PARAMETER EFFECTS FOR THE GROWTH OF THIN POROUS ANODIC ALUMINUM OXIDES

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1 / , The Electrochemical Society PARAMETER EFFECTS FOR THE GROWTH OF THIN POROUS ANODIC ALUMINUM OXIDES S. Yim a, C. Bonhôte b, J. Lille b, and T. Wu b a Dept. of Chem. and Mat. Engr., San Jose State University, San Jose, CA 95192, USA b Hitachi San Jose Research Center, San Jose, CA 95135, USA Production of porous anodic aluminum oxide (AAO) films from 100 nm evaporated aluminum (on silicon) was studied in order to determine the effects of voltage, temperature and acid concentration on the diameter, interpore distance, and long-range order of the holes. The largest change observed was found in the voltage experiments using concentrated sulfuric acid (H 2 SO 4 ), where the voltage was varied from 10-60V. Pores were produced even at low voltages with 30 nm interpore distance. This aforementioned arrangement has allowed for the smallest AAO pores to be found in any such experiment to date. Introduction One application of small, uniform holes is for use as magnetic storage devices, which could use smaller magnetic grains to accommodate the increase in data storage density. The lower grain size limit is governed by the superparamagnetic effect, where changes in the direction of magnetization in grains are generated by thermal fluctuations [1]. This effect limits scaling to smaller bits and restricts the achievable areal density. To avoid these issues, possible applications of processing arrays of dots (or pillars) have been implemented to create isolated grains (preventing this spontaneous magnetization reversal process). In addition, to achieve a 1Tb/in 2 areal density, the patterned magnetic media have requirements to create massive arrays of ~30 nm dots. However, one limit to implementing these requirements is fabrication of a durable and reusable mask with openings around 30 nm. One material that can be created from a thin film and creates a durable template with openings in this size regime is porous anodic aluminum oxide (AAO). These AAO structures form a porous pattern that can be used as a preformed template for many applications in magnetic, electronic, and optical devices [2-3]. The basic process to create AAO pores is by anodizing aluminum in acid solution. Several methods have been discussed to improve pore distribution, size, and repeatability [4-9]. Some have used silicon wafers with evaporated aluminum for optimization of optoelectronic device; others have used a separate e-beam lithography process to produce concave patterns in a pre-fabricated mold to initiate pore formation and produce uniform order [3, 7-9]. Herein, the production of anodic aluminum oxide (AAO) films from 100 nm evaporated aluminum on silicon was studied to determine the effects of hole diameter, interpore distance, and long-range order structure for future prospects in magnetic storage devices. The parameters of the anodization process itself, such as temperature, voltage, and electrolytic concentration, were utilized to investigate the anodizing conditions that have played a role in influencing the growth distance between pores and creating the ordered structure. 267

2 Experimental Set-up In this study, thin aluminum films were evaporated (placed as a monolayer) onto silicon wafers in an effort to preserve the silicon s smooth surface finish and ease of process integration. Temperature, time, electrolyte concentration, and voltage were considered the variables. H 2 SO 4 was used as the electrolyte, with varying concentrations of: 0.3M, 1.0M, and 6.0M; input voltage was varied, with voltages between 10V and 60V; and temperature was also varied, with values between 5 C and 37 C. The anodization of Al was carried out in 0.3M H 2 SO 4 for 15 minutes under a constant voltage of 20V at 22 C as a baseline (control) process. From this control process, only one variable was changed in order to determine their influence on the pore s size and long-range order. 100 nm of evaporated Al were deposited onto silicon wafers utilizing the evaporator tool. These wafers were evenly cut into pieces (1.5 cm x 1.5 cm). A schematic drawing of the fabrication process is shown in Figure 1. A t-cell was used as the electrochemical cell; sputtered gold was used as the counter electrode and evaporated aluminum was used as the anode (Figure 2). The anode and cathode, each having areas of 3.8 cm 2, were separated in the t-cell (10 cm). Al Si Si wafer with 1000Å Al evaporated Cathode T-cell Anode (a) Al 2 O 3 Anodized at 15 minutes Water cooled heatsink Ionmill 500Å of Al 2 O 3 Cathode Anode Etch in H 3 PO 4 for 3 DC power supply (b) Figure 1. Process steps (10). Figure 2. T-cell configuration (a) schematic view cross-section (b) photograph. After the aluminum film was anodized, about 50 nm of the resulting AAO was ion milled and subsequently etched in 5 wt% phosphoric acid (H 3 PO 4 ) for 3 minutes in order 268

3 to expose the pore pattern and to measure the pore density. A longer etching time such as 14 minutes using 5 wt% H 3 PO 4 was also conducted on both extreme cases of electrolyte concentration (0.3M and 6.0M H 2 SO 4 ) excluding the ion milling process to determine the relation between pore size and increases in acid concentration. The surface and topography of the pores were respectively analyzed (LEO 1500 Scanning Electron Microscopy (SEM) and the Nanoscope III Atomic Force Microscopy (AFM)). The average interpore distance and pore size from the obtained structure was basically determined by the annotation features in the SEM tool analysis. The roughness of the surface was determined using the AFM and a topographic view of the surface after anodizing Al was observed to demonstrate pore formation. Results and Discussion Initially, the pores were not visible under the SEM after anodizing the Al film. Hence, ion milling was utilized to remove the rough edges of the top layer and reveal the pores hidden beneath it (Figure 3). This process was more convenient than etching the alumina layer in order to view the bottom of the pores [8]. Before Anodization Anodized Ionmilled Figure 3. SEM image of the starting material that is smooth and after anodization created a rough surface from the top view Anodizing using concentrations of 6.0M H 2 SO 4 produced rounder pores as opposed to using 0.3M H 2 SO 4. SEM images of both electrolyte concentrations using longer 269

