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DOE OSTI2015

Hugoniot equation of state and dynamic strength of boron carbide

Boron carbide ceramics have been particularly problematic in attempts to develop adequate constitutive model descriptions for purposes of analysis of dynamic response in the shock and impact environment. Dynamic strength properties of boron carbide ceramic differ uniquely from comparable ceramics. Furthermore, boron carbide is suspected, but not definitely shown, to undergoing polymorphic phase transformation under shock compression. In the present paper, shock-wave compression measurements conducted over the past 40 years are assessed for the purpose of achieving improved understanding of the dynamic equation of state and strength of boron carbide. In particular, attention is focused on the often ignored Los Alamos National Laboratory (LANL) Hugoniot measurements performed on porous sintered boron carbide ceramic. The LANL data are shown to exhibit two compression anomalies on the shock Hugoniot within the range of 20–60 GPa that may relate to crystallographic structure transitions. More recent molecular dynamics simulations on the compressibility of the boron carbide crystal lattice reveal compression transitions that bear similarities to the LANL Hugoniot results. The same Hugoniot data are complemented with dynamic isentropic compression data for boron carbide extracted from Hugoniot measurements on boron carbide and copper granular mixtures. Other Hugoniot measurements, however, performed on near-full-density boron carbide ceramic differ markedly from the LANL Hugoniot data. These later data exhibit markedly less compressibility and tend not to show comparable anomalies in compressibility. Alternative Hugoniot anomalies, however, are exhibited by the near-full-density data. Experimental uncertainty, Hugoniot strength, and phase transformation physics are all possible explanations for the observed discrepancies. It is reasoned that experimental uncertainty and Hugoniot strength are not likely explanations for the observed differences. The notable mechanistic difference in the processes of shock compression between the LANL data and that of the other studies is the markedly larger inelastic deformation and dissipation experienced in the shock event brought about by compaction of the substantially larger porosity LANL test ceramics. High-pressure diamond anvil cell experiments reveal extensive amorphization, reasoned to be a reversion product of a higher-pressure crystallographic phase, which is a consequence of application of both high pressure and shear deformation to the boron carbide crystal structure. A dependence of shock-induced high-pressure phase transformation in boron carbide on the extent of shear deformation experienced in the shock process offers a plausible explanation for the differences observed in the LANL Hugoniot data on porous ceramic and that of other shock data on near-full-density boron carbide.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Customized Nanostructured Ceramics via Microphase Separation 3D Printing

To date, the restricted capability to fabricate ceramics with independently tailored nano- and macroscopic features has hindered their implementation in a wide range of crucial technological areas, including aeronautics, defense, and microelectronics. In this study, a novel approach that combines self- and digital assembly to create polymer-derived ceramics with highly controlled structures spanning from the nano- to macroscale is introduced. Polymerization-induced microphase separation of a resin during digital light processing generates materials with nanoscale morphologies, with the distinct phases consisting of either a preceramic precursor or a sacrificial polymer. By precisely controlling the molecular weight of the sacrificial polymer, the domain size of the resulting material phases can be finely tuned. Pyrolysis of the printed objects yields ceramics with complex macroscale geometries and nanoscale porosity, which display excellent thermal and oxidation resistance, and morphology-dependent thermal conduction properties. This method offers a valuable technological platform for the simplified fabrication of nanostructured ceramics with complex shapes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Additive Manufacturing: Assessing Metal Powder Quality Through Characterizing Feedstock and Contaminants

