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At least 919 records · Page 51

In-Situ Observation of FCC→HCP Transformation-Induced Plasticity Behavior During Dynamic Deformation of CoCrNi Multi-principal Element Alloys

CoCrNi multi-principal element alloys (MPEAs) have potential as high toughness, blast resistant materials, but limited studies of their high strain rate behavior have been performed. Their high toughness has been attributed to low stacking fault energies and the activation of toughness enhancing deformation mechanisms, such as twinning- and transformation-induced plasticity (TWIP and TRIP, respectively), that may be affected by increased strain rate. This work examines a series of CoCrNi MPEAs tested with a miniaturized pressure bar, while simultaneous synchrotron x-ray diffraction and imaging are performed, and compares these results to those collected during quasi-static deformation at elevated temperatures. Here, the collected diffraction indicates that TRIP was active at elevated strain rates for the most Co-rich alloys containing 50 or 55 at. pct. Co, while TRIP behavior was suppressed at elevated strain rates in a 40 at. pct. Co alloy anticipated to experience TRIP. The suppression of TRIP in the lower Co alloy at high strain rates is attributed to adiabatic heating, consistent with suppression of TRIP as a result of elevated temperatures.

36 MATERIALS SCIENCE↗

Understanding the Formation and Evolution of Oxide Inclusions in Si-Deoxidized Spring Steel

To illustrate the mechanism of the formation and evolution of inclusions in Si-deoxidized spring steel, pilot trials and systematic samplings were conducted, and detailed information about the inclusion density, morphology and composition was elucidated by electron probe X-ray microanalysis. The steel samples were collected from the vacuum degassing furnace, tundish furnace and spring rods after hot rolling. Based on the relationship between the mass ratio of X{sub (CaO)}/X{sub (SiO{sub 2)}} and diameters of inclusions, CaO-SiO{sub 2} inclusions were found to be formed by the coalescence between SiO{sub 2} and CaO-SiO{sub 2} inclusions. Most CaO-SiO{sub 2} inclusions > 10 μm were located in the melilite areas with liquidus temperatures < 1400 °C. The Al{sub 2}O{sub 3}-SiO{sub 2}-CaO inclusions in the steel samples from the vacuum degassing and tundish furnaces were considered to be formed by reduction of CaO-SiO{sub 2} inclusions by Al dissolved in steel. The increased number density of Al{sub 2}O{sub 3}-SiO{sub 2}-CaO inclusions in spring rods was primarily attributed to the entrapment of Na{sub 2}O-contained mould flux particles and inclusions crushed after hot rolling. Many Al{sub 2}O{sub 3}-SiO{sub 2}-MnO and SiO{sub 2}-MnO inclusions were observed in tundish furnace samples, which originated from inherent reactions between [Al], [Si], [Mn] and [O] in the molten steel. The SiO{sub 2} precipitation of Al{sub 2}O{sub 3}-SiO{sub 2}-MnO inclusions was attributed to the solubility decrease during the solidification process with temperature drop.

36 MATERIALS SCIENCE↗

Effects of High Current Pulsed Electron Beam Irradiation on the Mechanical Properties and Cutting Performance of TiAlN-Coated Tools

Commercial TiAlN-coated carbide tools were post-treated using the high current pulsed electron beam irradiation method. The influence of the energy density of the electron beam on the morphology, phase composition, surface roughness and Vickers hardness were investigated. The higher energy density imposed on TiAlN-coated carbide tools resulted in a flatter and harder modified surface. After the beam irradiation, the XRD diffraction peak intensity of the hardening phase (Ti,Al)N was changed, and the diffraction peak position was shifted; these changes are attributed to the improved microhardness of the irradiated coatings. Investigations on the cutting experiments of turning Ti-6Al-4V alloy showed that the irradiated TiAlN-coated carbide tool exhibited longer cutting life and better wear resistance than those of an unirradiated tool. This improvement is attributed to the combined effect of low surface roughness and high microhardness that resulted from the high current pulse electron beam irradiation.

