Fibrous Microstructure Research Articles

Impact of hydrothermal aging on microstructure transformation in Poly(L‐lactide) nonwovens under tension in condition close to a living organism

AbstractThe analysis of mechanical properties and structure of bioresorbable polymer nonwoven materials is an important area of research in the medical industry, the properties and structure of which directly affect the processes of cellular activity. In this work, the processes of reorganization of the fibrous microstructure of poly(l‐lactide) nonwoven materials under uniaxial tension in a water environment were investigated. The study which included volumetric ultrasound imaging, mechanical testing, differential scanning calorimetry, X‐ray diffraction, and melting rate measurements was the first attempt to identify correlations between the mechanical behavior of fibrous meshes and changes in the supramolecular structure of the polymer during 3 months of hydrothermal aging T = 37°C. An increase in crystallinity by 4%, a shift of glass transition temperature by 4°C, and a 2 times increase in melt flow rate under hydrolysis were indicated degradation of the amorphous phase. Local degradation of the amorphous phase of fibers led to the formation of surface cracks, an increase in the number of microcracks during hydrothermal aging resulted in a decrease in the mobility of fibers in the volume of the nonwoven material and a decrease in the elasticity of the entire nonwoven material, which was revealed using the volume ultrasound imaging and optical microphotographs.

Deep learning based segmentation of binder and fibers in gas diffusion layers

Gas diffusion layers (GDLs) are vital parts for the performance of proton-exchange membrane fuel cells (PEMFCs). In many cases, they are made of Carbon-Carbon Composite Paper (CCCP), which consists of carbon fibers and a carbonized binder material. The distribution of the fibers and binder in the GDL strongly influences the performance of a PEMFC. Synchrotron scans are a great way to obtain information about the microstructural composition of carbon paper GDLs (Figure 2), but there is one major obstacle. Binder and fibers tend to have the same attenuation and, consequently, the same gray values in the scans. To overcome this, we introduce a machine learning-based method that segments fibers and binder from the local morphology of a CCCP. The training data is generated using FiberGeo, a module in the GeoDict software for fibrous microstructure generation. FiberGeo creates fibers based on stochastic geometry and adds binder using morphological opening and closing operations. We applied the machine learning-based method to four Scans of samples of Toray Carbon Paper with varying amounts of binder in them. The result is the quantification of individual voxels as fiber or binder material that can be used, for example, in performance simulations of property simulations in PEMFCs [1–4]. Here, we focus on the differences in the spatial distribution of the binder both in the through-plane and in-plane directions.

Overcoming the intrinsic brittleness of high-strength Al2O3–GdAlO3 ceramics through refined eutectic microstructure

High-strength ceramic materials are known for their exceptional mechanical properties; however, they are often plagued by brittleness, limiting their applications. Because of the inherent difficulty of dislocation glide and multiplication in ceramics, efforts to overcome the brittleness of ceramics by activating plastic deformation have faced challenges. This work demonstrates that Al2O3–GdAlO3 (Gadolinium Aluminum Perovskite: GAP) eutectic micropillars with submicron-scale fibrous microstructures exhibit remarkable plastic deformability. They displayed engineering plastic strains of up to 5% even at 25 °C, while the micropillars of Al2O3 or GAP single crystals exhibited brittle fracture similar to conventional high-strength ceramics. The plasticity in Al2O3–GAP eutectic was attributed to the activation of primary prismatic slip and secondary basal slip in the Al2O3 phase, which is typically considered inactive at room temperature. These findings suggest that plastic deformability can be achieved in high-strength ceramic materials by fabricating refined eutectic microstructures.

Bioinspired Glycopeptide Hydrogel Reestablishing Bone Homeostasis through Mediating Osteoclasts and Osteogenesis in Periodontitis Treatment.

