High fatigue resistance in a titanium alloy via near-void-free 3D printing.

The advantage of 3D printing-that is, additive manufacturing (AM) of structural materials-has been severely compromised by their disappointing fatigue properties1,2. Commonly, poor fatigue properties appear to result from the presence of microvoids induced by current printing process procedures3,4. Accordingly, the question that we pose is whether the elimination of such microvoids can provide a feasible solution for marked enhancement of the fatigue resistance of void-free AM (Net-AM) alloys. Here we successfully rebuild an approximate void-free AM microstructure in Ti-6Al-4V titanium alloy by development of a Net-AM processing technique through an understanding of the asynchronism of phase transformation and grain growth. We identify the fatigue resistance of such AM microstructures and show that they lead to a high fatigue limit of around 1 GPa, exceeding the fatigue resistance of all AM and forged titanium alloys as well as that of other metallic materials. We confirm the high fatigue resistance of Net-AM microstructures and the potential advantages of AM processing in the production of structural components with maximum fatigue strength, which is beneficial for further application of AM technologies in engineering fields.

Significance of Melt Pool Structure on the Hydrogen Embrittlement Behavior of a Selective Laser-Melted 316L Austenitic Stainless Steel.

The hydrogen embrittlement (HE) behavior of a selective laser-melted (SLM) 316L austenitic stainless steel has been investigated by hydrogen charging experiments and slow strain rate tensile tests (SSRTs) at room temperature. The results revealed that compared to the samples without H, the ultimate tensile strength (UTS) and elongation (EL) of specimens were decreased from 572 MPa to 552 MPa and from 60% to 36%, respectively, after 4 h of electrochemical hydrogenation with a current density of 100 mA/cm2. The negative effects of hydrogen charging were more pronounced on the samples' ductility than on their strength. A quasi in situ EBSD observation proved that there was little phase transformation in the samples but an increased density of low angle grain boundaries, after 4 h H charging. After strain was applied, the surface of the H-sample displayed many hydrogen-induced cracks along the melt pool boundaries (MPBs) showing that these MPBs were the preferred areas for the gathering and transferring of hydrogen.

Getting tougher in the ultracold.

Certain alloys show exceptional toughness in a liquid helium environment.

Rapid Microstructure Homogenization of a Laser Melting Deposition Additive Manufactured Ti-6.5Al-3.5Mo-1.5Zr-0.3Si Alloy by Electropulsing.

The typical microstructure of the laser melting deposition (LMD) additive-manufactured Ti-6.5Al-3.5Mo-1.5Zr-0.3Si alloy (TC11) contains the heat-affected bands (HABs), the narrow bands (NBs) and the melting pools (MPs) that formed due to the reheating and superheating effects during the layer-by-layer manufacturing process. Characterization results indicated that the coarse primary α lath (αp) and transformed ß (ßt) structures were located in the HABs, while the fine basketweave structure was formed inside the MPs. The rapid modifications of microstructure and tensile properties of the LMD-TC11 via electropulsing treatment (EPT) were investigated. The initial heterogeneous microstructure transformed into a complete basketweave structure and the HABs vanished after EPT. Thus, a more homogeneous microstructure was achieved in the EPT sample. The ultrafast microstructural changes were mainly attributed to the solid state phase transformation during electropulsing. The tensile properties of the sample were basically stable, except that the yield strength decreased as EPT voltage increased. This study suggests that EPT could be a promising method to modify the microstructure and mechanical properties of the additive-manufactured alloys in a very short time.

Optimization of Thermo-Mechanical Fatigue Life for Eutectic Al-Si Alloy by the Ultrasonic Melt Treatment.

