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.     

Surface Topography Analysis When High-Speed Rough Milling Hardened Steel

This study is part of a bigger picture on investigating three main cutter path strategies—raster, single-direction raster, and offset—in order to evaluate the feasibility of employing high axial depths of cut (10 mm ≤ A_d ≤ 20 mm) when high-speed rough milling hardened AISI H13 hot work tool steel with the aim of achieving high volume of metal removed with short machining time. Here, comparative studies were made of the surface topography maps induced at various axial depths of cut in order to gain an in-depth understanding of their effects on the surface texture obtained via the parametric study of alternative cutter path strategies. Previous work has shown that the use of an offset cutter path strategy when high-speed rough milling hardened steel using an axial depth of 15 mm resulted in the lowest tool life, as compared with the use of raster and single-direction raster strategies.[1]This article also describes a novel approach on improving the offset cutter path strategy by selecting the proper entrance and exit conditions to improve surface texture. The effects of an offset strategy and a modified offset strategy are investigated in terms of surface roughness and surface texture.     

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.     

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.     

Investigation of CdTex and Cd1-xZnxTe Schottky Barrier Diode Structure Based γ-Ray Detectors

Cadmium Telluride (CdTe) and Cadmium Zinc Telluride (CdZnTe) based detectors have been developed for hard X-ray and γ -ray detection. These semiconducting materials have high resistivity because of the wide bandgap and also have high photon absorption efficiency because of the large atomic number (Z_Cd = 48, Z_Te = 52). CdTe and CdZnTe substrates (7 mm × 9 mm × 0.5 mm) with different stoichiometry were taken for the fabrication of γ-ray detectors. The substrate was prepared by polishing the bulk crystals grown by the rotational Bridgman method. Crystals with maximum electrical resistivity were grown in this way. For fabrication of Schottky barrier diode structures, the Schottky contacts were made by electroless deposition for gold (Au) and thermal evaporation for Indium (In). The Au/CdTe/In and Au/CdZnTe/In Schottky barrier diodes were linked to the charge sensitive preamplifier by gold wires. Then, I-V measurement and detector efficiency like charge collection performance with energy resolutions were analyzed at room temperature by using ⁵⁷Co and ¹³⁷Cs gamma sources. The good energy resolutions of ⁵⁷Co (122 KeV) and ¹³⁷Cs (662 KeV) sources are obtained for both CdTe and CdZnTe diode detectors.     

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.     

Synthesizing and Physical Properties of GdPr-123 High-Tc Superconductor

Ceramic Gd_1-xPr_xBa₂Cu₃O_7-y (GdPr-123) high-T_c superconductors have been synthesized by the standard solid state reaction method and characterized by XRD, SEM, TGA, and DT techniques in the range of x, 0.0 ≤ x ≤ 1.0 Samples have orthorhombic structure with Pmmm symmetry and there is a small percentage (less than 1%) of the Ba sites occupied by Pr ions in some Pr-rich samples. In these samples a small trace of BaCuO₂ and Pr BaO₃ secondary phases persist with the main peaks at 2θ = 29.3° and 28.9° respectively. Microstructure analysis indicates a uniform grain size distribution with a mean size of 5 μm. No significant change of grain size is shown throughout the range of x studied. The valence of Pr and Cu were determined by magnetization measurements in the temperature range 100 to 250°K. These data reveal a valence of 3.86+ for Pr in all samples independant of x. The similarity of the superconducting and insulating properties in this system to those of the oxygen deficient RBa₂Cu₃O₇ (R-123) (R: Y or rare earth) system implies that the mechanism of superconductivity in high-T_c. superconductors cannot be two-dimensional, even though the superconductive current occurs in two dimensions.     

