Anomalous Thermal Behavior of CuxMg1-xNb2O6 (x=0,0.4,0.6,1) for LTCC Substrate

LTCC (Low Temperature Co-fired Ceramics) being the most advantageous technology towards the multilayer substrates for various applications, demands an extensive study of its raw materials. In the present work, a series of CuxMg1-xNb2O6 (x=0,0.4,0.6,1) has been prepared using sol-gel synthesis route and sintered at a temperature of 900°C to study its applicability for LTCC technology as the firing temperature is 900°C in this technology. The phase formation has been confirmed using X-ray Diffraction. Thermal properties like thermal conductivity and thermal expansion being very important aspect as the former defines the heat flow to avoid thermal instability in layers and the later provides the dimensional congruency of the dielectric material and the conductors, are studied here over high temperature up to the firing temperature. Although the values are quite satisfactory from substrate requirement point view, results have shown anomaly over temperature. The anomalous thermal behavior has been further analyzed using TG-DTA.

Dye-Sensitized Solar Cell by Plasma Spray

This paper aims to scale up Dye-sensitized Solar Cell (DSSC) production using a commonly available industrial material – stainless steel - and industrial plasma equipment. A working DSSC electrode formed by (1) coating titania nanotube (TiO2 NT) film on 304 stainless steel substrate using a plasma spray technique; then, (2) filling the nano-pores of the TiO2 NT film using a TiF4 sol-gel method. A DSSC device consists of an anode absorbed photosensitive dye (N3), a transparent conductive cathode with platinum (Pt) nano-catalytic particles adhered to its surface, and an electrolytic solution sealed between the anode and the transparent conductive cathode. The photo-current conversion efficiency of the DSSC sample was tested under an AM 1.5 Solar Simulator. The sample has a short current (Isc) of 0.83 mA cm-2, open voltage (Voc) of 0.81V, filling factor (FF) of 0.52, and conversion efficiency (η) of 2.18% on a 0.16 cm2 DSSC work-piece.

Lipase Catalyzed Synthesis of Aromatic Esters of Sugar Alcohols

Commercially available lipases (Candida antarctica lipase B, Novozyme 435, Thermomyces lanuginosus lipase, and Lipozyme TL IM), as well as sol-gel immobilized lipases, have been screened for their ability to acylate regioselectively xylitol, sorbitol, and mannitol with a phenolic ester in a binary mixture of t-butanol and dimethylsulfoxide. HPLC and MALDI-TOF MS analysis revealed the exclusive formation of monoesters for all studied sugar alcohols. The lipases immobilized by the sol-gel entrapment method proved to be efficient catalysts, leading to high conversions (up to 60%) in the investigated acylation reactions. From a sequence of silane precursors with different nonhydrolyzable groups in their structure, the presence of octyl and i-butyl group was most beneficial for the catalytic activity of sol-gel entrapped lipases in the studied process.

A Matrix Evaluation Model for Sustainability Assessment of Manufacturing Technologies

Technology assessment is a vital part of decision process in manufacturing, particularly for decisions on selection of new sustainable manufacturing processes. To assess these processes, a matrix approach is introduced and sustainability assessment models are developed. Case studies show that the matrix-based approach provides a flexible and practical way for sustainability evaluation of new manufacturing technologies such as those used in surface coating. The technology assessment of coating processes reveals that compared with powder coating, the sol-gel coating can deliver better technical, economical and environmental sustainability with respect to the selected sustainability evaluation criteria for a decorative coating application of car wheels.

Structural and Electrical Properties of BNT-BT0.08 Ceramics Processed by Spark Plasma Sintering

(Bi0.5Na0.5)TiO3 doped with 8 mol % BaTiO3 powder (BNT-BT0.08), prepared by sol-gel method was compacted and sintered by Spark Plasma Sintering (SPS) process. The influence of SPS temperature on the densification of BNT-BT0.08 ceramic was investigated. Starting from sol-gel nanopowder of BNT-BT containing 8 mol % BaTiO3 with an average particles size of about 30 nm, were obtained ceramics with density around 98 % of the theoretical density value when the SPS temperature used was about 850 °C. The average grain size of the resulting ceramics was 80 nm. The BNT-BT0.08 ceramic sample obtained by SPS method has shown good electric properties at various frequencies.

