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At least 955 records · Page 53

Effect of build geometry on the β-grain structure and texture in additive manufacture of Ti-6Al-4V by selective electron beam melting

With titanium alloys, the solidification conditions in Additive Manufacturing (AM) frequently lead to coarse columnar β-grain structures. The effect of geometry on the variability in the grain structure and texture, seen in Ti-6Al-4V alloy components produced by Selective Electron Beam Melting (SEBM), has been investigated. Reconstruction of the primary β-phase, from α-phase EBSD data, has confirmed that in bulk sections where in-fill “hatching” is employed growth selection favours columnar grains aligned with an <001> {sub β} direction normal to the deposited powder layers; this results in a coarse β-grain structure with a strong < 001 > {sub β} fibre texture (up 8 x random) that can oscillate between a near random distribution around the fibre axis and cube reinforcement with build height. It is proposed that this behaviour is related to the highly elongated melt pool and the raster directions alternating between two orthogonal directions every layer, which on average favours grains with cube alignment. In contrast, the outline, or “contour”, pass produces a distinctly different grain structure and texture resulting in a skin layer on wall surfaces, where nucleation occurs off the surrounding powder and growth follows the curved surface of the melt pool. This structure becomes increasingly important in thin sections. Local heterogeneities have also been found within different section transitions, resulting from the growth of skin grain structures into thicker sections. Texture simulations have shown that the far weaker α-texture (∼ 3 x random), seen in the final product, arises from transformation on cooling occurring with a near random distribution of α-plates across the 12 variants possible from the Burgers relationship. - Highlights: • Distinctly different skin and bulk structures are produced by the contour and hatching passes. • Bulk sections contain coarse β-grains with a < 001 > fibre texture in the build direction. • This oscillates between a random distribution around the axis and cube reinforcement. • In the skin layer nucleation occurs off the surrounding powder bed and growth occurs inwards. • Simulations show that a weak α-texture results from a random distribution across habit variants.

36 MATERIALS SCIENCE↗

Microstructural analysis of martensite constituents in quenching and partitioning steels

A methodology to distinguish martensite formed in the first quench (M1) from martensite formed in the second quench (M2) of the Quenching and Partitioning process is presented, enabling the study of the structural characteristics of both microstructural constituents. Investigations show that M1 displays larger block size and less lattice imperfections than M2, differences that can be related to their respective carbon contents. - Highlights: • An approach to distinguish “old” from “new” martensite in Q and P steels is presented • Methodology allows separate characterization of microstructure and crystallography “Old” martensite has larger block size and more perfect lattice than the “new” one • The differences between the old and new martensite depend on their carbon contents.

36 MATERIALS SCIENCE↗

Microstructural characterization of aluminum alloys using Weck's reagent, part I: Applications

This paper focuses on the applications of a color etchant for aluminum alloys named Weck's reagent. The Al phase shows different colors from location to location after being etched by Weck's reagent. It is proved that Weck's reagent is very sensitive to the micro-segregations of Ti, Si and Mg in Al alloys so that characterization of the micro-segregations can be qualitatively realized which is usually done by electronic probe techniques. With the help of this characterization method, we are able to evaluate solid fractions for the semi-solid processed Al alloy with a better accuracy by excluding the Al grain growth during water quenching. To understand this reagent better, the color change during etching is investigated by applying different etching times at room temperature (25 °C). Among those results, 12 s shows the best color contrast after etching. Finally, we repeat the 12 second etching for four times through repeating a polishing–etching process. The result exhibits that Weck's reagent has a satisfying re-producibility with stable color and color distribution for the four times etching result. The second part of this study covers the coloring mechanism of Weck's reagent by characterizing the etched surface via various characterization methods. - Highlights: • The applications of Weck's reagent for Al alloys are introduced in detail. • Detailed relationship between micro-segregations in Al phase and the color difference revealed by Weck's reagent are studied. • Etching time has a strong influence on the color revealed by Weck's reagent. • Besides micro-segregation, grain boundaries can also be visualized by Weck's reagent, which was proved by EBSD analysis.

