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At least 91 records · Page 5

3D printing of ceramics: Advantages, challenges, applications, and perspectives

Abstract 3D printing (3DP) technologies have transformed the processing of advanced ceramics for small‐scale and custom designs during the past three decades. Simple and complex parts are designed and manufactured using 3DP technologies for structural, piezoelectric, and biomedical applications. Manufacturing simple or complex geometries or one‐of‐a‐kind components without part‐specific tooling saves significant time and creates new applications for advanced ceramic materials. Although development and innovations in 3DP of ceramics are far behind compared with metals or polymers, with the availability of different commercial machines in recent years for 3DP of ceramics, exponential growth is expected in this field in the coming decade. This article details various 3DP technologies for advanced ceramic materials, their advantages and challenges for manufacturing parts for various applications, and perspectives on future directions. We envision this work will be helpful to advanced ceramic researchers in industry and academia who are using different 3DP processes in the coming days.

36 MATERIALS SCIENCE↗

UHT-CAMANCHE: Ultra-High Temperature Ceramic Additively Manufactured Compact Heat Exchangers

The conceptual basis for this project is the convergence of advanced ultra-high temperature ceramic materials and additive manufacturing technologies to produce compact ceramic heat exchangers with complex internal flow path geometries. Task areas were broadly divided into materials and manufacturing development, heat exchanger design, component testing, and techno-economic analysis. Technical challenges included the design and commissioning of new test facilities, improving feature resolution and deposition rate of ceramic additive manufacturing techniques, establishing process-structure-property relationships in additively manufactured ultra-high temperature ceramics, and assessing high temperature materials compatibility in CO 2 environments. The primary candidate material evaluated in this work is a composite comprising zirconium diboride (ZrB2) with 30 vol. % silicon carbide (SiC) which was selected based on its desirable combination of high temperature mechanical properties, high thermal and electrical conductivities, and oxidation resistance. High solids loaded ZrB2-SiC pastes suitable for extrusion-based additive manufacturing were developed for the first time as part of this work. Materials compatibility studies indicate this material oxidizes in CO 2 to form a protective borosilicate scale which transforms to pure silica above 1000°C. Parts made by additive manufacturing displayed enlarged grain sizes produced by pressureless sintering as compared to hot-press sintering. Increases in microstructural coarseness have outsized effect on oxidation performance up to 1400°C due to incomplete oxidation of coarse large diameter SiC particles resulting in lower amounts of silica that apparently inhibit protective scale formation. Additive manufacturing as a forming technique did not appear to significantly affect thermal conductivity, hardness, or elastic modulus, though flexural strength was reduced by half or more as compared to traditionally hot-pressed materials. This effect was attributed to the presence of strength-limiting flaws (ca. 40 microns in size) originating from extrudate inhomogeneities that could potentially be eliminated with further process improvements. Attempts to attain economies of scale for production of multi-kilowatt scale heat exchangers by ceramic additive manufacturing proved difficult. Lack of automation and a modest extrusion rate while retaining fine feature resolution made the overall process labor intensive and limited experimental throughput. A number of full-scale components were taken through post-process heat treatments including drying, binder burnout, and sintering; however, none survived without significant flaws or cracks. Therefore, no operational data from a newly installed heat exchanger test loop were able to be obtained during the performance period. Continued research and development is recommended to improve economic feasibility of ceramic additive manufacturing by standardizing the use of advanced sensors, artificial intelligence, and automation tools to reduce associated labor costs and accelerate production rates. The materials and manufacturing techniques demonstrated in this work are likely to find applications in defense and energy applications.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Reliability comparisons between additively manufactured and conventional SiC–Si ceramic composites

Abstract An additively manufactured reaction‐bonded silicon carbide ceramic composite is fabricated using a bimodal powder feedstock and the binder‐jetting printing technique. On fabricating, the ceramic is investigated to report its composition, mechanical, and thermal properties at room temperature and high temperatures (up to 750). The ceramic has a density of 2.76 g/cc, and shows a hardness of 21.74 GPa, and a flexure strength of 207.5 MPa at room temperature. The mechanical property of flexure strength is used to estimate its failure probability under applied stress, using a Weibull distribution. The mechanical properties and failure probabilities are compared with those of conventionally fabricated reaction‐bonded silicon carbide ceramics reported in the literature. These ceramics were fabricated using methods such as slip‐casting, compacting, and tape‐casting. The comparison is used to elucidate the advantages and areas of improvement of the present additive manufacturing technique for reaction‐bonded ceramics.

