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At least 343 records · Page 19

Corrosion of Ceramic Materials

Non-oxide ceramics are promising materials for a range of high temperature applications. Selected current and future applications are listed. In all such applications, the ceramics are exposed to high temperature gases. Therefore it is critical to understand the response of these materials to their environment. The variables to be considered here include both the type of ceramic and the environment to which it is exposed. Non-oxide ceramics include borides, nitrides, and carbides. Most high temperature corrosion environments contain oxygen and hence the emphasis of this chapter will be on oxidation processes.

Opila, Elizabeth J.↗

Solid Freeform Fabrication of Continuous Fiber Reinforced Composites for Propulsion Applications

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500'C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible- manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. This is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths With carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites-, they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP process.

Vaidyanathan, R.↗

Solid Free-Form Fabrication of Continuous Fiber Reinforced Composites for Propulsion Application

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500 C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible-manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. M is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths with carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites; they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP processes.

Vaidyanathan, R.↗

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.↗

Molecular indicators for palaeoenvironmental change in a Messinian evaporitic sequence (Vena del Gesso, Italy). II: High-resolution variations in abundances and 13C contents of free and sulphur-bound carbon skeletons in a single marl bed

The extractable organic matter of 10 immature samples from a marl bed of one evaporitic cycle of the Vena del Gesso sediments (Gessoso-solfifera Fm., Messinian, Italy) was analyzed quantitatively for free hydrocarbons and organic sulphur compounds. Nickel boride was used as a desulphurizing agent to recover sulphur-bound lipids from the polar and asphaltene fractions. Carbon isotopic compositions (delta vs PDB) of free hydrocarbons and of S-bound hydrocarbons were also measured. Relationships between these carbon skeletons, precursor biolipids, and the organisms producing them could then be examined. Concentrations of S-bound lipids and free hydrocarbons and their delta values were plotted vs depth in the marl bed and the profiles were interpreted in terms of variations in source organisms, 13 C contents of the carbon source, and environmentally induced changes in isotopic fractionation. The overall range of delta values measured was 24.7%, from -11.6% for a component derived from green sulphur bacteria (Chlorobiaceae) to -36.3% for a lipid derived from purple sulphur bacteria (Chromatiaceae). Deconvolution of mixtures of components deriving from multiple sources (green and purple sulphur bacteria, coccolithophorids, microalgae and higher plants) was sometimes possible because both quantitative and isotopic data were available and because either the free or S-bound pool sometimes appeared to contain material from a single source. Several free n-alkanes and S-bound lipids appeared to be specific products of upper-water-column primary producers (i.e. algae and cyanobacteria). Others derived from anaerobic photoautotrophs and from heterotrophic protozoa (ciliates), which apparently fed partly on Chlorobiaceae. Four groups of n-alkanes produced by algae or cyanobacteria were also recognized based on systematic variations of abundance and isotopic composition with depth. For hydrocarbons probably derived from microalgae, isotopic variations are well correlated with those of total organic carbon. A resistant aliphatic biomacromolecule produced by microalgae is, therefore, probably an important component of the kerogen. These variations reflect changes in the depositional environment and early diagenetic transformations. Changes in the concentrations of S-bound lipids induced by variations in conditions favourable for sulphurization were discriminated from those related to variations in primary producer assemblages. The water column of the lagoonal basin was stratified and photic zone anoxia occurred during the early and middle stages of marl deposition. During the last stage of the marl deposition the stratification collapsed due to a significant shallowing of the water column. Contributions from anaerobic photoautotrophs were apparently associated with variations in depth of the chemocline.

Non-NASA Center↗

Non-contact Creep Resistance Measurement for Ultra-high temperature Materials

Continuing pressures for higher performance and efficiency in propulsion are driving ever more demanding needs for high-temperature materials. Some immediate applications in spaceflight include combustion chambers for advanced chemical rockets and turbomachinery for jet engines and power conversion in nuclear-electric propulsion. In the case of rockets, the combination of high stresses and high temperatures make the characterization of creep properties very important. Creep is even more important in the turbomachinery, where a long service life is an additional constraint. Some very high-temperature materials are being developed, including platinum group metals, carbides, borides, and silicides. But the measurement of creep properties at very high temperatures is itself problematic, because the testing instrument must operate at such high temperatures. Conventional techniques are limited to about 1700 C. A new, containerless technique for measuring creep deformation has been developed. This technique is based on electrostatic levitation (ESL) of a spherical sample, which is heated to the measurement temperature and rotated at a rate such that the centrifugal acceleration causes creep deformation. Creep of samples has been demonstrated at up to 2300 C in the ESL facility at NASA MSFC, while ESL itself has been applied at over 3000 C, and has no theoretical maximum temperature. The preliminary results and future directions of this NASA-funded research collaboration will be presented.