Irreversible alveolar bone resorption is one of the important clinical manifestations of periodontitis, which is initiated by a plaque biofilm and exacerbated by the imbalance of osteoclast activity and osteogenesis, affecting a patient's masticatory function and resulting in a high recurrence rate of periodontitis. Herein, to reestablish bone homeostasis in periodontitis, a minocycline hydrochloride (MH)-loaded glycopeptide hydrogel (MH/GRWgel) is fabricated to mediate alveolar bone absorption through sequential antibacterial and RANKL-blocking activities. GRWgel shows an ECM-like fibrous and porous microstructure serving as a scaffold for cell proliferation and differentiation and holds the merits including injectability, self-healing properties, and good biocompatibility. After injection in situ, MH is released rapidly from the hydrogel in the early stage, demonstrating a potent antimicrobial effect to combat the biofilm in the deep periodontal pocket. Moreover, MH/GRWgel exhibits a high specific binding efficiency with RANKL to suppress osteoclast maturation by shielding the RANKL/RANK interaction and enhancing osteogenic differentiation, thereby synergistically regulating bone homeostasis. In the rat periodontitis model, MH/GRWgel significantly curtails periodontitis progression through antimicrobial activity, inhibition of alveolar bone resorption, and promotion of bone regeneration, which is superior to the treatment of a commercial gel. These findings suggest that MH/GRWgel with superiority in regulating bone homeostasis provides a promising therapeutic strategy for periodontitis.

Textural improvement of pea protein-based high-moisture extrudates with corn zein and rice starch

High moisture extrusion allows the production of plant protein-based products, including meat analogues. Building upon our previous findings showing that zein mixed with rice starch provides the necessary textural properties to formulations, different pea protein-based formulations with varying amounts of zein and rice starch or wheat gluten (as control) were produced using high moisture extrusion and the rheological, textural, and microstructural characteristics were evaluated and associated with the secondary structure of proteins. Samples containing wheat gluten presented desirable rheological and mechanical properties in terms of texturization, which was evidenced by the generation of a layered and three-dimensional viscoelastic network. The addition of rice starch to zein significantly increased the viscoelasticity of the samples due to enhanced development of non-covalent interactions that led to higher and more stable β-sheets content and to the formation of a fibrous and layered microstructure and a 3D network nearly like those obtained with gluten. The sole replacement of pea protein by zein was not enough to develop these desired characteristics, demonstrating the importance of the non-covalent interactions between rice starch and zein for the generation of these properties. Overall, zein and rice starch improved texturization of pea protein-based gluten-free analogues made by high moisture extrusion.

Co-axially electrospun Li-rich layered Oxide@Spinel core-shell heterostructure nanofibers for enhanced stability and electrochemical performance

Lithium-rich layered oxides (LLO) possessing high specific capacity has the limitation of voltage fade, poor high C-rate performance and low conductivity. Spinel coating on LLO surface is known to mitigate the voltage fade, however, enabling high C-rate performance remains challenging. In this study, LLO nanofiber core with composition 0.6Li2MnO3·0.4LiMn0.25Ni0.38Co0.37O2 is prepared by electrospinning process and the same is coated with spinel LiMn1.5Ni0.5O4 shell to obtain LLO/spinel (LLO/S) core-shell heterostructure. The spinel shell coating is accomplished (i) by a novel co-axial (CA) electrospinning process and (ii) by wet chemical (WC) approach. The CA electrospinning process provides a uniform core-shell structure compared to the WC process. The electron microscopy studies reveal the fibrous microstructure in LLO/S heterostructures with energy dispersive spectroscopy compositional mapping showing the spinel composition on the surface. Higher concentration (>10 wt.%) of spinel coating are shown to break the fibers into particulates. X-ray diffraction and high-resolution transmission electron microscopy analysis confirm the spinel structure formation along with layered structure. While the capacity is slightly compromised compared to the pristine LLO nanofiber, the LLO/S heterostructure with 10 wt.% spinel coating exhibits a high reversible capacity of 268 mAhg-1 with minimal capacity loss during the 1st cycle (with coulombic efficiency 83.5%) and an excellent high C-rate capability (88 mAhg-1 at 10C-rate and 55 mAhg-1 at 20C-rate). The electrochemical studies also demonstrate the importance of optimal spinel content in the coating and the method of spinel coating on the layered material surface. The encapsulation of LLO with spinel layer which has 3D-diffusion pathways for Li-ion transport facilitates high ionic and electronic conductivity and hence leads to enhanced electrochemical performance of LLO/S heterostructured cathodes.