The eutectic cast Al-Si alloys with excellent high-temperature and casting performance are widely used in engine pistons. During frequent starts and stops, the thermo-mechanical fatigue (TMF) is the most important failure cause. Ultrasonic melt treatment (UT) was chosen to compare and investigate the influence of micro-structures on fatigue life and damage mechanisms of as-cast (AC) eutectic Al-Si alloys under TMF loading. After UT, the grain size, primary Si, and intermetallic particles are reduced significantly in the alloy; fatigue life increases obviously. As a result of pilling-up of dislocations, the competitive effects of the critical strain/stress for fatigue crack nucleation can be found. There are two different crack initiation mechanisms under TMF: one is primary Si fracture for AC alloys with limited critical strain/stress for fatigue crack nucleation at fractured Si particles, and the other is primary Si debonding for UT alloys with increasing critical fracture strain/stress. After the crack initiation, the fractured or debonded primary phases provide the advantages for the further development of main cracks for both alloys. The UT alloy (805 ± 253 cycles) has about twice the TMF life of the AC alloy (403 ± 98 cycles). The refinement of micro-structures is instrumental in improving the fatigue resistance and life of TMF for the UT alloy.

Biodegradability and Cytocompatibility of 3D-Printed Mg-Ti Interpenetrating Phase Composites.

Orthopedic hybrid implants combining both titanium (Ti) and magnesium (Mg) have gained wide attraction nowadays. However, it still remains a huge challenge in the fabrication of Mg-Ti composites because of the different temperatures of Ti melting point and pure Mg volatilization point. In this study, we successfully fabricated a new Mg-Ti composite with bi-continuous interpenetrating phase architecture by infiltrating Mg melt into Ti scaffolds, which were prepared by 3D printing and subsequent acid treatment. We attempted to understand the 7-day degradation process of the Mg-Ti composite and examine the different Mg2+ concentration composite impacts on the MC3T3-E1 cells, including toxicity, morphology, apoptosis, and osteogenic activity. CCK-8 results indicated cytotoxicity and absence of the Mg-Ti composite during 7-day degradation. Moreover, the composite significantly improved the morphology, reduced the apoptosis rate, and enhanced the osteogenic activity of MC3T3-E1 cells. The favorable impacts might be attributed to the appropriate Mg2+ concentration of the extracts. The results on varying Mg2+ concentration tests indicated that Mg2+ showed no cell adverse effect under 10-mM concentration. The 8-mM group exhibited the best cell morphology, minimum apoptosis rate, and maximum osteogenic activity. This work may open a new perspective on the development and biomedical applications for Mg-Ti composites.

Cytotoxicity and Bonding Property of Bioinspired Nacre-like Ceramic-Polymer Composites.

For clinical applications, non-cytotoxicity and good bonding property of dental restorative materials are the most essential and important. The aim of this study was to evaluate the potential for clinical applications of two novel bioinspired nacre-like ceramic (yttria-stabilized zirconia)-polymer (polymethyl methacrylate) composites in terms of the cytotoxicity and bonding property. The relative growth rates (24 h) of the Lamellar and Brick-and-mortar composites measured by CCK8 were 102.93%±0.04 and 98.91%±0.03, respectively. According to the results of cytotoxicity and proliferation experiments, the two composites were not cytotoxic to human periodontal ligament fibroblasts (HPDLFs) in vitro. Both composites exhibited improved bonding strength as compared to the Control group (Vita In-Ceram YZ). As the polymer content in the composite material increases, its bonding strength also increases, which enhances the application potential of the material in the field of dental restoration. Meanwhile, by controlling the direction of loading force in the shear test, the effect of microstructure on the bonding strength of anisotropic composites was studied. After sandblasted, the bonding strengths of the Lamellar group in the longitudinal and transverse shear directions were 17.56±1.56 MPa and 18.67±1.92 MPa, respectively, while of the Brick-and-mortar group were 16.36±1.30 MPa and 16.99±1.67 MPa, respectively. The results showed that the loading direction had no significant effect on the bonding strength of the composites.

On the damage tolerance of 3-D printed Mg-Ti interpenetrating-phase composites with bioinspired architectures.

Bioinspired architectures are effective in enhancing the mechanical properties of materials, yet are difficult to construct in metallic systems. The structure-property relationships of bioinspired metallic composites also remain unclear. Here, Mg-Ti composites were fabricated by pressureless infiltrating pure Mg melt into three-dimensional (3-D) printed Ti-6Al-4V scaffolds. The result was composite materials where the constituents are continuous, mutually interpenetrated in 3-D space and exhibit specific spatial arrangements with bioinspired brick-and-mortar, Bouligand, and crossed-lamellar architectures. These architectures promote effective stress transfer, delocalize damage and arrest cracking, thereby bestowing improved strength and ductility than composites with discrete reinforcements. Additionally, they activate a series of extrinsic toughening mechanisms, including crack deflection/twist and uncracked-ligament bridging, which enable crack-tip shielding from the applied stress and lead to "Γ"-shaped rising fracture resistance R-curves. Quantitative relationships were established for the stiffness and strengths of the composites by adapting classical laminate theory to incorporate their architectural characteristics.

