High-throughput measurement of elastic moduli of microfibers by rope coiling.

There are many fields where it is of interest to measure the elastic moduli of tiny fragile fibers, such as filamentous bacteria, actin filaments, DNA, carbon nanotubes, and functional microfibers. The elastic modulus is typically deduced from a sophisticated tensile test under a microscope, but the throughput is low and limited by the time-consuming and skill-intensive sample loading/unloading. Here, we demonstrate a simple microfluidic method enabling the high-throughput measurement of the elastic moduli of microfibers by rope coiling using a localized compression, where sample loading/unloading are not needed between consecutive measurements. The rope coiling phenomenon occurs spontaneously when a microfiber flows from a small channel into a wide channel. The elastic modulus is determined by measuring either the buckling length or the coiling radius. The throughput of this method, currently 3,300 fibers per hour, is a thousand times higher than that of a tensile tester. We demonstrate the feasibility of the method by testing a nonuniform fiber with axially varying elastic modulus. We also demonstrate its capability for in situ inline measurement in a microfluidic production line. We envisage that high-throughput measurements may facilitate potential applications such as screening or sorting by mechanical properties and real-time control during production of microfibers.

Soft, strong, tough, and durable protein-based fiber hydrogels.

Load-bearing soft tissues normally show J-shaped stress-strain behaviors with high compliance at low strains yet high strength at high strains. They have high water content but are still tough and durable. By contrast, naturally derived hydrogels are weak and brittle. Although hydrogels prepared from synthetic polymers can be strong and tough, they do not have the desired bioactivity for emerging biomedical applications. Here, we present a thermomechanical approach to replicate the combinational properties of soft tissues in protein-based photocrosslinkable hydrogels. As a demonstration, we create a gelatin methacryloyl fiber hydrogel with soft tissue-like mechanical properties, such as low Young's modulus (0.1 to 0.3 MPa), high strength (1.1 ± 0.2 MPa), high toughness (9,100 ± 2,200 J/m3), and high fatigue resistance (2,300 ± 500 J/m2). This hydrogel also resembles the biochemical and architectural properties of native extracellular matrix, which enables a fast formation of 3D interconnected cell meshwork inside hydrogels. The fiber architecture also regulates cellular mechanoresponse and supports cell remodeling inside hydrogels. The integration of tissue-like mechanical properties and bioactivity is highly desirable for the next-generation biomaterials and could advance emerging fields such as tissue engineering and regenerative medicine.

Ultrastretchable E-Skin Based on Conductive Hydrogel Microfibers for Wearable Sensors.

Conductive microfibers play a significant role in the flexibility, stretchability, and conductivity of electronic skin (e-skin). Currently, the fabrication of conductive microfibers suffers from either time-consuming and complex operations or is limited in complex fabrication environments. Thus, it presents a one-step method to prepare conductive hydrogel microfibers based on microfluidics for the construction of ultrastretchable e-skin. The microfibers are achieved with conductive MXene cores and hydrogel shells, which are solidified with the covalent cross-linking between sodium alginate and calcium chloride, and mechanically enhanced by the complexation reaction of poly(vinyl alcohol) and sodium hydroxide. The microfiber conductivities are tailorable by adjusting the flow rate and concentration of core and shell fluids, which is essential to more practical applications in complex scenarios. More importantly, patterned e-skin based on conductive hydrogel microfibers can be constructed by combining microfluidics with 3D printing technology. Because of the great advantages in mechanical and electrical performance of the microfibers, the achieved e-skin shows impressive stretching and sensitivity, which also demonstrate attractive application values in motion monitoring and gesture recognition. These characteristics indicate that the ultrastretchable e-skin based on conductive hydrogel microfibers has great potential for applications in health monitoring, wearable devices, and smart medicine.

Advanced 3D Electrospinning "Xspin" System: Fabrication of Bifiber Floating Oral Pharmaceutical Scaffolds for Controlled Drug Delivery.

