Morphology Of Nanofibers Research Articles

Radiation synthesized carboxyl-functionalized covalent organic framework adsorbent for efficient heavy metal decontamination

Carboxyl groups exhibit great potential in the field of heavy metal decontamination due to their good coordination ability. In this work, acrylic acid was grafted onto covalent organic framework (COF) by using a γ-ray radiation grafting approach. A carboxyl-functionalized adsorbent designated AA-TbDa-COF with high performance for multiple heavy metal removal was obtained. Infrared spectroscopy and thermogravimetric analysis proved the successful carboxyl modification. The porous nanofiber morphology and high accessibility of carboxyl functional groups give the resultant AA-TbDa-COF ultra-fast adsorption kinetics. The capacity for Pb2+, Cd2+ and Cu2+ decontamination was 127.9, 60.6 and 39.8 mg/g, respectively. The preparation of functional COFs by radiation method is extended to the field of heavy metal treatment, proving the great potential of radiation-prepared materials in environmental governance.

Optimization of electrospinning process parameters to develop the smallest ZnO + PVP nanofibres using Taguchi experimental design and ANOVA

Electrospinning is a well-known and straightforward technique for creating nanofibres from various materials, such as metals, ceramics, and polymers. The process takes place in a strong electric field, causing the polymer solution to stretch, resulting in micro/nanoscale fibres. The process parameters of electrospinning influence the morphology of nanofibres. In the present study, zinc oxide (ZnO) nanofibres were created in a polyvinylpyrrolidone (PVP) polymer combining electrospinning and sol–gel methods. To measure the effects of electrospinning and sol–gel on the diameter of ZnO + PVP nanofibres, a Taguchi design of experiment (DoE) approach was adopted, which comprised the “PVP concentrations, flow rate, needle tip-to-collector distances, and applied voltage”. S/N ratio, orthogonal L9 arrays with Taguchi design, and variance analysis. Several trials and investigations are planned using ANOVA to observe the best circumstances for synthesising ZnO + PVP. In DoE studies, it was analysed that the PVP concentration is the most crucial determinant of the nanofibre diameter, followed by flow rate. For electro-spun ZnO + PVP nanofibres, an optimal combination was also identified to produce the lowest diameters with the least variance. Interaction plot values were also recommended for experimentation with good interaction and a further selection of parameter values.

Introducing non-conjugated ionic spacer in metallo-supramolecular polymer: Generation of nanofibers for high-performance electrochromic supercapacitor

The use of indicative electrochromic (EC) supercapatteries is gaining significant attention for their ability to indicate their charging and discharging status through optical color changes and their high energy and power densities, making them a promising renewable alternative energy source. In this study, we performed molecular engineering to prepare a non-conjugated pyridinium cation-containing bisterpyridine ligand (TpyNTpy) and its metallo-supramolecular polymer (MSP), Fe-TpyNTpy. The MSP was thoroughly characterized through spectroscopic, morphological, and structural studies, revealing a homogeneous nanofiber morphology with good thermal stability. The gel-state EC devices, fabricated using Fe-TpyNTpy as the active layer, demonstrated EC color changes from purple to dirty white, with a large optical contrast of 47% at 570 nm, fast coloration (1.5 s) and bleaching (2.4 s) times, high coloration efficiency of 312.8 cm2C-1, longer optical memory, and extremely high EC cycle stability. Incorporating nonconjugated and ionic ligands helped address the opposite electrochemical behaviors, such as EC fastness and optical memory. The Fe-TpyNTpy film showed good supercapacitive properties in solution electrolytes, and the energy storage behavior was correlated with EC transmittance/color change. The energy storage properties were evaluated by preparing a hybrid ESD. The Fe-TpyNTpy and Prussian blue containing hybrid ESD exhibited an improved volumetric capacitance of 73 ± 2F/cm3 with low iR drop, high energy storage capacity (energy density 61 mWh/cm3 at a power density of 8.5 W/cm3), and 95% retention of initial volumetric capacitance after 10,000 charge–discharge cycles. The hybrid ESD can illuminate a single LED, demonstrating the practical applicability of the ESD.

