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1 1 w t œwz J. Kr. Inst. Surf. Eng. Vl. 44, N. 1, 011. < > Fe-%Cr-5.8%Al w š y ½ a, ya, b, œ c, ½»c,» a* a w œw, bw»» c w œw High-Temperature Oxidatin Behavir f Fe-%Cr-5.8%Al Ally Sng-Yi Kim a, Sung-Hwan Chi a, Jung-Yeul Yun b, Yung-Min Kng c, Byung-Kee Kim c, Kee-Ahn Lee a * a Schl f Advanced Materials Engineering, Andng Natinal University, Andng , Krea b Department f Materials Engineering, KIMM, Changwn , Krea c Schl f Materials Science Engineering, University f Ulsan, Ulsan , Krea (Received January 7, 011 ; revised February 18, 011 ; accepted February 7, 011) Abstract This study investigated the high temperature xidatin behavir f Fe-%Cr-5.8%Al ally and the xidatin kinetics f the ally were discussed. Bulk samples were prepared by VAM (vacuum arc melting) and ht frging. High temperature xidatin testes were isthermally cnducted up t 100 hurs in 79%N +1%O envirnment at three different temperatures (900 C, 1000 C, 1100 C). The weight gain was measured after xidatin accrding t xidatin time (, 4, 6, 8, 10, 15, 0, 5, 0, 60, 80, 100 hurs). The weight gain significantly increased with increasing xidatin temperature. As the temperature increased, the xidized samples shwed sequential frmatin f Al O, Cr-rich xide, Fe-rich xide. The activatin energy f high temperature xidatin was btained as 06.6 KJ/ml. Al O were develped n the surface in the early stage f xidatin, representing prtective rle f xidatin. Hwever, Fe-based and Cr-based xides leaded t breakaway f xide layer, thus resulted in the significant increase f additinal xidatin. Keywrds : Fe-%Cr-5.8%Al, High temperature xidatin, Oxidatin time, Oxidatin kinetics, Oxides 1. Fe-Cr-Al w š t y Al O x k. Al O y» x š ƒ š yw w 1). Fe-Cr- Al w yd w š š w ü, ü y ƒ -4). Fe-%Cr-5.8Al w 1400 C¾ ƒ w, š š. p k * Crrespnding authr. keeahn@andng.ac.kr»ƒ y e, (metal hney cmb) š» w ƒ w š 5). š y ü y w w š. wr x ¾ Fe-Cr-Al w w Fe- 5%Cr-5%Al 6), Fe-0%Cr-5%Al 7) š y w ƒ š. w w ü Al 8) Cr w y ü y w 9) w w. w ƒ Y 10-1), Zr 1), La 14,15), Hf m 16) ƒ» yd w w y w. ù

2 14 ½ /w t œwz 44 (011) 1-0 Fe-%Cr-5.8%Al w w š y w ƒ š j w š ü y p w w. p š y w y» ù y w ƒ 17) š,» š y ƒ š y y mw» ³ w ƒ w. Fe-%Cr-5.8%Al j 100 ƒ (900 C, 1000 C, 1100 C) š y x ww š y wš w y, w Fe-%Cr-5.8%Al š y» ³ wš w.. x Fe-Cr-Al w š p w š Fe-%Cr-5.8%Al(wt.%) w w.»», Φ0. mm w. š y r w w š œ j w (high vacuum arc melting furnace) w g. r ü ³ yw» w Trr œ 5z, w g p x k r w. w œ ü»œ w 1100 C 0 w z 50m w w» r w. z» r 7 7 1mm j» x ƒœwš š y x w š k 1.5 mm j» w. r t mm. y t e» w w w» w SiC Paper #000¾ w.» š y ƒœ r x 1 ùk ü. š y x 900 C, 1000 C, 1100 C ƒ ww. y» w gas»(79%n + 1%O ) w w x w bx electric furnace(tag ) w. š y w» w ƒƒ, 4, 6, 8, 10, 15, 0, 5, 0, 60, 80, 100 ww. ƒ š y x 5 C/ min g. ƒ ƒƒ 1 l/min w. r y x y yd w x (SEM) x x (FE-SEM) Ÿw x (OM) w. w y Áz X- ray EDS mw w.. x» Fe-Cr-Al w š y x ww w. ƒw ƒ y ƒw ƒƒ ü. 900 C ƒ y j ƒw y ƒƒ û C j ù» l 0 ¾ y ƒƒ û. Fig. 1.Specimen mrphlgy fr high-temperature xidatin test. Fig.. Effect f temperature and time n the xidatin weight gain f Fe-Cr-5.8Al in 79%N +1%O.