14 SOLAR ENERGY↗

Development of lithium ion conducting interface between lithium metal and a lithium ion conducting ceramic using block polymers

The lithium-air (Li-air) technology developed by EDF uses an air electrode which works with an aqueous electrolyte, which prevent the use of unprotected lithium metal electrode. A Li+ ionic conductor glass ceramic is used to separate the aqueous electrolyte compartment from the negative lithium electrode. However, this glass-ceramic is not stable in contact with lithium, it is thus necessary to add a protective buffer layer. In another hand, this protection should ideally resist to lithium dendritic growth. It is in this context that this research project which has as goal the development of a protective buffer layer based on block copolymer electrolytes (BCE) between the lithium metal and the lithium ionic conductor ceramic, for lithium-air battery. In a first part, the BCE is studied in lithium-lithium symmetric cells, in order to determine their electrochemical properties such as ionic conductivity, steady state transference number, and finally their resistance to dendritic growth during cycling. Several characterization techniques were employed and especially hard X-ray micro-tomography to analyze the lithium morphology before and after cycling. For single-ion BCE, we expect to suppress dendritic growth, however, we report here for the first time, the visualization of a homogeneous growth of lithium but the formation of dense lithium objects. In another part, the composite BCE-ceramic is studied by electrochemical impedance spectroscopy (EIS). The cycling of lithium-composite-lithium symmetric cells and the analysis of the EIS measurement after each cycle permit to determine if the dendrites have cross the protective layer and are in contact with the ceramic. Besides, the quantification of the polarization loss at the interface polymer-ceramic is evaluated by polarization experiments. This contribution is found to be small.

36 MATERIALS SCIENCE↗

Novel High Temperature Carbide and Boride Ceramics for Direct Power Extraction Electrode Applications. Final report

The current project aims to develop new carbide and boride ceramic materials that incorporate different metal elements (e.g., (Hf 1-x Zr x )B 2 , also called ceramic solid solutions) and understand the fundamental composition-processing-structure-property relationships for such materials. Specifically, nano powders and related nano-composites for selected mixed metal carbide and boride materials are synthesized from nano-scale mixed precursors obtained from solution-based processing via heat treatment in inert atmosphere. The obtained fine powders were then consolidated into dense ceramics via a novel flash sintering process. The mechanical properties and thermal oxidation resistance for the obtained materials were evaluated for these materials. It was found that different synthesis routes produced powders with somewhat different characteristics in terms of composition and microstructure, which then led to different properties for the final ceramics. The synthesis and processing methods demonstrated in this study might be adopted for developing other similar high temperature ceramics, while the mixed metal or solid solution ceramic materials obtained from this study might be used as hot electrodes for direction power extraction and other energy-related applications.

20 FOSSIL-FUELED POWER PLANTS↗

Counter-flow ceramic heat exchanger assembly and method

A heat exchanger assembly embodiment includes a plurality of laminated ceramic tape layers having at least one hole surrounded by at least one tape remainder portion. The plurality of layers is arranged in a build direction defined parallel to a counter-flow plane. Each laminated ceramic tape layer is stacked and sintered to define a ceramic core section integrally formed with a first ceramic manifold and a second ceramic manifold. The ceramic core section of the assembly includes a plurality of spaced apart counter-flow plates stacked along a stacking direction normal to the counter-flow plane and the build direction, defining a plurality of flow passages parallel to the counter-flow plane. Each flow passage is in communication with the first manifold and the second manifold. A plurality of counter-flow fins is disposed in at least one of the plurality of flow passages, between adjacent ones of the plurality of counter-flow plates.