Phase separation patterned films of natural materials: Preparation of mixed monolayers of nanocellulose integrates and organo‐modified nanoclays

AbstractMixed monolayers of cellulose acetate and organo‐modified montmorillonite were prepared on a water surface, and their morphologies and structures were evaluated. Cellulose acetate exhibited an integrated morphology of cellulose nanofibers. A mixed monolayer of nanocellulose and organo‐modified montmorillonite was found to be a phase‐separated system in the surface pressure‐area isotherm analysis. The surface morphology of the mixed film formed a patterned surface in which clay nanoparticles and nanofibers coexisted. As the cellulose acetate ratio in the mixed film increased, the size of the clay nanoparticles decreased. The surface free energy of the mixed film was intermediate between those of the two components; however, it showed the most hydrophilic characteristic by being wettable by water. The layered structure of the mixed films showed a longer spacing value than that of the organo‐modified nanoclay film, indicating a change in orientation. In contrast, the in‐plane order was amorphous, and no improvement in periodicity or crystallinity was observed even after annealing. In addition, the clay part of the phase‐separated film exhibited selective molecular adsorption ability, and it was possible to form adsorbent patterns.

Preparation and Characterization of Porous Cellulose Acetate Nanofiber Hydrogels.

The currently reported methods for preparing cellulose acetate hydrogels use chemical reagents as cross-linking agents, and the prepared ones are non-porous structured cellulose acetate hydrogels. Nonporous cellulose acetate hydrogels limit the range of applications, such as limiting cell attachment and nutrient delivery in tissue engineering. This research creatively proposed a facile method to prepare cellulose acetate hydrogels with porous structures. Water was added to the cellulose acetate-acetone solution as an anti-solvent to induce the phase separation of the cellulose acetate-acetone solution to obtain a physical gel with a network structure, where the cellulose acetate molecules undergo re-arrangement during the replacement of acetone by water to obtain hydrogels. The SEM and BET test results showed that the hydrogels are relatively porous. The maximum pore size of the cellulose acetate hydrogel is 380 nm, and the specific surface area reaches 62 m2/g. The porosity of the hydrogel is significantly higher than that of the cellulose acetate hydrogel reported in the previous literature. The XRD results show that the nanofibrous morphology of cellulose acetate hydrogels is caused by the deacetylation reaction of cellulose acetate.

Electrospun biopolymer polyvinyl alcohol/Centella asiatica extract nanofibers for antibacterial activity

Nonwoven mats of electrospun fibers have great potential for use in antibacterial activity, especially wound dressing. Our goal is to fabricate electrospun biopolymer nanofibers from polyvinyl alcohol (PVA)/Centella asiatica (CA) as potential wound dressings using the electrospinning technique. CA extracts were loaded into the biopolymer nanofibers with different contents (0, 1, 3, 5 and 7 %w/v). Field emission scanning electron microscopy (FE-SEM) was used to examine the morphology of the biopolymer nanofibers. FE-SEM micrographs revealed the biopolymer fibers to be round and smooth, with average diameters ranging from 100 to 450 nm. The mechanical properties of the biopolymer nanofibers decreased as the concentration of CA extract increased, and the antibacterial activity assays of the biopolymer nanofibers with the addition of CA extract were inhibition zone of 7 –15 mm for all bacteria, indicating their potential use as wound dressing materials.

Preparation and Characterization of Polycaprolactone (PCL) Antimicrobial Wound Dressing Loaded with Pomegranate Peel Extract.

In recent years, medicinal plant extracts have received remarkable attention due to their wound-healing properties. In this study, polycaprolactone (PCL) electrospun nanofiber membranes incorporated with different concentrations of pomegranate peel extract (PPE) were prepared. The results of the SEM and FTIR experiments demonstrated that the morphology of nanofiber is smooth, fine, and bead-free, and the PPE was well introduced into the nanofiber membranes. Moreover, the outcomes of the mechanical property tests demonstrated that the nanofiber membrane made of PCL and loaded with PPE exhibited remarkable mechanical characteristics, indicating that it could fulfill the essential mechanical requisites for wound dressings. The findings of the in vitro drug release investigations indicated that PPE was instantly released within 20 h and subsequently released gradually over an extended period by the composite nanofiber membranes. Meanwhile, the DPPH radical scavenging test confirmed that the nanofiber membranes loaded with PPE exhibited significant antioxidant properties. Antimicrobial experiments showed higher PPE loading, and the nanofiber membranes showed higher antimicrobial activity against Staphylococcus aureus, Escherichia coli, and Candida albicans. The results of the cellular experiments showed that the composite nanofiber membranes were nontoxic and promoted the proliferation of L929 cells. In summary, electrospun nanofiber membranes loaded with PPE can be used as a wound dressing.

