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Advanced Science Letters Vol. 23, 6582–6584, 2017
Growth of TiO
2Thin Films by High Energy Milling Assisted Pulsed Laser Deposition Method
Agus Subagio1∗, Wahyu Setia Budi1, Iis Nurhasanah1, Sudarji2, and Indras Marhendrajaya1
1Physics Department, Faculty of Sciences and Mathematics, Diponegoro University, Indonesia
2Alumnus of Physics Department, Faculty of Sciences and Mathematics, Diponegoro University, Indonesia
TiO2thin film can be deposited on the silicon substrate using pulse laser deposition method. To prove homo- geneity of grain size on surface, this study uses milling treatment for TiO2powder before it is deposited. Milling treatment was conducted on samples of commercial TiO2powder with high energy milling method. The variation of milling time was 0, 1, 3 and 6 hours. Furthermore, the samples were shaped as disc with diameter of 1 cm and used as a target source in growth of thin film. Variations in time for the milling treatment of the TiO2powder has no effect on the phase change, but rather on the homogeneity of grain size on a thin layer of TiO2. In this study, the optimum milling time to produce a homogeneous grain size of a thin layer of TiO2for 3 hours.
Keywords: TiO2, HEM-PLD, Milling Treatment, Thin Film.
1. INTRODUCTION
The development of science and technology of thin layers, espe- cially for electronic device applications was increasingly with a variety of methods. On the industrial scale, the method of chem- ical vapor deposition (CVD) has been established is used for thin film deposition. However, deposition of thin film with CVD methods required expensive support systems by utilizing precur- sors that are toxic and flammable. Some methods are more secure and cost, among others, pulsed laser deposition (PLD), sputter- ing and sol–gel. Especially for PLD and sputtering system can produce a thin layer with good quality. As for the sol–gel method usually produces relatively less homogeneous layer if deposited by spin coating system.
Titanium dioxide (TiO2is one of the electronic materials that have been widely used for various applications. There are three types of the crystal structure of TiO2, the rutile, anatase and brookite.1 Brookite structure is thermodynamically highly unsta- ble when compared with the structure of rutile and anatase.12 Rutile structure has better stability because it contains atoms which are solid.3 TiO2 thin film deposition using PLD method is relatively easier than the CVD method. Utilization of the high power laser pulses have been used to deposit a thin layer of TiO2 on silicon substrate.4 There are some drawbacks about PLD nat- urally. One of the major problems is the splashing or the depo- sition of particulates on the film. Two main causes for particle formation during laser evaporation are the breakaway of sur- face defects under thermal shock and splashing of liquid material
∗Author to whom correspondence should be addressed.
due to superheating of subsurface layers. Some methods have been developed to reduce splashing. One is using a mechanical particle filter that consists of a velocity selector that acts as a high-velocity pass filter to remove slow moving particulates. The second is using targets of high density and smooth surface. The third is using relatively low energy density or low deposition rate.
Using high density and smooth surface of target can be pre- pared with milling treatment of target powder. Milling treatment prior to deposition of the target sample is usually required to obtain homogeneity in the particle size of the powder targets.
This paper reported the results of thin layer deposition using PLD method with previously performed milling treatment of the TiO2 target material.
2. EXPERIMENTAL DETAILS
Materials used in this study was a commercial TiO2powder from Merck (M=7990 g/mol) and a silicon substrate (111). Equip- ment used for milling is high energy milling-3D motion ellipse (HEM-E3D) with a rotation speed of 1000 rpm, the motor power of 1 kW and a size of 100 ml vial. This system has a three- dimensional motion and rotation in the vial so that the formation of nano particles homogeneously can more quickly and effec- tively. PLD equipment used by utilizing high-power laser pulses on the order of nanoseconds narrow pulse type Nd-YAG (Lab series,=532 nm, 20 mJ, 6 ns).