Local chemical fluctuation mediated ultra-sluggish martensitic transformation in high-entropy intermetallics.

Superelasticity associated with martensitic transformation has found a broad range of engineering applications, such as in low-temperature devices in the aerospace industry. Nevertheless, the narrow working temperature range and strong temperature sensitivity of the first-order phase transformation significantly hinder the usage of smart metallic components in many critical areas. Here, we scrutinized the phase transformation behavior and mechanical properties of multicomponent B2-structured intermetallic compounds. Strikingly, the (TiZrHfCuNi)83.3Co16.7 high-entropy intermetallics (HEIs) show superelasticity with high critical stress over 500 MPa, high fracture strength of over 2700 MPa, and small temperature sensitivity in a wide range of temperatures over 220 K. The complex sublattice occupation in these HEIs facilitates formation of nano-scaled local chemical fluctuation and then elastic confinement, which leads to an ultra-sluggish martensitic transformation. The thermal activation of the martensitic transformation was fully suppressed while the stress activation is severely retarded with an enhanced threshold stress over a wide temperature range. Moreover, the high configurational entropy also results in a small entropy change during phase transformation, consequently giving rise to the low temperature sensitivity of the superelasticity stress. Our findings may provide a new paradigm for the development of advanced superelastic alloys, and shed new insights into understanding of martensitic transformation in general.

An Amorphous Peri-Implant Ligament with Combined Osteointegration and Energy-Dissipation.

Progress toward developing metal implants as permanent hard-tissue substitutes requires both osteointegration to achieve load-bearing support, and energy-dissipation to prevent overload-induced bone resorption. However, in existing implants these two properties can only be achieved separately. Optimized by natural evolution, tooth-periodontal-ligaments with fiber-bundle structures can efficiently orchestrate load-bearing and energy dissipation, which make tooth-bone complexes survive extremely high occlusion loads (>300 N) for prolonged lifetimes. Here, a bioinspired peri-implant ligament with simultaneously enhanced osteointegration and energy-dissipation is presented, which is based on the periodontium-mimetic architecture of a polymer-infiltrated, amorphous, titania nanotube array. The artificial ligament not only provides exceptional osteoinductivity owing to its nanotopography and beneficial ingredients, but also produces periodontium-similar energy dissipation due to the complexity of the force transmission modes and interface sliding. The ligament increases bone-implant contact by more than 18% and simultaneously reduces the effective stress transfer from implant to peri-implant bone by ≈30% as compared to titanium implants, which as far as is known has not previously been achieved. It is anticipated that the concept of an artificial ligament will open new possibilities for developing high-performance implanted materials with increased lifespans.

Shear Band Evolution under Cyclic Loading and Fatigue Property in Metallic Glasses: A Brief Review.

The fatigue damage and fracture of metallic glasses (MGs) were reported to be dominated by shear band. While there exist several reviews about the fatigue behavior of MGs, an overview that mainly focuses on shear bands under cyclic loading is urgent, and is of great importance for the understanding of fatigue mechanisms and properties. In this review paper, based on the previous research results, the shear band evolution under cyclic loading including shear band formation, propagation and cracking, was summarized and elucidated. Furthermore, one strategy of enhancing the fatigue property through manipulating the microstructure to suppress the shear band formation was proposed. Additionally, the applications of the effect of annealing treatment and processing condition on fatigue behaviors were utilized to verify the strategy. Finally, several future directions of fatigue research in MG were presented.

Deformation-induced crystalline-to-amorphous phase transformation in a CrMnFeCoNi high-entropy alloy.

