Magnetic Field and Displacement Sensor Based on Giant Magneto-Impedance Effect

A two-core transducer assembly using a Fe_73.5Nb₃Cu₁Si_13.5B₉ ribbon to detect a change of magnetic field is proposed and tested for displacement (linear and angular) and current sensor. Two identical inductors, with the ribbon as core, are part of a two-series resonance network, and are in a high impedance state when excited by a small AC field of 1 MHz in the absence of a DC biasing field (H_dc). When the magnetic state of one inductor is altered by the biasing field, produced by a bar magnet or current carrying coil, an AC signal proportional to H_dc is generated by the transducer. The results for the sensitivity and linearity with displacement (linear and angular) of a magnet and with field from the current carrying coil are presented for two particular configurations of the transducer. High sensitivities of voltage response as much as 12 µV/µm and 3 mV/degree have been obtained for the transducer as a linear and angular displacement sensor, respectively, in the transverse configuration of exciting AC and biasing DC fields.     

Thermolysis and Photolysis of C60 Diozonides

Ozonation of C₆₀ in o-xylene produced three C₆₀(O₃)₂ diozonides that were separated from one another and from two C₆₀(O₃)₃ triozonides by High Performance Liquid Chromatography (HPLC). Upon thermolysis at 10, 15, and 16.6°C, each of the diozonides dissociated sequentially, first to a C₆₀O(O₃) oxyozonide, then to a C₆₀O₂ diepoxide. The three diepoxides were stable in solution for at least 3 weeks. The mean lifetimes of the three diozonides were 52 ± 5, 62 ± 6, and 17.3 ± 1.8 min, respectively (all at 15°C). The mean lifetimes of the three oxyozonides were 69.7 ± 0.7 and 58 ± 6 min at 16.6°C, respectively and about 240 min at 10°C. Photolysis of the diozonides yielded two dioxidoannulenes with UV-Vis adsorption maxima at 333 and 332 nm, and what appeared to be an epoxide-oxidoannulene with UV-Vis adsorption maximum at 327 nm. These annulenes were observed to form dimers. We have synthesized and characterized six C₆₀O₂ dioxides, at least three and possibly four of which were hitherto unknown. We report the discovery of oxyozonides that form during the dissociation of diozonides.     

Transparent conducting F-doped SnO2 thin films grown by pulsed laser deposition

Transparent conducting fluorine-doped tin oxide (SnO₂:F) films have been deposited on glass substrates by pulsed laser deposition. The structural, electrical and optical properties of the SnO₂:F films have been investigated as a function of F-doping level and substrate deposition temperature. The optimum target composition for high conductivity was found to be 10 wt.% SnF₂ + 90 wt.% SnO₂. Under optimized deposition conditions (T_s = 300 °C, and 7.33 Pa of O₂), electrical resistivity of 5 × 10^− 4 Ω-cm, sheet resistance of 12.5 Ω/□, average optical transmittance of 87% in the visible range, and optical band-gap of 4.25 eV were obtained for 400 nm thick SnO₂:F films. Atomic force microscopy measurements for these SnO₂:F films indicated that their root-mean-square surface roughness ( 6 Å) was superior to that of commercially available chemical vapor deposited SnO₂:F films ( 85 Å).     

Low temperature metal oxide film deposition and reaction kinetics in supercritical carbon dioxide