Preparation of the TiO2 targets was done by preparing each 5 grams TiO2powder milling process was then performed with a 6582 Adv. Sci. Lett. Vol. 23, No. 7, 2017 1936-6612/2017/23/6582/003 doi:10.1166/asl.2017.9688
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variety of milling time 0, 1, 3 and 6 hours. Furthermore, the TiO2 powder was molded into cylindrical pellets or tablet measuring 1 cm and a thickness of 0.5 cm by applying pressure using a pressing apparatus. Results of TiO2 pellets with a variation of milling time were then used as the source or target material was deposited on silicon substrate using a PLD method. TiO2 pellets as the target and the silicon substrate were placed in the sample chamber. The silicon substrate was set to form angle of 45to the direction of the laser beam. The pressure in the vacuum chamber about 5 Torr was measured using digital Piranimeter (Diavac PT- 1DA). Samples and quartz lens can be driven in two directions relative to the direction of the laser radiation by using step motors and with a micrometer in the direction perpendicular to the laser radiation. In order to obtain a high power density on the target surface, the laser radiation pulse was focused with quartz lens (f =15 cm) through the quartz window to the target surface of TiO2. The laser was operated with a repetition frequency of 10 Hz.
Results of thin layer deposition of TiO2 with a variety of milling time were further characterized using XRD (X-ray diffraction) to determine the crystal structure and using SEM (scanning electron microscope) to determine of the surface morphology.
3. RESULTS AND DISCUSSION
Figure 1 shows the X-ray diffraction pattern of TiO2 powder used to make target. Based on the resulting diffraction pat- tern of the powder has a commercial TiO2 rutile and anatase phases.
Figure 2 shows the pattern of X-ray diffraction of a thin layer of TiO2 was deposited on silicon substrate (111) with the untreated milling (Fig. 2(a)) and treatment with milling for 1 hour (Fig. 2(b)), 3 hours (Fig. 2(c)) and 6 hours (Fig. 2(d)). It is seen that all the thin layer of TiO2 produced has the same phase con- sisting of rutile phase (R) and anatase (A). In the milling process is carried out both for 1, 3 or 6 hours does not lead to a new phase and is the same as that of the untreated milling. However, the highest intensity is generated in all the peaks in the samples with the treatment process of milling for 3 hours (Fig. 2(c)). It is shown from anatase peak FWHM value of the 400 orienta- tion (A400) in the samples #c are relatively small compared to other samples as shown in Table I, so that the quality of the crystallinity relatively better.
Fig. 1. Pattern of X-ray diffraction of commercial TiO2powder.
Fig. 2. The pattern of X-ray diffraction of a thin layer of TiO2was deposited on silicon substrate (111) with milling treatment of the TiO2powder for (a) 0, (b) 1, (c) 3 and (d) 6 hours.
Figure 3 shows the SEM image of a cross section of a thin layer of TiO2 with a variety of milling treatment for 0, 1, 3 and 6 hours. The thickness of all layers of thin TiO2 produced rel- atively the same, however the sample with milling treatment of 3 hours (Fig. 3(c)) relatively more regularly without the appear- ance of bumpy grains.
This is also shown in Figure 4 which shows SEM images of the surface of a thin layer of TiO2 with a variety of milling treatment for 0, 1, 3 and 6 hours. The size of the grain produced in the sample by milling treatment for 3 hours relatively uniform or homogeneous.
In the treatment without milling (Fig. 4(a)) and the milling treatment for 1 hour (Fig. 4(b)) still indicates a droplet that causes irregularities in the granules. Meanwhile, milling treatment for 6 hours (Fig. 4(d)) produces porosity in thin layers. Milling treat- ment on TiO2 material before it is made of pellets as the target aims to make more homogeneous material with a smaller particle size resulting compactness when made in the form of cylindri- cal pellets or tablets. The condition of the target density will affect the resulting film thickness. Increasing of the density and homogeneity of pellet sample will increase the rate of deposi- tion by the number of ions, atoms or radicals generated by laser ablation. It will be able to improve the efficiency of the result- ing thin layer deposition.57 However, on the other hand if the deposition rate is too high will lead to increased growth rate of grain, resulting in intense competition nucleation process. This is resulting in overlap between grains and irregularities occur on the surface nucleation. Overlap of these granules occurs in the treated sample milling for 6 hours (Fig. 4(d)).
Thin film growth process itself is an amalgamation of a ran- dom collection of single particles, such as atoms, molecules or clusters to form a set of granular solids above a substrate sur- face which eventually form a thin film. This process involves
Table I. Value of FWHM on TiO2peak of the (400) orientation.