Hyers, Robert W.↗

Ultra-High Temperature Materials Characterization for Propulsion Applications

Propulsion system efficiency increases as operating temperatures are increased. Some very high-temperature materials are being developed, including refractory metal alloys, carbides, borides, and silicides. System design requires data for materials properties at operating temperatures. Materials property data are not available for many materials of interest at the desired operating temperatures (up to approx. 3000 K). The objective of this work is to provide important physical property data at ultra-high temperatures. The MSFC Electrostatic levitation (ESL) facility can provide measurements of thermophysical properties which include: creep strength, density and thermal expansion for materials being developed for propulsion applications. The ESL facility uses electrostatic fields to position samples between electrodes during processing and characterization studies. Because the samples float between the electrodes during studies, they are free from any contact with a container or test apparatus. This provides a high purity environment for the study of high-temperature, reactive materials. ESL can be used to process a wide variety of materials including metals, alloys, ceramics, glasses and semiconductors. The MSFC ESL has provided non-contact measurements of properties of materials up to 3400 C. Density and thermal expansion are measured by analyzing digital images of the sample at different temperatures. Our novel, non-contact method for measuring creep uses rapid rotation to deform the sample. Digital images of the deformed samples are analyzed to obtain the creep properties, which match those obtained using ASTM Standard E-139 for Nb at 1985 C. Data from selected ESL-based characterization studies will be presented. The ESL technique could support numerous propulsion technologies by advancing the knowledge base and the technology readiness level for ultra-high temperature materials. Applications include non-eroding nozzle materials and lightweight, high-temperature alloys for turbines and structures.

Rogers, Jan↗

Ultra-High Temperature Materials Characterization for Space and Missile Applications

Numerous advanced space and missile technologies including propulsion systems require operations at high temperatures. Some very high-temperature materials are being developed to meet these needs, including refractory metal alloys, carbides, borides, and silicides. System design requires data for materials properties at operating temperatures. Materials property data are not available at the desired operating temperatures for many materials of interest. The objective of this work is to provide important physical property data at ultra-high temperatures. The MSFC Electrostatic Levitation (ESL) facility can provide measurements of thermophysical properties which include: creep strength, emissivity, density and thermal expansion. ESL uses electrostatic fields to position samples between electrodes during processing and characterization experiments. Samples float between the electrodes during studies and are free from any contact with a container or test apparatus. This provides a high purity environment for the study of high-temperature, reactive materials. ESL can be used to process a wide variety of materials including metals, alloys, ceramics, glasses and semiconductors. A system for the determination of total hemispherical emissivity is being developed for the MSFC ESL facility by AZ Technology Inc. The instrument has been designed to provide emissivity measurements for samples during ESL experiments over the temperature range 700-3400K. A novel non-contact technique for the determination of high-temperature creep strength has been developed. Data from selected ESL-based characterization studies will be presented. The ESL technique could advance space and missile technologies by advancing the knowledge base and the technology readiness level for ultra-high temperature materials. Applications include non-eroding nozzle materials and lightweight, high-temperature alloys for turbines and structures.

Rogers, Jan↗

Assessment of the State of the Art of Ultra High Temperature Ceramics

Ultra High Temperature Ceramics (UHTCs) are a family of materials that includes the borides, carbides and nitrides of hafnium-, zirconium- and titanium-based systems. UHTCs are famous for possessing some of the highest melting points of known materials. In addition, they are very hard, have good wear resistance, mechanical strength, and relatively high thermal conductivities (compared to other ceramic materials). Because of these attributes, UHTCs are ideal for thermal protection systems, especially those that require chemical and structural stability at extremely high operating temperatures. UHTCs have the potential to revolutionize the aerospace industry by enabling the development of sharp hypersonic vehicles or atmospheric entry probes capable of the most extreme entry conditions.

