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At least 829 records · Page 46

Precipitation Hardening in Ferroelectric Ceramics

Domain wall motion in ferroics, similar to dislocation motion in metals, can be tuned by well-concepted microstructural elements. In demanding high-power applications of piezoelectric materials, the domain wall motion is considered as a lossy hysteretic mechanism that should be restricted. Current applications for so-called hard piezoelectrics are abundant and hinge on the use of an acceptor-doping scheme. However, this mechanism features severe limitations due to enhanced mobility of oxygen vacancies at moderate temperatures. By analogy with metal technology, the authors present here a new solution for electroceramics, where precipitates are utilized to pin domain walls and improve piezoelectric properties. Through a sequence of sintering, nucleation, and precipitate growth, intragranular precipitates leading to a fine domain structure are developed as shown by transmission electron microscopy, piezoresponse force microscopy, and phase-field simulation. This structure impedes the domain wall motion as elucidated by electromechanical characterization. As a result, the mechanical quality factor is increased by ≈50% and the hysteresis in electrostrain is suppressed considerably. This is even achieved with slightly increased piezoelectric coefficient and electromechanical coupling factor. This novel process can be smoothly implemented in industrial production processes and is accessible to simple laboratory experimentation for microstructure optimization and implementation in various ferroelectric systems.

36 MATERIALS SCIENCE↗

Enhanced flexibility and thermal conductivity of HfC decorated carbon nanofiber mats

Future-generation spacecraft components allude discovery of novel materials that can withstand extreme environments (>2000 °C). The combined effect of ultra-high temperature ceramics (UHTCs) and carbon fibers (C f ) can satisfy the demanding requirements of aerospace applications. A novel, hybrid, and flexible hafnium carbide (HfC)-decorated carbon nanofiber (C nf ) mat was fabricated via electrospinning. Enhanced thermal stability of the flexible HfC decorated C nf over C nf can be elucidated from the 20-fold increment in thermal conductivity and the onset of degradation at higher temperatures (840 °C). Successful integration of multi-layered sandwich lattice using in-housed fabricated HfC decorated C nf showed retention of the fibrous structure even after extreme spark plasma sintering (SPS) process at 1850 °C. Fabricating a similar multi-layered structure using procured C f was unsuccessful due to bundled agglomeration and micron-sized fibers. High-load indentation suggests that HfC decorated C nf interlayer is stronger (~2.3 times) than the parent UHTC with no cracking at the interface. Compared with the HfC matrix, the indentation-damaged area at the interface reduced up to ~56% due to toughening mechanisms such as C nf , fiber pull-out and bridging. The synthesized HfC decorated Cnf mat is proposed as an ultra-thin filler material for joining similar or dissimilar UHTCs while maintaining similar chemistry and better mechanical integrity at the interface. Furthermore, the findings insinuate a new paradigm in designing hybrid and flexible ceramic-containing materials for thermal protection systems (TPS) of future-generation spacecraft components that can mitigate failure in extreme environments (>2000 °C).

36 MATERIALS SCIENCE↗

Mercury vapor hollow cathode component studies

An experimental study of starting and operating characteristics of conventional hollow cathodes and of hollow cathodes without alkaline earth emissive materials demonstrated that the emissive mix is essential to obtain the desired cathode operation. Loss of the emissive mix by evaporation and chemical reaction was measured. New insert designs consisting of emissive mix supported on nickel and of barium impregnated porous tungsten were studied. Cathodes with a modified orifice geometry operated in a low voltage, 'spot' mode over a broad range of discharge current. Thermal degradation tests on cathode heaters showed the flame sprayed SERT II type to be the most durable at high temperatures. Thermal shock was observed to be a significant factor in limiting cathode heater life. A cathode having a barium impregnated porous tungsten tip and a heater which is potted in sintered alumina was found to have favorable operating characteristics.

