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At least 1,261 records · Page 70

The structural and electrical properties of low-resistance Ni contacts to InP

We have investigated the electrical and metallurgical behavior of the Ni-InP contact system. Specific contact resistivity (Rc) values in the low 10 exp -7 Omega-sq cm range are achieved with Ni-only contacts on n-InP by sintering at 400 C for several minutes. The postsinter contact metallization consists of three layers, arranged in the sequence: InP/Ni3P/Ni2P/In. Extended sintering (40 min) at 400 C brings about a rise in Rc to the 10 exp -4 Omega-sq cm range. After extended sintering, the contact metallization is found to consist of only two layers, arranged in the sequence: InP/Ni2P/In. Based on the correlation between low Rc and the presence of Ni3P at the metal-InP interface, it is suggested that the presence of Ni3P is the cause of the low Rc values. We show that the sintering schedule used to achieve low values of Rc is accompanied by substantial metal-InP interdiffusion that results in severe device degradation.

Fatemi, Navid S.↗

Corrosion Issues for Ceramics in Gas Turbines

The requirements for hot-gas-path materials in gas turbine engines are demanding. These materials must maintain high strength and creep resistance in a particularly aggressive environment. A typical gas turbine environment involves high temperatures, rapid gas flow rates, high pressures, and a complex mixture of aggressive gases. Figure 26.1 illustrates the requirements for components of an aircraft engine and critical issues [1]. Currently, heat engines are constructed of metal alloys, which meet these requirements within strict temperature limits. In order to extend these temperature limits, ceramic materials have been considered as potential engine materials, due to their high melting points and stability at high temperatures. These materials include oxides, carbides, borides, and nitrides. Interest in using these materials in engines appears to have begun in the 1940s with BeO-based porcelains [2]. During the 1950s, the efforts shifted to cermets. These were carbide-based materials intended to exploit the best properties of metals and ceramics. During the 1960s and 1970s, the silicon-based ceramics silicon carbide (SiC) and silicon nitride (Si3N4) were extensively developed. Although the desirable high-temperature properties of SiC and Si3N4 had long been known, consolidation of powders into component-sized bodies required the development of a series of specialized processing routes [3]. For SiC, the major consolidation routes are reaction bonding, hot-pressing, and sintering. The use of boron and carbon as additives which enable sintering was a particularly noteworthy advance [4]. For Si3N4 the major consolidation routes are reaction bonding and hot pressing [5]. Reaction-bonding involves nitridation of silicon powder. Hot pressing involves addition of various refractory oxides, such as magnesia (MgO), alumina (Al2O3), and yttria (y2O3). Variations on these processes include a number of routes including Hot Isostatic Pressing (HIP), gas-pressure sintering, sinter-HIPing, and Encapsulation-HIPing. It is important to note that each process involves the addition of secondary elements, which later were shown to dramatically influence oxidation and corrosion behavior. As dense bodies of silicon-based ceramics became more readily available, their desirable high temperature properties were confirmed. These materials retained strength to very high temperatures (i.e. 1300-1400 C). Further, they were lightweight and made from abundant materials. SiC and Si3N4 therefore emerged as leading ceramic candidates for components in heat engines, designed to operate at higher temperatures for better performance and fuel efficiency. The first US programs for ceramics in heat engines have been reviewed [6]. Selected programs on ceramic engine parts are summarized here in regard to their contributions to understanding the corrosion behavior of a heat engine environment.

