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All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

Specific corrosion product on interior surface of a bronze wine vessel with loop-handle and its growth mechanism, Shang Dynasty, China

In this paper, a kind of specific stalactitic product was found on the interior surface of a covered bronze wine vessel with loop-handle (Chinese name is you), which was fabricated in Shang Dynasty (1700 B.C.-1100 B.C.) and now is collected in Xiaogan Museum, Hubei province of China. The microstructures of the product were characterized systematically by using optical microscopy, scanning electron microscope, transmission electron microscope, X-ray diffraction, and Raman microscopy. The experimental results revealed that the product belonged to a kind of malachite with high purity and high crystallinity. The growth of the product was considered to be a possible reason that the vessel was overly airtight within a museum display cabinet besides a lid of the vessel, which made the excess of H{sub 2}O and CO{sub 2} gas concentrations inside the vessel during long-term storage. This corrosion product is very harmful to bronze cultural relics, because of a large amount of copper consumption from the matrix which will reduce its life. The growth mechanism of the specific stalactitic product and the suggestions for preservation of the similar bronze relics in museum were proposed. - Highlights: Black-Right-Pointing-Pointer The stalactitic product was the high purity and good crystallinity malachite. Black-Right-Pointing-Pointer Its growth was related to the excess of H{sub 2}O and CO{sub 2} gas concentrations in museum. Black-Right-Pointing-Pointer It is harmful to the bronzes, because copper will be consumed from the matrix. Black-Right-Pointing-Pointer The suggestions for preservation of the similar bronzes in museum were proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Study on Texture Evolution and Shear Behavior of an Al/Ni/Cu Composite

The microstructure, texture, and mechanical properties of the Al/Ni/Cu composite during various accumulative roll bonding (ARB) cycles were studied using optical microscopy, scanning electron microscopy, x-ray diffraction, shear punch test, and hardness test. In addition, ImageJ software and Rietveld software were used in order to study microstructure and dislocation density variations, respectively. It was found that Ni and Cu layers were fractured and distributed in the Al matrix due to differences in their mechanical properties. Fracture and distribution of Cu and Ni particles after cycle five led to the alteration of the composite structure from a layered to a particle-reinforced structure. ARB process leads to the formation of strong orientation along the β-fiber and also to pronounced copper and dillamore components in both Al and Cu phases. Furthermore, the shear yield stress and ultimate shear strength of the composite increased as the ARB process advanced; however, shear elongation presented a non-uniform variation. Investigation of the fracture surfaces revealed that the mechanical properties of the composite are affected not only by the strain hardening of the Cu layer, but also by the structural change in the composite during the initial ARB cycles. During the last stages of the process, however, changes in mechanical properties were mostly governed by reinforcement particles serving as strain concentration zones and the strain hardening of the Al matrix.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effect of long-term aging on microstructure and local behavior in the heat-affected zone of a Ni–Cr–Mo–V steel welded joint

Evolution of microstructure, micro-hardness and micro-tensile strength behavior was investigated in the heat-affected zone of a Ni–Cr–Mo–V steel welded joint after the artificial aging at 350 °C for 3000 h. After detailed characterization of microstructures in optical microscopy, scanning electron microscopy and transmission electron microscopy, it is revealed that the change of martensite–bainite constituent promotes more homogeneous microstructure distribution. The aging treatment facilitates redistribution of carbon and chromium elements along the welded joint, and the micro-hardness is increased slightly through the welds due to enrichment of carbon. The types of precipitates in the weldment mainly include M{sub 3}C, MC, M{sub 2}C and M{sub 23}C{sub 6}. The carbides in base metal, weld metal and coarse-grained heat-affected zone are prone to change from ellipsoidal to platelet form whereas more uniform spherical carbides are observed in the fine-grained zone. Precipitation and coarsening of M{sub 23}C{sub 6} near the fusion line, and formation of MC and M{sub 2}C, are responsible for the tensile strength decrease and its smooth distribution in the aged heat-affected zone. This implies that the thermal aging can relieve strength mismatch in the weldments. - Highlights: • Microstructure homogeneity improved in HAZ after long-term aging. • Tensile strength decreased in HAZ due to precipitation and coarsening of M{sub 23}C{sub 6}. • Strength mismatch in NiCrMoV steel welds was relieved after aging at 350 °C × 3000 h.

