Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Optical Microscopy”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 577 records · Page 32
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Formation of Al{sub 15}Mn{sub 3}Si{sub 2} Phase During Solidification of a Novel Al-12%Si-4%Cu-1.2%Mn Heat-Resistant Alloy and Its Thermal Stability

The formation of Al{sub 15}Mn{sub 3}Si{sub 2} phase in Al-12Si-4Cu-1.2Mn (wt.%) alloy during solidification was investigated by adopting CALPHAD method and microstructural observation by optical microscopy, SEM–EDS, TEM–EDS/SAD and XRD analysis; SEM fixed-point observation method was applied to evaluate its thermal stability. As-cast microstructural observation consistently demonstrates the solidification sequence of the studied alloy predicted by phase diagram calculation. Based on the phase diagram calculation, SEM–EDS, TEM–EDS/SAD and XRD analysis, as well as evidences on Al-Si-Mn-Fe compounds from the literature, the primary and eutectic Mn-rich phases with different morphologies in the studied alloy are identified to be Al{sub 15}Mn{sub 3}Si{sub 2} that has a body-centered cubic (BCC) structure with a lattice constant of a = 1.352 nm. SEM fixed-point observation and XRD analysis indicate that Al{sub 15}Mn{sub 3}Si{sub 2} phase has more excellent thermal stability at high temperature than that of CuAl{sub 2} phase and can serve as the major strengthening phase in heat-resistant aluminum alloy that has to face a high-temperature working environment. Results of tension test show that addition of Mn can improve the strength of Al-Si-Cu alloy, especially at elevated temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Biocompatibility of Hydrogen-Diluted Amorphous Silicon Carbide Thin Films for Artificial Heart Valve Coating

Amorphous silicon carbide (a-SiC:H) thin films were synthesized using trichloromethylsilane by a hot wire chemical vapor deposition process. The deposited films were characterized by Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, x-ray diffraction and x-ray photoelectron spectroscopy to confirm its chemical bonding, structural network and composition of the a-SiC:H films. The optical microscopy images reveal that hydrogen dilution increased the surface roughness and pore density of a-SiC:H thin film. The Raman spectroscopy and FTIR spectra reveal chemical network consisting of Si-Si, C-C and Si-C bonds, respectively. The XRD spectroscopy and Raman spectroscopy indicate a-SiC:H still has short-range order. In addition, in vitro cytotoxicity test ensures the behavior of cell–semiconductor hybrid to monitor the proper coordination. The live–dead assays and MTT assay reveal an increase in green nucleus cell, and cell viability is greater than 88%, respectively, showing non-toxic nature of prepared a-SiC:H film. Moreover, the result indicated by direct contact assay, and cell prefers to adhere and proliferate on a-SiC:H thin films having a positive effect as artificial heart valve coating material.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Improvement of Electropolishing of 1100 Al Alloy for Solar Thermal Applications

Aluminum sheets-based mirrors are finding applicability in high-temperature solar concentrating technologies because they are cost-effective, lightweight and have high mechanical properties. Nonetheless, the reflectance percentages obtained by electropolishing are not close to the reflectance values of the currently used evaporated films. Therefore, controlling key factors affecting electropolishing processes became essential in order to achieve highly reflective aluminum surfaces. This study investigated the effect of both the electropolishing process and previous heat treatment on the total reflectance of the AA 1100 aluminum alloy. An acid electrolyte and a modified Brytal process were evaluated. Total reflectance was measured by means of UV–Vis spectrophotometry. Reflectance values higher than 80% at 600 nm were achieved for both electrolytes. Optical microscopy and scanning electron microscopy images showed uneven dissolution for the acid electropolished samples causing a reflectance drop in the 200-450 nm region. The influence of heat treatment, previously to electropolishing, was tested at two different temperatures and various holding times. It was found that reflectance increases around 15% for the heat-treated and electropolished samples versus the non-heat-treated ones. A heat treatment at low temperature combined with a short holding time was enough to improve the sample total reflectance.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Properties of Rolled AZ31 Magnesium Alloy Sheet Fabricated by Continuous Variable Cross-Section Direct Extrusion