36 MATERIALS SCIENCE↗

Investigation on the formation mechanism of Ti-bearing non-metallic inclusions in Fe-Al-Ti-O-N alloy by inductive separation method

Formation mechanism of Ti-bearing non-metallic inclusions was studied by inductive separation method, and characterization method was selected according to the type of each inclusion. The Al + Ti oxide was heterogeneous consisting of Al{sub 2}O{sub 3} with Ti rich oxide layer. Compositional and size distribution was characterized by automated SEM observation and EDS analysis. It is formed as the reduction of Al{sub 2}O{sub 3} by Ti in molten alloy at 1873 K. The Al-Ti oxide was homogenous. It was liquid at 1873 K characterized by EBSD. The Al/Ti molar ratio of oxide was consistent with that in each alloy as analyzed by manual SEM/EDS analysis. Its formation mechanism is proposed to be the reaction among dissolved Ti, Al, and O in molten alloy at 1873 K. TiN precipitated during solidification. The fraction of TiN smaller than 1 μm was larger in alloy2 than that in alloy1 as analyzed by automated SEM/EDS analysis. It is resulted from larger supersaturation degree in alloy2 during solidification.

36 MATERIALS SCIENCE↗

Microstructure control to improve creep strength of alumina-forming austenitic heat-resistant steel by pre-strain

Highlights: • The effect of pre-strain on creep strength of AFA steel was studied. • The creep test was performed at 700°C and 200Mpa, and the aging test was carried out using box furnace at 700°C to simulate the microstructural evolution during creep. • Microstuctural evolution was observed by using SEM, EBSD, and TEM to investigate the relationship between creep strength and microstructure. - Abstract: At 700 °C and 200 MPa, the creep rupture time of W-containing alumina-forming austenitic heat-resistant (WAFA) steel increases from 1044 to 3119 h by pre-strain. Pre-strain introduces a lot of dislocation into the matrix and most of the dislocations remain stable to the end of creep without recovery and recrystallization. In addition, the dislocations have enabled secondary NbC and Laves phase to be uniformly distributed and refined. However, the dislocations lower grain boundary strength due to the coarsening of precipitates along grain boundaries Therefore, the increase in the creep rupture time in spite of deterioration of grain boundary strength is attributed to the dislocation strengthening and enhanced precipitation hardening within grains.

36 MATERIALS SCIENCE↗

Microstructure, texture and mechanical properties of 6061 aluminum laser beam welded joints

Highlights: • Strong cube texture ({001}<100>) is observed in columnar dendrites. • The ratio of equiaxed dendrites shows proportional relationship with the strength. • The relations between process-microstructure-property are accurately established. - Abstract: In the present study, laser beam welding was carried out with 6061 Al alloy plate to study the microstructural evolution under various welding heat input (ηP/v = 30 J/mm, 38 J/mm, 46 J/mm, and 58 J/mm). The width of the weld metals increased continuously with the heat input values. Quantitatively correlation of the microstructure distribution with welding parameters was developed based on the EBSD results. The weld metals mainly consisted of coarse columnar dendrites and equiaxed dendrites. The ratio of equiaxed dendrites which were controlled by constitutional supercooling and heterogeneous nuclei showed directly proportional relationship with the weld strength. Strong cube texture ({001}<100>) was observed in columnar dendrites, which showed harmful effect on the weld strength. Slight softening in heat affected zone due to recrystallization was identified by nanoindentation tests. All specimens failed in weld metal and the fracture surfaces showed the characteristics of ductile fracture.

36 MATERIALS SCIENCE↗

Microstructure evolution and a new mechanism of B2 phase on room temperature mechanical properties of Ti-47Al-2Cr-2Nb alloy prepared by hot isostatic pressing

Highlights: • The microstructure evolution of Ti-47Al-2Cr-2Nb alolly was investigated in detail. • The foramtion of B{sub 2} phase can be adjusted in Ti-47Al-2Cr-2Nb alloy. • A new mechanism of B{sub 2} phase on room temperature mechanical properties of Ti-47Al-2Cr-2Nb alloy was proposed. - Abstract: The formation of B{sub 2} phase was adjusted via various hot isostatic pressing processes in Ti-47Al-2Cr-2Nb alloy. The microstructure evolution and a new mechanism of B{sub 2} phase on room temperature mechanical properties was investigated by BSE, EBSD and TEM in detail. The result shows that the formation of B{sub 2} phase leads to Cr element content decrease in γ matrix phase, which results in lattice parameter increase, namely the c/a ratio of γ matrix phase. Finally, at room temperature the mechanical properties of Ti-47Al-2Cr-2Nb alloy deteriorates.

