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At least 1,279 records · Page 71
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Development and Mechanical Properties of In Situ Al{sub 3}Ti-Reinforced Nanostructured AA6061 via Mechanical Alloying

Mechanical alloying (MA) was used to disperse 10 wt.% titanium powder in AA6061 powder. The resultant powder was degassed, and differential scanning calorimetry was performed to determine the temperature for formation of titanium aluminide (Al{sub 3}Ti). The MA powder was characterized by field emission scanning electron microscopy, x-ray diffraction (XRD) and transmission electron microscopy (TEM). Subsequently, the MA powder was consolidated by spark plasma sintering (SPS) at 500 °C under a pressure of 50 MPa. XRD and x-ray energy-dispersive spectroscopy of spark plasma sintered compact revealed in situ formation of Al{sub 3}Ti. TEM micrographs of spark plasma sintered sample exhibited Al nanograins (average size 50 nm) in the AA6061 matrix along with the dispersed Al{sub 3}Ti (average size 200 nm). Hardness, yield strength and compressive strength of the SPSed samples were also evaluated and compared with AA6061.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The Improved Thermal Conductivity of a Potting Material for High-Power Fast Warm-Up Cathodes

With higher power, frequency and longer life of microwave tubes, cathode heater assembly is being modified to enhance the warm-up performance and reliability, which are governed by ceramics thermal conductivity, electrical resistivity and shrinkage. In present work, a potting material with a high thermal conductivity of 22.14 W/(m K) and low linear shrinkage of 5.5% was prepared using two kinds of alumina powders with different size and morphology. Aqueous slurries were produced for centrifugal casting. The highest solid loading slurries with 70 vol.% were obtained. Green body with relative density above 70% was easily made from slurries using centrifugal casting. Relative sintered density reached 86.75% maximum without any sintering aids. Rheological behavior of slurries, potting microstructure, sintering shrinkage and thermal conductivity were analyzed. Continuous particle distribution, series and parallel models were used to guide the powders proportion and explain the thermal conductivity. The potting material thermal conductivity experimental data agreed with the series and parallel models when the weight parameter ξ was between 0.3 and 0.5.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Y{sub 2}O{sub 3} Addition on the Microstructure, Wear Resistance, and Corrosion Behavior of W-4.9Ni-2.1Fe Heavy Alloy

Binding and particle phases are the two important parameters influencing materials properties. In this study, a series of novel W-4.9Ni-2.1Fe-xY{sub 2}O{sub 3} (in weight%) alloys with different Y{sub 2}O{sub 3} contents are prepared by secondary ball milling and spark plasma sintering (SPS) techniques to obtain uniformly distributed γ-(Ni, Fe) binding phases and finer grains. The microstructure, mechanical, wear resistance, and corrosion behavior of the sintered bodies with different Y{sub 2}O{sub 3} were obtained by x-ray diffraction, scanning electron microscopy, Rockwell hardness tester, friction wear tester, and three-dimensional profile instruments. The results showed that a certain addition of Y{sub 2}O{sub 3} led to refined grains and uniformed microstructures; but, if excessive, a weak grain refinement would be appeared. Moreover, the grain size tends to be stable with enhancing of the Y{sub 2}O{sub 3} content. Considering properties such as density, hardness, compression yield strength, grain size, and uniform distribution of tungsten hard phase and γ-(Ni, Fe) binding phase, the comprehensive optimal amount of 0.7 wt.% of Y{sub 2}O{sub 3} was attained for the alloy. Meanwhile, the SPS sintered body also exhibited the best friction, wear behavior, and corrosion resistance in 3.5% of NaCl solution.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Direct in situ observation of electric field assisted densification of ZnO by energy dispersive X-ray diffraction

Electric field assisted sintering techniques are used to enhance the densification process, reducing sintering time and temperature. Here, we report the in situ characterization of non-isothermal densification behavior of zinc oxide under simultaneous application of thermal and electric field by energy dispersive X-ray diffraction. 99% density was achieved under the electric field of 50 V/mm in the 588–843 °C range in a short time without grain growth. The in-situ energy dispersive X-ray diffraction study revealed the abnormal volumetric unit cell expansion of 0.9% at 843 °C associated with the observed sudden rise of the power absorption by the specimen during densification. Furthermore, the variation in peak broadening as a function of time exhibited singularity in the 588–843 °C range implying the formation and rearrangement of defects correlated with densification during electric field assisted sintering.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Processing and characterization of the homologous Zr x Ta 2 O 2x+5 series