Ranjan, Ram↗

Ceramic High Efficiency Particulate Air (HEPA) Filter Research and Development at Lawrence Livermore National Laboratory

Ceramic high efficiency particulate air (HEPA) filter development program began at Lawrence Livermore National Laboratory (LLNL) over 20 years ago. Historical incidents motivated current safety systems at nuclear facilities. A ceramic filter that can survive a fire can provide robust, passive safety protection. Research has been conducted to improve the safety of nuclear facilities and to reduce operational and lifecycle costs, through ceramic filter technology that can survive fire conditions. Here, the research focused on applications in both new facilities as well as meeting operational requirements necessary to retrofit filters into existing DOE facilities. The research has developed multiple filter technologies spanning traditional HEPA filter materials to advanced manufacturing technologies (e.g., electrospinning, additive manufacturing, etc.). This communication will present highlights of selected development efforts for ceramic HEPA filter research, current state-of-the-art for ceramic filters, and future needs including technical, regulatory, and commercial efforts.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Correlation between Antimicrobial Activity and Bioactivity of Na-Mica and Na-Mica/Fluorapatite Glass and Glass-Ceramics and Their Corrosion Protection of Titanium in Simulated Body Fluid

The improvement in bioactivity of titanium (Ti) surface was achieved via coating it with Na-mica and Na-mica/fluorapatite glass and glass-ceramic using the low-cost electrophoretic deposition technique. Two compositions from pure Na-mica (M) and 80 Na-mica/20 fluorapatite glasses (MF) were prepared in the system SiO{sub 2}-Al{sub 2}O{sub 3}-MgO-MgF{sub 2}-Na{sub 2}O-B{sub 2}O{sub 3} using melting–quenching technique. Characterization of the as-prepared glasses and their counterpart glass-ceramics was studied using differential thermal analysis (DTA), x-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Fourier Transform-IR (FTIR) spectroscopy techniques. The bioactivity behavior was proved by studying the XRD, FTIR and SEM after immersing both glass and glass-ceramic samples in simulated body fluid (SBF). Both M and MF glasses and glass-ceramics showed high microhardness measurements and good antibacterial behavior. In vitro biodegradation was studied by using electrochemical corrosion behavior of the prepared glass- and glass-ceramic-coated Ti in SBF. The prepared coated Ti showed good corrosion resistance in SBF at 37 °C using potentiodynamic polarization technique, and the impedance data fitting explained the structure of the coating and the adsorption of SBF ions on the Ti surface. The MFGC provides the best corrosion-resistant coating, especially after sintering it.

36 MATERIALS SCIENCE↗

A constitutive model for glass–ceramic materials

Glass–ceramics have received recent attention for use in glass–ceramic to metal hermetic seals. Due to their heterogeneous microstructure, these materials exhibit a number of advantageous responses over conventional glass based seals. Key amongst them is the possibility of a controllable thermal strain response and apparent coefficient of thermal expansion which may be used to minimize thermally induced residual stresses for aforementioned seals. Furthermore, these behaviors result from an inorganic glass matrix and variety of crystalline ceramic phases including silica polymorph(s) that may undergo reversible solid-to-solid transformations with associated inelastic strain. Correspondingly, these materials exhibit complex thermomechanical responses associated with multiple inelastic mechanisms (viscoelasticity and phase transformation). While modeling these behaviors is essential for developing and analyzing the corresponding applications, no such model exists. Therefore, in this work a three-dimensional continuum constitutive model for glass–ceramic materials combining these various inelastic mechanisms is developed via an internal state variable approach. A corresponding fully implicit three dimensional numerical formulation is also proposed and implemented. The model is used to simulate existing experiments and validate the proposed formalism. As an example, the simple seal problem of a glass–ceramic seal inside a concentric metal shell is explored. Finally, the impact of the cooling rates, viscoelastic shift factors, and inelastic strain on final residual stress state are all investigated and the differing contributions highlighted.