36 MATERIALS SCIENCE↗

Austenitic Reversion of Cryo-rolled Ti-Stabilized Austenitic Stainless Steel: High-Resolution EBSD Investigation

In this study, AISI 321 austenitic stainless steel (ASS) was cryo-rolled and subsequently annealed at 650 and 800 °C to reverse BCC α′-martensite to FCC γ-austenite. The texture evolution associated with the reversion at the selected temperatures was investigated using high-resolution EBSD. After the reversion, TiC precipitates were observed to be more stable in 650 °C-annealed specimens than those reversed at 800 °C. {110} texture was mainly developed in specimens subjected to both annealing temperatures. However, specimens reversed at 650 °C have stronger texture than those annealed at 800 °C, even at the higher annealing time. The strong intensity of {110} texture component is attributed to the ability of AISI 321 ASS to memorize the crystallographic orientation of the deformed austenite, a phenomenon termed texture memory. The development of weaker texture in 800 °C-annealed specimens is attributed to the residual strain relief in grains, dissolution of grain boundary precipitates, and an increase in atomic migration along the grain boundaries. Based on the observed features of the reversed austenite grains and estimation from an existing model, it is suspected that the austenite reversion at 650 and 800 °C undergone diffusional and martensitic shear reversion, respectively.

36 MATERIALS SCIENCE↗

Mechanical Behavior of Commercially Pure Titanium Weldments at Lower Temperatures

Commercially pure titanium is used for low-temperature applications due to good toughness attributed to single-phase microstructure (α). Electron beam welding (EBW) and gas tungsten arc welding (GTAW) processes have been used for welding two grades of commercially pure titanium (Grade 2 and Grade 4). Martensitic microstructure is found to be finer in the case of EBW joint as compared to GTAW joint due to faster rate of cooling in the former process. Weldments have been characterized to study the mechanical behavior at ambient (298 K) and cryogenic temperatures (20 and 77 K). Strength of weldments increases with the decrease in temperature, which is found to be more prominent in case of Grade 4 titanium as compared to Grade 2. Weld efficiency of Grade 4 is found to be higher at all the temperatures (ambient, 77 and 20 K). However, ultimate tensile strength/yield strength ratio is higher for Grade 2 as compared to Grade 4. % Elongation is found to increase/retained at cryogenic temperatures for Grade 2, and it is found to decrease for Grade 4. Electron backscattered diffraction analysis and transmission electron microscopy of deformed samples confirmed the presence of extensive twinning in Grade 2 and the presence of finer martensitic structure in Grade 4. Fractography analysis of tested specimens revealed the presence of cleavage facets in Grade 4 and dimples in specimens of Grade 2. Higher strength in Grade 4 is attributed to higher oxygen restricting the twin-assisted slip, which is otherwise prominent in Grade 2 titanium.

36 MATERIALS SCIENCE↗

Effect of Al on Grain Refinement and Mechanical Properties of Mg-3Nd Casting Alloy

The effect of Al on the grain refinement and mechanical properties of as-cast Mg-3Nd alloy was investigated systematically by a series of microstructural analysis, solidification analysis and tensile tests. The results show that Al has an obvious refining effect on the as-cast Mg-3Nd alloy. With increasing Al content, the grain size of the as-cast Mg-3Nd alloy decreases firstly, then increases slightly after the Al content reaching 3 wt.%, and the minimum grain size of the Mg-3Nd alloy is 48 ± 4.0 μm. The refining mechanism can be attributed to the formation of Al{sub 2}Nd particles, which play an important role in the heterogeneous nucleation. The strength and elongation of the Mg-3Nd alloy refined by Al also increase with increasing Al content and slightly decrease when the Al content is more than 3 wt.%, and the strengthening mechanism is attributed to the grain refinement as well as dispersed intermetallic particles. Furthermore, the microstructural thermal stability of the Mg-3Nd-3Al alloy is higher than that of the Mg-3Nd-0.5Zr alloy. Overall, the Mg-3Nd alloy with Al addition is a novel alloy with wide and potential application prospects.

