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At least 433 records · Page 24

Development and Characterization of the Bonding and Integration Technologies Needed for Fabricating Silicon Carbide Based Injector Components

Advanced ceramic bonding and integration technologies play a critical role in the fabrication and application of silicon carbide based components for a number of aerospace and ground based applications. One such application is a lean direct injector for a turbine engine to achieve low NOx emissions. Ceramic to ceramic diffusion bonding and ceramic to metal brazing technologies are being developed for this injector application. For the diffusion bonding technology, titanium interlayers (coatings and foils) were used to aid in the joining of silicon carbide (SiC) substrates. The influence of such variables as surface finish, interlayer thickness, and processing time were investigated. Electron microprobe analysis was used to identify the reaction formed phases. In the diffusion bonds, an intermediate phase, Ti5Si3Cx, formed that is thermally incompatible in its thermal expansion and caused thermal stresses and cracking during the processing cool-down. Thinner interlayers of pure titanium and/or longer processing times resulted in an optimized microstructure. Tensile tests on the joined materials resulted in strengths of 13-28 MPa depending on the SiC substrate material. Nondestructive evaluation using ultrasonic immersion showed well formed bonds. For the joining technology of brazing Kovar fuel tubes to silicon carbide, preliminary development of the joining approach has begun. Various technical issues and requirements for the injector application are addressed.

Halbig,Michael C.↗

Bonding and Integration Technologies for Silicon Carbide Based Injector Components

Advanced ceramic bonding and integration technologies play a critical role in the fabrication and application of silicon carbide based components for a number of aerospace and ground based applications. One such application is a lean direct injector for a turbine engine to achieve low NOx emissions. Ceramic to ceramic diffusion bonding and ceramic to metal brazing technologies are being developed for this injector application. For the diffusion bonding, titanium interlayers (PVD and foils) were used to aid in the joining of silicon carbide (SiC) substrates. The influence of such variables as surface finish, interlayer thickness (10, 20, and 50 microns), processing time and temperature, and cooling rates were investigated. Microprobe analysis was used to identify the phases in the bonded region. For bonds that were not fully reacted an intermediate phase, Ti5Si3Cx, formed that is thermally incompatible in its thermal expansion and caused thermal stresses and cracking during the processing cool-down. Thinner titanium interlayers and/or longer processing times resulted in stable and compatible phases that did not contribute to microcracking and resulted in an optimized microstructure. Tensile tests on the joined materials resulted in strengths of 13-28 MPa depending on the SiC substrate material. Non-destructive evaluation using ultrasonic immersion showed well formed bonds. For the joining technology of brazing Kovar fuel tubes to silicon carbide, preliminary development of the joining approach has begun. Various technical issues and requirements for the injector application are addressed.

Halbig, Michael C.↗

Rapid Fabrication of Carbide Matrix/Carbon Fiber Composites

Composites of zirconium carbide matrix material reinforced with carbon fibers can be fabricated relatively rapidly in a process that includes a melt infiltration step. Heretofore, these and other ceramic matrix composites have been made in a chemical vapor infiltration (CVI) process that takes months. The finished products of the CVI process are highly porous and cannot withstand temperatures above 3,000 F (approx.1,600 C). In contrast, the melt-infiltration-based process takes only a few days, and the composite products are more nearly fully dense and have withstood temperatures as high as 4,350 F (approx.2,400 C) in a highly oxidizing thrust chamber environment. Moreover, because the melt- infiltration-based process takes much less time, the finished products are expected to cost much less. Fabrication begins with the preparation of a carbon fiber preform that, typically, is of the size and shape of a part to be fabricated. By use of low-temperature ultraviolet-enhanced chemical vapor deposition, the carbon fibers in the preform are coated with one or more interfacial material(s), which could include oxides. The interfacial material helps to protect the fibers against chemical attack during the remainder of the fabrication process and against oxidation during subsequent use; it also enables slippage between the fibers and the matrix material, thereby helping to deflect cracks and distribute loads. Once the fibers have been coated with the interfacial material, the fiber preform is further infiltrated with a controlled amount of additional carbon, which serves as a reactant for the formation of the carbide matrix material. The next step is melt infiltration. The preform is exposed to molten zirconium, which wicks into the preform, drawn by capillary action. The molten metal fills most of the interstices of the preform and reacts with the added carbon to form the zirconium carbide matrix material. The zirconium does not react with the underlying fibers because they are protected by the interfacial material(s). The success of the melt-infiltration step depends on interface material selection and uniform coating of the fibers, infiltration with the correct amount of carbon, and careful control of temperature and rate of heating.

