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Towards Flexible Sensors and Actuators : Application Aspect of Piezoelectronic Thin FilmJoshi, Sudeep January 2013 (has links) (PDF)
Man’s desire to replicate/mimic the nature’s creation provided an impetus and inspiration to the rapid advancements and progress made in the sensors and actuators technology. A normal human being has five basic sensory organs, which helps and guides him in performing the routine tasks. This underlines the importance of basic sensory organs in a human life. In a similar fashion, sensors and actuators are of paramount importance for most of the science and engineering applications.
The aim of the present thesis work is to explore the application of piezoelectric ZnO thin films deposited on a flexible substrate for the development of sensors and actuators. Detailed study was performed on the suitability of three different flexible substrates namely Phynox, Kapton and Mylar. However, Phynox alloy substrate was found to be a suitable substrate material for the above mentioned applications. Sputtering technique was chosen for the deposition of ZnO thin films on to Phynox substrate. The necessary process parameters were optimized to achieve good quality piezoelectric thin films.
In the present work, sensors have been developed by utilizing the direct piezoelectric effect of ZnO thin films deposited on Phynox alloy substrate. These includes a flow sensor for gas flow rate measurement, impact sensor for non-destructive material discrimination study and a Thin Film Sensor Array (TFSA) for monitoring the impact events. On the other hand, using the converse piezoelectric effect of ZnO thin films, actuators have also been developed. These include a thin film micro actuator and a Thin Film Micro Vibrator (TFMV) for vibration testing of micro devices. The thesis is divided into following seven chapters.
Chapter 1:
This chapter gives a general introduction about sensors and actuators, piezoelectric thin films, flexible substrates, thin film deposition processes and characterization techniques. A brief literature survey of different applications of piezoelectric thin films deposited on various flexible substrates in device development is presented.
Chapter 2:
A novel flexible metal alloy (Phynox) and its properties along with its applications are discussed in this chapter. ZnO thin films were deposited on Phynox substrate by Rf reactive magnetron sputtering technique. The sputtering process parameters such as: Ar:O2 gas ratio, substrate temperature and RF power were optimized for the deposition of good quality piezoelectric ZnO thin films. The deposited ZnO thin films were characterized using XRD, SEM, AFM and d31 coefficient measurement techniques.
Chapter 3:
It reports on the comparative study of properties of piezoelectric ZnO thin films deposited on three different types of flexible substrates. The substrate materials employed were a metal alloy (Phynox), polyimide (Kapton), and polyester (Mylar). Piezoelectric ZnO thin films deposited on these flexible substrates were characterized by XRD, SEM, AFM and d31 coefficient measurement techniques. A vibration sensing test was also performed for the confirmation of good piezoelectric property. Compared to the polymer flexible substrates, the metal alloy flexible substrate (Phynox) was found to be more suitable for integrating ZnO thin film for sensing applications.
Chapter 4:
The development of a novel gas flow sensor for the flow rate measurement in the range of L min-1 is presented in this chapter. The sensing element is a Phynox alloy cantilever integrated with piezoelectric ZnO thin film. A detailed theoretical analysis of the experimental set–up showing the relationship between output voltage generated and force at a particular flow rate has been discussed. The flow sensor is calibrated using an in-house developed testing set-up.
Chapter 5:
This chapter is divided into two sections. Section 5.1 reports on the development of a novel packaged piezoelectric thin film impact sensor and its application in non-destructive material discrimination studies. Different materials (Iron, Glass, Wood and Plastic) were successfully discriminated by using the developed impact sensor. The output response of impact sensor showed good linearity and repeatability. The impact sensor is sensitive, reliable and cost-effective. Section 5.2 reports on the development of a Thin Film Senor Array (TFSA) for monitoring the location and magnitude of the impact force. The fabricated TFSA consists of evenly distributed ZnO thin film sensor array.
Chapter 6:
It consists of two sections. Section 6.1 reports on the fabrication of micro actuator using piezoelectric ZnO thin film integrated with flexible Phynox substrate. A suitable concave Perspex mounting was designed for the actuator element. The actuator element was excited at different frequencies for the supply voltages of 2V, 5V and 8V. The developed micro actuator has the potential to be used as a micro pump for pumping nano liters to micro liters of fluids. Section 6.2 reports the design and development of a portable ready to use Thin Film Micro Vibrator (TFMV). The TFMV is capable of providing the vibration amplitude in the range of nanometer to micrometer. A thin silicon diaphragm was used as a test specimen for its vibration testing studies using the developed TFMV. The TFMV is light-weight and have internal battery, hence no external power supply is required for its functioning.
