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At least 559 records · Page 31

Gravitational Effects on the Morphology and Kinetics of Photodeposition of Polydiacetylene Thin Films From Monomer Solutions

The goal of this proposed work is to study gravitational effects on the photodeposition of polydiacetylene thin films from monomer solutions onto transparent substrates. Polydiacetylenes have been an extensively studied class of organic polymers because they exhibit many unusual and interesting properties, including electrical conductivity and optical nonlinearity. Their long polymeric chains render polydiacetylenes readily conducive to thin film formation, which is necessary for many applications. These applications require thin polydiacetylene films possessing uniform thicknesses, high purity, minimal inhomogeneities and defects (such as scattering centers), etc. Also, understanding and controlling the microstructure and morphology of the films is important for optimizing their electronic and optical properties. The lack of techniques for processing polydiacetylenes into such films has been the primary limitation to their commercial use. We have recently discovered a novel method for the formation of polydiacetylene thin films using photo-deposition from monomer solutions onto transparent substrates with UV light. This technique is very simple to carry out, and can yield films with superior quality to those produced by conventional methods. Furthermore, these films exhibit good third-order properties and are capable of waveguiding. We have been actively studying the chemistry of diacetylene polymerization in solution and the photo-deposition of polydiacetylene thin films from solution. It is well-known that gravitational factors such as buoyancy-driven convection and sedimentation can affect chemical and mass transport processes in solution. One important aspect of polydiacetylene thin film photodeposition in solution, relevant to microgravity science, is that heat generated by absorption of UV radiation induces thermal density gradients that under the influence of gravity, can cause fluid flows (buoyancy-driven convection). Additionally, changes in the chemical composition of the solution during polymerization may cause solutal convection. These fluid flows affect transport of material to and from the film surface and thereby affect the kinetics of the growth process. This manifests itself in the morphology of the resulting films; films grown under the influence of convection tend to have less uniform thicknesses, and can possess greater inhomogeneities and defects. Specifically, polydiacetylene films photodeposited from solution, when viewed under a microscope, exhibit very small particles of solid polymer which get transported by convection from the bulk solution to the surface of the growing film and become embedded. Even when carried out under conditions designed to minimize unstable density gradients (i.e., irradiating the solution from the top), some fluid flow still takes place (particles remain present in the films). It is also possible that defect nucleation may be occurring within the films or on the surface of the substrate; this, too, can be affected by convection (as is the case with crystal growth). Hence films grown in 1-g will, at best, still possess some defects. The objective of this proposal is to investigate, both in 1-g and in low-g, the effects of gravitational factors (primarily convection) on the dynamics of these processes, and on the quality, morphology, and properties of the films obtained.

Paley, Mark S.↗

An additively manufactured AlCuMnZr alloy microstructure and tensile mechanical properties

In this study, selective laser melting (SLM) was used to fabricate an AlCuMnZr alloy. The microstructural features that resulted from additive manufacturing (AM) were significantly refined compared to the corresponding cast alloy features. A combination of fine equiaxed and columnar grains along with in-situ formation of θ' precipitates during AM leads to enhanced yield strength (up to 300°C) in the as-fabricated AM alloy. The refinement of brittle intermetallics and a bimodal grain size distribution leads to improved tensile elongation in the AM alloy. The results illustrate the microstructural advantages that can result from additive processing over conventionally processed microstructures.