36 MATERIALS SCIENCE↗

Computational Materials Design for Ceramic Nuclear Waste Forms Using Machine Learning, First-Principles Calculations, and Kinetics Rate Theory

Ceramic waste forms are designed to immobilize radionuclides for permanent disposal in geological repositories. One of the principal criteria for the effective incorporation of waste elements is their compatibility with the host material. In terms of performance under environmental conditions, the resistance of the waste forms to degradation over long periods of time is a critical concern when they are exposed to natural environments. Due to their unique crystallographic features and behavior in nature environment as exemplified by their natural analogues, ceramic waste forms are capable of incorporating problematic nuclear waste elements while showing promising chemical durability in aqueous environments. Recent studies of apatite- and hollandite-structured waste forms demonstrated an approach that can predict the compositions of ceramic waste forms and their long-term dissolution rate by a combination of computational techniques including machine learning, first-principles thermodynamics calculations, and modeling using kinetic rate equations based on critical laboratory experiments. By integrating the predictions of elemental incorporation and degradation kinetics in a holistic framework, the approach could be promising for the design of advanced ceramic waste forms with optimized incorporation capacity and environmental degradation performance. Such an approach could provide a path for accelerated ceramic waste form development and performance prediction for problematic nuclear waste elements.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Evaluating Use of Boron- and Hafnium-Modified Polysilazanes for Ceramic Matrix Minicomposites

In this study, the potential of polymer-derived Ceramic Matrix Composites (CMCs) is demonstrated by addition of thin ceramic coatings on Carbon Fiber (CF) bundles. Boron- and hafnium- modified polysilazane liquid precursors were synthesized and used to infiltrate the fiber bundles of CF to fabricate lab-scale Si(B)CN/CF and Si(Hf)CN/CF CMC mini-composites, respectively. The precursor-to-ceramic conversion process was achieved at 800°C with crosslinked precursor to ceramic yield of approx. 90% in Ar environment. The Si(B)CN/CF contained Si-N and B-N bonds, while Si-N and Hf-O-Si bonds were observed for Si(Hf)CN/CF sample with uniform and dense surfaces. Room-temperature tensile tests showed that the Si(Hf)CN/CF sample could reach a tensile strength of ~790 MPa and elastic modulus of 66.88 GPa among the composites. Oxidation study of the Si(Hf)CN/CF mini-composites showed higher stability compared to SiCN/CF and Si(B)CN/CF mini-composites up to 1500°C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ball-on-ring test validation for equibiaxial flexural strength testing of engineered ceramics

The validation of a ball-on-ring, equibiaxial flexural strength method to obtain the transverse rupture strength (TRS) of right cylindrical ceramic specimens was performed in this study. Validation of the test method was achieved using commercially available engineered high purity alumina disks and finite element (FE) model analysis. The validated fixture was then used to obtain the TRS and Weibull statistical analysis of MgO-partially stabilized zirconia (MSZ) and Y 2 O 3 -partially stabilized zirconia (YSZ) ceramic disks. TRS data for alumina, MSZ, and YSZ agreed with the TRS values reported in the literature. A statistically relevant number of samples (N > 30) for each material were tested to allow for a Weibull statistical analysis. Weibull parameters for these materials were within the expected values for engineered ceramics. The characteristic strength for alumina, MSZ, and YSZ were determined to be 289, 786, and 814 MPa, respectively. The Weibull modulus was determined between 10 and 25 for each material, which is typical of engineered ceramics. In addition, FE model results were in close agreement with experimental fracture values for the three ceramic materials tested in this study.

36 MATERIALS SCIENCE↗

Processing and properties of hafnium-doped tin-modified lead zirconate titanate 95/5 ceramics