Chapter 7:
The first section summarizes the salient features of the work presented in this thesis. In the second section the scope for carrying out the further work is given.
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Investigations On The Effect Of Process Parameters On The Composition Of DC Magnetron Sputter Deposited NiTi Shape Memory Alloy Thin FilmsSumesh, M A 09 1900 (has links) (PDF)
No description available.
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Plasma Surface Engineering - Studies On Nitride Coatings And Surface Modification Of PolymersGuruvenket, S 10 1900 (has links) (PDF)
No description available.
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Investigations On The Properties Of TiN, NbN Thin Films And Multilayers By Reactive Pulsed Laser DepositionKrishnan, R 07 1900 (has links) (PDF)
Two technologies, namely Laser Technology and Surface Modification Technology, have made rapid strides in the last few decades. The lasers have evolved from a simple laboratory curiosity to a matured industrial tool and its applications are limited only by imagination. Intense, coherent and monochromatic laser sources with power outputs ranging over several orders of magnitude have found innumerable applications in the realm of materials engineering. Reactive Pulsed Laser Deposition (PLD) is a powerful technique that utilises the power of a nanosecond pulsed laser for materials synthesis. Unlike conventional PLD, which require high density targets that are difficult to synthesize at a reasonable cost, the RPLD circumvents the need for one such ceramic target. This thesis presents a detailed and judicious use of this technique for synthesis of hard ceramic multilayer coatings using elemental metal targets.
Transition metal nitrides having rock salt structure are known to exhibit superior properties such as hardness and wear resistance and hence formed the basis for the development of first generation coatings. Further improvements through alloying of these binary compounds with metal or metalloid components lead to the development of second generation coatings. As the demand for functional materials increased, surface modification technology alias surface engineering, grew in leaps and bounds. As the large number of coating requirements for optimal performance could not be fulfilled by a single homogeneous material, third generation coatings, comprising multilayer coatings, were developed. It is this aspect of combining the advantages of RPLD process to synthesize ceramic multilayer coatings, provides the main motivation for the present research work.
In this thesis, a systematic study presented for synthesis of nanocrystalline and stoichiometric TiN and NbN thin films using RPLD through ablation of high purity titanium and niobium targets, in the presence of low pressure nitrogen gas. A novel Secondary Ion Mass Spectrometry (SIMS) based analysis was developed to effectively deduce the important process parameters in minimum trials to arrive at desired composition. The validity of this SIMS based method, for optimization of process parameters to get stoichiometric nitride films, was proved beyond any speculation by corroborative Proton Elastic Backscattering Spectrometric (PEBS) analysis. SIMS was also used to characterize the [NbN/TiN] multilayers. The feasibility of growing nanocrystalline multilayers with varying thicknesses has been demonstrated. Nanomechanical properties including hardness and adhesion strength of monolithic TiN and NbN films and multilayers were evaluated.
The thesis is organised into six chapters. The first chapter gives a brief account on the history and development of ‘surface engineering’. The second chapter provides a comprehensive description of the experimental facility developed in-house to pursue research on PLD grown ceramic thin films and multilayers. Thin film synthesis procedure for ex-situ SIMS and TEM analyses is described. Brief introduction is also presented on the characterization techniques used in this study to investigate the surface, interface and microstructural aspects of PLD grown films with underlying basic principles. The third and fourth chapter describes the synthesis and characterization of titanium nitride and niobium nitride thin films using RPLD technique, respectively. SIMS was used in depth profiling mode, for optimization of three important process parameters, viz., nitrogen gas pressure, substrate temperature and laser pulse energy, to get stoichiometric nitride films. Further, films were characterized using GIXRD, TEM, XPS and PEBS for their structure and composition. AFM measurements were made to elucidate the surface morphological features. PEBS was effectively used to estimate the nitrogen concentration in a quantitative manner and the results corroborate well with the SIMS measurements. Having succeeded in synthesizing stoichiometric TiN and NbN films, further studies on the nanomechanical properties of monolithic TiN and NbN films and their multilayers were carried out and these results form the contents of the fifth chapter. The findings of the work reported in this thesis are concluded in Chapter 6 and few possible suggestions were presented as future directions.