Rolling is currently a widely used method for manufacturing and processing high-performance magnesium alloy sheets and has received widespread attention in recent years. Here, we combined continuous variable cross-section direct extrusion (CVCDE) and rolling processes. The microstructure and mechanical properties of the resulting sheets rolled at different temperatures from CVCDE extrudate were investigated by optical microscopy, scanning electron microscope, transmission electron microscopy and electron backscatter diffraction. The results showed that a fine-grained microstructure was present with an average grain size of 3.62 μm in sheets rolled from CVCDE extrudate at 623 K. Dynamic recrystallization and a large strain were induced by the multi-pass rolling, which resulted in grain refinement. In the 573-673 K range, the yield strength, tensile strength and elongation initially increased and then declined as the CVCDE temperature increased. The above results provide an important scientific basis of processing, manufacturing and the active control on microstructure and property for high-performance magnesium alloy sheet.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Hot Rolling on the Microstructure and Mechanical Properties of Nitrogen Alloyed Austenitic Stainless Steel

In the present investigation, the effect of multi-pass hot rolling in the temperature range of 700–1000 °C on the microstructure and mechanical properties of nitrogen alloyed austenitic stainless steel was studied with the aid of optical microscopy, tensile testing and x-ray diffraction measurements. The microstructural changes that occurred in the hot rolled specimens were elongation of grains in rolling direction, nucleation of new grains at the grain boundaries of elongated grains and growth of nucleated grains to form fully recrystallized grains. Elongated grains formed at lower rolling temperature (700–800 °C) due to inadequate strain/temperature for the initiation of dynamic recrystallization. At higher rolling temperature (900–1000 °C), fine grains formed due to dynamic recrystallization. Tensile properties showed strong dependency on the rolling temperature. Tensile strength increased with the decrease in the rolling temperature at the cost of ductility. Maximum strength was observed in samples hot rolled at 700 °C with yield strength of 917 MPa and ductility of 25%. This variation in the tensile properties with the rolling temperature is attributed to changes in the dislocation density and grain structure. The estimated yield strength from the dislocation density, solid solution and grain boundary strengthening closely matched with experimentally determined yield strength confirming the role of dislocation density and grain size in the strengthening.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural Characteristics and Mechanical Properties of an Electron Beam-Welded Ti/Cu/Ni Joint

Electron beam welding experiments of TA15 titanium alloy to GH600 nickel superalloy with and without a copper sheet interlayer were carried out. Surface appearance, microstructure and phase constitution of the joint were examined by optical microscopy, scanning electron microscopy and x-ray diffraction analysis. Mechanical properties of Ti/Ni and Ti/Cu/Ni joint were evaluated based on tensile strength and microhardness tests. The results showed that cracking occurred in Ti/Ni electron beam weldment for the formation of brittle Ni-Ti intermetallics, while a crack-free electron beam-welded Ti/Ni joint can be obtained by using a copper sheet as filler metal. The addition of copper into the weld affected the welding metallurgical process of the electron beam-welded Ti/Ni joint significantly and was helpful for restraining the formation of Ti-Ni intermetallics in Ti/Ni joint. The microstructure of the weld was mainly characterized by a copper-based solid solution and Ti-Cu interfacial intermetallic compounds. Ti-Ni intermetallic compounds were almost entirely suppressed. The hardness of the weld zone was significantly lower than that of Ti/Ni joint, and the tensile strength of the joint can be up to 282 MPa.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Multiphase Microstructure in a Metastability-Assisted Medium Carbon Alloy Steel

A medium carbon alloy steel is processed by austenizing at 900 °C for 30 min, then rapid quenching into a patented quenching liquid and holding at 170 °C for 5 min, finally isothermally holding at 250 °C for different times. The morphology and mechanical properties are performed by using optical microscopy and scanning electron microscopy. A multiphase microstructure characterized by a mixture of lenticular prior martensite (PM), fine needle bainitic ferrite and filmy retained austenite (RA) is obtained. It is found that the PM formed firstly upon quenching can accelerate the subsequent bainitic transformation and promote refinement of multiphase colonies. The results show that an optimum mechanical property of a 4000.9 MPa bending strength and a 2030 MPa tensile strength is achieved at 250 °C for 120 min, which is attributed to the multiphase microstructural characteristics and a high product of the volume fraction of RA and the carbon content of austenite.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural Investigation of VPPA–GMAW Welded 7A52 Aluminum Alloys

