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1 Jurnal f the Krean Magnetics Sciety, Vlume 19, Number 5, Octber 2009 DOI: /JKMS » p «xá yá ŸtÁ Ÿ w, w w œ, 322, Ÿ w, ÁŸ v w, 344-2, ( , , y ) Sl-gel w w w, w w p, j»,» p w w. ƒ (Fe Fe 1:2 Fe ) 2+ 2-methxyethanl w refluxingw z,» 200~600 C w r p w w. X- z» w w w y w 250 C spinel r pƒ y w. x w dw w ƒ j» ƒ dw. Mössbauer Ÿ x j» y dw. 1:2 yw z 250 C w j»ƒ ew 78 % p 22 % p ƒ. Fe w C spinel ƒ ù j»ƒ p. 250 C w w x p š, ƒ sy yƒ ƒwš w ƒw y w. : r p, Mössbauer Ÿ, -» y I. r p yw, ü w» p»» p y w w š [1]. w y w t y ƒ w w. w y w š. y w w, w w š, q w y w š. w wš w y» ƒ y w š [2].» p pw p ùkü, w r p w ƒ w [3-6]. j»» p w ƒ 2+ƒ 3+ Fe Fe y α-fe 2 O 3 x w w š [7]. w w» w y w Ar y N 2» ƒ v w [6]. sl-gel w yw *Tel: (043) , wš» w w. X- z» w w y wš, x (FESEM) j» dwš w. Fe s» w w Mössbauer Ÿ» r (VSM) w y» p d w w. II. x Sl-gel w ƒ w. 98 % Fe(CO 2 CH 3 ) % Fe(NO 3 ) 3Á9H 2 O a) 1:2 b) Fe(CO 2 CH 3 ) 2 w 2-methxyethanl(2-MOE) ww z 80 C 12» w k. 150 cc 6~8 g w w. w 90 C» 24 w 2-MOEƒ w. w w z, r p p w» w 200, 250, 300, 400, C ƒƒ 6»w spinel r 180

2 » p «xá yá ŸtÁ ŸÁ 181 p.» w w ƒ w» w w ù, w wš ù 5~ 10 cc w. w w» w Cu-Kα w X- z» (Philips PW1700: XRD) w j» y d w. w, j» w š d w x (FESEM) w dw. y - y r p ü Fe s d w Mössbauer Ÿ x w. r p» p w r w ( j») y sy y y w w. d w Mössbauer Ÿ spectrum Lrentzian w w w ful v w data fitting w. yp d w 6kOe» w ù, w» r p sy y ƒ w» w» ù, p ƒ j»» p ww» w»». III. x Figure 1(a) (1 : 2) w XRD d. XRD w 200 C r p (311) w peak d» w, 250 C w r p peak d. 250 C sl-gel w w w spinel x w. w, y w ƒ peak s w w ùküš ƒ f». y peak e y d š. Fig. 1. (a) X-ray diffractin diagrams f pwders made with Fe 2+ /+ = 1/2 as a functin f annealing temperatures: a) 200, b) 250, c) 300, d) 400, e) 500 and f) 600 C. (b) X-ray diffractin diagrams f pwders made with nly Fe 2+ as a functin f annealing temperatures: a) 200, b) 250, c) 300 and d) 400 C.