The Cantor high-entropy alloy (HEA) of CrMnFeCoNi is a solid solution with a face-centered cubic structure. While plastic deformation in this alloy is usually dominated by dislocation slip and deformation twinning, our in situ straining transmission electron microscopy (TEM) experiments reveal a crystalline-to-amorphous phase transformation in an ultrafine-grained Cantor alloy. We find that the crack-tip structural evolution involves a sequence of formation of the crystalline, lamellar, spotted, and amorphous patterns, which represent different proportions and organizations of the crystalline and amorphous phases. Such solid-state amorphization stems from both the high lattice friction and high grain boundary resistance to dislocation glide in ultrafine-grained microstructures. The resulting increase of crack-tip dislocation densities promotes the buildup of high stresses for triggering the crystalline-to-amorphous transformation. We also observe the formation of amorphous nanobridges in the crack wake. These amorphization processes dissipate strain energies, thereby providing effective toughening mechanisms for HEAs.

Wood-Inspired Cement with High Strength and Multifunctionality.

Taking lessons from nature offers an increasing promise toward improved performance in man-made materials. Here new cement materials with unidirectionally porous architectures are developed by replicating the designs of natural wood using a simplified ice-templating technique in light of the retention of ice-templated architectures by utilizing the self-hardening nature of cement. The wood-like cement exhibits higher strengths at equal densities than other porous cement-based materials along with unique multifunctional properties, including effective thermal insulation at the transverse profile, controllable water permeability along the vertical direction, and the easy adjustment to be water repulsive by hydrophobic treatment. The strengths are quantitatively interpreted by discerning the effects of differing types of pores using an equivalent element approach. The simultaneous achievement of high strength and multifunctionality makes the wood-like cement promising for applications as new building materials, and verifies the effectiveness of wood-mimetic designs in creating new high-performance materials. The simple fabrication procedure by omitting the freeze-drying treatment can also promote a better efficiency of ice-templating technique for the mass production in engineering and may be extended to other material systems.

Study on fracture of tungsten wire induced by acoustic cavitation at different hydrostatic pressures and driving electric powers.

The near-solid wall multi-bubble cavitation is an extremely complex phenomenon, and cavitation has strong erosiveness. The melting point (about 3410 °C) of tungsten is highest among all pure metals, and its hardness is also very high (its yield strength is greater than 1 GPa). What would happen to pure tungsten wire under extreme conditions caused by collapsing cavitation bubbles at high hydrostatic pressure? In this paper, we have studied the fracture process of pure tungsten wire with diameter of 0.2 mm mounted at the focus of a standing acoustic wave produced by a spherical cavity transducer with two open ends placed in a near spherical pressure container, and also studied the macro and micro morphological characteristics of the fracture and the surface damage at different fracture stages of tungsten wire under various hydrostatic pressures and driving electric powers. The results have shown that the fracture time of tungsten wire is inversely proportional to avitation intensity with hydrostatic pressure and driving electric power, the higher the acoustic pressure caused by higher electric power, the shorter the fracture time. The possible fracture mechanisms of tungsten wire in this situation we found mainly contributed to asymmetrically bubbles collapse near the surface of tungsten wire, leading to tearing the surface apart; consequently cracks along the radial and axial directions of a tungsten wire extend simultaneously, classified as trans-granular fracture and inter-granular fracture, respectively. With the increase of cavitation intensity, the cracks tend to extend more radially and the axial crack propagation path becomes shorter, that is, mainly for trans-granular fracture; with the decrease of cavitation intensity, intergranular fracture becomes more obvious. When the hydrostatic pressure was 10 MPa and the driving electric power was 2 kW, the fibers became softener due to the fracture of the tungsten wire. The fracture caused by acoustic cavitation was different from conventional mechanical fracture, such as tensile, shear, fatigue fracture, on macro and micro morphology.

3D printed Mg-NiTi interpenetrating-phase composites with high strength, damping capacity, and energy absorption efficiency.

It is of significance, but still remains a key challenge, to simultaneously enhance the strength and damping capacities in metals, as these two properties are often mutually exclusive. Here, we provide a multidesign strategy for defeating such a conflict by developing a Mg-NiTi composite with a bicontinuous interpenetrating-phase architecture through infiltration of magnesium melt into three-dimensionally printed Nitinol scaffold. The composite exhibits a unique combination of mechanical properties with improved strengths at ambient to elevated temperatures, remarkable damage tolerance, good damping capacities at differing amplitudes, and exceptional energy absorption efficiency, which is unprecedented for magnesium materials. The shape and strength after deformation can even be largely recovered by heat treatment. This study offers a new perspective for the structural and biomedical applications of magnesium.