Cellulose reinforcement of plant-based protein hydrogels: Effects of cellulose nanofibers and nanocrystals on physicochemical properties

This study explored the impact of cellulose-derived fillers, cellulose nanofibers (CNFs) and cellulose nanocrystals (CNCs), on the microstructure and texture of potato protein hydrogels (20 wt% protein). Particle size analysis, surface charge analysis, and molecular docking simulations suggested that the cellulose nanofibers and nanocrystals acted as inactive fillers within the potato protein matrix. Texture profile analysis showed that incorporation of small amounts of CNFs (<1%) increased the gel strength (by up to 69%), but the addition of larger amounts decreased it, which was attributed to disruption of the protein network by aggregated nanofibers at higher concentrations. The incorporation of CNCs had a much smaller effect on the gel strength of the potato protein hydrogels, only increasing it by up to 15% at 2% CNC. Shearing the cellulose-reinforced hydrogels in a shear rheometer had little impact on their gel strength at lower filler concentrations (<2 wt%) but increased it at higher concentrations. Microscopy analysis showed that the cellulose fibers could be aligned at sufficiently high shearing rates, leading to a fibrous microstructure. This study provides valuable insights into the optimization of the properties of cellulose fillers for application in plant protein hydrogels. In particular, it suggests that they may be utilized in plant-based meat analogs to enhance their textural attributes and optimize their appearance.

A facile electrospinning strategy to prepare cost-effective carbon fibers as a self-supporting anode for lithium-ion batteries

Carbon materials with fibrous morphology and enhanced mechanical properties have shown to be promising materials as self-supporting anode materials for lithium-ion batteries (LIBs). In this study, coal-based carbon fibers (CFs) with favorable flexibility and superior tensile strength were prepared from lignite and coal derivatives such as coal-based humic acid and coal tar pitch via electrospinning in the assistance of polyacrylonitrile. All these coal-based CFs have an 1D dense fibrous microstructure with controllable diameter and appreciable specific surface area with enriched in O/N-containing groups by rationally choosing the precursor type. The organic macromolecules enriched aromatic ring in lignite and coal derivatives cross-link with linear polyacrylonitrile molecular chains to form a more solid three-dimensional (3D) network framework under the conditions of electrospinning and carbonization. Such 3D microstructure not only can significantly improve the flexibility and tensile strength of coal-based CFs, but also can increase the content of graphite-like microcrystalline carbon (sp2 carbon) in carbon fibers, thereby improving the electrical conductivity. Due to the smaller molecular structure, coal tar pitch can be more easily combined with polyacrylonitrile by electrostatic force. The CFs derived from coal tar pitch (CTP-CFs) exhibited the largest average diameter (156.2 nm), a higher microporous surface area (2.6 m2·g−1), higher pyrrole nitrogen and contained reasonable proportions of amorphous carbon (sp3 carbon) and sp2 carbon. As a consequence, among the various derived coal-based CFs applied as self-supporting anode materials for LIBs, CTP-CFs showed the highest first reversible capacity (770.8 mAh·g−1 at 20 mA·g−1) and excellent cycling performance with capacity retention rate of 89.1 % after 200 cycles. This work paves a new strategy to prepare CFs as flexible self-supporting anodes for LIBs from low-cost carbon precursors that can be rationally chosen to further tune the property of the CFs.