36 MATERIALS SCIENCE↗
DOE OSTI2014

The microstructure and mechanical behaviors of the Ti–6.5Al–3.5Mo–1.5Zr–0.3Si alloy produced by laser melting deposition

The microstructure and mechanical properties of the Ti–6.5Al–3.5Mo–1.5Zr–0.3Si alloy produced by laser melting deposition have been investigated. The columnar grains of the Ti–6.5Al–3.5Mo–1.5Zr–0.3Si alloy due to the layer-by-layer epitaxial growth from the underlying template grains during laser melting deposition, which is roughly parallel to the deposition direction, had been found by optical microscopy; strong [101{sup ¯}2]{sub α} crystallographic texture has been confirmed by X-ray diffraction and electron backscattered diffraction. Depending on the last heating history, the microstructure of the alloy undergoes a continued change opposite to the deposition direction: martensitic α′ (transformed β); coarsened primary α laths with transformed β; coarsened primary α laths; and the fine basketweave microstructure with a few coarsened α laths or annealed martensitic α′. The average Vickers micro-hardness value of the alloy is 364 HV. The alloy parallel to the deposition direction presents lower tensile strength (925 MPa) and better elongation (18.8%), compared with 1025 MPa and 8.2% of that vertical to the deposition direction, which has been discussed using its microstructure characterization. - Highlights: • The columnar grains and strong [101{sup ¯}2]{sub α} crystallographic texture of the Ti–6.5Al–3.5Mo–1.5Zr–0.3Si alloy due to the epitaxial growth from the underlying template grains • The microstructure evolution of the alloy depends on the last heating history. • The specimen parallel to the deposition direction presents lower ultimate tensile strength and higher elongation than the specimen vertical to the deposition direction.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Nanostructured self-assembly materials from neat and aqueous solutions of C18 lipid pro-drug analogues of Capecitabine—a chemotherapy agent. Focus on nanoparticulate cubosomes™ of the oleyl analogue

A series of prodrug analogues based on the established chemotherapy agent, 5-fluorouracil, have been prepared and characterized. C18 alkyl and alkenyl chains with increasing degree of unsaturation were attached to the N 4 position of the 5-fluorocytosine (5-FC) base via a carbamate bond. Physicochemical characterization of the prodrug analogues was carried out using a combination of differential scanning calorimetry, cross-polarized optical microscopy, X-ray diffraction and small-angle X-ray scattering. The presence of a monounsaturated oleyl chain was found to promote lyotropic liquid crystalline phase formation in excess water with a fluid lamellar phase observed at room temperature and one or more bicontinuous cubic phases at 37 °C. The bulk phase was successfully dispersed into liposomes or cubosomes at room and physiological temperature respectively. In vitro toxicity of the nanoparticulate 5-FCOle dispersions was evaluated against several normal and cancer cell types over a 48 h period and exhibited an IC 50 of -100 μM against all cell types. The in vivo efficacy of 5-FCOle cubosomes was assessed against the highly aggressive mouse 4T1 breast cancer model and compared to Capecitabine (a water-soluble commercially available 5-FU prodrug) delivered at the same dosages. After 21 days of treatment, the 0.5 mmol 5-FCOle treatment group exhibited a significantly smaller average tumour volume than all other treatment groups including Capecitabine at similar dosage. These results exemplify the potential of self-assembled amphiphile prodrugs for delivery of bioactives in vivo.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2013

Characterization of 430L porous supports obtained by powder extrusion moulding for their application in solid oxide fuel cells

