Papers by Author: Ramesh Chandra Agarwala

Abstract: Since the introduction of Electroless (EL) coating in 1946 by Brenner and Riddle, the process has been the subject of steady growth. It is one of the most elegant methods available for the production of alloy coatings on surface. The technique involves the autocatalytic reduction, at the substrate/solution interface, of cations by EL bath released from suitable chemical reducing agents. EL coating technique is simple one, as can be manifested just by controlling pH and temperature of the coating bath. Such coatings are reported to provide excellent physical and mechanical properties. The electroless coatings are being studied at Indian Institute of Technology Roorkee since 1985. The structural and morphological behavior of Ni-P coatings for different phosphorous contents has been extensively studied. Sub-micron size coating islands and their transformations have been deduced. The metallography studies using hot stage within TEM to follow the phase transformations occurring at various temperatures have been studied for Ni-B EL coatings. The realization of mechanical bonding along with chemical bonding between EL coating and the substrate has been explained by coated copper on ceramic powder. As a forward step towards composite coatings, Ni-P-C, Ni-P-Al₂O₃, Ni-P-ZrO₂ has been developed by EL co-deposition technique. Ag-graphite coatings produced by EL technique exhibits nearly five times higher wear resistance and nearly two times better corrosion resistance apart from a good electrical conductor. The tribological behavior of electroless Ni-P-X and Ni-P coatings on steel and aluminium substrates in different conditions i.e., as coated, heat treated at various temperatures at different extents of time with different normal loads, have been studied in terms of dry sliding friction and wear against counter face of case hardened steel. In Ni-P-X nanocoating (X= ZrO₂-Al₂O₃-Al₃Zr), X has been produced in-situ and are of nanosize particles. Such coating could be done on carbon fibre of 7µ diameter uniformly. Ni-P-ferrite nanocoatings with thickness less than nearly 1mm thick, is exhibiting good absorption of microwave in the range of 12-18 GHz which can be exploited for radar applications. Micro-thickness coatings are paying ways to nanocoatings. Nanocoatings are the coatings in which either the thickness of the coating is in nanolevel or second phase that dispersed in the coat matrix is of nanosize. To further explore the field of EL nanocomposite coatings, now days, a work on EL Ni-P-ZnO, TiO₂, Al₂O₃, ZrO₂ and Ni-B-ZrO₂ for its mechanical properties has been carried out.

Abstract: M-type strontium hexaferrite nanocrystals of radar absorbing material (NRAM) i.e. SrFe12O19 were synthesized by modified flux method that combine the controlled chemical co-precipitation process for nucleation and complete uniform growth during annealing with NaCl flux. Uniform structural morphological transformation of nanocrystals from needle to hexagonal prism faces were noticed after annealing with increasing of heat treatment (HT) temperature from 800 to 1200°C for 4h. X-ray diffraction (XRD) results show the formation of various phases with increase in annealing temperature. The crystallinity and crystallite size are found to increase with increase in heat treatment temperature (15-40nm). The superparamagnetic behavior of strontium hexaferrite is confirmed by vibrating sample magnetometer (VSM) wherein it was noticed that magnetic field (10000 gauss max) did not have any effect on these materials. The transformation of magnetic properties i.e. from superparamagnetic to ferromagnetic behaviour after heating at various HT temperatures have been revealed by hysteresis loops under VSM study. The increase in saturation magnetization from 2.44 to 75.03 emu/gm is observed. Formation of ultrafine particles has been confirmed through field emission scanning electron microscope (FESEM). About 5 to10% of the needle like crystals in the ‘as synthesized’ condition were transformed to hexagonal pyramidal structure and most of the crystals are found to have plate like hexagonal structures with increase in heat treatment temperatures. The effect of such systematic morphological transformation of nanocrystals was observed in reflection loss properties in X band (8-12 GHz). The maximum reflection loss of -20.05, -24.31, -24.16, -25.22, -25.12, -24.01 dB at 8.1, 8.6, 9.2, 9.6, 10.7, and 12 GHz respectively are observed for the material heat treated at 1200°C. A significant increment from - 6.5 to -25.22 dB at 9.6 GHz in reflection loss (RL) is noticed due to symmetric morphological growth of RAM nanocrystal during annealing.