Using the Rods as Collector and Study of its Effect on Morphology and Uniformity of Nanofibers via Electrospinning

Nanotechnology research has lacked to provide new studies on nanofibers using the electrospinning method, the reasons are attributed that all parameters have been covered by previous studies. Believing that science is in a state of constant renewal leads to the possibility to study a parameter that has not been studied before, which affects the morphology of nanofibers. One of the disadvantages of nanofibers manufacturing is the formation of beads, and controlling the parameter helps reduce these beads. Field emission scanning electron microscope (FESEM) images reveal the formation of nanofibers and surface topography observations by atom force microscopy (AFM) indicates that the roughness is improved by changing the distance between rods of the collector. The rods function as a collector for nanofibers, changing this parameter improves the morphology and diameter of the nanofibers.

Hydrothermally reinforcing hydroxyaptatite and bioactive glass on carbon nanofiber scafold for bone tissue engineering.

As a bone tissue engineering scaffold, the objective of this study was to design hierarchical bioceramics based on an electrospun composite of carbon nanofibers (CNF) reinforced with hydroxyapatite (HA) and bioactive glasses (BGs) nanoparticles. The performance of the nanofiber as a scaffold for bone tissue engineering was enhanced by reinforcing it with hydroxyapatite and bioactive glass nanoparticles through a hydrothermal process. The influence of HA and BGs on the morphology and biological properties of carbon nanofibers was examined. The prepared materials were evaluated for cytotoxicity in vitro using the water-soluble tetrazolium salt assay (WST-assay) on Osteoblast-like (MG-63) cells, and oste-ocalcin (OCN), alkaline phosphatase (ALP) activity, total calcium, total protein, and tar-trate-resistant acid phosphatase (TRAcP) were measured. The WST-1, OCN, TRAcP, total calcium, total protein, and ALP activity tests demonstrated that scaffolds reinforced with HA and BGs had excellent in vitro biocompatibility (cell viability and proliferation) and were suitable for repairing damaged bone by stimulating bioactivity and biomarkers of bone cell formation.

Development of Cissus quadrangularis-Loaded POSS-Reinforced Chitosan-Based Bilayer Sponges for Wound Healing Applications: Drug Release and In Vitro Bioactivity.

Nowadays, antibiotic-loaded biomaterials have been widely used in wound healing applications. However, the use of natural extracts has come into prominence as an alternative to these antimicrobial agents in the recent period. Among natural sources, Cissus quadrangularis (CQ) herbal extract is used for treatment of bone and skin diseases in ayurvedic medicine due to its antibacterial and anti-inflammatory effects. In this study, chitosan-based bilayer wound dressings were fabricated with electrospinning and freeze-drying techniques. CQ extract-loaded chitosan nanofibers were coated on chitosan/POSS nanocomposite sponges using an electrospinning method. The bilayer sponge is designed to treat exudate wounds while mimicking the layered structure of skin tissue. Bilayer wound dressings were investigated with regard to the morphology and physical and mechanical properties. In addition, CQ release from bilayer wound dressings and in vitro bioactivity studies were performed to determine the effect of POSS nanoparticles and CQ extract loading on NIH/3T3 and HS2 cells. The morphology of nanofibers was investigated with SEM analysis. Physical characteristics of bilayer wound dressings were determined with FT-IR analysis, swelling study, open porosity determination, and mechanical test. The antimicrobial activity of CQ extract released from bilayer sponges was investigated with a disc diffusion method. Bilayer wound dressings' in vitro bioactivity was examined using cytotoxicity determination, wound healing assay, proliferation, and the secretion of biomarkers for skin tissue regeneration. The nanofiber layer diameter was obtained in the range of 77.9-97.4 nm. The water vapor permeability of the bilayer dressing was obtained as 4021 to 4609 g/m2day, as it is in the ideal range for wound repair. The release of the CQ extract over 4 days reached 78-80% cumulative release. The release media were found to be antibacterial against Gram-negative and Gram-positive bacteria. In vitro studies showed that both CQ extract and POSS incorporation induced cell proliferation as well as wound healing activity and collagen deposition. As a result, CQ-loaded bilayer CHI-POSS nanocomposites were found as a potential candidate for wound healing applications.

