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Nanofabrication Via Laser Interference Lithography and Integration Of Nanofabrication via Laser Interference Lithography and Integration of Various Optical Systems for Remote Sensing Applications By Muhammad Waqas Khalid A thesis submitted to The University of Birmingham For the degree of DOCTOR OF PHILOSOPHY School of Engineering The University of Birmingham (04/02/2019) University of Birmingham Research Archive e-theses repository This unpublished thesis/dissertation is copyright of the author and/or third parties. The intellectual property rights of the author or third parties in respect of this work are as defined by The Copyright Designs and Patents Act 1988 or as modified by any successor legislation. Any use made of information contained in this thesis/dissertation must be in accordance with that legislation and must be properly acknowledged. Further distribution or reproduction in any format is prohibited without the permission of the copyright holder. Abstract Nanophotonic devices help to manipulate light at nanometric scale through various optical phenomena in near infrared and visible regions of the electromagnetic spectrum. This research aims to present the fabrication, modelling, optical characterisation and real life applications of optical devices based on materials such as ink, soft polymer, gelatine, leuco dye and liquid crystals. Laser interference-based ablation is utilised to generate phase conjugate nanostructures on ink, gelatine based edible nanostructures for food decoration purposes, and flexible polymeric nanostructures on polydimethylsiloxane substrate to demonstrate their use for remote sensing applications. Replication of Cornercube Retroreflector array and diffusing surface is conducted in this research to construct flexible force and temperature sensors. CCRs are mainly exploited in this research due to their retroreflection property. Reflected light from CCRs is sent back towards the source through total internal reflection and is independent of the incident angle. A silver coated CCR is used to fabricate a 2D conjugate periodic gratings structure on ink coated glass substrate through Denisyuk reflection holography. Diffractive gratings (super prism) fabricated from simple mirror-based interference reflection have less features to manipulate as compared to the conjugate diffractive gratings made by using interference obtained from CCRs. Nanometric holographic CCR showed somewhat similar optical properties as shown by master centimetric CCR e.g. phase conjugation. Predictions through computational modelling were also in good agreement with the experimental (optical characterisation) results. CCR array structures are most commonly encountered in everyday life activities such as traffic signals, vehicle safety systems and nightwear clothing. The use of brittle optical devices is limited due to their rigidity. In this research, PDMS was used to replicate rigid CCRs array structures into a flexible form. Polymeric CCRs array was examined and compared to the i stencil by utilising optical microscopy. Optical characterisations were performed under various mechanical and thermal stress levels. Optical properties dependent on structure’s dimension were tuned based on the external stimuli such as force. It is concluded in this study that polymeric optical structures have a potential to be employed in numerous sensing applications for stretch, temperature, pH, and humidity. Combination of CCRs and thermochromatic materials can yield remote temperature sensors based on active components. This research also demonstrates two different systems including liquid crystals and leuco dyes to record temperature changes within a region of interest. Glass based CCRs were coated with leuco dye and liquid crystals and were treated at various known temperatures under continuous monochromatic light illumination. Reflected power from thermochromatic CCR was tuned based on supplied temperature and was found to be dependent on the colour scheme. These novel systems may help to monitor environmental conditions such as temperature changes within hazardous areas, where human access is restricted. Finally, edible, flexible and multi-layered materials were engineered with photonic structures to examine the flexibility of Nd:YAG laser ablation in Denisyuk reflection mode. Fabricated structures were examined by scanning electron microscopy and optically characterised with monochromatic and broadband light sources. Various shapes of nanostructures were achieved by utilising provided parameters for fabrication. It is hence concluded that laser interference- based ablation is simple, fast, cost-effective and flexible technique to copy reflective objects in nanometric scale. ii Dedicated to my Family and Teachers iii Acknowledgement I wish to express my