FWHM (degree)
Peak Sample #a Sample #b Sample #c Sample #d
A400 0,3 0,4 0,2 0,3
6583
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Fig. 3. SEM image of a cross section of the TiO2thin film grown on Si substrate (111) using PLD method with milling treatment of the TiO2powder for (a) 0, (b) 1, (c) 3 and (d) 6 hours.
a b c d
Fig. 4. SEM images of the surface of a thin layer of TiO2with a variety of milling treatment for 0, 1, 3 and 6 hours.
the transfer mechanism particles to the surface of the substrate which then undergo a process of lateral transport that will form a monomer which will be nucleated with characterized by adsorp- tion, diffusion surface, re-evaporation and nucleation.7 After nucleation occurs on the surface of the substrate, the next process is crystal growing, cultivation of grain, the coalition between the grains and the growth of film thickness. In samples with milling treatment for 3 hours allowed the coalition between the grains than other samples.
4. CONCLUSIONS
In conclusion, this study shows that a thin layer of TiO2 pro- duced relatively homogeneous for a given sample milling treat- ment during the manufacture of TiO2target as target material for 3 hours.
Acknowledgments: This study was supported by Ministry of Research and Higher Education, the grant from Hibah Ber- saing 2016 and PT. Maju Makmur Mandiri Reseach Center Foun- dation has supported the laser system.
References and Notes
1. S. D. Mo and W. Y. Ching,Phys. Rev. B51, p13023(1995).
2. C. K. Jung, B. C. Kang, H. Y. Chae, Y. S. Kim, M. K. Seo, S. K. Kim, S. B.
Lee, J. H. Boo, Y. J. Moon, and J. Y. Lee,Journal of Crystal Growth235, p450 (2002).
3. A. Fahmi, C. Minot, B. Silvi, and M. Causa,Phys. Rev. B47, 11 717(1993).
4. W. Setiabudi and A. Subagio,Proc. of Seminar of Physics, Semarang State University(2010).
5. M. Zhu, J. Zhu, J. M. Liu, and Z. G. Liu,Appl. Phys. A80, 135(2005).
6. N. Sato, M. Matsuda, M. Yoshinaga, T. Nakamura, S. Sato, and A. Muramatsu, Top Catal.52, 1592(2009).
7. C. E. Sittner and A. Bergauer,Mat. Res. Soc. Proc. of Spring Meeting1 (2001).
Received: 5 September 2016. Accepted: 13 December 2016.
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Growth of TiO thin films by high energy milling assisted pulsed laser deposition method (Article)
, , , ,
Physics Department, Faculty of Sciences and Mathematics, Diponegoro University, Indonesia
Alumnus of Physics Department, Faculty of Sciences and Mathematics, Diponegoro University, Indonesia
Abstract
TiO thin film can be deposited on the silicon substrate using pulse laser deposition method. To prove homogeneity of grain size on surface, this study uses milling treatment for TiO powder before it is deposited. Milling treatment was conducted on samples of commercial TiO powder with high energy milling method. The variation of milling time was 0, 1, 3 and 6 hours. Furthermore, the samples were shaped as disc with diameter of 1 cm and used as a target source in growth of thin film. Variations in time for the milling treatment of the TiO powder has no effect on the phase change, but rather on the homogeneity of grain size on a thin layer of TiO . In this study, the optimum milling time to produce a homogeneous grain size of a thin layer of TiO for 3 hours. © 2017 American Scientific Publishers All rights reserved.
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HEM-PLD Milling treatment Thin film TiO
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Ministry of Higher Education and Scientific Research
Funding text
Acknowledgments: This study was supported by Ministry of Research and Higher Education, the grant from Hibah Ber-saing 2016 and PT. Maju Makmur Mandiri Reseach Center Foundation has supported the laser system.
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(1995) Physical Review B, 51 (19), pp. 13023-13032. . doi: 10.1103/PhysRevB.51.13023
Jung, C.-K., Kang, B.-C., Chae, H.-Y., Kim, Y.-S., Seo, M.-K., Kim, S.-K., Lee, S.-B., (...), Lee, J.-Y.