In this study, Zr x Ta 2 O 2x+5 (ZTOx) was systematically studied to determine ideal solid-state synthesis and pressureless sintering conditions. For Zr 6 Ta 2 O 17 (ZTO6) and other compositions with values of x in ZTOx the optimal synthesis temperature of 1100 °C with 1 h dwell time was optimal. XRD phase analysis of the homologous series indicated that for ZTOx, x = 5, 6, 7, and 8 were within the phase stability field while x = 4 and x = 9 were outside the phase stability field. Unit cell lattice parameters changed anisotropically with Zr:Ta ratio with an overall <0.1% change in unit cell volume across the solid solution. Some Raman modes red shifted while others blue shifted, indicating competing tensile and compressive strains. Sintering of ZTOx required a progressively higher temperature as Zr-content increased despite the same starting powder grain sizes and synthesis temperature. Higher Vickers hardness for Zr-rich (12.7–12.8 GPa) than Ta-rich Zr x Ta 2 O 2x+5 (11.6–11.7 GPa) disappeared when accounting for different sintering temperatures. Indentation toughness was similar for all compositions (1.2–1.4 MPa m 1/2 ). Properties of Zr x Ta 2 O 2x+5 series indicate tunability of Zr:Ta composition ratio while maintaining the structure and room temperature mechanical properties comparable to Hf 6 Ta 2 O 17 and 8 mol% yttria stabilized zirconia ceramics.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Physicochemical properties of digital light processing 3D-Printed alumina and mullite ceramics

Alumina ceramics fabricated using conventional techniques such as uniaxial pressing or injection molding are popular due to their low density, excellent insulation, and mechanical properties. However, these methods often limit the fabrication of complex geometries with high dimensional accuracy due to tooling constraints and limited design freedom. To overcome these limitations, this study employed Digital Light Processing (DLP) additive manufacturing (AM), which enables the production of precise structures. In addition, the optimization of sintering parameters to enhance the densification and performance of alumina and mullite ceramics was investigated, with a specific focus on how varying sintering temperatures and hold times affect part shrinkage, geometric accuracy, and material integrity. Flexural strength of both alumina and mullite specimens was clearly influenced by the way the layers was stacked. When layers were arranged across the direction of the applied load (Z = 4; XZ), the strength was higher than when they were stacked along the same direction as the load (Z = 3; XY). Weibull analysis based on these results showed high modulus values across all samples, indicating good reliability in the flexural strength measurements. This reliability, combined with the clear influence of sintering parameters, highlights how processing conditions effect the material properties and mechanical performance of parts produced through DLP additive manufacturing. In conclusion, these findings open new avenues for ceramic AM across various applications, enhancing the potential for innovation in fields such as aerospace, biomedical engineering, and energy.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Manufacturing porous U10Zr fuels with controlled porosities by SPS and thermal properties

To accommodate the swelling of metallic fuels induced by the fission gas release during burnup in sodium fast reactor for a sodium-free fuel option, advanced U-10Zr fuels with controlled porosity were designed and demonstrated by spark plasma sintering. U-10Zr fuel pellets with manufactured porosities varying from 35% up to fully dense fuel pellets have been fabricated by controlling ball milling times of the starting uranium powders, sintering temperature, pressure, and duration, and the correlation among the microstructure control – porosity – sintering conditions has been established. To further mimick the pore structure in irradiated fuels, different pore formers (NaCl and NH4HCO3) have been used to control the pore size and distribution. Microstructure characterization indicates a lamellar reaction zone of U and Zr, differing from the arc-melted U-10Zr as a result of rapid consolidation of SPS at lower temperature and short durations. The thermal conductivity of U10Zr with different porosities are also measured. Here this work demonstrates the success in manufacturing new metallic fuel forms with controlled porosities and pore distribution, which can be used as model systems to investigate the thermal transfer behavior of metallic fuels in the reactor.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Unraveling the conundrum of electronic leakage in protonic ceramic cells: Operation-specific insights and rational design strategies