A Coarse Grained Molecular Dynamics Model for the Simulation of Lubricating Greases

The rheological properties of lubricating greases are determined by the viscosity of the base oil, the interaction between base oil and thickener, and the interaction between thickener particles. The contribution of the oil–thickener interactions to the viscosity is well known, but the contribution of the thickener–thickener interactions has not yet been studied by employing theoretical or computational frameworks. In this paper, we use coarse-grained molecular dynamics to simulate a fibrous microstructure, and we show that the experimentally observed viscoelastic/plastic behaviour can be well reproduced. A parametric study shows that the apparent viscosity increases with increasing fibre length, fibre stiffness and thickener concentration. This is as expected, showing that this modelling approach is useful to study effects on grease rheology that are not accessible experimentally, such as impact of fibre entanglement or agglomeration.

Amorphous carbon derived from daily carbon ink for wide detection range, low-cost, eco-friendly and flexible pressure sensor

Flexible pressure sensor has important applications in wearable electronic system. However, most reported flexible pressure sensors still face problems such as expensive raw materials, complex preparation processes, and narrow pressure detection ranges. Inspired by low-cost daily carbon ink and filter paper, a flexible pressure sensor is designed and fabricated using a simple dip-coating method. The proposed pressure sensor consists of two filter papers coated with carbon ink as sensitive layers, fabric conductive tapes as flexible electrodes, and polyimide tape as packaging layer. The filter paper has a fibrous microstructure, which is beneficial for improving the pressure sensing performance of the pressure sensor. The main component of carbon ink is amorphous carbon, which has a moderate conductivity. The results indicate that the pressure sensor exhibits wide detection range (0.1–100 kPa), high sensitivity of 0.627 kPa−1 (0.1–15 kPa), short response/recovery times (230 ms/290 ms) and good durability (4000 cycles at 50 kPa). In addition, the pressure sensor can be used for physiological and motion monitoring, such as pulse and step count. This work provides an optional strategy for developing wide detection range, low-cost, eco-friendly and flexible pressure sensor.

Constructing sandwich-like microstructure based on multi-nanofibers to accelerate proton conduction at subzero temperature

The well-ordered microstructure has been demonstrated to accelerate the proton conduction process through reducing proton conduction resistance. In this research, the proton exchange membranes (PEMs) with sandwich-like microstructure have been constructed based on Kevlar nanofibers and bifunctional nanofibers of chitosan (CS) with polyvinyl alcohol (PVA). The CS/PVA bifunctional nanofibers (CPNF) layer has been prepared with electrospinning process, which is stably adhered to the Kevlar nanofibers layer owing to compatible interfacial property. The fine structure stability without layer separation is achieved even with phosphoric acid (PA) molecules doping in the prepared PA doped composite membranes. The fibrous microstructure accelerats proton conduction through regulating proton conduction pathways. The objective of accelerating proton conduction at subzero temperature has been realized, reflecting in high and stable proton conductivities. For instance, the (Kevlar/CPNF/Kevlar)/PA membrane exhibits proton conductivities of 9.75 × 10−3 S/cm at −30 °C and 8.22 × 10−2 S/cm at 30 °C. Most importantly, the fine proton conductivity stability is identified by the results of the cycle test and long-term test. Specifically, the proton conductivities are respectively 8.62 × 10−3 S/cm at −30 °C and 8.07 × 10−2 S/cm at 30 °C after a five heating/cooling cycle process. The proton conductivities remain 2.97 × 10−2 S/cm at −25 °C and 7.19 × 10−2 S/cm at 30 °C after a 1032 h non-stop test. Additionally, the single proton exchange membrane fuel cell with the (Kevlar/CPNF/Kevlar)/PA membrane exhibits the peak power densities of 279.5 mW/cm2 at 100 °C and 352.7 mW/cm2 at 130 °C.

