Effect of Enhanced Plasma Density on the Properties of Aluminium Doped Zinc Oxide Thin Films Produced by DC Magnetron Sputtering

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1 J. Mater. Sci. Technol., 2011, 27(5), Effect of Enhanced Plasma Density on the Properties of Aluminium Doped Zinc Oxide Thin Films Produced by DC Magnetron Sputtering Jun Gong, Xiaobo Zhang, Zhiliang Pei, Chao Sun and Lishi Wen Institute of Metal Research, Chinese Academy of Sciences, Shenyang , China [Manuscript received April 13, 2010, in revised form August 9, 2010] Aluminum doped zinc oxide (AZO) thin films were prepared by DC magnetron sputtering at low substrate temperature. A coaxial solenoid coil was placed near the magnetron target to enhance the plasma density (J i ). The enhanced plasma density improved significantly the bulk resistivity (ρ) and its homogeneity in spatial distribution of AZO films. X-ray diffraction (XRD) analysis revealed that the increased J i had influenced the crystallinity, stress relaxation and other material properties. The AZO films deposited in low plasma density (LPD) mode showed marked variation in ρ (ranging from to Ω cm), whereas those deposited in high plasma density (HPD) mode showed a better homogeneity of films resistivity (ranging from to Ω cm) at different substrate positions. The average visible transmittance in the wavelength range of nm was over 80%, irrespective of the deposition conditions. The atomic force microscopy (AFM) surface morphology showed that AZO films deposited in HPD mode were smoother than that in LPD mode. The high plasma density produced by the coaxial solenoid coil improved the electrical property, surface morphology and the homogeneity in spatial distribution of AZO films deposited at low substrate temperature. KEY WORDS: Sputtering; Electronic conductivity; Ion bombardmentplasma density 1. Introduction The increasing use of transparent electrodes in liquid crystal displays, solar cells, and various other opto-electronic devices has promoted the development of inexpensive transparent conducting oxides (TCOs) such as zinc oxide (ZnO) and aluminium (Al)-doped zinc oxide (AZO) films. As a result, these films have been investigated extensively as TCO materials [1,2]. Low temperature deposition technology, i.e., a substrate temperature (T s ) below 100 C, was desired for the escalating research on flexible substrates [3]. In general, it is difficult to deposit high quality thin films at low T s, but it is rather easy to produce high quality AZO films with a bulk resistivity (ρ) of 10 4 Ω cm Corresponding author. Prof., Ph.D.; Tel.: ; Fax: ; address: jgong@imr.ac.cn (J. Gong). at higher T s ( 200 C) irrespective of the deposition methods used [4]. Numerous techniques such as sputtering [5], evaporation [6], spray pyrolysis [7], sol-gel process [8] and plasma-enhanced chemical vapor deposition (PECVD) [9] were reported in literature to produce high quality AZO thin films at higher T s. Sputtering process was studied extensively for low T s thin films preparation owing to its high deposition rate, good adhesion, good uniformity combined with superior performances. The electrical properties of AZO thin films produced at low T s were inferior to those grown at elevated T s, and were strongly influenced by the deposition conditions. In addition, the films exhibited heterogeneity in ρ across the substrate surface, especially when deposited by DC magnetron sputtering [10 13]. In order to solve the problem of homogeneity, we have introduced an innovative idea of enhancing the