36 MATERIALS SCIENCE↗

Evolution of microstructure and strength of a high entropy alloy undergoing the strain-induced martensitic transformation

In a recent work, we have reported outstanding strength and work hardening exhibited by a metastable high entropy alloy (HEA), Fe 42 Mn 28 Co 10 Cr 15 Si 5 (in at. %), undergoing the strain-induced martensitic transformation from metastable gamma austenite (γ) to stable epsilon martensite (ε). However, the alloy exhibited poor ductility, which was attributed to the presence of the brittle sigma (σ) phase in its microstructure. The present work reports the evolution of microstructure, strength, and ductility of a similar HEA, Fe 38.5 Mn 20 Co 20 Cr 15 Si 5 Cu 1.5 (in at. %), designed to suppress the formation of σ phase. A cast and then rolled plate of the alloy was processed into four conditions by annealing for 10 and 30 min at 1100 °C and by friction stir processing (FSP) at tool rotation rates of 150 and 400 revolutions per minute (RPM) to facilitate detailed examinations of variable initial grain structures. Neutron diffraction and electron microscopy were employed to characterize the microstructure and texture evolution. The initial materials had variable grain size but nearly 100% γ structure. Diffusionless strain induced γ→ε phase transformation took place under compression with higher rate initially and slower rate at the later stages of deformation, independent on the initial grain size. The transformation facilitated part of plastic strain accommodation and rapid strain hardening owing to a transformation-induced dynamic Hall-Petch-type barrier effect, increase in dislocation density, and texture. Here, the peak strength of nearly 2 GPa was achieved under compression using the structure created by double pass FSP (150 RPM followed by 150 RPM). Remarkably, the tensile elongation exhibited by the alloy was nearly 20% with fracture surfaces featuring a combination of ductile dimples and cleavage.

36 MATERIALS SCIENCE↗

Microstructural Characterization of Thin Polyimide Films by Positron Lifetime Spectroscopy

Positron lifetimes have been measured in a series of thin aromatic polyimide films. No evidence of positronium formation was observed in any of the films investigated. All test films exhibited only two positron lifetime components, the longer component corresponding to the positrons annihilating at shallow traps. Based on these trapped positron lifetimes, free volume fractions have been calculated for all the films tested. A free volume model has been developed to calculate the dielectric constants of thin polyimide films. The experimental and the calculated values for the dielectric constants of the films tested are in reasonably good agreement. It has been further noted that the presence of bulky CF(sub 3) groups and meta linkages in the polyimide structure results in higher free volume fraction and, consequently, lower dielectric constant values for the films studied.

Eftekhari, A.↗

Creep ductility limiting mechanisms in an additively manufactured Al-Ce-Ni-Mn-Zr alloy

Tensile creep response and cavitation damage evolution in an additively manufactured Al-7.5Ce-4.5Ni-0.4Mn-0.7Zr (wt%) alloy with peak-aging and overaging treatments were investigated in the 300–400 ºC range. Microstructural heterogeneity and its response to heat treatment and subsequent creep deformation were studied to understand the interplay between cavity formation, creep lifetime and ductility. Increasing the applied stress activated the nucleation of more cavities, an experimental observation that is well described using the vacancy accumulation model. Cavities nucleated prematurely due to localized plasticity in the denuded zones that formed at/near melt-pool or grain boundaries. Microstructure/deformation heterogeneity with consequent evolution of stress triaxiality, especially at lower stresses, causes accelerated cavitation, thus producing low creep ductility (∼ 0.2–2.4 %), compared to (∼12–21 %) ductility of the alloy measured by regular tensile tests at equivalent temperatures. A constrained diffusional cavity growth mechanism with continuous cavity nucleation during creep is established as the dominant mechanism, implying that cavitation involves vacancy diffusion, yet its growth rate is dictated by the minimum creep rate. In conclusion, the ductility-limiting creep and cavitation mechanisms discussed here provide new insight into the creep behavior of 3D-printed metallic alloys.

