Department of Chemistry-BK 21, SungKyunKwan Univ.

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Department of Chemistry-BK 21, SungKyunKwan Univ. Selective deposition of iron oxide films on Self-assembled organic monolayers using microcontact printing. 송여진, 이종현, 이석우, 정덕영* Department of Chemistry-BK 21, SungKyunKwan Univ.

Iron oxides Introduction In situ patterning of crystalline iron oxide thin layers has been achieved via microcontact printing (CP) and selective deposition. The CP was used to pattern surface of self-assembled organic monolayers(OTS, n-octadecyltrichlorosiloxane) on Si(100) substrate using an elastomeric stamp (PDMS). The aqueous solutions of ferric nitrate(or ferric chloride) were used for selective depositions which could be controlled by the various process parameters, e.g., solution concentration, temperature, and deposition time. Scanning electron microscopy (SEM), X-ray diffration method and optical microscopy were used to characterize the patterned thin films and their crystal structures. SKKU Inoganic Material Lab.

- Fe2O3 (maghemite) : metastable ferrimagnetic form Iron oxides Preparation of Iron oxides <<Magnetic oxides >> - Fe2O3 (hematite) : thermodynamically stable antiferromagnetic for precursor of  - Fe2O3 , Fe3O4 Fe3O4 (magnetite) magnetic recording materials - Fe2O3 (maghemite) : metastable ferrimagnetic form : The properties of the films are largely dependent on film preparation methods and conditions. (Terminal functionality of SAMs can alter the surface’s reactivity and physical characteristics) SKKU Inoganic Material Lab.

Experimental Chemical solution deposition (CSD)* Iron oxides Experimental wafer dipping Fe(NO3)3 (+ urea) or FeCl3 aqueous soln. at 75C Silicon oil Magnetic stirrer Chemical solution deposition (CSD)* Sonication (10-20 mins) Reduction under H2 (350~ 850°C) SKKU Inoganic Material Lab.

Outline Fe(NO3)3 soln. FeCl3 soln. CSD* CSD* -FeOOH (akaganetite) Iron oxides Outline PDMS stamp Ink solution (OTS in Hexane) Fe(NO3)3 soln. FeCl3 soln. HO-Terminated Si wafer Surface CP CSD* CSD* SAMs Si wafer Selective Deposition -FeOOH (akaganetite) -Fe2O3 (hematite) Iron(lll) oxides Annealing Si wafer 850C for 5hr Under H2 Annealing 850C for 5hr Under H2 Annealing (under H2) Iron metal Fe3O4 (magnetite) Fe (iron metal) Fe3O4 (magnetite) Fe (iron metal) Si wafer SKKU Inoganic Material Lab.

SEM images 1. Fe(NO3)3 soln. SiO2 SiO2 SiO2 Hematite/OTS Iron oxides SEM images 1. Fe(NO3)3 soln. Hematite/OTS Hematite(- Fe2O3)/OTS (- Fe2O3) SiO2 SiO2 SiO2 200m 100m 20m 20m SKKU Inoganic Material Lab.

Calcining Fe(NO3)3 soln. -Fe2O3/OTS SiO2 (Fe + Fe3O4)/OTS Iron oxides Fe(NO3)3 soln. (Fe + Fe3O4)/OTS Calcining SiO2 850C for 5hrs under H2 (about 2~3hrs) 100m (Fe + Fe3O4)/OTS SiO2 Thickness ~ 150nm -Fe2O3/OTS 200nm 1m SKKU Inoganic Material Lab.

2. FeCl3 soln. Akaganeite/OTS (-FeOOH) SiO2 500m 100m 1m Iron oxides 2. FeCl3 soln. 500m Akaganeite/OTS (-FeOOH) SiO2 100m 1m SKKU Inoganic Material Lab.

Calcining FeCl3 soln. SiO2 (Magnetite + Iron)/OTS 850C for 5hrs Iron oxides FeCl3 soln. Calcining 850C for 5hrs under H2 (about 2~3hrs) 100m SiO2 (Magnetite + Iron)/OTS (Fe3O4 +Fe) 1m 1m SKKU Inoganic Material Lab.

XRD - Fe2O3(Hematite) -FeOOH (Akaganeite) Iron oxides XRD - Fe2O3(Hematite) -FeOOH (Akaganeite) from ferric nitrate from ferric chloride Intensity Intensity 2 2 Annealing 850oC, 5hr (under H2) (Magnetite) + Fe (Iron) Fe3O4 Intensity 2 SKKU Inoganic Material Lab.

AES (Auger Electron Spectroscopy) analysis Iron oxides AES (Auger Electron Spectroscopy) analysis A Particle(-FeOOH)/OTS B A B SiO2 Counts (E dN(E)/dE) A B Kinetic energy(eV) SKKU Inoganic Material Lab.

Conclusion Acknowlegement Iron oxides Conclusion Crystalline films of - Fe2O3 (or -FeOOH) were deposited onto SAMs (OTS) from iron nitrate (or iron chloride) aqueous solution at 75oC for 2hrs. Selective deposition was realized precipitates of iron oxide phases from aqueous solutions at temperature below 100℃. Subsequently, Fe3O4 and Fe were obtained by annealing under H2 at 850C for 5hrs. Acknowlegement We acknowledge support by the Korean Science and Engineering Foundation through Grant R02-2000-00065. SKKU Inoganic Material Lab.