The characterization of 430L stainless steel planar porous supports obtained by powder extrusion moulding was performed in this work. A thermoplastic multicomponent binder based on high density polyethylene and paraffin wax was selected for the process. Green supports were shaped by extrusion moulding, and subsequently the binder was removed by a thermal cycle previously optimized. Sintering was carried out at different temperatures in low vacuum. Density of sintered parts was measured by Archimedes' method and porosity was also evaluated through a microstructural analysis by optical microscopy. The porosity degree of samples sintered at low temperature was close to 35% which is a very suitable value for their application in SOFCs. Tensile tests were carried out in order to determine mechanical strength as a function of porosity degree. Based on these results, the best feedstock composition and processing parameters were selected. The oxidation behaviour in static air at high temperature was studied, and formed oxides were characterized in a scanning electron microscope equipped with energy dispersive analysis of X-rays. X-ray diffraction experiments were performed in order to identify the formed oxides based on formula Fe{sub 2−x}Cr{sub x}O{sub 3}. The results of these studies showed that this kind of ferritic stainless steel would be more suitable to be used as anodic supports where a rich hydrogen atmosphere is employed. Preliminary deposition tests allowed obtaining a homogeneous Ni–YSZ anode layer with a thickness of 10 μm on the porous metallic substrates. - Highlights: • 430L stainless steel porous supports were obtained by powder extrusion moulding. • Porosity degree was controlled sintering at different temperatures in low vacuum. • Tensile tests allowed determining mechanical strength of porous supports. • A study about its oxidation behaviour in static air at high temperature was realized. • After oxidation, formed oxides were characterized by EDS–SEM and XRD.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Compatibility of molten plutonium with wrought and additively manufactured metal crucibles

Understanding plutonium’s interaction with metals is crucial for optimizing pyrochemical operations, nuclear fuel containment, and various actinide processing techniques. Traditionally, tantalum crucibles are employed for plutonium processing due to their high durability, excellent temperature stability, and low solubility in plutonium. However, tantalum faces challenges such as plutonium wetting and diffusion, making surface coatings particularly important for crucibles in pyrochemical applications to enhance corrosion resistance against plutonium. Tantalum is also expensive and difficult to machine, prompting the need for advanced manufacturing techniques to address these challenges. Here, in this work, we investigate the interaction of Pu with tantalum and titanium crucibles fabricated using both traditional machining methods and laser powder bed fusion (LPBF) additive manufacturing (AM). LPBF-AM is an advanced technique that allows for the creation of complex geometries from traditionally difficult-to-machine metals by using a high-powered laser to build parts. Previous studies of conventional manufactured tantalum have utilized oxidation and carburization of the surface to mitigate plutonium wetting; however, no studies of surface modified LPBF-AM material have been undertaken. These studies are crucial, given the typical differences in the grain structure between conventional and LPBF-AM materials. All crucibles underwent differential scanning calorimetry to confirm the melting of plutonium. Subsequently, the crucibles were sectioned and mounted in epoxy for microstructural analysis using optical microscopy and scanning electron microscopy. This investigation, comparing the performance of wrought vs AM metal crucibles, provides a basis for future tooling applications in actinide processing techniques and can address the challenges associated with traditional machining, particularly in pyrochemical applications.

Actinides↗
DOE OSTI2017

Effect of CeLa addition on the microstructures and mechanical properties of Al-Cu-Mn-Mg-Fe alloy

Development of high strength lithium battery shell alloy is highly desired for new energy automobile industry. The microstructures and mechanical properties of Al-Cu-Mn-Mg-Fe alloy with different CeLa additions were investigated through optical microscopy (OM), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Rietveld refinement and tensile testing. Experimental results indicate that Al{sub 8}Cu{sub 4}Ce and Al{sub 6}Cu{sub 6}La phases formed due to CeLa addition. Addition of 0.25 wt.% CeLa could promote the formation of denser precipitation of Al{sub 20}Cu{sub 2}Mn{sub 3} and Al{sub 6}(Mn, Fe) phases, which improved the mechanical properties of the alloy at room temperature. However, up to 0.50 wt.% CeLa addition could promote the formation of coarse Al{sub 8}Cu{sub 4}Ce phase, Al{sub 6}Cu{sub 6}La phase and Al{sub 6}(Mn, Fe) phase, which resulted in weakened mechanical properties. - Highlights: •Al-Cu-Mn-Mg-Fe alloys with different CeLa addition were fabricated through casting and rolling. •Al{sub 8}Cu{sub 4}Ce and Al{sub 6}Cu{sub 6}La phases formed after CeLa addition. •Addition of 0.25 wt.% CeLa promoted formation of denser precipitates of Al{sub 20}Cu{sub 2}Mn{sub 3} and Al{sub 6}(Mn, Fe). •Mechanical properties of the alloy was improved after 0.25 wt.% CeLa addition.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Effect of heat treatment on microstructure and interface of SiC particle reinforced 2124 Al matrix composite