36 MATERIALS SCIENCE↗

Formation of intermetallic structures at the interface of steel-to-aluminium explosive welds

Highlights: • The interface of Fe-Al explosive welds was characterised by SEM/EDS and EBSD. • The intermetallics formed at the weld interface are rich in Al (Fe{sub 4}Al{sub 13}, Fe{sub 2}Al{sub 5}). • The presence of intermetallic phases on the interface deeply affects the weldability. • Al-rich intermetallics increase the solidification time of the weld interface. - Abstract: The formation of intermetallic structures at the interface of carbon steel to 6082 aluminium alloy explosive welds and their influence on the weldability of these two materials were studied. The morphology, the microstructure, the chemical and phase compositions of the welds were characterised by several types of microscopy techniques. The interface characterisation proved that explosive mixtures with a lower detonation velocity were revealed as being more suitable for achieving consistent welds since jet entrapment was prevented and continuous molten layers were not formed at the weld interface. It was also found that the physical properties of the intermetallic phases generated at the weld interface have a strong influence on the weldability of steel-to-aluminium explosive welds. Specifically, it was shown that the formation of aluminium-rich intermetallic phases at the weld interface increases the solidification time of the interfacial molten material, decreasing the weldability of these two materials. The formation of these intermetallic compounds should be avoided by reducing the interaction between the flyer and the baseplate as well as by avoiding excessive molten layers.

36 MATERIALS SCIENCE↗

Effect of microstructures on hot compression behavior of a Ti-43Al-2Si alloy fabricated by cold crucible continuous casting

Highlights: • TiAl alloys with different lamellar colonies were fabricated by cold crucible continuous casting. • EBSD was used to investigate the evolution of lamellae during the hot compression. • Lamellar colony boundaries promote the dynamic recrystallization process. - Abstract: To investigate the influence of lamellar orientation and colony boundary on deformation behavior, fully lamellar Ti-43Al-2Si alloys were prepared by cold crucible continuous casting and isothermal compression tests were conducted at different temperatures in the range 1373–1523 K with a strain rate of 0.01 s{sup −1}. The as-cast microstructures were elongated colony with lamellae oriented at nearly 45° to the compression direction and equiaxed colony with various lamellae orientations, respectively. The results revealed that serious cracking or sliding traces appeared on the surface of deformed specimens with elongated colony original microstructure and that their peak stresses were lower compared to those of specimens with equiaxed colony original microstructure. The relationship between deformation behaviors and as-cast microstructure was analyzed in detail. It was found that the recrystallization/globularization level is significantly lower than that in specimens with equiaxed colony original microstructure during hot deformation owing to the preferred nucleation sites in colony boundaries. Finally, the lamellae conversion process was characterized to reveal the softening mechanisms of full lamellar TiAl-based alloy during hot compression.

36 MATERIALS SCIENCE↗

Structural characterization of epitaxial CrxMo1-x alloy thin films

To develop a model system containing regularly-spaced misfit dislocations for studies of the radiation resistance of nanoscale defects, epitaxial thin films of Cr, Mo, and Cr{sub x}Mo{sub 1-x} alloys were deposited on MgO(001) by molecular beam epitaxy. Film compositions were chosen to vary the lattice mismatch with MgO. The film structure was investigated with x-ray diffraction (XRD), Rutherford backscattering spectrometry (RBS), and scanning transmission electron microscopy (STEM). Epitaxial films with reasonably high crystalline quality and abrupt interfaces were achieved at a relatively low deposition temperature, as confirmed by STEM. However, it was found by XRD and RBS in the channeling geometry that increasing the Mo content of the CrMo alloy films degraded the crystalline quality, despite the improved lattice match with MgO. XRD rocking curve data indicated that regions of different crystalline order may be present within the films with higher Mo content. This is tentatively ascribed to spinodal decomposition into Cr-rich and Mo-rich regions, as predicted by the Cr{sub x}Mo{sub 1-x} phase diagram.

