Non-destruct|ve testing of non-metallic materials using microwaves

The motivatitni for" the present work is from .a project sanctioned by TSRO. The work involved the development of a quick and reliable test procedure using microwaves, for tflue inspection of cured propellant samples and a method to monitor the curing conditions of propellant mix undergoing the curing process.Normal testing CHE the propellant samples involvecuttimg a piece from each carton and testing it for their tensile strength. The values are then compared with standard ones and based on this result the sample isaccepted or rejected. The tensile strength is a measure ofdegree of cure of the propellant mix. But this measurementis a destructive procedure as it involves cutting of the sample. Moreover, it does not guarantee against nonuniform curing due to power failure, hot air-line failure,operator error etc. This necessitated the need for the development of a quick and reliable non-destructive test procedure.

Ultrasonic measurement of the elastic properties of benzoyl glycine single crystals

Certain organic crystals are found to possess high non- linear optical coefficients,often one to two orders of magnitude higher than those of the well known inorganic non-linear optical materials.Benzoyl glycine is one such crystal whose optical second-harmonic generation efficiency is much higher than that of potassium dihydrogen phosphate. Single crystals of benzoyl glycine are grown by solvent evaporation technique using N,N-dimethyl formamide as the solvent.All the nine second-order elastic stiffness constants of this orthorhombic crystal are determined from ultrasonic wave velocity measurements employing the pulse echo overlap technique.The anisotropy of elastic wave propagation in this crystal is demonstrated by plotting the phase velocity, slowness,Young's modulus and linear compressibility surfaces along symmetry planes.The volume compressibility, bulk modulus and relevant Poisson's ratios are also determined. Variation of the diagonal elastic stiffness constants with temperature over a limited range are measured and reported.

Development of Free Space Method for Material Characterisation and GPR Study & A Case Study on Biological Samples

The thesis mainly focuses on material characterization in different environments: freely available samples taken in planar fonn, biological samples available in small quantities and buried objects.Free space method, finds many applications in the fields of industry, medicine and communication. As it is a non-contact method, it can be employed for monitoring the electrical properties of materials moving through a conveyor belt in real time. Also, measurement on such systems at high temperature is possible. NID theory can be applied to the characterization of thin films. Dielectric properties of thin films deposited on any dielectric substrate can be determined. ln chemical industry, the stages of a chemical reaction can be monitored online. Online monitoring will be more efficient as it saves time and avoids risk of sample collection.Dielectric contrast is one of the main factors, which decides the detectability of a system. lt could be noted that the two dielectric objects of same dielectric constant 3.2 (s, of plastic mine) placed in a medium of dielectric constant 2.56 (er of sand) could even be detected employing the time domain analysis of the reflected signal. This type of detection finds strategic importance as it provides solution to the problem of clearance of non-metallic mines. The demining of these mines using the conventional techniques had been proved futile. The studies on the detection of voids and leakage in pipes find many applications.The determined electrical properties of tissues can be used for numerical modeling of cells, microwave imaging, SAR test etc. All these techniques need the accurate determination of dielectric constant. ln the modem world, the use of cellular and other wireless communication systems is booming up. At the same time people are concemed about the hazardous effects of microwaves on living cells. The effect is usually studied on human phantom models. The construction of the models requires the knowledge of the dielectric parameters of the various body tissues. lt is in this context that the present study gains significance. The case study on biological samples shows that the properties of normal and infected body tissues are different. Even though the change in the dielectric properties of infected samples from that of normal one may not be a clear evidence of an ailment, it is an indication of some disorder.ln medical field, the free space method may be adapted for imaging the biological samples. This method can also be used in wireless technology. Evaluation of electrical properties and attenuation of obstacles in the path of RF waves can be done using free waves. An intelligent system for controlling the power output or frequency depending on the feed back values of the attenuation may be developed.The simulation employed in GPR can be extended for the exploration of the effects due to the factors such as the different proportion of water content in the soil, the level and roughness of the soil etc on the reflected signal. This may find applications in geological explorations. ln the detection of mines, a state-of-the art technique for scanning and imaging an active mine field can be developed using GPR. The probing antenna can be attached to a robotic arm capable of three degrees of rotation and the whole detecting system can be housed in a military vehicle. In industry, a system based on the GPR principle can be developed for monitoring liquid or gas through a pipe, as pipe with and without the sample gives different reflection responses. lt may also be implemented for the online monitoring of different stages of extraction and purification of crude petroleum in a plant.Since biological samples show fluctuation in the dielectric nature with time and other physiological conditions, more investigation in this direction should be done. The infected cells at various stages of advancement and the normal cells should be analysed. The results from these comparative studies can be utilized for the detection of the onset of such diseases. Studying the properties of infected tissues at different stages, the threshold of detectability of infected cells can be determined.