Electrospinning has become a widely used and efficient method for manufacturing nanofibers from diverse polymers. This study introduces an advanced electrospinning technique, Xspin - a multi-functional 3D printing platform coupled with electrospinning system, integrating a customised 3D printhead, MaGIC - Multi-channeled and Guided Inner Controlling printheads. The Xspin system represents a cutting-edge fusion of electrospinning and 3D printing technologies within the realm of pharmaceutical sciences and biomaterials. This innovative platform excels in the production of novel fiber with various materials and allows for the creation of highly customized fiber structures, a capability hitherto unattainable through conventional electrospinning methodologies. By integrating the benefits of electrospinning with the precision of 3D printing, the Xspin system offers enhanced control over the scaffold morphology and drug release kinetics. Herein, we fabricated a model floating pharmaceutical dosage for the dual delivery of curcumin and ritonavir and thoroughly characterized the product. Fourier transform infrared (FTIR) spectroscopy demonstrated that curcumin chemically reacted with the polymer during the Xspin process. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) confirmed the solid-state properties of the active pharmaceutical ingredient after Xspin processing. Scanning electron microscopy (SEM) revealed the surface morphology of the Xspin-produced fibers, confirming the presence of the bifiber structure. To optimize the quality and diameter control of the electrospun fibers, a design of experiment (DoE) approach based on quality by design (QbD) principles was utilized. The bifibers expanded to approximately 10-11 times their original size after freeze-drying and effectively entrapped 87% curcumin and 84% ritonavir. In vitro release studies demonstrated that the Xspin system released 35% more ritonavir than traditional pharmaceutical pills in 2 h, with curcumin showing complete release in pH 1.2 in 5 min, simulating stomach media. Furthermore, the absorption rate of curcumin was controlled by the characteristics of the linked polymer, which enables both drugs to be absorbed at the desired time. Additionally, multivariate statistical analyses (ANOVA, pareto chart, etc.) were conducted to gain better insights and understanding of the results such as discern statistical differences among the studied groups. Overall, the Xspin system shows significant potential for manufacturing nanofiber pharmaceutical dosages with precise drug release capabilities, offering new opportunities for controlled drug delivery applications.

Exposure to bisphenol A and fiber-type microplastics induce oxidative stress and cell damage in disk abalone Haliotis discus hannai: Bioaccumulation and toxicity.

Along with environmental pollution caused by rapid economic development and industrialization, plastic waste is emerging as a global concern in relation to marine ecosystems and human health. Among the microplastics, fiber-type microfibers (MF) and bisphenol A (BPA), which are widely used as plasticizers, do not decompose well in the ocean, and tend to accumulate in organisms, generating an increased oxidative stress response. This study investigated the abalones' antioxidant and cell death responses following exposure to the environmental pollutants MF and BPA. Levels of malondialdehyde (MDA) and DNA damage increased over time, demonstrating the degree of lipid peroxidation and DNA damage in abalones exposed to individual and combined environmental conditions of MF and BPA. Compared to the single MF and BPA exposure groups, the combined exposure group showed a higher expression of antioxidant enzymes. A similar pattern was seen in the expression of the apoptosis enzyme caspase-3. Both MF and BPA caused oxidative stress and antioxidant enzymes were expressed to alleviate it, but it is believed that cell damage occurred because the stress level exceeded the allowed range.

Study on the simultaneous release of microfiber and indigo dye in denim fabric home washing.

In recent years, with the increasing global focus on environmental protection, the issue of microfiber release from denim during the washing process has gained attention. In this study, a programmable washing device simulating household drum washing was designed and developed, microfibers and indigo dyes released from denim washing were quantitatively detected, and we have also developed a novel method for estimating the release of microfibers during washing. The effects of washing time, washing temperature, and washing load on microfiber and indigo dye release from denim were explored. The results showed that the effect of washing load on microfiber and indigo dye release was greater than washing temperature and washing time. The research findings indicate that with an increase in washing time (35-95 min) and washing load (100-250 g), the shedding of microfibers and indigo dye significantly increases, reaching peak release levels of 343.6 µg/g fabric and 0.027 mg/L, respectively. However, there is a decreasing trend in the release of microfibers and indigo dye when the washing temperature exceeds 50 °C. Furthermore, our data suggests that an increase in washing load leads to a significant change in the number of microfibers (from 978 items/g fabric to 1997 items/g fabric) and their mass (from 156.87 µg/g fabric to 343.56 µg/g fabric). The influence of washing time, washing temperature, and washing load on microfiber length shows relatively small fluctuations within the range of 600-900 µm. This study provides new ideas and methods for estimating the release of microfiber and indigo dye in denim washing around the world.