3 한국자기학회지 제19권 5호, 2009년 10월 182 Figure 1(b)는 Fe2+ 이온의 조건으로 준비한 분말을 200, 250, 300와 400 C에서 열처리한 Fe3O4 분말의 XRD 측정 결과이다. 200와 250 C에서 열처리한 분말의 XRD 결과에 의하면 2θ 21 근처에 spinel 페라이트와 다른 구조에 의한 peak이 관측되었으나, 300 C 이상의 열처리에서는 Fe3O4 분 말에 의한 peak을 관측됨을 알 수 있다. 이러한 결과는 N2 분위기의 열처리 중 Fe2+의 일부가 Fe3+로 변화하여 spinel 페라이트를 구성하는 것으로 해석할 수 있다. Figure 1(a)의 결과에 비교하여 Fe2+ 이온만을 이용하여 합성한 페라이트는 낮은 온도(200 C)의 열처리로 spinel 페라이트의 모든 peak 의 관측이 되고 있다. 이것은 당량비의 조건으로 준비한 시 료에 비하여 Fe2+의 이온만을 이용하여 합성한 분말이 보다 낮은 온도에서 합성됨을 알 수 있다. 열처리 온도가 높아짐 에 따라 XRD 측정 결과는 당량비의 조건으로 준비한 시료 와 유사한 XRD 특성을 보인다. Figure 2는 당량비의 조건으로 준비한 시료를 250, 300, 400, 및 500 C의 온도에서 열처리한 Fe3O4 분말을 20만 배 의 배율로 확대하여 관측한 전계전자현미경 사진이다. 이러한 전자현미경 사진은 sl-gel법을 이용하여 제작한 시료의 전형 적인 모양을 나타내고 있으며, 열처리 온도의 높아짐에 따라 입자의 크기가 증가하는 경향을 보인다. 500 C에서 열처리한 입자는 30~40 nm의 입자 크기와 250 C에서 열처리한 입자 의 크기는 10~20 nm의 크기를 보인다. 저온서 고온으로 열처 리 온도가 높아짐에 따라 입자의 크기가 급진적으로 커지지 는 경향을 보이지는 않으나, 입자의 모양이 보다 선명하고 크 기가 증가하는 것을 확인 할 수 있었다. 이러한 입자 크기의 변화는 Fig. 1(a)에서 열처리온도의 증가에 따른 (311) 면의 peak 폭이 감소하는 것과 같은 결과를 의미한다. Figure 3(a)는 철의 당량비(1 : 2) 조건으로 준비한 분말을 다양한 온도에서 열처리한 후에 상온에서 측정한 Fe O 분말 의 Mössbauer 흡수 spectrum이다. 200 C 열처리한 입자의 Mössbauer spectrum은 두 개의 dublet 공명흡수선으로 fitting한 결과이다. 입자가 상자성 측성을 보이고 있음을 의 미한다. Spectrum의 분석 결과는 Fe 로 독립된 입자 형태를 유지하는 분석결과를 보이고 있으나, 정확한 구조나 산화물 형태에 관하여서는 좀 더 많은 연구를 필요로 한다. Figure 3(a)의 b)는 250 C에서 열처리한 입자의 경우 상자성 특성과 준강자성 특성을 동시에 가짐을 보여준다. 이것은 sl-gel법으 로 합성 열처리한 분말의 크기는 준강자성-상자성 전이가 일 어나는 입자의 크기를 중심으로 Gaussian 분포를 하며, 22 % 의 분말은 입자 크기가 너무 작아서 상자성체의 특성이고, 78 %의 분말은 충분한 입자크기로 준강자성의 특성을 가지는 것을 뜻한다. 열처리 온도가 300 C보다 높은 경우에는 전형 적인 Fe O 분말의 Mössbauer 흡수 spectrum과 같은 형태 를 보이고 있다. 이것은 Fig. 1(a)과 Fig. 2의 실험 결과와 같이 열처리 온도를 높임에 따라 입자의 크기가 증가하게 되 고, 입자 크기의 변화로 인한 준강자성-상자성의 변위가 발생 하는 것을 Mössbuaer 분광실험을 통하여 확인할 수 있었다 Scanning electrn micrgraphs f Fe O pwders annealed at varius temperatures: a) 250, b) 300, c) 400, and d) 500 C. The marked length is 10 nm. Fig

4 » p «xá yá ŸtÁ ŸÁ 183 Fig. 3. (a) Mössbauer spectra f pwders made with Fe 2+ /+ = 1/2 as a functin f annealing temperatures: a) 200, b) 250, c) 300, d) 400, e) 500 and f) 600 C. (b) Mössbauer spectra f pwders made with nly Fe 2+ as a functin f annealing temperatures: a) 250, b) 300, c) 400, and 600 C. Figure 3(b) Fe w w , 250, C w Mssbuaer spectrum. 200 C w x w œ š. ù Fig. 3(a) 200 C spectrum 2+ Fe w dublet œ d. Fig. 1(b) XRD d Fe 2+ spinel š Fe ƒ w»» 2+ w. 250 C w Mössbauer spectrum Fig. 3(a) b) spinel ƒ w spectrum.» p p ƒ w w l C w j» - ƒ w w C w œ spectrum Fig. 3(a) spectrum w w š. Fe ƒ 2+ N 2» 3+ Fe y spinel w w w. š w w œ Mössbauer parameter y d w parameter w ƒ. Figure 4(a) w w VSM d w p sy y ƒ. sy y ƒ j» y w, 300 C w w x p š. 200 C w û sy y ƒ spinel ƒ š super-paramagnetic p ƒ». 82 Oe ùküš ù sy y y w d w» w j. 250 C w Mössbauer Ÿ x ùkù 22 % p wš 200 C w sy yƒ ƒw ù, š w û ƒ. û p ƒ p ƒ y y w».