The microstructure and interface between metal matrix and ceramic reinforcement of a composite play an important role in improving its properties. In the present investigation, the interface and intermetallic compound present in the samples were characterized to understand structural stability at an elevated temperature. Aluminum based 2124 alloy with 10 wt.% silicon carbide (SiC) particle reinforced composite was prepared through vortex method and the solid ingot was deformed by hot rolling for better particle distribution. Heat treatment of the composite was carried out at 575 °C with varying holding time from 1 to 48 h followed by water quenching. In this study, the microstructure and interface of the SiC particle reinforced Al based composites have been studied using optical microscopy, scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDS), electron probe micro-analyzer (EPMA) associated with wavelength dispersive spectroscopy (WDS) and transmission electron microscopy (TEM) to identify the precipitate and intermetallic phases that are formed during heat treatment. The SiC particles are uniformly distributed in the aluminum matrix. The microstructure analyses of Al–SiC composite after heat treatment reveal that a wide range of dispersed phases are formed at grain boundary and surrounding the SiC particles. The energy dispersive X-ray spectroscopy and wavelength dispersive spectroscopy analyses confirm that finely dispersed phases are CuAl{sub 2} and CuMgAl{sub 2} intermetallic and large spherical phases are Fe{sub 2}SiAl{sub 8} or Al{sub 15}(Fe,Mn){sub 3}Si. It is also observed that a continuous layer enriched with Cu and Mg of thickness 50–80 nm is formed at the interface in between Al and SiC particles. EDS analysis also confirms that Cu and Mg are segregated at the interface of the composite while no carbide is identified at the interface. - Highlights: • The composite was successfully heat treated at 575°C for 1-48 hrs. • A layer of 50-75 nm is formed at interface after heat treatment. • No Carbide formation and SiC dissolution is observed at this temperature. • MgAl{sub 2}O{sub 4}, CuMgAl{sub 2} phases are segregated at interface of Al-SiC composite. • Mg and Cu are also segregated at near to the grain boundary.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Solid Collection Efforts: Ta Collimator Evaluation

Ta collimator sets that were part of the gated x-ray detector diagnostic (GXD) at NIF were analyzed for debris distribution and damage in 2011. These disks (ranging in thickness from 250 to 750 {mu}m) were fielded approximately 10 cm from target chamber center (TCC) on various symcap, THD and re-emit shots. The nose cone holder and forward Ta collimator (facing target chamber center, TCC) from all shots show evidence of surface melt. Non-destructive analysis techniques such as optical microscopy, surface profilometry, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and x-ray fluorescence (XRF) were used to determine debris composition and degree of deformation associated with each Ta disk. Molten debris from the stainless steel nose cone contaminated the surface of the collimators along with other debris associated with the target assembly (Al, Si, Cu, Au and In). Surface elemental analysis of the forward collimator Ta disks indicates that Au hohlraum debris is less concentrated on these samples versus those fielded 50 cm from TCC in the wedge range filter (WRF) assembly. It is possible that the Au is distributed below or within the stainless steel melt layer covering the disk, as most of the foreign debris is captured in the melted coating. The other disks (fielded directly behind the forward collimator in a sandwiched configuration) have visible forms of deformation and warping. The degree of warping increases as the shock wave penetrates the assembly with the most damage sustained on the back collimator. In terms of developing a solid collection capability, the collimator analyses suggests that close proximity may cause more interference with capsule debris collection and more damage to the surface of the collector diagnostic. The analyses of the Ta collimators were presented to the Target and Laser Interaction Sphere (TaLIS) group; a representative presentation is attached to this document.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Microstructural characterization and mechanical property of active soldering anodized 6061 Al alloy using Sn-3.5Ag-xTi active solders