In this study, the microstructural features of 7A52 heat-treatable aluminum alloys welded by variable polarity plasma arc (VPPA) combined with gas metal arc welding (GMAW) (VPPA–GMAW) were investigated and compared with those of 7A52 aluminum alloys welded by GMAW. The grain structures and modification of the precipitates were analyzed by optical microscopy and transmission electron microscopy. Complementary to modification of the precipitates, the precipitation evolution in the heat-affected zone and magnesium loss in the fusion zone were measured by differential scanning calorimetry and inductively coupled plasma spectroscopy. In VPPA–GMAW, the weld only needs one pass by depositing on one side of the 10-mm-thick aluminum alloy plates because of the large penetration capability of VPPA and good fluidity of the molten metal in the weld pool. Accordingly, the effect of excessive heat input on the microstructure can be minimized. The results show that the grain growth is not obvious and the magnesium loss is small in the fusion zone of VPPA–GMAW compared with that of GMAW under the condition of equal heat input to the workpiece. Small precipitates inside the grains remain homogeneously distributed, and a large volume fraction of the η′ phase exists. The VPPA–GMAW weld exhibits less tendency to soften; thus, VPPA–GMAW is appropriate for welding thick-plate aluminum alloys with a high production rate.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Fabrication of Ta-Reinforced Cu-Based Bulk Metallic Glass Composites by High-Pressure Torsion

Ex situ Cu{sub 54}Zr{sub 22}Ti{sub 18}Ni{sub 6} matrix bulk metallic glass composites (BMGCs) reinforced with Ta particles (10–30 vol.%) were fabricated by high-pressure torsion (HPT) under applied pressure of 6 GPa for 1–3 turns at temperatures of 25 or 200 °C. The densification, structure, thermal, and mechanical properties of BMGC samples were investigated by Archimedes densitometry, optical microscopy, x-ray diffraction, differential scanning calorimetry, small punch test, and microhardness measurements. Near full-density BMGC disks (relative densities higher than 0.97) are fabricated using HPT, irrespective of the processing strain and temperature. The microhardness of BMGCs is improved by increasing the number of turns, or the processing temperature due to the improvement in the deformation degree of both the amorphous and Ta particles as well as the reduction in the interlayer spacing of Ta particles. Nevertheless, there is an optimal amount of Ta which gives rise to the peak hardness in the BMGC samples, depending on the amount of imposed strain during HPT. The results of small punch test indicate that the addition of Ta to the monolithic BMG and increasing the HPT temperature significantly enhance the fracture load and deflection.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Neutron Diffraction Residual Stress Study of a AA2219-T87 Self-Reacting Friction Stir Weld

2219-T87 is a precipitation hardenable aluminum-copper alloy which sees wide use in structural aerospace components. Thick panels of this alloy are joined via self-reacting friction welding (SRFSW); however, this thermomechanical process can result in significant loss of the alloy’s strengthening precipitates and large residual stresses which are detrimental to mechanical behavior and performance. High-resolution maps of the residual strain and stress states along the normal, transverse, and longitudinal directions of 2219-T87 SRFSW were obtained using neutron diffraction measurements. Residual stress had the highest tensile value in the heat-affected zone (HAZ) and the largest compressive stress in the base metal region of the normal and transverse directions. Line profile residual stress distributions displayed an “M”-shaped distribution in each direction with the longitudinal direction being the most pronounced while 2D residual stresses displayed an hourglass-shaped pattern. Further, average maximal longitudinal residual stress values ranged from 60.6 to 85.6% of yield. Microhardness testing across the transverse weld section produced a “V”-shaped curve with slight hardness recovery in the stir zone. Maximal and minimal microhardness values were observed in the base metal (154 HV) and thermomechanically affected zone (82 HV), respectively. Microstructural evolution was recorded using optical microscopy and showed decreasing grain size from the HAZ to the stir zone.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Texture Evolution During Laser Direct Metal Deposition of Ti-6Al-4V

Titanium alloys are used in a wide variety of high performance applications and hence the processing of the titanium and the resulting microstructures after additive manufacturing has received significant attention. During additive manufacturing the processing route involves the transition from a liquid to solid state. The addition of successive layers results in a complex microstructure due to solid-state transformations. The current study focuses on understanding the phase transformations and relate it to the transformation texture in Ti-6Al-4V to identify conditions leading to a strong alpha transformation texture. The as deposited builds were characterized using optical microscopy and electron backscattered diffraction. The results showed columnar prior β grains with a martensitic structure after the deposition of a single layer. On subsequent depositions the martensitic microstructure decomposes to a colony and basketweave microstructure with a stronger transformation texture. The alpha texture with a colony and basketweave microstructure shows a stronger transformation texture as a result of variant selection. Thus by controlling the cooling rate of the build from the β transus it is possible to control the alpha transformation texture.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure and mechanical properties of pure copper wire produced by shear assisted processing and extrusion

