Spray pyrolysis of YBCO precursors

1994 ◽  
Vol 9 (10) ◽  
pp. 2490-2500 ◽  
Author(s):  
Gideon S. Grader ◽  
Darío R. Machado ◽  
Raphael Semiat

Acetate, nitrate, and oxalate precursors for YBCO have been spray pyrolyzed under different conditions. Shelled and nonhollow microparticles were obtained from acetate and nitrate precursors, while nonhollow agglomerates were obtained from the oxalate suspension. At low furnace temperatures, the temperature and residence time of the particles were insufficient for complete decomposition of the precursors leading to Cu2O and Cu metal in the product. At 900 °C and above, reduced forms of CuO were not detected by x-ray measurements, and up to ∼60 wt.% YBCO was obtained. An approximate model predicting the particle and gas temperatures along the reactor under different operating conditions was developed. The model demonstrates that under the experimental conditions used here, the absorbed radiation heat by the particles from the furnace walls is significant in heating the gas. The gas and the particle temperatures are fairly close due to the effective heat transfer to the particles. At furnace temperatures of 700 °C, the maximum predicted particle temperature is about 500 °C (for ∼1 s). This explains the incomplete reactions obtained under these conditions. Above 900 °C the reactions are predicted to be complete within the first half of the furnace, leaving sufficient residence time for partial conversion into YBCO. Finally, an approximate expression predicting the relative contribution to the gas heating by the walls and the aerosol has been developed.

2021 ◽  
Vol 8 (1) ◽  
pp. 017002
Author(s):  
Hem Moktan ◽  
Raj Kumar Panta ◽  
Sang Hyun Cho

Abstract Commercially available fully spectroscopic pixelated cadmium telluride (CdTe) detector systems have been adopted lately for benchtop x-ray fluorescence (XRF) imaging/computed tomography (XFCT) of objects containing metal nanoprobes such as gold nanoparticles (GNPs). To date, however, some important characteristics of such detector systems under typical operating conditions of benchtop XRF/XFCT imaging systems are not well known. One important but poorly studied characteristic is the effect of detector bias-voltage on photon counting efficiency, energy resolution, and the resulting material detection limit. In this work, therefore, we investigated these characteristics for a commercial pixelated detector system adopting a 1-mm-thick CdTe sensor (0.25-mm pixel-pitch), known as HEXITEC, incorporated into an experimental benchtop cone-beam XFCT system with parallel-hole detector collimation. The detector system, operated at different bias-voltages, was used to acquire the gold XRF/Compton spectra from 1.0 wt% GNP-loaded phantom irradiated with 125 kVp x-rays filtered by 1.8-mm Tin. At each bias-voltage, the gold XRF signal, and the full-width-at-half-maximum at gold Kα 2 XRF peak (∼67 keV) provided photon counting efficiency and energy resolution, respectively. Under the current experimental conditions, the detector photon counting efficiency and energy resolution improved with increasing bias-voltage by ∼41 and ∼29% at −300V; ∼54 and ∼35% at −500V, respectively, when compared to those at −100V. Consequently, the GNP detection limit improved by ∼26% at −300V and ∼30% at −500V. Furthermore, the homogeneity of per-pixel energy resolution within the collimated detector area improved by ∼34% at −300V and ∼54% at −500V. These results suggested the gradual improvements in the detector performance with increasing bias-voltage up to −500V. However, at and beyond −550V, there were no discernible improvements in photon counting efficiency and energy resolution. Thus, the bias-voltage range of −500 to −550V was found optimal under the current experimental conditions that are considered typical of benchtop XRF/XFCT imaging tasks.


Author(s):  
N. J. Zaluzec

The ultimate sensitivity of microchemical analysis using x-ray emission rests in selecting those experimental conditions which will maximize the measured peak-to-background (P/B) ratio. This paper presents the results of calculations aimed at determining the influence of incident beam energy, detector/specimen geometry and specimen composition on the P/B ratio for ideally thin samples (i.e., the effects of scattering and absorption are considered negligible). As such it is assumed that the complications resulting from system peaks, bremsstrahlung fluorescence, electron tails and specimen contamination have been eliminated and that one needs only to consider the physics of the generation/emission process.The number of characteristic x-ray photons (Ip) emitted from a thin foil of thickness dt into the solid angle dΩ is given by the well-known equation


Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2518
Author(s):  
Dorota Kołodyńska ◽  
Yongming Ju ◽  
Małgorzata Franus ◽  
Wojciech Franus

