Effect of Time on Anodized Al2O3 Nanopore FESEM Images ... · installed on PC (hp: G42, 2012) used...

International Journal of Emerging Trends & Technology in Computer Science (IJETTCS) Web Site: www.ijettcs.org Email: [email protected]

Volume 4, Issue 3, May-June 2015 ISSN 2278-6856

Volume 4, Issue 3, May – June 2015 5

Abstract The scientific interest has been focused not only on the fabrication of various nano structured materials but also on their industrial and technological applications. Manufacturing of well-ordered nanostructures on the length scales less than dozens nm by conventional optical lithography is a great challenge. Automated microscopic image analysis provides an efficient tool for qualitative analysis in modern material science and biological studies. The main objective of the present study is to develop an automatic tool to determine the effect of time on nanopore structures formed via electrochemical anodization of high purity Al2O3 films in digital microscopic FE-SEM and EDX nano pore images. Geometric shape features are used to measure the variance of nano pore size depending on the chemical compounds, namely, concentration (%), time (min), temperature (oC) and voltage (V). The current methods rely on the subjective reading of profiles by a human expert based on the various manual staining methods. In this paper, an automated method is proposed for the effect of time on nanopore structures formed via electrochemical anodization of high purity Al2O3 films in digital microscopic nano pore images and extracting geometric shape features for the growth of Al2O3 films. It is observed that the regularity of nanopores arrangement can be significantly improved by increasing anodizing time at constant temperature and voltage, and after the anodizing process, at every interval of time there is a significant decrease in wall thickness from 58-26nm and increase in the nanopore diameter size about 31-86 nm. The experimental results are compared with the manual results obtained by the chemical expert and demonstrate the efficacy of the proposed method. Keywords: Anodizaion, computational chemistry, nanopore image analysis, image segmentation, nanopores

1. INTRODUCTION The nanopore sensor, made by drilling a tiny hole

through a thin film of aluminium oxide, could ultimately prove capable of performing DNA analysis with a single molecule, offering tremendous possibilities for personalized medicine and advanced diagnostics. Solid-state nanopore sensors have shown superior chemical, thermal and mechanical stability over their biological counterparts, and can be fabricated using conventional semiconductor processes. Nanostructures represent the

transition from atom to solid. It is essential to obtain particles or pores with uniform diameters and shapes and, for the purpose of particular applications, to arrange and embed them in a superstructure. The various applications of nano structures or pores are; size quantization effects, high number of surface atoms, and special surface states, special optical, electronic, magnetic and chemical properties. Some of the biomedical applications are decontamination and antibacterial agents, slow release drugs, filter in hemodialysis, enzyme mimetics and biosensors and adjuvant in anticancer therapy. In the past decade, the nano pore structures have been extensively investigated as the building blocks for various technological applications such as electronics, optoelectronics [1, 2] and sensors [3]. Recently, as an emerging field, NWs have been utilized for energy harvesting devices, for instance, to convert thermal [4], mechanical [5], and solar energy into electricity [6]. On the other hand, the NPL axial and radial junctions provide a three dimensional (3-D) geometric configuration for reduced surface optical reflection and enhanced absorption. The enhanced carrier collection and optical absorption can in principle enable more efficient PVs as compared to planar structures. However, the surface and the interface area enhancement also result in an increase in surface/interface recombination events. The ordering of the NPL arrays may be used as light trapping schemes analogous to random surface texturization or periodic grating couplers in thin films [7]. A porous anodization of aluminium oxide (AAO) template is fabricated for subsequent NPL growth at the bottom of each pore. The AAO template is etched back, exposing the pillars, and the semiconductor absorber layer is then deposited. This process enables the fabrication of an NPL cell on a low-cost Al metal foil. When anodized in an acidic environment with proper process conditions, aluminum oxidizes to form a pores alumina layer consisting of hexagonally packed arrays of nanopores [9], the pores are normal to the aluminum surface and extend from the surface to the alumina/aluminum interface where there is an oxide barrier layer with near hemispherical geometry. The shape and size of the pores are relatively uniform, with the pitch and diameter being directly proportional to the anodization voltage, and the height controlled by the

Effect of Time on Anodized Al2O3 Nanopore FESEM Images using Digital Image Processing

Techniques: A Study on Computational Chemistry

1.Parashuram Bannigidad , C. C. Vidyasagar2

1Department of Computer science, Rani Channamma University, Belgaum 591156, India