2 394 J. Gong et al.: J. Mater. Sci. Technol., 2011, 27(5), Fig. 2 Lateral distributions of J i and V f under different plasma modes Fig. 1 Schematic diagram of the DC magnetron sputtering system with an external solenoid coil near-substrate plasma characteristics in our earlier report [14]. In the present work, AZO thin films were deposited by DC magnetron sputtering with an external solenoid coil surrounding the magnetron source, which resulted in enhancing the plasma density (J i ) during the growth of AZO films. The effect of increased J i on the structural, electrical, optical and morphological properties was studied and the obtained results were interpreted in detail. 2. Experimental AZO thin films were sputtered from a Φ80 mm Zn (98 wt%): Al (2 wt%) alloy target and deposited on the optical glass substrates at a fixed deposition pressure of 0.8 Pa. The target-substrate distance was 70 mm. A coaxial solenoid coil around the magnetron source was utilized as illustrated in Fig. 1 to create an external magnetic field for varying the near-substrate J i. The coil was made of insulated Cu wire and excited by DC power supply to provide an additional external magnetic field. By changing the coil current strength and direction, the magnetic field lines were extended toward the substrate and an increase in the ion/neutral arrival flux was obtained. A Langmuir flat probe mounted on the substrate holder was used to determine the plasma characteristics within a radius of 4 mm. Two nearsubstrate plasma modes denoted as low plasma density (LPD) and high plasma density (HPD) were adopted in the present study. The LPD denotes the deposition without an external magnetic field (B ext ), and HPD refers the deposition with a B ext (0.01 T) surrounding the outer pole of the magnetron. High purity (99.99%) argon and oxygen (99.99%) were introduced through a mass flow controller after the vacuum chamber was pumped to below Pa. Prior to each deposition, the target was pre-sputtered in a pure Ar atmosphere for 5 min in order to remove the natural surface oxide layer on the target. The glass substrate was placed on the substrate holder with a resistive heater. The substrate temperature T s was measured and controlled by a thermocouple connecting to the substrate. The sputtering power was maintained at about 50 W with a typical voltage of V, while the T s was about 90 C. Structural properties were analyzed by using X- ray diffractometer (XRD) with CuKα radiation (λ = nm) in Bragg-Brentano geometry (θ/2θ coupled). The full width half maximum (FWHM) values were obtained with the XRD data. The film thickness (d) was determined by a profilometer (Surfcom 480A, Tokyo seimitsu) with accuracy of ± 20 nm and from a fitting of optical transmittance (FTG software). The obtained thickness values were in agreement with each other. The sheet resistance (R sh ) was measured with a four-point probe and the resistivity, ρ was calculated by the formula, ρ=r sh d. The optical transmittance of the films was measured with an UVvisible-NIR double-beam spectrophotometer (Hitachi U-2800) with an uncoated substrate in the reference path of the beam. Hence, the transmittance values quoted in the present work refer only that of films. The surface microstructure was analyzed by atomic force microscopy (AFM, SPA-400, Japan). 3. Results and Discussion In this work, saturation ion density was a measured value for describing the variation in the nearsubstrate plasma intensity under HPD mode, which was a crucial factor for the films growth and the homogeneity in spatial distribution. As shown in Fig. 2, the saturation plasma density (J i ) and substrate floating potential (V f ) were dependent on the substrate position (R). The values of R represent the position of the substrate: R=0 means that the substrates at the position opposite to the target center, and R=1, 2, 3, 4 represent the substrates positions at the circle of radius 1, 2, 3 and 4 cm, respectively. The J i under HPD mode was enhanced remarkably in comparison with that under LPD mode due to the introduction of the external solenoid coil. However, the distribution was heterogeneous across the substrate. A max-

3 J. Gong et al.: J. Mater. Sci. Technol., 2011, 27(5), Fig. 3 Lateral distribution of the bulk resistivity of AZO films under different modes imum J i of 1.2 ma cm 2 was got at R=0 and then decreased to a minimum of 0.1 ma cm 2, whereas the V f increased from about 23 to 7 V with increasing R from 0 to 4 cm. On the other hand, the J i under LPD mode showed almost negligible difference in plasma characteristics irrespective of the variation in R. The V f also varied within a narrow range, i.e., increasing from about 13 to 11 V. The resistivity ρ of AZO films varied with R, which reflected its spatial distribution, as shown in Fig. 3. It is perceptible that ρ of the AZO films prepared under LPD mode exhibited an obvious heterogeneous distribution. Particularly, more than one order of magnitude difference was observed between the AZO films grown in the center and in the border area. A maximum ρ of Ω cm was obtained at R=0 and then decreased gradually to a minimum of Ω cm with increasing R from 0 to 4. On the other hand, under HPD mode a significant improvement in homogeneity of ρ was observed. The ρ varied between and Ω cm. The obtained ρ values were almost similar and shown more uniformity in the spatial distribution, which may be attributed to the enhancement in the near-substrate J i, as shown in Fig. 2. The results substantiated that the increase in J i near-substrate could be beneficial to the AZO films growth and distribution of electrical properties. This situation can be considered as on a par with the deposition at elevated T s, because an additional energy is provided by the external solenoid coil. The XRD patterns of AZO films deposited under different modes are shown in Fig. 4. It can be observed that all the AZO films showed the preferred (002) crystallographic orientation and no other diffraction peaks were detected. For AZO films deposited under HPD mode, the intensity of the (002) orientation was much stronger than that under LPD mode, and decreased with increasing R from 0 to 2 and 4. The present situation indicated that the increase in J i improved the crystallinity of AZO films and decreased the ρ. Furthermore, the (002) peak was shifted towards lower 2θ values Fig. 4 X-ray diffraction patterns of AZO films deposited under different modes Fig. 5 Lateral distribution of 2θ and FWHM of (002) obtained from XRD data (standard 2θ=34.45 deg.). This was probably caused by the residual compressive stress, which elongated the c-axis in the AZO films. This phenomenon could be explained in terms of the atomic peening mechanism [15], where lattice distortions originated from the bombardment on the grown films by energetic species. The lateral distribution of 2θ ( 2θ: the absolute value of difference in the measured Bragg diffraction angle and the standard one) and FWHM of the (002) peak are compared in Fig. 5 as a function of R. Under LPD mode, the values of 2θ and FWHM get maximum at R=0 and then reduced gradually with R increasing 2 and 4. AZO films deposited at R=0 position were bombarded by stronger energy particles and produced larger residual compressive stress. However, under HPD mode, the values of 2θ was much lower than that under LPD mode and FWHM get a minimum values at R=0. Since the films stress was proportional to 2θ, and FWHM could represent the crystallinity of the films, obviously, increasing the J i could improve the crystallinity and relax stress of the films prepared at low T s. As a result, ρ was decreased pronouncedly in the trend as shown in Fig. 3. Despite the fact that the high energy ion bombardment would degrade the properties of the films, it was also beneficial to the film growth if the incident particle energy was lower than the penetration threshold of the deposited films.