Efficient hydrolysis of cellulose into sugars in aqueous systems using fibrous core-shell structure FS@C/HPW

Phosphotungstic acid hydrate (HPW)-doped hydroxyl-rich hydrothermal carbon-coated fibrous silica catalyst (FS@C/HPW) is fabricated to induce the highly efficient hydrolysis of cellulose to sugar in an ultra-low acid aqueous system. The obtained FS90@C/HPW12 owns good thermal stability under 200 °C and the highest specific surface area at 28 m2/g. Owing to its special fibrous microstructures, FS90@C/HPW12 can cause linear damage and structural fragmentation on the surface of cellulose during hydrolysis. Accordingly, rather highly efficient hydrolysis with the cellulose conversion of 100 %, total reducing sugar and glucose yields at 92.2 % and over 85 % is achieved in the aqueous system with FS90@C/HPW12 and 5 mmol/L H2SO4. FS90@C/HPW12 also exhibits good reusability in multiple hydrolysis. This research provides a particular way for the design and synthesis of solid catalysts to induce the highly efficient hydrolysis of cellulose to sugar by chemical catalysis in a full aqueous system.

Study on anisotropy orientation due to well-ordered fibrous biological microstructures.

Most biological fibrous tissues have anisotropic optical characteristics, which originate from scattering by their fibrous microstructures and birefringence of biological macromolecules. The orientation-related anisotropic interpretation is of great value in biological tissue characterization and pathological diagnosis. We focus on intrinsic birefringence and form birefringence in biological tissue samples. By observing and comparing the forward Mueller matrix of typical samples, we can understand the interpretation ability of orientation-related polarization parameters and further distinguish the sources and trends of anisotropy in tissues. For glass fiber, silk fiber, skeletal muscle, and tendon, we construct a forward measuring device to obtain the Mueller matrix image and calculate the anisotropic parameters related to orientation. The statistical analysis method based on polar coordinates can effectively analyze the difference in anisotropic parameters. For those birefringent fibers, the statistical distribution of fast-axis values derived from Mueller matrix polar decomposition was found to exhibit bimodal characteristics, which is a key point in distinguishing the single-layer birefringent fiber sample from a layered, multioriented fibrous sample. The application conditions and interference factors of anisotropic orientation parameters are analyzed. Based on the parameters extracted from the orientation bimodal distribution, we can evaluate the relative change trend of intrinsic birefringence and form birefringence in anisotropic samples. The cross-vertical bimodal distribution of the fast axis of anisotropic fibers is beneficial to accurately analyze the anisotropic changes in biological tissues. The results imply the potential of anisotropic orientation analysis for applications in pathological diagnosis.

COMBINING MAGNETICALLY ASSISTED AND MATRIX-ASSISTED 3D BIOPRINTING FOR ANISOTROPIC TISSUE ENGINEERING

A major obstacle in biofabrication is replicating the organization of the extracellular matrix and cellular patterns found in anisotropic tissues within bioengineered constructs. While magnetically-assisted 3D bioprinting techniques have the potential to create scaffolds that mimic natural biological structures, they currently lack the ability to accurately control the dispersion of magnetic substances within the bioinks without compromising the fidelity of the intended composite. To overcome this dichotomy, the concepts of magnetically- and matrix-assisted 3D bioprinting are combined here. This method preserves the resolution of printed structures by keeping low viscosity bioinks uncrosslinked during printing, which allows for the arrangement of magnetically-responsive microfibers without compromising the structural integrity of the design. Solidification is induced after the microfibers are arranged in the desired pattern. Furthermore, the precise design of these magnetic microfillers permits the utilization of low levels of inorganic materials and weak magnetic field strengths, which reduces the potential risks that may be associated with their use. The effectiveness of this approach is evaluated in the context of tendon tissue engineering, and the results demonstrate that combining the tendons like anisotropic fibrous microstructure with remote magneto-mechanical stimulation during in vitro maturation provides both biochemical and biophysical cues that effectively guide human adipose-derived stem cells towards a tenogenic phenotype In summary, the developed strategy allows the fabrication of anisotropic high-resolution magnetic composites with remote stimulation functionalities, opening new horizons for tissue engineering applications.Acknowledgments: ERC Grant CoG MagTendon nr 772817, BioChips PoC project nr 10106930, (PD/BD/129403/2017), (CEECIND/01375/2017), (2020.03410.CEECIND), (2022.05526.PTDC), (ED481B2019/025).

