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At least 469 records · Page 26

Synthesis and Characterization of Copolymers and Nanocomposites from Limonene, Styrene and Organomodified-Clay Using Ultrasonic Assisted Method

In the present work, we report a simple synthesis method for preparation of copolymers and nanocomposites from limonene and styrene using clay as a catalyst. The copolymerization reaction is carried out by using a proton exchanged clay as a catalyst called Mag-H+. The effect of temperature, reaction time and amount of catalyst were studied, and the obtained copolymer structure (lim-co-sty) is characterized by Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (1H-NMR) and differential scanning calorimetry (DSC). The molecular weight of the obtained copolymer is determined by gel permeation chromatography (GPC) and is about 4500 g·mol−1. The (lim-co-sty/Mag 1%, 3%, 7% and 10% by weight of clay) nanocomposites were prepared through polymer/clay mixture in solution method using ultrasonic irradiation, in the presence of Mag-CTA+ as green nano-reinforcing filler. The Mag-CTA+ is organophilic silicate clay prepared through a direct exchange process, using cetyltrimethylammonuim bromide (CTAB). The prepared lim-co-sty/Mag nanocomposites have been extensively characterized by FT-IR spectroscopy, X-ray diffraction (XRD), scanning electronic microscopy (SEM) and transmission electronic microscopy (TEM). TEM analysis confirms the results obtained by XRD and clearly show that the obtained nanocomposites are partially exfoliated for the lower amount of clay (1% and 3% wt) and intercalated for higher amounts of clay (7% and 10% wt). Moreover, thermogravimetric analysis (TGA) indicated an enhancement of thermal stability of nanocomposites compared with the pure copolymer.

Derdar, Hodhaifa↗

CO 2 /Brine/Rock Interactions in the Cedar Keys-Lawson Formation

It has been reported that among the various geologic storage options, deep saline aquifers have the largest estimated capacity for CO 2 storage. Obtaining knowledge of possible artificially geochemically induced changes to the permeability and porosity of host CO 2 storage deposits will enable us to gain insight on long-term reservoir behavior under CO 2 storage conditions. An experimental study of the interaction of CO 2 /brine/rock on saline formations was conducted in a static system under CO 2 storage conditions. Chemical interactions in the Cedar Keys-Lawson Formation carbonate during exposure to CO 2 and brine under sequestration conditions were studied. Samples were exposed to the simulated in-situ reaction conditions for one and six months. The samples were exposed to a model brine at 55 °C and CO 2 pressure of 23.8 MPa (3,500 psig). Computed tomography (CT), x-ray diffraction (XRD), scanning electron microscopy (SEM)-energy dispersive x-ray spectroscopy (EDS), brine composition, core porosity, and core permeability analyses were conducted prior to and after the exposure experiments. Preliminary permeability measurements obtained from the core samples showed changes after they were exposed to CO 2 -saturated brine for one and six months. This observation suggests that mineral dissolution and mineral precipitation could occur in the host deposit altering its characteristics for CO 2 storage over time. The 3D images of the pore space clearly illustrate the degree of dissolution that occurred during exposure. It is noted that the dissolution that occurred during the six-month exposure could have enhanced the connectivity between voids. This may contribute the increase of permeability after the CO 2 /brine exposure. In addition, the primary minerals comprising the core are dolomite and gypsum. Both minerals could dissolve in the CO 2 /brine environment resulting in the increase of permeability after the six-month exposure.

58 GEOSCIENCES↗

Structure and properties of solid surfaces

Difficulties in experimental studies of crystalline surfaces are related to the fact that surface atoms have an intrinsic tendency to react with their environment. A second problem is connected with the effective thickness of surfaces, which ranges from one to several atom layers. The phenomenology of surface interactions with gases are considered, taking into account physical adsorption, chemisorption, and the oxidation of surfaces. Studies of the surface structure are discussed, giving attention to field emission microscopy, field-ion microscopy, electron diffraction techniques, Auger spectroscopy, scanning electron microscopy, electron probe microanalysis, ion microprobe methods, and low-energy backscattering spectroscopy. Investigations of semiconductor surfaces are also described.

