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At least 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

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↗
NASA NTRS1978

Evaluation of ceramics for stator application: Gas turbine engine report

Current ceramic materials, component fabrication processes, and reliability prediction capability for ceramic stators in an automotive gas turbine engine environment are assessed. Simulated engine duty cycle testing of stators conducted at temperatures up to 1093 C is discussed. Materials evaluated are SiC and Si3N4 fabricated from two near-net-shape processes: slip casting and injection molding. Stators for durability cycle evaluation and test specimens for material property characterization, and reliability prediction model prepared to predict stator performance in the simulated engine environment are considered. The status and description of the work performed for the reliability prediction modeling, stator fabrication, material property characterization, and ceramic stator evaluation efforts are reported.

Trela, W.↗
DOE OSTI2015

Controlling the sol–gel process of nano-crystalline lithium-mica glass-ceramic by its chemical composition and synthesis parameters

This paper aims to explore the impact of the parameters such as pH of the system, refluxing temperature, water quantity and chemical composition on the sol–gel synthesis of lithium-mica glass-ceramic nano-powder. The synthesis process was accomplished using two chemical composition formula (Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} and LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2}). X-ray diffraction, Brunauer–Emmett–Teller surface area measurement and scanning electron microscopy techniques were applied to evaluate a variety of as-synthesized samples. Consequently, a transparent homogeneous sol was obtained under the conditions as pH ≤ 4, synthesis temperature ≤ 50 °C, and mol ratio of water to chemicals ≤ 2. The prepared nano-powders under such conditions were in the range of 60–100 nm. The results also revealed that the mica glass-ceramics prepared based on the composition Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} possessed finer powders due to their slow hydrolysis process. Moreover, any reduction in the stoichiometric deviation of lithium mica (x) leads to acquiring finer powders. - Highlights: • A transparent homogeneous sol leads to prepare nanopowders in the range of 60–100 nm. • The particles synthesized at lower temperatures possess finer sizes. • The acquired product which is prepared with excessive water offers larger sizes. • Any reduction in stoichiometric deviation leads to acquiring finer powders. • Taking synthesis composition as Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} offers finer powders.

36 MATERIALS SCIENCE↗
DOE OSTI2014

KNN–NTK composite lead-free piezoelectric ceramic

A (K,Na)NbO₃-based lead-free piezoelectric ceramic was successfully densified. It exhibited an enhanced electromechanical coupling factor of kₚ=0.52, a piezoelectric constant d₃₃=252 pC/N, and a frequency constant Nₚ=3170 Hz m because of the incorporation of an elaborate secondary phase composed primarily of KTiNbO₅. The ceramic's nominal composition was 0.92K₀.₄₂Na₀.₄₄Ca₀.₀₄Li₀.₀₂Nb₀.₈₅O₃–0.047K₀.₈₅Ti₀.₈₅Nb₁.₁₅O₅–0.023BaZrO₃ –0.0017Co₃O₄–0.002Fe₂O₃–0.005ZnO, abbreviated herein as KNN–NTK composite. The KNN–NTK ceramic exhibited a dense microstructure with few microvoids which significantly degraded its piezoelectric properties. Elemental maps recorded using transmission electron microscopy with energy-dispersive X-ray spectroscopy (TEM–EDS) revealed regions of high concentrations of Co and Zn inside the NTK phase. In addition, X-ray diffraction patterns confirmed that a small portion of the NTK phase was converted into K₂(Ti,Nb,Co,Zn)₆O₁₃ or CoZnTiO₄ by a possible reaction between Co and Zn solutes and the NTK phase during a programmed sintering schedule. TEM studies also clarified a distortion around the KNN/NTK interfaces. Such an NTK phase filled voids between KNN particles, resulting in an improved chemical stability of the KNN ceramic. The manufacturing process was subsequently scaled to 100 kg per batch for granulated ceramic powder using a spray-drying technique. The properties of the KNN–NTK composite ceramic produced using the scaled-up method were confirmed to be identical to those of the ceramic prepared by conventional solid-state reaction sintering. Consequently, slight changes in the NTK phase composition and the distortion around the KNN/NTK interfaces affected the KNN–NTK composite ceramic's piezoelectric characteristics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Scaling microstructural processes in the sintering of ionic ceramics

