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Binder Jet Additive Multi-Material Manufacturing for the Transformational Challenge Reactor
Additive manufacturing (AM) is a process in which material is deposited in a layer-by-layer fashion, thereby building up a geometry. This contrasts with subtractive manufacturing in which material is removed from bulk feedstock to create a final geometry. Binder jet AM (BJAM) is a specific process in the AM field in which a binder, or glue, is selectively deposited on a bed of spread powder feedstock and cured. Binder is deposited with an inkjet printhead, which allows for high-resolution shaping of the powder layers. Compared with other AM processes, BJAM is fast, efficient, and scalable. Further, BJAM has one of the largest material selections of the powder AM processes as it can process ceramics, plastics, metals, and virtually any powdered material. Thus, the opportunity exists to leverage the versatility and productivity of BJAM to enable multi-material printing, the next generation of AM technology. The aim of this research is the design and manufacture of a purpose-built BJAM machine that can process multiple materials in its normal operation. This binder jet additive multi-material manufacturing (BJAM 3 ) machine will be able to produce parts that have multiple materials intra- and inter-layer. An example of this would be encapsulating metal spheres inside of a ceramic cube or vice versa. This BJAM 3 process adds another step of freedom to designing and manufacturing complex parts. The milestone for this work is to provide details on the technical progress made to date on the development of multi-material binder jetting and to facilitate simultaneous additive manufacturing of at least two different powder feedstocks.
Processing liquid organic wastes at the NNL Preston laboratory
Organic compounds of various kinds have been used in the nuclear industry for numerous duties in uranium chemical, metal and ceramic processing plants. In the course of the various operations undertaken, these organic compounds have become contaminated with uranic material, either accidentally or as an inevitable part of the process. Typically, the chemical/physical form and/or concentration of the uranic content of the organics has prevented disposal. In order to address the issue of contaminated liquid organic wastes, the National Nuclear Laboratory (NNL) has developed a suite of treatments designed to recover uranium and to render the waste suitable for disposal. The developed processes are operated at industrial scale via the NNL Preston Laboratory Residue Processing Plant. The Oil Waste Leaching (OWL) Process is a fully industrialised process used for the treatment of contaminated oils with approximately 200 tonnes of uranium contaminated oil being treated to date. The process was originally developed for the treatment of contaminated tributyl phosphate and odourless kerosene which had been adsorbed onto sawdust. However, over the years, the OWL process has been refined for a range of oils including 'water emulsifiable' cutting oils, lubricating oils, hydraulic oils/fluids and 'Fomblin' (fully fluorinated) oils. Chemically, the OWL process has proved capable of treating solvents as well as oils but the highly volatile/flammable nature of many solvents has required additional precautions compared with those required for oil treatment. These additional precautions led to the development of the Solvent Treatment Advanced Rig (STAR), an installation operated under an inert atmosphere. STAR is a small 'module' (100 dm{sup 3} volume) which allows the treatment of both water miscible and immiscible solvents. This paper discusses the challenges associated with the treatment of liquid organic wastes and the process developments which have allowed a wide range of materials to be successfully treated. (authors)
Morphologies, Processing and Properties of Ceramic Foams from Pre-Ceramic Foams from Pre-Ceramic Polymer Routes
The current research is focused on processing ceramic foams that have potential as a thermal protection material. Ceramic foams with different architectures were formed from the pyrolysis of pre-ceramic polymers at 1200 C in different atmospheres. In some systems a sacrificial polyurethane was used as the blowing agent. We have also processed foams using sacrificial fillers to introduce controlled cell sizes. Each sacrificial filler or blowing agent leads to a unique morphology. The effect of different fillers on foam morphologies will be presented. The presentation will also focus on characterization of these foams in terms of mechanical and thermal properties. Foams processed using these approaches having bulk densities ranging from 0.15 to 0.9 g per cubic centimeter and a cell sizes from 5 to 500 micrometers. Compression strengths ranged from 2 to 7 MPa for these materials.