The quality of powder feedstock for additive manufacturing (AM) metal powder bed fusion methods can significantly affect the quality of parts built from it. Particle size distribution (PSD) and shape factors influence flowability as well as the thickness and uniformity of each powder layer in the build box. For high-performance applications such as aerospace, medical, power generation and military, it becomes important to identify critical additional factors: the types, numbers and sizes of particulate contaminants that may be present in the powder. This is true for virgin, used and blended powders. Contaminants may be introduced during powder manufacture (e.g., ceramic insulation fragments from gas atomization equipment), handling (building insulation, talc) or possibly during the build process itself. Contaminants contained within a batch of powder can be physically built into an additive part when they are incorporated into the melt pool, and they can remain as discrete particulates or non-fused interfaces that act as stress concentrators. Their presence may decrease fatigue life by increasing the likelihood of fatigue crack initiation. This article describes three methods to rapidly and quantifiably characterize powder feedstock. (1) Computer-controlled scanning electron microscopy (CCSEM) provides quantitative size and shape parameters, as well as fine surface details from individual images on a particle-by-particle basis in large populations of powder. (2) Energy-dispersive spectroscopy (EDS) can be included, providing insights into variations within a batch of powder, as well as contaminant compositions. (3) For critical applications, the heavy liquid separation (HLS) method physically extracts low-density contaminants from a sample of powder metal down to part-per-billion detection limits to allow direct examination of contaminants and enhance identification and prevention of their sources. Altogether, these methods permit direct comparisons among powder metal samples. Better quantification of powder characteristics aids determination of suitability for end uses.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Behavior of yttria-stabilized zirconia (YSZ) during laser direct energy deposition of an Inconel 625-YSZ cermet

Thermal barrier coatings (TBC) are regularly used today to protect and extend the service life of several superalloys which are extensively used in high temperature applications. The existing TBCs are typically between 0.1 to 0.5 mm in thickness, are deposited on metal substrates using plasma spray or electron beam vapor deposition, and can reduce temperatures at the substrate surface by up to 300 °C. For greater temperature reductions there is a need for thicker TBCs. The building of thick TBCs has to date been stymied by poor adhesion, and cracking during deposition. It has been suggested that a functionally graded approach may reduce the residual stresses which result in these defects. To date there have been few reports on the deposition of ceramic or cermet coatings using laser AM and none have reported on the phase stability of ceramic particles post-deposition. This article is a first report on the phase stability of ceramic particles following the compositional segregation of elements during deposition using a powder feed additive manufacturing process. Functionally graded (FG), thick TBCs (>3 mm) consisting of Inconel 625 (IN625) and yttria-partially stabilized zirconia (8YSZ) were deposited on an A516 steel substrate via laser direct energy deposition (LDED). Good interfaces were observed between the bond coat (BC) and first cermet layer and between the graded cermet layers. However, cermet layers deposited with 10 wt.% or more YSZ developed a thin layer of YSZ on the surface. The thin layer of YSZ greatly hindered additional deposition of new cermet layers. In cermet layers that did exhibit good interfaces, fine, re-solidified, YSZ particles were homogenously distributed within the Inconel 625 matrix. The YSZ particles exhibited a tetragonal lattice structure and were depleted of yttrium. In contrast, the thin YSZ layer formed on a cermet surface showed no yttrium depletion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Continuous flow system for controlling phases separation near λ transition

As demands on 3He are increasing and conventional 3He production through tritium decay is decreasing, alternative 3He production methods are becoming economically viable. One such possibility is to use entropy filters for extraction of the 3He isotope from natural gas. According to the phase diagram of the 3He, its solidification is impossible by only lowering of the temperature. Hence during the cooling process at stable pressure we can reach λ-point and pass to the special phase - He II. The total density of HeII is a sum of the two phases: normal the superfluid ones. It is possible to separate these two phases with an entropy filter - the barrier for the classically-behaving normal phase. This barrier can also be used to separate the two main isotopes of He: 4He and 3He, because at temperatures close to the 4He-λ-point the 3He isotope is part of the normal phase. The paper presents continuous flow schemes of different separation methods of 3He from helium commodity coming from natural gas cryogenic processing. An overall thermodynamic efficiency of the 3He/4He separation process is presented. A simplified model of continuous flow HeI -HeII recuperative heat exchanger is given. Ceramic and carbon porous plugs have been tested in entropy filter applications.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Uncovering microstructure and composition susceptibility of high permittivity ceramic granules to plasma-induced arc breakdown