An effective method is developed for low temperature metal oxide deposition through thermal decomposition of metal diketonates in supercritical carbon dioxide (scCO₂) solvent. The rates of Al(acac)₃ (Aluminum acetyl acetonate) and Ga(acac)₃ (Gallium acetyl acetonate) thermal decomposition in scCO₂ to form conformal Al₂O₃ and Ga₂O₃ thin films on planar surfaces were investigated. The thermal decomposition reaction of Al(acac)₃ and Ga(acac)₃ was found to be initialized at  150 °C and 160 °C respectively in scCO₂ solvent, compared to  250 °C and 360 °C in analogous vacuum-based processes. By measuring the temperature dependence of the growth rates of metal oxide thin films, the apparent activation energy for the thermal decomposition of Al(acac)₃ in scCO₂ is found to be 68 ± 6 kJ/mol, in comparison with 80–100 kJ/mol observed for the corresponding vacuum-based thermal decomposition reaction. The enhanced thermal decomposition rate in scCO₂ is ascribed to the high density solvent which effectively reduces the energy of the polar transition states in the reaction pathway. Preliminary results of thin film deposition of other metal oxides including ZrO_x, FeO_x, Co₂O₃, Cr₂O₃, HfO_x from thermal decomposition of metal diketonates or fluorinated diketonates in scCO₂ are also presented.     

Controllable formation of Er–Yb codoped Al2O3 films by the non-aqueous sol–gel method

1 mol%Er³⁺–10 mol%Yb³⁺ codoped Al₂O₃ thin films have been prepared on thermally oxidized SiO₂/Si(110) substrates by a dip-coating process in the non-aqueous sol–gel method from the hydrolysis of aluminum isopropoxide [Al(OC₃H₇)₃] under isopropanol environment. Addition of N,N-dimethylformamide (DMF) as a drying control chemical additive (DCCA) into the sol suppresses formation of the cracks in the Er³⁺–Yb³⁺ codoped Al₂O₃ thin films when the rare-earth ion is doped with a high doping concentration. Homogeneous, smooth and crack-free Er³⁺–Yb³⁺ codoped Al₂O₃ thin films form at the conditions by a molar ratio of 1:1 for DMF:Al(OC₃H₇)₃. A strong photoluminescence spectrum with a broadband extending from 1.400 to 1.700 µm centered at 1.533 µm is obtained for the Er³⁺–Yb³⁺ codoped Al₂O₃ thin films, which is unrelated to the addition of DMF. Controllable formation of the Er³⁺–Yb³⁺ codoped Al₂O₃ thin films may be explained by the fact that the DMF assisted the deprotonation process of Al–OH at the surfaces of gel particles, resulting in enhancement of the degree of polymerization of sols and improvement of the mechanical properties of gel thin films.     

Kinetics of Carbon Multi-wall Nanotube Synthesis by Catalytic Pyrolysis of Methane

By method of isothermal gravimetry at 600-700°C, CH₄ concentration 32-100% in Ar and 91-100% in H₂ under atmospheric pressure the kinetics of CH₄ pyrolysis under Ni/La₂O₃ catalysts is studied. Estimated apparent activation energy of reaction is 73 kJ/mol for fresh catalyst and 71 kJ/mol for aged one. The reaction order on CH₄ changes from 1.05 at 600°C to 1.3 at 700°C. The influence of H₂ concentration on the reaction rate is more complicated. On the basis of kinetics measurements continuously working laboratory-scale reactor with gas and catalyst counter-flow is constructed and tested.     

Piroxicam benzoate--synthesis,HPLC determination,and hydrolysis

An improved method of piroxicam benzoate synthesis was described, and an isocratic reversed-phase high-performance liquid chromatography method for its determination was developed and fully validated. The method was found to be specific, precise (relative standard deviation 0.3%), accurate (mean recovery 99.9%), and robust. Limit of detection was estimated at 0.055 µg mL^-1 and limit of quantification at 0.185 µg mL^-1. The kinetics of piroxicam benzoate hydrolysis in aqueous buffer solutions (pH 1.1 and 10), simulated gastric and intestinal fluids was studied. The hydrolysis followed first-order kinetics. The following rate constants were obtained at pH 10: k = 1.8 × 10^-3 hr^-1 at 37°C and k = 3.4 × 10^-2 hr^-1 at 60°C. In acidic media, no significant hydrolysis was observed after 24 hr. During the 24-hr period in simulated intestinal fluid, only 10.9% of the starting ester was hydrolyzed.     