New studies on the versatile roles of Polyaniline and its composites in polymer based optoelectronic and energy storage devices

From the early stages of the twentieth century, polyaniline (PANI), a well-known and extensively studied conducting polymer has captured the attention of scientific community owing to its interesting electrical and optical properties. Starting from its structural properties, to the currently pursued optical, electrical and electrochemical properties, extensive investigations on pure PANI and its composites are still much relevant to explore its potentialities to the maximum extent. The synthesis of highly crystalline PANI films with ordered structure and high electrical conductivity has not been pursued in depth yet. Recently, nanostructured PANI and the nanocomposites of PANI have attracted a great deal of research attention owing to the possibilities of applications in optical switching devices, optoelectronics and energy storage devices. The work presented in the thesis is centered around the realization of highly conducting and structurally ordered PANI and its composites for applications mainly in the areas of nonlinear optics and electrochemical energy storage. Out of the vast variety of application fields of PANI, these two areas are specifically selected for the present studies, because of the following observations. The non-linear optical properties and the energy storing properties of PANI depend quite sensitively on the extent of conjugation of the polymer structure, the type and concentration of the dopants added and the type and size of the nano particles selected for making the nanocomposites. The first phase of the work is devoted to the synthesis of highly ordered and conducting films of PANI doped with various dopants and the structural, morphological and electrical characterization followed by the synthesis of metal nanoparticles incorporated PANI samples and the detailed optical characterization in the linear and nonlinear regimes. The second phase of the work comprises the investigations on the prospects of PANI in realizing polymer based rechargeable lithium ion cells with the inherent structural flexibility of polymer systems and environmental safety and stability. Secondary battery systems have become an inevitable part of daily life. They can be found in most of the portable electronic gadgets and recently they have started powering automobiles, although the power generated is low. The efficient storage of electrical energy generated from solar cells is achieved by using suitable secondary battery systems. The development of rechargeable battery systems having excellent charge storage capacity, cyclability, environmental friendliness and flexibility has yet to be realized in practice. Rechargeable Li-ion cells employing cathode active materials like LiCoO2, LiMn2O4, LiFePO4 have got remarkable charge storage capacity with least charge leakage when not in use. However, material toxicity, chance of cell explosion and lack of effective cell recycling mechanism pose significant risk factors which are to be addressed seriously. These cells also lack flexibility in their design due to the structural characteristics of the electrode materials. Global research is directed towards identifying new class of electrode materials with less risk factors and better structural stability and flexibility. Polymer based electrode materials with inherent flexibility, stability and eco-friendliness can be a suitable choice. One of the prime drawbacks of polymer based cathode materials is the low electronic conductivity. Hence the real task with this class of materials is to get better electronic conductivity with good electrical storage capability. Electronic conductivity can be enhanced by using proper dopants. In the designing of rechargeable Li-ion cells with polymer based cathode active materials, the key issue is to identify the optimum lithiation of the polymer cathode which can ensure the highest electronic conductivity and specific charge capacity possible The development of conducting