The possibility of application of chitosan-modified zeolite as sorbent for Cu(II), Zn(II), Mn(II), and Fe(III) ions and their mixtures in the presence of N-(1,2-dicarboxyethyl)-D,L-aspartic acid, IDHA) under different experimental conditions were investigated. Chitosan-modified zeolite belongs to the group of biodegradable complexing agents used in fertilizer production. NaP1CS as a carrier forms a barrier to the spontaneous release of the fertilizer into soil. The obtained materials were characterized by Fourier transform infrared spectroscopy (FTIR); surface area determination (ASAP); scanning electron microscopy (SEM-EDS); X-ray fluorescence (XRF); X-ray diffraction (XRD); and carbon, hydrogen, and nitrogen (CHN), as well as thermogravimetric (TGA) methods. The concentrations of Cu(II), Zn(II), Mn(II), and Fe(III) complexes with IDHA varied from 5–20 mg/dm3 for Cu(II), 10–40 mg/dm3 for Fe(III), 20–80 mg/dm3 for Mn(II), and 10–40 mg/dm3 for Zn(II), respectively; pH value (3–6), time (1–120 min), and temperature (293–333 K) on the sorption efficiency were tested. The Langmuir, Freundlich, Dubinin–Radushkevich, and Temkin adsorption models were applied to describe experimental data. The pH 5 proved to be appropriate for adsorption. The pseudo-second order and Langmuir models were consistent with the experimental data. The thermodynamic parameters indicate that adsorption is spontaneous and endothermic. The highest desorption percentage was achieved using the HCl solution, therefore, proving that method can be used to design slow-release fertilizers.


Catalysts ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 290
Author(s):  
Tim Karsten ◽  
Vesna Middelkoop ◽  
Dorota Matras ◽  
Antonis Vamvakeros ◽  
Stephen Poulston ◽  
...  

This work presents multi-scale approaches to investigate 3D printed structured Mn–Na–W/SiO2 catalysts used for the oxidative coupling of methane (OCM) reaction. The performance of the 3D printed catalysts has been compared to their conventional analogues, packed beds of pellets and powder. The physicochemical properties of the 3D printed catalysts were investigated using scanning electron microscopy, nitrogen adsorption and X-ray diffraction (XRD). Performance and durability tests of the 3D printed catalysts were conducted in the laboratory and in a miniplant under real reaction conditions. In addition, synchrotron-based X-ray diffraction computed tomography technique (XRD-CT) was employed to obtain cross sectional maps at three different positions selected within the 3D printed catalyst body during the OCM reaction. The maps revealed the evolution of catalyst active phases and silica support on spatial and temporal scales within the interiors of the 3D printed catalyst under operating conditions. These results were accompanied with SEM-EDS analysis that indicated a homogeneous distribution of the active catalyst particles across the silica support.


1987 ◽  
Vol 113 ◽  
Author(s):  
Scott Schlorholtz ◽  
Ken Bergeson ◽  
Turgut Demirel

ABSTRACTThe physical and chemical properties of fly ash produced at Ottumwa Generating Station have been monitored since April, 1985. The fly ash is produced from burning a low sulfur, sub-bituminous coal obtained from the Powder River Basin near Gillette, Wyoming. One-hundred and sixty samples of fly ash were obtained during the two year period. All of the samples were subjected to physical testing as specified by ASTM C 311. About one-hundred of the samples were also subjected to a series of tests designed to monitor the self-cementing properties of the fly ash. Many of the fly ash samples were subjected to x-ray diffraction and fluorescence analysis to define the mineralogical and chemical composition of the bulk fly ash as a function of sampling date. Hydration products in selected hardened fly ash pastes, were studied by x-ray diffraction and scanning electron microscopy. The studies indicated that power plant operating conditions influenced the compressive strength of the fly ash paste specimens. Mineralogical and morphological studies of the fly ash pastes indicated that stratlingite formation occurred in the highstrength specimens, while ettringite was the major hydration product evident in the low-strength specimens.


2012 ◽  
Vol 45 (4) ◽  
pp. 674-678 ◽  
Author(s):  
Lukas Lomb ◽  
Jan Steinbrener ◽  
Sadia Bari ◽  
Daniel Beisel ◽  
Daniel Berndt ◽  
...  

Serial femtosecond crystallography (SFX) using X-ray free-electron laser (FEL) sources has the potential to determine the structures of macromolecules beyond the limitation of radiation damage and without the need for crystals of sufficient size for conventional crystallography. In SFX, a liquid microjet is used to inject randomly oriented crystals suspended in their storage solution into the FEL beam. Settling of crystals in the reservoir prior to the injection has been found to complicate the data collection. This article details the development of an anti-settling sample delivery instrument based on a rotating syringe pump, capable of producing flow rates and liquid pressures necessary for the operation of the injector. The device has been used successfully with crystals of different proteins, with crystal sizes smaller than 20 µm. Even after hours of continuous operation, no significant impairment of the experiments due to sample settling was observed. This article describes the working principle of the instrument and sets it in context with regard to the experimental conditions used for SFX. Hit rates for longer measuring periods are compared with and without the instrument operating. Two versions of the instrument have been developed, which both deliver sample at a constant flow rate but which differ in their minimum liquid flow rates and maximum pressures.