4 etching times (such as 14 minutes) with no prior ion milling are shown in Figure 4. An average pore size was found to be 27 ± 3.2 nm and interpore distance of 42 ± 8.1 nm for the specimen anodized at 6.0M H 2 SO 4. At this high acid concentration, the increased time of etching noticeably has wider pore diameters. Hence, there appears to be a correlation between electrolyte concentration and pore size; large increases in acid concentration appear to lead to slightly larger and denser pores in alumina. (a) (b) Figure 4. Anodized at 20v, 15min, 22 C, and etched 14 minutes in 5 wt% phosphoric acid for (a) 0.3M H 2 SO 4, and (b) 6.0M H 2 SO 4. In addition, the starting substrate of evaporated aluminum on silicon, exhibited a(n) Root Mean Square (RMS) roughness of approximately 0.3 nm. After the anodization process, the RMS roughness value was found to be 8.1 nm, a much rougher surface than the starting material (Figure 5). This topographic view clearly indicates pore formation after the anodization process. 270

5 Figure 5. Baseline process using 6.0M H 2 SO 4 and etching for 14 minutes in 5 wt% H 3 PO 4. With regard to all variances in voltage, the average pore size is found to be in the range of ± 2-3 nm. There did not appear to be a statistically significant change for pore size. However, the interpore distance deviates from this initial result. An increase of interpore distance from 30 ± 4.5 nm to 69 ± 11.8 nm was observed from voltages between 10V-30V. This increase appeared to conclude at 72 ± 12.6 nm for the experiment done at 40V. Additionally, at 60V, the interpore distance decreased to 58 ± 14.9 nm. 10V, etched 3 min (a) 271

6 (b) (c) (d) (e) Figure 6. Anodized 15 minutes under constant voltages of (a) 10V; (b) 15V; (c) 30V; (d) 40V; (e) 60V at 22 C with 0.3M H 2 SO 4, ionmilled and etched. Plots of interpore distance and pore diameter in relation to voltage are shown in Figure 7. Growth at 10V does indeed follow the linear trend. However, the uniformity of pore shape appears to decrease at this low voltage. 272

7 22 26 Avg Pore Size (nm) Temperature ( C) (a) Avg Pore Size (nm) Voltage (V) (b) Interpore Distance (nm) Interpore Distance (nm) Temperature ( C) (c) Voltage (V) (d) Figure 7. Plot of average pore diameter as a function of (a) temperature and (b) voltage; plot of interpore distance as a function of (c) temperature and (d) voltage with standard deviation. Previous AAO experiments were performed at low temperatures, where repeatable pores were achieved [11] using 0.3M oxalic acid solutions instead of sulfuric acid. In this work, no significant pore size and density change is observed with bath temperature variations. Hence, similar pores were produced at temperatures between 5ºC and 37ºC. This result is shown in Figure 7 with an average interpore distance of ± 8-10 nm and average pore size of ± nm. Ordering of the AAO film is known to be strongly dependent on the anodizing conditions involving the type of electrolytic solution, anodizing voltage, and temperature. In this study, the pore size and interpore distance results were dependent mostly on the concentration and voltage parameters. Higher concentrations improved the density of the pores; and at lower voltages, the distance between holes reduced. The anodization voltage affects the average pore density without significantly altering the pore size. (why???) In addition to the high dense pores, further reduction of the interpore distance is displayed, achieving the 30 nm distance between pores. Moreover, these variables did 273

8 not have an influence in establishing the long ordered pattern as observed in Figure 4 and Figure 6. Conclusion Appropriate anodizing conditions are essential for the fabrication of an ordered structure. Temperature did not have an effect on both pore size and interpore distance. Anodizing at higher concentrations produced rounder and denser pores. This was shown using 6.0M H 2 SO 4, a much higher concentration from the baseline process. Varying the voltage from 10-40V, show tremendous change in interpore distance. It is shown that even as low as 10V, the lowest voltage to date, AAO pores are formed with an average interpore distance of 30 ± 4.5 nm, the ideal size regime for fabricating a durable mask. In this work, the parameters varied did not reveal any long-range order structure. Nonetheless, it is observed that concentration and voltage both play a major role in optimizing the diameter and density of the pores. References 1. B. D. Terris and T. Thomson, J. Phys. D: Appl. Phys., 38, R199 (2005). 2. K. Yasui, T. Morikawa, K. Nishio, and H. Masuda, Jpn. J. Appl. Phys., 44, L469 (2005). 3. B. Das and S. P. McGinnis, Appl. Phys. A, 71, 681 (2000). 4. H. Masuda, and F. Hasegwa, J. Electrochem. Soc., 144, L127 (1997). 5. H. Masuda, M. Nagae, T. Morikawa, K. Nishio, Jpn. J. Appl. Phys., 45, L406 (2006). 6. C. C. Chen, J. H. Chien and C. G. Chao, Jpn. J. Appl. Phys., 44, 1529 (2005). 7. D. Crouse, Y. H. Lo, A. E. Miller, and M. Crouse, Appl. Phys. Lett., 76, 49 (2000). 8. H. Asoh, K. Nishio, M. Nakao, A. Yokoo, T. Tamamura, and H. Masuda, J. Vac. Sci. Technol. B, 19, 569 (2001). 9. H. Masuda, H. Yamada, M. Satoh, H. Asoh, M. Nakao, and T. Tamamura, Appl. Phys. Lett., 71, 2770 (1997). 10. H. Masuda, and M. Satoh, Jap. Journal of App. Phys., Part 2: Letters, 35, No. 1B, L126-L129 (1996). 11. M. A. Kashi and A. Ramazani, J. Phys. D: Appl. Phys., 38, 2396 (2005). 274

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