Synthesis of Peptide Amides using Sol-Gel Immobilized Alcalase in Batch and Continuous Reaction System

Two commercial proteases from Bacillus licheniformis (Alcalase 2.4 L FG and Alcalase 2.5 L, Type DX) were screened for the production of Z-Ala-Phe-NH2 in batch reaction. Alcalase 2.4 L FG was the most efficient enzyme for the C-terminal amidation of Z-Ala-Phe-OMe using ammonium carbamate as ammonium source. Immobilization of protease has been achieved by the sol-gel method, using dimethyldimethoxysilane (DMDMOS) and tetramethoxysilane (TMOS) as precursors (unpublished results). In batch production, about 95% of Z-Ala-Phe-NH2 was obtained at 30°C after 24 hours of incubation. Reproducibility of different batches of commercial Alcalase 2.4 L FG preparations was also investigated by evaluating the amidation activity and the entrapment yields in the case of immobilization. A packed-bed reactor (0.68 cm ID, 15.0 cm long) was operated successfully for the continuous synthesis of peptide amides. The immobilized enzyme retained the initial activity over 10 cycles of repeated use in continuous reactor at ambient temperature. At 0.75 mL/min flow rate of the substrate mixture, the total conversion of Z-Ala-Phe-OMe was achieved after 5 hours of substrate recycling. The product contained about 90% peptide amide and 10% hydrolysis byproduct.

Double Immobilized Lipase for the Kinetic Resolution of Secondary Alcohols

Sol-gel immobilization of enzymes, which can improve considerably their properties, is now one of the most used techniques. By deposition of the entrapped lipase on a solid support, a new and improved biocatalyst was obtained, which can be used with excellent results in acylation reactions. In this paper, lipase B from Candida antarctica was double immobilized on different adsorbents. These biocatalysts were employed in the kinetic resolution of several aliphatic secondary alcohols in organic medium. High total recovery yields of enzymatic activity, up to 560%, were obtained. For all the studied alcohols the enantiomeric ratios E were over 200. The influence of the reaction medium was studied for the kinetic resolution of 2-pentanol.

New SUZ-4 Zeolite Membrane from Sol-Gel Technique

A new SUZ-4 zeolite membrane with tetraethlyammonium hydroxide as the template was fabricated on mullite tube via hydrothermal sol-gel synthesis in a rotating autoclave reactor. The suitable synthesis condition was SiO2:Al2O3 ratio of 21.2 for 4 days at 155 °C crystallization under autogenous pressure. The obtained SUZ-4 possessed a high BET surface area of 396.4 m2/g, total pore volume at 2.611 cm3/g, and narrow pore size distribution with 97 nm mean diameter and 760 nm long of needle crystal shape. The SUZ-4 layer obtained from seeding crystallization was thicker than that of without seeds or in situ crystallization.

Efficiency Improvements of GaAs-based Solar Cells by Hydrothermally-deposited ZnO Nanostructure Array

ZnO nanostructures including nanowires, nanorods, and nanoneedles were successfully deposited on GaAs substrates, respectively, by simple two-step chemical method for the first time. A ZnO seed layer was firstly pre-coated on the O2-plasma treated substrate by sol-gel process, followed by the nucleation of ZnO nanostructures through hydrothermal synthesis. Nanostructures with different average diameter (15-250 nm), length (0.9-1.8 μm), density (0.9-16×109 cm-2) were obtained via adjusting the growth time and concentration of precursors. From the reflectivity spectra, we concluded ordered and taper nanostructures were preferential for photovoltaic applications. ZnO nanoneedles with an average diameter of 106 nm, a moderate length of 2.4 μm, and the density of 7.2×109 cm-2 could be synthesized in the concentration of 0.04 M for 18 h. Integrated with the nanoneedle array, the power conversion efficiency of single junction solar cell was increased from 7.3 to 12.2%, corresponding to a 67% improvement.

