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1 Journal of the Korean Ceramic Society Vol. 46, No. 3, pp. 295~300, DOI: /KCERS Analysis of Oxide Coatings Formed on Al1050 Alloy by Plasma Electrolytic Oxidation Bae-Yeon Kim, Deuk Yong Lee*, Yong-Nam Kim**, Min-Seok Jeon**, Whan-Sik You***, and Kwang Youp Kim*** Department of Advanced Materials Engineering, University of Incheon, Incheon , Korea *Department of Materials Engineering, Daelim University College, Anyang , Korea **Korea Testing Laboratory, Seoul , Korea ***MST Technology, Incheon , Korea (Received April 6, 2009; Revised April 14, 2009, April 22, 2009; Accepted April 28, 2009) Al1050 w Plasma Electrolytic Oxidation x yv ½ Á *Á½ û**á **Á ***Á½Ÿ *** w œw * w w **w» x ***MST Technology ( ; ; ; ) ABSTRACT The crystal structure of surface coatings on Al1050 alloy by PEO (Plasma Electrolytic Oxidation), were investigated. The electrolyte for PEO was Na-Si-P system solution. The main crystalline phase were γ-alumina and α-alumina. Crystallinity was increased with applied voltage and applied time. The dominant crystalline phase were affected not only chemical composition of Al alloy substrate and electrolyte, but also the +/ ratio of applied voltage. Key words : PEO, Coating, Alumina, Crystal structure, XRD 1. t j yw,»yw. yw t yw mw y k ü t v x w y (chemical conversion)ƒ, t w ù w t j ù üyw w w.»yw. k (Passive Metal) w Mg, Al, Ti, Zn, Nb w 15 ~ 50 V ƒw t É y v x j y ƒ r. w t y ƒx xk» w ü Corresponding author : Bea-Yeon Kim Tel : Fax : w mw»»œ x. ƒ» ü»œ» z œ š»œ w. w k t y v x k» Plasma Electrolytic Oxidation( w PEO, MAO(Micro Arc Oxidation)) š».»» w ü 15 V ~ 50 V ü ƒw w PEO 350 V ~ 550 V ƒw y v x j.»» y v w w t w yv x k ey., 10 v { wš ü, ü ù., Cu Si w wš» t ƒ ƒ w š dicasting Al w t 295

2 296 Al1050 w Plasma Electrolytic Oxidation x yv Table 1. Chemical Composition of Al1050 (%) Si Fe Cu Mn Mg Cr Zn Ti Cu+Si Al more than Fig. 1. Schematic diagram of Plasma Electrolytic Oxidation coating layer. There are three different layers, (1) inner Transition Layer, (2) Main Functional layer, which has high hardness, and (3) external so-called Technological layer, which has high porosity and low hardness. 2) ƒ ƒ w š. PEO» 1970 gq wœ. p» Fe š Carbonizing ù Nitriding ƒƒ ww.» 1990 z» wù A. L. Yerokhin PEO w review paper t 1) wš, z Keronite 2) ƒ» y w w y y» w. PEO w k y v y v x» w w ü» gq. Plasma ù q mismatch w stressƒ ù,»» w { y v x» üyw w ù š., PEO»», p w ù, w ü ù w w gq œ š, gq t Fig. 1 Technological layer š»œ 20% t d w š. ƒ ûš, ü w» technological layer gq z w w. ù t d w Keronite PEO gq d w Ni ù PTFE (lv ) š ƒ gqw w wš.,» PEO œ w PEO œ z ù š gq x handphone, l e OIS(Optical Image Stabilizer, e) frame, BGA(Ball Grid Array) frame particle w t š. w Mg w ƒ t gq wš. 3) ù PEO gq w y w w. PEO w t y gq w w ø. PEO w Al y gq ƒ y v» w wš w. 2. x Al q Al1050 w. Al1050 w w Al 99% w» w w q w. Al1050 q Al w Si, Cu, Mn, Mg, Fe, Cr, Ti ƒƒ w» w ƒ» x ú y š w. x Al1050 t yw ùkü. PEO ü M ƒ w n-pec PEO e 300 V ~ 600 V, 300A e pulse w. w l p q w mm j» w. w w kj ü stirrer ew x w w x ú w y w w. x w w NaOH w Na 2 SiO 3 ƒw 2~3%. x w w, w w w. w wz