A multi-scale framework, combining a multiphase field formulation and large deformation mechanics, was developed as a stepping stone to perform the data analytics of the microstructural level kinetics of a sintering solid. Relevant microstructural information from this framework, such as grain, stress, and porosity statistics, was scaled up to describe the macroscopic level sintering kinetics. Here, the developed formulation was applied to describe the electric field assisted sintering of Y 2 O 3 . Microstructural inhomogeneities in a multi-granular solid result in the formation of a field of compressive stress networks, which interleave with low compression and weakly tensile regions, defining a scaffolding for sintering concentration regions to develop. A Poisson effect-induced lateral stress network is also naturally self-induced as a result of the mechanical constraints imposed by the sintering apparatus. For long sintering times, localized shear stresses enhancing mass flow along grain boundaries and internal surfaces develop. Three-sided pores are removed by either vacancy transport to the surrounding pores, or move towards the external surfaces through grain boundary diffusion. Four- and higher order-sided pores stabilize because an equal amount of vacancies are gained and lost through the connecting grain boundaries. Grain dewetting contributes to pore coalescence, suggesting that pore kinetics and grain growth are coupled and should be analyzed in concert. The combined sintering and grain growth kinetics define six regimes of sintering behavior: (1) T, the transient regime; (2) E$_Υ$, the surface energy dominated, early sintering regime, where the grain growth exponent, p = 1, and the stress concentration factor, $f$ ~ $1/\hat{ρ}^{4.6}$; (3) E S , the stress dominated, early sintering regime, where p = 1 and $f$ ~ $1/\hat{ρ}^{4}$; (4) I$_Υ$, the surface energy dominated, intermediate sintering regime, where p = 2 and $f$ ~ $1/\hat{ρ}^{4.6}$; (5) I S , the stress dominated, intermediate sintering regime, where p = 2 and $f$ ~ $1/\hat{ρ}^{4}$; and (6) L, the late sintering regime, where p = 3 and $f$ ~ 1. At the macroscopic level, the rapid densification and suppression of grain growth observed in the electric field assisted sintering process is a consequence of the compounding effects of the underlying stress-, transport-, and interfacial-energy-induced energy minimization kinetics, as predicted by the multi-scale framework.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1988

Fast Measurements Of Thermal Diffusivities Of Ceramics

Temperature rises of samples compared with reference sample. Apparatus quickly measures thermal diffusivities of ceramics at high temperatures. Produces data on relative thermal diffusivities of as many as six ceramic specimens per hour. Thermal-diffusivity tester makes it easy to determine thermal diffusivities of ceramics. Pronounced effects of processing parameters on thermal properties of ceramics evaluated quickly.

Smith, Marnell↗
NASA NTRS1991

Improving the temperature performance of low-density ceramic heatshields through sol-gel processing

The performance of rigid insulations for use as thermal protection materials on reentry vehicles can be characterized by their resistance to dimensional and morphological change when exposed to an isothermal environment equivalent to that generated in entry. Improvements in these material characteristics for alumina-enhanced thermal barrier insulation by compositional modification through sol-gel processing are reported.

Bull, Jeffrey↗
DOE OSTI2019

Template-based methods of making and using ceramic solids

Various embodiments relate to a method comprising forming a template from a template precursor, wherein the template contains an entrapped ceramic precursor, which can be further processed to form a ceramic solid, such as an oxide ceramic solid. In one embodiment, the template precursor is a hydrogel precursor and the template is a hydrogel template. The hydrogel template can include, for example, agarose, chitosan, alginate or a photo-initiating receptive hydrogel template such as a functionalized poly(ethylene glycol). Various devices, including electrolyte interfaces and energy storage devices, as well as thermoelectric devices are also provided. In one embodiment, the oxide ceramic solid is a cubic garnet having a nominal formula of Li7La3Zr2O12 (LLZO).