3 김송이 외 한국표면공학회 / 0시간에서 50시간까지는 점차적으로 기울기가 증가 하였으며, 50시간 이후에는 급격한 기울기로 산화 증량이 증가하는 것을 알 수 있다. 1100C에서는 이전 온도와는 확연한 차이를 보였는데, 초기부터 5시간까지 급격한 기울기로 직선적 무게 증가 거 동을 나타냈다. 그 이후 60시간까지 산화 증량의 증가가 거의 일어나지 않는 거동을 보였다. 그러나 60시간 이후 또 다시 급격한 기울기로 산화 증량의 증가 거동을 보였다. 1100C에서는 900C와 1000C 44 (011) 에 비해 모든 시간에서 가장 큰 산화 증량 값을 나 타냈다. 100시간에는 900 C에서 1100 C로 산화 온 도가 증가함에 따라 산화 증량이 mg/cm 에서 1.56 mg/cm 으로 10배 가량 증가하였으며 이에 현 저히 낮은 내산화성을 보였다. 그림 에 세 온도(900 C, 1000 C, 1100 C)에서 100 시간 동안 산화 실험한 산화층의 표면을 관찰한 결 과 중 온도 및 시간별로 대표적인 것들을 나타내었 다. 그림에서 온도에 따라 각각 다른 형태의 표면 Fig.. Surface mrphlgies f xide layer n Fe-Cr-Al ally with xidatin time (a) 900C, (b) 1000C, (c) 1100C.

4 김송이 외 한국표면공학회 16 / 산화물이 관찰되는 것에 주목할 만하다. 그림 (a)는 900 C에서 산화된 시편의 표면으로, 시간이 지남에 따라 초기 시간에서 60시간까지는 산화물의 성장 이 이루어 졌지만 60시간 이후 100시간까지 표면 산화물의 성장이 거의 일어나지 않는 것을 관찰할 수 있다. 형성된 산화물은 whisker 형태로 관찰되 었으며 EDS 분석 결과 대부분이 Al O 로 나타났다. (b)의 1000 C에서 산화된 시편에서도 초기 시간부 44 (011) 1-0 터 60시간까지 산화물 입자가 성장하는 경향을 나 타냈다. 그러나 60시간 이후 100시간까지는 입자 크기가 거의 유사하게 나타났다. 상기의 결과에서 60시간 이후 산화 증량값(그림 )의 급격한 증가가 나타났지만 표면의 산화층은 거의 변화가 없었다. 또한 900 C에서 whisker형으로 형성된 산화물과 달 리 glbular한 형태로 산화물이 성장한 것을 알 수 있었다. 산화물의 입자 크기는 900 C와 유사하게 나타났다 C의 표면EDS 분석 결과 역시 대부 분이 Al O 인 것으로 나타났다. 그림 (c)는 1100 C 에서 산화된 시편의 표면으로 900 C와 1000 C에 비 해 초기 시간부터 산화물 크기가 조대하게 나타남 을 알 수 있었다. 시간의 증가에 따라 60시간 이후 다른 온도(900 C, 1000 C)에 비해 산화물 입자의 크 기가 확연히 커진 것을 관찰할 수 있다. 또한 입자 들이cluster를 이루며 거대한 산화물로 형성되어 산 화층의 성장이 일어난 것도 확인할 수 있었다. 세 가지 온도에서 시간의 증가에 따른 산화물 성장의 차이가 나타났으며 온도에 따라 다른 형태의 산화 물이 나타났다. 산화 실험 후 시편의 산화층 단면을 관찰한 결과, 기본적으로 모든 온도 조건(900 C, 1000 C, 1100 C) 에서 시간이 증가함에 따라서 산화층의 두께가 증 가하였다. 그림 4에 시편의 단면을 보여 주는 예로 써 1100 C에서 시간의 증가에 따라, 15, 60, 100 시간 동안 산화한 시편의 산화층 두께 차이를 나타 내었다. 초기 시간(a)에서 약 µm로 외부에 얇은 산화층이 형성되었다. 이후 15시간 (b) 이후 산화층의 성장이 일어나 1. µm 두께의 산화층을 형성하였다. 시간의 증가에 따라 계속적인 산화층 성장이 일어나 60시간 (c) 후에는.46 µm로 약 배 정도 두께의 산화물을 관찰할 수 있었다. 최종적으 로 100시간 (d) 후 매우 많은 양의 산화가 일어남 을 확인하였으며 내부로 산소 확산이 활발하게 일 어나 다량의 산화물이 내부에 형성되어 있는 것을 알 수 있다. 세 온도 조건에서 산화 시간에 따른 XRD 분석 을 수행하였으며 그 중 대표적인 시간들의 실험 결 과들을 그림 5에 나타내었다. 산화 전 XRD 결과에 서는 α-fe 단상의 peak만 나타났으며 산화물의 peak 는 검출되지 않았다. 900 C에서는 시간이 증가함에 따라 산화 초기인 시간 후에 α-al O 가 검출되었 다. 또한 5시간 이후 이전 시간에서 희미하게 나 타나던 α-al O peak가 명확히 검출되었다 C 에서도 900 C에서 관찰되었던 산화물이 검출되었 다. 시간 후에 α-al O 가 검출되었으며, 900 C보 다 더 빠른 시간인 15시간 후에 α-al O peak가 Fig. 4. Grwth f xide layer n Fe-Cr-Al ally with xidatin time at 1100C (a) h, (b) 15 h, (c) 60 h, (d) 100 h.