The role of ceramic and glass science research in meeting societal challenges: Report from an NSF-sponsored workshop
Under the sponsorship of the U.S. National Science Foundation, a workshop on emerging research opportunities in ceramic and glass science was held in September 2016. Reported here are proceedings of the workshop. The report details eight challenges identified through workshop discussions: Ceramic processing: Programmable design and assembly; The defect genome: Understanding, characterizing, and predicting defects across time and length scales; Functionalizing defects for unprecedented properties; Ceramic flatlands: Defining structure-property relations in free-standing, supported, and confined two-dimensional ceramics; Ceramics in the extreme: Discovery and design strategies; Ceramics in the extreme: Behavior of multimaterial systems; Understanding and exploiting glasses and melts under extreme conditions; and Rational design of functional glasses guided by predictive modeling. It is anticipated that these challenges, once met, will promote basic understanding and ultimately enable advancements within multiple sectors, including energy, environment, manufacturing, security, and health care.
Small-scale Assessment of Simplified Ceramic Waste Form Processing
The feasibility of directly processing glass-bonded sodalite ceramic waste form materials by heating a mixture of Zeolite 4A, chloride salt, and sodium borosilicate binder glass was demonstrated by generating laboratory-scale materials. This direct processing method eliminates pre-setting the moisture content of the Zeolite 4A, eliminates the step of occluding salt in the prepared Zeolite 4A prior to processing, and can be conducted using larger particle sizes of crushed Zeolite 4A and crushed borosilicate glass than those called for in the current method. These simplifications are expected to facilitate material transfer and handling in a hot cell or controlled atmosphere environment and be more readily implemented at large scale than the current method. Most materials made to assess these simplifications were directly processed at 925 °C for two hours in an argon atmosphere glovebox, but one material was processed at 925 °C for four hours and one material was processed at 880 °C for two hours. Sodalite was generated and became microencapsulated by the binder glass in all materials. The microstructures were uniform throughout each product, were similar in all products, and were similar to the microstructures of materials made previously using the pressureless consolidation or hot isostatic pressing methods. Various formulations showed the efficiency of sodalite generation was not sensitive to the salt-to-Zeolite 4A ratio or salt-to-glass mass ratio, although a greater relative mass of glass is required to encapsulate sodalite generated from large particles of aggregated Zeolite 4A. The upper limit of salt loadings that can be effectively processed remains to be determined. The effectiveness of direct processing provided new insights into the conversion mechanism. The salt was likely dissolved into the glass that transported NaCl into the Zeolite 4A aggregates and sodalite was generated in situ as NaCl migrated from the outside of the aggregate inward. Other salt cations (e.g., potassium, strontium, cesium, and probably lithium) remain dissolved in the glass encapsulating the zeolite/sodalite domains. When the glass solidifies during cooling, small halite inclusion phases form in glass within sodalite domains and large mixed salt inclusions form in glass surrounding the sodalite due to the low solubility of chloride in the (solid) glass. Other salt cations were oxidized during processing and formed inclusions in the bulk glass (e.g., neodymium). Initial degradation tests show the dissolution behavior of directly processed CWF (SCWF) materials is similar to CWF materials made using different methods.