Jacobson, Nathan S.↗

Fossilization Processes in Thermal Springs

To create a comparative framework for the study of ancient examples, we have been carrying out parallel studies of the microbial biosedimentology, taphonomy and geochemistry of modem and sub-Recent thermal spring deposits. One goal of the research is the development of integrated litho- and taphofacies models for siliceous and travertline sinters. Thermal springs are regarded as important environments for the origin and early evolution of life on Earth, and we seek to utilize information from the fossil record to reconstruct the evolution of high temperature ecosystems. Microbial contributions to the fabric of thermal spring sinters occur when population growth rates keep pace with, or exceed rates of inorganic precipitation, allowing for the development of continuous biofilms or mats. In siliceous thermal springs, microorganisms are typically entombed while viable. Modes of preservation reflect the balance between rates of organic matter degradation, silica precipitation and secondary infilling. Subaerial sinters are initially quite porous and permeable and at temperatures higher than about 20 C, organic materials are usually degraded prior to secondary infilling of sinter frameworks. Thus, organically-preserved microfossils are rare and fossil information consists of characteristic biofabrics formed by the encrustation and underplating of microbial mat surfaces. This probably accounts for the typically low total organic carbon values observed in thermal spring deposits. In mid-temperature, (approx. 35 - 59 C) ponds and outflows, the surface morphology of tufted Phormidium mats is preserved through mat underplating by thin siliceous: crusts. Microbial taxes lead to clumping of ceils and/or preferred filament orientations that together define higher order composite fabrics in thermal spring stromatolites (e.g. network, coniform, and palisade). At lower temperatures (less than 35 C), Calothrix mats cover shallow terracette pools forming flat carpets or pustular surfaces that produce palisade and "shrub" fabrics, respectively. At finer scales, composite fabrics are seen to consist distinctive associations of microstructures formed by the encrustation of individual cells and filaments. Composite fabrics survive the diagenetic transitions from primary opaline silica to quartz and are known from subaerial thermal spring deposits as old as Lower Carboniferous. However, fossil microorganisms tend to be rare in older deposits, and are usually preserved only where cells or sheaths have been stained by iron oxides. In subaqueous mineralizing springs at lower temperatures, early infilling leads to a more rapid and complete reduction in porosity and permeability. This process, along with the slower rates of microbial degradation at lower temperatures, creates a more favorable situation for organic matter preservation. Application of this taphonomic model to the Rhynie Chert, previously interpreted as subaerial, suggest it was probably deposited in a subaqueous spring setting at lower temperatures.

Farmer, Jack D.↗

Pulsed Laser Deposition of BaCe(sub 0.85)Y(sub 0.15)0(sub 3) FILMS

Pulsed laser deposition has been used to grow nanostructured BaCe(sub 0.85)Y(sub 0.15)0(sub 3) films. The objective is to enhance protonic conduction by reduction of membrane thickness. Sintered samples and laser targets were prepared by sintering BaCe(sub 0.85)Y(sub 0.15)O(sub 3) powders derived by solid state synthesis. Films 2 to 6 m thick were deposited by KrF excimer laser on Si and porous Al2O3 substrates. Nanocrystalline films were fabricated at deposition temperatures of 600-800 C deg at O2 pressure of 30 mTorr and laser fluence of 1.2 J/cm square. Films were characterized by x-ray diffraction, scanning electron microscopy and electrical impedance spectroscopy. Dense single phase BaCe(sub 0.85)Y((sub 0.15) 0(sub 3) films with a columnar growth morphology is observed, preferred crystal growth was found to be dependent upon deposition temperature and substrate type. Electrical conductivity of bulk samples produced by solid state sintering and thin film samples were measured over a temperature range of 100 C deg to 900 C deg in moist argon. Electrical conduction of the fabricated films was 1 to 4 orders of magnitude lower than the sintered bulk samples. With respect to the film growth direction, activation energy for electrical conduction is 3 times higher in the perpendicular direction than the parallel direction.

Dynys, F. W.↗

Method for fabricating ceramic filaments and high density tape casting method

An apparatus and method is disclosed for fabricating mats of ceramic material comprising preparing a slurry of ceramic particles in a binder/solvent, charging the slurry into a vessel, forcing the slurry from the vessel into spinneret nozzles, discharging the slurry from the nozzles into the path of airjets to enhance the sinuous character of the slurry exudate and to dry it, collecting the filaments on a moving belt so that the filaments overlap each other thereby forming a mat, curing the binder therein, compressing and sintering the mat to form a sintered mat, and crushing the sintered mat to produce filament shaped fragments. A process is also disclosed for producing a tape of densely packed, bonded ceramic particles comprising forming a slurry of ceramic particles and a binder/solvent, applying the slurry to a rotating internal molding surface, applying a large centrifugal force to the slurry to compress it and force excess binder/solvent from the particles, evaporating solvent and curing the binder thereby forming layers of bonded ceramic particles and cured binder, and separating the binder layer from the layer of particles. Multilayers of ceramic particles are cast in an analogous manner on top of previously formed layers. When all of the desired layers have been cast the tape is fired to produce a sintered tape. For example, a three-layer tape is produced having outer layers of highly compressed filament shaped fragments of strontium doped lanthanum (LSM) particles and a center layer of yttria stabilized zicronia (YSZ) particles.