Both the monolithic TiN and NbN coatings showed a deposition pressure dependent hardness variation. The hardness of these monolithic films was found to be around 30 GPa, higher than the hardness values obtained by other conventional techniques. Keeping total thickness of the multilayers constant at 1 μm, [NbN/TiN] multilayers having bilayer periods ranging from 50 nm to 1000 nm, were synthesized. A systematic enhancement in hardness upto ~ 40 GPa was observed for [NbN/TiN]10 with the modulus of the multilayer remaining almost constant. The pileup observed around the indentation edge is indicative of toughening in multilayers. The tribological properties of multilayer films showed a better performance in terms of low coefficient of friction and regeneration of coating surfaces as revealed from the nanotribological studies. Overall, the multilayer coatings exhibited better performance in terms of hardness, toughness and adhesion with the substrate material.
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Tuning Zinc Oxide Layers Towards White Light EmissionChirakkara, Saraswathi 01 1900 (has links) (PDF)
White light emitting diodes (LED) have drawn increasing attention due to their low energy consumption, high efficiency and potential to become primary lighting source by replacing conventional light sources. White light emission is usually generated either by coating yellow phosphor on a blue-LED or blending red, green and blue phosphor in an appropriate ratio. Maintaining appropriate proportions of individual components in the blend is difficult and the major demerit of such system is the overall self-absorption, which changes the solution concentration. This results in uncontrolled changes in the whiteness of the emitted light. Zinc Oxide (ZnO), a wide bandgap semiconductor with a large exciton binding energy at room temperature has been recognized as a promising material for ultraviolet LEDs and laser diodes. Tuning of structural, optical and electrical properties of ZnO thin films by different dopants (Lithium, Indium and Gallium) is dealt in this thesis. The achievement of white light emission from a semiconducting material without using phosphors offers an inexpensive fabrication technology, good luminescence, low turn-on voltage and high efficiency.
The present work is organized chapter wise, which has 8 chapters including the summary and future work.
Chapter 1: Gives a brief discussion on the overview of ZnO as an optoelectronic material, crystal structure of semiconductor ZnO, the effect of doping, optical properties and its possible applications in optoelectronic devices.
Chapter 2: Deals with various deposition techniques used in the present study, includes pulsed laser deposition and thermal evaporation. The experimental set up details and the deposition procedures are described in detail. A brief note on the structural characterization equipments, namely X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and the optical characterization techniques namely Raman spectroscopy, transmission spectroscopy and photoluminescence (PL) spectroscopy is presented. The electrical properties of the films were studied by current- voltage, capacitance - voltage and Hall Effect measurements and the experimental details are discussed.
Chapter 3: High quality ZnO/Si heterojunctions fabricated by growing ZnO thin films on p-type Si (100) substrate by pulsed laser deposition without using buffer layers are discussed in this chapter. The crystallinity of the heterojunction was analyzed by high resolution X-ray diffraction and atomic force microscopy. The optical quality of the film was analyzed by room temperature (RT) photoluminescence measurements. The high intense band to band emission confirmed the high quality of the ZnO thin films on Si. The electrical properties of the junction were studied by temperature dependent resistivity, current- voltage measurements and RT capacitance-voltage (C-V) analysis. ZnO thin film showed the lowest resistivity of 6.4x10-3 Ω.cm, mobility of 7 cm2/V.sec and charge carrier concentration of 1.58x1019cm-3 at RT. The charge carrier concentration and the barrier height (BH) were calculated to be 9.7x1019cm-3 and 0.6 eV respectively from the C-V plot. The BH and ideality factor, calculated by using the thermionic emission (TE) model were found to be highly temperature dependent. We observed a much lower value in Richardson constant, 5.19x10-7 A/cm2K2 than the theoretical value (32 A/cm2K2) for ZnO. This analysis revealed the existence of a Gaussian distribution (GD) with a standard deviation of σ2=0.035 V. By implementing GD to the TE, the values of BH and Richardson constant were obtained as 1.3 eV and 39.97 A/cm2K2 respectively from the modified Richardson plot. The obtained Richardson constant value is close to the theoretical value for n-ZnO. These high quality heterojunctions can be used for solar cell applications.