Active solders Sn-3.5Ag-xTi varied from x = 0 to 6 wt.% Ti addition were prepared by vacuum arc re-melting and the resultant phase formation and variation of microstructure with titanium concentration were analyzed using X-ray diffraction, optical microscopy and scanning electron microscopy. The Sn-3.5Ag-xTi active solders are used as metallic filler to join with anodized 6061 Al alloy for potential applications of providing a higher heat conduction path. Their joints and mechanical properties were characterized and evaluated in terms of titanium content. The mechanical property of joints was measured by shear testing. The joint strength was very dependent on the titanium content. Solder with a 0.5 wt.% Ti addition can successfully wet and bond to the anodized aluminum oxide layers of Al alloy and posses a shear strength of 16.28 {+-} 0.64 MPa. The maximum bonding strength reached 22.24 {+-} 0.70 MPa at a 3 wt.% Ti addition. Interfacial reaction phase and chemical composition were identified by a transmission electron microscope with energy dispersive spectrometer. Results showed that the Ti element reacts with anodized aluminum oxide to form Al{sub 3}Ti-rich and Al{sub 3}Ti phases at the joint interfaces. - Highlights: Black-Right-Pointing-Pointer Active solder joining of anodized Al alloy needs 0.5 wt.% Ti addition for Sn-3.5Ag. Black-Right-Pointing-Pointer The maximum bonding strength occurs at 3 wt.% Ti addition. Black-Right-Pointing-Pointer The Ti reacts with anodized Al oxide to form Al{sub 3}Ti-rich and Al{sub 3}Ti at joint interface.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Effect of a copper filler metal on the microstructure and mechanical properties of electron beam welded titanium-stainless steel joint

Cracking in an electron beam weld of titanium to stainless steel occurred during the cooling process because of internal thermal stress. Using a copper filler metal, a crack free joint was obtained, which had a tensile strength of 310 MPa. To determine the reasons for cracking in the Ti/Fe joint and the function of the copper filler metal on the improvement of the cracking resistance of the Ti/Cu/Fe joint, the microstructures of the joints were studied by optical microscopy, scanning electron microscopy and X-ray diffraction. The cracking susceptibilities of the joints were evaluated with microhardness tests on the cross-sections. In addition, microindentation tests were used to compare the brittleness of the intermetallics in the welds. The results showed that the Ti/Fe joint was characterized by continuously distributed brittle intermetallics such as TiFe and TiFe(Cr){sub 2} with high hardness ({approx} 1200 HV). For the Ti/Cu/Fe joint, most of the weld consisted of a soft solid solution of copper with dispersed TiFe intermetallics. The transition region between the weld and the titanium alloy was made up of a relatively soft Ti-Cu intermetallic layer with a lower hardness ({approx} 500 HV). The formation of soft phases reduced the cracking susceptibility of the joint. - Highlights: Black-Right-Pointing-Pointer Electron beam welded Ti/Fe joint cracked for the brittleness and residual stress. Black-Right-Pointing-Pointer Electron beam welded Ti/Cu/Fe joint with tensile strength of 310 MPa was obtained. Black-Right-Pointing-Pointer Cu diluted Ti and Fe contents in weld and separated the TiFe{sub 2} into individual blocks. Black-Right-Pointing-Pointer Interfacial hard Ti-Fe compounds were replaced by soft Ti-Cu compounds in the weld. Black-Right-Pointing-Pointer A large amount of solid solution of copper formed in the weld.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructural Characterization of Irradiated U{sub 0.17}ZrH{sub 1.6} Using Ultrasonic Techniques

In recent years, there has been an increased level of effort to understand the changes in microstructure that occur due to irradiation of nuclear fuel. The primary driver for this increased effort is the potential for designing new fuels that are safer and more reliable, in turn enabling new and improved reactor technologies. Much of the data on microstructural change in irradiated fuels is generated through a host of post irradiation examination techniques such as optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) to determine grain structure, porosity, crack geometry, etc. in irradiated fuels. Such 'traditional' examination techniques were recently used to characterize a novel new fuel consisting of U{sub 0.17}ZrH{sub 1.6} pellets bonded to zircaloy-2 cladded with lead-bismuth eutectic before and after irradiation. In addition to the conventional suite of post-irradiation examination tools, several nondestructive interrogation techniques exist which bring the potential for in-situ assessment of microstructural changes. One such method, ultrasonic examination, was tested on each of the samples. This paper describes the results of this examination. Ultrasonic measurements have a long and successful history of use for nondestructive materials characterization, including nondestructive evaluation (NDE) of degradation and damage, microstructure characterization, and measurement of physical parameters for process control. Ultrasonic NDE is critical to the nuclear power industry's in-service inspection program for maintaining pressure boundary integrity, and is being actively investigated for PIE of fuels. Ultrasonic measurements, typically performed at 10 MHz or higher, performed post irradiation show that fuel microstructural parameters, such as porosity and grain size, can be correlated to ultrasonic velocity. The objective of this examination was to assess the feasibility of using ultrasonic measurements on irradiated fuel to determine sensitivity to microstructural changes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Well-aligned polycrystalline lanthanum silicate oxyapatite grown by reactive diffusion between solid La{sub 2}SiO{sub 5} and gases [SiO+1/2O{sub 2}]