Li4SiO4 Prepared by Sol-gel Method as Potential Host for LISICON Structured Solid Electrolytes

In this study, Li4SiO4 powder was successfully synthesized via sol gel method followed by drying at 150oC. Lithium oxide, Li2O and silicon oxide, SiO2 were used as the starting materials with citric acid as the chelating agent. The obtained powder was then sintered at various temperatures. Crystallographic phase analysis, morphology and ionic conductivity were investigated systematically employing X-ray diffraction, Fourier Transform Infrared, Scanning Electron Microscopy and AC impedance spectroscopy. XRD result showed the formation of pure monoclinic Li4SiO4 crystal structure with lattice parameters a = 5.140 Å, b = 6.094 Å, c = 5.293 Å, β = 90o in the sample sintered at 750oC. This observation was confirmed by FTIR analysis. The bulk conductivity of this sample at room temperature was 3.35 × 10-6 S cm-1 and the highest bulk conductivity of 1.16 × 10-4 S cm-1 was obtained at 100°C. The results indicated that, the Li4SiO4 compound has potential to be used as host for LISICON structured solid electrolyte for low temperature application.

Development of a Porous Silica Film by Sol-gel Process

In the present work homogeneous silica film on silicon was fabricated by colloidal silica sol. The silica sol precursor with uniformly granular particle was derived by the alkaline hydrolysis of tetraethoxyorthosilicate (TEOS) in presence of glycerol template. The film was prepared by dip coating process. The templated hetero-structured silica film was annealed at elevated temperatures to generate nano- and meso porosity in the film. The film was subsequently annealed at different temperatures to make it defect free and abrasion resistant. The sol and the film were characterized by the measurement of particle size distribution, scanning electron microscopy, XRD, FTIR spectroscopy, transmission electron microscopy, atomic force microscopy, measurement of the refractive index, thermal conductivity and abrasion resistance. The porosity of the films decreased whereas refractive index and dielectric constant of it `increased with the increase in the annealing temperature. The thermal conductivity of the films increased with the increase in the film thickness. The developed porous silica film holds strong potential for use in different areas.

Physical and Electrical Characterization of ZnO Thin Films Prepared by Sol-Gel Method

In this paper, Zinc Oxide (ZnO) thin films are deposited on glass substrate by sol-gel method. The ZnO thin films with well defined orientation were acquired by spin coating of zinc acetate dehydrate monoethanolamine (MEA), de-ionized water and isopropanol alcohol. These films were pre-heated at 275°C for 10 min and then annealed at 350°C, 450°C and 550°C for 80 min. The effect of annealing temperature and different thickness on structure and surface morphology of the thin films were verified by Atomic Force Microscopy (AFM). It was found that there was a significant effect of annealing temperature on the structural parameters of the films such as roughness exponent, fractal dimension and interface width. Thin films also were characterizied by X-ray Diffractometery (XRD) method. XRD analysis revealed that the annealed ZnO thin films consist of single phase ZnO with wurtzite structure and show the c-axis grain orientation. Increasing annealing temperature increased the crystallite size and the c-axis orientation of the film after 450°C. Also In this study, ZnO thin films in different thickness have been prepared by sol-gel method on the glass substrate at room temperature. The thicknesses of films are 100, 150 and 250 nm. Using fractal analysis, morphological characteristics of surface films thickness in amorphous state were investigated. The results show that with increasing thickness, surface roughness (RMS) and lateral correlation length (ξ) are decreased. Also, the roughness exponent (α) and growth exponent (β) were determined to be 0.74±0.02 and 0.11±0.02, respectively.

Acoustic Study on the Interactions of Coconut Oil Based Copper Oxide Nanofluid

Novel Coconut oil nanofluids of various concentrations have been prepared through ultrasonically assisted sol-gel method. The structural and morphological properties of the copper oxide nanoparticle have been analyzed with respectively and it revealed the monoclinic end-centered structure of crystallite and shuttle like flake morphology of agglomerates. Ultrasonic studies have been made for the nanofluids at different temperatures. The molecular interactions responsible for the changes in acoustical parameter with respect to concentration and temperature are discussed.