Gatos, H. C.↗

Oxidation in oxygen at 900 deg and 1000 deg C of four nickel-base cast superalloys: NASA-TRW VIA, B-1900, alloy 713C, and IN-738

The oxidation at 900 and 1,000 C of four nickel-base superalloys in 1 atmosphere of slowly flowing oxygen was investigated. Thermogravimetric rate data were obtained for periods to 100 hours. The morphology and composition of the oxide scales formed after 100 hours were studied by optical microscopy, X-ray diffraction, electron microprobe, scanning electron microscopy, and X-ray photoelectron spectroscopy (ESCA). Alloys B-1900 and VIA were found to be primarily alumina formers, though probably 25 percent of their surface was covered by CR2O3-containing oxides at 900 C. Alloys 713C and IN-738 were primarily chromia formers, though the surface of 713C at 1,000 C was covered with NiO, and the surface of IN-738 at both temperatures was covered with a thin layer of TiO2.

Fryburg, G. C.↗

The effect of zirconium on the isothermal oxidation of nominal Ni-14Cr-24Al alloys

The isothermal oxidation of Ni-14Cr-24Al-xZr-type alloys was performed in still air at 1100, 1150, and 1200 C for times up to 200 hr. The zirconium content of the alloys varied from 0-0.63 atom percent (a/o). The oxidized surfaces were studied by optical microscopy, X-ray diffraction, and scanning electron microscopy. The base alloy was an alumina former with the zirconium-containing alloys also developing some ZrO2. The addition of zirconium above 0.066 a/o increased the rate of weight gain relative to the base alloy. Due to oxide penetratio, the weight gain increased with Zr content; however, the scale thickness did not increase. The Zr did increase the adherence of the oxide, particularly at 1200 C. The delta W/A vs. time data fit the parabolic model of oxidation. The specific diffusion mechanism operative could not be identified by analysis of the calculated activation energies. Measurements of the Al2O3 scale lattice constants yielded the same values for all alloys.

Kahn, A. S.↗

Effects of MAR-M247 substrate (modified) composition on coating oxidation coating/substrate interdiffusion

The effects of gamma+gamma' Mar-M247 substrate composition on gamma+beta Ni-Cr-Al-Zr coating oxidation and coating/substrate interdiffusion were evaluated. These results were also compared to a prior study for a Ni-Cr-Al-Zr coated gamma Ni-Cr-Al substrate with equivalent Al and Cr atomic percentages. Cyclic oxidation behavior at 1130 C was investigated using change in weight curves. Concentration/distance profiles were measured for Al, Cr, Co, W, and Ta. The surface oxides were examined by X-ray diffraction and scanning electron microscopy. The results indicate that variations of Ta and C concentrations in the substrate do not affect oxidation resistance, while additions of grain boundary strengthening elements (Zr, Hf, B) increase oxidation resistance. In addition, the results indicate that oxidation phenomena in gamma+beta/gamma+gamma' Mar-M247 systems have similar characteristics to the l gamma+beta/gamma Ni-Cr-Al system.

Pilsner, B. H.↗

Advanced hydrogen electrode for hydrogen-bromide battery

Binary platinum alloys are being developed as hydrogen electrocatalysts for use in a hydrogen bromide battery system. These alloys were varied in terms of alloy component mole ratio and heat treatment temperature. Electrocatalyst evaluation, performed in the absence and presence of bromide ion, includes floating half cell polarization studies, electrochemical surface area measurements, X ray diffraction analysis, scanning electron microscopy analysis and corrosion measurements. Results obtained to date indicate a platinum rich alloy has the best tolerance to bromide ion poisoning.

Kosek, Jack A.↗

Chemical durability of high-temperature superconductor YBa2Cu3O(7-x) in aqueous environments

The stability of YBa2Cu3O(7-x) in water and 100-percent humidity has been investigated at three temperatures, using pH measurements, X-ray diffraction, and scanning electron microscopy. The oxide-ceramic superconductor is highly unstable; it reacts rapidly with water and degrades in moisture. Dissolution of the oxide perovskite in water is highly incongruent. The corrosion products are found to be BaCO3, CuO, O2, etc. Barium hydroxide is first formed and further reacts with atmospheric CO2 to form needle-shaped crystals of BaCO3. For any practical applications, devices made from these materials would have to be protected with an impermeable coating to prevent deterioration from atmosphere.