36 MATERIALS SCIENCE↗

Characterization of bismuth nanospheres deposited by plasma focus device

A new method for producing thin layer of bismuth nanospheres based on the use of low energy plasma focus device is demonstrated. Various techniques such as scanning electron microscopy, Rutherford backscattering spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy have been used to characterize the morphology and the composition of the nanospheres. Experimental parameters may be adjusted to favour the formation of bismuth nanospheres instead of microspheres. Therefore, the formation of large surface of homogeneous layer of bismuth nanospheres with sizes of below 100 nm can be obtained. The natural snowball phenomenon is observed to be reproduced in nanoscale where spheres roll over the small nanospheres and grow up to bigger sizes that can reach micro dimensions. The comet-like structure, a reverse phenomenon to snowball is also observed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Materials and Electrical Characterization of Physical Vapor Deposited LaxLu1-xO3 Thin Films on 300 mm Silicon

La{sub x}Lu{sub 1-x}O{sub 3} thin films were deposited on 300 mm silicon wafers by physical vapor deposition and fabricated into field-effect transistors using a gate-first process flow. The films were characterized using transmission electron microscopy, Rutherford backscattering spectrometry, and synchrotron x-ray diffraction. The results show the films remain amorphous even at temperatures of 1000 C. The dielectric properties of La{sub x}Lu{sub 1-x}O{sub 3} (0.125 {<=} x {<=} 0.875) thin films were evaluated as a function of film composition. The amorphous La{sub x}Lu{sub 1-x}O{sub 3} thin films have a dielectric constant (K) of 23 across the composition range. The inversion thickness (T{sub inv}) of the La{sub x}Lu{sub 1-x}O{sub 3} thin films was scaled to <1.0 nm.

36 MATERIALS SCIENCE↗

HEAT TRANSFER ASPECTS OF TWO PISTON SPLAT QUENCHING

This thesis investigates the heat transfer aspects of the two-piston splat quench system by modifying surface roughness and by using copper and stainless steel platens. In additive manufacturing, specifically selective laser melting (SLM), metal is subjected to a very rapid heating and cooling that produces cooling rates in the range from 105-106 °C/s. This rapid solidification produces microstructures that deviate far from equilibrium. Splat quenching is an experimental method that produces rapidly solidified structures under cooling rates that are comparable to those found in additive manufacturing. The splat quenching approach allows for more efficient testing of the rapid solidification behavior of a wide variety of alloys. In this thesis, two platen characteristics, surface roughness and material thermal conductivity, were examined to determine their role in controlling the heat transfer and the subsequent cooling rate during splat quenching of austenitic stainless steel 316L. To that objective, 5 surface finishes were produced using metallographic techniques, from 7046-203 Å Rms. Copper and 316L stainless steel platen material were used to reach different levels of thermal conductance. The combination of these 2 variables created 10 scenarios, which were examined using, backscatter imaging, secondary imaging, and electron back scatter diffraction. Cooling rates were estimated using cell sizing obtained through electrolytic etching and secondary imaging. This thesis determined that both surface modification and changes in material type had a statistically significant impact on the cell sizes observed. Where material type far outweighed surface roughness in its effect on cell size.

Roze, Jonathan↗

Synthesis, Structure, and Spectroscopy of Epitaxial EuFeO 3 Thin Films

Rare earth iron perovskites RFeO3, where R is a rare earth cation, exhibit an array of magnetic, catalytic, optical, and electrochemical properties. Here we study EuFeO3 films synthesized by molecular beam epitaxy to improve our understanding of the optical properties of ferrites. A combination of X-ray diffraction, X-ray reflectivity, Rutherford backscattering spectroscopy, and scanning transmission electron microscopy was used to characterize the film structure and cation composition. X-ray absorption spectroscopy confirms the nominal 3+ valence states of Eu and Fe. The optical properties of EuFeO3 were investigated using variable-angle spectroscopic ellipsometry between the photon energies of 1.25 and 5 eV. We find that EuFeO3 is a semiconductor with an onset of optical absorption near 2.5 eV. The absorption spectrum of EuFeO3 is blue-shifted with respect to LaFeO3 films, a result that is attributed to the structural differences between the two materials.