5 ½ /w t œwz 44 (011) Fig. 5. XRD analysis results f Fe-Cr-5.8Al Bulk specimen, xidized fr 100 hurs at 900 C (a), 1000 C (b), 1100 C (c).. 5 z 900 C ùkù α-al O peakƒ 1000 C y. w Fe O 4 peakƒ w. y 5 z y ƒw w ùk üš C š y k y, y ƒ. z 900 C, 1000 C α-al O ƒ w. w w FeCr O 4 Fe O 4 peak ùkû. peak 6 z y w.» y ƒw ùkù. wì ƒ ƒw x y yw. w ƒ x y ƒ wš yƒ w. 6 yd s» w (900 C, 1000 C, 1100 C) 100 y k z EDS w ùkü. (a) 900 C yw yd r t x. w ü yd x w, EDS d Al O ù kû. ù (b) 1000 C ƒ ƒw ¾ ¾ ü y (internal xide) swš š, Al O y ƒ ùkû. ƒ x y Cr Fe y Al O d x. XRD y ùkù EDS mw y w. w» ü Al ww ü Al O ƒ x w. ü Cr, (Fe, Cr)- y, w y w C(c) ƒ É yd x w ü y ƒ ¾ ùkù x w yƒ ù. w Al O d Fe-rich y wì w. 4. š x Fe-%Cr-5.8%Al w š y w. w mw ƒ ƒ w y ù.» y ( ) k w y wš y» (0 :» 0 ¾ parablic y ùký) w y (K p ) d w. y mw w

6 김송이 외 한국표면공학회 18 / 44 (011) 1-0 Fig. 6. Crss-sectinal micrstructure and EDS analysis result f Fe-Cr-Al ally at (a) 900 C, (b) 1000C, (c) 1100C. 른 산화가 일어남을 의미한다. 그림 7을 바탕으로 Fe-%Cr-5.8%Al 합금에 대한 활성화 에너지 값을 900 C에서 1100 C까지 온도 구간에서 각각의 K 값 을 온도의 역수에 관해 나타낸 그림의 기울기와 다 음의 식 ()를 통해 계산하였다. 얻어진 값은 06.6 KJ/ml로 나타났다. p K = K exp( Q/RT) p () 0 이때 K : 상수, R: 기체상수, T: 절대 온도이다. Shin 등 은 온도가 1 K에서 147 K일 때 Fe0%Cr-5%Al의 활성화 에너지를 8 KJ/ml이라 발 표하였다. 이것은 Al O 산화층을 통과하는 산소이 0 19) 온의 활성화 에너지로 제시되었으며 본 연구 결과 에서도 유사한 값을 얻었다. 이상의 결과들을 요약하여 Fe-%Cr-5.8%Al 합 금의 시간 및 온도에 따른 고온 산화 거동 모식도 를 그림 8에 나타내었다. 세 온도 모두 시간이 증 가함에 따라 산화층 성장이 일어나며 온도가 증가 함에 따라 산화물이 단계적으로 생성된다. 즉 900 C 에서는 표면에 고온에서 안정한 Al O 가 whisker형 으로 생성되었으며 일부가 내부에 산화물이 형성 되지만 비교적 안정하게 기지를 보호하는 역할을 한다. 이러한 whisker 형의 산화물과 관련하여 Fig. 7. Parablic xidatin rate cnstant and activatin energy in xidatin f Fe-Cr-Al at 900C~1100C. 그 결과를 그림 7에 도시하였다. W =K t (1) p 그 결과 온도에 따라 K 값은 직선적인 관계를 나 타냈으며, 900 C에서 1100 C로 온도가 증가함에 따 라 7.8(mg cm sec )에서 5.49(mg cm sec )로 값이 증가하여 나타났다. 이것은 산화 속도가 온도 에 의존해 나타나는 결과로 높은 온도에서 가장 빠 p