Shear assisted processing and extrusion (ShAPE) process can consolidate powdered materials and simultaneously extrude wire or tube with improved properties. We successfully produced copper wire extrusions from powder and solid materials for the first time. The extrusion pressure of ShAPE process is at least two times less than that required for conventional extrusion. We used optical microscopy to inspect and validate the integrity of extrudates. It shows that the microstructure was refined and dynamically recrystallized to equiaxial grains. Compared to the annealed copper wire, ShAPE processed wire has 80% higher yield strength, 15% higher ultimate tensile strength and 20% higher ductility. These were correlated with refined grain size and sub-structuring observed via electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM).

Copper, Wire, Shear Assisted Processing and Extrus↗
DOE OSTI2023

Cladding and Butt-Joining Dissimilar Aluminum Alloys Simultaneously via Shear Assisted Processing and Extrusion

Shear assisted processing and extrusion has been used to fabricate multi-metallic tubing that incorporates regions with clad and butt-joined structures. In this work, aluminum alloys 6061, 7075, and 1100 are combined to create a monolithic extruded tubing with weldable ends (6061), a high strength center (7075), and a corrosion-resistant cladding (1100). Optical microscopy shows a gradual, defect-free, transition between alloys at the butt-joint interfaces and a sharp transition between alloys at the clad interface. Tensile testing proved the mechanical coherency of the joint, with failure occurring outside the tri-metallic structure. In conclusion, smoothed particle hydrodynamic simulations identified a spiral pattern of the cladding alloy that leads to inconsistent cladding thickness, and identified a simplified 2-alloy combination of aluminum alloys 6082 and 2014 that accomplished the design objectives of the tri-metallic structure.

Coatings↗
DOE OSTI2017

Experiments and modeling to characterize microstructure and hardness in 304L

Drawn 304L stainless steel tubing was subjected to 42 different annealing heat treatments with the goal of initializing a microstructural model to select a heat treatment to soften the tubing from a hardness of 305 Knoop to 225–275 Knoop. The amount of recrystallization and grain size caused by 18 heat treatments were analyzed via optical microscopy and image analysis, revealing the full range of recrystallization from 0 to 100%. The formation of carbides during the longer duration and higher-temperature heat treatments was monitored via transmission electron microscope evaluation. The experimental results informed a model which includes recovery, recrystallization, and grain growth to predict microstructure and hardness. After initialization of the model, it was able to predict hardness with a R 2 value of 0.95 and recrystallization with an R 2 value of 0.99. As a result, the model was then utilized in the design and testing of a heat treatment to soften the tubing.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Microstructural Development in Inconel 718 Nickel-Based Superalloy Additively Manufactured by Laser Powder Bed Fusion

Excellent weldability and high temperature stability make Inconel 718 (IN718) one of the most popular alloys to be produced by additive manufacturing. Here in this study, we investigated the effects of laser powder bed fusion (LPBF) parameters on the microstructure and relative density of IN718. The samples were fabricated with independently varied laser power (125 - 350W), laser scan speed (200 - 2200 mm/s), and laser scan rotation (0° - 90°). Archimedes’ method, optical microscopy, and scanning electron microscopy were employed to assess the influence of LPBF parameters on the relative density and microstructure. Optimal processing windows were identified for a wide range of processing parameters and relative density greater than 99.5% was achieved using volumetric energy density between 50 and 100 J/mm3. Microstructural features including melt pool geometry, lack of fusion defect, keyhole porosity, and sub-grain cellular microstructure were examined and quantified to correlate to LPBF parameters. A simple empirical model was postulated to relate relative sample density and LPBF volumetric energy density. Melt pool dimensions were quantitatively measured and compared to estimations based on Rosenthal solution, which yielded a good agreement with the width, but underestimated the depth, particularly at high energy input, due to lack of consideration for keyhole mode. In addition, the sub-grain cellular-dendritic microstructure in the as-built samples was observed to decrease with increasing laser scan speed. Quantification of the sub-micron cellular-dendritic microstructure yielded estimated cooling rate in the order of 10 5 – 10 7 K/s.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Microstructural Coarsening Kinetics and Mechanical Property Changes in Long-Term Aged Sn–Pb–Sb Solder Joints