Scalable fabrication of silver covered polyurethane nanofibers as flexible SERS nanosensors for aflatoxin detection

Flexible surface enhanced Raman spectroscopy (SERS) nanosensors, constructed by integration of plasmonic nanostructures with polymeric substrates, have received increasing research interests for recent decades. When compared to abundant works on optimization of the plasmonic nanostructures, the research involving the influence of polymeric substrates on analytical performance of resultant flexible SESR nanosensors is unexpectedly limited. Herein, the ultra-thin silver layer has been deposited on the electrospun polyurethane (ePU) nanofibrous membranes via vacuum evaporation to prepare the flexible SRES nanosensors. Interestingly, we find that the molecular weight and polydispersion index of synthesized PU play important roles in regulating the fine morphology of electrospun nanofibers, which in turns determine the Raman enhancement of resultant flexible SERS nanosensors. Specifically, the optimized SERS nanosensor, obtained by evaporating 10 nm silver layer on top of nanofibers derived from electrospinning of PU with a weight-average molecular weight of 140,354 and polydispersion index of 1.26, enables label-free detection of the carcinogen of aflatoxin down to 0.1 nM. Thanks to its scalable fabrication and good sensitivity, the current work opens new way for design of cost-effective flexible SERS nanosensors for environmental monitoring and food security applications.

Production and characterization of zinc oxide nanofibers derived from waste material as precursor

The emergence of industrial wastes brings with it a series of global environment issues. However, using these wastes including valuable metals as a source of value-added materials will lead to many advantages. The metals can be recovered and transformed for nanomaterial production which offers utility in many applications such as energy conversion and hydrogen evaluation. In this study, recycling techniques were used to synthesize zinc oxide nanofibers from waste brass flue dust. Initially, characterization and experimental analyses were used to confirm the synthesized nanofibers phase purity, morphology, and optical properties. The X-Ray diffraction (XRD) analysis and X-ray photoelectron spectroscopy (XPS) confirmed the nanofibers produced after recycling process were predominantly ZnO and have high purity. It was determined from scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis that the produced samples were in fiber form in nanoscale and high crystallinity. According to the ultraviolet visible spectroscopy (UV-Vis) analysis, the optical band of ZnO nanofibers was found as 3.19 eV. It has been demonstrated with this study that the ZnO nanofibers derived from industrial waste can be used in several energy applications. Also, it was revealed that metal-containing wastes can be disposed of by producing value-added nanomaterials directly from industrial wastes with economical value.

Influence of nano-fibrous and nano-particulate morphology on the rate capability of Li3V2(PO4)3/C Li-ion battery cathode

We demonstrate contrasting differences in the electrochemical performances of Li3V2(PO4)3 with thin-carbon coating (LVP/C) in the nanoparticulate (LVP/C-np) and nanofibrous (LVP/C-nf) morphologies synthesized by a sol-gel and electrospinning processes, respectively. LVP/C-nf exhibits a highly-interconnected pearl-like microstructure, and LVP/C-np has discontinuous aggregates of nanoparticles, as evidenced by high-resolution scanning and transmission electron microscopy. Electrochemical studies show that the nanoparticle cathodes exhibit higher capacity fading than nanofibrous cathodes with increasing C-rate. LVP/C-np and LVP/C-nf cathodes exhibit a discharge capacity of 137 mA h g−1 and 124 mA h g−1 at 0.1 C rate. Large carbon content in LVP/C-nf (∼23.3%) unlike the LVP/C-np (∼2.5%) underestimates the actual capacity. The high C-rate performance is better for LVP/C-nf (58.74 mA h g−1 at 10C-rate and 28.75 mA h g−1 at 30 C-rate) compared to LVP/C-np (37.23 mA h g−1 at 10C-rate) as tested in the voltage range 3 V-4.8 V. The most prominent observation is that LVP/C-np cathodes show lower capacity retention of only 48.6%. In contrast, the cathodes with nanofibrous morphology retain nearly 77.2% of their initial discharge capacities after 500 cycles at 1C-rate. Present study highlights the importance of the well-connected microstructure of the cathode as an essential criterion to achieve the high-rate capability and long cycling stability of high voltage cathodes for quick charge battery applications.