Abstract: Nanocrystalline strontium hexaferrite (SrFe12O19) and barium hexaferrite (BaFe12O19) powders were synthesized by co-precipitation method. The ‘as synthesized’ powders were heat treated (HT) at different temperatures ranging from 800 to 1200°C at a heating rate of 30°C /min in nitrogen atmosphere. Decomposition behaviour and the phases associated therein are investigated by thermal analysis (DTA/DTG/TG) and X-ray diffraction (XRD). Formations of ultrafine particles have been confirmed through field emission scanning electron microscop (FESEM). The superparamagnetic behavior of both, barium and strontium hexaferrite is confirmed by vibrating sample magnetometer (VSM). The increase in saturation magnetization from 1.94 to 31.05 emu/gm in case of barium hexaferrite and from 2.44 to 43.38 emu/gm for strontium hexaferrite is observed with HT temperatures. The changes in coercivity and remanence with HT temperatures for both the ferrites are analysed.

Abstract: Nano radar absorbing material (NRAM) i.e. BaMe2Fe16O27 (Me2+=Fe2+) powder (10 nm) is coated with amorphous Ni-P nano layer (5-10 nm) by using electroless (EL) technology to develop EL Ni-P/NRAM nanocomposite powder. The experimental processes parameters and EL Ni-P bath composition were optimized to obtain the deposition. As-deposited nanocomposite powder was microwave annealed (MWA) with increasing radiation power from 160 to 760 watts for 5 minutes. The surface morphology, elemental contents, phase transformation and magnetic properties of NRAM powders were examined under field emission scanning electron microscope (FESEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) respectively. Maximum reflection loss (RL) 33.75 dB at 15.80 GHz for nanocomposite powder MWA at 760 watt was obtained the absorption range under −15 dB is from 13.76 to 16.77 GHz with 2 mm thickness layer in Ku Band. Excellent microwave absorption properties due to accurate electromagnetic (EM) match in the nanocomposite microstructure, a strong natural resonance and multipolarization. Such (Ni+ Ni3P)/NRAM nanocomposite powders may be attractive candidates for EM absorption.

Abstract: High energy ball milling (HEBM) had been carried out to produce submicron size titanium aluminide intermetallics (TiAl) using elemental powders of Ti and Al alongwith Ni-P coated graphite. 1% graphite powders was added to stoichiometric composition of Ti48Al and ball milling was conducted for different milling time at varying rpm. The effect of milling time and rpm on particle size has been studied. The prepared samples have been characterized using X-ray diffraction, differential scanning calorimetry (DSC) and scaning elecron microscopy (SEM). Grain size as low as 500 nm could be achieved. Formation of Ti3Al, TiAl and carbon containing intermetallic compounds had been confirmed through X-ray diffraction. Milling time and rpm of mill is found to be important factors which control the final particle size.

Abstract: Single phase M-type barium hexaferrite nano radar absorbing material (NRAM) i.e., BaFe12O19 were synthesized by modified flux method that combines the controlled chemical co-precipitation process for nucleation and complete uniform growth during annealing with NaCl flux under microwave annealing (MWA) and vacuum annealing (VA). Uniform morphological transformation of nano crystals from spherical (~ 10 nm) to prism faces (~ 35 nm) were observed under TEM during annealing. The effect of such systematic nano morphological transformation of NRAM was observed on magnetic and reflection loss (RL) properties. Maximum reflection loss (RL) was improved to 37.15 dB at 16.00 GHz for MWA at 760 watt and 27.56 dB at 15.75 GHz for VA at 1200 oC with continuous increasing absorption range under −10 dB for 2 mm thick coating layer in the Ku Band (12.4-18.0 GHz).. Excellent microwave absorption properties are a consequence of accurate EM match in the nano morphological planes, a strong natural resonance, as well as multipolarization. This process of crystal growth, morphology evolution and RL enhancement with respect to the heat treatments were also explained in terms of Ostwald ripening and quantum size effect.