36 MATERIALS SCIENCE↗

Development of Graphene Nanoplatelet-Reinforced AZ91 Magnesium Alloy by Solidification Processing

It is a challenging task to effectively incorporate graphene nanoplatelets (GNPs) which have recently emerged as potential reinforcement for strengthening metals into magnesium-based matrices by conventional solidification processes due to their large surface areas and poor wettability. A solidification processing which combines mechanical stirring and ultrasonic dispersion of reinforcements in liquid matrix was employed to develop AZ91 magnesium alloy matrix composites reinforced with 0.25 and 0.5 wt.% GNPs. The microstructural studies conducted with scanning and transmission electron microscopes revealed that fairly uniform distribution and dispersion of GNPs through the matrix were achieved due to effective combination of mechanical and ultrasonic stirring. The GNPs embedded into the magnesium matrix led to significant enhancement in the hardness, tensile strength and ductility of the composites compared to those of unreinforced AZ91 alloy. The strength enhancement was predominantly attributed to the grain refinement by the GNP addition and dislocation generation strengthening due to the coefficient of thermal expansion mismatch between the matrix and reinforcement. The improved ductility was attributed to the refinement of β eutectics by transforming from lamellar to the divorced eutectics due to the GNP additions. In addition, the strengthening efficiency of the composite with 0.25 wt.% GNP was found to be higher than those of the composite with 0.5 wt.% GNP as the agglomeration tendency of GNPs is increased with increasing GNP content. These results were compared with those of the GNP-reinforced magnesium composites reported in the literature, indicating the potential of the process introduced in this study in terms of fabricating light and high-performance metal matrix composites.

36 MATERIALS SCIENCE↗

Effect of Cold Rolling and Heat Treatment on Microstructure and Mechanical Properties of Ti-4Al-1Mn Titanium Alloy

Mechanical behavior of Ti-4Al-1Mn titanium alloy has been studied in annealed, cold-rolled and heat-treated conditions. Room temperature tensile strength as well as % elongation has been found to be low with increasing amount of cold rolling. Lowering of strength in cold worked condition is attributed to premature failure. However, the same has been mitigated after heat treatment. Significant effect of cooling media (air and water) from heat treatment temperature on microstructure was not found except for the degree of fineness of α plates. Optimum properties (strength as well as ductility) were exhibited by samples subjected to 15% cold rolling and heat treatment below β transus temperature, which can be attributed to presence of recrystallized microstructure. In cold worked condition, the microstructure shows fine fragmented α plates/Widmanstätten morphology with high dislocation density along with a large amount of strain fields and twinning, which gets transformed to recrystallized equiaxed microstructure and with plate-like morphology after near β heat treatment. Prior cold work is found to have a significant effect on mechanical properties supported by evolution of microstructure. Twinning is found to be assisting in deformation as well as in recrystallization through the formation of deformation and annealing twins during cold working and heat treatment. Fracture analysis of the tested sample with prior cold work and heat-treated condition revealed quasi-ductile failure as compared to only ductile failure features seen for samples heat treated without prior cold work.

36 MATERIALS SCIENCE↗

Effects of Nb on the Microstructure and Properties of Ti-Added Hypereutectic High-Cr Cast Iron

Effects of Nb on the microstructure and properties of Ti-added hypereutectic high-Cr cast iron were studied. With the addition of Nb, a new phase (Nb,Ti)C was formed. The microstructure analysis revealed that the amount of primary carbides was decreased from 18.6 to 8.8% and the primary and eutectic carbides were greatly refined. The decrease in the amount of primary carbides was attributed with the shrinking of primary M{sub 7}C{sub 3} phase zone in the phase diagram, while the refinement of primary carbides was attributed to the heterogeneous nucleus of (Nb,Ti)C phase for the primary M{sub 7}C{sub 3} carbides. The macrohardness of the alloy increased from 60.8 to 63.5HRC, and the impact toughness increased from 3.8 to 5.2 J cm{sup −2}. Furthermore, the wear resistance was enhanced with the addition of Nb due to the formation of hard (Nb,Ti)C carbides.