polymer based rechargeable Li-ion cells with high specific capacity and excellent cycling characteristics is a highly competitive area among research and development groups, worldwide. Polymer based rechargeable batteries are specifically attractive due to the environmentally benign nature and the possible constructional flexibility they offer. Among polymers having electrical transport properties suitable for rechargeable battery applications, polyaniline is the most favoured one due to its tunable electrical conducting properties and the availability of cost effective precursor materials for its synthesis. The performance of a battery depends significantly on the characteristics of its integral parts, the cathode, anode and the electrolyte, which in turn depend on the materials used. Many research groups are involved in developing new electrode and electrolyte materials to enhance the overall performance efficiency of the battery. Currently explored electrolytes for Li ion battery applications are in liquid or gel form, which makes well-defined sealing essential. The use of solid electrolytes eliminates the need for containment of liquid electrolytes, which will certainly simplify the cell design and improve the safety and durability. The other advantages of polymer electrolytes include dimensional stability, safety and the ability to prevent lithium dendrite formation. One of the ultimate aims of the present work is to realize all solid state, flexible and environment friendly Li-ion cells with high specific capacity and excellent cycling stability. Part of the present work is hence focused on identifying good polymer based solid electrolytes essential for realizing all solid state polymer based Li ion cells.The present work is an attempt to study the versatile roles of polyaniline in two different fields of technological applications like nonlinear optics and energy storage. Conducting form of doped PANI films with good extent of crystallinity have been realized using a level surface assisted casting method in addition to the generally employed technique of spin coating. Metal nanoparticles embedded PANI offers a rich source for nonlinear optical studies and hence gold and silver nanoparticles have been used for making the nanocomposites in bulk and thin film forms. These PANI nanocomposites are found to exhibit quite dominant third order optical non-linearity. The highlight of these studies is the observation of the interesting phenomenon of the switching between saturable absorption (SA) and reverse saturable absorption (RSA) in the films of Ag/PANI and Au/PANI nanocomposites, which offers prospects of applications in optical switching. The investigations on the energy storage prospects of PANI were carried out on Li enriched PANI which was used as the cathode active material for assembling rechargeable Li-ion cells. For Li enrichment or Li doping of PANI, n-Butyllithium (n-BuLi) in hexanes was used. The Li doping as well as the Li-ion cell assembling were carried out in an argon filled glove box. Coin cells were assembled with Li doped PANI with different doping concentrations, as the cathode, LiPF6 as the electrolyte and Li metal as the anode. These coin cells are found to show reasonably good specific capacity around 22mAh/g and excellent cycling stability and coulombic efficiency around 99%. To improve the specific capacity, composites of Li doped PANI with inorganic cathode active materials like LiFePO4 and LiMn2O4 were synthesized and coin cells were assembled as mentioned earlier to assess the electrochemical capability. The cells assembled using the composite cathodes are found to show significant enhancement in specific capacity to around 40mAh/g. One of the other interesting observations is the complete blocking of the adverse effects of Jahn-Teller distortion, when the composite cathode, PANI-LiMn2O4 is used for assembling the Li-ion cells. This distortion is generally observed, near room temperature, when LiMn2O4 is used as the cathode, which significantly reduces the cycling stability of the cells.

