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Fine grained fully lamellar structure acquisition and microstructure characteristics of Ti-44Al-4Nb-4V-0.3Mo-Y alloy
Highlights: • Cellular structure is the component of the microstructure of hot forging in α + β two-phase-field. • Inhomogeneous lamellar structure could be eliminated by hot forging in β+γ binary phase field. • After hot forging and annealing at β+γ two-phase-region, fine grained fully-lamellar microstructure is obtained. - Abstract: In this paper, the microstructure characteristic of a β solidifying TiAl alloy Ti-44Al-4Nb-4V-0.3Mo-Y (at. %) was investigated systematically. Cylindrical blanks were isothermal forged at 1250 °C within (α + β) two-phase-field and 1200 °C within (β + γ) two-phase-field under the strain rate of 0.02 s{sup −1} and 0.03 s{sup −1}, with a total reduction of 75%. The microstructure of the alloy forged in α + β two-phase-field consists of lamellar colonies (only represents α{sub 2}/γ lamellar colonies), mixture structure of β/B2 phase and γ phase as well as β/γ lamellae resulted from cellular reaction. However, a large amount of equiaxed γ grains appear with no β/γ lamellae available under forging in β + γ two-phase-field, and the average size of γ grain is about 10 μm. By further annealed at 900 °C for about 0.5 h, the structure of hot forging at 1250 °C is composed of β/B2 phase and equiaxed γ grains with the mean size about 5 μm. After heat treated at 1200 °C for 2 h, the microstructure of this annealed samples is characterized by fine grained fully lamellar (FFL) structure with size of 20 μm. A specially designed hot forging process is proposed, which prevents the existence of inhomogeneous lamellar structure.
Strong, ductile, and hierarchical hetero-lamellar-structured alloys through microstructural inheritance and refinement
The strength−ductility trade-off exists ubiquitously, especially in brittle intermetallic-containing multiple principal element alloys (MPEAs), where the intermetallic phases often induce premature failure leading to severe ductility reduction. Hierarchical heterogeneities represent a promising microstructural solution to achieve simultaneous strength−ductility enhancement. However, it remains fundamentally challenging to tailor hierarchical heterostructures using conventional methods, which often rely on costly and time-consuming processing. Here, we report a multiscale microstructural inheritance and refinement strategy to process “structural hierarchy precursors” in as-cast heterogeneous Al 0.7 CoCrFeNi MPEAs, which lead directly to a hierarchical hetero-lamellar structure (HLS) after simple rolling and annealing. Interestingly, it takes only 10 min of annealing time, two orders of magnitude less than that required to render the state-of-the-art properties during conventional processing of Al 0.7 CoCrFeNi, for us to achieve record-high strength−ductility combinations via the hierarchical HLS design that sequentially stimulates multiple unusual deformation and reinforcement mechanisms. In particular, the HLS-enabled high hetero-deformation-induced (HDI) internal stress triggers profuse <111>-type dislocations on over five independent slip systems in the supposedly brittle intermetallic phase and activates extensive stacking faults (SFs) and nanotwinning in the adjoining soft phase with a rather high SF energy. These unexpected, dynamically reinforcing hetero-deformation mechanisms across multiple length scales facilitate high sustained HDI strain hardening, along with a salient microcrack-mediated extrinsic ductilization effect, suggesting that the proposed microstructural inheritance and refinement strategy provides an efficient, fast, and low-cost approach to overcome the strength−ductility trade-off in a broad range of structural materials.
Alternating crystalline lamellar structures from thermodynamically miscible poly(ε-caprolactone) H/D blends
Thermodynamic interaction and non-isothermal crystallization behavior in a series of protiated (H-) and deuterated (D-) poly(ε-caprolactone) (PCL) blends have been systematically investigated. The blends were thermodynamically miscible in the melt. The Flory–Huggins interaction parameter (χ) between H- and D-PCL segments was estimated. The hydroxyl groups in the PCL chain-ends were found to contribute significantly to the negative χ values. Combined characterization of small-angle X-ray scattering (SAXS) and small-angle neutron scattering (SANS) revealed that upon slow cooling, unique alternating H-rich and D-rich PCL lamellar structures are formed regardless of the blend ratio, which is attributed to the T c difference between H- and D-PCLs. While upon rapid cooling, mixed crystals of H- and D-PCLs are predominantly formed. These results provide insightful information on the melt thermodynamics as well as detailed chain arrangements in lamellar crystals for semi-crystalline H/D polyester blends.