Williams, Brian E.↗

Silicon Carbide Mounts for Fabry-Perot Interferometers

Etalon mounts for tunable Fabry- Perot interferometers can now be fabricated from reaction-bonded silicon carbide structural components. These mounts are rigid, lightweight, and thermally stable. The fabrication of these mounts involves the exploitation of post-casting capabilities that (1) enable creation of monolithic structures having reduced (in comparison with prior such structures) degrees of material inhomogeneity and (2) reduce the need for fastening hardware and accommodations. Such silicon carbide mounts could be used to make lightweight Fabry-Perot interferometers or could be modified for use as general lightweight optical mounts. Heretofore, tunable Fabry-Perot interferometer structures, including mounting hardware, have been made from the low-thermal-expansion material Invar (a nickel/iron alloy) in order to obtain the thermal stability required for spectroscopic applications for which such interferometers are typically designed. However, the high mass density of Invar structures is disadvantageous in applications in which there are requirements to minimize mass. Silicon carbide etalon mounts have been incorporated into a tunable Fabry-Perot interferometer of a prior design that originally called for Invar structural components. The strength, thermal stability, and survivability of the interferometer as thus modified are similar to those of the interferometer as originally designed, but the mass of the modified interferometer is significantly less than the mass of the original version.

Lindemann, Scott↗

Development of an Extreme High Temperature n-type Ohmic Contact to Silicon Carbide

We report on the initial demonstration of a tungsten-nickel (75:25 at. %) ohmic contact to silicon carbide (SiC) that performed for up to fifteen hours of heat treatment in argon at 1000 C. The transfer length method (TLM) test structure was used to evaluate the contacts. Samples showed consistent ohmic behavior with specific contact resistance values averaging 5 x 10-4 -cm2. The development of this contact metallization should allow silicon carbide devices to operate more reliably at the present maximum operating temperature of 600 C while potentially extending operations to 1000 C. Introduction Silicon Carbide (SiC) is widely recognized as one of the materials of choice for high temperature, harsh environment sensors and electronics due to its ability to survive and continue normal operation in such environments [1]. Sensors and electronics in SiC have been developed that are capable of operating at temperatures of 600 oC. However operating these devices at the upper reliability temperature threshold increases the potential for early degradation. Therefore, it is important to raise the reliability temperature ceiling higher, which would assure increased device reliability when operated at nominal temperature. There are also instances that require devices to operate and survive for prolonged periods of time above 600 oC [2, 3]. This is specifically needed in the area of hypersonic flight where robust sensors are needed to monitor vehicle performance at temperature greater than 1000 C, as well as for use in the thermomechanical characterization of high temperature materials (e.g. ceramic matrix composites). While SiC alone can withstand these temperatures, a major challenge is to develop reliable electrical contacts to the device itself in order to facilitate signal extraction

Evans, Laura J.↗

Implementation Challenges for Sintered Silicon Carbide Fiber Bonded Ceramic Materials for High Temperature Applications

During the last decades, a number of fiber reinforced ceramic composites have been developed and tested for various aerospace and ground based applications. However, a number of challenges still remain slowing the wide scale implementation of these materials. In addition to continuous fiber reinforced composites, other innovative materials have been developed including the fibrous monoliths and sintered fiber bonded ceramics. The sintered silicon carbide fiber bonded ceramics have been fabricated by the hot pressing and sintering of silicon carbide fibers. However, in this system reliable property database as well as various issues related to thermomechanical performance, integration, and fabrication of large and complex shape components has yet to be addressed. In this presentation, thermomechanical properties of sintered silicon carbide fiber bonded ceramics (as fabricated and joined) will be presented. In addition, critical need for manufacturing and integration technologies in successful implementation of these materials will be discussed.

Singh, M.↗

Extreme-Environment Silicon-Carbide (SiC) Wireless Sensor Suite

Phase II objectives: Develop an integrated silicon-carbide wireless sensor suite capable of in situ measurements of critical characteristics of NTP engine; Compose silicon-carbide wireless sensor suite of: Extreme-environment sensors center, Dedicated high-temperature (450 deg C) silicon-carbide electronics that provide power and signal conditioning capabilities as well as radio frequency modulation and wireless data transmission capabilities center, An onboard energy harvesting system as a power source.