Influence of Coconut Fiber Waste and Rice Husk Ash on Green Concrete

Purpose: To develop cementitious materials, concrete, incorporating coconut fiber waste (CFW) and rice husk ash (RHA), with the aim of producing innovative, cost-effective, and readily available products for use in economically and environmentally friendly construction applications. Environmental impacts can be minimized by making these practices efficient and sustainable through the utilization of these waste materials. Theoretical framework: The use of agro-industrial waste in concrete matrices has been extensively studied due to their effectiveness in influencing material properties. The incorporation of coconut fiber waste and rice husk ash into concrete can lead to improvements in compressive strength, increased durability, and a reduction in the amount of CO2 generated during production. The concrete developed with the incorporation of waste products has the potential to minimize environmental impacts, reduce costs, and extend its lifespan. The pursuit of sustainability drives the exploration of innovative materials to preserve natural resources and mitigate ecological impact in the construction industry. Method: The coconut fiber waste was subjected to 24-hour drying process in an oven at 100°C to remove moisture and was subsequently crushed in a ball mill until its particle size exhibited characteristics similar to the binder. The CFW and RHA were characterized through Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), and Specific Surface Area analysis. Different percentages of CFW (0.25% - 0.75%) and RHA (2% - 10%) were separately incorporated into the concrete mix. The mixing ratio used was 1:1.9:3.1 (cement, sand, aggregate), with a water-to-cement (w/c) ratio of 0.60. Workability tests, electrical resistivity tests, capillary water absorption by capillary rise, and axial compressive strength tests were conducted. Additionally, a sulfate ion penetration test was performed by immersing specimens in a 2.5% sulfuric acid (H2SO4) solution for 7 days. Results: SEM images of CFW reveal an angular and fibrous microstructure, maintaining the original properties of the waste even after its transformation into ash. RHA particles exhibit irregular shapes and sizes with microporous cellular structures on the surface, consistent with literature. X-Ray Diffraction patterns of CFW indicate a material without a distinct crystalline structure. However, Electron Dispersive Spectroscopy analysis suggests the predominance of carbon (C), potassium oxide (K2O), and silica (SiO2). RHA shows broad amorphous diffraction at 22° and some sharp diffraction peaks, suggesting the formation of crystallites, consistent with cristobalite. There was a slight improvement in the workability of fresh concrete compared to the reference mix as the percentage of waste incorporation increased. The electrical resistivity of the produced specimens showed a significant increase in all cases, except for the 0.25% RHA sample. The 5.0% CFW content exhibited the best performance, with a 29.47% increase, indicating a microstructure with few voids and suggesting greater material durability. Samples with higher fiber percentages showed higher water absorption values. Concrete incorporated with RHA exhibited higher porosity and suboptimal performance. However, the incorporation of 0.25% CFW showed a slight improvement compared to the reference concrete. The best performances observed in the compressive strength test were with 5.0% RHA and 0.5% CFW, with the latter showing the best result compared to the reference specimens. In the sulfate attack test, only the concrete with 5.0% RHA showed better performance in an aggressive environment. Increasing the percentage of CFW also reduced mass loss, suggesting potential improvement of the compound at higher proportions. The study demonstrated that agro-industrial residues can be satisfactorily utilized in construction, and the implementation of this new process can reduce global warming and mineral resource depletion. Research implications: This work contributes to a sustainable circular economy with a novel process for utilizing agro-industrial waste in concrete. Originality/Value: The findings will be promising for the utilization of coconut fiber waste and rice husk ash in the production of environmentally sustainable concrete.