3 ½ Á Á½ ûá Á Á½Ÿ 297 Table 2. Formation of PEO Coating Layer with Various Applied Voltage in Type A and B Solution. A Electrolyte System Contains NaOH and Phosphoric Acid and B, Na 2 SiO 3 with Phosphoric Acids. Note that ø Means Successful Coating, and ÿ Means Intermediate State, Means Failure Volt Electro. A B Ü ÿ ÿ ÿ ø ø ø ø ø ø ø Ü Ü ÿ ÿ ø ø ø ø ø ø ø Volt Electro. A B ø ø ø ø ÿ ÿ ÿ ÿ Ü Ü Ü ø ø ø ø ø ø ÿ ÿ ÿ ÿ Ü Applied Voltage w Table 2 ƒ x y t d k w ùkü. t ÿ t œ t t v x w w w r ùkü. w gq ù r ƒ r t ù ƒ. z x ygq d š, w ü ew r ƒ r ƒ r ƒ w» x w. y r ew gq q Al1050 þƒ w segregation ³x w x, Al1050 q ƒœw œ w y w w q. t solution A NaOH H 3 PO 4 ww, solution B Na 2 SiO 3 H 3 PO 4 ww w. w. z x Si w w w» w A w» w ww v x Fig. 2 A w ü Al r ƒ ƒ 450 V, 420 V, 400 V ƒw t yv x Ì w. Fig. 2. Thickness of PEO-coated alumina layer on Al1100 substrate with PEO coating time. Note that; þ is at 450 V, ø, at 420 V, and ÿ, at 400 V. Fig. 2 ƒ j» w š ƒ ƒw t gq d wš. ƒw 400 V, 420 V, 450 V 1µm/min ü t gq w. w, 30 ƒw t gq d ƒ, 200 µm ƒ t gq d Ì w. w x r 50 mm 50 mm 1.0 mm j» w, e» w tank j» w r j» y v x r t» t gq d ƒ w š q. r j»ƒ jš t Fig. 1 1 µm/min t gq.» š w 4) š. t yd ̃ É ü Al t t Al y t yd y w r t ƒ j» w y v d ̃ É û» ù x w. ww PEO w t gq w w» w,»k r j» w kj j», j» w e ƒ. 46«3y(2009)

4 298 Al1050 w Plasma Electrolytic Oxidation x yv Fig. 3. XRD pattern of PEO-alumina coated Al 1050 substrate, (a) 2 min, (b) 5 min, (c) 15 min, and (d) 30 min. Note that ø is Aluminum, is α-alumina, and is γ- alumina t yv Fig. 3 A w PEO gq x t yv XRD w. v x» 2 5 y v ̃» y v Al substrate peak. ƒ û γ- aluminaƒ ùš z α- alumina peakƒ w.» 1,4-6) w y v α-alumina γ-alumina š šw š w. A.L. Yerokin 1,4) Mgƒ w γ- aluminaƒ 1)š w š, Cu swwš Al alloy α-aluminaƒ w 4)š w. x w Mg Cu ƒ, A.L. Yerokin 1) wš w» w w q. š X. Nie 5,6) Si(ß 1.3%), Cu(0.4 ~ 1%) Mn(0.6 ~ 1.2%) w w Al6082 w yv» ƒ w ƒƒ α-alumina γ-aluminaƒ x š w šw. w XRD substrate t I/I 0ƒ 100 (111) intensityƒ ùkù š š, (200) peak intensityƒ f cubic structure γ-aluminaƒ x š ƒw. Al FCC ¼ wù, PEO y v x x file-up w v š t v w Fig. 4. XRD pattern of PEO-alumina coated Al 1050 substrate at (a) 400 V, (b) 420 V, and (c) 450 V. Note that ø is Aluminum, is α-alumina, and is γ-alumina. t w yv x e» substrate w š». w t yv x. PEO yv substrate transition layerƒ w. d substrate w v w w q š. z γ-aluminaƒ ùkù w. yv x» γ- aluminaƒ x ƒ v w ƒ. Fig. 4 ƒƒ 400 V, 420 V 450 V 15 PEO w r t ùkü.» ƒw w wš w. ƒw f y v f w. PEO w x yv y. ƒw w ƒw ƒ» x q., γ-aluminaƒ. γ-aluminaƒ α-alumina w ƒ û» z t ü w e w. Fig. 5 w 400 V, 420 V, 450 V pulse ƒw +/- 4:3 w 30 y v x k t XRD w. x Fig. 3 4 α-aluminaƒ x š. γ-alumina» x w q ù, α-alumina ƒ f w wz