7 ½ /w t œwz 44 (011) Fig. 8. Schematic illustratin f temperature xidatin behavirs f Fe-Cr-5.8Al ally. Brchardt 4,18) Fe-Cr-5Al w Al O y û y whiskerx y x y f ü Al y w w š š w. t y ( ) 1000 C, 1100 C whiskerx y 900 C w C É yd x w ƒ ƒw Al ùš O y y w» Cr ww Al O d Cr-rich y ƒ xk y d x w. w ü (Fe, Cr)-rich xideƒ» w. ü x y t y d ùkù ƒ weight gain ƒ( )» w. ƒ yƒ w w y»» 1100 C» ü Al y y ù Al O g É yd x k. w» ü Al š y x w w O y ƒ» ü Fe, Cr w w (Fe, Cr)- rich y k. Ishii 0) Fe-(0-5)%Cr-5%Al w š y(14k-147) Fe O ƒ Al O d q w y œw breaka way w š š w. 6 (c) w» Feƒ y t Fe y x breakawayƒ ù w, Fe y z l w y ƒ w ù y w. Fe-%Cr-5.8%Al w y Cr ù Fe y y w w Al O yd ³ g w ü y w j w q. 5. Fe-%Cr-5.8%Al w š y w y w š y» w ³ w w ý. (1) Fe-%Cr-5.8%Al w ƒ š y x ƒ y ƒƒ ùkû. 900 C w 1100 C x y ùkù ƒ yƒ w. w š y w y y 06.6 KJ/ml. () š y y w t y x ùkû 900 C Whisker xk y x š yƒ w 1100 C yd cluster w yd x. () ƒ š y y 900 C 1000 C Al O, Crrich y 1100 C FeCr O 4, Fe O 4ƒ ƒ. ƒƒ y 900 C 1100 C ƒ ƒw y w y Al y x w wš y x ƒ y x.

8 0 ½ /w t œwz 44 (011) 1-0 (4) Fe-%Cr-5.8%Al w y»(0 ) ü Al O g Al O yƒ w. z Al ü ü yd x yƒ ùkù. z û Cr ù Fe y yd ³ g w y ƒ ùkû. z»» w. š x 1. J. G. Smeggil, A. W. Funkenbusch, N. S. Brnstein, Metall. Trans., 17 (1986) 9.. J. L. Smialek, Metall. Trans., 9A (1979) 09.. P. A. Mari, J. M Chaiz, J. P. larin, Oxidatin f Metal, 17 (198) J. Jedlinski, G. Brchardt, Oxidatin f Metals 6 (1991) M. H. Lagrange, A. M. Huntz, J. Y. Laval, Ann. Chim. Fr, 1 (1987) I. M. Wlff, L. E. Iri et al., Mater. Sci. Eng., A41 (1998) Z. L. Zhang, D. Y. Li, X. Q. Dng, Acta Metall. Sin., 0 (007) S. E. Sadique, A. H. Mllah, M. M. Ali et al., J. Crrs. Sci. Eng., 1 (000) Y. Niu, S. Wang, F. Ga et al., Crrs. Sci., 50 (008) R. Cueff, H. Buscail, E. Caudrn et al., Crrs. Sci., 45 (00) D. P. Whittle, J. Stringer, Phil. Trans. R. Sc. Lnd, A95 (1980) F. Clemendt, J. M. Gras, J. C. van Duysen, J. de Physique IV, (199) S. C. Chi, S. Park et al., Kr. J. Met. Mater, 5(1) (1997) K. S. Lee, H. Y. Ra, J. Met. Mater., 4(1) (1996) S. Hirshi, K. Masski, Y. Keiichi, Kawasaki Steel Technical Reprt N., 1 (1994). 16. B. G. Mn, S. C. Kang, G. M. Kim, J. Crrs Sci. Sc. f Krea, 5() (1996) Z. L. Zhang, X. J. Ahang, T. J. Pan et al., Gangtie Yanjiu, 5() (007) W. J. Quadakkers, J. Jedlinski, G. Brchardt et al., Appl Surf. Sci., 47 (1991) Y. C. Shin, K. S. Lee, W. W. Park, Kr. J. Met. Mater., 4(7) (1996) K. Ishii, T. Kawasaki, J. Jpn. Inst. Met., 56 (199) 854.

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