Chapter 4: This chapter describes the structural and optical properties of Li doped ZnO thin films and the properties of ZnO/Li doped ZnO multilayered thin film structures. Thin films of ZnO, Li doped ZnO (ZLO) and multilayer of ZnO and ZLO (ZnO/ZLO) were grown on silicon and Corning glass substrates by pulsed laser deposition technique. Single phase formation and the crystalline qualities of the films were analyzed by X-ray diffraction and Li composition in the film was investigated to be 15 Wt % by X-ray photoelectron spectroscopy. Raman spectrum reveals the hexagonal wurtzite structure of ZnO, ZLO and ZnO/ZLO multilayer, confirms the single phase formation. Films grown on Corning glass show more than 80 % transmittance in the visible region and the optical band gaps were calculated to be 3.245, 3.26 and 3.22 eV for ZnO, ZLO and ZnO/ZLO respectively. An efficient blue emission was observed in all films that were grown on silicon (100) substrate by photoluminescence (PL). PL measurements at different temperatures reveal that the PL emission intensity of ZnO/ZLO multilayer was weakly dependent on temperature as compared to the single layers of ZnO and ZLO and the wavelength of emission was independent of temperature. Our results indicate that ZnO/ZLO multilayer can be used for the fabrication of blue light emitting diodes.
Chapter 5: This chapter is divided in to two parts. The fabrication and characterization of In doped ZnO thin films grown on Corning glass substrate is discussed in the first section. Zinc Oxide (ZnO) and indium doped ZnO (IZO) thin films with different indium compositions were grown by pulsed laser deposition technique. The effect of indium concentration on the structural, morphological, optical and electrical properties of the film was studied. The films were oriented along the c-direction with wurtzite structure and are highly transparent with an average transmittance of more than 80 % in the visible wavelength region. The energy band gap was found to be decreasing with increasing indium concentration. High transparency makes the films useful as optical windows while the high band gap values support the idea that the film could be a good candidate for optoelectronic devices. The value of resistivity observed to be decreasing initially with doping concentration and subsequently increasing. The XPS and Raman spectrum confirm the presence of indium in indium doped ZnO thin films. The photoluminescence spectrum showed a tunable red light emission with different In concentrations.
Undoped and In doped ZnO (IZO) thin films were grown on Pt coated silicon substrates (Pt/Si) to fabricate Pt/ZnO:Inx Schottky contacts (SC) is discussed in the second section. The SCs were investigated by conventional two probe current-voltage (I-V) measurement and by the I-V spectroscopy of conductive atomic force microscopy (C-AFM). X-ray diffraction technique was used to examine the thin film quality. Changes in various parameters like Schottky barrier height (SBH) and ideality factor (IF) as a function of temperature were presented. The estimated BH was found to be increasing and the IF was found to be decreasing with increase in temperature. The variation of SBH and IF with temperature has been explained by considering the lateral inhomogeneities in nanometer scale lengths at metal–semiconductor (MS) interface. The inhomogeneities of SBH in nanometer scale length were confirmed by C-AFM. The SBH and IF estimated from I-V spectroscopy of C-AFM showed large deviation from the conventional two probe I-V measurements. IZO thin films showed a decrease in SBH, lower turn on voltage and an enhancement in forward current with increase in In concentration.
Chapter 6: In this chapter the properties of Ga doped ZnO thin films with different Ga concentrations along with undoped ZnO as a reference is discussed. Undoped and Ga doped ZnO thin films with different Ga concentrations were grown on Corning glass substrates by PLD. The structural, optical and electrical properties of Ga doped ZnO thin films are discussed. The XRD, XPS and Raman spectrum reveal the phase formation and successful doping of Ga on ZnO. All the films show good transmittance in the visible region and the photoluminescence of Ga doped ZnO showed a stable emission in the blue- green region. The resistivity of Ga doped ZnO thin films was found to be first decreasing and then increasing with increase in Ga concentrations.
Chapter 7: The effect of co-doping to ZnO on the structural, optical and electrical properties was described in this chapter. Ga and In co-doped ZnO (GIZO) thin films together with ZnO, In doped ZnO (IZO), Ga doped ZnO (GZO), IZO/GZO multilayer for comparison, were grown on Corning glass and boron doped Si substrates by PLD. GIZO showed better structural, optical and electrical properties compared with other thin films. The Photoluminescence spectra of GIZO showed a strong white light emission and the current-voltage characteristics showed relatively lower turn on voltage and larger forward current. The CIE co-ordinates for GIZO were observed to be (0.31, 0.33) with a CCT of 6650 K, indicating a cool white light and established a possibility of white light emitting diodes.