Zuccaro, D. E.↗

Radiant heating tests of several liquid metal heat-pipe sandwich panels

Integral heat pipe sandwich panels, which synergistically combine the thermal efficiency of heat pipes and the structural efficiency of honeycomb sandwich construction, were conceived as a means of alleviating thermal stress problems in the Langley Scramjet Engine. Test panels which utilized two different wickable honeycomb cores, facesheets with screen mesh sintered to the internal surfaces, and a liquid metal working fluid (either sodium or potassium) were tested by radiant heating at various heat load levels. The heat pipe panels reduced maximum temperature differences by 31 percent with sodium working fluid and 45 percent with potassium working fluid. Results indicate that a heat pipe sandwich panel is a potential, simple solution to the engine thermal stress problem. Other interesting applications of the concept include: cold plates for electronic component and circuit card cooling, radiators for large space platforms, low distortion large area structures (e.g., space antennas) and laser mirrors.

Camarda, C. J.↗

Sintering behavior of ultrafine silicon carbide powders obtained by vapor phase reaction

The sintering behavior of ultrafine SiC powder with average particle size of about 0.01-0.06 microns produced by a vapor phase reaction of the Me4Si-H2 system was studied at the temperature range of 1400-2050 deg. It was found that the homogeneous dispersion of C on SiC particles is important to remove the surface oxide layer effectively. B and C and inhibitive effect on SiC grain growth.

Okabe, Y.↗

Millimeter wave surface resistance of RBa2Cu3O(7-delta) (R=Y,Eu,Dy,Sm,Er) superconductors

The measurements are reported of the millimeter wave surface resistance R(sub s) at 58.6 GHz of bulk samples of RBa2Cu3O(7-delta) (R = Y,Eu,Dy,Sm,Er) and of YBa2Cu3O(7-delta) superconducting films, in the temperature range from 20 to 300 K. The bulk samples were prepared by cold pressing the powders of RBa2Cu3O(7-delta) into one in. disks. The powders were prepared by several sinterings in one atmosphere of oxygen at 925 C, with grindings between sinterings, to obtain the superconducting phase. The thin films were deposited on SrTiO3 and LaGaO3 substrates by pulsed laser ablation. Each sample was measured by replacing the end wall of a gold-plated Te sub 013 circular mode copper cavity with the sample and determining the cavity quality factor . From the difference in the Q-factor of the cavity, with and without the sample, the R(sub s) of the sample was determined.

Miranda, F. A.↗

Rhenium Redefined

Through a Small Business Innovation Research (SBIR) contract with NASA's Glenn Research Center, Rhenium Alloys, Inc., of Elyria, Ohio, developed a new method for producing rhenium combustion chambers. Using room temperature isostatic pressing, Rhenium Alloys, Inc., compacted rhenium powder to a high density and into the approximated end shape and dimension of the rocket thruster. The item was then subjected to sintering and containerless hot isostatic pressing, increasing the density of the powder metallurgy part. With the new manufacturing process, both production time and costs are reduced while quality is significantly increased. The method enabled the company to deliver two chemical rocket thrusters to Glenn Research Center. The company makes rhenium a practical choice in manufacturing fields, including the aerospace, nuclear, and electronic industries, with upcoming opportunities projected in medical instrumentation.

Source record↗

Synthesis and behavior of bulk iron nitride soft magnets via high-pressure spark plasma sintering

Abstract In this study, dense bulk iron nitrides (Fe x N) were synthesized for the first time ever using spark plasma sintering (SPS) of Fe x N powders. The Fe 4 N phase of iron nitride in particular has significant potential to serve as a new soft magnetic material in both transformer and inductor cores and electrical machines. The density of SPSed Fe x N increased with SPS temperature and pressure. The microstructure of the consolidated bulk Fe x N was characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. XRD revealed a primary phase of Fe 4 N with secondary phases of Fe 3 N and metallic iron. Finite element analysis (FEA) was also applied to investigate and explain localized heating and temperature distribution during SPS. The effects of processing on interface bonding formation and phase evolution were investigated and discussed in detail to provide insight into fundamental phenomena and microstructural evolution in SPSed Fe x N. Graphic abstract