Yang, Jie↗

Simultaneous Ohmic Contact to Silicon Carbide

A simultaneous ohmic contact to silicon carbide includes a mixture of platinum, titanium, and silicon compounds deposited on a silicon carbide substrate. The silicon carbide substrate includes an n-type surface and a p-type surface.

Okojie, Robert S.↗

Composite materials and bodies including silicon carbide and titanium diboride and methods of forming same

Methods of forming composite materials include coating particles of titanium dioxide with a substance including boron (e.g., boron carbide) and a substance including carbon, and reacting the titanium dioxide with the substance including boron and the substance including carbon to form titanium diboride. The methods may be used to form ceramic composite bodies and materials, such as, for example, a ceramic composite body or material including silicon carbide and titanium diboride. Such bodies and materials may be used as armor bodies and armor materials. Such methods may include forming a green body and sintering the green body to a desirable final density. Green bodies formed in accordance with such methods may include particles comprising titanium dioxide and a coating at least partially covering exterior surfaces thereof, the coating comprising a substance including boron (e.g., boron carbide) and a substance including carbon.

36 MATERIALS SCIENCE↗

Methods of depositing an alpha-silicon-carbide-containing film at low temperature

Described methods are useful for depositing a silicon carbide film including Alpha-SiC at low temperatures (e.g., below about 1400.degree. C.), and resulting multi-layer structures and devices. A method includes introducing a chlorinated hydrocarbon gas and a chlorosilicon gas into a reaction chamber, and reacting the chlorinated hydrocarbon gas with the chlorosilicon gas at a temperature of less than about 1400.degree. C. to grow the silicon carbide film. The silicon carbide film so-formed includes Alpha-SiC.

36 MATERIALS SCIENCE↗

Radiolytic Damage and Hydrogen Generation at Carbide – Water Interfaces

To understand the performance of carbides under irradiation, the behavior of SiC and ZrC as well as water slurries of these carbides have been systematically studied using gamma-rays and 5.5 MeV He ions. Radiolytic damage to the carbides was determined using a range of analytical techniques including thermogravimetric analysis (TGA), elemental analysis, inductively-coupled plasma optical emission spectroscopy (ICP-OES) and scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Methods for producing metal carbide materials

Methods of producing silicon carbide, and other metal carbide materials. The method comprises reacting a carbon material (e.g., fibers, or nanoparticles, such as powder, platelet, foam, nanofiber, nanorod, nanotube, whisker, graphene (e.g., graphite), fullerene, or hydrocarbon) and a metal or metal oxide source material (e.g., in gaseous form) in a reaction chamber at an elevated temperature ranging up to approximately 2400° C. or more, depending on the particular metal or metal oxide, and the desired metal carbide being produced. A partial pressure of oxygen in the reaction chamber is maintained at less than approximately 1.01×102 Pascal, and overall pressure is maintained at approximately 1 atm.

Garnier, John E.↗

Metal carbides and methods of making the same

The present disclosure relates to a method for producing a metal carbide, where the method includes thermally treating a molecular precursor in an oxygen-free environment, such that the treating produces the metal carbide and the molecular precursor includes where M is the metal of the metal carbide, N* includes nitrogen or a nitrogen-containing functional group, and x is between zero and six, inclusively.

Baddour, Frederick G.↗

Synthesis of Aluminum-Titanium Carbide Micro and Nanocomposites by the Rotating Impeller In-Situ Gas–Liquid Reaction Method

The Rotating Impeller In-Situ Gas–Liquid Reaction Method is employed for the production of Al-TiC composites. The method relies on injecting a carbon-bearing gas by means of a rotating impeller into a specially formulated molten aluminum-titanium alloy. Under the optimal conditions of temperature and composition, the gas reacts preferentially with titanium to form titanium carbide particles. The design of the apparatus, the process operation window, and the routes for forming titanium carbide particles with different sizes are elucidated.