Atmospheric plasma discharge chemical vapor deposition of SnOx thin films using various tin precursors

A series of 0.2–0.6 μm thick SnO_x films were deposited onto borosilicate and sodalime silica glass substrates by atmospheric plasma discharge chemical vapor deposition at 80 °C. SnO_x films deposited from monobutyltin trichloride contained a large percentage of SnCl₂:2H₂O, and therefore were partially soluble in water. SnO_x coatings deposited from tetrabutyltin were not soluble in water or organic solvents, had good adhesion even at growth rates as high as 2.3 nm/s, had high transparency of  90% and electrical resistivity of 10⁷ Ω cm. As-grown tin oxide coatings were amorphous with a small concentration of SnO₂, SnO and Sn crystalline phases as determined by grazing angle X-ray diffraction and X-ray photoelectron spectroscopy measurements. Upon annealing in air at 600 °C the resistivity of SnO_x films decreased to 5–7 Ω cm. Furthermore, optical and X-ray measurements indicated that SnO_x was converted into SnO₂ (cassiterite) with a direct band gap of 3.66 eV. Annealing of as-grown SnO_x films in vacuum at 340 °C led to formation of the p-type conductor SnO/SnO_x. The indirect band gap of SnO was calculated from the optical spectra to be 0.3 eV.     

Porous Titania Thin Films Grown by Anodic Oxidation for Hydrogen Sensors

Porous titanium dioxide (Titania) thin films were grown by anodic oxidation using high purity (99.7%) titanium foil in a dilute sulphuric acid (1 M) medium. The anodization process was carried out for 30 minutes with 20 mA/cm² and 50 mA/cm² current densities. The samples were characterized by XRD, SEM, and AFM techniques. It was found that the grown porous titania films were less sensitive to 500 ppm hydrogen in air ambient below 300°C; however, the sensitivity and response behavior of the film at 300°C are very much dependent on the growth conditions. Particularly, the films grown at current density 50 mA/cm² and 1 M acid concentration exhibited the lowest response time of 151 sec at 300°C.     

MASS TRANSFER OF SULFUR DIOXIDE TO CONDENSING AQUEOUS AEROSOLS

Sodium chloride aerosols were generated from a 1.0 percent solution and passed through a tubular furnace, then recondensed at 29°C in a cooling section in the presence of SO₂. The dry particles ranged from 0.711 to 0.843 µm and the condensed droplets were in the 1.66 to 2.88 µm range. Final droplet size was varied by controlling the temperature of the nebulizer solution between 17 and 50°C. The SO₂ concentration in the gas phase of the condensing cloud was varied between 0.5x10 - ³ and 2.5 xl0 - ³ atm.

Cloud droplets were separated from the gas stream in a point-to-plane electrostatic precipitator and the droplets analyzed colorimetrically for total sulfur content.

Concentrations of SO₂ in the aqueous phase were about one order of magnitude greater than values obtained from equilibrium constants. The collection rate of SO₂ at 29°C appeared to be first order in SO₂ gas phase concentrations.

A model for this process was constructed, based on the hydrate formation in the gas-water interface[SO₂]_g + n[H₂O]ℓ ⇋ [SO₂ · n(H₂O)]ℓ

The order of the hydrate n was estimated to be 4.0.     

Surface Preparation of Aluminum Nitride for Metallization: Effect of Temperature on Surface Reactivity

The current aqueous cleaning step in the surface preparation of aluminum nitride (AlN) prior to metallization causes performance and reliability issues for the substrates used for microelectronic packaging due to surface reactions. These issues limit the use of AlN and its replacing of BeO, an environmentally hazardous material currently used. The aim of this investigation was to determine the effects of different solutions on the surface of AlN substrates under varying conditions at times up to 2419.2 ks (28 days). Concentration of the solutions, temperature, and immersion time were varied for the AlN samples in the solutions. Both elevated temperatures (50°C and 90°C) and low temperatures (5°C) were investigated.

Four general types of behavior were observed: minor changes in average surface roughness and microstructure, linear change in average surface roughness and pitted grains, nonlinear change in average surface roughness and product formation on AlN surface, and miscellaneous change in average surface roughness with surface product formation.