Electronic conduction through proton-conducting electrolytes significantly impairs the efficiency of protonic ceramic cells (PCCs). Here, in this study, we explore the electron and ion mixed transport properties of four common protonic ceramics, BaZr 0.8 Y 0.2 O 3-δ (BZY82), BaZr 0.7 Ce 0.2 Y 0.1 O 3-δ (BZCY721), BaZr 04 Ce 0.4 Y 0.1 Yb 0.1 O 3-δ (BZCYYb4411), and BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ (BZCYYb1711). It marks the first instance of investigating these properties under operation-specific scenarios: fuel side of electrolysis cell, air side of electrolysis cell, fuel side of fuel cell, and air side of the fuel cell. BZCYYb1711 exhibits the highest ionic conductivity, but two to three times higher electronic leakage when exposed to oxygen-containing environments than the others. BZY82 exhibits approximately two times higher electronic leakage in a hydrogen-containing environment. BZCY721 demonstrates excellent ion transport numbers (~0.95) across these four operating conditions. BZCYYb4411 behaves quite similarly to BZCY721. The most challenging operating environment for all candidates is the air side of fuel cell mode. This mode leads to a high initial electronic leakage, followed by a significant increase with polarization. The probable cause for this behavior is a H 2 -free, polarization-induced reduction that leads to the formation of V$^•_O$. The electron small polaron associated with V$^•_O$ is released by the electrical field due to the Poole-Frenkel effect. ZnO and NiO sintering aids are found to be detrimental to the ionic conductivity of the electrolytes. In particular, NiO substantially lowers the ion transport number. The correlation of the operation-specific electronic leakage to full cells is discussed. It is suggested that a rational PCC design should synergistically couple BZCYYb1711 at fuel side with BZCY4411 at air side to deliver a well-balanced performance and faradaic efficiency simultaneously, and the high temperature sintering process with a NiO fuel electrode should be shortened or replaced by ultra-fast sintering techniques or using a fuel electrode scaffold-infiltration fabrication strategy.

42 ENGINEERING↗
DOE OSTI2015

Comparative study of phase transition and textural changes upon calcination of two commercial titania samples: A pure anatase and a mixed anatase-rutile

The effect of calcination temperature and time on structural and textural changes of two commercial TiO{sub 2} samples (pure anatase and a mixture of anatase and rutile) has been investigated using N{sub 2} physisorption, ex-situ and in-situ X-ray powder diffraction, differential scanning calorimetry and UV–vis diffuse reflectance spectroscopy. The increase of the calcination temperature (up to 700 °C) and time (up to 8 h) causes only textural changes in the pure anatase, whereas a transformation of the anatase to rutile takes place, in addition, in the mixed titania (containing anatase and rutile). The textural changes observed in pure anatase sample were attributed to solid state diffusion leading to an increase in the size of anatase nanocrystals, through sintering. Thus, the mean pore diameter shifts to higher values and the pore volume and specific surface area decrease. The successful application of the Johnson–Mehl–Avrami–Kolmogorov model in the kinetic data concerning the pure anatase indicates a mass transfer control of sintering process. Similar textural changes were also observed upon calcination of the sample containing anatase and rutile. In this case not only sintering but the anatase to rutile transformation contributes also to the textural changes. Kinetic analysis showed that the rutile nanocrystals in the mixed titania served as seed for by-passing the high energy barrier nucleation step allowing/facilitating thus the anatase to rutile transformation. A fine control of the anatase to rutile ratio and thus of energy-gap and the population of hetero-junctions may be obtained by adjusting the calcination temperature and time. - Graphical Abstract: Dependence of anatase content of P25 on the calcination temperature (600 °C (■), 650 °C (●), 700 °C (▲)) and time. - Highlights: • Increase of calcination temperature up to 800 °C and time up to 8 h causes only textural changes in pure anatase • Progressive transformation of anatase to rutile with time takes place in the mixed titania above 600 °C • A high activation energy barrier inhibits the solid state transformation in pure anatase • Rutile nanocrystals in mixed titania serve as seeding for favouring transformation • Calcination temperature and time allow a fine control of E{sub g} and heterojunctions population in mixed titania.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