36 MATERIALS SCIENCE↗

The evolution of model Rh/Fe 3 O 4 (001) catalysts in hydrogen environments

Single metal atoms dispersed on oxides are a new emerging class of catalysts owing to their unique electronic and chemical properties. Here, in this study, we have prepared a series of model single-atom catalysts possessing well-characterized Rh sites that include Rh adatoms (Rh ad ), mixed surface layers with octahedrally-coordinated Rh (Rh oct ), as well as metallic Rh clusters and nanoparticles (Rh met ) on Fe 3 O 4 (001). Using X-ray photoelectron spectroscopy (XPS) and scanning tunneling microscopy (STM), we investigated the activity of such model systems towards H2 and their stability in reducing environments. Our results show that the atomically dispersed Rhad and Rhoct species do not activate H 2 , which would result in the formation of surface hydroxyls on Fe 3 O 4 (001). In contrast, the presence of Rh met in H 2 results in the formation of hydroxyls and subsequent etching of the Fe 3 O 4 (001) at higher temperatures (≥ 500 K) due to water formation via the Mars-van Krevelen mechanism. Additionally, such surface etching leads to the release of the Rh oct from the surface lattice and their sintering to Rh met . To bridge the material gap between the surface science models and high surface area catalysts, we perform parallel studies on powder Rh/Fe 3 O 4 catalysts. The XPS characterization shows remarkable similarities between these systems. Further, our surface science studies provide an atomistic picture of the behavior of high surface area catalysts in the H 2 atmosphere.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Investigation of Cu Species in Dealuminated Beta Zeolite Studied by Operando Closed-Cell Gas Reaction STEM

Direct conversion of ethanol to C3+ olefins is an attractive pathway to produce sustainable aviation fuels [1]. We recently reported a copper-containing catalyst supported on dealuminated (DeAl) beta zeolite that is capable of catalyzing cascade ethanol to olefins reactions with high olefins selectivity (88% C3+ olefin selectivity at 100% ethanol conversion). However, one of the deactivation mechanisms of the catalyst is copper sintering [2]. It was found that copper agglomerates can be redispersed through a simple oxidative treatment. To better understand the kinetics and process conditions conducive to redispersion, we studied the atmosphere and temperature dependent Cu species in Cu/DeAl-Beta catalyst under conditions matching those of the working catalyst.

beta zeolite↗

Development of large-scale, 3D Printed high temperature ceramic material

Through this collaborative effort, a new 3D printing platform for ceramics called laser-induced slip casting (LIS) was explored and developed for improving the processing and manufacture of silicon carbide (SiC), a high temperature ceramic material. This method prints layers of ceramic slips/slurries with subsequent selective-laser heating to dry each layer to build a 3D structure. The completed and dried part is then sintered. This manufacturing process is inherently lower cost than alternative ceramic printing methods such as binder jet technology or stereolithography when it comes to the feedstock material but is more expensive than robocasting or direct ink writing. However, it has the potential to make more controlled parts with less defects compared to robocasting. The largest cost is the heating source for the printer. With this technique, there is potential to make large ceramic parts in a near-net shape. Further, there is no known commercial manufacturing of 3D printed ceramics that creates a large range of different high-density ceramics at large scale. The goals and outcomes for the development of the new printing technology were: 1) assessing the technology with alumina by characterizing coupons, 2) printing and sintering of silicon carbide (SiC), and 3) characterization and properties testing of materials printed and a scale-up of SiC part(s). Through this collaborative project, it was sought to provide the best solution to achieving highly dense and near-net shaped ceramic parts at large scale and reduced cost. The goal was to produce high density sintered materials for applications in defense, energy generating systems, armor, and wear parts using 3D printing methods. Variables including powder particle sizes, dispersant molecular weights (MWs), binders, printing parameters, and post processing were explored as well as the characterization of the physical properties (add specifics here).