Bansal, Narottam P.↗

Synthesis and characterization of high-Tc superconductors in the Tl-Ca-Ba-Cu-O system

Both Tl2Ca2Ba2Cu3O10 and TlCa3BaCu3O8.5 are investigated for superconductivity as a function of the sintering temperature, time, atmosphere, and quench rate in an effort to synthesize the high-Tc superconducting phase in the thallium system. The samples are characterized by electrical resistivity measurements, X-ray diffraction, and scanning electron microscopy. Samples of starting composition Tl2Ca2Ba2Cu3O10 fired in air at 860-900 C and rapidly quenched show a Tc of 96-107 K. In contrast, specimens of starting composition TlCa3BaCu3O8.5 when baked at 900 C and slowly cooled in oxygen superconduct at 116 K and above and consist of Tl2Ca2Ba2Cu3O(10+x) as the dominant phase. The results also show that, in contrast to the case of YBa2Cu3O(7-x), doping with a small concentration of fluorine sharpens the resistive transition and produces a large Tc increase in thallium-based superconductors.

Bansal, Narottam P.↗

Oxidation characteristics of Beta-21S in air in the temperature range 600 to 800 C

The metastable beta-Ti alloy Beta-21S, Ti-15Mo-2.7Nb-3Al-0.2Si (weight percent), has been proposed as a candidate for use in metal matrix composites in future hypersonic vehicles. The present study investigated the oxidation behavior of Beta-21S over the temperature range 600 C to 800 C. Oxidation weight gain was evaluated using thermogravimetric analysis. Oxidized specimens were evaluated using x ray diffraction techniques, scanning electron microscopy, energy dispersive x ray analysis, and electron microprobe analysis to identify oxidation products and evaluate oxidation damage to the alloy.

Wallace, Terryl A.↗

Composition dependence of superconductivity in YBa2(Cu(3-x)Al(x))Oy

Eleven different compositions in the system YBa2(Cu(3-x)Al(x))O(y) (x = 0 to 0.3) have been synthesized and characterized by electrical resistivity measurements, powder x-ray diffraction, and scanning electron microscopy. The superconducting transition temperature T sub c (onset) was almost unaffected by the presence of alumina due to its limited solubility in YBa2Cu3O(7-x). However, T sub c(R = 0) gradually decreased, and the resistive tails became longer with increasing Al2O3 concentration. This was probably due to formation of BaAl2O4 and other impurity phases from chemical decomposition of the superconducting phase by reaction with Al2O3.

Bansal, Narottam P.↗

Composition dependence of superconductivity in YBa2(Cu(3-x)Al(x))O(y)

Eleven different compositions in the system YBa2(Cu(3-x)Al(x))O(y) (x = 0 to 0.3) have been synthesized and characterized by electrical resistivity measurements, powder X-ray diffraction, and scanning electron microscopy. The superconducting transition temperature T sub c (onset) was almost unaffected by the presence of alumina due to its limited solubility in YBa2Cu3O(7-x). However, T sub c(R = 0) gradually decreased, and the resistive tails became longer with increasing Al2O3 concentration. This was probably due to formation of BaAl2O4 and other impurity phases from chemical decomposition of the superconducting phase by reaction with Al2O3.

Bansal, N. P.↗

Room temperature degradation of YBa2Cu3O(7-x) superconductors in varying relative humidity environments

An aging study was performed to determine the stability of YBa2Cu3O(7-x) ceramics in humid environments at 20 C. In this study, fired ceramic specimens were exposed to humidity levels ranging from 30.5 to 100 percent for 2-, 4-, and 6-week time intervals. After storage under these conditions, the specimens were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and electrical resistance measurements. At every storage condition evaluated, the fired ceramics were found to interact with H2O present in the surrounding environment, resulting in the decomposition of the YBa2Cu3O(7-x) phase. XRD data showed that BaCO3, CuO, and Y2BaCuO5 were present after aging and that the peak intensities of these impurity phases increased both with increasing humidity level and with increasing time of exposure. Additionally, SEM analyses of the ceramic microstructures after aging revealed the development of needle-like crystallites along the surface of the test specimens after aging. Furthermore, the superconducting transition temperature T(sub c) was found to decrease both with increasing humidity level and with increasing time of exposure. All the specimens aged at 30.5, 66, and 81 percent relative humidity exhibited superconducting transitions above 80 K, although these values were reduced by the exposure to the test conditions. Conversely, the specimens stored in direct contact with water (100 percent relative humidity) exhibited no superconducting transitions.