Influence of a Weak Magnetic Field on Photoconductivity Spectrum of C60 Single Crystal

Comparative research of the excitation photoconductivity spectra (quantum light energy 2-5 eV) of C₆₀ single crystal in and out of magnetic field at the temperature T = 250-350 K has been carried. The spectral evolution at this temperature range is described. It is shown that the spectra changes abrupt at temperature T₁ ∼ 260 K and T₂ ∼ 315 K. An increase in the photoconductivity up to 15% was observed in the magnetic field (B = 0.4 T) within the photon energy range 2.5-4.5 eV. Local photoconductivity peak's appearances in the magnetic field have been proven that the charge transfer excitons take part in a photoconductivity.     

Numerical Study of Air Compressibility During Horizontal Pneumatic Transport

Using numerical simulations, the effect of the compressibility of air on the flow pattern of particles and pressure drop in the presence of particles during horizontal pneumatic transport operating under negative pressure was examined. The length and inside diameter of the pipeline were 30 m and 40 mm, respectively, and the chosen particles (4 mm in diameter) had densities of ρ_p = 1000 and 2000 kg/m³. The mean air velocities at pipe the inlet were U_inlet = 19, 22, and 28 m/s, and the range of the mass flow rate ratios of particle to air, μ, was varied up to 2.0. For a given inlet air velocity, the difference in the flow pattern between compressible and incompressible flow calculation is generally small. For ρ_p = 1000 kg/m³ particles the additional pressure drop in compressible flow increases when μ is above 0.5 and U_inlet is 28 m/s, μ is above 1.3 and U_inlet is 22 m/s, and μ is above 1.5 and U_inlet is 19 m/s. In these cases, the particle flow pattern is homogeneous. For ρ_p = 2000 kg/m³ particles, the pressure drop increases only when μ is above 1.5 and U_inlet is 28 m/s. The difference is not noticeable when the particle flow pattern is heterogeneous. Also, the difference in the additional pressure drop is much larger during homogeneous flow than heterogeneous flow.     

Chemical vapour deposition of praseodymium oxide films on silicon: influence of temperature and oxygen pressure

Metal-organic chemical vapour deposition (MOCVD) of various phases in PrO_x system has been studied in relation with deposition temperature (450–750 °C) and oxygen partial pressure (0.027–100 Pa or 0.2–750 mTorr). Depositions were carried out by pulsed liquid injection MOCVD using Pr(thd)₃ (thd = 2,2,6,6-tetramethyl-3,5-heptanedionate) precursor dissolved in toluene or monoglyme. By varying deposition temperature and oxygen partial pressure amorphous films or various crystalline PrO_x phases (Pr₂O₃, Pr₇O₁₂, Pr₆O₁₁) and their mixtures can be grown. The pure crystalline Pr₂O₃ phase grows only in a narrow range of partial oxygen pressure and temperature, while high oxygen pressure (40–100 Pa) always leads to the most stable Pr₆O₁₁ phase. The influence of annealing under vacuum at 750 °C on film phase composition was also studied. Near 90% step coverage conformity was achieved for PrO_x films on structured silicon substrates with aspect ratio 1:10. In air degradation of Pr₂O₃ films with transformation to Pr(OH)₃ was observed in contrast to Pr₆O₁₁ films.     

Microwave dielectric characteristics of Ba(Mg1/3Ta2/3)O3 ceramics sintered at low-temperatures

The microwave dielectric properties and microstructures of Ba(Mg_1/3Ta_2/3)O₃ (BMT) ceramics sintered at low temperatures with 2–3 wt.% NaF additives were investigated. BMT ceramics sintered at 1340 °C for 3–12 h showed dielectric constants (_r) of 25.5–25.7, Qf values of 41 500–50 400 GHz and temperature coefficients of the resonator frequency (τ_f) of 10.9–21.4 ppm °C⁻¹. The variation of sintering time almost had no effect on the dielectric constant. The Qf value increased and the τ_f decreased with increasing sintering time. The ordering degree of Mg²⁺ and Ta⁵⁺ at B-sites increased with increasing sintering time.     