36 MATERIALS SCIENCE↗

Effect of Minor Er on the Microstructure and Properties of Al-6.0Mg-0.4Mn-0.1Cr-0.1Zr Alloys

As-cast Al-6.0Mg-0.4Mn-0.1Cr-0.1Zr alloys containing different additions of Er were prepared. Then, the specimens were carried out homogenization heat treatment, hot rolling, cold rolling, and annealing. The effects of minor Er on the microstructure and properties of Al-6.0Mg-0.4Mn-0.1Cr-0.1Zr alloy were investigated. Results show that addition of Er can refine the microstructure and improve the mechanical properties of the alloys. As for the annealed alloys, the addition of 0.33%Er can increase the tensile strength by 29 MPa. Strength increment is mainly attributed to refinement and the precipitation of Al{sub 3}Er and Al{sub 3}(Er, Zr). Additionally, the minor Er can improve the corrosion resistance of the alloys, which can be attributed to the compact composite oxide film of Er-O and Al-O, purification, and modification.

36 MATERIALS SCIENCE↗

Microstructural Analysis of Powder Metallurgy Tool Steels in the Context of Abrasive Wear Behavior: A New Computerized Approach to Stereology

The present work describes a new methodology designed to characterize the microstructures of tool steels containing carbide hard phases, with the focus set on their abrasive wear resistance. A series of algorithms were designed and implemented in MATLAB® to (i) recognize each of the features of interest, (ii) measure relevant quantities and (iii) characterize each of the phases and the alloy in function of attributes usually neglected in wear description applications: size distribution, shape and contiguity of the hard phases. The new framework incorporates new parameters to describe each one of these attributes, as observed in SEM micrographs. All three aforementioned stages contain novel contributions that can be potentially beneficial to the field of materials design in general and to the field of alloy design for severely abrasive environments in particular. Models of known geometry and micrographs of different powder metallurgy steels were analyzed, and the obtained results were compared with the obtained by the linear intercept method. The relation between the new parameters and the ones available in the scientific literature is also discussed.

36 MATERIALS SCIENCE↗

Effect of Anisotropy on Microstructures and Mechanical Properties of Rolled Ti/Al/Mg/Al/Ti Laminates

TA2/5052Al/AZ31/5052Al/TA2 five-ply laminates were fabricated by hot rolling, and the effect of anisotropy on their microstructures and mechanical properties was studied. After rolling, the Mg/Al and Al/Ti interfaces were both closely connected, but the interfacial shapes were totally different. For the Mg layer microstructures in the middle area, regardless of the direction, dynamic recrystallized (DRXed) grains appeared around the deformation bands. However, twins and a shear zone appeared in the RD sample; the twins decreased in the sample along the 45° angle, and no twins appeared in the TD sample. The Ti layer showed equiaxed grains in different directions, which were attributed to the ability of Ti alloy to anti-deform. The tensile testing results showed that the fracture of the Ti/Al/Mg/Al/Ti laminates can be divided into four stages. The laminate had an ultimate tensile strength of 434 MPa and excellent elongation along the rolling direction (RD), which were attributed to its DRXed grains and twins. In conclusion, the laminates had significant anisotropy due to the presence of Mg alloys.