Additive manufacturing↗

Surface and grain boundary carbon heterogeneity in CH 3 NH 3 PbI 3 perovskites and its impact on optoelectronic properties

Rivaling state-of-the-art crystalline silicon, organic-inorganic hybrid perovskites have been intensely studied in recent years. Surface and interfacial engineering have been a focus for performance improvement. Even though significant progress has been made during the last decade in terms of the diversity and capability of perovskite-based devices, the structure-property relationship, particularly at the surface, which governs the real-world performance of these applications, is still unresolved. In the article, this issue was addressed by employing synchrotron-related experimental measurements, and a mechanism that correlates microstructure with surface chemistry was resolved. As a powerful and highly sensitive spectromicroscopy, soft x ray photoemission electron microscopy (X-PEEM) was used to probe the surface of perovskite films varying in post solvent annealing. Furthermore, static and in situ grazing incidence hard x ray diffraction (GIXD) was used to track the grain growth dynamics during the film formation process. It was found that the nature of the surfaces was dictated by the local chemistry that varied due to mass flow during the development of the microstructure. Combining optical and electronic characterizations, it was confirmed that a more homogenous chemistry, i.e., uniform chemical components and properties, along with reduced strain and grain boundary energies, yielded more defect-tolerant films. Grain boundaries were more favorable for screening carriers than those in the control film. Our findings underscore the importance of the uniformity in the surface for developing a chemistry-structure-property relationship in perovskite materials, as well as engineering local chemistry toward high-performance and stable devices.

42 ENGINEERING↗

The Influence of Nominal Composition on the Microstructure, Tensile Properties, and Weldability of Cast Monel Alloys

Cast Monel alloys are used in many industrial applications that require a combination of good mechanical properties and excellent resistance to corrosion. Despite relative widespread use, there has been limited prior research investigating the fundamental composition–structure–property relationships. Here in this work, microstructural characterization, thermal analysis, electron probe microanalysis, tensile testing, and Varestraint testing were used to assess the effects of variations in nominal composition on the solidification path, microstructure, mechanical properties, and solidification cracking susceptibility of cast Monel alloys. It was found that Si segregation caused the formation of silicides at the end of solidification in grades containing at least 3 wt pct Si. While increases to Si content led to significant improvements in strengthening due to the precipitation of β 1 -Ni 3 Si, the silicide eutectics acted as crack nucleation sites during tensile loading which severely reduced ductility. The solidification cracking susceptibility of low-Si Monel alloys was found to be relatively low. However, increases to Si concentration and the onset of associated eutectic reactions increased the solidification temperature range and drastically reduced cracking resistance. Increases in the Cu and Mn concentrations were found to reduce the solubility limit of Si in austenite which promoted additional eutectic formation and exacerbated the reductions in ductility and/or weldability.

36 MATERIALS SCIENCE↗

Computational modeling of grain boundary segregation: A review

Nearly all metals, alloys, ceramics, and their associated composites are polycrystalline in nature, with grain boundaries that separate well-defined crystalline regions that influence materials properties. In all but the most pure elemental systems, intentional solutes or impurities are present and can segregate to, or less commonly away from, the grain boundaries, in turn influencing boundary behavior, their stability, and associated materials properties. In some cases, grain-boundary segregation can also trigger “phase-like” structural transitions that dramatically alter the essential nature of the boundary. With the development of advanced electron microscopy techniques, researchers can directly observe grain-boundary structures and segregation with atomic precision. Despite such spatial resolution, the underlying mechanisms governing grain-boundary segregation remain difficult to characterize. As a result, computational modeling techniques such as density functional theory, molecular dynamics, mesoscale phase-field, continuum defect theory, and others are important complementary tools to experimental observations for studying grain-boundary segregation behavior. In conclusion, these computational methods offer the ability to explore the underlying formation mechanisms of grain-boundary segregation, elucidate complex segregation behavior, and provide insights into solutions to effectively controlling microstructure.