Niobium (Nb)-doped lead-tin-zirconate-titanate (PSZT) ceramics near the lead-zirconate-titanate 95/5 orthorhombic AFE-rhombohedral FE morphotropic phase boundary (PSZT 13.5/81/5.5 -1.6Nb) were prepared with up to 10 mol.% of hafnium (Hf) substituted for zirconium. The ceramics were prepared by a traditional solid-state synthesis route and sintered to near full density at 1150°C for 6 h in sealed alumina crucibles with self-same material as the lead vapor source. All compositions were ~98% dense with no detectable secondary phases by X-ray diffraction. The grain size was ~3 μm for all compositions, consisting of equiaxed grains with intergranular porosity. The compositions exhibited remnant polarization values of ~32 μC/cm 2 . Depolarization by the hydrostatic pressure-induced FE-AFE phase transition occurred at 310 MPa for all compositions, resulting in a total depolarization output of 32.4 μC/cm 2 for the PSZT ceramics. Evaluation of the R3c-R3m and R3m-Pm $\bar{3}$ m phase transition temperatures by impedance spectroscopy showed temperatures on heating ranging from 86 to 92°C and 186 to 182°C, respectively, for increasing nominal Hf content. Thermal hysteresis of the phase transitions was also observed in the ceramics, with the transition temperature on cooling being 1–4°C lower. The study demonstrated that the PSZT ceramics are relatively insensitive to variations in Hf content in the range of 0 to 10 mol.%.

36 MATERIALS SCIENCE↗

Processing and properties of PSZT 95/5 ceramics with varying Ti and Nb substitution

Niobium doped lead-tin-zirconate-titanate ceramics near the PZT 95/5 orthorhombic AFE – rhombohedral FE morphotropic phase boundary Pb 1-0.5y (Zr 0.865-x Ti x Sn 0.135 ) 1-y Nb y O 3 were prepared according to a 2 2+1 factorial design with x = 0.05, 0.07 and y = 0.0155, 0.0195. The ceramics were prepared by a traditional solid-state synthesis route and sintered to near full density at 1250°C for 6 hours. All compositions were ~98% dense with no detectable secondary phases by XRD. The ceramics exhibited equiaxed grains with intergranular porosity and grain size was ~5 μm, decreasing with niobium substitution. Compositions exhibited remnant polarization values of ~32 μC/cm 2 , increasing with Ti substitution. Depolarization by the hydrostatic pressure induced FE-AFE phase transition was drastically affected by variation of the Ti and Nb substitution, increasing at a rate of 113 MPa / 1% Ti and 21 MPa / 1% Nb. Total depolarization output was insensitive to the change in Ti and Nb substitution, ~32.8 μC/cm 2 for the PSZT ceramics. The R3c-R3m and R3m-Pm3m phase transition temperatures on heating ranged from 90 to 105°C and 183 to 191°C, respectively. Ti substitution stabilized the R3c and R3m phases to higher temperatures, while Nb substitution stabilized the Pm3m phase to lower temperatures. Thermal hysteresis of the phase transitions was also observed in the ceramics, with transition temperature on cooling being as much as 10°C lower.

36 MATERIALS SCIENCE↗

Synthesis and characteristics of porous ceramic tubes: a comparison of centrifugal casting and cold isostatic pressing methods

Short porous ceramic tubes in small quantities are needed for membrane-related research and development efforts and can be synthesized by centrifugal casting (CC) or cold isostatic pressing (CIP) methods. Here, this work evaluates the characteristics of porous ceramic tubes prepared by both methods and provides a strategy for selecting the proper method for ceramic tube fabrication, depending on its application. Samarium-doped ceria (SDC) with an average crystallite size of 10 nm was synthesized by a citrate method and used to make porous SDC tubes by the CC and CIP methods under different conditions. Porous SDC tubes were prepared from an aqueous suspension of the SDC powder with polyvinyl alcohol (PVA) using a cylindrical metallic mold, centrifugated at 4000–6000 rpm, followed by sintering in 1200–1500 °C. SDC tubes were also made by the CIP method from the SDC powder placed inside a cylindrical rubber bag followed by isostatic compression at 1379 bar. The pore structure of the SDC tubes was characterized by helium permeation and liquid nitrogen Archimedes method. Due to high compression pressure giving a low porosity green tube, the CIP method with lower sintering temperature produces SDC tubes with much lower porosity and average pore size and similar tortuosity compared to the CC methods. The CIP method should be used to prepare low porosity or dense ceramic tubes, and the CC method should be used for preparing high-porosity ceramic tubes or tubes with pore gradient tube wall.