Conducting Polyaniline Composites as Microwave Absorbers

Conducting polymers are excellent microwave absorbers and they show technological advantage when compared with inorganic electromagnetic absorbing materials, being light weight , easily processable, and the ability of changing the electromagnetic properties with nature and amount of dopants, synthesis conditions, etc. In this paper we report the synthesis, dielectric properties, and expected application of conducting composites based on polyaniline (PAN). Cyclohexanone soluble conducting PAN composites of microwave conductivity 12.5 S/m was synthesized by the in situ polymerization of aniline in the presence of emulsion grade polyvinyl chloride. The dielectric properties of the composites, especially the dielectric loss, conductivity, dielectric heating coefficient , absorption coefficient, and penetration depth, were studied using a HP8510 vector network analyzer. The microwave absorption of the composites were studied at different frequency bands i.e, S, C, and X bands (2-12 GHz). The absorption coefficient was found to be higher than 200 m -' and it can be used for making microwave absorbers in space applications .

Conducting Polyaniline Composites as Microwave Absorbers

Conducting polymers are excellent microwave absorbers and they show technological advantage when compared with inorganic electromagnetic absorbing materials, being light weight , easily processable, and the ability of changing the electromagnetic properties with nature and amount of dopants, synthesis conditions, etc. In this paper we report the synthesis, dielectric properties, and expected application of conducting composites based on polyaniline (PAN). Cyclohexanone soluble conducting PAN composites of microwave conductivity 12.5 S/m was synthesized by the in situ polymerization of aniline in the presence of emulsion grade polyvinyl chloride. The dielectric properties of the composites, especially the dielectric loss, conductivity, dielectric heating coefficient , absorption coefficient, and penetration depth, were studied using a HP8510 vector network analyzer. The microwave absorption of the composites were studied at different frequency bands i.e, S, C, and X bands (2-12 GHz). The absorption coefficient was found to be higher than 200 m -' and it can be used for making microwave absorbers in space applications

Studies on grain refinement and alloying additions on the microstructure and mechanical properties of Mg-8Zn-4Al alloy

MAGNESIUM ALLOYS have strong potential for weight reduction in a wide range of technical applications because of their low density compared to other structural metallic materials. Therefore, an extensive growth of magnesium alloys usage in the automobile sector is expected in the coming years to enhance the fuel efficiency through mass reduction. The drawback associated with the use of commercially cheaper Mg-Al based alloys, such as AZ91, AM60 and AM50 are their inferior creep properties above 100ºC due to the presence of discontinuous Mg17A112 phases at the grain boundaries. Although rare earth-based magnesium alloys show better mechanical properties, it is not economically viable to use these alloys in auto industries. Recently, many new Mg-Al based alloy systems have been developed for high temperature applications, which do not contain the Mg17Al12 phase. It has been proved that the addition of a high percentage of zinc (which depends upon the percentage of Al) to binary Mg-Al alloys also ensures the complete removal of the Mg17Al12 phase and hence exhibits superior high temperature properties.ZA84 alloy is one such system, which has 8%Zn in it (Mg-8Zn-4Al-0.2Mn, all are in wt %) and shows superior creep resistance compared to AZ and AM series alloys. These alloys are mostly used in die casting industries. However, there are certain large and heavy components, made up of this alloy by sand castings that show lower mechanical properties because of their coarse microstructure. Moreover, further improvement in their high temperature behaviour through microstructural modification is also an essential task to make this alloy suitable for the replacement of high strength aluminium alloys used in automobile industry. Grain refinement is an effective way to improve the tensile behaviour of engineering alloys. In fact, grain refinement of Mg-Al based alloys is well documented in literature. However, there is no grain refiner commercially available in the market for Mg-Al alloys. It is also reported in the literature that the microstructure of AZ91 alloy is modified through the minor elemental additions such as Sb, Si, Sr, Ca, etc., which enhance its high temperature properties because of the formation of new stable intermetallics. The same strategy can be used with the ZA84 alloy system to improve its high temperature properties further without sacrificing the other properties. The primary objective of the present research work, “Studies on grain refinement and alloying additions on the microstructure and mechanical properties of Mg-8Zn-4Al alloy” is twofold: 1. To investigate the role of individual and combined additions of Sb and Ca on the microstructure and mechanical properties of ZA84 alloy. 2. To synthesis a novel Mg-1wt%Al4C3 master alloy for grain refinement of ZA84 alloy and investigate its effects on mechanical properties.

Biopulping of Paddy Straw by Pleurotus eous

Biopulping being less energy intensive, inexpensive and causing lesser pollution, can be a viable alternative to chemical and mechanical pulping in paper and pulp industry. In view of shrinking forest reserves, agricultural residues are considered as an alternative raw material for making paper and board. By suitable treatment agriwaste can be converted into substrate for mushroom cultivation. Mushrooms of Pleurotus sp. can preferentially remove lignin from agriwaste with limited degradation to cellulose. The present study examines utilization of Pleurotus eous for biopulping of paddy straw by solid substrate fermentation. SMS, the mushroom growing medium that results from cultivation process, is a good source of fibre and can be pulped easily. Ligninases present in SMS were able to reduce lignin content to nearly half the initial amount by 21st day of cultivation. Highest cellulose content (% dry weight) was observed on 21st day, while cellulase production commenced from 28th day of cultivation. SEM images revealed that SMS fibres are still associated with non-cellulosic materials when compared to chemically (20% w/v NaOH) extracted fibres.