5 184 Fig. 4. (a) Saturatin magnetizatin and cercivities f the pwders made with Fe 2+ /+ =1/2as a functin f annealing temperatures. (b) Saturatin magnetizatin and cercivities f the pwders made with nly Fe 2+ as a functin f annealing temperatures. ƒ f sy y ƒ ƒ slgel w spinel r p x x. 500 C sy y ƒƒ Fe r p š, j»ƒ f ƒ p ƒ». 700 C j sy y yƒ. Figure 4(b) 2+ Fe w w w y yp p w. Figure 4(a) ƒ sy y ƒ š. 200 C w sy y 43 emu/g 8Oe š. Fig. 4(a) 200 C w»wz 19«5y, spinel r p j»ƒ super-paramagnetic p». 250 C w sy y x p. 600 C w 157 Oe sy y 52 emu/g w w. IV. 2+ Fe Fe y w 3+ Fe 2 O 3ƒ e» p ƒ. y w» w» 250 C ƒ spinel r p. ƒ r p j»ƒ f» p y dw. w j» y XRD x, FESEM d Mössbauer Ÿ x mw y w. w VSM w d w š w x r p p š. w Fe w 2+ w w û x. 2003w w w. š x [1] A. Gldman, Mdern Ferrite Technlgy, Van Nstrand Reinhld, New Yrk(1990). [2] S. W. Hyun, T. Kuh, S. J. Kim, and C. S. Kim, J. Appl. Phys., 105, 07A506-1(2009). [3] J. L. Drmann and D. Firani (Eds.), Magnetic Prperties f Fine Particles, Nrth-Hlland, Amsterdam(1992). [4] G. C. Hadjipanayis and R. W. Siegel (Eds.), Nanphase Materials: Synthesis, Prperties, Applicatin, Kluwer Academic Publishers, Drdrecht(1994). [5] R. C. Ashri, Nature, 379, 413(1996). [6] y, Ÿ, Ÿt, «x, ½, w»wz, 19, 57(2009). [7] R. Y. Hng, J. H. Li, H. Z. Li, J. Ding, and D. J. Wei, J. Mag. Mag. Mat., 239, 160(2002).

6 » p «xá yá ŸtÁ ŸÁ 185 Grwth f Particles and Their Magnetic Prperties W Hyun Kwn, Seung Wha Lee, Kwang Py Chae, and Jae-Gwang Lee Department f Applied Physics, Knkuk University, Chungju , Krea Jung Chul Sur Department f Physics, Wnkwang University, Iksan , Krea (Received 28 August 2009, Received in final frm 29 September 2009, Accepted 30 September 2009) particles, prepared by a sl-gel methd, were examined fr their structural characteristic, particle shapes and sizes, and their magnetic prperties. Tw different chemical cmpsitins (using a ml rate Fe 2+ /+ = 1/2 and nly Fe 2+ ) and 2-methxyethanl were used fr making prper slutins. And the slutins were refluxed and dry in a dry ven and the samples were fired at 200~600 C in the N 2 atmsphere. The frmatin f single-phased spinel ferrite pwders was identified with the X-ray diffractin measurement as they were fired at abve 250 C. The result f scanning electrn micrscpy measurement shwed the increase f annealing temperature yielded the particle size increased. The magnetic transitin was bserved using the Mössbaur spectrscpy measurement. As the ferrite, prepared with the chemical cmpsitin (Fe 2+ /+ = 1/2), was fired at 250 C, 78 % f the ferrite had a ferrimagnetic prperty and 22 % f the ferrite was nn-magnetic. In case f preparing the sample with nly Fe 2+ and annealed at 200 C, it had a single phased spinel structure but its particle size was t small t be ferrimagnetic. The annealing temperature abve 250 C made pwders a spinel structure regardless f the preparatin methd. They had a typical sft magnetic prperty and their saturatin magnetizatin and cercivity became larger as the annealing temperature increased. Keywrds : ferrite, Mössbaur spectrscpy, sl-gel methd and magnetic transitin

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