2Department of Chemistry, Rani Channamma University, Belgaum 591156, India



Volume 4, Issue 3, May – June 2015 Page 16

anodization time. Anodized aluminumoxide (AAO) has proven to be a highly versatile material system that has found important applications in photonics, energy devices including supercapacitors, filtration and purification and architectural and anticorrosive finishes [10-12]. Furthermore, given the uniformity of size-controlled nanopores, AAO has been widely utilized as a template for ordered synthesis of nanostructured materials, including metallic and semiconductor nanorods [13-14] nanowires [15-17] nanotubes [18] and nanoparticles [19] Importantly, aluminium anodization, in principle, is a highly scalable process as long as a stable voltage and current density are applied with a constant electrolyte temperature anodization time and composition. The protection or decoration of Al surfaces by anodization has been used commercially since 1923. Self-organized “nanopore” structures in anodic alumina films, called “alumite”, have attracted great attention due to their high pore density and their potential use for masking or information storage. When the pores are filled with metals or semiconductors in a subsequent alternating-current reductive electrolysis, these films can be fabricated into interesting magnetic recording, electronic, and electro optical devices [18-20]. By considering these constraints, here demonstrated continuous change in pore diameter, wall thickness and inter pore distance as anodization time increases. A synthetic diagram of nano pore development and sample Al2O3 film nano pore images are shown in the Fig. 1. When you submit your paper print it in two-column format, including figures and tables. In addition, designate one author as the “corresponding author”. This is the author to whom proofs of the paper will be sent. Proofs are sent to the corresponding author only.

Fig.1 Synthetic diagram of nano pore development and a

sample nano pore structure images

The microscopic image analysis of nanoparticles by edge detection using ant colony optimization has been investigated by Shwetabh Singh [21]. The estimation of nanopores size distributions by image analysis using deformable ellipse model was carried out by Fishker et. al. [22-23]. The Advanced morphological analysis of patterns of thin anodic porous alumina was investigated using geometrical features by Toccafondi et. al.[24]. Fast Fourier transform based arrangement analysis of poorly organized alumina nanopores formed via self-organized anodization in chromic acid has been investigated by Wojciech et. al.[25]. A Study of voltage, acid concentration, and temperature on nanopore structures has been proposed by Virk and Rajvinder [26]. Computer analysis of the AFM images of the nano pore system on

the SiO2/Si structure surface obtained by Zn Ion implantation is proposed by Sokolova et. al. [27]. The automated Gram-staining characterisation of bacterial cells using colour and cell wall properties by extracting geometric features has been carried out by Hiremath et. al. [28]. Automated identification and classification of white blood cells (leukocytes) in digital microscopic images using colour and geometric features of the bacterial cells by Hiremath et. al. [29]. In this paper, the anodic oxide formed on pure Al TLC film without any pre-anneal is investigated and the effects of anodizing time, concentration and temperature on the structural properties of the oxide films are examined in detail through digital image analysis. Automated microscopic image analysis provides an efficient tool for qualitative analysis in modern material science and biological studies. The main advantages of using digital image processing and pattern recognition techniques in conjunction with microscopy for quantitative studies of anodizing alumina; automatic image analysis reduces the amount of tedious work with microscopes needed to perform a more accurate quantitative analysis and these techniques provide an important quantitative tool to analyze the structures and spatial features of Al2O3 films.

2. MATERIALS AND METHODS TLC Silica Gel 60 F254 plates were procured from Merck. Orthophosphoric acid was procured from s-d fine Chem. Ltd. Mumbai. Double distilled water was used throughout the experiments. DC power supply source- measure unit was used as the power supply to measure voltage or current simultaneously (Aplab: L6405). MATLAB version 7.9.0.529 (R2009) software, which was installed on PC (hp: G42, 2012) used for image analysis. TLC plates were cut into proper size of 2x4 cm (0.5 mm thickness) of the following chemical composition (wt%) : Al 99. 79% (Aluminium), Cu 0.05% (Cupper), Mg 0.05% (Magnesium), Si 0.05% (Silicon), Mn 0.05% (Manganese) and Zn 0.01% (Zinc). Coated silica was removed by rubbing the surface using emery sheet grit 600. The Al plates were washed with distilled water, rinsed with ethanol, degreased with acetone in ultrasonic bath for 15 min. Finally the Al plates were purged by distilled water in ultrasonic bath for another 10 min. Before anodizing, the electrochemical polishing of samples was carried out in a 0.75 M NaOH solution. Al plates were immersed in NaOH solution for 4 min to remove alkaline impurities. The samples were rinsed with distilled water and acetone. Later onwards Al plates were rinsed thoroughly and kept undisturbed in distilled water for 10 min. Anodization was performed in a conventional cell using a platinum helical wire as a cathode. Al was used as the counter-electrode, and typically about 90% of the Al was immersed in the electrolyte while the exposed one was connected to the anode through a crocodile clips. The electrical contact was made at the edge of the electrodes. Pt electrode served as the cathode