Morphologies, Processing and Properties of Ceramic Foams and Their Potential as TPS Materials
The current research is focused on processing ceramic foams with compositions that have potential as a thermal protection material. The use of pre-ceramic polymers with the addition of sacrificial blowing agents or sacrificial fillers offers a viable approach to form either open or closed cell insulation. Our work demonstrates that this is a feasible method to form refractory ceramic foams at relatively low processing temperatures. It is possible to foam complex shapes then pyrolize the system to form a ceramic while retaining the shape of the unfired foam. Initial work focused on identifying suitable pre-ceramic polymers with desired properties such as ceramic yield and chemical make up of the pyrolysis product after firing. We focused on making foams in the Si system (Sic, Si02, Si-0-C), which is in use in current acreage TPS systems. Ceramic foams with different architectures were formed from the pyrolysis of pre-ceramic polymers at 1200 C in different atmospheres. In some systems a sacrificial polyurethane was used as the blowing agent. We have also processed foams using sacrificial fillers to introduce controlled cell sizes. Each sacrificial filler or blowing agent leads to a unique morphology. The effect of different fillers on foam morphologies and the characterization of these foams in terms of mechanical and thermal properties are presented. We have conducted preliminary arc jet testing on selected foams with the materials being exposed to typical re-entry conditions for acreage TPS and these results will be discussed. Foams processed using these approaches have bulk densities ranging from 0.15 to 0.9 g/cm3 and cell sizes ranging from 5 to 500 pm. Compression strengths ranged from 2 to 7 MPa for these systems. Finally, preliminary oxidation studies have been conducted on selected systems and will be discussed.
Containerless processing of amorphous ceramics
The absence of gravity allows containerless processing of materials which could not otherwise be processed. High melting point, hard materials such as borides, nitrides, and refractory metals are usually brittle in their crystalline form. The absence of dislocations in amorphous materials frequently endows them with flexibility and toughness. Systematic studies of the properties of many amorphous materials have not been carried out. The requirements for their production is that they can be processed in a controlled way without container interaction. Containerless processing in microgravity could permit the control necessary to produce amorphous forms of hard materials.
Direct ink write fabrication of transparent ceramic gain media
Solid-state laser gain media based on the garnet structure with two spatially distinct but optically contiguous regions have been fabricated. Transparent gain media comprised of a central core of Y 2.97 Nd 0.03 Al 5.00 O 12.00 (Nd:YAG) and an undoped cladding region of Y 3 Al 5 O 12 (YAG) were fabricated by direct ink write and transparent ceramic processing. Direct ink write (DIW) was employed to form the green body, offering a general route to preparing functionally structured solid-state laser gain media. Lastly, fully-dense transparent optical ceramics in a “top hat” geometry with YAG/Nd:YAG have been fabricated by DIW methods with optical scatter at 1064 nm of <3%/cm.
Investigation of Solid Particle Reactors for Nonoxidative Dehydrogenation of Ethane: Toward Solar Thermal Ethylene Production
Concentrating solar power plants can generate renewable heat at temperatures well above those of most industrial processes. Ceramic particles irradiated with concentrated sunlight can store high-quality sensible heat and transfer this to power generation systems. These concepts and materials hold great potential to also enable thermal processes in the chemical industry, but effective strategies for transferring heat from thermal energy storage media into chemical reactors are still under development. This present work evaluated the thermal and chemical compatibility of various solid particle media (including quartz, bauxite, and alumina particles) integrated directly into tube reactors and the subsequent effects on reactor performance for the nonoxidative dehydrogenation of ethane reaction. Empty tube reactors without loaded particles (representing conventional ethane cracking coils) showed significant heat transfer limitations as the tube diameter was scaled. The incorporation of media into the reactor significantly aided heat transfer to the gaseous ethane reactant and increased its conversion by as much as 10% at similar space velocities. Despite direct contact with hydrocarbon gases, alumina and quartz media showed negligible coke formation. Even during reaction in 100% ethane feed gas at 825 °C, the average selectivity of the coke product was only 0.57% when using the quartz media. These materials further demonstrated excellent thermal stability during subsequent reoxidation in air at 800 °C, which simulated the reheating of particles in a circulating particle solar receiver. Conversely, high rates of coke formation, with a product selectivity of 27.5%, were observed on sintered bauxite particles during the reaction, likely promoted by transition metal constituents. These particles fractured upon reoxidation due to exotherms generated from coke combustion. In conclusion, while the use of cofed steam could mitigate attrition of redox-active particles, the ability of inert metal oxide particles to efficiently transfer heat to concentrated ethane reactant gas while suppressing side reactions or degradation suggests that these media could effectively couple solar thermal plants to reactors for next-generation production of ethylene and other critical chemicals.