Polyester Microfibers Exposure Modulates Mytilus galloprovincialis Hemolymph Microbiome.

Microplastic (MP) contamination in the aquatic environment is a cause of concern worldwide since MP can be taken up by different organisms, altering different biological functions. In particular, evidence is accumulating that MP can affect the relationship between the host and its associated microbial communities (the microbiome), with potentially negative health consequences. Synthetic microfibers (MFs) represent one of the main MPs in the marine environment, which can be accumulated by filter-feeding invertebrates, such as bivalves, with consequent negative effects and transfer through the food chain. In the mussel Mytilus galloprovincialis, polyethylene terephthalate (PET) MFs, with a size distribution resembling that of an MF released from textile washing, have been previously shown to induce multiple stress responses. In this work, in the same experimental conditions, the effects of exposure to PET-MF (96 h, 10, and 100 µg/L) on mussel hemolymph microbiome were evaluated by 16S rRNA gene amplification and sequencing. The results show that PET-MF affects the composition of bacterial communities at the phylum, family and genus level, with stronger effects at the lowest concentration tested. The relationship between MF-induced changes in hemolymph microbial communities and responses observed at the whole organism level are discussed.

Multiple Bio-Actives Loaded Gellan Gum Microfibers from Microfluidics for Wound Healing.

Wound healing, known as a fundamental healthcare issue worldwide, has been attracting great attention from researchers. Here, novel bioactive gellan gum microfibers loaded with antibacterial peptides (ABPs) and vascular endothelial growth factor (VEGF) are proposed for wound healing by using microfluidic spinning. Benefitting from the high controllability of microfluidics, bioactive microfibers with uniform morphologies are obtained. The loaded ABPs are demonstrated to effectively act on bacteria at the wound site, reducing the risk of bacterial infection. Besides, sustained release of VEGF from microfibers helps to accelerate angiogenesis and further promote wound healing. The practical value of woven bioactive microfibers is demonstrated via animal experiments, where the wound healing process is greatly facilitated because of the excellent circulation of air and nutritious substances. Featured with the above properties, it is believed that the novel bioactive gellan gum microfibers would have a remarkable effect in the field of biomedical application, especially in promoting wound healing.

Textile microfibers in wild Antarctic whelk Neobuccinum eatoni (Smith, 1875) from Terra Nova Bay (Ross Sea, Antarctica).

Antarctica has been affected directly and indirectly by human pressure for more than two centuries and recently plastic pollution has been recognized as a further potential threat for its unique biodiversity. Global long-range transport as well as local input from anthropogenic activities are potential sources of plastic pollution in both terrestrial and marine Antarctic territories. The present study evaluated the presence of microplastics in specimens of the Antarctic whelk Neobuccinum eatoni, a key species in benthic communities of the Ross Sea, one of the largest marine protected areas worldwide. To this aim, a thermo-oxidative extraction method was applied for microplastic isolation and quantification, and polymer identification was performed by manual µ-FTIR spectroscopy. Textile (semi-)synthetic or composite microfibers (length range: 0.8-5.7 mm) were found in 27.3% of whelk specimens, suggesting a low risk of bioaccumulation along Antarctic benthic food webs in the Ross Sea. Their polymer composition (of polyethylene terephthalate and cellulose-polyamide composites) matched those of outdoor technical clothing in use by the personnel of the Italian "Mario Zucchelli" station near Terra Nova Bay in the Ross Sea. Such findings indicate that sewage from base stations may act as potential local sources of textile microplastic fibers in this remote environment. More in-depth monitoring studies aiming at defining the extent of microplastic contamination related to such sources in Antarctica are encouraged.

Immobilization of biomolecular anthocyanin natural sensor into plasma-cured polyethylene terephthalate fibers from recycled plastic waste for determination of ammonia.