Effective diversion of surge currents is vital to prevent unwanted damage to sensitive electronics. Among the most successful and efficient strategies relies on a dielectric stimulated arc breakdown mechanism with high permittivity ceramic granules in a spark-gap geometry. Although generally regarded as a self-healing process, substantial energy deposition may occur that, over time, diminishes the ability to withstand repeated electrical assaults. We investigate the susceptibility of lead–magnesium–niobate–lead titanate (PMN–PT) granule microstructure and composition changes following many exposures to high voltage impulses resulting in arc breakdown. Scanning electron microscopy and energy-dispersive spectroscopy mapping reveal a broad range of thermal and mechanical defects entailing thermal reduction of constituent PMN–PT metal ions and recasting due to rapid eruption of volatile species. Additionally, evidence of local melting and microcracking are apparent that can have deleterious impact on the proper function of the granules, namely, the ability to concentrate electric fields across air gaps to establish and sustain discharge pathways. We propose that the localized nature of damage and stochasticity associated with the dielectric stimulated breakdown mechanism may allow granules to maintain functionality provided no permanent conduction paths are established.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Alternative High-Performance Ceramic Waste Forms

This final report (M5NU-12-NY-AU # 0202-0410) summarizes the results of the project titled “Alternative High-Performance Ceramic Waste Forms,” funded in FY12 by the Nuclear Energy University Program (NEUP Project # 12-3809) being led by Alfred University in collaboration with Savannah River National Laboratory (SRNL). The overall focus of the project is to advance fundamental understanding of crystalline ceramic waste forms and to demonstrate their viability as alternative waste forms to borosilicate glasses. We processed single- and multiphase hollandite waste forms based on simulated waste streams compositions provided by SRNL based on the advanced fuel cycle initiative (AFCI) aqueous separation process developed in the Fuel Cycle Research and Development (FCR&D). For multiphase simulated waste forms, oxide and carbonate precursors were mixed together via ball milling with deionized water using zirconia media in a polyethylene jar for 2 h. The slurry was dried overnight and then separated from the media. The blended powders were then subjected to melting or spark plasma sintering (SPS) processes. Microstructural evolution and phase assemblages of these samples were studied using x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion analysis of x-rays (EDAX), wavelength dispersive spectrometry (WDS), transmission electron spectroscopy (TEM), selective area x-ray diffraction (SAXD), and electron backscatter diffraction (EBSD). These results showed that the processing methods have significant effect on the microstructure and thus the performance of these waste forms. The Ce substitution into zirconolite and pyrochlore materials was investigated using a combination of experimental (in situ XRD and x-ray absorption near edge structure (XANES)) and modeling techniques to study these single phases independently. In zirconolite materials, a transition from the 2M to the 4M polymorph was observed with increasing Ce content. The resulting powders were consolidated via SPS. Ce was reduced to the trivalent oxidation state and the zirconolite was converted into undesirable perovskite. The zirconolite polymorphs found in the synthesized powders were recovered after a post-SPS heat treatment in air. These results demonstrated the potential of processing in controlling the phase assemblage in these waste forms. Hollandites with Cr 3+ trivalent cations were identified as potential hosts for Cs immobilization and are being investigated for Cs retention properties. Series of compositions Ba 1.15-x Cs 2x Cr 2.3 Ti 5.7 O 16 , with increasing Cs loadings, were prepared by sol-gel process and characterized for structural parameters. Structural characterization was performed by a combination of powder XRD and neutron powder diffraction. Phase pure hollandite adapting monoclinic symmetry (I2/m) was observed for 0 ≤ x ≤ 0.55. These results were used to develop a new structural model to interpret Cs immobilization in these hollandites. Performance of these waste forms were evaluated for chemical durability and radiation resistance. Product consistency testing (PCT) and vapor hydration testing (VHT) were used for testing of chemical durability. Radiation resistance was tested using He + ions to simulate $\alpha$ particles and heavy ions such as Au 3+ to simulate a recoil. These results showed that these waste forms were chemically durable. The waste forms also amorphized to various degrees on exposure to simulated radiation.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1972

Field repair of coated columbium Thermal Protection System (TPS)

The requirements for field repair of coated columbian panels were studied, and the probable cause of damage were identified. The following types of repair methods were developed, and are ready for use on an operational system: replacement of fused slurrey silicide coating by a short processing cycle using a focused radiant spot heater; repair of the coating by a glassy matrix ceramic composition which is painted or sprayed over the defective area; and repair of the protective coating by plasma spraying molybdenum disilicide over the damaged area employing portable equipment.

