분위기 (HT.4, 5, 6)에서 열처리 한 분말보다 공기중(HT.1, 2, 3)에 서 열처리 한 분말이 보자력과 자화 값이 대체적으로 높은 값을 나타내었다. 그러나 ph 10인 경우에는 Fe : Ba 에 따 2 3

5 연구논문 공침법으로 합성한 바륨 페라이트 (BaM) 의 형성과 자기적 성질에 미치는 금속이온 몰 비 백인승 남인탁 213 FESEM micrgraph f BaM pwder btained at different ph (Fe : Ba = 12 : 1.5, 800 C, 2 hrs, HT.4: Furnace cling after heat treatment in O ). (a) ph 8, (b) ph 10. Fig Fig. 7. Hysteresis curves f BaM pwder btained at different ph (Fe : Ba = 12 : 1.5, 800 C, 2 hrs). (a) ph 8, (b) ph 10. Hysteresis curves f BaM pwder btained at different ph and Fe : Ba (800 C, 2 hrs HT.4: furnace cling after heat treatment in O ). (a) ph 8, (b) ph 10. Fig. 8. 2

6 214 Table I. Magnetic prperties f the samples as a functin f the relative amunt f Fe :Ba and heat treatment cnditins at ph 8 (H max =10kOe). Heat treatment Fe :Ba 13.6 : : : 1.3 8:1 σ (emu/g) H C (Oe) σ (emu/g) H C (Oe) σ (emu/g) H C (Oe) σ (emu/g) H C (Oe) Table II. Magnetic prperties f the samples as a functin f the relative amunt f Fe :Ba and heat treatment cnditins at ph 10 (H max =10kOe). Heat treatment Fe :Ba 13.6 : : : 1.3 8:1 σ (emu/g) H C (Oe) σ (emu/g) H C (Oe) σ (emu/g) H C (Oe) σ (emu/g) H C (Oe) j y ùkü, Fe Fe Ba ƒw y s ƒw. w œ» (HT.1, 2, 3) w»(ht.4, 5, 6) w y ùkü. ph 8 ƒ j ùkü (5.3 KOe), ph 10 ƒ j y (55.7 emu/g) ùkü. Table I Table II VSM w» w ùkü. IV. Fe :Ba ƒ 8 Fe Ba wš ph y œe w w M-type r p» w. ph 10 ù Fe Ba j w M-type r p w w»wz 19«6y, w. t j» m 50~200 nm, ³ew q xk ùkü.» ph 8 Fe Ba y yƒ j ùkû Fe Ba ƒw y ƒ w ù w w. ph 10 y j yƒ ù Fe Ba ƒw y s ƒw, HT.1 HT.4 j y ùkü. ph 8 ph 10 jš y ùkû ph 10 ph 8 y jš ùkû. š x [1] X. Liu, J. Wang, L.M. Gan, S.C. Ng, and J. Ding, J. Magn. Magn. Mater., 184, 344 (1998). [2] T. Fujiwara, IEEE Trans. Magn., 21, 1480 (1985). [3] V.B. Bregar, IEEE Trans. Magn., 40, 1679 (2004). [4] K.K. Mallick and Philip Shepherd, Rger J. Green, J. Eur. Ceram. Sc., 27, 2045 (2007). [5] J. Matutes-Aquin, S. Diaz-Castann, M. Mirabal-Garcia, and S.A. Palmares-Sanchez, J. Script. Mater., 42, 295 (2000). [6] Silvia E, Jacb, Lenard Civale, and Miguel A. Blesa, J. Magn. Magn. Mater., 260, 37 (2003). [7] Osami Abe and Masayuki Narita, J. Slid. State. Inic., 101, 103 (1997). [8] G. Xu, H. Ma, M. Zhng, J. Zhu, Y. Yue, and Z. He, J. Magn. Magn. Mater., 301, 383 (2006). [9] X. Liu, J. Wang, L.-M. Gan, and S.-C. Ng, J. Magn. Magn. Mater., 199, 452 (1992). [10] D. Mishra, S. Anand, R.K. Panda, and R.P. Das, J. Mater. Chem. Phys., 86, 132 (2004). [11] M. El-Hil, H. Pfeiffer, K. OGrady, W. Schuppel, E. Sinn, P. Grnert, M. Rsler, D.P.E. Dicksn, and R.W. Chantrell, J. Magn. Magn. Mater., 129, 339 (1994). [12] H. Szeri, J. Magn. Magn. Mater., 321, 2717 (2009). [13] H. Sakai, K. Hanawa, and K. Ayagi, IEEE Trans. Magn., 28, 3355 (1992). [14] S.E. Jacb, C. Dming-Pascual, R. Rdriguez-Clemente, and M.A. Blessa, J. Mater. Sci., 32, 1025 (1997). [15] U. Tpal, H. Ozkanb, and L. Drsinskii, J. Ally. Cmp., 428, 17 (2007). [16] S.R. Janasi, M. Emura, F.J.G. Landgraf, and D. Rdrigues, J. Magn. Magn. Mater., 238, 168 (2002). [17] M. Radwan, M.M. Rashad, and M.M. Hessien, J. Mater. Prc. Tech., 181, 106 (2007). [18] M.M. Rashad, M. Radwan, and M.M. Hessien, J. Allys. Cmp., 453, 304 (2008).

7 œe w w r p (BaM) x» e Áû k 215 [19] H.-F. Yu and P.-C. Liu, J. Allys. Cmp., 416, 222 (2006). [20] S.R. Janasi, D. Rdrigues, M. Emura, and F.J.G. Landgraf, Phys. Stat. Sl., 185, 479 (2001). [21] H.-S. Shin, J. Kr. Ceram. Sc., 34, 1045 (1997). Effects f Metal Ins Mle Rati, ph and Heat Treatment Cnditin n the Magnetic Prperties and Frmatin f C-precipitated M-type Barium Ferrite Pwders In Seung Baek and In Tak Nam Department f Advanced Materials Science and Engineering, Kangwn Natinal University, Chunchen , Krea (Received 7 Octber 2009, Received in final frm 20 Nvember 2009, Accepted 21 Nvember 2009) M-type barium ferrite (BaFe 12 ) pwders were synthesized thrugh the c-precipitatin methd. Starting material cmpsitin Fe :Ba mle rati was fixed as 8 and the relative amunt f Fe and Ba was cntrlled. Structure and magnetic prperties and pwder mrphlgy were investigated using XRD, SEM, VSM. Pwder shwing high cercivity and small magnetizatin was btained at ph8 and Fe :Ba f 12 : 1.5. Small magnetizatin value was riginated frm the existence f α-fe 2 O 3. Single-phase M- type barium ferrite were btained regardless f the heat treatment cnditin and the amunt f Fe and Ba at ph 10. The largest value f magnetizatin (55.7 emu/g) under investigatin were btained when Fe :Ba f 13.6 : 1.7 and furnace cled pwder in O 2. Particle size f pwder was in the range f 50~200 nm. Keywrds : M-type barium ferrite, c-precipitatin, metal ins mle rati, ph, Heat treatment cnditin

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