SCALING LAWS FOR PARTICLE BREAKUP IN NOZZLE GENERATED SHOCKS

Conditions for the onset of particle breakup in normal shock waves have been investigated. A normalized particle drag behind the shock has been determined in terms of gas stagnation conditions and particle diameter for a range of gas Mach numbers 1 ≤ M₁ ≤ 5 by introducing appropriately defined particle Knudsen and Reynolds numbers into analytical expressions for the drag coefficient. Numerical computations of the particle drag, normalized with gas stagnation pressure and particle area, indicate a peak at a gas Mach number M₁ ≳ 2.2, The magnitude of the peak was found to decrease with increasing particle diameter and reservoir gas density.

Criteria for the onset of agglomerate breakup were defined in terms of a modified Weber number for the adhesion mechanisms due to Van der Waals forces, electrostatic attraction and adsorbed surface films. These results indicate that larger more closely packed agglomerates made up of smaller constituent particles have a greater tendency to resist breakup for a given set of stagnation conditions and shock Mach number.     

Molecular beam epitaxial growth of SmBa2Cu3O7−δ thin films and effect of substrate temperature on the surface roughness

Stoichiometrically optimized, epitaxial SmBa₂Cu₃O_7-δ thin films with high T_{c, R = 0} and high critical current densities j_c have been prepared for the first time in a tightly controlled molecular beam epitaxy process in non-reactive molecular oxygen, followed by an in situ loading process with molecular oxygen. The surface roughness (on a submicrometre scale) of single-crystal films with their c axes perpendicular to the surface depends markedly on the surface temperature of the substrate during the deposition of the epitaxial films, within a range of only a few degrees centigrade. The calibrated optimal temperature for the preparation of epitaxial films 200 nm thick of this single orientation is found to be 680 ± 5 °C. In scanning tunnelling microscopy investigations, they show a surface roughness of less than 6 nm (five SmBa₂Cu₃O_7−δ unit cells) on a 2 μm × 2 μm scale. At deposition temperatures below this optimal deposition temperature, the well-known a-axis growth increases rapidly, whereas higher temperatures give a significantly higher surface roughness, which can be observed by scanning electron microscopy.     

Compression Testing of Ti-6Al-4V in the Temperature Range of 303-873K

Compression testing of Ti-6Al-4V alloy has been carried out at temperatures between 303 K to 873 K. To prevent embrittlement due to atmospheric oxygen and nitrogen, the samples were given a glass coating, which also acts as a lubricant simultaneously. Dynamic Strain Aging was observed to occur in the temperature range of 600 K to 800 K. Below 600 K stresses were high. Warm working has to be done above 800 K but below 1163 K (0.6 T_m where T_m = 1940 K) which is the recrystallization temperature. Based on these conclusions, warm extrusion has been successfully carried out in the Materials Forming Laboratory of I.I.T., Madras, Chennai, India.     

A damping analysis of composite laminates using the closed form expression for the basic damping of Poisson's ratio

Various methods have been presented to obtain the effective damping of a symmetric laminated composite. In this paper, modified classical lamination theory based upon the elastic–viscoelastic correspondence principle was utilized by developing the basic damping of Poisson's ratio for accurately predicting the damping of laminated composite beams. The analysis involves an extension of the elastic–viscoelastic approach. Futhermore, Ni and Adams' theory was used for verifying the modified classical lamination theory. Six typical laminated composites with [±θ]_s,[0/θ]_s,[0/±θ/90]_s,[90/±θ/0]_s,[0/90/±θ]_s and [90/0/±θ]_s, stacking sequences were employed for this study. Numerical results have shown that damping values were in some difference among prediction methods over the particular range of fiber orientation.     