Physical and optical properties of phthalocyanine doped inorganic glasses

Physical and optical properties of various free base and metallic phthalocyanine (Pc) doped glass matrix are reported for the first time. Absorption spectral measurements of H2Pc, MnPc, NiPc, CoPc, CuPc, MoOPc, ZnPc and FePc doped borate glass matrix have been made in the 200–1100 nm region and the spectra obtained are analyzed in the 2.1–6.2 eV region to obtain the optical band gap (Eg) and the width of the band tail (Et). Other important optical and physical parameters viz. refractive index (n), molar extinction coefficient ("), density (½), glass transition temperature (Tg), molecular concentration (N ), polaron radius (rp), intermolecular separation (R), molar refractivity (Rm) are also reported

Physical and optical properties of phthalocyanine doped inorganic glasses

Physical and optical properties of various free base and metallic phthalocyanine (Pc) doped glass matrix are reported for the first time. Absorption spectral measurements of H2Pc, MnPc, NiPc, CoPc, CuPc, MoOPc, ZnPc and FePc doped borate glass matrix have been made in the 200–1100 nm region and the spectra obtained are analyzed in the 2.1–6.2 eV region to obtain the optical band gap (Eg) and the width of the band tail (Et). Other important optical and physical parameters viz. refractive index (n), molar extinction coefficient ("), density (½), glass transition temperature (Tg), molecular concentration (N ), polaron radius (rp), intermolecular separation (R), molar refractivity (Rm) are also reported.

Physical and optical properties of phthalocyanine doped inorganic glasses

Physical and optical properties of various free base and metallic phthalocyanine (Pc) doped glass matrix are reported for the first time. Absorption spectral measurements of H2Pc, MnPc, NiPc, CoPc, CuPc, MoOPc, ZnPc and FePc doped borate glass matrix have been made in the 200–1100 nm region and the spectra obtained are analyzed in the 2.1–6.2 eV region to obtain the optical band gap (Eg) and the width of the band tail (Et). Other important optical and physical parameters viz. refractive index (n), molar extinction coefficient ("), density (½), glass transition temperature (Tg), molecular concentration (N ), polaron radius (rp), intermolecular separation (R), molar refractivity (Rm) are also reported.

Non-destructive evaluation of photovoltaic materials and solar cells using Photoluminescence

Photoluminescence (PL) spectroscopy is an optical technique that has emerged successful in the field of semiconductor material and device characterization. This technique is quite a powerful one which gives idea about the defect levels in a material, the band gap of the material, composition as well as material quality. Over the recent years it has received an elevation as a mainstream characterization technique. This thesis is an attempt to characterize each individual layer used in a thin film solar cell with special focus on the electrical properties. This will be highly beneficial from the lab as well as industrial point of view because electrical measurements generally are contact mode measurements which tend to damage the surface. As far as a thin film solar cell is concerned, the constituent layers are the transparent conducting oxide (TCO), absorber layer, buffer layer and top electrode contact. Each layer has a specific role to play and the performance of a solar cell is decided and limited by the quality of each individual layer. Various aspects of PL spectroscopy have been employed for studying compound semiconductor thin films [deposited using chemical spray pyrolysis (CSP)] proposed for solar cell application. This thesis has been structured in to seven chapters

Nonlinear and magneto-optical transmission studies on magnetic nanofluids of non-interacting metallic nickel nanoparticles

Oxide free stable metallic nanofluids have the potential for various applications such as in thermal management and inkjet printing apart from being a candidate system for fundamental studies. A stable suspension of nickel nanoparticles of ∼5 nm size has been realized by a modified two-step synthesis route. Structural characterization by x-ray diffraction and transmission electron microscopy shows that the nanoparticles are metallic and are phase pure. The nanoparticles exhibited superparamagnetic properties. The magneto-optical transmission properties of the nickel nanofluid (Ni-F) were investigated by linear optical dichroism measurements. The magnetic field dependent light transmission studies exhibited a polarization dependent optical absorption, known as optical dichroism, indicating that the nanoparticles suspended in the fluid are non-interacting and superparamagnetic in nature. The nonlinear optical limiting properties of Ni-F under high input optical fluence were then analyzed by an open aperture z-scan technique. The Ni-F exhibits a saturable absorption at moderate laser intensities while effective two-photon absorption is evident at higher intensities. The Ni-F appears to be a unique material for various optical devices such as field modulated gratings and optical switches which can be controlled by an external magnetic field