Development of ITM Oxygen Technology for Low-cost and Low-emission Gasification and Other Industrial Applications
Air Products is carrying out a scope of work under DOE Award No. DE-FE0012065 “Development of ITM Oxygen Technology for Low-cost and Low-emission Gasification and Other Industrial Applications.” The Statement of Project Objectives (SOPO) includes a Task 4f in which a Decision Point shall be reached, necessitating a review of Tasks 2-5 with an emphasis on Task 4f. This Topical Report constitutes the Decision Point Application pertaining to Task 4f. The SOPO under DOE Award No. DE-FE0012065 is aimed at furthering the development of the Ion Transport Membrane (ITM) Oxygen production process toward a demonstration scale facility known as the Oxygen Development Facility (ODF). It is anticipated that the completion of the current SOPO will advance the technology significantly along a pathway towards enabling the design and construction of the ODF. Development progress on several fronts is critical before an ODF project can commence; this Topical Report serves as an early update on the progress in critical development areas. Progress was made under all tasks, including Materials Development, Ceramic Processing Development, Engineering Development, and Performance Testing. Under Task 4f, Air Products carried out a cost and performance study in which several process design and cost parameters were varied and assessed with a process model and budgetary costing exercise. The results show that the major variables include ceramic module reliability, ITM operating temperature, module production yield, and heat addition strategy. High-temperature compact heat exchangers are shown to contribute significant cost benefits, while directly firing into the feed stream to an ITM are even a mild improvement on the high-temperature recuperation approach. Based on the findings to-date, Air Products recommends no changes to the content or emphasis in the current SOPO and recommends its completion prior to another formal assessment of these factors.
Deformation processes in forging ceramics Progress report, 19 Jun. - 19 Sep. 1969
Deformation processes involved in forging of polycrystalline oxide ceramics
High-temperature X-ray analysis of phase evolution in lithium ion conductor Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3}
Series of Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} glass ceramic samples were prepared in this work through the change of heat treatment temperature from 650 to 1050 °C. The structures of glass ceramic samples were characterized by means of high temperature X-ray diffraction and Field Emission Scanning Electron Microscope. And the lithium ionic conductivity was analyzed through AC impedance spectroscopy. Through heat treatment at 850 °C for 4 h for the base glass sample, we obtained a maximum conductivity of 5.8 × 10{sup −4} S/cm at room temperature. - Graphical Abstract: High temperature X-ray diffraction (HT-XRD) and Rietveld refinement of Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} (LAGP) glass-ceramics were recorded to investigate the phase transformation, cell parameters and the mass fraction of each crystal phase, which occur in the glass to glass-ceramics process during different crystallization temperatures. The relationship between the average grain size and conductivity that originate from and relate to the crystallization temperature was analyzed by SEM micrograph and AC impedance spectroscopy. - Highlights: • Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} glass-ceramics were prepared from as-prepared glass. • The phases decomposition and mass fraction of each phase were analyzed by HT-XRD. • Conductivity is relate to grain size that influenced by crystallization temperature.
Preparing Li-garnet electrodes with engineered structures by phase inversion and high shear compaction processes
We report solid-state lithium batteries are promising for safety and energy density com-pared with traditional lithium-ion batteries. However, the large interfacial resistance between the electrode and electrolyte is a bottleneck to achieving high-performance solid-state batteries. Engineered electrode structures with a porous scaffold of the solid electrolyte material are promising to lower the interfacial resistance and provide a mechanical support for a thin solid electrolyte layer. In this work, two ceramic processing techniques are used to fabricate porous/dense bilayer architectures based on a Li 6.25 Al 0.25 La 3 Zr 2 O 12 (LLZO) Li-garnet material. Finger-like vertically aligned pores are created by the phase inversion (PI) process. A water bath presaturated with Li salt prevents Li loss during the PI solvent exchange step. Pore size and porosity can be optimized by adjusting the bath temperature. The high shear compaction process was used to prepare LLZO tapes with 40, 60, and 80 vol% poreformer. The porosity of the tapes after sintering is 39.5%, 58.4%, and 75.4%, respectively. Microtomography exhibits the porosity, pore shape, and pore distribution of the tapes. A typical cathode material LiNi 0.33 Mn 0.33 Co 0.33 O 2 (NMC) is filled into the pores via vacuum infiltration, and a dense cathode layer is formed within the garnet scaffold.