Polyester textiles have been applied in numerous industrial applications. Polyester fibers are characterized with being excellent insulators to electricity, having excellent flexural and impact strength, ease of manufacture, low-cost, as well as having resistance to moisture and chemicals. However, polyester fibers cannot be stained due to the absence of active dyeing sites on the surface of the fibrous structure. Thus, polyester cannot be dyed after it has been extruded. Herein, we report the development of novel-colored polyester fabrics using plasma-assisted dyeing and anthocyanin natural probe for determination of ammonia that may cause severe harmful effects to human organs and even death. Anthocyanin was extracted from red cabbage and characterized. The water-soluble anthocyanin was fastened to polyester fibers by mordant (potash alum) to generate anthocyanin-mordant coordinative complex nanoparticles. Polyester can be treated with thin layer of anthocyanin probe after activation with plasma. The results showed excellent colorfastness, ultraviolet blocking, and antibacterial performance of the anthocyanin-dyed polyester (APET) fibers. The APET fibers showed great potential for developing a portable colorimetric device for an on-site detection of ammonia. APET displayed a detection limit of aqueous ammonia in the range of 25-200 ppb, displaying a change in color from purple (542 nm) to white (387 nm).

Smart Cementitious Sensors with Nano-, Micro-, and Hybrid-Modified Reinforcement: Mechanical and Electrical Properties.

The current paper presents the results of an experimental study of carbon nano-, micro-, and hybrid-modified cementitious mortar to evaluate mechanical performance, energy absorption, electrical conductivity, and piezoresistive sensibility. Three amounts of single-walled carbon nanotubes (SWCNTs), namely 0.05 wt.%, 0.1 wt.%, 0.2 wt.%, and 0.3 wt.% of the cement mass, were used to prepare nano-modified cement-based specimens. In the microscale modification, 0.05 wt.%, 0.5 wt.%, 1.0 wt.% carbon fibers (CFs) were incorporated in the matrix. The hybrid-modified cementitious specimens were enhanced by adding optimized amounts of CFs and SWCNTs. The smartness of modified mortars, indicated by their piezoresistive behavior, was investigated by measuring the changes in electrical resistivity. The effective parameters that enhance the composites' mechanical and electrical performance are the different concentrations of reinforcement and the synergistic effect between the types of reinforcement used in the hybrid structure. Results reveal that all the strengthening types improved flexural strength, toughness, and electrical conductivity by about an order of magnitude compared to the reference specimens. Specifically, the hybrid-modified mortars presented a marginal reduction of 1.5% in compressive strength and an increase in flexural strength of 21%. The hybrid-modified mortar absorbed the most energy, 1509%, 921%, and 544% more than the reference mortar, nano-modified mortar, and micro-modified mortar, respectively. The change rate of impedance, capacitance, and resistivity in piezoresistive 28-day hybrid mortars improved the tree ratios by 289%, 324%, and 576%, respectively, for nano-modified mortars and by 64%, 93%, and 234%, respectively, for micro-modified mortars.

Microfibers in anaerobic digestion: Effect of ozone pretreatment.

Wastewater treatment plants receive significant microplastics, which are eventually discharged into the environment. Previous studies indicated that over 90% of microplastics, especially microfibers from laundry wastewater, are retained in primary sludge. The effect of microfibers from household laundry on anaerobic digestion has yet to be fully understood, which is the objective of the present study. The results in this study showed a positive correlation between methane production and the presence of microfibers. Compared to the control, the methane production increased by 2%, 27% and 43% with 20 mg/L, 100 mg/L and 1000 mg/L microfibers spiked into primary sludge, respectively. The present study suggests that microfibers at 20 mg/L insignificantly affected methane production in controlled anaerobic digestion. In contrast, ozone pretreatment of microfibers enhanced gas production by 12% in the same concentration level. Interestingly, ozone pretreatment at a higher concentration (100 mg/L-1000 mg/L) of microfibers did not affect methane production. SEM/EDX results imply that the ozone pretreatment has changed the surface characteristics of the microfibers, which provide more surface area for adsorption. The significant reduction of soluble phosphorus by 58% indicates that microfibers potentially act as a site for adsorption during anaerobic digestion. Overall, the presence of microfibers had a positive effect on anaerobic digestion. However, this work also indicated that the microfibers were not biodegraded during anaerobic digestion. Therefore, microfibers accumulate on biosolids, potentially affecting the final disposal of microfibers.