Johnson, Sylvia↗

Ceramic Paste for Patching High-Temperature Insulation

A ceramic paste that can be applied relatively easily, either by itself or in combination with one or more layer(s) of high-temperature ceramic fabrics, such as silicon carbide or zirconia, has been invented as a means of patching cracks or holes in the reinforced carbon-carbon forward surfaces of a space shuttle in orbit before returning to Earth. The paste or the paste/fabric combination could also be used to repair rocket-motor combustion chambers, and could be used on Earth to patch similar high-temperature structures. The specified chemical composition of the paste admits of a number of variations, and the exact proportions of its constituents are proprietary. In general, the paste consists of (1) silicon carbide, possibly with addition of (2) hafnium carbide, zirconium carbide, zirconium boride, silicon tetraboride, silicon hexaboride, or other metal carbides or oxides blended with (3) a silazane-based polymer. Because the paste is viscous and sticky at normal terrestrial and outer-space ambient temperatures, high-temperature ceramic fabrics such as silicon carbide or zirconia fabric impregnated with the paste (or the paste alone) sticks to the damaged surface to which it is applied. Once the patch has been applied, it is smoothed to minimize edge steps as required [forward-facing edge steps must be < or equal to 0.030 in. (< or equal to 0.76 mm) in the original intended space-shuttle application]. The patch is then heated to a curing temperature thereby converting it from a flexible material to a hard, tough material. The curing temperature is 375 to 450 F (approx.190 to 230 C). In torch tests and arc-jet tests, the cured paste was found to be capable of withstanding a temperature of 3,500 F (approx. 1,900 C) for 15 minutes. As such, the material appears to satisfy the requirement, in the original space-shuttle application, to withstand re-entry temperatures of approx.3,000 F (approx. 1,600 C).

Adam, Steven J.↗

Oxidation Characterization of Hafnium-Based Ceramics Fabricated by Hot Pressing and Electric Field-Assisted Sintering

Ceramic borides, such as hafnium diboride (HfB2) and zirconium diboride (ZrB2), are members of a family of materials with extremely high melting temperatures referred to as Ultra High Temperature Ceramics (UHTCs). UHTCs constitute a class of promising materials for use in high temperature applications, such as sharp leading edges on future-generation hypersonic flight vehicles, because of their high melting points. The controlled development of microstructure has become important to the processing of UHTCs, with the prospect of improving their mechanical and thermal properties. The improved oxidation resistance of HfB2 has also become important if this material is to be successfully used at temperatures above 2000 C. Furthermore, the use of UHTCs on the leading edges of vehicles traveling at hypersonic speeds will mean exposure to a mixed oxidation environment comprised of both molecular and atomic oxygen. The current study has investigated the high-temperature oxidation behavior of HfB2-based materials in a pure O2 environment, as well as in environments containing different levels of dissociated oxygen (O/O2). Materials were processed by two techniques: conventional hot pressing (HP) and electric field-assisted sintering (FAS). Their oxidation behavior was evaluated in both a tube furnace at 1250 C for 3 hours and in a simulated re-entry environment in the Advanced Heating Facility (AHF) arcjet at NASA Ames Research Center, during a 10-minute exposure to a cold wall heat flux of 250W/sq cm and stagnation pressure of 0.1-0.2 atm. The microstructure of the different materials was characterized before and after oxidation using scanning electron microscopy (SEM).

Gasch, Matt↗

Formation of Minor Phases in a Nickel-Based Disk Superalloy

The minor phases of powder metallurgy disk superalloy LSHR were studied. Samples were consistently heat treated at three different temperatures for long times to approximate equilibrium. Additional heat treatments were also performed for shorter times, to then assess non-equilibrium conditions. Minor phases including MC carbides, M23C6 carbides, M3B2 borides, and sigma were identified. Their transformation temperatures, lattice parameters, compositions, average sizes and total area fractions were determined, and compared to estimates of an existing phase prediction software package. Parameters measured at equilibrium sometimes agreed reasonably well with software model estimates, with potential for further improvements. Results for shorter times representing non-equilibrium indicated significant potential for further extension of the software to such conditions, which are more commonly observed during heat treatments and service at high temperatures for disk applications.

Gabb, T. P.↗

Characterization and Computational Modeling of Minor Phases in Alloy LSHR

The minor phases of powder metallurgy disk superalloy LSHR were studied. Samples were consistently heat treated at three different temperatures for long times to approach equilibrium. Additional heat treatments were also performed for shorter times, to assess minor phase kinetics in non-equilibrium conditions. Minor phases including MC carbides, M23C6 carbides, M3B2 borides, and sigma were identified. Their average sizes and total area fractions were determined. CALPHAD thermodynamics databases and PrecipiCalc(TradeMark), a computational precipitation modeling tool, were employed with Ni-base thermodynamics and diffusion databases to model and simulate the phase microstructural evolution observed in the experiments with an objective to identify the model limitations and the directions of model enhancement.