Collins, Jr., Earl R.↗

High Thermal Conductivity NARloy-Z-Diamond Composite Combustion Chamber Liner For Advanced Rocket Engines

Advanced high thermal conductivity materials research conducted at NASA Marshall Space Flight Center (MSFC) with state of the art combustion chamber liner material NARloy-Z showed that its thermal conductivity can be increased significantly by adding diamond particles and sintering it at high temperatures. For instance, NARloy-Z containing 40 vol. percent diamond particles, sintered at 975C to full density by using the Field assisted Sintering Technology (FAST) showed 69 percent higher thermal conductivity than baseline NARloy-Z. Furthermore, NARloy-Z-40vol. percent D is 30 percent lighter than NARloy-Z and hence the density normalized thermal conductivity is 140 percent better. These attributes will improve the performance and life of the advanced rocket engines significantly. By one estimate, increased thermal conductivity will directly translate into increased turbopump power up to 2X and increased chamber pressure for improved thrust and ISP, resulting in an expected 20 percent improvement in engine performance. Follow on research is now being conducted to demonstrate the benefits of this high thermal conductivity NARloy-Z-D composite for combustion chamber liner applications in advanced rocket engines. The work consists of a) Optimizing the chemistry and heat treatment for NARloy-Z-D composite, b) Developing design properties (thermal and mechanical) for the optimized NARloy-Z-D, c) Fabrication of net shape subscale combustion chamber liner, and d) Hot fire testing of the liner for performance. FAST is used for consolidating and sintering NARlo-Z-D. The subscale cylindrical liner with built in channels for coolant flow is also fabricated near net shape using the FAST process. The liner will be assembled into a test rig and hot fire tested in the MSFC test facility to determine performance. This paper describes the development of this novel high thermal conductivity NARloy-Z-D composite material, and the advanced net shape technology to fabricate the combustion chamber liner. Properties of optimized NARloy-Z-D composite material will also be presented.

Bhat, Biliyar N.↗

Method to synthesize bulk iron nitride

Bulk iron nitride can be synthesized from iron nitride powder by spark plasma sintering. The iron nitride can be spark plasma sintered at a temperature of less than 600°C. and a pressure of less than 600 MPa, with 400 MPa or less most often being sufficient. High pressure SPS can consolidate dense iron nitrides at a lower temperature to avoid decomposition. The higher pressure and lower temperature of spark discharge sintering avoids decomposition and limits grain growth, enabling enhanced magnetic properties. The method can further comprise synthesis of nanocrystalline iron nitride powders using two-step reactive milling prior to high-pressure spark discharge sintering.

36 MATERIALS SCIENCE↗

DC bulk conductive ceramic with low RF and microwave loss

A DC conductive, low RF/microwave loss titanium oxide ceramic provides, at room temperature, a bulk DC resistivity of less than 1×10 11 ohm-meters and an RF loss tangent of less than 2×10 −4 at 7.5 GHz and less than 2×10 −5 at 650 MHz. The resistivity is reduced by oxygen vacancies and associated Ti 3+ and/or Ti 4+ centers created by sintering in an atmosphere containing only between 0.01% and 0.1% oxygen. The reduced resistivity prevents DC charge buildup, while the low loss tangent provides good RF/microwave transparency and low losses. The ceramic is suitable for forming RF windows, electron gun cathode insulators, dielectrics, and other components. An exemplary Mg 2 TiO 4 —MgTiO 3 embodiment includes mixing, grinding, pre-sintering in air, and pressing 99.95% pure MgO and TiO 2 powders, re-sintering in air at 1400° C.-1500° C. to reduce porosity, and sintering at 1350° C.-1450° C. for 4 hours in an 0.05% oxygen and 99.05% nitrogen atmosphere.