Deep eutectic solvent PCL-based nanofibers as drug delivery system

Polycaprolactone nanofibers can be promising drug delivery systems. The current study aims to prepare ibuprofen containing polycaprolactone based nanofibrous systems as sustained-release drug delivery systems. Two deep eutectic solvents (choline chloride/acetic acid and choline chloride/glycerine) were used as additive in the electrospinning processes. The morphology of resulted beads-free nanofibers was confirmed through scanning electron microscopy.The ibuprofen adsorption and desorption were investigated using UV-VIS spectrophotometry. The release mechanism of the model drug in vitro was studied through different release kinetic models. Based on the obtained results, the drug release is mostly diffusion controlled. The DES did not affect the adsorption and desorption characteristics, but changes the nanofibers morphology, modifying the strong hydrophobic nature of PCL.

Fabric-like Electrospun PVAc-Graphene Nanofiber Webs as Wearable and Degradable Piezocapacitive Sensors.

Flexible piezocapacitive sensors utilizing nanomaterial-polymer composite-based nanofibrous membranes offer an attractive alternative to more traditional piezoelectric and piezoresistive wearable sensors owing to their ultralow powered nature, fast response, low hysteresis, and insensitivity to temperature change. In this work, we propose a facile method of fabricating electrospun graphene-dispersed PVAc nanofibrous membrane-based piezocapacitive sensors for applications in IoT-enabled wearables and human physiological function monitoring. A series of electrical and material characterization experiments were conducted on both the pristine and graphene-dispersed PVAc nanofibers to understand the effect of graphene addition on nanofiber morphology, dielectric response, and pressure sensing performance. Dynamic uniaxial pressure sensing performance evaluation tests were conducted on the pristine and graphene-loaded PVAc nanofibrous membrane-based sensors for understanding the effect of two-dimensional (2D) nanofiller addition on pressure sensing performance. A marked increase in the dielectric constant and pressure sensing performance was observed for graphene-loaded spin coated membrane and nanofiber webs respectively, and subsequently the micro dipole formation model was invoked to explain the nanofiller-induced dielectric constant enhancement. The robustness and reliability of the sensor have been underscored by conducting accelerated lifetime assessment experiments entailing at least 3000 cycles of periodic tactile force loading. A series of tests involving human physiological parameter monitoring were conducted to underscore the applicability of the proposed sensor for IoT-enabled personalized health care, soft robotics, and next-generation prosthetic devices. Finally, the easy degradability of the sensing elements is demonstrated to emphasize their suitability for transient electronics applications.

Formulation and Characterization of Electrospun Nanofibers for Melatonin Ocular Delivery.

The poor ocular bioavailability of melatonin (MEL) limits the therapeutic action the molecule could exert in the treatment of ocular diseases. To date, no study has explored the use of nanofiber-based inserts to prolong ocular surface contact time and improve MEL delivery. Here, the electrospinning technique was proposed to prepare poly (vinyl alcohol) (PVA) and poly (lactic acid) (PLA) nanofiber inserts. Both nanofibers were produced with different concentrations of MEL and with or without the addition of Tween® 80. Nanofibers morphology was evaluated by scanning electron microscopy. Thermal and spectroscopic analyses were performed to characterize the state of MEL in the scaffolds. MEL release profiles were observed under simulated physiological conditions (pH 7.4, 37 °C). The swelling behavior was evaluated by a gravimetric method. The results confirmed that submicron-sized nanofibrous structures were obtained with MEL in the amorphous state. Different MEL release rates were achieved depending on the nature of the polymer. Fast (20 min) and complete release was observed for the PVA-based samples, unlike the PLA polymer, which provided slow and controlled MEL release. The addition of Tween® 80 affected the swelling properties of the fibrous structures. Overall, the results suggest that membranes could be an attractive vehicle as a potential alternative to liquid formulations for ocular administration of MEL.

Template-free synthesis of M/g-C3N4 (M = Cu, Mn, and Fe) porous one-dimensional nanostructures for green hydrogen production

Herein, we synthesized porous one-dimensional graphitic carbon nitride (g-C3N4) doped atomically with metal atoms (M/g-C3N4) (M = Cu, Mn, and Fe) for the electrochemical and photo-electrochemical hydrogen evolution reaction (HER). This is driven by the direct acidification of an aqueous solution of metal precursors and melamine followed by pyrolysis at 550 °C under N2. The as-obtained M/g-C3N4 had well-defined pore sizes (5–10 nm), nanofibers (90 ± 5 nm in width and 5 ± 1 μm in length) morphology, high surface area, and M atomic contents (1.7 ± 0.2 wt.%). The HER performance is in the order of Cu/g-C3N4 > Fe/g-C3N4 > Mn/g-C3N4 in terms of the overpotential, onset potential, H2 production rate, and mass/specific activity. Notably, Cu/g-C3N4 achieved turnover frequency (TOF) close to that of commercial 10 wt.% Pt/C, but higher mass/specific activity and great H2 production rate of (222.15 μmol· g−1·h−1). This work open the doorway for the utilization of g-C3N4 doped metal-atoms at low content in electrocatalytic and photocatalytic HER.