Interfacial toughening effect of suture structures.

Suture interfaces are one of the most common architectural designs in natural material-systems and are critical for ensuring multiple functionalities by providing flexibility while maintaining connectivity. Despite intensive studies on the mechanical role of suture structures, there is still a lack of understanding on the fracture mechanics of suture interfaces in terms of their interactions with impinging cracks. Here we reveal an interfacial toughening effect of suture structures by means of "excluding" cracks away from interfaces based on a dimensionless micro-mechanical model for single-leveled and hierarchical suture interfaces with triangular-shaped suture teeth. The effective stress-intensity driving forces for crack deflection along, versus penetration through, an interface at first impingement and on subsequent kinking are formulated and compared with the corresponding resistances. Quantitative criteria are established for discerning the cracking modes and fracture resistance of suture interfaces with their dependences on sutural tooth sharpness and interfacial toughness clarified. Additionally, the effects of structural hierarchy are elucidated through a consideration of hierarchical suture interfaces with fractal-like geometries. This study may offer guidance for designing bioinspired suture structures, especially for toughening materials where interfaces are a key weakness. STATEMENT OF SIGNIFICANCE: Suture interfaces are one of the most common architectural material designs in biological systems, and are found in a wide range of species including armadillo osteoderms, boxfish armor, pangolin scales and insect cuticles. They are designed to provide flexibility while maintaining connectivity. Despite many studies on the mechanical role of suture structures, there is still little understanding of their role in terms of interactions with impinging cracks. Here we reveal an interfacial toughening effect of suture structures by means of "excluding" cracks away from interfaces based on a dimensionless micro-mechanical model for single-leveled and hierarchical suture interfaces with triangular-shaped suture teeth. Quantitative criteria are established for discerning the cracking mode and fracture resistance of the interfaces with their dependences on sutural tooth sharpness and interfacial toughness clarified.

Nature-Inspired Nacre-Like Composites Combining Human Tooth-Matching Elasticity and Hardness with Exceptional Damage Tolerance.

Making replacements for the human body similar to natural tissue offers significant advantages but remains a key challenge. This is pertinent for synthetic dental materials, which rarely reproduce the actual properties of human teeth and generally demonstrate relatively poor damage tolerance. Here new bioinspired ceramic-polymer composites with nacre-mimetic lamellar and brick-and-mortar architectures are reported, which resemble, respectively, human dentin and enamel in hardness, stiffness, and strength and exhibit exceptional fracture toughness. These composites are additionally distinguished by outstanding machinability, energy-dissipating capability under cyclic loading, and diminished abrasion to antagonist teeth. The underlying design principles and toughening mechanisms of these materials are elucidated in terms of their distinct architectures. It is demonstrated that these composites are promising candidates for dental applications, such as new-generation tooth replacements. Finally, it is believed that this notion of bioinspired design of new materials with unprecedented biologically comparable properties can be extended to a wide range of material systems for improved mechanical performance.

Adaptive structural reorientation: Developing extraordinary mechanical properties by constrained flexibility in natural materials.

Seeking strategies to enhance the overall combinations of mechanical properties is of great significance for engineering materials, but still remains a key challenge because many of these properties are often mutually exclusive. Here we reveal from the perspective of materials science and mechanics that adaptive structural reorientation during deformation, which is an operating mechanism in a wide variety of composite biological materials, functions more than being a form of passive response to allow for flexibility, but offers an effective means to simultaneously enhance rigidity, robustness, mechanical stability and damage tolerance. As such, the conflicts between different mechanical properties can be "defeated" in these composites merely by adjusting their structural orientation. The constitutive relationships are established based on the theoretical analysis to clarify the effects of structural orientation and reorientation on mechanical properties, with some of the findings validated and visualized by computational simulations. Our study is intended to give insight into the ingenious designs in natural materials that underlie their exceptional mechanical efficiency, which may provide inspiration for the development of new man-made materials with enhanced mechanical performance. STATEMENT OF SIGNIFICANCE: It is challenging to attain certain combinations of mechanical properties in man-made materials because many of these properties - for example, strength with toughness and stability with flexibility - are often mutually exclusive. Here we describe an effective solution utilized by natural materials, including wood, bone, fish scales and insect cuticle, to "defeat" such conflicts and elucidate the underlying mechanisms from the perspective of materials science and mechanics. We show that, by adaptation of their structural orientation on loading, composite biological materials are capable of developing enhanced rigidity, strength, mechanical stability and damage tolerance from constrained flexibility during deformation - combinations of attributes that are generally unobtainable in man-made systems. The design principles extracted from these biological materials present an unusual yet potent new approach to guide the development of new synthetic composites with enhanced combinations of mechanical properties.