36 MATERIALS SCIENCE↗

Effect of Strain Rate on the Tensile Behavior of CoCrFeNi and CoCrFeMnNi High-Entropy Alloys

High-entropy alloys (HEAs), a novel class of metal alloys, have been receiving increasing attention from the scientific community. HEAs have the potential to be used in critical load-bearing applications in replacement of conventional alloys such as stainless steel and nickel-base superalloys. Tensile experiments at quasi-static to dynamic strain rates (10{sup −4}-10{sup 3} s{sup −1}) were performed on two single-phase face-centered cubic HEAs, CoCrFeNi and CoCrFeMnNi. Electron backscatter diffraction was used to study the microstructure of the samples before the experiments, and transmission electron microscopy was performed postmortem. The dominant deformation mechanisms were dislocation slip at quasi-static strain rates with the addition of deformation nano-twins at dynamic strain rates. Ultimate dynamic tensile strength and ductility improved with the increase in strain rate, which can be attributed to the activation of deformation nano-twins in HEAs. CoCrFeNi and CoCrFeMnNi both have low stacking fault energies, which could promote twinning at high strain rates to accommodate plastic deformation. The strain rate sensitivity of the flow stress increased with increasing strain rate, beginning with negligible strain rate sensitivity in the quasi-static range to high strain rate sensitivity in the dynamic range. CoCrFeMnNi showed greater strain rate sensitivity of flow stress. CoCrFeNi, with less configurational entropy, had higher mechanical properties and strain-hardening rates compared to CoCrFeMnNi, which was attributed to the weakening effect of the addition of Mn on the solid solution hardening.

36 MATERIALS SCIENCE↗

Grain-Refined Microstructure and Hard Surface Layer Produced by SMRGT Process for Improved Corrosion Behavior of Mg-3Al-1Zn Alloy

To improve the surface properties and performance, a grain-refined surface layer was produced on AZ31B Mg alloy by a newly developed surface nano-crystallization and hardening process called surface mechanical rolling grinding treatment (SMRGT). The grain size refinement and minimal surface hardening were confirmed by the microstructure observations, XRD results and microhardness tests and were attributed to the multipass small strain-induced plastic deformation of the material during the SMRGT process. A nano-grain surface layer (average grain size of ~ 100 nm) and a graded microhardness variation (average ~ 113 HV adjacent to surface) along the thickness direction were generated. The E{sub corr} values of the as-SMRGTed samples were − 1.43 ± 0.03 and − 1.42 ± 0.02 V, increasing by ~ 30-40 mV compared with the values of the as-received (AR) sample (− 1.46 ± 0.02 V), corresponding to i{sub corr} ranging from 3.0 × 10{sup −5} to 1.0 × 10{sup −5} and 5.0 × 10{sup −6} A/cm{sup 2}, respectively. Charge transfer resistance (R{sub ct}) increased from 93.4 to 292.4 and 578.3 Ω (~ 3-6 times) with the increasing number of SMRGT passes. The corrosion resistance improvement was attributed mainly to the dramatic strain-induced surface grain refinement and minimal surface hardening that give rise to a more smooth and densely packed surface state.

36 MATERIALS SCIENCE↗

Process-Structure-Property Relationships for 316L Stainless Steel Fabricated by Additive Manufacturing and Its Implication for Component Engineering

We investigate the process-structure-property relationships for 316L stainless steel prototyping utilizing 3-D laser engineered net shaping (LENS), a commercial direct energy deposition additive manufacturing process. Our study concluded that the resultant physical metallurgy of 3-D LENS 316L prototypes is dictated by the interactive metallurgical reactions, during instantaneous powder feeding/melting, molten metal flow and liquid metal solidification. This study also showed 3-D LENS manufacturing is capable of building high strength and ductile 316L prototypes due to its fine cellular spacing from fast solidification cooling, and the well-fused epitaxial interfaces at metal flow trails and interpass boundaries. However, without further LENS process control and optimization, the deposits are vulnerable to localized hardness variation attributed to heterogeneous microstructure, i.e., the interpass heat-affected zone (HAZ) from repetitive thermal heating during successive layer depositions. Most significantly, the current deposits exhibit anisotropic tensile behavior, i.e., lower strain and/or premature interpass delamination parallel to build direction (axial). This anisotropic behavior is attributed to the presence of interpass HAZ, which coexists with flying feedstock inclusions and porosity from incomplete molten metal fusion. Our current observations and findings contribute to the scientific basis for future process control and optimization necessary for material property control and defect mitigation.

