International Journal of Computer Engineering and Applications, Volume XII, Issue I, Jan. 18, ISSN

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1 International Journal of Computer Engineering and Applications, Volume XII, Issue I, Jan. 18, ISSN EFFECT OF CONCENTRATION AND TEMPERATURE ON ALUMINIUM OXIDE NANOPORE FESEM IMAGES Parashuram Bannigidad 1, Jalaja Udoshi 1 and C. C. Vidyasagar 2 1 Dept. of Computer Science, Rani Channamma University, Belgaum , Karnataka, India 2 Dept. of Chemistry, Rani Channamma University, Belgaum , Karnataka, India ABSTRACT: The paper intends to provide an efficient automated tool for quantitative analysis of the nano membrane using FESEM images. The honeycomb structure formed due to oxidization on aluminium metal during the anodization is the membrane of self-ordered array of nanopores with prominent properties like area, pore size, interpore distance, wall thickness and porosity. These membranes with customized features are used as templates for various industrial applications. The geometrical features depend on the anodization variables namely, concentration (%), time (min), temperature ( o C) and voltage (V). It is observed that, the wall thickness and size of the nanopore has increased, when the concentration (%) and temperature ( o C) has been increased from 4% to 5% and 20 0 C to 25 0 C respectively at constant time (20 mins) and voltage (50V). The experimental investigation profile depicts that, the change in acidic concentration and temperature shows significant increase in wall thickness, nanopore size and porosity from 52 to 55nm, 55 to 83nm and to 1.862nm respectively. The proposed results are juxtaposed with the manual results provided by the chemists and demonstrate the efficiency of the proposed method. Keywords: Aluminium nanopore, Computational chemistry, Nanopore image analysis, Image segmentation, Porosity, FESEM, Nanomaterial [1] INTRODUCTION Nano particles fabrication has retrieved considerable attention in the last few decades because of their enormous applications in making of electronic and optoelectronic materials [1]. Parashuram Bannigidad, Jalaja Udoshi and C. C. Vidyasagar 222

2 EFFECT OF CONCENTRATION AND TEMPERATURE ON ALUMINIUM OXIDE NANOPORE FESEM IMAGES Nanopores itched on anodic alumina films have been of great use in both scientific and technological fields. They are been acting as building materials for most of the nanotechnological applications due to their unique properties as compared to their bulk counterparts. Synthesis of nanopores using aluminium oxide is most uncomplicated and economical approach as compared to other metal oxides [2]. Some of the recent approach of nanoporous anodic aluminium oxide (AAO) is their utilization as membrane in separation of gas, delivery of drugs and bone fixation [3]. The other potential application of the membrane is in hemodialysis, where the size of the nanopore plays a vital role in filtering the small and medium molecular weight solutes like urea or creatinine and vancomycin or inulin respectively from large molecular weight solutes like albumin [4]. The challenge lies in obtaining tailored made membrane with uniform pore size, regular pore distribution, high porosity along with good chemical resistance and temperature stability because the nanopore characteristics such as diameter of the pore, interpore distance and thickness of the membrane depends on the anodization variables like applied voltage (V), anodization time (min), electrolyte concentration (%) and temperature ( o C) [5]. It has been depicted that under any anodization conditions the self-ordering of nanopores has a porosity of 10% [10-11]. The synthetic diagram of nanopore synthesis is depicted in the Figure: 1. Figure: 1. Synthetic diagram of nanopore synthesis Many researchers have contributed their study towards the fabrication of customized AAO sheet membranes and presented their interpretation about relation between processing parameters and membrane morphology. Array of nanohole on Al 2O 3, depicting the honeycomb structures was emphasized by Masuda and Fukuda [6]. Masuda and Satoh presented a study on array of nanodot used as evaporation mask [7]. The effect of voltage on anodization of aluminum was contributed by Araoyinbo et. al.[2]. Alaba O. investigated on the effect of room temperature in the itching of nanopores [8]. Anodization time effect on Al 2O 3 nanopore was investigated by P Bannigidad et. al.[9]. In this study, pure aluminium TLC films without subjecting to any pre-anneal is utilized to form an anodic oxide. This anodic oxide is then scrutinized to find the effect of anodizing Parashuram Bannigidad, Jalaja Udoshi and C. C. Vidyasagar 223