The c-axis-oriented polycrystalline lanthanum silicate oxyapatite, La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} (□ denotes a vacancy in the Si site), was successfully prepared by the reactive diffusion between randomly grain-oriented La{sub 2}SiO{sub 5} polycrystal and [SiO+1/2O{sub 2}] gases at 1873 K in Ar atmosphere. The polycrystal was characterized using optical microscopy, scanning electron microscopy equipped with energy dispersive X-ray spectroscopy, micro-Raman spectroscopy, X-ray diffractometry, and impedance spectroscopy. The crystal structure (space group P6{sub 3}/m) showed the deficiency of Si site at ca. 1.9%. The bulk oxide-ion conductivity along the grain-alignment direction steadily increased from 9.2 × 10{sup −3} to 1.17 × 10{sup −2} S/cm with increasing temperature from 923 to 1073 K. The activation energy of conduction was 0.23(2) eV. - Graphical abstract: We have successfully prepared the highly c-axis-oriented polycrystalline La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} by the reactive diffusion between randomly grain-oriented La{sub 2}SiO{sub 5} polycrystal and [SiO + 1/2O{sub 2}] gases at 1873 K in Ar atmosphere. The crystal structure (space group P6{sub 3}/m) showed the deficiency of Si site of ca. 1.9%. - Highlights: • The c-axis-oriented polycrystalline La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} is successfully prepared. • Crystal structure of La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} is determined by single-crystal XRD. • The polycrystal shows relatively high oxide ion conductivity along the common c-axis. • Reactive diffusion is successfully used for the preparation of grain-aligned ceramics.

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

Dielectric strength of parylene HT

The dielectric strength of parylene HT (PA-HT) films was studied at room temperature in a wide thickness range from 500 nm to 50 μm and was correlated with nano- and microstructure analyses. X-ray diffraction and polarized optical microscopy have revealed an enhancement of crystallization and spherulites development, respectively, with increasing the material thickness (d). Moreover, a critical thickness d{sub C} (between 5 and 10 μm) is identified corresponding to the beginning of spherulite developments in the films. Two distinct behaviors of the dielectric strength (F{sub B}) appear in the thickness range. For d ≥ d{sub C}, PA-HT films exhibit a decrease in the breakdown field following a negative slope (F{sub B} ∼ d{sup −0.4}), while for d < d{sub C}, it increases with increasing the thickness (F{sub B} ∼ d{sup 0.3}). An optimal thickness d{sub optim} ∼ 5 μm corresponding to a maximum dielectric strength (F{sub B} ∼ 10 MV/cm) is obtained. A model of spherulite development in PA-HT films with increasing the thickness is proposed. The decrease in F{sub B} above d{sub C} is explained by the spherulites development, whereas its increase below d{sub C} is induced by the crystallites growth. An annealing of the material shows both an enhancement of F{sub B} and an increase of the crystallites and spherulites dimensions, whatever the thickness. The breakdown field becomes thickness-independent below d{sub C} showing a strong influence of the nano-scale structural parameters. On the contrary, both nano- and micro-scale structural parameters appear as influent on F{sub B} for d ≥ d{sub C}.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2012

Effect of cooling rate on the microstructure and microhardness of the CuZrAgAl alloy