(2002) Journal of Crystal Growth, 235 (1-4), pp. 450-456. . doi: 10.1016/S0022-0248(01)01939-X
Fahmi, A., Minot, C., Silvi, B., Causá, M.
(1993) Physical Review B, 47 (18), pp. 11717-11724. . doi: 10.1103/PhysRevB.47.11717
Setiabudi, W., Subagio, A.
(2010) Proc. of Seminar of Physics Semarang State University
Zhu, M., Zhu, J., Liu, J.M., Liu, Z.O.
(2005) Applied Physics A: Materials Science and Processing, 80 (1), pp. 135-139. . doi: 10.1007/s00339-003-2107-7
Sato, N., Matsuda, M., Yoshinaga, M., Nakamura, T., Sato, S., Muramatsu, A.
(2009) Topics in Catalysis, 52 (11), pp. 1592-1597. . doi: 10.1007/s11244-009-9286-1
Sittner, C.E., Bergauer, A.
(2001) Mat. Res. Soc. Proc. of Spring Meeting, p. 1.
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Rubric Validation for the Review of Didactic Planning in Initial Teaching Training Maribel Brito-Lara, José López-Loya, and Sergio Tobón
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d-Level (n, n) Quantum Secret Sharing Protocol Nayereh Majd and Abdolmajid Nazari
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Business Processes of Managing Media Assets: Technology and Practice of Implementation MAM-Class Systems Roman R. Veynberg and Valeriy A. Titov
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Educational Factors Correlated to Ethnic Identity of Independent Chinese Secondary School Students in Malaysia Pei Yao Ho, Fong Peng Chew, and Ker Pong Thock
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Social Participation Activities Towards Urban Wellbeing Among Multi-Ethnic Community in Malaysia Juhari Ahmad, Abdul Razaq Ahmad, and Fong Peng Chew
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A Two-Step Local Search Enhancement with the Novel Solution Representation for Solving Capacitated Vehicle Routing Problems
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Development and Validation of Smartphone Addiction Scale Based on the Human Evaluation Model (HEM) Man-Ki Moon
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The Effectiveness of Training for Parents in Improving the Social Skills of Children with Autism Spectrum Disorder Herlina, Ishak Abdulhak, Zaenal Alimin, and Rudi Susilana
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Factor Analysis of the Companies Demands to the Polytechnic Graduates in Indonesia Achmad Muhammad, Emma Dwi Ariyani, Supriyadi Sadikin, and Dede Sujana
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Effectiveness of Applied Behavior Analysis and Floortime Methods Combination in Enhancing Cognitive and Functional Emotionals Ability Simultaneously of Children with Autism Spectrum Disorders
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Exploring the Meaning of Care in the Teaching Case of North Korean Defector Elementary School Students Hyunhee Yoon and Youngsoon Kim
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Forgiveness Among Maduraness Ethnic: The Relation Between Religiosity, Interpersonal Attachment and Personality Trait
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Holistic Wellness of Neglected Children
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Advanced Science Letters
ISSN 1936-6612 (Print)
Publisher: American Scientific Publishers More about this publication?
ADVANCED SCIENCE LETTERS is an international peer-reviewed journal with a very wide-ranging coverage, consolidates research activities in all areas of (1) Physical Sciences, (2) Biological Sciences, (3) Mathematical Sciences, (4) Engineering, (5) Computer and Information Sciences, and (6) Geosciences to publish original short communications, full research papers and timely brief (mini) reviews with authors photo and biography
encompassing the basic and applied research and current developments in educational aspects of these scientific areas.