Tin-lead-antimony (50Sn–47Pb–3Sb wt.%) soldered assemblies were mechanically tested approximately 30 years after initial production and found to have solder joints of reduced strength. The microstructure of this solder alloy exhibits a ternary eutectic structure with Sn-rich, Pb-rich, and SnSb phases. Accelerated aging was performed to evaluate solder microstructural coarsening and associated strength of laboratory solder joints to correlate these properties to the “naturally aged” solder joints. Isothermal aging was conducted at room temperature, 55, 70, 100, and 135 °C and aging times that ranged from 0.1 to 365 days. The coarsening kinetics of the Pb-rich phase were determined through optical microscopy and image analysis methods established in previous studies on binary Sn–Pb solder. A kinetic equation was developed with time exponent n of 0.43 and activation energy of 24000 J/mol, suggesting grain boundary diffusion or other fast diffusion pathways controlling the microstructural evolution. Compression testing and Vickers microhardness showed significant strength loss within the first 20–30 days after soldering; then, the microstructure and mechanical properties changed more slowly over long periods of time. Further, by combining accelerated aging data and the microstructure-based kinetics, strength predictions were made that match well with the properties of the actual soldered assemblies naturally aged for 30 years. However, aging at the highest temperature of 135 °C produced anomalous behavior suggesting that extraneous aging mechanisms are active. Therefore, data obtained at this temperature or higher should not be used. Overall, the combined microstructural and mechanical property methods used in this study confirmed that the observed reduction in strength of ~ 30-year-old solder joints can be accounted for by the microstructural coarsening that takes place during long-term solid-state aging.

36 MATERIALS SCIENCE↗
DOE OSTI2025

A New Method for Polishing Laminated Dissimilar Metals

Here, this paper presents a novel method for preparing metallographic samples of laminated dissimilar metals, specifically a layered structure of zirconium (Zr), vanadium (V), and tungsten (W), which pose a challenge due to their differing crystal structures and hardness levels. The work was motivated by the need to develop a cladding for tungsten targets in spallation neutron sources, where a zirconium face is applied over an interlayer of either vanadium or titanium to prevent the formation of brittle intermetallic compounds such as ZrW 2 . Traditional polishing techniques prove inadequate because each constituent metal requires a different polishing approach based on its unique material properties. The methodology outlined includes a sequential process involving conductive epoxy mounting, successive grinding and polishing with specific abrasives, and a final chemical-mechanical polish using a colloidal silica-based solution. Optical microscopy confirmed that this multi-step process successfully produced scratch-free surfaces and minimized surface relief across the different metal interfaces. Although developed for refractory metals, this approach shows promise for other layered structures comprised of transition metals, offering a meticulous yet effective technique for high-quality metallographic sample preparation.

Newberry, Daniel [Oak Ridge National Laboratory (O↗
DOE OSTI2023

A Workflow for Accelerating Multimodal Data Collection for Electrodeposited Films

Abstract Future machine learning strategies for materials process optimization will likely replace human capital-intensive artisan research with autonomous and/or accelerated approaches. Such automation enables accelerated multimodal characterization that simultaneously minimizes human errors, lowers costs, enhances statistical sampling, and allows scientists to allocate their time to critical thinking instead of repetitive manual tasks. Previous acceleration efforts to synthesize and evaluate materials have often employed elaborate robotic self-driving laboratories or used specialized strategies that are difficult to generalize. Herein we describe an implemented workflow for accelerating the multimodal characterization of a combinatorial set of 915 electroplated Ni and Ni–Fe thin films resulting in a data cube with over 160,000 individual data files. Our acceleration strategies do not require manufacturing-scale resources and are thus amenable to typical materials research facilities in academic, government, or commercial laboratories. The workflow demonstrated the acceleration of six characterization modalities: optical microscopy, laser profilometry, X-ray diffraction, X-ray fluorescence, nanoindentation, and tribological (friction and wear) testing, each with speedup factors ranging from 13–46x. In addition, automated data upload to a repository using FAIR data principles was accelerated by 64x.

36 MATERIALS SCIENCE↗