Jou, Herng-Jeng↗

Ab initio Computations of the Electronic, Mechanical, and Thermal Properties of Ultra High Temperature Ceramics (UHTC) ZrB2 and HfB2

Refractory materials such as metallic borides, often considered as ultra high temperature ceramics (UHTC), are characterized by high melting point, high hardness, and good chemical inertness. These materials have many applications which require high temperature materials that can operate with no or limited oxidation. Ab initio, first principles methods are the most accurate modeling approaches available and represent a parameter free description of the material based on the quantum mechanical equations. Using these methods, many of the intrinsic properties of these material can be obtained. We performed ab initio calculations based on density functional theory for the UHTC materials ZrB2 and HfB2. Computational results are presented for structural information (lattice constants, bond lengths, etc), electronic structure (bonding motifs, densities of states, band structure, etc), thermal quantities (phonon spectra, phonon densities of states, specific heat), as well as information about point defects such as vacancy and antisite formation energies.

Lawson, John W.↗

In-situ Formation of Reinforcement Phases in Ultra High Temperature Ceramic Composites

A tough ultra-high temperature ceramic (UHTC) composite comprises grains of UHTC matrix material, such as HfB.sub.2, ZrB.sub.2 or other metal boride, carbide, nitride, etc., surrounded by a uniform distribution of acicular high aspect ratio reinforcement ceramic rods or whiskers, such as of SiC, is formed from uniformly mixing a powder of the UHTC material and a pre-ceramic polymer selected to form the desired reinforcement species, then thermally consolidating the mixture by hot pressing. The acicular reinforcement rods may make up from 5 to 30 vol % of the resulting microstructure.

Stackpoole, Margaret M↗

Microstructural and Creep Properties of Boron- and Zirconium-Containing Cobalt-Based Superalloys

The effects of micro-additions of boron and zirconium on grain-boundary (GB) structure and strength inpolycrystalline γ(f.c.c.) plus γ’(L12) strengthened Co-9.5Al-7.5W-X at. % alloys (X=0-Ternary, 0.05B, 0.01B,0.05Zr, and 0.005B-0.05Zr at. %) are studied. Creep tests performed at 850 °C demonstrate that GB strength and cohesion limit the creep resistance and ductility of the ternary B- and Zr-free alloy due to intergranular fracture. Alloys with 0.05B and 0.005B-0.05Zr both exhibit improved creep strength due to enhanced GB cohesion,compared to the baseline ternary Co-9.5Al-7.5W alloy, but alloys containing 0.01B or 0.05Zr additions displayed no benefit. Atom-probe tomography (APT) is utilized to measure GB segregation, where B and Zr are demonstrated to segregate at GBs. A Gibbsian interfacial excess of 5.57 ± 1.04 atoms nm(exp) -2 was found for B at aGB in the 0.01B alloy and 2.88 ± 0.81 and 2.40 ± 0.84 atoms nm2 for B and Zr, respectively, for the 0.005B-0.05Zr alloy. The GBs in the highest B-containing (0.05B) alloy exhibit micrometer-sized boride precipitates with adjacent precipitate denuded-zones (PDZs), whereas secondary precipitation at the GBs is absent in theother four alloys. The 0.05B alloy has the smallest room temperature yield strength, by 6%, which is attributedto the PDZs, but it exhibits the largest increase in creep strength (with an ~2.5 order of magnitude decrease inthe minimum strain rate for a given stress at 850 °C) over the baseline Co-9.5Al-7.5W alloy.