Kanareykin, Alexei↗

Microstructure development of novel composite heating elements for steel decarbonization

The iron and steel industry is critical for the modern world but is also responsible for 7% of the total energy sector CO2 emissions. It is a difficult industry to decarbonize due to the high temperature heat required for the production of steel, such as reheating steel slabs to ~1250 °C for hot rolling. Electrification of this process using resistive heating is currently not possible due to the poor creep resistance of MoSi2 heating elements, which need to be operated well below their maximum temperatures when mounted horizontally. To solve this problem, novel MoSi2 composite heating elements with SiBCN ceramic reinforcements are being developed using high energy ball milling and electric field assisted sintering (EFAS). The microstructure and density of the composites after sintering depends on the sintering parameters chosen. Herein we present the effects of EFAS sintering parameters on the microstructure and density of the MoSi2-SiBCN composites.

36 - MATERIALS SCIENCE↗

Embedding of Fiber Optic Sensors in Stainless Steel for Sensing in Harsh Environments

Structural health monitoring is critical for components working in harsh environments to assess their safety and integrity. This can be realized with advanced sensors, such as fiber optic sensors, embedded in these components. Recent studies have used ultrasonic consolidation (UC) and laser-based additive manufacturing (AM) techniques to embed fiber optic sensors in metals. However, sensor embedding using these techniques has been challenging, with gaps and voids around the embedded fiber. Successful embedding of fiber optic sensors requires good contact between the fiber and the matrix to eliminate potential gas/liquid leaks in critical systems such as in nuclear and aerospace services. Defect-free fiber/matrix bond is also essential for accurate measurement of parameters of interest, such as temperature and strain. This study developed a novel fiber embedding technique based on electric field-assisted sintering (EFAS). Sapphire optical fibers with diameters of 125 µm and 250 µm were embedded in stainless steel (SS) 316L using EFAS. The embedding was completed by sintering SS 316L powders at a pressure of 50MPa, hold time of 5 min, and temperatures of 1000°C, 1100°C, and 1200°C. Joule heating mechanism during EFAS enabled rapid sintering of the SS 316L powder with resulting sample densities over 99%. Microscopy analysis performed on the cross-sections revealed a defect-free bond between the embedded fiber and SS 316L. The good integrity of the embedded fiber was evidenced by optical transmittance measurement. Optical attenuation of the fiber before and after embedment was examined in the near-infrared region. Scanning electron microscopy was employed to investigate the grain morphology of SS 316L near the embedded fiber. Hardness distribution in the sintered part was also investigated to study the effect of the embedded fiber on the mechanical properties of the as-fabricated component. The results indicated that EFAS was able to embed fiber in SS with good fiber functionality and part quality.

36 - MATERIALS SCIENCE↗

Effect of Aluminum Dissolved in Hematite on Formation of Calcium Ferrites at 1473 K

Silico-ferrite of calcium and aluminum (SFCA) is a primary bonding phase, which determines the quality of high basicity sinter used widely as raw materials in blast furnace ironmaking. Calcium ferrite containing aluminum (CFA) is a key precursor during the formation process of SFCA and is influenced by Al{sub 2}O{sub 3} content in iron ore fines. In this work, the experiment was conducted to investigate the effect of the aluminum occurrence state on the formation of calcium ferrite by the simulating sintering process of different types of aluminum-bearing hematite at 1473 K. X-ray diffraction, optical microscope, scanning electron microscopy, and energy-dispersive spectroscopy were used to characterize the mineral change in sintered samples. The result shows that the formation of CFA was promoted by both granular Al{sub 2}O{sub 3} wrapped in Fe{sub 2}O{sub 3} and aluminum dissolved in Fe{sub 2}O{sub 3} solid solution, especially for the latter, due to the formation of the CFA directly from the reaction between Fe{sub 2}O{sub 3}-Al{sub 2}O{sub 3} solid solution and CaO, and the aluminum content in CFA formed was influenced obviously by the solid solution amount of alumina into Fe{sub 2}O{sub 3} as raw materials.