The surface roughening kinetics were very complex due to changes in both the reaction product morphology and reaction mechanism with temperature, solvent, and pH for a specific solvent. Minor changes in average surface roughness and microstructure were observed for HCl pH = 5, H₂ SO₄ pH = 5, NaOH pH = 8, NaOH pH = 10, NaOH pH = 12, deionized water and Alfred tap water at 5°C, HCl pH = 3 and oleic acid at 50°C and citric acid and oleic acid at 90°C. Linear changes in average surface roughness and pitted grains were observed for HCl pH = 2 and H₂SO₄ pH = 3 at 50°C and HCl pH = 2, H₂SO₄ pH = 3, and deionized water at 90°C. Non-linear change in average surface roughness and product formation on AlN surface was observed for HCl pH = 5, NaOH pH = 8 and Alfred tap water at 50°C and HCl pH = 5 and H₂SO₄ pH = 2 at 90°C. Miscellaneous changes in average surface roughness with surface product formation were observed for H₂SO₄ pH = 2, H₂SO₄ pH = 5, NaOH pH = 10, NaOH pH = 12, citric acid, Micro-90 and deionized water at 50°C and HCl pH = 3, H₂SO₄ pH = 5, NaOH pH = 8, NaOH pH = 10, NaOH pH = 12, Micro-90 and Alfred tap water at 90°C.     

AC impedance spectroscopy of porous silicon thin films containing metallic cations

Thin porous silicon (PS) films were prepared by HF/HNO₃ vapor etching on silicon wafers. The infiltration of metallic cations inside the porous silicon matrix followed by slow heating in air leads to an interesting electrical and optical physical phenomena. Al³⁺, Cu⁺, K⁺, Li⁺ metallic cations as chloride or as nitrate solutions are infiltrated inside the silicon porous matrix. After annealing in air at 500 °C during 2 h a structure was achieved in order to measure the Nyquist diagram corresponding to the cations embedded in PS/silicon. The real and imaginary parts of the whole structure depend on the voltage bias and on the frequency. Those signify that the junction is a Schotky-barrier junction.

From the variation of Ln(σT) versus absolute temperature T, where σ is the conductivity, we have deduced the activation energy of the metallic impurities in the [100 °C–400 °C] temperature range. We have found that the activation energies are of about 0.19 eV, 0.25 eV, 0.49 eV and 0.71 eV for Cu⁺, K⁺, Al³⁺ and Li⁺ cations respectively. These kinds of structures are suitable for gas sensing, optical sensing or for the fabrication of fuel cell membranes.     

Electrochromic properties of nanocrystalline MoO3 thin films

Electrochromic MoO₃ thin films were prepared by a sol–gel spin-coating technique. The spin-coated films were initially amorphous; they were calcined, producing nanocrystalline MoO₃ thin films. The effects of annealing temperatures ranging from 100 °C to 500 °C were investigated. The electrochemical and electrochromic properties of the films were measured by cyclic voltammetry and by in-situ optical transmittance techniques in 1 M LiClO₄/propylene carbonate electrolyte. Experimental results showed that the transmittance of MoO₃ thin films heat-treated at 350 °C varied from 80% to 35% at λ = 550 nm (ΔT =  45%) and from 86% to 21% at λ ≥ 700 nm (ΔT =  65%) after coloration. Films heat-treated at 350 °C exhibited the best electrochromic properties in the present study.     