Rapid Determination of Biochemical Oxygen Demand

Biochemical Oxygen Demand (BOD) is a measure of the oxygen used in bacteria mediated oxidation of organic substances in water and wastewater. Theoretically an infinite time is required for complete biochemical oxidation of organic matter, but the measurement is made over 5-days at 20 0C or 3-days at 27 0C test period with or without dilution. Researchers have worked to further reduce the time of measurement. The objective of this paper is to review advancement made in BOD measurement primarily to minimize the time and negate the measurement difficulties. Survey of literature review in four such techniques namely BOD-BARTTM, Biosensors, Ferricyanidemediated approach, luminous bacterial immobilized chip method. Basic principle, method of determination, data validation and their advantage and disadvantages have been incorporated of each of the methods. In the BOD-BARTTM method the time lag is calculated for the system to change from oxidative to reductive state. BIOSENSORS are the biological sensing element with a transducer which produces a signal proportional to the analyte concentration. Microbial species has its metabolic deficiencies. Co-immobilization of bacteria using sol-gel biosensor increases the range of substrate. In ferricyanidemediated approach, ferricyanide has been used as e-acceptor instead of oxygen. In Luminous bacterial cells-immobilized chip method, bacterial bioluminescence which is caused by lux genes was observed. Physiological responses is measured and correlated to BOD due to reduction or emission. There is a scope to further probe into the rapid estimation of BOD.

Kinetics of Palm Oil Cracking in Batch Reactor

The kinetics of palm oil catalytic cracking over aluminum containing mesoporous silica Al-MCM-41 (5% Al) was investigated in a batch autoclave reactor at the temperatures range of 573 – 673 K. The catalyst was prepared by using sol-gel technique and has been characterized by nitrogen adsorption and x-ray diffraction methods. Surface area of 1276 m2/g with average pore diameter of 2.54 nm and pore volume of 0.811 cm3/g was obtained. The experimental catalytic cracking runs were conducted using 50 g of oil and 1 g of catalyst. The reaction pressure was recorded at different time intervals and the data were analyzed using Levenberg- Marquardt (LM) algorithm using polymath software. The results show that the reaction order was found to be -1.5 and activation energy of 3200 J/gmol.

Influence of Taguchi Selected Parameters on Properties of CuO-ZrO2 Nanoparticles Produced via Sol-gel Method

The present paper discusses the selection of process parameters for obtaining optimal nanocrystallites size in the CuOZrO2 catalyst. There are some parameters changing the inorganic structure which have an influence on the role of hydrolysis and condensation reaction. A statistical design test method is implemented in order to optimize the experimental conditions of CuO-ZrO2 nanoparticles preparation. This method is applied for the experiments and L16 orthogonal array standard. The crystallites size is considered as an index. This index will be used for the analysis in the condition where the parameters vary. The effect of pH, H2O/ precursor molar ratio (R), time and temperature of calcination, chelating agent and alcohol volume are particularity investigated among all other parameters. In accordance with the results of Taguchi, it is found that temperature has the greatest impact on the particle size. The pH and H2O/ precursor molar ratio have low influences as compared with temperature. The alcohol volume as well as the time has almost no effect as compared with all other parameters. Temperature also has an influence on the morphology and amorphous structure of zirconia. The optimal conditions are determined by using Taguchi method. The nanocatalyst is studied by DTA-TG, XRD, EDS, SEM and TEM. The results of this research indicate that it is possible to vary the structure, morphology and properties of the sol-gel by controlling the above-mentioned parameters.

Electrical Properties of n-CdO/p-Si Heterojunction Diode Fabricated by Sol Gel

n-CdO/p-Si heterojunction diode was fabricated using sol-gel spin coating technique which is a low cost and easily scalable method for preparing of semiconductor films. The structural and morphological properties of CdO film were investigated. The X-ray diffraction (XRD) spectra indicated that the film was of polycrystalline nature. The scanning electron microscopy (SEM) images indicate that the surface morphology CdO film consists of the clusters formed with the coming together of the nanoparticles. The electrical characterization of Au/n-CdO/p–Si/Al heterojunction diode was investigated by current-voltage. The ideality factor of the diode was found to be 3.02 for room temperature. The reverse current of the diode strongly increased with illumination intensity of 100 mWcm-2 and the diode gave a maximum open circuit voltage Voc of 0.04 V and short-circuits current Isc of 9.92×10-9 A.