36 MATERIALS SCIENCE↗

Anomalous Annealing Response of Directed Energy Deposited Type 304L Austenitic Stainless Steel

Directed energy deposited (DED) and forged austenitic stainless steels possess dissimilar microstructures but can exhibit similar mechanical properties. In this study, annealing was used to evolve the microstructure of both conventional wrought and DED type 304L austenitic stainless steels, and significant differences were observed. In particular, the density of geometrically necessary dislocations and hardness were used to probe the evolution of the microstructure and properties. Forged type 304L exhibited the expected decrease in measured dislocation density and hardness as a function of annealing temperature. Here, the more complex microstructure–property relationship observed in the DED type 304L material is attributed to compositional heterogeneities in the solidification microstructure.

36 MATERIALS SCIENCE↗

A Retrospective Evaluation of the Use of Mass Spectrometry in FDA Biologics License Applications

The characterization sections of biologics license applications (BLAs) approved by the United States Food and Drug Administration (FDA) between 2000 and 2015 were investigated to examine the extent of the use of mass spectrometry. Mass spectrometry was found to be integral to the characterization of these biotherapeutics. Of the 80 electronically submitted monoclonal antibody and protein biotherapeutic BLAs included in this study, 79 were found to use mass spectrometric workflows for protein or impurity characterization. To further examine how MS is being used in successful BLAs, the applications were filtered based on the type and number of quality attributes characterized, the mass spectrometric workflows used (peptide mapping, intact mass analysis, and cleaved glycan analysis), the methods used to introduce the proteins into the gas phase (ESI, MALDI, or LC-ESI), and the specific types of instrumentation used. Analyses were conducted over a time course based on the FDA BLA approval to determine if any trends in utilization could be observed over time. Additionally, the different classes of protein-based biotherapeutics among the approved BLAs were clustered to determine if any trends could be attributed to the specific type of biotherapeutic. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Reactive Landing of Gramicidin S and Ubiquitin Ions onto Activated Self-Assembled Monolayer Surfaces

Using mass-selected ion deposition combined with in situ infrared reflection absorption spectroscopy (IRRAS), we examined the reactive landing of gramicidin S and ubiquitin ions onto activated self-assembled monolayer (SAM) surfaces terminated with N-hydroxysuccinimidyl ester (NHS-SAM) and acyl fluoride (COF-SAM) groups. Doubly protonated gramicidin S, [GS+2H]2+, and two charge states of ubiquitin, [U+5H]5+ and [U+13H]13+, were used as model systems, allowing us to explore the effect of the number of free amino groups and the secondary structure on the efficiency of covalent bond formation between the projectile ion and the surface. For all projectile ions, ion deposition resulted in the depletion of IRRAS bands corresponding to the terminal groups on the SAM and the appearance of several new bands not associated with the deposited species. These new bands were assigned to the C=O stretching vibrations of COOH and COO- groups formed on the surface as a result of ion deposition. The presence of these bands was attributed to an alternative reactive landing pathway that competes with covalent bond formation. This pathway with similar yields for both gramicidin S and ubiquitin ions is analogous to the hydrolysis of the NHS ester bond in solution. The covalent bond formation efficiency increased linearly with the number of free amino groups and was found to be lower for the more compact conformation of ubiquitin compared with the fully unfolded conformation. This observation was attributed to the limited availability of amino groups on the surface of the folded conformation. Our results have provided new insights on the efficiency and mechanism of reactive landing of peptides and proteins onto activated SAMs

Environmental Molecular Sciences Laboratory↗