Hooker, M. W.↗

Improvement of critical current density in thallium-based (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) superconductors

Epitaxial (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) ((Tl,Bi)-1223) thin films on (100) single crystal LaAlO3 substrates were synthesized by a two-step procedure. Phase development, microstructure, and relationships between film and substrate were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Resistance versus temperature, zero-field-cooled and field cooled magnetization, and transport critical current density (J(sub c)) were measured. The zero-resistance temperature was 105-111 K. J(sub c) at 77 K and zero field was greater than 2 x 10(exp 6) A/sq cm. The films exhibited good flux pinning properties.

Ren, Z. F.↗

Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

Nanjundaswamy, K. S.↗

Structure and Morphology of Phthalocyanine Films Grown in Electrical Fields by Vapor Deposition

Phthalocyanine (Pc) films have been synthesized by vapor deposition on quartz substrates, some of which were coated with a very thin gold film before depositing Pc films. Electrical fields up to 6200 V/cm between a mech electrode and the substrate are introduced during film growth. These films have been characterized by x-ray diffraction and scanning electron microscopy. The molecular orientations and surface morphology of Pc films were changed under the electrical fields. The surface of these films grown without electrical field shows whisk-like morphology. When films are deposited under an electrical field, a dense film with flat surface is obtained.

Zhu, Shen↗

Oxidation of ZrB2-SiC

In this paper the oxidation behavior of ZrB2-20 vol% SiC is examined. Samples were exposed in stagnant air in a zirconia furnace (Deltech, Inc.) at temperatures of 1327, 1627, and 1927 C for ten ten-minute cycles. Samples were removed from the furnace after one, five, and ten cycles. Oxidized material was characterized by mass change when possible, x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). Oxidation kinetics, oxide scale development, and matrix recession were monitored as a function of time and temperature. Oxidation and recession rates of ZrB2 - 20 vol% SiC were adequately modeled by parabolic kinetics. Oxidation rates of this material are rapid, allowing only very short-term application in air or other high oxygen partial pressure environments.

Opila, Elizabeth J.↗

The Effects of Gravity on the Crystallization Behavior of Heavy Metal Fluoride Glasses

Heavy metal fluoride glasses are used in such applications as fiber lasers and laser amplifiers. ZrF4-BaF2-LaF3-AlF3-NaF (ZBLAN) is one of the more commonly used heavy metal fluoride glasses. ZBLAN is an infrared transmitter and has a theoretical attenuation coefficient of 0.002 db/km. However, due to impurities and small crystallites this attenuation coefficient has not been achieved to date. ZBLAN is a fragile glass which can lead to rapid crystallization, if the glass is not cooled rapidly to below the glass transition temperature or if the glass is reheated near the crystallization temperature for any period of time. Studies carried on at Marshall Space Flight Center and the University of Alabama in Huntsville since 1993 have shown that heating ZBLAN glass at the crystallization temperature in reduced gravity results in a suppression of crystallization when compared to ZBLAN processed in unit gravity. These studies utilized NASA's KC-135 aircraft and the Conquest sounding rocket. In the first series of experiments, short lengths of ZBLAN fiber were heated to the crystallization temperature in reduced gravity on board the KC- 135 and the Conquest sounding rocket and compared with fibers heated in unit gravity. The fibers processed in reduced gravity showed no evidence of crystallization when studied with x-ray diffraction and scanning electron microscopy. However, the fibers processed in unit gravity were completely crystallized. Subsequent experiments included heating small pieces of ZBLAN glass at the crystallization temperature while viewing with a video camera to follow the crystallization phenomenon. In this experiment crystallization was observed in reduced gravity, however, it was suppressed when compared to heating in unit gravity. In the most recent experiment on board the KC-135, rapid thermal analysis of ZBLAN was performed. A mechanism to explain the observations has been proposed. This mechanism is based on shear thinning whereby, the glass undergoes a reduction in viscosity in the 10(exp 5) - 10(exp 7) poise range, allowing more rapid diffusion and thus crystallization. It is proposed that this mechanism is suppressed in reduced gravity. An experiment is presently being conducted to test this theory. With increased knowledge of ZBLAN behavior in reduced gravity, three low earth orbit tiber drawing facilities have been designed. One would be suitable for use on the International Space Station, another while aboard the Space Shuttle and the third system is a fully automated facility which would operate independently of the ISS or Shuttle in a free float mode. The primary benefits of free floating a facility in LEO includes a higher quality of microgravity and reduced safety concerns since it is not in a manned environment.

Tucker, Dennis S.↗