Culp, J. D.↗

NASA NTRS1973

Development and fabrication of sealed silver-zinc cells, phase 1

A facility was designed, constructed and equipped for the production of prismatic alkaline rechargeable battery cells using inorganic (ceramic) separators. This unique facility is environmentally controlled and contains separate areas for electrode fabrication, separator processing, cell assembly, cell finishing and testing. An initial production run of 125 sealed silver zinc cells, using inorganic separators, was made in the facility in order to provide samples for baseline performance tests. Ten of these cells were given performance characterization and life cycle tests.

Blake, I. C.↗

NASA NTRS1989

Analysis of whisker-toughened ceramic components - A design engineer's viewpoint

The analysis of components fabricated from whisker-toughened ceramic matrix composites requires a departure from the 'factor-of-safety' design philosophy prevalent in the design of metallic structural component, which are more tolerant of flaws. A public-domain computer algorithm has been developed which, in conjunction with a general-purposed FEM program, can predict the fast-fracture reliability of a structural component under multiaxial loading conditions. The present version of the algorithm, designated 'Toughened Ceramics Analysis and Reliability Evaluation of Structures', accounts for material symmetry imposed by whisker orientation; the processes of crack deflection and crack pinning are also addressed.

Duffy, Stephen F.↗

NASA NTRS1992

Space Station Furnace Facility Core. Requirements definition and conceptual design study. Volume 2: Technical report. Appendix 6: Technical summary reports

The Space Station Furnace Facility (SSFF) is a modular facility for materials research in the microgravity environment of the Space Station Freedom (SSF). The SSFF is designed for crystal growth and solidification research in the fields of electronic and photonic materials, metals and alloys, and glasses and ceramics and will allow for experimental determination of the role of gravitational forces in the solidification process. The facility will provide a capability for basic scientific research and will evaluate the commercial viability of low-gravity processing of selected technologically important materials. The facility is designed to support a complement of furnace modules as outlined in the Science Capabilities Requirements Document (SCRD). The SSFF is a three rack facility that provides the functions, interfaces, and equipment necessary for the processing of the furnaces and consists of two main parts: the SSFF Core Rack and the two Experiment Racks. The facility is designed to accommodate two experimenter-provided furnace modules housed within the two experiment racks, and is designed to operate these two furnace modules simultaneously. The SCRD specifies a wide range of furnace requirements and serves as the basis for the SSFF conceptual design. SSFF will support automated processing during the man-tended operations and is also designed for crew interface during the permanently manned configuration. The facility is modular in design and facilitates changes as required, so the SSFF is adept to modifications, maintenance, reconfiguration, and technology evolution.

Source record↗

NASA NTRS1992

Space Station Furnace Facility. Volume 2: Summary of technical reports

The Space Station Furnace Facility (SSFF) is a modular facility for materials research in the microgravity environment of the Space Station Freedom (SSF). The SSFF is designed for crystal growth and solidification research in the fields of electronic and photonic materials, metals and alloys, and glasses and ceramics, and will allow for experimental determination of the role of gravitational forces in the solidification process. The facility will provide a capability for basic scientific research and will evaluate the commercial viability of low-gravity processing of selected technologically important materials. In order to accommodate the furnace modules with the resources required to operate, SSFF developed a design that meets the needs of the wide range of furnaces that are planned for the SSFF. The system design is divided into subsystems which provide the functions of interfacing to the SSF services, conditioning and control for furnace module use, providing the controlled services to the furnace modules, and interfacing to and acquiring data from the furnace modules. The subsystems, described in detail, are as follows: Power Conditioning and Distribution Subsystem; Data Management Subsystem; Software; Gas Distribution Subsystem; Thermal Control Subsystem; and Mechanical Structures Subsystem.

Source record↗

NASA NTRS2010

High efficiency tantalum-based ceramic composite structures

Tantalum-based ceramics are suitable for use in thermal protection systems. These composite structures have high efficiency surfaces (low catalytic efficiency and high emittance), thereby reducing heat flux to a spacecraft during planetary re-entry. These ceramics contain tantalum disilicide, molybdenum disilicide and borosilicate glass. The components are milled, along with a processing aid, then applied to a surface of a porous substrate, such as a fibrous silica or carbon substrate. Following application, the coating is then sintered on the substrate. The composite structure is substantially impervious to hot gas penetration and capable of surviving high heat fluxes at temperatures approaching 3000.degree. F. and above.