Multiscale designs of the chitinous nanocomposite of beetle horn towards an enhanced biomechanical functionality.

Operating mainly as a type of weapon, the beetle horn develops an impressive mechanical efficiency based on chitinous materials to maximize the injury to opponent and simultaneously minimize the damage to itself and underlying brain under stringent loading conditions. Here the cephalic horn of the beetle Allomyrina dichotoma is probed using multiscale characterization combined with finite element simulations to explore the origins of its biomechanical functionality from the perspective of materials science. The horn is revealed to be highly regulated from the macroscopic shape, geometry, and connection with the body to the meso- and microscopic architecture, moisture content, and chemical and structural characteristics. Varying kinds of gradients are integrated at all length-scales. Such designs are demonstrated to benefit the mechanical performance by mitigating stress concentrations, retarding crack propagation, and modulating local properties to better adapt to stress. Enhanced rigidity, robustness and stability are additionally generated from the constrained flexibility endowed by the nanocomposite plywood structure through the reorientation of chitin nanofibrils within the proteinaceous matrix. These findings shed light on the intriguing materials-design strategies of nature in creating synergy of offence and persistence. They may even offer inspiration for the synthesis of high-performance materials and structures, in particular beams to resist bending and torsion.

Hydration-induced nano- to micro-scale self-recovery of the tooth enamel of the giant panda.

The tooth enamel of vertebrates comprises a hyper-mineralized bioceramic, but is distinguished by an exceptional durability to resist impact and wear throughout the lifetime of organisms; however, enamels exhibit a low resistance to the initiation of large-scale cracks comparable to that of geological minerals based on fracture mechanics. Here we reveal that the tooth enamel, specifically from the giant panda, is capable of developing durability through counteracting the early stage of damage by partially recovering its innate geometry and structure at nano- to micro- length-scales autonomously. Such an attribute results essentially from the unique architecture of tooth enamel, specifically the vertical alignment of nano-scale mineral fibers and micro-scale prisms within a water-responsive organic-rich matrix, and can lead to a decrease in the dimension of indent damage in enamel introduced by indentation. Hydration plays an effective role in promoting the recovery process and improving the indentation fracture toughness of enamel (by ∼73%), at a minor cost of micro-hardness (by ∼5%), as compared to the dehydrated state. The nano-scale mechanisms that are responsible for the recovery deformation, specifically the reorientation and rearrangement of mineral fragments and the inter- and intra-prismatic sliding between constituents that are closely related to the viscoelasticity of organic matrix, are examined and analyzed with respect to the structure of tooth enamel. Our study sheds new light on the strategies underlying Nature's design of durable ceramics which could be translated into man-made systems in developing high-performance ceramic materials. STATEMENT OF SIGNIFICANCE: Tooth enamel plays a critical role in the function of teeth by providing a hard surface layer to resist wear/impact throughout the lifetime of organisms; however, such enamel exhibits a remarkably low resistance to the initiation of large-scale cracks, of hundreds of micrometers or more, comparable to that of geological minerals. Here we reveal that tooth enamel, specifically that of the giant panda, is capable of partially recovering its geometry and structure to counteract the early stages of damage at nano- to micro-scale dimensions autonomously. Such an attribute results essentially from the architecture of enamel but is markedly enhanced by hydration. Our work discerns a series of mechanisms that lead to the deformation and recovery of enamel and identifies a unique source of durability in the enamel to accomplish this function. The ingenious design of tooth enamel may inspire the development of new durable ceramic materials in man-made systems.