진공증착법을 이용한 철프탈로시아닌 박막의 합성과 그 특성

지종기; 이재구; 황동욱; 임윤묵; 양현수; 류해일; 박하선

Journal of the Korean Industrial and Engineering Chemistry, Vol.10, No.5, 644-651, August, 1999

Export Citation

진공증착법을 이용한 철프탈로시아닌 박막의 합성과 그 특성

Preparation and Characterization of Iron Phthalocyanine Thin Films by Vacuum Sublimation

지종기, 이재구, 황동욱, 임윤묵, 양현수, 류해일, 박하선

초록

본 연구에서는 진공 증착법을 이용하여 철프탈로시아닌(FePc) 박막을 실리콘 웨이퍼와 알루미나 기판 위에 합성하였으며, 박막의 증착 온도와 두께를 변화시켜 실험한 후 일부의 박막을 열처리하였다. 박막의 두께 변화에 따른 표면 구조 변화, 상전이와 전기 저항 감도 변화를 SEM, XRD, 그리고 전기저항의 측정으로 관찰하였다. 증착 온도가 370℃에서 350℃로 감소함에 따라 α상의 (200)면, (011)면, (211)면, 그리고 (114)면이 사라지며 β상의 (100)면의 피크가 나타났다. 전구물질의 양을 달리하며 고속 증착시켜 박막 두께를 조절한 결과, 두께 증가에 따라 결정 크기가 증가하고 또한 α상에서 β상으로의 상 전이가 일어남을 알 수 있었다. 열처리한 박막의 결정성을 측정한 결과 열처리 온도가 증가함에 따라 150℃으로부터 α상에서 β상으로의 상 전이가 일어나기 시작하여 350℃에서 완전히 β상으로 전이되었다. NO_x에 대한 철프탈로시아닌 박막의 온도에 따른 전기저항감도를 측정한 결과 박막의 두께가 얇을수록 더 좋고 안정된 전기 저항 감도를 보여주었다. 즉 박막의 표면구조가 조밀하게 성장할수록 전기 저항 감도가 더욱 좋아짐을 확인하였다.

In this experiment the Iron phthalocyanine (FePc) films on Si-wafer and alumina pallet were prepared using vacuum sublimation with conditions of changing reaction time, temperature, and deposition rate. Then, some samples were annealed following annealing. Techniques such as XRD, SEM, and resistance measurement method, were dedicated to characterize the changes of surface structure, phase transformation and electric resistance sensitivity in accordance with change of film thickness. In proportion to the decrease of deposition temperature from 370℃ to 350℃, intensities of (200), (011), (211) and (114) planes of α-phase were decreased and (100) plane of β-phase were appeared. The film thickness were controlled by regulating the volume of precursor material during rapid deposition. As a result, it was observed that crystalline particle size had been increased according to the increase of film thickness and α-phase transformed to β-phase. In consequence of measuring the crystallinity of films annealed between 150℃ and 350℃, α- to β-phase transformation was appeared to begin at 150℃ and completely transformed to β-phase at 350℃. Electric resistance sensitivity of FePc film to NO_x gas along temperature change of FePc films was observed to be more stable with the decrease of the film thickness.

Keywords:Iron phthalocyanine thin film;Gas sensor

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[1] Lever ABP, Adv. Inorg. Radiochem., 7, 27 (1965)

[2] Boucher LJ, Cooedination Chemistry of Macrocyclic Compounds, G.A. Melson, Plenum Press, New York, Chap. 7

[3] Kasuga K, Tsutsui M, Coord. Chem. Rev., 32, 67 (1980)

[4] Lever ABP, Adv. Inorg. Radiochem., 7, 92 (1965)

[5] Giraudeau A, Fan FF, Bard AJ, J. Am. Chem. Soc., 102, 5237 (1980)

[6] Shepard VR, Armstrong NR, J. Phys. Chem., 83, 1268 (1983)

[7] Greenand JM, Faulkner LR, J. Am. Chem. Soc., 105, 2950 (1983)

[8] Tang CN, Appl. Phys. Lett., 48, 83 (1986)

[9] Perrier G, Dao LH, J. Electrochem. Soc., 134, 1148 (1987)

[10] Gopel W, Hesse J, Zemel JN, Sensors, VCH (1995)

[11] Saji T, Phthalocyanines Properties and Applications, Chap. 4, 163 (1993)

[12] Hanack M, Lang M, Adv. Mater., 11, 6 (1994)

[13] Temofonte TA, Schoch KF, J. Appl. Phys., 3, 65 (1989)

[14] Speiser B, Leverenz A, Hanack M, Synth. Met., 41-43, 2979 (1991)

[15] Assour JM, J. Phys. Chem., 69, 2295 (1965)

[16] Iwatsu F, Kobayashi T, Uyeda N, J. Phys. Chem., 84, 3223 (1980)

[17] Shihub SI, Gould RD, Phys. Stat. Sol., 139, 129 (1993)

[18] Hassan AK, Gould RD, Phys. Stat. Sol., 132, 91 (1992)

[19] Sharp JH, Abkwitz M, J. Phys. Chem., 77, 477 (1973)

[20] Vimcett PS, Ppovic ZD, Mcintyre L, Thin Solid Films, 82, 357 (1981)

[21] 이형직, 윤상옥, 최두진, 박막프로세스의 기초, 반도출판사 (1992)

[22] O'Keefe MJ, Rigsbef JM, Material and Process for Surface and Interface Engineering, Kluber Academic Publishers (1994)

[23] 최동한, 청주대학교 산업과학연구소, 제12권, 171 (1994)

[24] Cranny AWJ, Atkinson JK, Barr PM, Mack D, Sens. Actuators B-Chem., 4, 169 (1991)

[25] Jan CD, Park HD, Cho DH, Lee DD, 센서학회지(별책), 3, 40 (1994)