3 International Journal of Computer Engineering and Applications, Volume XII, Issue I, Jan. 18, ISSN parameters (time, voltage, concentration and temperature) on the geometrical properties of the oxide films using digital image analysis. The quantitative analysis of the anodized alumina using non-automated mechanism is found to be more cumbersome and tedious. The novelty in this paper is, an automated tool using digital image processing and pattern recognition techniques in association with field emission scanning electron microscope is provided for an efficient analysis of Al 2O 3 images. [2] MATERIALS AND METHODS The materials used for the synthesis of the Al 2O 3 nanopores are TLC Silica Gel 60 F254 plates cut into 2x4 cm (0.5 mm thickness), Orthophosphoric acid, Double distilled water and Aplab: L6405 (DC power supply source- measure unit). Pt electrode was utilized as cathode electrode. The automated tool used for image analysis was developed using MATLAB R2010 software installed on Intel(R) Core(TM) Duo 220GHz with 2 GB RAM. [3] PROPOSED METHOD The objective of the present study is to develop an automated tool to determine the effect of change in concentration (4% and 5%) and temperature (20 o C and 25 o C) at constant time (20 mins) and voltage (50V) on nanopore structures formed through electrochemical anodization of highly pure Al 2O 3 films in digital microscopic (FESEM)) nanopore images. The current methods employed are subjective reading of the structures by an expert, based on the various manual staining techniques. The proposed method emphasize on the effect of variable anodizing properties on surface chemistry of an anodic oxide layer. Oxidation of aluminium through electro-chemical process produce highly ordered array of cylindrical shaped pores and their characteristics like pore size, pore diameter, porosity and other geometrical features depend on the anodization parameters. The top view of anodized Al 2O 3 FESEM images at 4% and 5% concentration, 20 o C and 25 o C temperature, 20 mins time and 50V voltage are shown in the Figure:2. [A] [B] Figure: 2. Top view of anodized Al2O3 FESEM Images [A] Concentration (4%), temperature (20 0 C), time (20min) and voltage (50V), [B] Concentration (5%), temperature (25 0 C), time (20min) and voltage (50V) The five prominent geometrical features of the nanopore are defined below: Parashuram Bannigidad, Jalaja Udoshi and C. C. Vidyasagar 224

4 EFFECT OF CONCENTRATION AND TEMPERATURE ON ALUMINIUM OXIDE NANOPORE FESEM IMAGES Figure: 3. Flow diagram of proposed method 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. Nanopore diameter (D p) : The average ratio of major axis and minor axis Interpore Distance (D i) : The average ratio of neighboring nanopore centroid distance. Porosity (α) : The porosity is calculated from below equation: Dp 2 3 Di 2 The flow diagram of the proposed method is depicted in the below Figure: 3.: The algorithm for segmentation and feature extraction of nanopore regions of FESEM images is given below: Algorithm: Steps for segmentation and feature extraction of nanopore regions. 1. Input nanopore FESEM image. 2. Perform pre-processing operations on input image (Image enhancement and morphological operations). 3. Perform segmentation by applying global thresholding on pre-processed image to obtain binarized image (0 representing background and 1 representing objects) and labeled the segments. Parashuram Bannigidad, Jalaja Udoshi and C. C. Vidyasagar 225

5 International Journal of Computer Engineering and Applications, Volume XII, Issue I, Jan. 18, ISSN Compute geometric shape features; area, pore diameter, interpore distance and porosity for each labeled objects on step Calculate mean and standard deviation on step Repeat the steps 1-5 for all segments. 7. Analysis and interpretation of the results. [4] EXPERIMENTAL RESULTS AND DISCUSSION Al 2O 3 FESEM images with 230 nano pores are used in the experiment. The experimentation of the proposed method is carried out on Intel(R) Core(TM) Duo 220GHz with 2 GB RAM using MATLAB R2010 software. Every Al 2O 3 FESEM image used in the experiment is captured at varied concentration (4% and 5%) and temperature (20 o C and 25 o C) and at constant time (20 mins) and voltage (50V) (Figure: 4. (i)). The input images are converted into grayscale image (Figure: 4. (ii)) and morphological operations such as erosion, reconstructions and dilation are applied. Then, segmentation is performed by applying global thresholding (Figure: 4(iii)) to separates background and foreground (nanopores). Geometric shape features, i.e., area, pore diameter, interpore distance and porosity was computed for each labeled segment. Finally, the results are interpreted and compared with manual results obtained by the chemical experts and these results are shown in the Table 2. The details of chemical compositions used for preparation of Al 2O 3 nanopores during synthesis are given in the Table 1. A B Figure: 4. (i) Original FESEM images at different concentration and temperature and constant time and velocity (ii) Grayscale images, (iii) Segmented images (i) (ii) (iii) Parashuram Bannigidad, Jalaja Udoshi and C. C. Vidyasagar 226

6 EFFECT OF CONCENTRATION AND TEMPERATURE ON ALUMINIUM OXIDE NANOPORE FESEM IMAGES Table: 1. The details of chemical compositions for syntheses of sample Al2O3 nanopore images Sample Images Concentration (%) Time (min) Temperature ( o C) Velocity (V) A B Table: 2. Geometric feature values of sample Al2O3 nanopore images of Figure.2 Sample Images Wall Thickness (nm) Pore Size (nm) Porosity Manual Proposed Manual Proposed Manual Proposed A B Figure: 5. Manual versus proposed nanopore wall thickness of Al2O3 image Parashuram Bannigidad, Jalaja Udoshi and C. C. Vidyasagar 227