Sakamoto, Jeffrey↗
DOE OSTI2021

Thermal Processing Conditions for the Synthesis of Near Theoretical Density Li 5 La 3 Ta 2 O 12 Ceramics for Ceramic Dual-Mode Detectors

A family of Li-containing garnet compounds, extensively investigated for Li-ion solid electrolyte applications, show great potential to be developed into transparent ceramic dual-mode scintillators. In particular, Li 5 La 3 Ta 2 O 12 (LLTaO) shows promise as an efficient dual-mode scintillator due to its high Li content, high density, non-hygroscopicity, and high effective-Z. Often the synthesis of LLTaO ceramics involves solid state processing techniques starting with oxide and carbonate powders, calcining, sintering for the removal of residual porosity, and post-processing. This study focuses on two objectives: (1) establishing thermal processing boundary conditions for a flexible alkoxide-based sol-gel method for synthesizing fine-grained powders; and (2), consolidating powders via hot-pressing to form high-density ceramics. In this study, near single-phase ceramics were achieved by hot-pressing sol-gel powders with varying amounts of excess Li. Rietveld refinements were used to analyze X-ray diffraction data and provide a quantitative evaluation of the phases present in the hot pressed ceramics. Some of the diffraction data showed large low angle peak asymmetry, suggesting the presence of two cubic Li 5 La 3 Ta 2 O 12 garnet phases with different lattice parameters. Depending on the synthesis and processing conditions, the refinement revealed ~ 90 wt% concentration of a phase with a ≈ 12.8 Å and ~ 10 wt% concentration of a phase with a ≈ 12.9 Å, indicating a remaining excess of Li in the hot pressed ceramics in the large lattice parameter phase. These synthesis experiments allowed for the determination of a baseline for Li loss during hot-pressing. X-ray excited radioluminescence and photoluminescence excitation and emission spectra were obtained from the hot pressed ceramics. In conclusion, the measured emission spectra featured broad tantalate emission and line emissions likely from a rare-earth impurity.

36 MATERIALS SCIENCE↗
NASA NTRS1983

Evaluation of ceramics for stator applications: Gas turbine engines interim report. Stator fabrication and evaluation

The objective was to assess current ceramic materials, fabrication processes, reliability prediction, and stator durability when subjected to simulated automotive gas turbine engine operating conditions. Ceramic one-piece stators were fabricated of two materials, silicon nitride and silicon carbide, using two near-net-shape processes, slip casting and injection molding. Non-destructive evaluation tests were conducted on all stators identifying irregularities which could contribute to failures under durability testing. Development of the test rig and automatic control system for repeatably controlling air flow rate and temperature over a highly transient durability duty cycle is discussed. Durability results are presented for repeated thermal cycle testing of the ceramic one-piece stators. Two duty cycles were used, encompassing the temperature ranges of 704 to 1204 C (1300 to 2200 F) and 871 to 1371 C (1600 to 2500 F). Tests were conducted on 28 stators, accumulating 135,551 cycles in 2441 hours of hot testing. Cyclic durability for the ceramic one-piece stator was demonstrated to be in excess of 500 hours, accumulating over 28,850 thermal cycles. Ceramic interface forces were found to be the significant factor in limiting stator life rather than the scatter in material strength properties or the variation in component defects encountered.

Arnon, N.↗
DOE OSTI2020

Solid-State Sintering of Core-Shell Ceramic Powders Fabricated by Particle Atomic Layer Deposition