Abstract: Single phase W-type barium hexaferrite nano crystals of radar absorbing material (RAM) i.e., BaMe2Fe16O27 (Me2+=Fe2+) were synthesized by a modified flux method that combines the controlled chemical co-precipitation process for nucleation and complete uniform growth during in-situ annealing with NaCl flux under vacuum furnace. Uniform structure morphological transformation of nano crystals from spherical to prism faces were noticed after annealing with increasing temperatures from 200 to 1200 oC for 4 h in vacuum. XRD results showed the single phase nanocrystals of BaFe18O27 with increasing crystallanity and size from 10 to 90 nm during annealing. FESEM and TEM were used to investigate the systematic growth processes of various morphologies of nano crystals. The effect of such systematic morphological transformation of nanocrystals was observed in dielectric, dynamic magnetic and refection loss (RL) properties in Kuband (12.4 -18.0 GHz). A significant increment from -15.23 dB to -43.65 dB with wide range of bandwidth in RL loss is noticed due to the symmetric morphological growth of single phase nano crystals of RAM during annealing. This process of crystal growth, morphology evolution and RL enhancement with respect to increasing temperature were also explained in terms of ostwald ripening and quantum size effect.

Abstract: Since the introduction of Electroless (EL) coating in 1946 by Brenner and Riddle, the process has been the subject of steady growth. It is one of the most elegant methods available for the production of protective coatings on surface. The technique involves the autocatalytic reduction, at the substrate/solution interface, of cations released from suitable chemical reducing agents with in the EL bath. EL coating technique is simple one, as can be manifested just by controlling pH and temperature of the coating bath. Such coatings are reported to provide excellent physical and mechanical properties. The nickel, silver and copper based alloy and composite EL coatings are being studied at Indian Institute of Technology Roorkee since 1985 and this paper deals with the gist of the same. The structural behavior of Ni-P coatings for different phosphorus contents has been extensively studied. Transmission electron microscopy (TEM) and magnetic movement studies have been used as tools for structural and kinetic studies, respectively. Submicron size coating islands and their transformations have been deduced. The metallography studies using hot stage within TEM to follow the phase transformations occurring at various temperatures have been studied for Ni-B, EL coatings. As a forward step towards composite coatings, Ni-P-C, Ni-P-Al2O3, Ni-P-ZrO2 etc. have been developed by co-deposition techniques. Ag-graphite composite coatings produced by EL technique exhibits ~5 times higher wear resistance and ~ 2 times better corrosion resistance apart from being a good electrical conductor. The tribological behavior of EL Ni-P-X and Ni-P coatings on steel and aluminium substrates in different conditions i.e., as-coated, heat treated at various temperatures at different extents of time with different normal loads, have been studied in terms of dry sliding friction and wear against counter face of case hardened steel. In Ni-P-X nanocoatings (X= ZrO2-Al2O3-Al3Zr), X has been produced in-situ and are composed of nano-sized particles. Such coating could be produced uniformly on carbon fibre of 7µ diameter. Ni-P and Cu are also coated successfully on graphite/ oxide powders of ~ 120µ sizes. Micro-thickness coatings are paving ways to nanocoatings. These are the coatings in which either the thickness of the coating is in nano level or the second phase, that dispersed in the coating matrix is of nano-size. Ni-P-Ferrite nano coatings with thickness less than ~0.1mm thick, is found to exhibit about 20db of absorption of microwave in the rage of 12-18 GHz which can be exploited for radar applications. Here the nano-sized ferrite particles are co-deposited along with the Ni-P EL coatings.