Finally the chapter 8 presents the summary derived out of the work and a few suggestions on future work.
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Studies on AgInS2 Films as Absorber Layer for Heterojunction Solar CellsSunil, Maligi Anantha January 2016 (has links) (PDF)
Currently conventional sources like coal, petroleum and natural gas meet the energy requirements of developing and undeveloped countries. Over a period of time there is high risk of these energy sources getting depleted. Hence an alternate source of energy i.e. renewable energy is the need of the hour. The advantages of renewable energy like higher sustainability, lesser maintenance, low cost of operation, and minimal impact on the environment make the role of renewable energy sources significant. Out of the various renewable energy sources like solar energy, wind energy, hydropower, biogas, tidal and geothermal, usage of solar energy is gradually increasing. Among various solar energy sources, Photovoltaics has dominated over the past two decades since it is free clean energy and availability of abundant sunlight on earth.
Over the past few decades, thin film solar cells (TFSC) have gained considerable interest as an economically feasible alternative to conventional silicon (Si) photovoltaic devices. TFSCs have the potential to be as efficient as Si solar cells both in terms of conversion efficiency as well as cost. The advantages of TFSC are that they are easy to prepare, lesser thickness, requires lesser materials, light weight, low cost and opto-electronic properties can be tuned by varying the process parameters. The present study is focused on the fabrication of AgInS2/ZnS heterojunction thin film solar cell. AgInS2 absorber layer is deposited using both vacuum (sputtering/sulfurization) and non-vacuum (ultrasonic spray pyrolysis) techniques. ZnS window layer is prepared using thermal evaporation technique, detailed experimental investigation has been conducted and the results have been reported in this work. The thesis is divided into 6 chapters.
Chapter 1 gives general introduction about solar cells and working principle of solar cell. It also discusses thin film solar cell technology and its advantages. Layers of thin film solar cell structure, Significance of each layers and possible materials to be used are emphasized. A detailed overview of the available literature on both AgInS2 absorber layer and ZnS window layer has been presented. Based on the literature review, objectives of the present work are defined.
Chapter 2 explains the theory and experimental details of deposition techniques used for the growth of AgInS2 and ZnS films. Details of characterization techniques to study film properties are described in detail.
Chapter 3 presents a systematic study of AgInS2 thin films deposited by sulfurization of sputtered Ag-In metallic precursors. Initially, AgInS2 films are deposited by varying the substrate temperature and properties of as-deposited films are characterized. Structural, morphological, electrical and optical properties of AgInS2 films are explained. From these studies, samples with better properties at particular substrate temperature are optimized. By fixing the substrate temperature, deposition time of silver is varied by keeping other deposition conditions same and the properties of films are discussed. It was observed that deposition time of silver doesn’t have much impact on structural properties of AgInS2 films. However, opto-electric properties of AgInS2 films are enhanced. Based on characterization studies, deposition time of silver is optimized. Deposition time of indium is varied by keeping substrate temperature and silver deposition to optimized value. The properties of as-deposited films are discussed. Based on the above studies, the optimized p type films have a band gap of 1.64 eV, carrier concentration of 1013 ions/cm3 and Resistivity of order 103 Ω-cm.
Chapter 4 presents a systematic study of AgInS2 thin films deposited by ultrasonic spray pyrolysis. AgInS2 films are deposited by varying the substrate temperature and properties of as deposited films are characterized. Structural, morphological, electrical and optical properties of AgInS2 films are explained. From these studies, samples with better properties at particular substrate temperature are optimized. By fixing the substrate temperature, concentration of silver molarity in the precursor solution is varied by keeping other deposition conditions same and the properties of films are discussed. Structural, optical and electrical properties of AgInS2 films are
enhanced with the increase in silver concentration. Based on characterization studies, concentration of silver is optimized. Similarly concentration of indium molarity in the precursor solution is varied and the properties of as-deposited films are discussed. Finally, sulfur molarity in the precursor solution is varied and properties of films are discussed. It was observed that increasing sulfur after certain limit does not have any effect on the properties of the films. Based
on the above studies, this method resulted in the films with resistivity of 103 Ω-cm and band gap of 1.64 eV. These films showed a carrier concentration of 1013 ions/cm3.