Diffusion characteristics of water molecules in a lamellar structure formed by triblock copolymers
The distribution and diffusion of water molecules are playing important roles in determining self-assembly and transport properties of polymeric systems. Small-angle neutron scattering (SANS) experiments and molecular dynamics (MD) simulation have been applied to understand the distribution of water molecules and their dynamics in the lamellar membrane formed by Pluronic L62 block copolymers. Penetration of water molecules into the polyethylene oxide (PEO) layers of the membranes has been estimated using scattering length density (SLD) profiles obtained from SANS measurements, which agree well with the molecular distribution observed from MD simulations. The water diffusion coefficient at different regions of the lamellar membrane was further investigated using MD simulation. The diffusion characteristic shows a transition from normal to anomalous diffusion as the position of the water molecule changes from the bulk to PEO and to the polypropylene oxide (PPO) layer. Here we find that water molecules within the PEO or PPO layers follow subdiffusive dynamics, which can be interpreted by the model of fractional Brownian motion.
Influence of warm rolling temperature on multi-scale lamellar structure and mechanical properties of
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RGO/BaFe12O19/Fe3O4 nanocomposite as microwave absorbent with lamellar structures and improved polarization interfaces
Highlights: • RGO/BaFe{sub 12}O{sub 19}/Fe{sub 3}O{sub 4} nanocomposite are prepared via a two-step solvothermal method. • The maximum reflection loss can reach −46.04 dB, and the effective absorption bandwidth under −10 dB is 5.68 GHz. • Interfacial polarization as one of the mechanism for the enhanced absorption properties was detailedly analyzed. - Abstract: In this paper, we designed and prepared a composite of BaFe{sub 12}O{sub 19} (BFO) flakes, two-dimensional graphene and Fe{sub 3}O{sub 4} nanoparticles using a two-step solvothermal method. The combination of BFO flakes and two-dimensional graphene could effectively enhance the heterointerface and is believed to be favorable to enhance the interface polarization. The introduction of inverse spinel Fe{sub 3}O{sub 4} as the third phase could increase the saturated magnetization. The phase structure, morphology, magnetic properties and electromagnetic wave absorption performance of the as-prepared samples were characterized. Due to the enhanced interfacial polarization between the BaFe{sub 12}O{sub 19} flakes and graphene, the composite of RGO/BaFe{sub 12}O{sub 19}/Fe{sub 3}O{sub 4} exhibits excellent microwave absorption properties. The maximum reflection loss can reach -46.04 dB at 15.6 GHz with a thickness of 1.8 mm, and the effective absorption bandwidth reaches 5.68 GHz (from 11.60 GHz to 17.28 GHz). It is believed that the RGO/BaFe{sub 12}O{sub 19}/Fe{sub 3}O{sub 4} composites can find potential application in the field of microwave absorption due to their excellent absorption properties.
One-step synthesis of mesoporous pentasil zeolite with single-unit-cell lamellar structural features
A method for making a pentasil zeolite material includes forming an aqueous solution that includes a structure directing agent and a silica precursor; and heating the solution at a sufficient temperature and for sufficient time to form a pentasil zeolite material from the silica precursor, wherein the structure directing agent includes a quaternary phosphonium ion.
Bidirectional freeze casting for fabricating lamellar structures
This disclosure provides systems, methods, and apparatus related to freeze casting. In one aspect, a method comprises providing an apparatus. The apparatus comprises a container and a cooling surface. A bottom of the container comprises a wedge. The wedge comprises a first substantially planar surface and a second substantially planar surface with an angle between the first and the second substantially planar surfaces. An interior bottom of the container comprises the second substantially planar surface. The cooling surface is in contact with the first substantially planar surface. A slurry is deposited on the second substantially planar surface, the slurry comprising a plurality of particles in a liquid. The cooling surface is cooled to cool the slurry at a specified cooling rate.