electrode and the distance from the anode electrode was 3 cm. The samples were anodized in an acidic aqueous solution at different time interval at constant concentration and voltage. Ice cold water was used to maintain low temperatures using thermometer. During anodization the electrolyte was kept undisturbed, and the values of voltage, current, time and temperature were recorded. After the anodization process, the samples were rinsed thrice in deionized water and acetone and dried at 90 °C for 1 hour in an oven and was wrapped in aluminium foil. The variation in the time could be attributed to change in the pore size and wall thickness of the anodized Al2O3 thin films.

3.PROPOSED METHOD The main aim of the present study is to develop an automatic tool to determine the effect of time on nanopore structures formed via electrochemical anodization of high purity Al2O3 films in digital microscopic (Field Emission Scanning Electron Microscope (FE-SEM) and Energy Dispersive Spectroscopy (EDX)) nano pore images. Geometric shape features are used to identify the different characteristics of nano pore structures, namely, concentration (%), time (min), temperature (oC) and voltage (V). The current methods rely on the subjective reading of profiles by a human expert based on the various manual staining methods. In this paper, an automated method is proposed for the effect of time on nanopore structures formed via electrochemical anodization of high purity Al2O3 films in digital microscopic nano pore images and extracting geometric shape features ofAl2O3 films. The EDAX spectra of pure samples as prepared Al2O3 films is shown in the Fig. 2. The FE-SEM images of the top view of anodized Al2O3 films at different time intervals (A) 5 min, (B) 9 min, (C) 20 min and (D) 30 min (E) Change in concentration (4%) at constant temperature, voltage at 20min and (F) change in temperature (25oC) at constant concentration, time and voltage is shown in the Fig. 3.

Fig. 2. EDAX spectra pure samples prepared Al2O3 films.

Fig. 3 FE-SEM images of the top view of anodized Al2O3 films at different time intervals (A) 5 min, (B) 9 min, (C)

20 min and (D) 30 min (E) Change in concentration (4%) at constant temperature, voltage at 20min and (F) change in temperature (25oC) at constant concentration, time and

voltage. 3.1 Image Analysis The aim of the present study is to develop an automated method to determine the average growth size of the nanopore Al2O3 films, based on their geometric and statistical shape features. Many geometric and statistical features have been used by various authors in the literature [20-22, 30, 31]. It is observed that there are five geometric features, namely, length, width, area, box area ratio (BAR) and perimeter, which provide better results. Hence, we have used these five features, which are defined as given below: Length: The longer side of smallest circumscribed rectangle. Width: The shorter side of smallest circumscribed rectangle Area : The number of pixels belonging to the object provides a measure of the object size. Box Area Ratio (BAR): Length*Width/Area – The area of the smallest rectangle that can be drawn around an object, divided by the area of the object. Perimeter: The grain boundaries of the pores. The algorithm for segmentation and feature extraction of nanopore regions in FE-SEM images is given below: Algorithm: Segmentation and feature extraction of

(B)

(C) (D)

(E) (F)

(A)




nanopore regions. Step 1: Input nanopores image (anodized TLC plate) Step 2: Perform pre-processing method by using morphological operations, namely, erosion, reconstruction and dilation. Step3: Segment the input image using global thresholding (i.e. 0 for background and 1 for objects) to obtain nano pore regions. Step4: Remove border touching nano cells and then perform labeling the segmented image, where each segment is known to be a nano cell region. Step5: For each labeled segment, compute geometric shape features, namely, length, width, area, box area ratio (BAR) and perimeter. Step6: Repeat the Steps 1 to 5 for all nanopores of FE-SEM images of the top view of anodized Al2O3 films at different time intervals (A) 5, (B) 9, (C) 20 and (D) 30 min (E) change in concentration (4%) at constant temperature, voltage at 20 min and (F) change in temperature (25oC) at constant concentration, time and voltage. Step7: Calculate the statistical features, Mean (average), Minimum and Maximum values of nanopore regions on Step 6. Step8: Determine the average nano pore diameter and its thickness based on the geometric feature values computed on Step 7 and analyse the nano pore size on various data sets collected from different combination of concentration(%), time(min), temperature (oC) and voltage (V).