Chapter 5 describes the growth of ZnS films using thermal evaporation technique. Influence of thickness on the properties of ZnS films is explained. Samples with good crystallinity, high transmission, and wider gap are selected for device fabrication. This p type layer showed a band gap of 3.52 eV. Solar cells have been fabricated using the AgInS2 films developed by both sputtering and ultrasonic spray pyrolysis techniques. A maximum cell efficiency of 0.92 percent has been achieved for the cell with 0.950 µm thick sputtered AgInS2 layer and thermally evaporated 42 nm thick ZnS layer. In comparison, the ultrasonic spray pyrolysis deposited films gave an efficiency of 0.54 percent. These values are comparable to those mentioned in a couple of reports earlier.
Chapter 6 summarizes the conclusions drawn from the present investigations and scope of future work is suggested.
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"Developing Device Quality Vanadium Dioxide Thin Films for Infrared Applications"Bharathi, R January 2016 (has links) (PDF)
Vanadium oxides are being used as the thermal sensing layer because of their applications in infrared detectors. They have high temperature coefficient of resistance, favorable electrical resistance and compatibility with the MEMS technology. Of all oxides of vanadium, only vanadium dioxide (VO2)has been highly investigated as it shows first order transition (semiconducting to metal transition-SMT)at 68 oC. First order transition is understood as the sharp change in the electrical resistance. The change in resistivity in this case is of the order of 105 over a temperature change of 0.1 oC at 68 oC in a single crystal. Doping vanadium oxides with elements like Mo and W reduce the transition temperature. This is very important for room temperature electrical and optical detection. Though most of the research groups subscribe to PLD, cost-effective methods with large area deposition are major focus of this research. Hence for synthesizing VO2 in bulk and thin films, Solution Combustion Synthesis (SCS), Ultrasonic Nebulized Spray Pyrolysis of Aqueous Combustion Mixture (UNSPACM) Chemical vapour deposition (CVD)and microwave are explored. Synthesis of doped VO2 films in CVD has not been done extensively to yield optical quality thin films.
Chapter I surveys the use of phase transition in oxides system for a variety of practical applications. In particular, Vanadium dioxide (VO2) is chosen as it is found to be very useful for infrared and metamaterials based applications. VO2 is known for its first-order semiconducting to metallic transition (SMT). This chapter attempts to explain the influence of processing, doping, annealing, etc on the SMT characteristics. Important aspects such as the idea of hysteresis in VO2 and similarity to martensitic transformation are discussed. The scope and objectives of the thesis are discussed here.
Chapter II explains in detail the materials and methods used to synthesize VO2 both in bulk and in thin lm form and methods used to study their characteristics. Brief description on the principle and the working of the home-built experimental set up needed for this study is elicited.
In chapter III, attempts were made to understand the phase stability of VO2 and the evolution of crystal structures during the phase transition. VO2 crystallizes in P21/c space group at room temperatures with lattice parameters a=5.752 Ab=4.526 Ac=5.382 Aα=90 β=122.60 γ=90 . Precise control of synthesis parameters is required in stabilizing pure phase in bulk as well as thin lm form. This study focuses on the novel large scale two step synthesis of VO2 using Solution Combustion Synthesis. This involves synthesis of product utilizing redox reaction between metal nitrate and suitable fuel. Generally the products are nanocrystalline in nature due to self-propagation of the exothermic combustion reaction. First step involved the synthesis of V2O5 by combustion reaction between Vanadyl nitrate and urea. In the second step, the as-synthesized V2O5 has been reduced by a novel reduction technique to form monophasic VO2. The presence of competing phases like M1, M2, M3 and R are investigated by XRD, Raman spectroscopy, DSC, Optical and high temperature X-ray diffraction.
Chapter IV deals with the reduction in phase transition temperature by doping the SCS synthesized VO2 with W and Mo. Effect of doping on the transition temperature was studied using differential scanning calorimetry (DSC) in both W and Mo. Electrical characteristics of Mo doped VO2 and Optical characteristics of the W-doped VO2 were also studied using four probe resistivity measurements and UV-VIS Spectroscopy respectively. W addition was found to be more effective in reducing the phase transition temperature. To understand further more on the W addition, X-ray photo-electron spectroscopy measurements were performed. W-addition alters the V4+-V4+ bonding and with W addition it is observed that V was present in V3+state. W was present in W6+ state. The addition of W to VO2 introduces more electrons to the systems and disturbs the V4+-V4+ thus reducing the phase transition temperature of VO2.