Choquette, Amber K.↗

Radiation effects in nuclear materials: Role of nuclear and electronic energy losses and their synergy

Ceramic oxides and carbides are promising matrices for the immobilization and/or transmutation of nuclear wastes, cladding materials for gas-cooled fission reactors and structural components for fusion reactors. For these applications there is a need of fundamental data concerning the behavior of nuclear ceramics upon irradiation. This article is focused on the presentation of a few remarkable examples regarding ion-beam modifications of nuclear ceramics with an emphasis on the mechanisms leading to damage creation and phase transformations. Results obtained by combining advanced techniques (Rutherford backscattering spectrometry and channeling, X-ray diffraction, transmission electron microscopy, Raman spectroscopy) concern irradiations in a broad energy range (from keV to GeV) with the aim of exploring both nuclear collision (Sn) and electronic excitation (Se) regimes. Finally, the daunting challenge of the demonstration of the existence of synergistic effects between Sn and Se is tackled by discussing the healing due to intense electronic energy deposition (SHIBIEC) and by reporting results recently obtained in dual-beam irradiation (DBI) experiments.

Thomé, Lionel↗

Effect of high temperature deposition on CoSi{sub 2} phase formation

This paper discusses the nucleation behaviour of the CoSi to CoSi{sub 2} transformation from cobalt silicide thin films grown by deposition at elevated substrate temperatures ranging from 375 Degree-Sign C to 600 Degree-Sign C. A combination of channelling, real-time Rutherford backscattering spectrometry, real-time x-ray diffraction, and transmission electron microscopy was used to investigate the effect of the deposition temperature on the subsequent formation temperature of CoSi{sub 2}, its growth behaviour, and the epitaxial quality of the CoSi{sub 2} thus formed. The temperature at which deposition took place was observed to exert a significant and systematic influence on both the formation temperature of CoSi{sub 2} and its growth mechanism. CoSi films grown at the lowest temperatures were found to increase the CoSi{sub 2} nucleation temperature above that of CoSi{sub 2} grown by conventional solid phase reaction, whereas the higher deposition temperatures reduced the nucleation temperature significantly. In addition, a systematic change in growth mechanism of the subsequent CoSi{sub 2} growth occurs as a function of deposition temperature. First, the CoSi{sub 2} growth rate from films grown at the lower reactive deposition temperatures is substantially lower than that grown at higher reactive deposition temperatures, even though the onset of growth occurs at a higher temperature, Second, for deposition temperatures below 450 Degree-Sign C, the growth appears columnar, indicating nucleation controlled growth. Elevated deposition temperatures, on the other hand, render the CoSi{sub 2} formation process layer-by-layer which indicates enhanced nucleation of the CoSi{sub 2} and diffusion controlled growth. Our results further indicate that this observed trend is most likely related to stress and changes in microstructure introduced during reactive deposition of the CoSi film. The deposition temperature therefore provides a handle to tune the CoSi{sub 2} growth mechanism.

36 MATERIALS SCIENCE↗

Evaluation of microstructure anisotropy on room and medium temperature ECAP deformed F138 steel

The microstructure developed during severe plastic deformation results in improved mechanical properties because of the decrease in domain sizes and accumulation of defects, mainly dislocation arrays. The characteristic deformation stages observed in low stacking fault energy (SFE) face centered cubic (FCC) materials are highly influenced by the development of the primary and secondary twinning that compete with dislocation glide. In this paper, a low SFE F138 stainless steel is deformed by equal channel angular pressing (ECAP) up to 4 passes at room temperature (RT) and at 300 °C to compare the grain refinement and twin boundary development with increasing deformation. Tensile tests were performed to determine the deformation stages reached by the material before and after ECAP deformation, and the resulting microstructure was observed by TEM. X-ray diffraction and EBSD, average technique the first and local the second one, were used to quantify the microstructural changes, allowing the determination of diffraction domain sizes, dislocation and stacking fault densities and misorientation indices, which lead to a complete analysis of the deformation introduced in the material, with comparative correlations between various microstructural parameters. - Highlights: • The microstructure of ECAP pressed F138 steel was studied using TEM, EBSD and XRD. • Increasing deformation reduced domain sizes and increased dislocation densities. • Dislocation array compactness and misorientation increased with higher deformation. • Largest dislocation densities, mostly screw, match with simultaneous activation of twins. • Several correlations among microstructural features and parameters have been disclosed.

36 MATERIALS SCIENCE↗