4. EXPERIMENTAL RESULTS AND DISCUSSIONS The implementation is done on a Pentium Core 2 Duo @ 2.83 GHz machine using MATLAB R2009b. Each input FE-SEM nanopore image (Fig. 4(i)) is converted into gray scale image (Fig. 4(ii)) and the morphological operations such as erosion, reconstruction and dilation are applied. The resulting image is thresholded to obtain segmented binary image (Fig. 4(iii)) and obtained the perimeter of the nanopore particles are shown in Fig. 4(iv). The segmented image is labelled and for each segmented region (known nano pores), the geometric and statistical features are computed. The Table 2 presents the minimum and maximum geometric feature values computed for the segmented nanopore regions at different combination of concentration (%)-time (min)-temperature (oC)-voltage (V). The nano pore images captured at different combination of concentration(%), time(min), temperature (oC) and voltage (V) are considered for the measurement of nano pore diameter are:

The determination of nano pore diameter size (area and perimeter) and thickness of the various data sets are extracted. In the above nano pore image data set from A-D, it is observed that, the extracted geometric feature values of length, width, area and perimeter are in increasing order, and its diameter is also increased, i.e. 32, 54, 58 and 81nm with constant concentration(%), temperature (oC) and voltage (V) and by varying time (min), i.e. 5, 9, 20 and 30, respectively. The wall thickness around the nano pore is also decreased as its size of the diameter (area) is increased, i.e. 58, 56, 48, 26 nm, respectively, which proves the effect of time (min) in Al2O3 films, is depicted in the Table 1. Whereas, in the E and F image data set; is observed that, the nano pore diameter size and wall thickness both were increased under constant in voltage (V) and time (min) and varying in concentration(%) and temperature (oC), i.e., 4,5; 20,25 and the values are 52;58, 58;81, pore size and thickness, respectively.

Fig. 6 shows with increasing anodizing time an increasing porosity and diameter at the surface of the (anodizing aluminium oxide) AAO was plotted. This inclining evolution became more pronounced for the increasing time, leading to an increase in porosity. The type of electrolyte, time and temperature of the electrolyte solution can affect the pore size and pore distribution of anodic alumina. The effect of anodizing time and image analyzed pore diameter with respect to area is shown in the Fig. 7 5. CONCLUSIONS Porous alumina films were successfully fabricated at ambient temperature. At different time intervals, Al2O3 films were found to produce nanopores that are well ordered; the FE-SEM results show the effect of time on nanopores Al2O3 films. As increase in anodizing time significantly the rate of chemical dissolution and pore formation proceed rapidly. The pore diameters were found to be dependent on the time. As increasing anodizing time results in increase in pore diameter, decrease in wall thickness of pure Al2O3 films. Domain structures form in circularly ordered anodic alumina films; the average domain sizes are a linear function of time. The domains form by pores moving and/or merging, but the mobility of ions within the barrier oxide and of Al atoms within the metal may explain why pores can rearrange dynamically and why linear domain growth with time is possible. In this paper, an automated method is proposed for the effect of time on nanopore structures formed via electrochemical anodization of high purity Al2O3 films in digital microscopic nano pore images and extracting geometric shape features for the growth of Al2O3 films. It is observed that the regularity of nanopores arrangement can be significantly improved by increasing anodizing time at constant temperature and voltage, and after the anodizing process, at every found to be dependent on the time. As increasing anodizing time results in increase in pore diameter,




decrease in wall thickness of pure Al2O3 films. Domain structures form in circularly ordered anodic alumina films; the average domain sizes are a linear function of time. The domains form by pores moving and/or merging, but the mobility of ions within the barrier oxide and of Al atoms within the metal may explain why pores can rearrange

interval of time there is a significant decrease in wall thickness from 58-26nm and increase in the nanopore diameter size about 31-86 nm. The experimental results are compared with the automated computational results obtained by chemical expert. There is still a huge space in the research of nano-porous materials, which will be considered in the future work. These results explore the collaborative research for applied science.

(i) (ii) (iii) (iv) Fig. 4 (i) Original FE-SEM images at different times A-D, (ii) Grayscale image , (iii) Segmented image on (ii), (iv)

Perimeter image on (iii)

Fig. 5 (i) Original FE-SEM images at different times E-F, (ii) grayscale image , (iii) segmented image on (ii), (iv)

perimeter image on (iii)

(i) (ii) (iii) (iv)




Table 1. Content of the pore diameter wall thickness and depth of the pores of all the samples anodized at constant concentration, temperature and voltage.

