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Microwave studies of thermally oxidized vacuum evaporated bismuth thin films on alumina

This article has been downloaded from IOPscience. Please scroll down to see the full text article. 2008 J. Phys.: Conf. Ser. 114 012040 (http://iopscience.iop.org/1742-6596/114/1/012040) View the table of contents for this issue, or go to the journal homepage for more

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International Symposium on Vacuum Science and Technology (IVS 2007) IOP Publishing Journal of Physics: Conference Series 114 (2008) 012040 doi:10.1088/1742-6596/114/1/012040

Microwave Studies of Thermally Oxidized Vacuum Evaporated Bismuth Thin Films on Alumina
S. Patil, D. Kulkarni, Vijaya Puri. Thick and Thin Film Device Lab, Department of Physics, Shivaji University, Kolhapur India. 416004. E mail: vrp_phy@unishivaji.ac.in
Abstract: The bismuth thin films of various thicknesses (100nm-550nm) were deposited on alumina substrate by vacuum evaporation technique. These films were thermally oxidized in air at three different temperatures (125C, 150C, and 175C). The films were characterized by XRD and SEM. X-ray diffraction studies shows dominant -Bi2O3 crystal structure. Surface morphology shows granular shaped particles of Bi2O3 on alumina substrate. Microwave properties were studied in the X band (8-12 GHz) using waveguide setup. The Bismuth oxide thin film showed higher microwave transmittance in the 10 to 10.8GHz range and lower reflectance. The dielectric constant and impedance at 12 GHz was measured using waveguide slotted section. The microwave dielectric constant of these Bi2O3 thin films varied from 17 to 46 at 12 GHz and was dependent on thickness and oxidation temperature

1. Introduction Bismuth oxide is a very useful dielectric material because it exhibits considerable resistivity, permittivity and thermal stability. However, it is used only in ceramic form [1]. Bismuth oxide exists in five main polymorphic forms such as , , , , and -Bi2O3. There is great interest in -Bi2O3 due to its high oxide ion mobility arising from numerous oxygen vacancies in the crystal structure [2]. It is well known that many oxides when heated in air at high temperature dissociates to their lower oxides. Similar dissociations and the formation of new species have also been observed during the vacuum deposition of several oxides by Goswami et al. [3]. Recently, Bismuth oxide has been investigated extensively due to its optical and electrical properties [2] as well as for microwave components such as phase shifter, tunable filters and in phased array antennas [4]. Bismuth oxide is characterized by the values of dielectric permittivity, impedance and losses in microwave region. There are various reports about electrical and optical properties of bismuth oxide thin film [5, 6] but very few reports on the microwave properties of these films [4]. In the present paper, crystalline bismuth oxide thin films have been obtained by thermal oxidation of vacuum evaporated bismuth thin films. Structural, surface morphological and microwave properties have been carried out. 2. Experimental Bismuth oxide thin films were prepared by thermal oxidation of bismuth thin films, deposited on alumina substrate by thermal evaporation under vacuum (resistive heating under a vacuum of 5 x 10-5 mbar). High purity element bismuth was used as a source material. Prior to vacuum deposition the alumina substrate were cleaned using chromic acid and soap solution, finally rinsed with distilled

c 2008 IOP Publishing Ltd

International Symposium on Vacuum Science and Technology (IVS 2007) IOP Publishing Journal of Physics: Conference Series 114 (2008) 012040 doi:10.1088/1742-6596/114/1/012040

water. The bismuth was deposited onto a cleaned alumina substrate by vacuum deposition technique. The films were thermally oxidized in air at different temperatures of 125C, 150C, and 175C. Thickness of bismuth oxide thin films was varied from 100nm-550nm which was measured by surface profiler. The structural analysis was performed by X-ray diffraction technique (Philips PW 3710). The surface morphology was studied by SEM (JSM-6360 JEOL, Japan). Microwave transmission and reflection were studied in the X-band (8-12 GHz) for different temperature with different thickness using waveguide reflectometer setup which is shown in fig.1. The dielectric constant and impedance of bismuth oxide thin film at microwave frequency was measured by Voltage Standing Wave Ratio (VSWR) slotted section method. The measurement of the perturbation in the position of the maxima and minima gives the permittivity and impedance of the medium. The real and imaginary parts of the permittivity and impedance can be calculated by using smith chart. Detector For Reflection

Oscillator

Isolator

Attenuator

3db directional Coupler

Bi2O3 Film

Detector for transmission

Fig. 1 Microwave reflectometer setup 3. Results and Discussion 3.1 X-ray Diffraction studies Figure 2 shows XRD pattern of bismuth oxide thin film. The X-ray diffraction patterns of Bi2O3 thin films obtained for different oxidation temperature indicate predominance of -Bi2O3 (222) mixed with - Bi2O3 phase. For all temperatures polycrystalline and multiphase structure of Bi2O3 was obtained. The low temperature oxidation below 2000 C results in -phase of Bi2O3.The substrate temperature has a great influence on the crystal structure of the as grown thin films.[2] 3.2 Surface Morphological studies Figure 3 shows SEM image of bismuth oxide thin film deposited on alumina using vacuum deposition technique. The SEM graph shows the granular structure. Similar granular structure was observed by Fan et al. [2]. The diameter of the grain is approximately 2 to 3 m. 3.3 Microwave Transmission and Reflection studies Figure 4 shows microwave transmission and reflection of bismuth oxide thin films oxidized in air at different temperature. From the figure, it is seen that, due to higher oxidation temperature, the transmittance increases by ~ 25% for all thicknesses of the bismuth oxide thin film. At lower oxidation temperature bismuth oxide of 100nm thickness shows lower transmittance than alumina. The film of 550nm thickness shows transmittance independent of oxidation temperature.