36 MATERIALS SCIENCE↗

Production of superconductor/carbon bicomponent fibers

Certain materials are unable to be drawn or spun into fiber form due to their improper melting characteristics or brittleness. However, fibrous samples of such materials are often necessary for the fabrication of intricate shapes and composites. In response to this problem, a unique process, referred to as the piggyback process, was developed to prepare fibrous samples of a variety of nonspinnable ceramics. In this technique, specially produced C-shaped carbon fibers serve as micromolds to hold the desired materials prior to sintering. Depending on the sintering atmosphere used, bicomponent or single component fibers result. While much has been demonstrated worldwide concerning the YBa2Cu3O(7-x) superconductor, fabrication into unique forms has proven quite difficult. However, a variety of intricate shapes are necessary for rapid commercialization of the superconducting materials. The potential for producing fibrous samples of the YBa2Cu3O(7-x) compound by the piggyback process is being investigated. Various organic and acrylic materials were investigated to determine suspending ability, reactivity with the YBa2Cu3O(7-x) compound during long term storage, and burn out characteristics. While many questions were answered with respect to the interfacial reactions between YBa2Cu3O(7-x) and carbon, much work is still necessary to improve the quality of the sintered material if the fibers produced are to be incorporated into useful composites or cables. Additional research is necessary to evaluate quality of the barrier layer during long soakings at the peak temperature; adjust the firing schedule to avoid microcracking and improve densification; and increase the solids loading in the superconductive suspension to decrease porosity.

Wise, S. A.↗

The liquid/vapor boundary in a porous plug

Results are presented from measurements of pressure and temperature differences as a function of the flow rate and hydrostatic head for two types of porous plugs for phase separation of superfluid He and He vapor: (1) a plug made of sintered stainless steel, similar to that in the IRAS, IRT, and COBE dewars except for larger pores, and (2) a glass plug with pores of uniform cross section. Results show that a liquid/vapor phase boundary exists at the outer surface of the porous plug for low flows or large hydrostatic heads; as the flow increases or the hydrostatic head decreases, the boundary retreats into the plug. Some hysteresis near the phase boundary retreat was observed in the stainless steel plug.

Dipirro, M. J.↗

Principles of gas phase processing of ceramics during combustion

In recent years, ceramic materials have found applications in an increasingly wider range of industrial processes, where their unique mechanical, electrical and optical properties are exploited. Ceramics are especially useful for applications in high temperature, corrosive environments, which impose particularly stringent requirements on mechanical reliability. One approach to provide such materials is the manufacture of submicron (and more recently nanometer scale) particles, which may subsequently be sintered to produce a material with extremely high mechanical integrity. However, high quality ceramic materials can only be obtained if particles of known size, polydispersity, shape and chemical purity can be produced consistently, under well controlled conditions. These requirements are the fundamental driving force for the renewed interest in studying particle formation and growth of such materials.

Zachariah, Michael R.↗

Thermal Conductivity of Ceramic Thermal Barrier and Environmental Barrier Coating Materials

Thermal barrier and environmental barrier coatings (TBC's and EBC's) have been developed to protect metallic and Si-based ceramic components in gas turbine engines from high temperature attack. Zirconia-yttria based oxides and (Ba,Sr)Al2Si2O8(BSAS)/mullite based silicates have been used as the coating materials. In this study, thermal conductivity values of zirconia-yttria- and BSAS/mullite-based coating materials were determined at high temperatures using a steady-state laser heat flux technique. During the laser conductivity test, the specimen surface was heated by delivering uniformly distributed heat flux from a high power laser. One-dimensional steady-state heating was achieved by using thin disk specimen configuration (25.4 mm diam and 2 to 4 mm thickness) and the appropriate backside air-cooling. The temperature gradient across the specimen thickness was carefully measured by two surface and backside pyrometers. The thermal conductivity values were thus determined as a function of temperature based on the 1-D heat transfer equation. The radiation heat loss and laser absorption corrections of the materials were considered in the conductivity measurements. The effects of specimen porosity and sintering on measured conductivity values were also evaluated.