Functionally Active Microheterogeneous Systems for Elastomer Fire- and Heat-Protective Materials.

Elastomeric materials are utilized for the short-term protection of products and structures operating under extreme conditions in the aerospace, marine, and oil and gas industries. This research aims to study the influence of functionally active structures on the physical, mechanical, thermophysical, and fire- and heat-protective characteristics of elastomer compositions. The physical and mechanical properties of elastomer samples were determined using Shimazu AG-Xplus, while morphological research into microheterogeneous systems and coke structures was carried out on a scanning electronic microscope, Versa 3D. Differential thermal and thermogravimetric analyses of the samples were conducted on derivatograph Q-1500D. The presence of aluminosilicate microspheres, carbon microfibers, and a phosphor-nitrogen-organic modifier as part of the aforementioned structures contributes to the appearance of a synergetic effect, which results in an increase in the heat-protective properties of a material due to the enhancement in coke strength and intensification of material carbonization processes. The results indicate an 8-17% increase in the heating time of the unheated surface of a sample and a decrease in its linear burning speed by 6-17% compared to known analogues. In conclusion, microspheres compensate for the negative impact of microfibers on the density and thermal conductivity of a composition.

Programmable Knot Microfibers from Piezoelectric Microfluidics.

Microfibers have demonstrated significant application values in a large number of areas. Current efforts focus on developing new technologies to prepare microfibers with controllable morphological and structural features to enhance their functions. Here, a piezoelectric microfluidic platform is presented for consecutive spinning of functional microfibers with programmable spindle-knots. In this platform, a jet of a pregel-solution flowing in the channel can be subjected to a programmable piezoelectric signal and vibrates synchronously. Following a rapid polymerization of the wavy jet, microfibers with corresponding morphologies can be generated, including uniform, gradient, and symmetrical knots. Such a unique knot structure contributes to a water-collection mechanism. Thus, it has been observed that microfibers with programmed knots enable even more flexible droplet handling and active water transport. In addition, by constructing higher-order knot fiber networks, practical applications including spray reaction, lab-on-a-chip vapor detection, etc., can also be demonstrated. it is believed that this platform opens a new avenue for fiber spinning, and the programmable microfibers would be highly applicable in chemical, biomedical, and environmental areas.

Centrifugal Assembly of Helical Bijel Fibers for pH Responsive Composite Hydrogels.

In microfluidics, centrifugal forces are important for centrifugal microfluidic chips and curved microchannels. Here, an unrecognized use of the centrifugal effect in microfluidics is introduced. The assembly of helical soft matter fibers in a rotating microcapillary is investigated. During assembly, the fibers undergo phase separation, generating particle stabilized bicontinuous interfacially jammed emulsions gels. This process is accompanied by a transition of the fiber density over time. As a result, the direction of the centrifugal force in the rotating microcapillary changes. The authors analyze this effect systematically with high-speed video microscopy and complementary computer simulations. The resulting understanding enables the control of the helical fiber assembly into microropes. These microropes can be converted into pH responsive hydrogels that swell and shrink with potential applications in tissue engineering, soft robotics, controlled release, and sensing. More generally, the knowledge gained from this work shows that centrifugal forces potentially enable directed self-assembly or separation of colloids, biological cells, and emulsions in microfluidics.

Microplastic Textile Fibers Accumulate in Sand and Are Potential Sources of Micro(nano)plastic Pollution.

Agricultural soils have been identified as sinks for microplastic fibers; however, little information is available on their long-term fate in these soils. In this study, polyester and nylon fibers were precisely cut to relevant environmental lengths, using novel methodology, and their behavior in sand columns was studied at environmental concentration. The longer fibers (>50 µm) accumulated in the upper layers of the sand, smaller fibers were slightly more mobile, and nylon showed marginally higher mobility than polyester. Previous studies have overlooked changes in microplastic morphology due to transport in soil. Our study is the first to show that fibers exhibited breakage, peeling, and thinning under flow conditions in soil, releasing smaller, more mobile fragments. Furthermore, the peelings exhibited different adsorption properties compared to the core fiber. This suggests that microplastic fibers can become a source of smaller micro(nano)plastics and potential vectors for certain molecules, risking continuous contamination of nearby soils, surfaces, and groundwater.