36 MATERIALS SCIENCE↗

Cluster dynamics modeling of Mn-Ni-Si precipitates coupled with radiation-induced segregation in low-Cu reactor pressure vessel steels

Formation of precipitates enhanced or induced by irradiation causes hardening and embrittlement of nuclear structural materials. Post-irradiation microstructure characterization of reactor pressure vessel (RPV) steels has shown that precipitation can be strongly associated with radiation-induced segregation (RIS) of solutes on dislocations. However, RIS and precipitation have not been coupled in previous precipitation modeling of RPV steels. Here in this study, a new hybrid and spatially-dependent precipitation model is developed that couples cluster dynamics with RIS, providing an unique way to account for concurrent evolution of heterogeneous cluster densities as well as solute and point defect concentration profiles. The model is applied to study the segregation of Mn, Ni, and Si on dislocations and heterogeneous nucleation of Mn-Ni-Si rich precipitates (MNSPs) in a low-Cu RPV steel. The result shows that the onset of MNSP nucleation on dislocations occurs at the fluence of 2 x 10 23 n.m -2 . The number density and mean radius can reach ~ 10 24 m -3 and 1-2 nm at high fluence, respectively. These observations suggest that the role of RIS and heterogeneous nucleation can be significant for RPV steels under a high fluence of irradiation. Results of simulations adopting various dose rates and dislocation densities show an increased fraction of MNSPs on dislocations at the condition of low dose rate, high dislocation density, and high fluence.

36 MATERIALS SCIENCE↗

Microstructural evolution and transmutation in tungsten under ion and neutron irradiation

This study aims to compare the effects of neutron and self-ion irradiation on the mechanical properties and microstructural evolution in W. Neutron irradiation at the HFR reactor to 1.67 dpa at 800 °C resulted in the formation of large Re and Os rich clusters and voids. The post-irradiation composition was measured using APT and verfified against FISPACT modelling. The measured Re and Os concentration was used to create alloys with equivalent concentrations of Re and Os. These alloys were exposed to self-ion irradiation to a peak dose of 1.7 dpa at 800 °C. APT showed that self-ion irradiation leads to the formation of small Os clusters, wheras under neutron irradiation large Re/Os clusters form. Voids are formed by both ion and neutron irradiation, but the voids formed by neutron irradiation are larger. By comparing the behaviour of W-1.4Re and W-1.4Re-0.1Os, suppression of Re cluster formation was observed. Irradiation hardening was measured using nanoindentation and was found to be 2.7 GPa, after neutron irradiation and 1.6 GPa and 0.6 GPa for the self-ion irradiated W-1.4Re and W-1.4Re-0.1Os. The higher hardening is attributed to the barrier strength of large voids and Re/Os clusters that are observed after neutron irradiation.

36 MATERIALS SCIENCE↗

Carbonylative Co- and Terpolymerizations of 10-Undecen-1-ol: A Route to Polyketoesters with Tunable Compositions

A strategy to synthesize branched polyketoesters from the carbonylative polymerization of bifunctional α,ω-alkenols such as 10-undecen-1-ol is presented. This strategy hinges on the competitive application of two related catalytic manifolds, alternating alkene/CO copolymerization, and alkene hydroesterification, which share a common metal acyl intermediate. Small molecule model studies of cationic Pd-catalyzed alkene carbonylation in the presence of alcohols demonstrate that the relative rates of ketone formation (through alternating alkene/CO insertion) and ester formation (through metal acyl alcoholysis) can be tuned across a wide range through judicious bis(phosphine) ligand design. Carbonylative polymerization of 10-undecen-1-ol with a (dppp(3,5-CF 3 ) 4 )Pd(OTs) 2 catalyst (dppp(3,5-CF 3 ) 4 = 1,3-bis[bis[3,5-bis(trifluoromethyl)phenyl]-phosphino]propane) led to the formation of high molecular weight polyketoesters with intermediate dispersity (M n > 20,000 g/mol, D- = 2.6) and a ketone/ester microstructure ratio of approximately 1:2. In these polymerization reactions, deploying electron-deficient bis(phosphines) to suppress deleterious alkene isomerization was the key to accessing the high molecular weight polymer. Further, terpolymerization reactions of 1-hexene/10-undecen-1-ol/CO or 1-fluoro-10-undecene/10-undecen-1-ol/CO by (dppp(3,5-CF 3 ) 4 )Pd(OTs) 2 were also successful. Furthermore, this proof of concept polymerization unlocks access to tunable polymer microstructures without extensive postpolymerization treatment.