Chapter V describes the large scale, large area deposition of thin films of VO2 by a cost effective method. A novel technique to deposit vanadium dioxide thin films namely, UNSPACM is developed. This simple two-step process involves synthesis of a V2O5 lm on an LaAlO3(LAO) substrate followed by a controlled reduction to form single phase VO2. The formation of M1 phase (P21/c) is confirmed by Raman spectroscopic studies. A thermally activated metal{insulator transition (MIT) was observed at 61 oC, where the resistivity changes by four orders of magnitude. The infrared spectra also show a dramatic change in reflectance from 13% to over 90% in the wavelength range of 7-15 m. This indicates the suitability of the films for optical switching applications at infrared frequencies. A trilayer metamaterial absorber, composed of a metal structure/dielectric spacer/vanadium dioxide (VO2) ground plane, is shown to switch reversibly between reflective and absorptive states as a function of temperature. The VO2 lm, which changes its conductivity by four orders of magnitude across an insulator{metal transition, enables the switching by forming a resonant absorptive structure at high temperatures while being inactive at low temperatures. The fabricated metamaterial shows a modulation of the reflectivity levels of 58% at a frequency of 22.5 THz and 57% at a frequency of 34.5 THz.
Chapter VI explains the W doped VO2 thin films synthesized by UN-SPACM. Morphology of the thin films was found to be consisting of globular and porous nanoparticles having size 20 nm. Transition temperature decreased with the addition of W. 1.8 at. %W doping in VO2 transition temperature has reduced upto 25 oC. It is noted that W-doping in the pro-cess of reducing the transition temperature, alters the local structure and also increases room temperature carrier concentration. The presence of W, as was seen in Chapter IV, altered V4+-V4+ bonds and introduced V3+. W was found to be in W6+ state suggesting W addition increased the carrier concentration. Hall Effect measurements suggested the increased carrier con-centration.
The roughness of the synthesized films were very high for them to be of de-vice quality, despite encouraging results obtained by electrical measurements. Hence in order to further improve the smoothness and thereby the optical quality of thin films, Chemical Vapour Deposition (CVD) is employed.
Chapter VII outlines the effect of processing parameters and post pro-cessing annealing on the semiconductor-metallic transition of VO2. Here in this chapter, the influence of substrate temperature on the SMT properties of VO2 is explored. At different substrate temperatures, the percentage of phase fraction of V in V3+, 4+ and V5+ differed. Besides, the morphology also varied with substrate temperatures. Similarly it is observed that with annealing the VO2 film deposited on glass substrates, SMT properties enhanced which was attributed to filling out of oxygen vacancies. Si based substrates and non-Si based substrates were used for depositing VO2 thin films by CVD. Their temperature coefficient of resistance and SMT properties were studied in order to understand their potential in bolometer and thermal to optical valve based applications.
Chapter VIII involves the study of VO2 thin films for thermal to optical valves. ITO coated glass substrates were used for the purpose. Thin films were deposited by both UNSPACM and CVD. It was observed that the reflectivity pro les of the films synthesized by the above said methods were very different. Hence in the process of understanding the huge difference in the reflectivity pro les, classical harmonic oscillator, Lorentzian model was employed to t the experimental data at room temperature whereas Drude-Lorentzian model was used to t the data at higher temperature (at 100 oC- after transition). With this fitting plasma frequencies of the CVD films were calculated. It was observed that defect chemistry of films synthesized by these methods were different.
In order to further improve the smoothness of the films, microwave method was proposed in Chapter IX. The preliminary results showed the presence of uniform spheres and 3 D hierarchical structures of VO2 consisting of nanorods. This was extended to deposit VO2 thin films on ITO. DSC and Infrared reflectance pro le of VO2 nanopowder suggested the phase transition.
Chapter X summarizes the work done for the thesis and provides insights to the applications and to the future work.
The work reported in this thesis has been carried out by the candidate as part of the Ph.D.program. She hopes that this would constitute a worth-while contribution towards development of VO2 thin film technology and its challenges for reliable infrared device applications.
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