On fabrication procedures of Li-ion conducting garnets

Ceramic oxides exhibiting high lithium-ion mobility at room temperature receive broad attention as candidate electrolytes for lithium batteries. Lithium-stuffed garnets from the Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} group seem to be especially promising because of their high ionic conductivity at room temperature and their electrochemical stability. In this work, we discuss factors that affect formation of the garnet in its bulk form or in the form of thick and thin films. We demonstrate that zinc oxide can be applied as a sintering aid that facilitate the formation of the highly conducting cubic Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} garnet phase in a single-step sintering procedure. Based on our experience with the single-step sintering experiments, we successfully fabricated a thick-film membrane consisting of a garnet solid electrolyte using the tape casting technique. In order to reduce the thickness of the electrolyte even further we investigated the fabrication of a thin-film Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} electrolyte by means of the pulsed laser deposition technique.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Tribological properties of self-lubricating NiAl/Mo-based composites containing AgVO{sub 3} nanowires

Silver vanadate (AgVO{sub 3}) nanowires were synthesized by hydrothermal method and self-lubricating NiAl/Mo-AgVO{sub 3} composites were fabricated by powder metallurgy technique. The composition and microstructure of NiAl/Mo-based composites were characterized and the tribological properties were investigated from room temperature to 900 °C. The results showed that NiAl/Mo-based composites were consisted of nanocrystalline B2 ordered NiAl matrix, Al{sub 2}O{sub 3}, Mo{sub 2}C, metallic Ag and vanadium oxide phase. The appearance of metallic Ag and vanadium oxide phase can be attributed to the decomposition of AgVO{sub 3} during sintering. Wear testing results confirmed that NiAl/Mo-based composites have excellent tribological properties over a wide temperature range. For example, the friction coefficient and wear rate of NiAl/Mo-based composites containing AgVO{sub 3} were significantly lower than the composites containing only metallic Mo or AgVO{sub 3} lubricant when the temperature is above 300 °C, which can be attributed to the synergistic lubricating action of metallic Mo and AgVO{sub 3} lubricants. Furthermore, Raman results indicated that the composition on the worn surface of NiAl-based composites was self-adjusted after wear testing at different temperatures. For example, Ag{sub 3}VO{sub 4} and Fe{sub 3}O{sub 4} lubricants were responsible for the improvement of tribological properties at 500 °C, AgVO{sub 3}, Ag{sub 3}VO{sub 4} and molybdate for 700 °C, and AgVO{sub 3} and molybdate for 900 °C of NiAl-based composites with the addition of metallic Mo and AgVO{sub 3}. - Highlights: • NiAl/Mo-AgVO{sub 3} nanocomposites were prepared by mechanical alloying and sintering. • AgVO{sub 3} decomposed to metallic Ag and vanadium oxide during the sintering process. • NiAl/Mo-AgVO{sub 3} exhibited superior tribological properties at a board temperature range. • Phase composition on the worn surface was varied with temperatures. • Self-adjusted action was responsible for the improvement of tribological properties.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Infiltrated W–Cu composites with combined architecture of hierarchical particulate tungsten and tungsten fibers

In this article, novel W–Cu composites reinforced with topologically-inserted tungsten fibers (W{sub f}) have been fabricated by hot-press sintering and infiltration method. By pre-sputtering of ~ 100 nm thick chromium layer onto the surface of W{sub f}, the contiguity or connectivity between W{sub f} and neighboring tungsten particles (W{sub p}) or Cu after sintering and infiltration was enhanced. Combined SEM, TEM and STEM techniques confirmed that the intact interfaces of W{sub f}/W{sub p} and W{sub f}/Cu free from precipitates, impurities and porosities would provide desirable strength and ductility. Further mechanical tests also validated its superior compressive strength and plasticity at various temperatures, together with significantly improved tensile strength (by 23.6%) and hardness (by 9.3%) for the W–Cu composite after reinforcement with Cr-coated W{sub f}, which promotes the engineering application of the composite greatly. - Highlights: • W-fibers reinforced W–Cu composites were fabricated by sintering and infiltration. • The sputtered Cr onto W{sub f} has dissolved into adjacent W{sub f} and W{sub p} during fabrication. • The intact interfaces of W{sub f}/W{sub p} and W{sub f}/Cu confer enhanced strength and ductility. • Tensile strength and hardness improve by 23.6% and 9.3% after interface tuning.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effect of vanadium carbide on dry sliding wear behavior of powder metallurgy AISI M2 high speed steel processed by concentrated solar energy