Acrylate-based transdermal therapeutic system of nitrendipine

The objective of the present research investigation was to fabricate an acrylate-based transdermal therapeutic system (TTS) of nitrendipine, which could deliver drug at maximum input rate so as to deliver drug in minimum patch size. Transdermal patches were fabricated using synthesized acrylate pressure-sensitive adhesives (PSAs): PSA1, PSA2, and commercially available PSA3 and PSA4 using d-limonene as permeation enhancer. Effect of concentration of d-limonene on permeation kinetics of nitrendipine in PSAs was studied. Fabricated TTS in mentioned PSAs were evaluated for in-vitro release and permeation kinetics through guinea-pig skin. Cumulative release of drug in PSA1, PSA2, PSA3, and PSA4 was observed to be 45%, 40%, 25%, and 25%, respectively, upto 24 hr. Flux of drug through guinea-pig skin calculated at 48 hr in PSA1, PSA2, PSA3, and PSA4, with and without d-limonene, was observed to be 0.346 ± 0.10, 0.435 ± 0.17, 0.410 ± 0.17, and 0.162 ± 0.06, and 0.625 ± 0.19, 1.161 ± 0.46, 0.506 ± 0.17, and 0.520 ± 0.18 (µg/cm²/hr), respectively. The TTS in PSA2 showed comparatively high flux and could deliver drug at high input rate through transdermal route. PSA2 was found to have good rate-controlling property and could be successfully employed in transdermal delivery of nitrendipine.     

Effect of negatively charged species on the growth behavior of silicon films in hot wire chemical vapor deposition

The deposition behavior of silicon in hot wire chemical vapor deposition was investigated, focusing on the generation of negatively charged species in the gas phase using a gas mixture of 20% SiH₄ and 80% H₂ at a 450 °C substrate temperature under a working pressure of 66.7 Pa. A negative current of 6–21 µA/cm² was measured on the substrate at all processing conditions, and its absolute value increased with increasing wire temperature in the range of 1400 °C–1900 °C. The surface roughness of the films deposited on the silicon wafers increased with increasing wire temperature in the range of 1510 °C–1800 °C. The film growth rate on the positively biased substrates (+ 100 V, + 200 V) was higher than that on the neutral (0 V) and negatively biased substrates (− 100 V, − 200 V, − 300 V). These results indicate that the negatively charged species are generated in the gas phase and contribute to deposition. The surface roughness evolved during deposition was attributed to the electrostatic interaction between these negatively charged species and the negatively charged growing surface.     

Atomic-layer doping in Si by alternately supplied PH3 and SiH4

Atomic-layer doping of P in Si epitaxial growth by alternately supplied PH₃ and SiH₄ was investigated using ultraclean low-pressure chemical vapor deposition. Three atomic layers of P adsorbed on Si(100) are formed by PH₃ exposure at a partial pressure of 0.26 Pa at 450°C. By subsequent SiH₄ exposure at 220 Pa at 450°C, Si is epitaxially grown on the P-adsorbed surface. Furthermore, by 12-cycles of exposure to PH₃ at 300–450°C and SiH₄ at 450°C followed by 20-nm thick capping Si deposition, the multi-layer P-doped epitaxial Si films of average P concentrations of 10²¹ cm⁻³ are formed. The resistivity of the film is as low as 2.4×10⁻⁴ Ω cm. By annealing the sample at 550°C and above, it is found that the resistivity increases and the surface may become rough, which may be due to formation of SiP precipitates at 550°C and above. These results suggest that the epitaxial growth of very low-resistive Si is achieved only at a very low-temperature such as 450°C.     

Indium Tin Oxide Thin-Film Sensor for Detection of Volatile Organic Compounds (VOCs)

Indium tin oxide (ITO) (In₂O₃ + 17% SnO₂) thin films were grown on glass substrate by direct evaporation method. Two thick gold pads were deposited to take out contacts. The response of these films at different operating temperatures, when exposed to various volatile organic compounds (VOCs) such as methanol, ethanol, butanol, and acetone in the concentration range 200-2500 ppm was evaluated. Additionally, the effect of film thickness on the response charateristics of methanol and acetone was studied. The linearity and sensitivity of the sensors were measured. The ITO thin-film sensors showed a sensitivity of 0.256 ohms/ppm to acetone vapors, which was almost linear in the range 200-2500 ppm. In order to improve sensitivity and selectivity, a thin layer of various metal and metal oxides such as Cu and PbO was deposited on the sensor surface to work as catalytic layer and the effect on the performance of the sensor was studied. The response and recovery times of the sensor were determined for acetone vapors and were found to be 155 sec and 110 sec, respectively.     