A Novel Fullerene Hydroxamic Acid for the Liquid-Liquid Extraction, Separation, Preconcentration, and Spectrophotometric and ICP-AES Determination of Vanadium

A new reagent N-phenyl-(1,2 methanofullerene C₆₀)61-formohydroxamic acid (PMFFA) is reported for extraction and trace determination of vanadium(V) in nutritional and biological substrates. The extraction mechanism of vanadium from 6 M HCl media is investigated. The influence of PMFFA, diverse ions, and temperature on the distribution constant of vanadium examined. The over all stability constant (log β₂K_e) and extraction constant (K_ex) are 20.89 ± 0.02 and 8.0 ± 0.02 × 10^-15, respectively in chloroform. The thermodynamics parameters are calculated and kinetics of vanadium transport is discussed. The system obeys Beer's law in the range of 3.2-64.0 ng mL^-1 of vanadium(V). The molar absorptivity is 7.96 × 10⁵ L mol^-1 cm^-1, at 510 nm. The PMFFA-vanadium(V) complex chloroform extract in chloroform was directly inserted into plasma for ICP-AES measurement, which increases the sensitivity by 50 folds and obey Beer's law in the range of 50-1200 pg mL^-1 of vanadium(V). The method is applied for determination vanadium in real standard samples, sea water, and environmental samples.     

EFFECT OF PARTICLE SIZE DISTRIBUTION ON TRANSFER EFFICIENCY AND APPEARANCE IN POWDER COATINGS

Three powder samples of identical chemistry were taken from the same lot under different conditions: (1) relatively wide size distribution (Sample A) d₅₀ = 18.1μm, (2) narrow size distribution, d₅₀ = 22.4μm (Sample B), and (3) wide size distribution with more fines than Sample A, d₅₀ = 15.1μm (Sample C). Within this relatively minor variation of Particle Size Distribution (PSD) with respect to d₅₀, the appearance of the powder with minimum d₅₀ (15.1μm) was best. The results show two trends: (1) PSD with d₅₀ about 15μm can result in excellent appearance (GM Tension in the range of 18 to 19 on a scale of 0 to 20), and (2) the width of the distribution need not be narrow when d₉₀ is less than 40μm.

Polymer powders in this size range do not fluidize well without agitation, but when vibration was applied, all three samples had R values (fluidity) 200 or above, which is adequate for fluidization and transport. The maximum R value was obtained for Sample A, which had the widest size distribution. Thus, the fluidity tests agreed with the expected results.     

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).     

RE-ENTRAINMENT OF DUSTS FROM THE DUST LAYER ON THE THE DEPOSITED DUSTS IN THE CYCLONE DUST COLLECTORS

There were many papers concerning the experimental results of the collection efficiency, but up to this time there are a few papers concerning the experimental results of the re-entrainment or dispersion of the dust particles from the dust layer by the turbulent rotational air flow in the dust bunker for the cyclone dust collector. Then in this paper, the author described the experimental results of the re-entrainment of the test dust ( talc X_R50 = 8.O µm ) for the four kinds of the throat diameter D₃ = 50, 80, 100 and 150 mm. Especially it is very importance to take into consideration of flow rate Qb into the dust bunker which is a function of D₃ and cyclone diameter D₁ and the maximum tangential velocity Vet in the dust bunker which depends on D₁,D₃ and Qb.     

Enhancement of gene transfer to cervical cancer cells using transferrin-conjugated liposome

Transferrin-conjugated cationic liposome (T_f -DDAB liposome) was developed as a targeted gene delivery system by using heterobifunctional cross-linking agent, N-succimidyl-3-(2-pyridyldithio)propionate (SPDP), and gradient metrizamide ultracentrifugation method. Physico-chemical properties of T_f -liposome were determined by scanning/transmission electron microscopy (SEM/TEM) and dynamic laser-light scattering method (DLS) with a mean diameter of 584±15 nm. Gel retardation assay was performed using various DDAB:DNA ratios, and proved that the 6:1 weight ratio formulation gave the most neutralized complex. In vitro transfection was done in human cervical cancer cells, HeLa, and the transfection efficiency of T_f -liposome was found to be fivefold higher than that of unconjugated (plain) DDAB liposome and twofold higher than that of Lipofectin™. In conclusion, a target-oriented T_f -DDAB liposome was made successfully and proved to be very efficient in DNA delivery into the cervical cancer cells in culture.