A high-performance β-solidifying TiAl alloy sheet: Multi-type lamellar microstructure and phase transformation
Highlights: • A high-performance β-solidifying TiAl alloy sheet is fabricated via hot rolling. • Fine multi-type β/γ and α{sub 2}/γ lamellar structures are formed during hot-rolling. • These lamellar structures are induced by the β → γ and α + γ → α{sub 2} + γ/γ{sub T} transformations. • The nano-scaled antiphase domain is induced by α → α{sub 2} disorder-order transformation. • The fine multi-type lamellar structures contribute to the strength enhancement. - Abstract: TiAl alloys are widely used in the aerospace industry and, hence, a thorough understanding of the corresponding microstructural evolution is crucial for providing insight into the fabrication of high-performance TiAl alloy sheets. In this study, a high-performance β-solidifying Ti-43Al-9V-0.2Y alloy sheet with multi-type lamellar structures was obtained via hot-rolling at an initial rolling temperature of 1260 °C. Owing to the temperature drop and reheat associated with multi-pass rolling, relatively fine irregular β/γ and regular α{sub 2}/γ lamellar microstructures (average size: ~25 μm) with nano-scaled antiphase domains (APDs) were generated by the β → γ and α + γ → α{sub 2} + γ/γ{sub T} phase transformations. These two lamellar structures have different formation mechanisms. The results of electron backscatter diffraction and transmission electron microscopy revealed that the nucleation and growth of (i) β/γ and (ii) α{sub 2}/γ lamellar structures are induced mainly by (i) stress and (ii) a combination of the stress and temperature drop during hot-rolling, respectively. Thin γ{sub T} precipitates from the α/α{sub 2} or γ phases. This precipitation is induced by the higher stress and lower temperature associated with the later stage (compared with those occurring in the initial stages) of hot-rolling. Moreover, compared with the corresponding as-forged alloy, the as-rolled TiAl alloy sheet exhibits better performance at both room and elevated temperatures. The improvement in the tensile properties is attributed to the duplex microstructure consisting of fine multi-type lamellar structures with nano-scaled APDs. The interface boundaries of β/γ, α{sub 2}/γ and APDs, which are effective in retarding dislocation motion, contribute mainly to strengthening of the alloy sheet.
Grain Refinement of Co-Cr-Mo-C Through Plastic Deformation Followed by Reversion of Lamellar Eutectoid Structure
Small plastic straining was combined with a two-step heat treatment to obtain grain refinement of the Co-28Cr-6Mo-0.33C alloy. The solution-treated specimens were furnace cooled to room temperature, obtaining partially transformed pearlite at grain boundaries. Afterward, the specimens were compressed up to 10% of engineering strain, followed by aging at 850 °C that contributed to the decomposition of the austenite phase into a lamellar eutectoid structure (α + M{sub 23}C{sub 6}). The full lamellar structure was then reverse-treated at temperatures from 1000 to 1237 °C, where the austenite phase was stable. The reversion treatment led to the nucleation of a fine-grained austenitic structure (with average size of 48.23 ± 21.30 μm—i.e., about 1/10 of its initial average size) at the lamellar eutectoid structure. Compression tests carried out on reverse-transformed samples showed better mechanical properties compared to those of the samples tested before reversing transformation.
Influence of Homogenization on the Mechanical Properties and Microstructure of the U-10Mo Alloy
In Phase 1 of this study, the mechanical properties of as-cast, depleted uranium alloyed with 10 weight percent molybdenum alloy (U-10Mo) samples were evaluated by high-temperature compression testing. Compression testing was conducted at three strain rates over a temperature range of 400 to 800°C. The results indicated that with increasing test temperature, the material flow stress decreases and the material becomes more sensitive to strain rate. In addition, above the eutectoid transformation temperature (~ 550°C), the drop in material flow stress is prominent and shows a strain-softening behavior, especially at lower strain rates. In the second part of this research, we studied the effect that homogenization heat treatment had on the high temperature mechanical properties and microstructure of the cast U-10Mo alloy. Various homogenization times and temperatures were studied ranging between 800 and 1000°C for 4 to 48 hours. Based on the microstructural response in this homogenization study, a heat treatment cycle of 800°C for 24 hours and another at 1000°C for 16 hours were selected as the times at temperature to achieve a fully homogenized sample. Samples from these conditions were then compression tested at a variety of temperatures ranging from 500 to 800°C. The microstructure of these samples were compared to the as-cast samples and to a baseline sample homogenized at 1000°C for 16 hours. The results indicate that below the eutectoid temperature (~ 550°C) all three samples showed strain hardening and followed similar trends. Above the eutectoid temperature, the yield strength of the material decreased linearly. For the as-cast sample and the sample homogenized at 800°C for 24 hours, the n-values were negative, whereas for the samples homogenized at 1000°C for 16 hours the material exhibited a perfectly plastic behavior. The as-cast sample, heat treated at 800°C for 24 hours, showed significant lamellar structure transformation that seems to have precipitated along the grain boundaries in the molybdenum-lean regions. In similar samples, homogenized at 800°C for 24 hours and tested at 650°C, the backscattered-electron scanning electron microscopy images revealed a composite structure of lamellar phase and nano-scale molybdenum-rich and -lean phases along the grain boundaries. These phases may have been responsible for the lowering of the flow stress in the material observed in the Phase 1 work. For comparison, the samples homogenized at 1000°C for 16 hours showed no such transformations.