International Symposium on Vacuum Science and Technology (IVS 2007) IOP Publishing Journal of Physics: Conference Series 114 (2008) 012040 doi:10.1088/1742-6596/114/1/012040
1000 900 800 Intensity (A.U) 700 600 500 400 300 200 100 0 10 20 30 40 50 2 60 70 80 90 100

(-212,210)

(222)

(422) (210) (112)

(420)

Fig.2 XRD patterns of bismuth oxide thin film

Fig. 3 SEM image of bismuth oxide thin film.

International Symposium on Vacuum Science and Technology (IVS 2007) IOP Publishing Journal of Physics: Conference Series 114 (2008) 012040 doi:10.1088/1742-6596/114/1/012040
1
T ra n s m it t a n c e

1250C

1 0.8
R e f lle c t a n c e

0.8 0.6 0.4 0.2 0 8.2 9.2 10.2 Frequency GHz 11.2

0.6 0.4 0.2 0 8.2 9.2

1250C Alumina 210nm 550nm

100nm 344nm

Alumina

100nm 344nm

210nm 550nm

10.2 Frequency GHz

11.2

1 0.8
T ra n s m it t a n c e

1500C

1 0.8
R e f lc t a n c e

1500C

Alumina

100nm

0.6 0.4 0.2 0 8.2 9.2 10.2 Frequency GHz 11.2

210nm

344nm

0.6 0.4 0.2 0 8.2 9.2

550nm

Alumina 210nm

100nm

344nm

550nm

10.2 frequency GHz

11.2

1
T ra n s m it t a n c e

1750C
R e f le c t a n c e

1 0.8 0.6 0.4 0.2 11.2 0 8.2 9.2

1750C
Alumina
210nm 550nm 100nm 344nm

0.8 0.6 0.4 0.2 0 8.2 9.2 10.2 Frequency GHz

Alumina 210nm 550nm

100nm 344nm

10.2 Frequency GHz

11.2

Figure 4: Microwave Transmittance and Reflectance of Bi2O3 Thin Film. The reflectance does not show any thickness or oxidation temperature dependent effect. For higher oxidation temperature high band gap was observed [6] which might be responsible for high transmittance and low reflectance. 3.4 Dielectric constant measurement The graph of real ( ) and imaginary part ( ) of dielectric constant versus thickness is shown in fig. 5.

International Symposium on Vacuum Science and Technology (IVS 2007) IOP Publishing Journal of Physics: Conference Series 114 (2008) 012040 doi:10.1088/1742-6596/114/1/012040

50 45 40 35 30 25 20 15 10 5 0 0

Permittivity

0.200 0.160 0.120

T1 T3

T2

'

T1 T3
200 400 Thickness(nm)

T2
600

"

0.080 0.040 0.000 0 200 400 Thickness (nm) 600

(T1= 1250C, T2= 1500C and T3= 1750C) Fig. 5 Dielectric constant of Bismuth oxide thin film. Dielectric constant measurement was carried out by VSWR slotted section method. The real and imaginary part of dielectric constant was calculated using the following relation [7]

0 ' = 1 + 360 d

"=

Where, =Phase angle in degree

A0 ' 8.686d

0 = Guided wavelength
d = Thickness A = Difference in attenuation in dB
of bismuth oxide thin film at 12 GHz varies from 17 to 46. Low dielectric constant was observed for low oxidation temperature and for high oxidation temperature high dielectric constant was observed. Similar results were obtained by Valant at al. [4] for bulk material. Imaginary part of dielectric constant ( ) varies between 0.021 and 0.172. Imaginary part indicates the extent dielectric loss in the film. As temperature of oxidation increases the dielectric loss decreases and dielectric constant increases. Impedance of bismuth oxide thin films varied from 47.5 + j0.5 to 51 + j1 for all temperature. It was inductive in nature. 4. Conclusion Bismuth thin films deposited by vacuum evaporation followed by thermal oxidation are polycrystalline in nature and multiphase with predominance of -Bi2O3. These Bismuth oxide thin films have more transmitting nature and it was observed that transmittance increases with oxidation temperature. The reflectance in the X-band is very low. The permittivity is in the range suitable for miniaturized antenna fabrication. Acknowledgment One of the authors Vijaya Puri gratefully acknowledges the UGC India for Award of Research Scientist B. The authors also acknowledge UGC DRS-SAP II funding.

International Symposium on Vacuum Science and Technology (IVS 2007) IOP Publishing Journal of Physics: Conference Series 114 (2008) 012040 doi:10.1088/1742-6596/114/1/012040

References [1] Dharmadhikari V S, Badrinarayan S and Goswami A 1982 J. Ele.Spectro. and related phenomena. 25 181. [2] Fan H T, Pan S S, Teng X M, Ye C , Li G H and Zhang L D 2006 Thin solid films. 513 142. [3] Goswami A and Ojha S 1974 Thin solid films. 20 307. [4] Valant M and Suvorov D 2003 J. Amer. Chem. Soc. 86 939. [5] Leonite L, Caraman M, Alexe M and Harnagea C 2002 Surface Sci. 507-510 480. [6] Patil R B, Yadhav J B, Puri R K and Puri V 2007 J. of Phys. Chem. Solids. 68 665. [7] Kim J, Kim K and Noh S 1997 J. Ele. Eng. Inf. Sci. 2 72.