Creep↗

Metallic Powder Core Tubular Wire (PCTW) Development for Additive Manufacturing

NASA Langley Research Center (LaRC) in Hampton, VA, and the Center for Welding, Joining, and Coating Research (CWJCR) in the Department of Metallurgical and Materials Engineering at the Colorado School of Mines (CSM) in Golden, CO, have collaborated for nearly fifteen years to develop metallic powder core tubular wire (PCTW) feedstock for additive manufacturing (AM) using electron beam deposition. The motivation for this development was to offset dealloying observed during deposition of titanium and aluminum alloy solid wire feedstock in the LaRC electron beam freeform fabrication (EBF3) system and to explore novel alloy compositions by tailoring the powder fill. EBF3 is a fusion-based AM process that is performed under vacuum and is consequently prone to vaporization loss of low vapor pressure alloying elements. Research spanning four graduate student research projects succeeded in developing the basic methodology to fabricate PCTW, the mass balance equations used to define the powder fill, microstructure control through particulate inoculation, and the feasibility of producing metal matrix composite materials. Metallic PCTW is comprised of a thin foil sheath wrapped around a powder blend. Fabrication of PCTW at CSM was accomplished using a tubular wire mill system to first bend a flat strip into a u-shaped cross section, deposit a powder fill, create a lap joint to seal the wire, and draw to final diameter. Powder management systems were developed to ensure uniform mixing of powder constituents and identify feed rates for optimum fill ratios. Processing parameters were successfully developed for titanium and aluminum alloy sheaths to account for material work hardening during drawing. Mass balance equations were developed to account for compositional contributions of the sheath and powder fill. PCTW composition can be adjusted through selection of the sheath or powder materials. PCTWs were successfully developed to offset Al loss in deposits of Ti-6-4 and Mg loss in Al 6061, resulting in deposits that were within the composition limits for each material. Ti-6-4 deposits were fabricated using PCTW comprised of commercially pure (CP) titanium sheath and a fill of pre-alloyed Ti-6-4 powder with additions of elemental Al and V powders. Additions of both elements were required to account for the CP Ti from the sheath, and Al was further enhanced to offset documented losses in EBF3 deposits. For Al 6061 deposits, composition was modulated through the choice of sheath material. The PCTW was made using an Al 5052 sheath to supplement Mg content and a fill composition of pre-alloyed 6061 powder with additions of Si and Cu.The slower solidification rate of the EBF3 process compared with laser powder bed fusion processes can lead to coarse-grained microstructures and mechanical property anisotropy. EBF3deposits of Ti-6-4 exhibited large epitaxially grown β grains, which result in degraded mechanical properties in the deposition direction. Microstructure refinement was achieved through a combination of electron beam modulation and the use of a PCTW designed for Ti-6-4 deposits and modified by the addition of powder made from Fe and B. Resulting deposits exhibited reductions in β grain size, α phase colony intercept length and lath width, and an increased volume fraction of β phase. The mechanism of microstructure refinement was related to precipitation of boride particles. Hardness testing confirmed that mechanical property anisotropy was reduced and an overall increase in hardness was achieved.Metal matrix composite (MMC) materials offer strength and stiffness benefits over unreinforced materials. Two methods were investigated using PCTW technology for producing Al 6061 basedMMC materials; the direct addition of SiC reinforcing particles and the in-situ generation of reinforcements through reaction synthesis of precursor powders. Al 6061 based MMCs reinforced with SiC exhibited particle clustering and formation of aluminum carbides during deposition. The application of a Ni coating to the SiC particles prior to incorporation into the powder fill eliminated aluminum carbide formation and aided particle distribution during deposition. Modulation of beam focus and power further reduced aluminum carbide formation and aided particle distribution. In reaction synthesis, precursor additions undergo an exothermic reaction during deposition to form new ceramic products, generally of finer scale than the initial precursor components. The product phases provide reinforcement in the MMC and act as nucleation sites during solidification, resulting in grain refinement, improved mechanical properties, and reduced susceptibility to solidification cracking. Higher tensile strength and stiffness were demonstrated in Al 6061 based MMCs with 2 vol% reinforcement. These combined research efforts demonstrate the potential of PCTW technology for customizing of alloy composition and achieving microstructure control. A manufacturing process for titanium- and aluminum-based PCTWs was developed based on iterative design, theoretical calculations, and empirical data. PCTW technology successfully mitigated Al loss from Ti-6-4 and Mg loss in Al 6061, resulted in grain refinement in Ti-6-4, and demonstrated fabrication of Al based MMCs

Marcia S Domack↗

Laser Ablative Patterning of B4C and MoAlB Ceramics for Hydrophobic Surfaces

Through a novel laser ablative patterning (LAP) process, the present work reports the increase in wetting contact angle of molybdenum aluminum boride (MoAlB) and the reduction of dust adhesion. The LAP technique employed picosecond laser pulses to form a crosshatch pattern with micropillars on ceramic surfaces. The wetting behavior was successfully transitioned from hydrophilic (θ < 90°) to hydrophobic (θ > 90°), which may be related to Wenzel or Cassie-Baxter mechanisms. Parameters such as laser fluence and number of laser scans were varied to study their effects on ceramic surface characteristics. Dust adhesion experiments were performed on these hydrophobic ceramic surfaces, which showed that the adhesion of lunar soil simulant dust particles was significantly reduced in the patterned MoAlB surface. The patterned MoAlB samples were further examined using the surveying lunar dust influence on device efficacy (SLIDE) testbed to evaluate the wear performance.

Bai Cui↗