The properties of technical ceramics are highly dependent on their microstructure, which evolves during sintering. Sintering is the process by which ceramic parts are subjected to high temperatures to activate chemical diffusion and the consumption of porosity. During the initial stage of sintering, interparticle necks between neighboring particles form and subsequently increase in size, consuming porosity as the particle centers move closer together. To experimentally determine how this process depends on particle surface composition, particle atomic layer deposition (ALD) was used to deposit a thin film of amorphous aluminum oxide (Al2O3) onto yttria-stabilized tetragonal zirconia (3YSZ) particles, producing core-shell structured powders. The uniformity of the Al2O3 film was confirmed with transmission electron microscopy and energy dispersive spectroscopy. Scanning electron microscopy was used to observe microstructural evolution during sintering, and the dihedral angles of Al2O3 and 3YSZ grains were measured to determine the ratio of interfacial energies between the 3YSZ|3YSZ, 3YSZ|Al2O3, and Al2O3|Al2O3 interfaces. Analysis of the densification kinetics revealed that the initial stage of densification is dependent on the material at the surface of the particles (ie, the Al2O3 film) and is controlled by the diffusion of Al3+ cations through Al2O3. Once the Al2O3 film has coalesced, the sintering behavior is controlled by the densification of the core material (3YSZ). Thus, core-shell powders fabricated by particle ALD sinter by a two-step process where the kinetics are dependent on the material present at interparticle contacts.

alumina↗
DOE OSTI2020

The Influence of Printing Parameters, Post-Processing, and Testing Conditions on the Properties of Binder Jetting Additive Manufactured Functional Ceramics

This article outlines the current state-of-the-art binder jetting (BJT) additive manufacturing of functional ceramics. The impact of printing parameters, heat treatment processing, and testing conditions on the observed performance of these ceramics is discussed. Additionally, this article discusses the impact of physical properties such as density and mechanical strength on the overall performance of these functional ceramics. Although printing parameters and initial feedstock are crucial for the printability of the desired parts, other factors play an important role in the performance of the ceramic. Thermal post-processing is crucial to achieve optimized functional properties, while the testing orientation is key to obtaining the maximum output from the part. Finally, future research directions for this field are also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Gas turbine blade with intra-span snubber

A gas turbine blade (10) including a hollow mid-span snubber (16). The snubber is affixed to the airfoil portion (14) of the blade by a fastener (20) passing through an opening (24) cast into the surface (22) of the blade. The opening is defined during an investment casting process by a ceramic pedestal (38) which is positioned between a ceramic core (32) and a surrounding ceramic casting shell (48). The pedestal provides mechanical support for the ceramic core during both wax and molten metal injection steps of the investment casting process.

42 ENGINEERING↗
DOE OSTI2024

Simplified, Infiltration-free Ceramic Matrix Composite Manufacturing

Manufacturing of ceramic matrix composites (CMCs) with carbon fiber and carbon matrix includes a time- and labor-intensive ceramic infiltration step that is responsible for more than half of the total manufacturing cost. To make CMCs cost-competitive in price-sensitive markets, like concentrated solar power, it is essential to develop a CMC manufacturing process that skips the ceramic infiltration process. In this work, we will show how a high-char-yield preceramic resin can eliminate the infiltration step while maintaining material density and evaluate the technoeconomic impact of our CMC manufacturing process. Here, we monitor both morphology and porosity to determine the quality of CMCs made with different preceramic resins and evaluate the impact of polymer infiltration and pyrolyzing cycles.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Additive Manufacturing of C/C-SiC Ceramic Matrix Composites by Automated Fiber Placement of Continuous Fiber Tow in Polymer with Pyrolysis and Reactive Silicon Melt Infiltration

An additive manufacturing process for fabricating ceramic matrix composites has been developed based on the C/C-SiC system. Automated fiber placement of the continuous carbon fibers in a polyether ether ketone matrix was performed to consolidate the carbon fibers into a printed preform. Pyrolysis was performed to convert the polymer matrix to porous carbon, and then Si was introduced by reactive melt infiltration to convert a portion of the carbon matrix to silicon carbide. The densities and microstructures were characterized after each step during the processing, and the mechanical properties were measured. The C/C-SiC composites exhibited a porosity of 10–20%, characteristic flexural strength of 234.91 MPa, and Weibull modulus of 3.21. The composites displayed toughness via a significant displacement to failure.

36 MATERIALS SCIENCE↗