Table 2 Geometric feature values of nanopores of Al2O3 films at different times of concentration (%), time (min), temperature (oC) and voltage (V)

Samples

%

T

oC

V

Geometric feature values of nano pore of Nanopores Al2O3 film images Length (x-size)

Width (y-size)

Area Box area ratio Perimeter

Min Max Min Max Min Max Min Max Min Max

A 5 5 20 50 16 52 17 46 237 1033 1.2827 2.3368 67 194 B 5 9 20 50 17 63 18 69 338 1496 1.2500 2.6362 100 430 C 5 20 20 50 30 86 27 132 558 4153 1.2361 2.0952 140 541 D 5 30 20 50 36 117 40 118 889 6141 1.2276 1.7229 227 542 E 4 20 20 50 19 65 18 73 264 2731 1.2734 1.9012 82 461 F 5 20 25 50 23 65 16 52 296 1800 1.2247 1.8595 74 270

Table 3 Average nano pore size Al2O3 film images of Fig. 3 Samples

%

T

To

V

Geometric feature values of nano pore Al2O3 film images of Fig. 3 Average nano pore size

Length (x-size)

Width (y-size)

Box area ratio Area Perimeter

A 5 5 20 50 28.91 25.65 1.6385 450.57 114.1707 32 B 5 9 20 50 31.31 31.62 1.6957 590.01 143.2135 54 C 5 20 20 50 52 54.91 1.5087 1957.67 231.2353 58 D 5 30 20 50 71.29 68.41 1.4360 3467.04 301.9583 81

Geometric feature values of nano pore Al2O3 film images of Fig. 4 with change in concentration (%) and temperature (T) at constant time and voltage (V)

E 4 20 20 50 32.2469 35.086 1.4519 807.01 142.5062 55 F 5 20 25 50 37.7767 33.437 1.4118 907.13 144.4196 83

Fig. 6 Shows the effect of anodizing time on pore diameter and wall thickness of the Al2O3 films of Fig. 3

Fig. 7. Shows the effect of anodizing time and image analyzed pore diameter with respect to area.

Sl. No.

Concentration H3PO4 v/v%

Time min

Temperature o C

Voltage V

Wall Thickness

nm

Average Pore Sizes

nm A 5 5 20 50 58 32 B 5 9 20 50 56 54 C 5 20 20 50 48 58 D 5 30 20 50 26 81 E 4 20 20 50 52 55 F 5 20 25 50 58 83

5 10 15 20 25 30

25

30

35

40

45

50

55

60

65

70

75

80

85

Size

nm

Time

Wall thickness Nanopore diameter

0 500 1000 1500 2000 2500 3000 35000

10

20

30

40

50

60

70

80

Ano

dize

d Ti

me/

Imag

e A

naly

zed

Pore

Dia

met

er

Area of the pores nm

Image analyzed area with diameter by X length Image analyzed area with diameter by Y width Image analyzed area v/s Anodized time




ACKNOWLEDGMENTS The authors are grateful to the Indian Institute of Science (IISc), Bangalore for providing FE-SEM images and manual results of the nano pore images by visual inspection. This research work is financially supported by Vision Group on Science and Technology, Department of Information Technology, Biotechnology and Science and Technology, Govt. of Karnataka, Bangalore, India. REFERENCES [1] Zhong, Z. H., Qian, F., Wang, D. L., Lieber, C. M.

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AUTHOR

Dr. Parashuram Bannigidad, Assistant Professor, Department of Computer Science, Rani Channamma University, Belagavi, Karnataka, India. He has obtained M.Sc. (Information

Technology) Degree in 2003, M.Phil. (Computer Science) Degree in 2006 and Ph.D. Degree in 2012. He has started his teaching career since 2007. His research areas of interest are Image Processing, Biomedical and Pattern Recognition. He has published 30 research papers in peer reviewed International Journals and Proceedings of Conferences. He has been awarded ‘Young Scientist’ from Vision Group on Science and Technology, Dept. of Information Technology, Biotechnology and Dept. of Science & Technology, Government of Karnataka.

Dr. Vidyasagar C. C. Assistant Professor, Dept. of Chemistry, Rani Channamma University, Belgaum. He has obtained Post-Doctoral Felloship (PDF) from Indian Institute of Science

(IISc), Bangalore and Ph. D. in Physical Chemistry. He was awarded JRF and SRF from UGC, New Delhi. His research work has been identified in industry news provided by news edge in Ametek (U.S.A). He has published 15 articles in reputed international journals.

Effect of Time on Anodized Al2O3 Nanopore FESEM Images ... · installed on PC (hp: G42, 2012) used...

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