Structure and electrical properties of (100)-oriented Pb(Zn1/3Nb2/3)O3–Pb(Mg1/3Nb2/3)O3–PbTiO3 thin films on La0.7Sr0.3MnO3 electrode by chemical solution deposition

(100)-oriented 0.462Pb(Zn_1/3Nb_2/3)O₃–0.308Pb(Mg_1/3Nb_2/3)O₃–0.23PbTiO₃ (PZN-PMN-PT) perovskite ferroelectric thin films were prepared on La_0.7Sr_0.3MnO₃/LaAlO₃ (LSMO/LAO) substrate via a chemical solution deposition route. The perovskite LSMO electrode was found to effectively suppress the pyrochlore phase while promote the growth of the perovskite phase in the PZN-PMN-PT film. The film annealed at 700 °C exhibited a high dielectric constant of 2130 at 1 kHz, a remnant polarization, 2P_r, of 29.8 μC/cm², and a low leakage current density of 7.2 × 10^− 7 A/cm² at an applied field of 200 kV/cm. The ferroelectric polarization was fatigue-free at least up to 10¹⁰ cycles. Piezoelectric coefficient, d₃₃, of 48 pm/V was also demonstrated. The results showed that much superior properties could be achieved with the PZN-PMN-PT thin films on the solution derived LSMO electrode than on Pt electrode by sputtering.     

Preceramic polymer derived cellular ceramics

Ceramic foams were prepared by a self-blowing process of a poly(silsesquioxane) melt at 270 °C. The cell size, the interconnectivity density and the shape of the foam cells were adjusted by a thermal pre-curing procedure of the polymer at 200 °C. Inorganic fillers were used to modify processing behaviour and properties of the pyrolysed ceramic foam. After pyrolysis in inert atmosphere at 1200 °C ceramic composite foams with a total porosity up to 87% were obtained. The open cell ceramic foams had a mean cell diameter of 1.2 mm and a mean strut thickness of 0.2 mm. Interpenetrating phase composites (IPCs) were fabricated by infiltrating the open cellular ceramic preform with Mg alloy melt at 680 °C and a pressure of 86 MPa. The mechanical properties were found to depend on the reactions between the metal and the ceramic forming MgO, Mg₂Si and Al₁₂Mg₁₇ as the major reaction products. The IPCs showed a significantly higher creep resistance at 135 °C, compression strength and elastic modulus compared to the unreinforced magnesium alloys.     

Alkoxide route to La0.5Sr0.5CoO3 epitaxial thin films on SrTiO3

An all alkoxide based sol–gel route was investigated for preparation of epitaxial La_0.5Sr_0.5CoO₃ (LSCO) films on 100 SrTiO₃ (STO) substrates. Films with 20–30 to 80–100 nm thickness were prepared by spin-coating 0.2–0.6 M (metal) solutions on the STO substrates and heat treatment to 800 °C at 2 °C min^− 1, 30 min, in air. The films were epitaxial with a cube-on-cube alignment and the LSCO cell was strained to match the STO substrate of 3.905 Å closely; a and b = 3.894 Å and 3.897 Å for the 20–30 and 80–100 nm films, respectively. The c-axis was compressed to 3.789 Å and 3.782 Å for the 20–30 and 80–100 nm films, respectively, which resulted in an almost unchanged cell volume as compared to polycrystalline film and nano-phase powders prepared in the same way. The SEM study showed mainly very smooth, featureless surfaces, but also some defects. A film prepared in the same way on an -Al₂O₃ substrate was dense and polycrystalline with crystallite sizes in the range 10–50 nm and gave cubic cell dimensions of a_c = 3.825 Å. The conductivity of the ca 30–40 nm thick polycrystalline film was 1.7 mΩcm, while the epitaxial 80–100 nm film had a conductivity of around 1.9 mΩcm.