10-undecen-1-ol↗

Processing, texture and mechanical properties of sintered silicon carbide

With regard to its favorable properties, in particular those shown at high temperatures, silicon carbide is of great interest for applications related to the construction of engines and turbines. Thus, silicon carbide could replace heat-resisting alloys with the objective to achieve a further increase in operational temperature. The present investigation is concerned with approaches which can provide silicon carbide material with suitable properties for the intended applications, taking into account the relations between characteristics of the raw material, material composition, sinter conditions, and results of the sintering process. The effects of density and texture formation on the mechanical properties are studied. It is found that a dense material with a fine-grained microstructure provides optimal mechanical properties, while any deviation from this ideal condition can lead to a considerable deterioration with respect to the material properties.

Landfermann, H.↗

The effects of ion implantation on the tribology of perfluoropolyether-lubricated 440C stainless steel couples

The lubricating lifetime of thin films of a perfluoropolyether (PFPE) based on hexafluoropropene oxide in the presence of ion implanted 440C stainless steel is presented. Stainless steel discs, either unimplanted or implanted with N2, C, Ti, Ti + N2, or Ti + C had a thin film of PFPE (60-400 A) applied to them reproducibly (+/- 20 percent) and uniformly (+/- 15 percent) using a device developed for this study. The lifetimes of these films were quantified by measuring the number of sliding-wear cycles required to induce an increase in the friction coefficient from an initial value characteristic of the lubricated wear couple to a final, or failure value, characteristic of an unlubricated, unimplanted couple. The tests were performed in a dry nitrogen atmosphere (less than 1 percent RH) at room temperature using a 3 N normal load with a relative sliding speed of 0.05 m/s. The lubricated lifetime of the 440C couple was increased by an order of magnitude by implanting the disc with Ti. Ranked from most to least effective, the implanted species were: Ti; Ti+C; unimplanted; N2; C approximately equals Ti+N2. The mechanism postulated to explain these results involves the formation of a passivating or reactive layer which inhibits or facilitates the production of active sites. The corresponding surface microstructures induced by ion implantation, obtained using x-ray diffraction and conversion electron Mossbauer spectroscopy, ranked from most to least effective in enhancing lubricant lifetime were: amorphous Fe-Cr-Ti; amorphous Fe-Cr-Ti-C + TiC; unimplanted; epsilon-(Fe,Cr)(sub x)N, x = 2 or 3; amorphous Fe-Cr-C approximately equals amorphous Fe-Cr-Ti-N.

Shogrin, Bradley↗

The Effects of Substrate Material and Thermal Processing Atmosphere on the Strength of PS304: A High Temperature Solid Lubricant Coating

PS304, a plasma spray deposited solid lubricant coating developed for high temperature sliding contacts was deposited on nine different substrate metals, heat treated at 650C in either air or argon and subsequently tested for strength using a commercially available pull-off adhesion test. Some samples were examined metallographically to help elucidate and explain the results. As deposited coatings exhibit pull-off strengths typically between 16 and 20 MPa with failure occuring (cohesively) within the coating. Heat treatment in argon at 650 C results in a slight increase in coating (cohesive) strength of about 30 percent to 21 to 27 MPa. Heat treatment in air at 650 C results in a dramatic increase in strength to over 30 MPa, exceeding the strength of the epoxy used in the pull test. Cross section metallographic analyses show that no microstructural coating changes occur following the argon heat treatments, however, exposure to air at 650C gives rise to the formation of a second chromium-rich phase precipitate within the PS304 NiCr constituent which provides a strengthening effect and a slight (approximately 5 percent) coating thickness increase. Subsequent heat treatments do not result in any further coating changes. Based upon these studies, PS304 is a suitable coating for use on a wide variety of high temperature substrates and must be heat treated following deposition to enhance strength and ensure dimensional stability.