Stabilized Alumina/Ethanol Colloidal Dispersion for Seeding High Temperature Air Flows
Seeding air flows with particles to enable measurements of gas velocities via laser anemometry and/or particle image velocimetry techniques can be quite exasperating. The seeding requirements are compounded when high temperature environments are encountered and special care must be used in selecting a refractory seed material. The pH stabilization techniques commonly employed in ceramic processing are used to obtain stable dispersions for generating aerosols of refractory seed material. By adding submicron alumina particles to a preadjusted pH solution of ethanol, a stable dispersion is obtained which when atomized produces a high quality aerosol. Commercial grade alumina powder is used with a moderate size distribution. The technique is not limited to alumina/ethanol and is also demonstrated with an alumina/H2O system. Other ceramic powders in various polar solvents could also be used once the point of zero charge (pH(sub pzc)) of the powder in the solvent has been determined.
Dielectric, ferromagnetic and maganetoelectric properties of BaTiO{sub 3}–Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} composite ceramics
Graphical abstract: - Highlights: • The lead-free ME ceramic composites BaTiO{sub 3}–Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} were successfully synthesized. • The composites showed high dielectric constant and low dielectric loss. • The composite with 30% NiZn ferrite presented good soft magnetic properties and ME performance. - Abstract: Lead-free magnetoelectric composite ceramics (1 − x)BaTiO{sub 3}–xNi{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} (x = 0.15, 0.3, 0.45) were successfully prepared by conventional oxide ceramic process. The tetragonal perovskite BaTiO{sub 3} and cubic spinel Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} were confirmed by X-ray diffraction. The dielectric behaviors of all composite samples show a normal response to the increasing measurement frequency and Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} ferrite content. Well defined ferromagnetic hysteresis loops and obvious magnetoelectric coupling effect are observed in the composite ceramics. The influence of applied dc bias magnetic field and Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} ferrite content on the magnetoelectric coupling responding voltage is investigated. The strongest peak magnetoelectric coupling voltage coefficient is 124 μV/cm Oe when x = 0.3, which corresponds to the maximum magnetoelectric coupling responding voltage of 200 μV.
The processing of screened resistors on ceramic substrates
Pilot process for fabrication of screened resistors on ceramic substrates
Effects of MnO doping on the electronic properties of zinc oxide: 406 GHz electron paramagnetic resonance spectroscopy and Newman superposition model analysis
MnO-doped ZnO ceramics have been synthesized through the conventional ceramic processing route. Mn{sup 2+} ions have been incorporated into the ZnO lattice within the limits of solid solubility. By using X-band-frequency and high-field electron paramagnetic resonance (EPR), we have resolved some of the main electronic transitions for the S = 5/2, I = 5/2 high-spin system and have determined accurately the EPR spin-Hamiltonian parameters. By combining data from crystallographic X-ray diffraction and EPR with the semi-empirical Newman superposition model, we have found the local configurational position of Mn{sup 2+} and have confirmed the symmetry of the lattice. The results presented in this contribution indicate that Mn ions substitute at Zn sites in ZnO. The effect of Mn{sup 2+} ions on the intrinsic defects becomes remarkable, thus the vacancy related intrinsic defect signals cannot be visible in the EPR spectrum. MnO doping affects the band gap energy of ZnO system which was confirmed via UV-Vis spectroscopy.