sincere gratitude to my supervisors Dr Haider Butt and Dr Carl Anthony for their guidance, ideas, support and encouragement throughout my doctoral research. I am extremely grateful to Dr Haider Butt for inspiring me through his innovative ideas and his noteworthy passion towards research. I have greatly benefitted from his knowledge and am very thankful to him for his patience and kindness during this research study. I feel fortunate to be supervised by such a great personality. I am thankful to Dr Rajib Ahmed for his help with numerical modelling according to my experimental parameters input and all my colleagues, especially Tawfiq Alqureshi, Ijaz Rashid, Catherine Whitehouse, Bader Alqattan, Yousef Alqureshi, and Mohamed Elsherif for their useful discussions and motivations. I am also grateful to Dr Ali K. Yetisen, Mushfiqur Rahman, Dr Umair Hassan and Dr Ali Raza for their kind help and valuable suggestions during my PhD research. I would also like to thank all my teachers, since my childhood who enabled me to procced step by step during my studies and have helped me in successfully conducting this research. Finally, I would like to give my sincere thanks to my parents, my aunty and all my family and friends for their prayers, support and encouragement during my research study. iv List of Publications [1] Khalid, M.W., et al., Holographic Writing of Ink-Based Phase Conjugate Nanostructures via Laser Ablation. Scientific Reports, 2017. 7(1): p. 10603. [2] Khalid, M.W., et al., Flexible cornercube retroreflector array for temperature and strain sensing. RSC advances, 2018. 8(14): p. 7588-7598. [3] Khalid, M.W., et al., Remote Thermal Sensing by Integration of Corner‐Cube Optics and Thermochromic Materials. Advanced Optical Materials, 2019. 7(2): p. 1801013. v Abbreviations Bright Field BF Light Emitting Diode LED Back Scattered Electron BSE Milli Joule mJ Cornercube Retroreflector CCR Neodymium-doped Yttrium Nd:YAG Aluminium Garnet Dynamic Cornercube Retroreflector DCCR Nanosecond Ns Dark Field DF Optical Phase Conjugation OPC Detection Limit DoL Optical Microscopy OM Electromagnetic Radiations EMRs One/Two/Three dimensional 1/2/3D Electron Beam Lithography EBL Phase Conjugate Mirror PCM Electromagnetic Spectrum EMS Polydimethylsiloxane PDMS Electron Beam Lithography EBL Poly-methyl methacrylate PMMA Energy Dispersive X-Ray EDX Phase Conjugated Wave PCW Fast Fourier Transform FFT Plane Mirror PM Finite Element Method FEM Position Pos Focussed Ion Beam FIB Refractive Index RI Femtosecond Fs Silver Ag Gold Au Secondary Electrons SE Light Amplification by Simulated LASER Scanning Electron Microscopy SEM Emission of Radiation Liquid Crystal Display LCD Total Internal Reflection TIR Ultraviolet Ultraviolet vi Nomenclature A Amplitude Tc Critical Temperature B Magnetic Field 푣 Velocity C Speed of light 푑0 Original Gratings Period D Spacing ΔS Change of Sensitivity E Electric Field Λ Grating’s spacing E Energy É Young’s Modulus F Force Ɛ Strain H Height * conjugate/reversal of polarization I Intensity ℏ Reduced Planck’s Constant 퐽 Electric Current Density ɳ Index of Refraction K Wave number σ Stress 푙 Length 휔 Angular frequency M Phase modulation of reflection ϴ Angle P Pitch ɸ Phase R Reflection Λ Wavelength S̅ Pointing vector ρ Density T Transmission µo Free space permeability t Time Ɛo Free Space Permativity vii Table of Contents Abstract .................................................................................................................................. i Acknowledgement ...................................................................................................................... iv List of Publications ....................................................................................................................... v Abbreviations ............................................................................................................................. vi Nomenclature ............................................................................................................................ vii Table of Contents ...................................................................................................................... viii List of Figures .............................................................................................................................. xi List of Tables ............................................................................................................................. xvii Chapter 1 Introduction .............................................................................................................. 1 1.1 Overview ................................................................................................................................. 1 1.2 Aims and objectives
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