36 MATERIALS SCIENCE↗

Effect of Sintering Temperature on Density and Mechanical Properties of Solid-State Sintered Silicon Carbide Ceramics and Evaluation of Failure Origin

Densified silicon carbide (SiC) is prepared through dry pressing of SiC powder followed by pressureless sintering in the presence of boron carbide and carbon as the additives. Sintering of SiC parts shows the increase in density with the increase in temperature (1950-2180 °C) by resulting in higher than 98% relative density (RD) at 2150 °C and above for 1 h. Sintered specimens are evaluated concerning the phase, microstructure and mechanical properties including hardness and flexural strength. The machined surface of SiC parts with about 98% RD is studied for the origin of failure. The estimated size of critical flaws (32-110 µm) based on flexural strength and fracture toughness indicates that machining defects are one of the primary reasons for failure in SiC ceramics. The order of magnitude of defects on machined surfaces of sintered SiC by SEM studies is found to be comparable with the estimated size of critical flaws. The failure behavior of SiC is discussed with the help of Weibull statistics with respect to the variation of four-point flexural strength.

36 MATERIALS SCIENCE↗

Achieving Phase Control of Polymorphic Tungsten Carbide Catalysts

The polymorphism of tungsten carbide (W x C) and the challenge of selectively synthesizing pure phases have impeded a precise understanding of catalytic structure−property relationships. This study establishes a framework for phase-selective synthesis of W x C through controlling carburization kinetics. By maintaining particle sizes below 10 nm, β-W 2 C is selectively synthesized using gaseous carbon precursors (CH 4 /H 2 ) via temperature-programmed carburization (TPC). Our findings reveal that W 2 C stabilization is predominantly dictated by particle size and carburization kinetics rather than support interactions, providing a tunable approach to synthesize tungsten carbide catalysts. We elucidate the mechanistic pathway of WO x carburization, demonstrating that CH 4 activation occurs at mild temperatures via lattice oxygen. Our reactor studies establish ex situ synthesized β- W 2 C as an active and stable catalyst for the reverse water-gas shift (RWGS) reaction. However, the need for passivation and reduction pretreatment leads to a complex surface structure with diminished intrinsic activity. In contrast, our in situ synthesis protocol for β-W 2 C eliminates the need for passivation and exhibits increased CO STY during RWGS, illustrating the intrinsically higher activity compared to metallic W, WC 1−x (0.5 < x < 1), and stoichiometric WC.

CO2 conversion↗

Phase evolution in carbide dispersion strengthened nanostructured copper composite by high energy ball milling

In this study, high-energy ball milling was applied to synthesis in situ nanostructured copper based composite reinforced with metal carbides. Cu, M (M=W or Ti) and graphite powder mixture were mechanically alloyed for various milling time in a planetary ball mill with composition of Cu-20vol%WC and Cu-20vol%TiC. Then the as-milled powder were compacted at 200 to 400 MPa and sintered in a vacuum furnace at 900 Degree-Sign C. The results of X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy analysis showed that formation of tungsten carbides (W{sub 2}C and WC phases) was observed after sintering of Cu-W-C mixture while TiC precipitated in as-milled powder of Cu-Ti-C composite after 5 h and become amorphous with longer milling. Mechanism of MA explained the cold welding and fracturing event during milling. Cu-W-C system shows fracturing event is more dominant at early stage of milling and W particle still existed after milling up to 60 h. While in Cu-Ti-C system, cold welding is more dominant and all Ti particles dissolved into Cu matrix.

36 MATERIALS SCIENCE↗

Sintered tantalum carbide coatings on graphite substrates: Highly reliable protective coatings for bulk and epitaxial growth

Highly reliable low-cost protective coatings have been sought after for use in crucibles and susceptors for bulk and epitaxial film growth processes involving wide bandgap materials. Here, we propose a production technique for ultra-thick (50–200 μmt) tantalum carbide (TaC) protective coatings on graphite substrates, which consists of TaC slurry application and subsequent sintering processes, i.e., a wet ceramic process. Structural analysis of the sintered TaC layers indicated that they have a dense granular structure containing coarse grain with sizes of 10–50 μm. Furthermore, no cracks or pinholes penetrated through the layers, i.e., the TaC layers are highly reliable protective coatings. The analysis also indicated that no plastic deformation occurred during the production process, and the non-textured crystalline orientation of the TaC layers is the origin of their high reliability and durability. The TaC-coated graphite crucibles were tested in an aluminum nitride (AlN) sublimation growth process, which involves extremely corrosive conditions, and demonstrated their practical reliability and durability in the AlN growth process as a TaC-coated graphite. The application of the TaC-coated graphite materials to crucibles and susceptors for use in bulk AlN single crystal growth, bulk silicon carbide (SiC) single crystal growth, chemical vapor deposition of epitaxial SiC films, and metal-organic vapor phase epitaxy of group-III nitrides will lead to further improvements in crystal quality and reduced processing costs.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