Volume 23, Number 7, July 2017
research-article
Selected Peer-Reviewed Articles from the International Conference on Architecture and Built Environment 2016 (ICABE 2016), Kuala Lumpur, Malaysia, 5–6 October, 2016
pp. 6029-6030(2)
Authors: Osman, Mariana Mohammed; Abdullah, Muhammad Faris; Abdullah, Alias
Demand for Low-Cost Housing Among Local People in Perak
pp. 6031-6034(4)
Authors: Osman, Mariana Mohamed; Khalid, Najihan; Syuid, Syafiee
The Challenges of Quantity Surveyor in Sustainable Construction Projects
pp. 6035-6039(5)
Authors: Haron, Roziha Che; Ibrahim, Putri Haryati; Rawi, Azya Binti Mat Contents
Supplementary Data
11/30/2019 Advanced Science Letters: Ingenta Connect Table Of Contents
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Illegal Occupation of State Land in Perak: A Review of the State’s Legalisation Program (PATUH)
pp. 6040-6043(4)
Authors: Osman, Mariana Mohamed; Wahab, Hanisah Ab; Abdullah, Muhammad Faris;
Mohamed, Mohd Zain
Linking Motivation, Satisfaction and Academic Performance of Construction Management Programmes: A Case Study of Malaysia
pp. 6044-6048(5)
Authors: Tey, Kim Hai; Lim, Shun Jinn; Song, Poh Choo; Olanrewaju, AbdulLateef
Housing Affordability Index for Districts in Perak
pp. 6049-6052(4)
Authors: Osman, Mariana Mohamed; Yusop, Siti Wahidah Muhamad; Shuid, Syafiee;
Abdullah, Muhammad Faris
Critical Factors Affecting Productivity for Table Form System in the Malaysian Construction Industry
pp. 6053-6056(4)
Authors: Wah-Peng, Lee; See-Seng, Ng; Tien-Choon, Toh; Cheng-Sim, Lim; Jeffrey, Yap Boon- Hui
Assessment of Gated Community and Guarded Neighbourhood from Public Perspective
pp. 6057-6059(3)
Authors: Abdullah, Muhammad Faris; Daniar, Nurul Ain Mohd; Osman, Mariana Mohamed;
Bachok, Syahriah
Sustainability Assessment of Community-Based Poverty Reduction Projects (CPRP) in Nigeria
pp. 6060-6063(4)
Authors: Zayyanu, Muhammad; Johar, Foziah; Zungwenen, Utange J; Siddiq, Usman A
Distribution of Special Education Programs in Mainstream Schools in Selangor
pp. 6064-6067(4)
Authors: Osman, Mariana Mohamed; Shuhaimi, Ainul Ashiqin Ahmad; Rabe, Noor Suzilawati
Design Factors Contributing to Active Urban Squares in Malaysia
pp. 6068-6072(5)
Authors: Zakariya, Khalilah; Harun, Nor Zalina; Mansor, Mazlina
11/30/2019 Advanced Science Letters: Ingenta Connect Table Of Contents
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Solid Waste Management Practice and Environmental Awareness Level of Postgraduate and Undergraduate Students: Case Study of UTM
pp. 6073-6077(5)
Authors: Hashim, Kamil; Rabe, Noor Suzilawati; Osman, Mariana Mohamed; Zahari, Rustam Khairi
Vacant Land Utilization Agreement Model Based on Community Aspiration to Strengthen Food Security: A Case Study in Sleman District, Yogyakarta Special Region, Indonesia
pp. 6078-6082(5) Author: Suparwoko
Parents’ Perception on Children Safe Distance: A Case Study of Kuala Lumpur and Selangor
pp. 6083-6086(4)
Authors: Rabe, Noor Suzilawati; Osman, Mariana Mohamed; Bachok, Syahriah; Abdullah, Muhammad Faris; Shuid, Syafiee; Ponrahono, Zakiah
Communities’ Local Knowledge of Flood Disaster Management in Pakistan
pp. 6087-6090(4)
Authors: Khan, Muhammad Gohram; Johar, Foziah; Chado, Jiman
Awareness and Involvement of Downstream Residents Toward the Mitigation Plan of Dam Failure: A Case Study of Klang Gate Dam
pp. 6091-6094(4)
Authors: Ibrahim, Illyani; Ghazali, Ahmad Aiman; Jaafar, Samsuddin; Mahamood, Lukman Hakim
Memory, Hope, and Sense—Design as Generator (DAG) Premises for Empowering Community
pp. 6095-6101(7)
Authors: Katoppo, Martin L; Triyadi, Sugeng; Siregar, M. Jehansyah
Assessment on Public Perception Towards the Development of 1Malaysia Youth Cities
pp. 6102-6105(4)
Authors: Rabe, Noor Suzilawati; Osman, Mariana Mohamed; Abdullah, Muhammad Faris