36 MATERIALS SCIENCE↗

Powder bed binder jet 3D printing of Inconel 718: Densification, microstructural evolution and challenges

Traditional manufacturing of Inconel 718 components from castings and thermomechanical processing routes involve extensive post processing and machining to attain the desired geometry. Additive manufacturing (AM) technologies including direct energy deposition (DED), selective laser melting (SLM), electron beam melting (EBM) and binder jet 3D printing (BJ3DP) can minimize scrap generation and reduce lead times. While there is extensive literature on the use of melting and solidification based AM technologies, there has been limited research on the use of binder jet 3D printing. In this paper, a brief review on binder jet additive manufacturing of Inconel 718 is presented. In addition, existing knowledge on sintering of Inconel 718 has been extended to binder jet 3D printing. We found that supersolidus liquid phase sintering (SLPS) is necessary to achieve full densification of Inconel 718. SLPS is sensitive to the feedstock chemistry that has a strong influence on the liquid volume fraction at the processing temperature. Based on these results, we discuss an empirical framework to determine the role of powder particle size and liquid volume fraction on sintering kinetics. In conclusion, the role of powder packing factor and binder saturation on microstructural evolution is discussed. The current challenges in the use of BJ3DP for fabrication of Inconel 718, as well as, extension to other metal systems, are presented.

36 MATERIALS SCIENCE↗

Entrapment Behavior of Solid Surrogate Fission Products at Engineered UN Nano‐Hetero‐Interfaces Within Metallic Nuclear Fuels

Nanometric hetero-interfaces provide a wealth of scientific and engineering opportunities due to their complex and often misunderstood properties that can differ from their respective bulk constituents. In this work, the ability for engineered nanostructures within a bulk U─Mo alloy to arrest simulant fission products is investigated experimentally and computationally. Nanostructured 90 wt% U/ 10 wt% Mo (U-10Mo) with 7.1 at% Nd is consolidated using spark-plasma- sintering (SPS) techniques and is heat-treated at 500 °C under vacuum for 24, 100, 500, and 1000 h. Analysis on the sintered and heat-treated U-10Mo reveals rapid kinetics in Nd diffusion to nanocluster sites, with evidence of Nd diffusion occurring during sintering and during the following heat-treatment. The segregation behavior of Nd at two different U─Mo/UN interfaces is computationally verified using density functional theory (DFT) to reinforce experimental data.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Time-Dependent Diffusion Coefficient of Fe in MgB{sub 2} Superconductors

The iron (Fe) diffusion in superconducting MgB{sub 2} bulk samples has been studied for sintering time durations of 15 min, 30 min, 1 h, 2 h, and 4 h at 900{sup ∘}C. Fe coating bulk polycrstalline superconducting MgB{sub 2} samples for Fe coating were prepared by pelletizing and used in the diffusion experiments with initial sintering at 800{sup ∘}C for 1 h. A thin layer of Fe was coated on MgB{sub 2} pellets by evaporation in vacuum. Effects of Fe diffusion on the structural, electrical, and superconducting properties of MgB{sub 2} have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (IR), energy-dispersive X-ray spectroscopy (EDS), and resistivity measurements. Fe diffused samples have slightly increased critical transition temperatures and have larger lattice parameter c values, in comparison with bare samples. Fe diffusion coefficients were calculated from depth profiles of c parameter and room temperature resistivity values. Depth profiles were obtained by successive removal of thin layers from Fe diffused surfaces of the samples. Our results have shown that the Fe diffusion coefficient decreases with increasing sintering time and resistivity measurements can be utilized for determination of diffusion coefficient.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Investigation of Superparamagnetism in Microwave and Conventional Processed Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} Nanoparticles

Nanoparticles of spinel cubic Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} are first prepared by the coprecipitation method and then subjected to conventional solid-state sintering and microwave processing techniques. Particle sizes are estimated by field emission scanning electron microscopy (FESEM) to be in the nanometer (5–13 nm) range. Transmission electron microscopy (TEM) also supports the FESEM data. The magnetization measurement by vibration sample magnetometry of the conventionally sintered sample shows a paramagnetic nature at room temperature, a superparamagnetic behaviour at low temperature, and a ferromagnetic nature at even lower temperature. The blocking temperature is estimated to be nearly 110 K. Microwave-processed samples show a superparamagnetic nature even at room temperature. The Fe{sup 3+} cations are found at both the sites confirmed by X-ray photoelectron spectroscopy (XPS), are prepared by microwave processing, and have better magnetic properties as compared to the conventionally sintered particles.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Structural Characterization and Magnetic Properties of SrCo{sub 2}Fe{sub 16}O{sub 27} Hexaferrite Synthesized by Citric Acid Sol-Gel Method