Facile Fabrication of Anisotropic Multicompartmental Microfibers Using Charge Reversal Electrohydrodynamic Co-Jetting.

Anisotropic microstructures are utilized in various fields owing to their unique properties, such as reversible shape transitions or on-demand and sequential release of drug combinations. In this study, anisotropic multicompartmental microfibers composed of different polymers are prepared via charge reversal electrohydrodynamic (EHD) co-jetting. The combination of various polymers, such as thermoplastic polyurethane, poly(D,L-lactide-co-glycolide), poly(vinyl cinnamate), and poly(methyl methacrylate), results in microfibers with distinct compositional boundaries. Charge reversal during EHD co-jetting enables facile fabrication of multicompartmental microfibers with the desired composition and tunable inner architecture, broadening their spectrum of potential applications, such as functional microfibers and cell scaffolds with multiple physical and chemical properties.

Adsorption-desorption dynamics of synthetic and naturally weathered microfibers with toxic heavy metals and their ecological risk in an estuarine ecosystem.

Microfibers (MFs) in aquatic and marine ecosystems adsorb toxic heavy metals and then transfer the heavy metals enriched MFs to living organisms. In this research paper, the adsorption-desorption dynamics of heavy metals onto MFs was studied by using theoretical models and experimental investigations. The adsorption of metals onto MFs was well correlated for the Freundlich model and the adsorption kinetics follows pseudo-second order rate equation. The adsorption capacity of naturally weathered MFs was 30.8 mg g-1 which is about 35% higher than the synthetic fiber of similar range of size of MFs. The leaching of heavy metals from MFs was found that 90-95% of adsorbed metals were leached within 24 h. The leaching of Ti(II) and Al(III) were slower than the other metal ions. The salinity has shown decrease in adsorption capacity of MFs for heavy metals. Based on the Nemerov pollution index (PN), the naturally weathered MFs enriched with heavy metals in sediments became heavily polluted with PN values between 2.98 and 3.49. The risk index value of 396 represents that the bottom dwellers and other marine organisms in the Narmada estuary high risk from MFs and MFs enriched with metals. This study indicates that MFs play dominant role in fate and distribution of heavy metals in the estuarine ecosystems.

Low-Dimensional Palladium on Graphite-on-Paper Substrate for Hydrogen Sensing.

To stabilize the detection signal of palladium-based hydrogen sensors on paper substrates, a graphite intermediate layer was painted on the surface of paper. The graphite-on-paper (GOP) substrate offers advantages such as good thermo-electrical conductivity, low cost, and uncomplicated preparation technology. Quasi-1-dimensional palladium (Pd) thin films with 8 nm and 60 nm thicknesses were deposited on the GOP substrates using the vacuum evaporation technique. Thanks to the unique properties of the GOP substrate, a continuous Pd microfiber network structure appeared after deposition of the ultra-thin Pd film. Additionally, the sensing performance of the palladium-based hydrogen sensor was not affected, whether using GOP or paper substrate at 25 °C. Surprisingly, heating-induced loss of sensitivity was restrained due to the increased electrical conductivity of the GOP substrate at 50 °C.

Carbon Microfiber-Doped Smart Concrete Sensors for Strain Monitoring in Reinforced Concrete Structures: An Experimental Study at Various Scales.

Concrete constructions need widespread monitoring for the control of their state of integrity during their service life. In particular, after critical events such as earthquakes, this type of structure may experience the formation and development of cracks and damage. A quick and affordable assessment of structural behavior is indicated to identify conditions of danger for users and the incipient collapse of structural elements. This work presents investigations on multifunctional concretes with self-sensing capabilities to carry out static and dynamic monitoring. The materials were produced by the addition of conductive carbon microfibers to the concrete matrix. Electrical and sensing tests were carried out on samples with small-, medium-, and full-scale dimensions. The tests demonstrated the good electrical and electromechanical properties of the proposed smart concrete sensors, which appear promising for their use in civil elements or structures. In particular, tests on real-scale beams demonstrated the capability of the material to monitor the dynamic behavior of full-scale structural elements.