The effect of cooling rate on the microstructure and microhardness of the Cu{sub 40}Zr{sub 44}Ag{sub 8}Al{sub 8} (at.%) alloy has been studied. The crystalline phases were characterized by X-ray diffraction, optical microscopy and scanning electron microscopy with energy dispersive X-ray spectroscopy, and identified as AlCu{sub 2}Zr, Cu{sub 10}Zr{sub 7} and CuZr{sub 2}. The solidification sequence was established as following: the Cu{sub 10}Zr{sub 7} phase forms first in the periphery of the rod, then following with AlCu{sub 2}Zr phase in the rod center and finally CuZr{sub 2} crystals in Cu-depleted areas. The effect of crystals on the mechanical properties of the Cu{sub 40}Zr{sub 44}Ag{sub 8}Al{sub 8} alloy was also estimated through the microhardness. According to the value of microhardness, inhomogeneous structure of the amorphous matrix is more easily formed for the alloy in the low cooling rate (i.e., 9 mm) as compared with the alloy with fully amorphous state in the large cooling rate (i.e., 3 mm). This inhomogeneous structure was attributed to the composition change of amorphous matrix arising from the forming of crystalline phases due to the low cooling rate. - Highlights: Black-Right-Pointing-Pointer The crystalline phases in the Cu{sub 40}Zr{sub 44}Ag{sub 8}Al{sub 8} alloy were identified. Black-Right-Pointing-Pointer The solidification sequence of Cu{sub 40}Zr{sub 44}Ag{sub 8}Al{sub 8} alloy was verified. Black-Right-Pointing-Pointer The softening and hardening of alloy could be observed due to the crystallization.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Nb Content on Microstructures and Mechanical Properties of Ti-xNb-2Fe Alloys

β-Type Ti-Nb-based alloys exhibit satisfactory biocompatibility and low Young’s modulus for biomedical applications. The microstructure and mechanical properties of a series of Ti-(14, 16, 18, 20, 22, 24)Nb-2Fe alloys fabricated by arc melting were investigated by XRD, optical microscopy, and tensile tests. Both ω and α″ phases existed in the Ti-14Nb-2Fe alloy, while just a single β phase existed in the other alloys. Twinning is an important deformation mechanism that causes work hardening and twinning-induced plasticity. It was found in the Ti-(14, 16, 18, 20)Nb-2Fe alloys and not in the Ti-22Nb-2Fe alloy. The Ti-14Nb-2Fe alloy exhibited the highest tensile strength and the highest Young’s modulus owing to the existence of the ω phase. The tensile strength decreased gradually from 830 MPa (highest) for the Ti-14Nb-2Fe alloy to 540 MPa (lowest) for the Ti-24Nb-2Fe alloy with an increase in the Nb content. The Young’s modulus decreased from 90 GPa for the Ti-14Nb-2Fe alloy to 63 GPa for the Ti-22Nb-2Fe alloy and then increased to 71 GPa for the Ti-24Nb-2Fe alloy. Elongation shows the same trend as the Young’s modulus. The Ti-22Nb-2Fe alloy, with a low Young’s modulus of 63 GPa, tensile strength of 570 MPa, and 15% elongation, was found suitable for biomedical applications. The Ti-20Nb-2Fe alloy also exhibits a high tensile strength, a Young’s modulus ratio of 9.24 × 10{sup −3}, and 18% elongation and is thus considered another valuable Ti alloy for biomedical applications.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Characterization of microstructure and texture across dissimilar super duplex/austenitic stainless steel weldment joint by super duplex filler metal

In the present paper, microstructural changes across an as-welded dissimilar austenitic/duplex stainless steel couple welded by a super duplex stainless steel filler metal using gas tungsten arc welding process is characterized with optical microscopy and electron back-scattered diffraction techniques. Accordingly, variations of microstructure, texture, and grain boundary character distribution of base metals, heat affected zones, and weld metal were investigated. The results showed that the weld metal, which was composed of Widmanstätten austenite side-plates and allotriomorphic grain boundary austenite morphologies, had the weakest texture and was dominated by low angle boundaries. The welding process increased the ferrite content but decreased the texture intensity at the heat affected zone of the super duplex stainless steel base metal. In addition, through partial ferritization, it changed the morphology of elongated grains of the rolled microstructure to twinned partially transformed austenite plateaus scattered between ferrite textured colonies. However, the texture of the austenitic stainless steel heat affected zone was strengthened via encouraging recrystallization and formation of annealing twins. At both interfaces, an increase in the special character coincident site lattice boundaries of the primary phase as well as a strong texture with <100> orientation, mainly of Goss component, was observed. - Graphical abstract: Display Omitted - Highlights: • Weld metal showed local orientation at microscale but random texture at macroscale. • Intensification of <100> orientated grains was observed adjacent to the fusion lines. • The austenite texture was weaker than that of the ferrite in all duplex regions. • Welding caused twinned partially transformed austenites to form at SDSS HAZ. • At both interfaces, the ratio of special CSL boundaries of the primary phase increased.

36 MATERIALS SCIENCE↗