Author(s):  
Laslo Šereš ◽  
Ljubica Dokić ◽  
Bojana Ikonić ◽  
Dragana Šoronja-Simović ◽  
Miljana Djordjević ◽  
...  

Cross-flow microfiltration using ceramic tubular membrane was applied for treatment of steepwater from corn starch industry. Experiments are conducted according to the faced centered central composite design at three different transmembrane pressures (1, 2 and 3 bar) and cross-flow velocities (100, 150 and 200 L/h) with and without the usage of Kenics static mixer. For examination of the influence of the selected operating conditions at which usage of the static mixer is justified, a response surface methodology and desirability function approach were used. Obtained results showed improvement in the average permeate flux by using Kenics static mixer for 211 % to 269 % depending on experimental conditions when compared to the system without the static mixer. As a result of optimization, the best results considering flux improvement as well as reduction of specific energy consumption were obtained at low transmembrane pressure and lower feed cross-flow rates.


Sensors ◽  
2021 ◽  
Vol 21 (2) ◽  
pp. 536
Author(s):  
Kenneth A. Goldberg ◽  
Antoine Wojdyla ◽  
Diane Bryant

New, high-coherent-flux X-ray beamlines at synchrotron and free-electron laser light sources rely on wavefront sensors to achieve and maintain optimal alignment under dynamic operating conditions. This includes feedback to adaptive X-ray optics. We describe the design and modeling of a new class of binary-amplitude reflective gratings for shearing interferometry and Hartmann wavefront sensing. Compact arrays of deeply etched gratings illuminated at glancing incidence can withstand higher power densities than transmission membranes and can be designed to operate across a broad range of photon energies with a fixed grating-to-detector distance. Coherent wave-propagation is used to study the energy bandwidth of individual elements in an array and to set the design parameters. We observe that shearing operates well over a ±10% bandwidth, while Hartmann can be extended to ±30% or more, in our configuration. We apply this methodology to the design of a wavefront sensor for a soft X-ray beamline operating from 230 eV to 1400 eV and model shearing and Hartmann tests in the presence of varying wavefront aberration types and magnitudes.


2011 ◽  
Vol 335-336 ◽  
pp. 1385-1390 ◽  
Author(s):  
Shuo Wiei Zhao ◽  
Hui Xu ◽  
Hua Ming Li ◽  
Yuan Guo Xu

In order to improve the photocatalytic activity, Co was successfully loaded into Ag3VO4 by using impregnation process. The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS) and diffuse reflectance spectroscopy (DRS). The XRD and SEM–EDS analyses revealed that Co ion was dispersed on Ag3VO4. The DRS results indicated that the absorption edge of the Co–Ag3VO4 catalyst shifted to longer wavelength. The enhanced photocatalytic activity of Co–Ag3VO4 for Methylene Blue(MB) dye degradation under visible light irradiation was due to its wider absorption edge and higher separation rate of photo-generated electron and holes. In the experimental conditions, it is demonstrated that the MB was effectively degraded by more than 95% within 40 min when the Co–Ag3VO4 catalyst was calcined at 300°C with 1 wt.% Co content.


2017 ◽  
Vol 140 (3) ◽  
Author(s):  
Christoph A. Schmalhofer ◽  
Peter Griebel ◽  
Manfred Aigner

The use of highly reactive hydrogen-rich fuels in lean premixed combustion systems strongly affects the operability of stationary gas turbines (GT) resulting in higher autoignition and flashback risks. The present study investigates the autoignition behavior and ignition kernel evolution of hydrogen–nitrogen fuel mixtures in an inline co-flow injector configuration at relevant reheat combustor operating conditions. High-speed luminosity and particle image velocimetry (PIV) measurements in an optically accessible reheat combustor are employed. Autoignition and flame stabilization limits strongly depend on temperatures of vitiated air and carrier preheating. Higher hydrogen content significantly promotes the formation and development of different types of autoignition kernels: More autoignition kernels evolve with higher hydrogen content showing the promoting effect of equivalence ratio on local ignition events. Autoignition kernels develop downstream a certain distance from the injector, indicating the influence of ignition delay on kernel development. The development of autoignition kernels is linked to the shear layer development derived from global experimental conditions.


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