7 International Journal of Computer Engineering and Applications, Volume XII, Issue I, Jan. 18, ISSN Figure: 6. Manual versus proposed nanopore size of Al2O3 image Figure: 7. The effect of anodizing parameters (Concentration-Time-Temperature-Velocity: (A) (B) ) on wall thickness, nanopore size and porosity of the Al2O3 films It is observed that, the wall thickness and size of the nanopore has increased, when the concentration (%) and temperature ( o C) has been increased from 4% to 5% and 20 0 C to 25 0 C respectively at constant time (20mins) and voltage (50V).The experimental investigation profile depicts that, the change in acidic concentration and temperature shows significant increase in wall thickness, nanopore size and porosity from 52 to 55nm, 55 to 83nm and to 1.862nm respectively. The manual results obtained by chemical experts and computed results of wall thickness is depicted in the Figure:5. Similarly, the results of nanopore size are shown in the Figure:6. Finally, the effect of anodizing parameters (Concentration-Time-Temperature-Velocity: (A) (B) ) on wall thickness, pore diameter and porosity of the Al 2O 3 films are shown in the Figure:7. [5] CONCLUSION Research on nanotechnology has emphasized on fabrication of customized nanopore structure. Anodized aluminium is widely accepted by the industry because of its inherent properties and ability to cater the structural needs of varied industrial applications. In this study, pure aluminium TLC films without subjecting to any pre-anneal is utilized to form an anodic oxide. This anodic oxide is then scrutinized to find the effect of anodizing parameters (time, voltage, concentration Parashuram Bannigidad, Jalaja Udoshi and C. C. Vidyasagar 228

8 EFFECT OF CONCENTRATION AND TEMPERATURE ON ALUMINIUM OXIDE NANOPORE FESEM IMAGES and temperature) on the geometrical properties of the oxide films using digital image analysis. An automated tool is proposed to analyze the FESEM images of Al 2O 3 nanopore images with varied anodization parameters. It is observed that, the wall thickness and size of the nanopore has increased, when the concentration (%) and temperature ( o C) has been increased from 4% to 5% and 20 0 C to 25 0 C respectively at constant time (20mins) and voltage (50V). The experimental investigation profile depicts that, the change in acidic concentration and temperature shows significant increase in wall thickness, nanopore size and porosity from 52 to 55nm, 55 to 83nm and to 1.862nm respectively. The proposed results are juxtaposed with the manual results provided by the chemists and demonstrate the efficiency of the proposed method. ACKNOWLEDGEMENT The authors are grateful to Rani Channamma University, Belagavi, Karnataka, India, for sanctioning the minor research project. The authors also extent their thanks to Department of Chemistry, Rani Channamma University, Belagavi for providing the Al 2O 3 FESEM nanopore images. REFERENCES [1] Jia L, Shu L, Haihui Z, Congjia X, Zhongyuan H, Chaopeng F, Yafei K, Preparation of Self- Ordered Nanoporous Anodic Aluminum Oxide Membranes by Combination of Hard Anodization and Mild Anodization, Thin Solid Films, vol. 552, 75 81, (2014). [2] A.O. Araoyinbo, A.F.M. Noor, S. Sreekantan, A. Aziz, Voltage Effect on Electrochemical Anodization of Aluminum at Ambient Temperature, IJMME, vol. 5, No. 1, 53-58, (2010). [3] A. Belwalkar, E. Grasing, W. Van Geertruyden, Z. Huang, W.Z. Misiolek, Effect of processing parameters on pore structure and thickness of anodic aluminum oxide (AAO) tubular membranes, Journal of Membrane Science, vol. 319, , (2008). [4] W. Chen, J. Yuan, X. Xia, Characterization and manipulation of the electroosmotic flow in porous anodic alumina membranes, Anal. Chem., vol. 77, (2005). [5] A. Belwalkar, Experimental study of nanoporous ceramic tubes for potential application in hemodialysis, Mechanical Engineering, M.S. Thesis, Widener University, Chester, 127, (2006). [6] H. Masuda, K. Fukuda, Ordered metal nanohole arrays made by a two-step replication of honeycomb structures of anodic alumina, Science, vol. 268, issue 5216, , (1995). [7] H. Masuda, M. Satoh, Fabrication of gold nanodot array using anodic porous alumina as an evaporation mask, Jpn. J. Appl. Phys., L126, 35, (1996). [8] Alaba O., Azmi Rahmat, Mohd Nazree Derman, Khairel Rafezi Ahmad, Room temperature anodization of aluminum and the effect of the electrochemical cell in the formation of porous alumina films from acid and alkaline electrolytes Adv. Mat. Lett. vol. 3(4), , (2012). [9] Parashuram Bannigidad, C. C. Vidyasagar, Effect of Time on Anodized Al 2O 3 Nanopore FESEM Images using Digital Image Processing Techniques: A Study on Computational Chemistry IJETTCS, ISSN , 4, 3, 15-22, (2015). [10] C. C. Vidyasagar, Parashuram Bannigidad, H. B. Muralidhara, Influence of anodizing time on porosity of nanopore structures grown on flexible TLC aluminium films and analysis of images using MATLAB software, Adv. Mater. Lett. VBRI Press, 7(1), 71-77, (2016). [11] K. Nielsch, J. Choi, K. Schwirn, R. Wehrspohn, U. Gosele, Self ordering regimes of porous alumina: 10% porosity rule, Nano Lett., vol. 2 (7), , (2002). Parashuram Bannigidad, Jalaja Udoshi and C. C. Vidyasagar 229

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