Development of Quasi-Two-Dimensional Nb2O5 for Functional Electrodes of Advanced Electrochemical Systems

In recent times there has been a growing interest in the development of quasi-two-dimensional niobium pentoxide (Nb2O5) as a semiconductor for the potential electronic applications such as capacitors, filtration, dye-sensitised solar cells and gas sensing platforms. Therefore once the purpose is established, Nb2O5 can be prepared in a number of nano- and sub-micron-structural morphologies that include rods, wires, belts and tubes. In this study films of Nb2O5 were prepared on gold plated silicon substrate using spin-coating technique and subsequently by mechanical exfoliation. The reason this method was employed was to achieve layers of less than 15nm in thickness. The sintering temperature of the specimen was 800oC. The morphology and structural characteristics of the films were analyzed by Atomic Force Microscopy (AFM), Raman Spectroscopy, X-ray Photoelectron Spectroscopy (XPS).

Silver Modified TiO2/Halloysite Thin Films for Decontamination of Target Pollutants

 Sol-gel method has been used to fabricate nanocomposite films on glass substrates composed halloysite clay mineral and nanocrystalline TiO2. The methodology for the synthesis involves a simple chemistry method utilized nonionic surfactant molecule as pore directing agent along with the acetic acid-based solgel route with the absence of water molecules. The thermal treatment of composite films at 450oC ensures elimination of organic material and lead to the formation of TiO2 nanoparticles onto the surface of the halloysite nanotubes. Microscopy techniques and porosimetry methods used in order to delineate the structural characteristics of the materials. The nanocomposite films produced have no cracks and active anatase crystal phase with small crystallite size were deposited on halloysite nanotubes. The photocatalytic properties for the new materials were examined for the decomposition of the Basic Blue 41 azo dye in solution. These, nanotechnology based composite films show high efficiency for dye’s discoloration in spite of different halloysite quantities and small amount of halloysite/TiO2 catalyst immobilized onto glass substrates. Moreover, we examined the modification of the halloysite/TiO2 films with silver particles in order to improve the photocatalytic properties of the films. Indeed, the presence of silver nanoparticles enhances the discoloration rate of the Basic Blue 41 compared to the efficiencies obtained for unmodified films.

Sonochemically Prepared SnO2 Quantum Dots as a Selective and Low Temperature CO Sensor

In this study, a low temperature sensor highly selective to CO in presence of methane is fabricated by using 4 nm SnO2 quantum dots (QDs) prepared by sonication assisted precipitation. SnCl4 aqueous solution was precipitated by ammonia under sonication, which continued for 2 h. A part of the sample was then dried and calcined at 400°C for 1.5 h and characterized by XRD and BET. The average particle size and the specific surface area of the SnO2 QDs as well as their sensing properties were compared with the SnO2 nano-particles which were prepared by conventional sol-gel method. The BET surface area of sonochemically as-prepared product and the one calcined at 400°C after 1.5 hr are 257 m2/gr and 212 m2/gr respectively while the specific surface area for SnO2 nanoparticles prepared by conventional sol-gel method is about 80m2/gr. XRD spectra revealed pure crystalline phase of SnO2 is formed for both as-prepared and calcined samples of SnO2 QDs. However, for the sample prepared by sol-gel method and calcined at 400°C SnO crystals are detected along with those of SnO2. Quantum dots of SnO2 show exceedingly high sensitivity to CO with different concentrations of 100, 300 and 1000 ppm in whole range of temperature (25- 350°C). At 50°C a sensitivity of 27 was obtained for 1000 ppm CO, which increases to a maximum of 147 when the temperature rises to 225°C and then drops off while the maximum sensitivity for the SnO2 sample prepared by the sol-gel method was obtained at 300°C with the amount of 47.2. At the same time no sensitivity to methane is observed in whole range of temperatures for SnO2 QDs. The response and recovery times of the sensor sharply decreases with temperature, while the high selectivity to CO does not deteriorate.