Characterization of Dispersion Strengthened Copper Alloy Prepared by Internal Oxidation Combined with Mechanical Alloying
Cu-3.6 vol.% Al{sub 2}O{sub 3} dispersion strengthened alloy was prepared by mechanical alloying (MA) of internal oxidation Cu-Al powders. The lattice parameter of Cu matrix decreased with milling time for powders milled in argon, while the abnormal increase of lattice parameter occurred in the air resulting from mechanochemical reactions. With a quantitative analysis, the combined method makes residual aluminum oxidized completely within 10-20 h while mechanical alloying method alone needs longer than 40 h. Lamellar structure formed and the thickness of lamellar structure decreased with milling time. The size of Al{sub 2}O{sub 3} particles decreased from 46 to 22 nm after 40 h milling. After reduction, core–shell structure was found in MAed powders milled in the air. The compacted alloy produced by MAed powders milled in the argon had an average hardness and electrical conductivity of 172.2 HV and 82.1% IACS while the unmilled alloy’s were 119.8 HV and 74.1% IACS due to the Al{sub 2}O{sub 3} particles refinement and residual aluminum in situ oxidization.
Effect of cooling rate on microstructure evolution of Ti-45Al-8.5Nb-0.2W-0.2B-0.02Y alloy during multi-step heat treatment
Highlights: • Novel ideas to control cooling rate during different phase transformation are proposed. • Cooling rates induced microstructure evolutions during the whole phase transformation are investigated. • Phase transformation texture and the characteristics of lamellar structures are related to cooling rate. - Abstract: Microstructure evolution of Ti-45Al-8.5Nb-0.2W-0.2B-0.02Y alloy (at.%) resulted from different cooling rates during the whole phase transformation process has been thoroughly investigated. The results show that the cooling rate during β → α transformation plays a crucial role in the modification of the crystallographic orientation relationship between the α grains and their parent β phase. The decrease of cooling rate can reduce the volume fraction of Burgers α grains and avoid the preferential distribution of lamellar interface traces. This could be attributed to the different nucleation and growth kinetics of α phase affected by the cooling rate. Moreover, the lamellar structure characteristics are closely related to the cooling rate during α → α{sub 2} + γ transformation and their responses to stabilization treatment shall vary accordingly. A fast cooling rate retains a high quantity of high temperature α/α{sub 2} phase. These α/α{sub 2} phase could decompose into ultrafine lamellar structure during subsequent stabilization treatment. While the average lamellar spacing of the slow cooled microstructure has a small increase by limited continuous growth of the pre-existing γ lamellae during stabilization treatment.
Evolution of intermetallic phases in an Al–Si–Ti alloy during solution treatment
A cast Al–Si–Ti alloy was solution treated at 540 °C for different periods between 0 and 72 h to understand the evolution of intermetallic phases. Only an (Al,Si) 3 Ti intermetallic phase with a low Si content was found in the as-cast alloy. The (Al,Si) 3 Ti particles were converted partly into a lamellar structure, a eutectoid phase, consisting of a Si-rich phase and an Al phase during solution treatment. The amount of the lamellar structure increased with the solution treatment time, but the composition of either constitute was kept almost unchanged regardless of the solution treatment times. The lamellar Si-rich phase is (Al,Si) 2 Ti (τ 2 ) with a TiSi 2 (C49-type) structure based on thermodynamic calculations and high-resolution TEM analyses. FCC Al phase is the product residing between the τ 2 lamellae after the completion of transformation from (Al,Si) 3 Ti to τ 2 phase. A near-rational orientation relationship (OR) between the Al and τ 2 phases is determined as Al [110]//τ 2 [100], Al ()//τ 2 [060]. The phase transformation from (Al,Si) 3 Ti to τ 2 being a result of the diffusion of Ti and Si within the original (Al,Si) 3 Ti particulates as well as the Si diffusion from the Al matrix during solution treatment is proposed. The formation of the lamellar structure in the microstructure is attributed mainly to the limited diffusivity of Ti element.