Mixtures of AISI M2 high speed steel and vanadium carbide (3, 6 or 10 wt.%) were prepared by powder metallurgy and sintered by concentrated solar energy (CSE). Two different powerful solar furnaces were employed to sinter the parts and the results were compared with those obtained by conventional powder metallurgy using a tubular electric furnace. CSE allowed significant reduction of processing times and high heating rates. The wear resistance of compacts was studied by using rotating pin-on-disk and linearly reciprocating ball-on-flat methods. Wear mechanisms were investigated by means of scanning electron microscopy (SEM) observations and chemical inspections of the microstructures of the samples. Better wear properties than those obtained by conventional powder metallurgy were achieved. The refinement of the microstructure and the formation of carbonitrides were the reasons for this. - Highlights: •Powder metallurgy of mixtures of M2 high speed steel and VC are studied. •Some sintering is done by concentrated solar energy. •Rotating pin-on-disk and linearly reciprocating ball-on-flat methods are used. •The tribological properties and wear mechanisms, under dry sliding, are studied.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural characterization and mechanical properties of a novel TiC-based cermet bonded with Ni3(Al,Ti) and NiAl duplexalloy

A novel TiC/Ni{sub 3}(Al,Ti)-NiAl composite has been designed and synthesized by in-situ reactive hot-pressing a mixture of Ti{sub 3}AlC{sub 2} and Ni powders. After hot-press sintering at 1500 °C and 30 MPa, almost fully dense composite was obtained and the in-situ formed TiC grains were well-bonded with Ni{sub 3}(Al,Ti) and NiAl alloys. Due to the nanolaminated structure in Ti{sub 3}AlC{sub 2} materials that weakly bonded Al layers are more prone to be out-diffused from Ti{sub 3}AlC{sub 2} lattice than that of Ti atoms. The deintercalated AlTi atoms would react with Ni to give rise to the formation of Ni{sub 3}(Al,Ti) and NiAl alloys, and meanwhile a crystal lattice structure transformation happened from hexagonal Ti{sub 3}AlC{sub 2} to cubic lattice TiC. The formation of phases, grains morphologies, sintering behavior and mechanical properties were associated with sintering temperature. The as prepared TiC/Ni{sub 3}(Al,Ti)-NiAl composite under 1500 °C exhibited superior mechanical properties comparing with the counterparts fabricated under 1350 °C and 1400 °C because of the enhanced microstructures and eliminations of pores. Hardness, flexural strength and fracture toughness of the TiC/Ni{sub 3}(Al,Ti)-NiAl composite at room temperature were determined as 9.9 ± 0.35 GPa, 665 ± 26 MPa and 10.23 ± 0.4 MPa·m{sup 1/2}, respectively. Interestingly, the flexural strength and fracture toughness increases with temperature rising from 600 to 800 °C, the maximum of flexural strength and fracture toughness could reach 775 ± 25 MPa and 11.6 ± 0.4 MPa·m{sup 1/2} at 800 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Compositional inhomogeneity and its effect on the hardness of nanostructured refractory high-entropy alloys

The pronounced compositional inhomogeneity observed in refractory high-entropy alloys (HEAs), as opposed to non-refractory HEAs, has an important influence on their mechanical properties, thereby posing a significant challenge for the development of high-performance refractory HEAs. In this work, by combining transmission electron microscopy imaging, chemical analysis, and nano-hardness tests, we investigate the compositional inhomogeneities in a series of sintered nanostructured HEAs and elucidate their influence on the material's hardness. Further, we reveal that the compositional inhomogeneity of the sintered nanostructured HEAs is temperature- and component- dependent. By correlating the hardness of nanostructured HEAs to the evolving compositional inhomogeneity, our work demonstrates that the compositional inhomogeneity in nanostructured HEAs can be tuned by sintering temperature or alloying towards optimized microstructure and hardness.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2013

Preparation of W–Sc{sub 2}O{sub 3} targets and scandate cathodes with film prepared by pulsed laser deposition