Stewart, David A.↗

NASA NTRS2009

Joining of Silicon Carbide Through the Diffusion Bonding Approach

In order for ceramics to be fully utilized as components for high-temperature and structural applications, joining and integration methods are needed. Such methods will allow for the fabrication the complex shapes and also allow for insertion of the ceramic component into a system that may have different adjacent materials. Monolithic silicon carbide (SiC) is a ceramic material of focus due to its high temperature strength and stability. Titanium foils were used as an interlayer to form diffusion bonds between chemical vapor deposited (CVD) SiC ceramics with the aid of hot pressing. The influence of such variables as interlayer thickness and processing time were investigated to see which conditions contributed to bonds that were well adhered and crack free. Optical microscopy, scanning electron microscopy, and electron microprobe analysis were used to characterize the bonds and to identify the reaction formed phases.

Halbig, Michael .↗

NASA NTRS2019

History of NASA's Determination of Offgassed Products (Test 7)

NASA's Determination of Offgassed Products (Test 7) from materials and assembled articles for spaceflight has evolved since the Apollo program for over 50 years to meet various habitable spacecraft nonmetallic programmatic requirements. Now mandated by NASA STD-6016A, Standard Materials and Processes Requirements for Spacecraft, all nonmetallic materials used in habitable flight compartments, with the exception of ceramics, metal oxides, inorganic glasses, and materials used in sealed containers, must meet the offgassing requirements in NASA-STD-6001B Test 7. This manuscript presents the history of Test 7, beginning with the Apollo spacecraft nonmetallic materials selection guidelines and test requirements in 1967, in which tests were performed in mostly oxygen atmospheres. It progresses through Skylab, Space Shuttle, International Space Station nonmetals testing, and acceptance requirements with milder test environments. This review of the history of Test 7 presents the reader with a perspective on the development and changes undergone since inception to the present. Related NASA standard tests (some now former, discontinued, combined, or supplemental) including Test 6, Odor Assessment, Test 16, Determination of Offgassed Products from Assembled Articles, and Test 12, Total Spacecraft Cabin Offgassing, are discussed in context

Greene, Benjamin↗

NASA NTRS2019

History of NASA's Determination of Offgassed Products (Test 7)

Greene, Benjamin↗

DOE OSTI2018

Improved Smoothing by a Tool with Ceramic Inserts

A dynamic system is analyzed by the simulation of two subsystems (for the part and the tool) that interact through the dynamic link formed by the machining process. This link corresponds to the smoothing forces, which may be expressed in terms of the state of the dynamic system. The dynamic stability and behavior of the system are expressed in terms of displacements from equilibrium.

42 ENGINEERING↗

DOE OSTI2025

Modeling a High-Temperature Electrochemically Driven Water-Gas-Shift Process Using a Mixed-Conducting Membrane without External Electrical Power

This paper develops a model to predict and interpret the performance of an elevated-temperature, electrochemical, membrane-assisted, water-gas-shift process. The process uses separated feed streams of H 2 O and CO to produce separated streams of H 2 and CO 2 , without an external electrical power source. The dense ceramic membrane is mixed ionic-electronic-conducting (MIEC) gadolinium-doped ceria (GDC) and the porous composite electrodes are Ni-YSZ. At elevated temperature, GDC conducts both oxygen ions and small polarons. The present process uses chemical potential to drive the process. Electrochemical oxidation of CO proceeds within the composite anode and H 2 O reduction proceeds within the composite cathode. At high temperature (e.g., T > 700 °C), GDC has significant electronic leakage in the form of a reduced-cerium small polaron, which supports the charge-transfer reactions. In a typical electrolyzer or fuel cell, this leakage is significantly problematic. However, the present process depends on the leakage current to complete the electrochemical circuit. Model development and validation is based on measured material properties and reactor performance. Potential applications include using CO-rich blast-furnace off gases in steel processing, producing separated streams of H 2 and CO 2 .

Zhu, Huayang↗