36 MATERIALS SCIENCE↗

Unravelling the sintering temperature-induced phase transformations in Ba(Fe 0.7 Ta 0.3 )O 3-δ ceramics

This work reports on the fundamental details of the crystal structure and phase transformations in Ba(Fe 0.7 Ta 0.3 )O 3-δ , the best known temperature-independent oxygen-sensing ceramic material for applications in extreme environments. Ba(Fe 0.7 Ta 0.3 )O 3-δ ceramics were synthesized using conventional solid-state ceramic reaction under variable sintering temperatures (T s = 1200–1350 °C). Combined X-ray diffraction (XRD) and high-resolution transmission electron microscopy (TEM) measurements revealed the T s -induced phase transformations and their origin in Ba(Fe 0.7 Ta 0.3 )O 3-δ . Associated with phase transformations, pseudo-cubic (PC) reflections, such as {200} PC , {211} PC , and {220} PC , exhibited distinct anomalies with increasing T s . At T s = 1200 °C, Ba(Fe 0.7 Ta 0.3 )O 3-δ stabilized in mixed orthorhombic + rhombohedral phases (Amm2 + R3m). With increasing T s (≥1250 °C), Ba(Fe 0.7 Ta 0.3 )O 3-δ ceramics stabilized in tetragonal/rhombohedral [P4mm + R3m] mixed phases, while variations in the quantity of the respective phases were observed. Because both structure and crystal chemistry play key roles in achieving enhanced performance in chemical sensing and catalytic converters, detailed understanding of the phase transformations and crystal structure of Ba(Fe 0.7 Ta 0.3 )O 3-δ ceramics, as derived in this work, will be useful to develop chemical sensors with optimum performance for high-temperature and corrosive environments.

36 MATERIALS SCIENCE↗

Entropy-Driven Structural Evolution in Ceramic Oxides

High-entropy ceramics, with five or more elements randomly occupying the same cation crystallographic sites, offer vast compositional diversity and unique properties for material design and applications. However, for many dissimilar elements, entropic stabilization cannot overcome the enthalpic barrier to cation substitution. As a result, most high-entropy ceramics incorporate only a few similar elements, limiting the in-depth exploration of the effect of entropy on ceramic properties. Here, we first use density functional theory to model fluorite crystal structures composed of 1-10 elements and then experimentally present practical fluorite oxide nanostructures containing 1, 3, 8, and 15 metals, as well as a record-breaking 25-element high-entropy ceramic incorporating a diverse palette of rare-earth, transition, alkaline, p-block, and noble metals. As entropy increases, structural and configurational disorder in the solid solution rises, altering structural features such as lattice distortion, crystallinity, homogeneity, defect density, and thermal stability. This research provides new insights and understanding of the role of entropy in stabilizing compositionally complex ceramics.

Liu, Shuo↗

Particle size influence on material properties of BaTiO 3 ceramics fabricated using freeze-form extrusion 3D printing

Barium titanate (BaTiO 3 ; BTO) is a well-known lead-free piezoelectric material commonly used for sensors and actuators applications. There are several traditional methods to fabricate bulk BTO ceramics; however, most of those methods have restrictions regarding being able to produce a functional and complex shape for specific application needs. Recently, additive manufacturing techniques such as binder jetting have enabled the fabrication of complex designs of piezoelectric ceramics. However, the density achieved is relatively low thus narrowing their applications. This paper presents the fabrication of high-density BaTiO 3 ceramics using Freeze-form Extrusion Fabrication (FEF). The influence on material properties for different ceramic particle size was assessed. It was found that parts printed using finer BaTiO 3 particle sizes achieved better results in terms of density, piezoelectric, and dielectric properties. For this study, the 100 nm BaTiO 3 samples achieved 85.24% density, a high piezoelectric property of 204.61pC/N and dielectric permittivity of 2551. These results demonstrated the feasibility of using FEF additive manufacturing to fabricate high-quality functional ceramics with designed geometry in a mold-free fashion.

36 MATERIALS SCIENCE↗