The W -type SrCo{sub 2}Fe{sub 16}O{sub 27} (SCFO) hexagonal ferrite samples were prepared by the sol-gel method using metal nitrate as raw material, citric acid as complexing agent, and water as solvent. The effects of different sintering temperatures and holding times on the phase composition and morphology properties were explored in detail by using the X-ray diffractometer and field emission scanning electron microscope. The X-ray diffraction, microstructure, and magnetic performance of most optimum sintering temperature and holding time of preparing single-phase SCFO hexagonal ferrite were investigated. The experimental results indicate that the best optimum sintering temperature and holding time of SCFO hexagonal ferrite are 1280 °C and 4 h, respectively. Field emission scanning electron microscopy results indicate that the size of the particles is about 5–10 μ m. The result of magnetic measurement shows that SCFO hexagonal ferrite exhibits the soft magnetic property and the Curie temperature (T{sub C}) is ∼ 850 K. Furthermore, by analyzing the Arrott plot, the phase transition near the T{sub C} is a secondary phase transition.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of TiO{sub 2} Addition on Grain Growth, Anodic Bubble Evolution and Anodic Overvoltage of NiFe{sub 2}O{sub 4}-Based Composite Inert Anodes

A two-step powder compaction and sintering process was employed to fabricate TiO{sub 2}-doped NiFe{sub 2}O{sub 4} ceramic-based inert anodes. Grain growth during isothermal sintering was analyzed using Brook grain growth model. The bubble behavior of NiFe{sub 2}O{sub 4} ceramic-based inert anodes was investigated in a two-compartment see-through quartz cell for aluminum electrolysis process. Anodic overvoltage and potential decay curves of the inert anodes were measured by using the steady state and current interruption technique. The results showed that the kinetic index of grain growth decreased with an increase in temperature. The average activation energy of grain growth for 1.0 wt.% TiO{sub 2}-doped NiFe{sub 2}O{sub 4} ceramic samples with a sintering temperature range from 1373 to 1673 K dropped from 675.30 to 183.47 kJ/mol. The diameter size of bubbles before releasing from the bottom surface of the anodes was reduced with increasing the current density, and the larger average releasing bubble size for carbon anode at the same current density could be obtained, which was compared to the NiFe{sub 2}O{sub 4} inert anodes. Besides, the cell voltage of carbon anodes fluctuated much more violently under the same experimental conditions. After adding small amount of TiO{sub 2}, a minor reduction in anodic overvoltage of NiFe{sub 2}O{sub 4}-based anodes can be observed.

36 MATERIALS SCIENCE↗

Analyzing the Effect of CeB{sub 6} on Microstructure and Mechanical Properties of High-Speed Steel Consolidated by Powder Metallurgy

By adding various amounts of CeB{sub 6}, high-speed steel (M3:2) was consolidated by powder metallurgy in the form of sintering. The addition of CeB{sub 6} improved the density of the sintered steel and the formation of M{sub 6}C phase in microstructure. It is speculated that CeB{sub 6} was decomposed into boron and cerium. Boron atoms were enriched in M{sub 6}C carbide phases, but cerium atoms were mainly clustered on grain boundary while they were converted to oxides, whereby the mechanical properties were improved. For example, upon the sintering at 1210 °C, relative density ~ 98.5% and average grain size ~ 18 μm were obtained with CeB{sub 6} content at 0.3 wt.%. Excellent mechanical properties, e.g., the Rockwell hardness ~ 52 HRC, flexural strength ~ 3.05 GPa, and fracture toughness ~ 40.92 MPa m{sup 1/2}, were achieved in the sample containing 0.3 wt.% CeB{sub 6}, which implies accordingly remarkable increases by 23.5, 38.1, and 23.7%, of the properties compared with those in the sample free of CeB{sub 6}.

36 MATERIALS SCIENCE↗