Zhu, Dong-Ming↗

Role of phosphate source in improving the proton conductivity of tin pyrophosphate and its composite electrolytes

Metal pyrophosphates (MPPs) in general, and tin pyrophosphate (TPP) in particular, have received significant interest in the last decade due to their potential as proton conductors for electrolyte application in intermediate temperature (IT)-fuel cells. However, for MPP based electrolytes, despite high reported proton conductivities, achieving good fuel cell performance and high open circuit voltage (OCV) remains a challenge with synthesis methods playing a crucial role in determining the final proton conductivity. Here we report the role of phosphate precursor in determining the TPP proton conductivity by examining five different precursors: (1) phosphoric acid (TPP-PA), (2) ammonium hydroxide + phosphoric acid (TPP-NH 4 OH), (3) diammonium phosphate (TPP-DAP), (4) tetramethylammonium sulphate + phosphoric acid (TPP-TMAP), and (5) tetrabutylammonium phosphate (TPP-TBAP), where a maximum conductivity of 88 mS cm -1 at 200 °C was obtained for TPP prepared from the TBAP precursor. TPP prepared from all of the different precursors formed the crystalline cubic Pa-3 with combining macron] phase after sintering at 650 °C for 2.5 hours. Furthermore, TPP-TBAP/Nafion® composite membranes prepared with a 90 : 10 ratio exhibited an OCV of 0.98 V and produced a maximum peak power density (PPD) of 630 mW cm -2 at an operating temperature of 220 °C. Our results demonstrate the significant impact of the TPP precursor on proton conductivity and fuel cell performance.

36 MATERIALS SCIENCE↗

Neural Learning Based Blind Source Separation for Detection of Material Defects in Pulsed Thermography Images

In this paper, we introduce a neural learning-based approach to blind source separation for detection of material flaws in pulsed thermography (PT) images. This approach can be used to detect internal defects (pores) in metallic Additively Manufactured (AM) materials. Such defects occur in high-strength alloys produced with direct laser sintering AM method for nuclear energy applications. Pulsed thermal imaging system utilizes a high intensity flash lamp to rapidly heat surface of sample, a high sensitivity infrared camera to capture data of surface temperature variations. The data cube obtained with PT (stack of surface temperature images at different times) can be analyzed with image processing algorithms to detect material defects. Compared with conventional nondestructive evaluation (NDE) methods, such as digital radiography and ultrasonic testing, the PT pulsed infrared thermal detection technique has advantages of one-sided non-contact measurements, fast processing of large sample areas captured in one image. Detection of small material defects requires finding features in thermal images, which have signal contrast levels approaching sensitivity limit of IR camera. In this study, an optimized Neural Learning based Blind Source Separation (NLBSS) algorithm, including Principal Component Analysis (PCA), and Independent Component Analysis (ICA) is demonstrated to automatically extract principal temporal and spatial features of thermography frames to enhance flaw detection. By using the NLBSS algorithm, material internal defects can be automatically detected. Furthermore, this processing approach compensates for experimental thermal imaging artifacts, such as noise and uneven heating. By merging artificial intelligence with the photothermic, the NDE system detects internal calibrated defects of various sizes and depths in AM nuclear-grade metallic alloys.

Zhang, Xin↗

Radiant heating tests of several liquid metal heat-pipe sandwich panels

Integral heat-pipe sandwich panels, which synergistically combine the thermal efficiency of heat pipes and the structural efficiency of honeycomb sandwich construction, were conceived as a means of alleviating thermal stress problems in the Langley Scramjet Engine. Test panels which utilized two different wickable honeycomb cores, facesheets with screen mesh sintered to the internal surfaces, and a liquid metal working fluid (either sodium or potassium) were tested by radiant heating at various heat-load levels. The heat-pipe panels reduced maximum temperature differences by 31 percent with sodium working fluid and 45 percent with potassium working fluid. Results indicate that a heat-pipe sandwich panel is a potential, simple solution to the engine thermal stress problem. Other interesting applications of the concept include: cold plates for electronic component and circuit card cooling, radiators for large space platforms, low-distortion large area structures (e.g., space antennas) and laser mirrors.

Camarda, C. J.↗