Advanced Synthetic Scaffolds Based on 1D Inorganic Micro-/Nanomaterials for Bone Regeneration.

Inorganic nanoparticulate biomaterials, such as calcium phosphate and bioglass particles, with chemical compositions similar to that of the inorganic component of natural bone, and hence having excellent biocompatibility and bioactivity, are widely used for the fabrication of synthetic bone graft substitutes. Growing evidence suggests that structurally anisotropic, or 1D inorganic micro-/nanobiomaterials are superior to inorganic nanoparticulate biomaterials in the context of mechanical reinforcement and construction of self-supporting 3D network structures. Therefore, in the past decades, efforts have been devoted to developing advanced synthetic scaffolds for bone regeneration using 1D micro-/nanobiomaterials as building blocks. These scaffolds feature extraordinary physical and biological properties, such as enhanced mechanical properties, super elasticity, multiscale hierarchical architecture, extracellular matrix-like fibrous microstructure, and desirable biocompatibility and bioactivity, etc. In this review, an overview of recent progress in the development of advanced scaffolds for bone regeneration is provided based on 1D inorganic micro-/nanobiomaterials with a focus on their structural design, mechanical properties, and bioactivity. The promising perspectives for future research directions are also highlighted.

Developing a ternary conductive hydrogel of polyacrylamide, polyaniline, and carbon nanotube: A potential chemiresistive gas sensor

Over the past few years, conductive hydrogels have received increasing attention for numerous electronic applications because of the concurrent provision of electrical conductivity, flexibility, and conformability. In the present study, a polyaniline-based conductive hydrogel was synthesized. Carbon nanotubes (CNTs) were associated with the hydrogel to impart higher electrical conductivity to the hydrogel, and ternary composites of polyacrylamide (PAM), polyaniline (PANI), and CNT were developed. To fulfill this, at first, CNT surface was decorated with carboxyl functionalities, and the carboxyl decorated CNT was included into the composition in two manners: firstly, CNTs were included during acrylamide polymerization, whereas in the second manner, CNTs were incorporated during aniline polymerization. The composite hydrogels' chemical, swelling, morphological, and electrical properties were evaluated. The experimental results corroborated that in the latter case, abundant intermolecular interactions were developed between the PANI chains and the CNT surface. Moreover, the swelling value was increased by 9% comapred to the former case. In the former case, a porous microstructure and in the latter case a fibrous microstructure was dominated. And more importantly, the electrical conductivity of the hydrogel in the latter case was 104 folds higher than that in the former case. The ternary composition prepared with the latter manner was employed for sensing the ammonia gas, and the analyses unveiled that the hydrogel represents an appropriate response in the range of 10.43%–16.87% to various concentrations of the target gas and has the potential to be a thriving chemiresistive gas sensor.

Versatile fiber-reinforced hydrogels to mimic the microstructure and mechanics of human vocal-fold upper layers