4 396 J. Gong et al.: J. Mater. Sci. Technol., 2011, 27(5), Fig. 6 Transmittance spectra of AZO films deposited in LPD mode films was reduced. The optical transmittance spectra of uncoated glass substrate and AZO films prepared under LPD are shown in Fig. 6. The transmittance of the uncoated glass substrate was around 92%, while the average visible transmittance (AVT) of AZO films in the wavelength ranging nm is between 81.5% and 83.9%. The transmittance spectra of AZO films deposited under HPD were similar to that under LPD mode, which were also shown in Fig. 6. The AFM surface morphology of the AZO films deposited at R=0 is shown in Fig. 7. It could be observed that the films grown under HPD mode (Fig. 7(b)) showed a smooth surface in comparison with that deposited under LPD (Fig. 7(a)). The surface roughness of AZO films deposited under HPD mode was about 3 nm, while that of the films deposited under LPD mode was about 8 nm. The enhanced mobility under HPD mode was propitious to a smooth surface [17]. The smooth surface of AZO films could be advantageous to the applications in various optoelectronic devices. Overall, the increase in J i has enhanced the material properties. Hence, the idea of increasing the near-substrate J i is promising to promote the development of TCOs. 4. Conclusion Fig. 7 AFM surface morphology of the AZO films (a) LPD mode and (b) HPD mode Aluminium-doped zinc oxide (AZO) thin films were deposited by DC reactive magnetron sputtering using an external solenoid coil. The plasma density (J i ) near-substrate was enhanced by using the additional solenoid coil. The obtained results substantiate that the structural, electrical, morphological properties of the deposited AZO films were strongly influenced by the increased J i. For AZO films deposited under HPD mode, the bulk resistivity ρ was improved and more homogeneous (ranging between and Ω cm), while the crystallinity was improved and the residual compressive stress was relaxied. Further, the AZO films grown under HPD mode showed a smooth surface in comparison with that under LPD. In conclusion, using external solenoid coil was proven to be an effective way to improve the overall properties of AZO films deposited at low temperature. The reasonable explanation could be given as follows: at low temperature deposition, mass transport and defect mobility were low enough to freeze the lattice distortion induced by the energy bombardment. The lattice distortion resulted in a considerable stress and severely degraded electrical properties of the films [16]. For the deposition under HPD mode, additional energy caused an increase in mobility of the adatoms trapped in subsurface positions of the growing layer, which could improve the lattice perfection, then considerably released the internal stress, and ρ of the Acknowledgement We gratefully acknowledge the financial support of the National Natural Science Foundation of China under contract No REFERENCES [1 ] D.S. Ginley and C. Bright: MRS Bull., 2000, 25, 15. [2 ] B.G. Lewis and D. C. Paine: MRS Bull., 2000, 25, 22. [3 ] P.F. Carcia, R.S. Mclean, M.H. Reilly, Z.G. Li, L.J. Pillione and R.F. Messi: Appl. Phys. Lett., 2002, 81,

5 J. Gong et al.: J. Mater. Sci. Technol., 2011, 27(5), [4 ] K. Ellmer: J. Phys. D: Appl. Phys., 2000, 33, R17. [5 ] J.F. Chang and M.H. Hon: Thin Solid Films, 2001, 386, 79. [6 ] K.L. Chopra, S. Major and D.K. Pandya: Thin Solid Films, 1983, 102, 1. [7 ] P. Nunes, E. Fortunato, P. Tonello, F. Braz Fernandes, P. Vilarinho and R. Martins: Vacuum, 2002, 64, 281. [8 ] M.J. Alam and D.C. Cameron: J. Vac. Sci. Technol. A, 2001, 19, [9 ] A. Martín, J.P. Espinós, A. Justo, J.P. Holgado, F. Yubero and A.R. González-Elipe: Surf. Coat. Technol., 2002, , 289. [10] N.W. Schmidt, T.S. Totushek, W.A. Kimes, D.R. Callender and J.R. Doyle: J. Appl. Phys., 2003, 94, [11] D. Herrmann, M. Oertel and R. Menner: Surf. Coat. Technol., 2003, , 229. [12] T. Minami, T. Miyata, T. Yamamoto and H. Toda: J. Vac. Sci. Technol. A, 2000, 18, [13] T. Minami, T. Miyata, Y. Ohtani and Y. Mochizuki: Jpn. J. Appl. Phys., 2006, 45, L409. [14] X.B. Zhang, Z.L. Pei, J. Gong and C. Sun: J. Appl. Phys., 2007, 101, [15] H. Windischmann: Crit. Rev. Solid State Mat. Sci., 1992, 17, 547. [16] K. Tominaga, K. Kuroda and O. Tada: Jpn. J. Appl. Phys. Part 1, 1988, 27, [17] B.W. Karr, D.G. Cahill, I. Petrov and J.E. Greene: Phys. Rev. B, 2000, 61,

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