Microstructure evolution and properties of graphene nanoplatelets reinforced aluminum matrix composites
Highlights: • Lamellar structure of GNPs fibers and Al matrix was obtained in the rolling direction. • Stacking faults were observed in Al grains due to greatly increased GNPs/Al interfaces. • Strength of Al-0.2 wt% GNPs increased 36.8% with negligible electrical conductivity loss. - Abstract: Aluminum matrix composites reinforced with graphene nanoplatelets (GNPs) were prepared by continuous casting and subsequent rolling. Al-GNPs master alloy, prepared by ball milling and cold pressing, was added into Al melts to fabricate the composites. Microstructure evolution of the composites were observed using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron back scattered diffraction (EBSD). GNPs distributed uniformly in the as-cast specimen and then transformed into fibers in the rolling direction after deformation and finally a lamellar structure formed in the composites. Raman spectra showed that the structural damage of GNPs mainly came from ball milling. The interface between GNPs and Al was well combined in general while a few microcracks were observed, which reduced the ductility of the composites and no adverse aluminum carbide (Al{sub 4}C{sub 3}) was detected at the interface. Stacking faults were observed interior of the aluminum grain, which may due to the existence of plentiful interface introduced by GNPs. Fracture observation revealed that the load transferred from Al matrix to GNPs. The ultimate tensile strength of Al-0.2 wt% GNPs composites was about 36.8% higher than that of pure Al with the same casting and rolling process, which should result from the lamellar structure and load transfer, while the conductivity of the composites decreased slightly, indicating that interface scattering between Al and GNPs is very limited. The investigation results show that Al-GNPs composite is potential for high strength and high conductivity application.
In-situ X-ray scattering study of isotactic polypropylene/graphene nanocomposites under shear during fused deposition modeling 3D printing
Complementary techniques were applied to characterize the structure property relationships of FDM printed isotactic polypropylene/graphene nanocomposites. Raman spectroscopy indicated that graphene was mostly exfoliated during the nozzle extrusion process. Rheological measurements of the viscosity indicated that the presence of graphene induced shear thinning during extrusion. Azimuthal scans of wide angle x-ray scattering indicate correlated thermal fluctuations of the graphene platelets which stops abruptly at the onset of transcrystallization, or templating of the iPP chains on the graphene. X-ray microbeam SAXS analysis show the formation of ‘shish-kebab’ structures at the core of the unfilled filaments, where the ‘kebab’ component vanishes at the fiber-fiber interface enabling interdiffusion. Weak lamellar structure, and a corresponding decrease in the storage modulus are observed with the addition of 5% graphene. The lamellar structure disappears entirely with the addition of 10% graphene, while the storage modulus is decreased by nearly 50%. Thermal imaging of heat flux dissipation across molded and printed samples shows no orientational effects in pure iPP despite differences in crystal structure. Thermal conductivity increases dramatically in the samples with 10% graphene, and strong orientational effects are observed where the thermal coefficients differ by 180% between samples printed parallel or perpendicular to the heat flux.
Multilaminate Energy Storage Films from Entropy‐Driven Self‐Assembled Supramolecular Nanocomposites
Abstract Composite materials comprising polymers and inorganic nanoparticles (NPs) are promising for energy storage applications, though challenges in controlling NP dispersion often result in performance bottlenecks. Realizing nanocomposites with controlled NP locations and distributions within polymer microdomains is highly desirable for improving energy storage capabilities but is a persistent challenge, impeding the in‐depth understanding of the structure–performance relationship. In this study, a facile entropy‐driven self‐assembly approach is employed to fabricate block copolymer‐based supramolecular nanocomposite films with highly ordered lamellar structures, which are then used in electrostatic film capacitors. The oriented interfacial barriers and well‐distributed inorganic NPs within the self‐assembled multilaminate nanocomposites effectively suppress leakage current and mitigate the risk of breakdown, showing superior dielectric strength compared to their disordered counterparts. Consequently, the lamellar nanocomposite films with optimized composition exhibit high energy efficiency (>90% at 650 MV m −1 ), along with remarkable energy density and power density. Moreover, finite element simulations and statistical modeling have provided theoretical insights into the impact of the lamellar structure on electrical conduction, electric field distribution, and electrical tree propagation. This work marks a significant advancement in the design of organic–inorganic hybrids for energy storage, establishing a well‐defined correlation between microstructure and performance.