DellaCorte, Christopher↗

Effect of hatch spacing and laser power on microstructure, texture, and thermomechanical properties of laser powder bed fusion (L-PBF) additively manufactured NiTi

This study systematically evaluates the effects of laser powder bed fusion additive manufacturing (L-PBF-AM) parameters (hatch spacing and laser power) on the thermomechanical behavior and microstructure of Ni 50.8 Ti 49.2 shape memory alloy. The samples were fabricated with hatch spacings from 40 to 240 µm and laser powers of 50 and 100 W at a constant scanning speed of 125 mm/s, resulting in parts with volumetric energy density levels from 55 to 666 J/mm 3 and two sets of linear energy densities of 0.4 and 0.8 J/mm. The results showed a reduced melt pool size and discontinuity of scan tracks with decreased laser power. Additionally, the porosity level was increased with larger hatch spacing and lower laser power. More notably, the transformation temperatures increased, and the critical stress, recoverable strain, and functional stability of samples improved with lower hatch spacing, where the recovery ratio of up to 90% was observed, regardless of the employed laser power. This study also discussed the relationship between the fabrication process and texture formation in the L-PBF-AM process. In conclusion, the advantage of L-PBF-AM was revealed in tailoring the microstructure from highly textured samples in [1 1 1] or [0 0 1] direction when hatch spacing lower than laser beam focused was employed, to the appearance of equiaxed solidification front with island grains and random orientations.

36 MATERIALS SCIENCE↗

Phase stability in cast and additively manufactured Al-rich Al-Cu-Ce alloys

Additively manufactured (AM) eutectic Al alloy systems have been studied extensively for advantageous thermal stability and mechanical properties due to their refined microstructures. Al-Cu-Ce alloys are one subset of these AM eutectic alloys. Here we studied phase stability in AM Al-Cu-Ce alloys and compared it to that of conventionally cast ones. A new phase, Al 8 Cu 3 Ce, was identified in the microstructures of both AM and cast Al-Cu-Ce alloys. This Al 8 Cu 3 Ce phase was not previously included on experimental or thermodynamically calculated phase diagrams of the Al-Cu-Ce system. Therefore, we performed additional thermodynamic modeling of the system. These models were experimentally validated with cast and subsequently heat-treated Al-Cu-Ce alloys. We found that despite the refined microstructure of the AM alloys, the phases formed were consistent with the cast alloys, suggesting that AM processing did not significantly alter the formation and stability of phases from that in the conventional alloys. In conclusion, this work has resolved inconsistent previous descriptions of the Al-Cu-Ce ternary phase diagram in the Al-rich region and resulted in the addition of the Al 8 Cu 3 Ce as an equilibrium phase above 500 °C.

36 MATERIALS SCIENCE↗

Thermoelectric Properties in the TiO2/SnO2 System

Nanotechnology has provided a new interest in thermoelectric technology. A thermodynamically driven process is one approach in achieving nanostructures in bulk materials. TiO2/SnO2 system exhibits a large spinodal region with exceptional stable phase separated microstructures up to 1400 C. Fabricated TiO2/SnO2 nanocomposites exhibit n-type behavior with Seebeck coefficients greater than -300 .V/K. Composites exhibit good thermal conductance in the range of 7 to 1 W/mK. Dopant additions have not achieved high electrical conductivity (<1000 S/m). Formation of oxygen deficient composites, TixSn1-xO2-y, can change the electrical conductivity by four orders of magnitude. Achieving higher thermoelectric ZT by oxygen deficiency is being explored. Seebeck coeffcient, thermal conductivity, electrical conductance and microstructure will be discussed in relation to composition and doping.

Dynys, F.↗