5 김배연 이득용 김용남 전민석 유완식 김광엽 Fig. 5. XRD pattern of PEO-alumina coated Al1050 substrate at (a) 400 V, (b) 420 V, and (c) 450 V, and the +/- pulse ratio is 4 : 3. Note that is Aluminum, is α-alumina, and is γ-alumina. Fig. 7. Fig SEM photograph of PEO treated Al Surface, (a) reflected electron image and (b) secondary electron image. 있다. 또한 전압의 크기가 커질수록 α-alumina의 형성이 많아지는 것을 관찰 할 수 있었다. 이러한 것은 산화 피 막의 경도 및 내마모성이 인가되는 전압의 형태에 따라 서 변화될 수도 있음을 말해 주는 것이라고 해석할 수 있 을 것이다. 이것은 또한 PEO에 의한 산화 피막 형성에 있어서 산 화피막의 결정상을 좌우하는 요소가 기존에 알려진 합금 성분에 의한 영향이라든지, 전해질의 종류 및 농도 등에 의한 것도 있지만, 전기적 신호에 의해서도 변수가 생길 수 있다는 것을 보여준다고 하겠다 표면 morphology 관찰 다음 Fig. 6의 사진은 PEO 처리한 산화피막의 표면을 전자현미경으로 관찰한 것이다. 표면에 규칙적인 6각 기 둥형태의 조직과 기공이 형성되는 아노다이징과는 달리 불규칙하게 기공이 존재하고 있음을 알 수 있다. 사진 우 측 상단에 있는 grain의 중앙에 작은 기공의 형태가 남아 있는 것을 볼 수 있다. 이는 표면에서 미세하게 폭발하는 고온의 플라즈마에 의하여 용융된 알루미늄이 전해질 성 분과 반응하면서 다시 굳으면서 생긴 흔적을 잘 보여주 고 있다. 또, 좌측 및 중앙의 grain에서도 같은 현상을 관 찰할 수 있으나, 이 두 grain의 경우에는 중앙 부분에서 SEM photograph and EDXA result of cross cut Al1050 alloy surface with oxidation layer oxidated by PEO. 미세 폭발과 이에 따르는 grain 중앙 부분의 수축과 함몰 로 인하여 밑으로 꺼지면서 형성되는 미세 crack이 발생 되어 있는 것을 볼 수 있다. 다음의 Fig. 7은 산화피막의 단면을 관찰한 사진이다. 알루미늄 substrate와 산화피막은 기공이나 crack 등이 없 이 알루미늄 표면에 잘 발달되어 있음을 알 수 있으며, 표면에 산화층이 균일한 두께로 존재하고 있음을 알 수 있다. 또한 앞서 지적한 표면의 푸석층의 존재도 관찰되 지 않음을 알 수 있었다. 4. 결 론 Al1050 알루미늄 합금을 Na-P 및 Na-Si-P계의 전해액을 이 용하는 Plasma Electrolytic Oxidation 방법으로 400 V~450 V 부근에서 표면 산화 피막을 형성시킨 다음 표면을 관찰 하여 다음과 같은 결론을 얻을 수 있었다. 1. PEO에 의하여 형성되는 산화 피막의 결정상은 주로 α-alumina와 γ-alumina가 얻어졌다. 2. 인가되는 전압이 높을수록, PEO 산화 처리 시간이 길어질수록 산화피막의 전체적인 결정성이 커지는 것을 알 수 있었다. 3. 산화 피막에 형성되는 결정상의 종류는 기존에 알려 진 모재 금속의 합금성분과 전해질의 원소 종류 및 농도 등에도 영향을 받지만 인가되는 전원의 +/- ratio에 의하 여서도 변화될 수 있다. Acknowledgment 이 논문은 2007년도 인천대학교 자체연구비에 의하여 연구되었습니다. 제 46 권 제 3호(2009)

6 300 Al1050 w Plasma Electrolytic Oxidation x yv REFERENCES 1. A.L. Yerokin, X. Nie, A. Leyland, A. Matthews, and S.J. Dowey, Plasma Electrolysis for Surface Engineering, Surface and Coatings Technology, (1999) A.L. Yerokin, A. Shatrov, V. Samsonov, P. Shahkov, A. Pilkington, A. Leyland, and A. Matthews, Oxide Ceramic Coatings on Aluminium Alloys Produced by a Pulsed Bipolar Plasma Electrolytic Oxidation Process, Surface and Coatings Technology, (2005). 5. X. Nie, A. Leyland, H.W. Song, A.L. Yerokin, S.J. Dowey, and A. Matthews, Thickness Effects on the Mechanical Properties of Micro-arc Discharge Oxide Coatings on Aluminum Alloys, Surface and Coatings Technology, (1999). 6. X. Nie, E.I. Meltis, J.C. Jiang, A. Leyland, A.L. Yerokin, and A. Matthews, Abrasive Waer/Corrosion Properties and TEM Analysis of Al 2 O 3 Coatings Fabricated using Plasma Electrolysis, Surface and Coatings Technology, (2002). w wz

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