Graphical abstract: - Highlights: • W–Sc{sub 2}O{sub 3} film containing 5% Sc{sub 2}O{sub 3} and 95% W were prepared by pulsed laser deposition. • W–Sc{sub 2}O{sub 3} film on scandate cathode surface improves emission property. • The film improves Sc distribution uniformity and is favorable for forming Ba–Sc–O layer. - Abstract: Sub-micrometer Sc{sub 2}O{sub 3}–W powder with a narrow particle size distribution has been obtained by a sol–gel method combined with two-step hydrogen reduction process. Based on the obtained powder, the W–Sc{sub 2}O{sub 3} targets have been sintered via spark plasma sintering (SPS) at 1300 °C. The W–Sc{sub 2}O{sub 3} targets have the average grain size of about 1 μm. Both the sintering temperature and holding time are much lower than those of the targets prepared with micrometer sized powders. The obtained W–Sc{sub 2}O{sub 3} targets have a high comparative density of 96.4% and rockwell hardness of 86.4 HRC. Using the target, the scandate cathode deposited with a film containing 5% Sc{sub 2}O{sub 3} and 95% W has been obtained by pulsed laser deposition (PLD) method. This cathode has good emission property, i.e., the highest thermionic emission current density reaches 43.09 A/cm{sup 2} of J{sub div} at 900 °C{sub b} after being activated for 8 h, which is much higher than that of scandate cathode without film. Scandium (Sc) supplied by the film on the surface during the activation forms a Ba–Sc–O active layer, which helps to the emission.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Highly porous ZnS microspheres for superior photoactivity after Au and Pt deposition and thermal treatment

Graphical abstract: Highly porous ZnS microsphere of size 2–5 μm having large surface area ca. 173.14 m{sup 2} g{sup −1} exhibits superior photocatalytic activity for the oxidation of 4-nitrophenol under UV light irradiation. The rate of photooxidation has been significantly improved by Au and Pt deposition and after sintering, respectively, due to rapid electron acceptance by metal from photoexcited ZnS and growth of crystalline ZnS phase. - Highlights: • Photoactive ZnS microsphere of size 2–5 μm was prepared by hydrothermal route. • Highly porous cubic spherical ZnS crystals possess a large surface area, 173 m{sup 2} g{sup −1}. • 1 wt% Au and Pt photodeposition highly quenched the photoluminescence at 437 nm. • Sintering and metal loading notably improve the photooxidation rate of 4-nitrophenol. • Pt co-catalyst always exhibits superior photoactivity of ZnS microsphere than Au. - Abstract: This work highlights the enhanced photocatalytic activity of porous ZnS microspheres after Au and Pt deposition and heat treatment at 500 °C for 2 h. Microporous ZnS particles of size 2–5 μm with large surface area 173.14 m{sup 2} g{sup −1} and pore volume 0.0212 cm{sup 3} g{sup −1} were prepared by refluxing under an alkaline medium. Photoluminescence of ZnS at 437 nm attributed to sulfur or zinc vacancies were quenched to 30% and 49%, respectively, after 1 wt% Au and Pt loading. SEM images revealed that each ZnS microparticle consist of several smaller ZnS spheres of size 2.13 nm as calculated by Scherrer's equation. The rate of photooxidation of 4-nitrophenol (10 μM) under UV (125 W Hg arc–10.4 mW/cm{sup 2}) irradiation has been significantly improved by Au and Pt deposition followed by sintering due to better electron capturing capacity of deposited metals and growth of crystalline ZnS phase with less surface defects.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Investigation of grain-boundary geometry and pores morphology in dense and porous cubic zirconia polycrystals

Highlights: • Cubic zirconia sinters were investigated in three dimensions using dual-beam FEGSEM. • The 3D-EBSD technique was successfully applied to non-conductive ceramics. • New sample preparation approach to automated 3D-EBSD was proposed. • Grain boundary microstructures were reconstructed from inverse pole figure maps. • Pore microstructures were reconstructed from image quality maps. - Abstract: Three-dimensional electron backscatter diffraction technique was used for the visualization of grain boundary geometry and pore morphology in cubic zirconia. A set of four samples sintered under different conditions was investigated. Specimens which were characterized by energy dispersive spectroscopy and X-ray diffraction were entirely composed of cubic phase. Investigations of boundaries and pore structures were carried out in a dual-beam scanning electron microscope. For each sample, a volume of 1000 μm{sup 3} was investigated. The analysis of grain boundary networks reconstructed from inverse pole figure maps revealed a strong dependence between grain boundary density and sample preparation parameters. Sintering also affects the size and distribution of pores. The total number of grains analyzed varied from 17 to 357 and the calculated volume of cavities from 0.01% to 21%. This paper shows the application of three-dimensional crystallographic orientation analysis to characterize the microstructure of yttria stabilized zirconia ceramics.

36 MATERIALS SCIENCE↗