Human vocal folds are remarkable soft laryngeal structures that enable phonation due to their unique vibro-mechanical performances. These properties are tied to their specific fibrous architecture, especially in the upper layers, which comprise a gel-like composite called lamina propria. The lamina propria can withstand large and reversible deformations under various multiaxial loadings. Despite their importance, the relationships between the microstructure of vocal folds and their resulting macroscopic properties remain poorly understood. There is a need for versatile models that encompass their structural complexity while mimicking their mechanical features. In this study, we present a candidate model inspired by histological measurements of the upper layers of human vocal folds. Bi-photonic observations were used to quantify the distribution, orientation, width, and volume fraction of collagen and elastin fibers between histological layers. Using established biomaterials, polymer fiber-reinforced hydrogels were developed to replicate the fibrillar network and ground substance of native vocal fold tissue. To achieve this, jet-sprayed poly(ε-caprolactone) fibrillar mats were successfully impregnated with poly(L-lysine) dendrimers/polyethylene glycol hydrogels. The resulting composites exhibited versatile structural, physical and mechanical properties that could be customized through variations in the chemical formulation of their hydrogel matrix, the microstructural architecture of their fibrous networks (i.e., fiber diameter, orientation and volume fraction) and their assembly process. By mimicking the collagen network of the lamina propria with polymer fibers and the elastin/ground substance with the hydrogel composition, we successfully replicated the non-linear, anisotropic, and viscoelastic mechanical behavior of the vocal-fold upper layers, accounting for inter/intra-individual variations. The development of this mimetic model offers promising avenues for a better understanding of the complex mechanisms involved in voice production. Statement of significanceHuman vocal folds are outstanding vibrating soft living tissues allowing phonation. Simple physical models that take into account the histological structure of the vocal fold and recapitulate its mechanical features are scarce. As a result, the relations between tissue components, organisation and vibro-mechanical performances still remain an open question. We describe here the development and the characterization of fiber-reinforced hydrogels inspired from the vocal-fold microstructure. These systems are able to reproduce the mechanics of vocal-fold tissues upon realistic cyclic and large strains under various multi-axial loadings, thus providing a mimetic model to further understand the impact of the fibrous network microstructure in phonation.

Highly sensitive piezoresistive and thermally responsive fibrous networks from the in situ growth of PEDOT on MWCNT-decorated electrospun PU fibers for pressure and temperature sensing

Flexible electronics have demonstrated various strategies to enhance the sensory ability for tactile perception and wearable physiological monitoring. Fibrous microstructures have attracted much interest because of their excellent mechanical properties and fabricability. Herein, a structurally robust fibrous mat was first fabricated by electrospinning, followed by a sequential process of functionalization utilizing ultrasonication treatment and in situ polymerization growth. Electrospun polyurethane (PU) microfibers were anchored with multi-walled carbon nanotubes (MWCNTs) to form conductive paths along each fiber by a scalable ultrasonic cavitation treatment in an MWCNT suspension. After, a layer of poly(3,4-ethylene dioxythiophene) (PEDOT) was grown on the surface of PU fibers decorated with MWCNTs to enhance the conductive conjunctions of MWCNTs. Due to the superior electromechanical behaviors and mechanical reinforcement of PEDOT, the PEDOT/MWCNT@PU mat-based device exhibits a wide working range (0–70 kPa), high sensitivity (1.6 kPa−1), and good mechanical robustness (over 18,000 cycles). The PEDOT/MWCNT@PU mat-based sensor also demonstrates a good linear response to different temperature variations because of the thermoelectricity of the PEDOT/MWCNT composite. This novel strategy for the fabrication of multifunctional fibrous mats provides a promising opportunity for future applications for high-performance wearable devices.

Microstructure and activation volume of a Cu-6 wt %Zn brass processed by equal channel angular pressing

The generation of a high density of twins few tens nanometers in size can enhance both strength and ductility. The present work aims to produce highly twinned microstructure in Cu-6 wt % Zn alloy of a moderate stacking fault energy (SFE) by equal channel angular pressing (ECAP) using a die with angles ϕ= 110° and Ψ = 0. X ray diffraction (XRD) shows that a high density of defects is stored up to 2 passes then a recovery takes place. EBSD imaging reveals a high density of twins and a fibrous microstructure. Grains close to 100 nm in size are formed. Strain rate sensitivity (SRS) was investigated in compression and nanoindentation (NI). Compression curves show that deformation occurs by slipping with a contribution of twins to hardening. A high contribution of shear bands was revealed during ECAP and compression tests. The activation volume V* in compression and NI is in the range 70b3 - 100b3, consistent with the emission of dislocations from grain boundaries and twin boundaries The experimental values of V* were compared to those expected from defect densities.