A feruloyl esterase/cellulase integrated biological system for high-efficiency and toxic-chemical free isolation of tobacco based cellulose nanofibers

Tobacco based cellulose nanofiber (TCNF) is a novel nanocellulose that has recently been used to replace undesirable wood pulp fibers in the preparation of reconstructed tobacco sheets (RTS). However, given the strict requirements for controlling toxic chemical content in tobacco products, there is a global interest in developing a green, efficient, and toxic-chemical free approach to isolate TCNF from tobacco stem as a bioresource. In this study, we propose a creative and environmentally friendly method to efficiently and safely isolate TCNF from tobacco stem pulp, which involves integrated biological pretreatment followed by a facile mechanical defibrillation process. Feruloyl esterase is used to pretreat the stem pulp by disrupting the ether and ester bonds between lignin and polysaccharide carbohydrates within the fiber wall, which effectively facilitates cellulase hydrolysis and swelling of the stem pulp fiber, as well as the following mechanical shearing treatment for TCNF isolation. The results demonstrate that TCNF obtained by the comprehensive feruloyl esterase/cellulase/mechanical process exhibit uniform and well-dispersed nanofiber morphology, higher crystallinity, and stronger mechanical properties than those of the control. The addition of 0.5 % TCNF can replace wood pulp by 18 wt% ~ 25 wt% in the production of RTS samples while maintaining their reasonable strength properties.

High-Speed Centrifugal Spinning Polymer Slip Mechanism and PEO/PVA Composite Fiber Preparation.

Composite nanofibers with excellent physical and chemical properties are widely used in new energy, biomedical, environmental, electronic, and other fields. Their preparation methods have been investigated extensively by many experts. High-speed centrifugal spinning is a novel method used to fabricate composite nanofibers. The slip mechanism of polymer solution flows is an important factor affecting the morphology and quality of composite nanofibers prepared by high-speed centrifugal spinning. As the polymer solution flows, the liquid wall slip occurs inside the nozzle, followed by liquid-liquid interface slip and gas-liquid interface slip. The factors affecting polymer slip were investigated by developing a mathematical model in the nozzle. This suggests that the magnitude of the velocity is an important factor that affects polymer slip and determines fiber quality and morphology. Under the same rotational speed, the smaller the nozzle diameter, the greater the concentration of velocity distribution and the smaller the diameter of the produced composite nanofibers. Finally, PEO/PVA composite nanofibers were prepared using high-speed centrifugal spinning equipment at 900-5000 rpm and nozzle diameters of 0.2 mm, 0.4 mm, 0.6 mm, and 0.8 mm. The morphology and quality of the collected PEO/PVA composite nanofibers were analyzed using scanning electron microscopy (SEM) and TG experiments. Then, the optimal parameters for the preparation of PEO/PVA composite nanofibers by high-speed centrifugal spinning were obtained by combining the external environmental factors in the preparation process. Theoretical evaluation and experimental data were provided for the centrifugal composite spinning slip mechanism and for the preparation of composite nanofibers.

Fabrication of highly dispersed bimetallic Ni-Mo@CNFs by sol–gel assisted electrospinning for methanol oxidation electrocatalysis

The development of efficient electrocatalysts using low-cost nanostructured transition metals as an alternative to noble metals is receiving strong interest in the field of clean and sustainable energy technology. In this study, highly dispersed bimetallic nickel-molybdenum nanoparticles on electrospun carbon nanofibers (Ni-Mo/CNFs) were prepared using a sol-gel-assisted electrospinning technique followed by calcination. The chemical composition of the Ni-Mo/CNFs with different ratios of Mo and their morphology have been characterized by various techniques. The SEM and TEM images revealed that the Ni0.6Mo0.4/CNFs had a nanofibrous morphology, the Ni-Mo nanoparticles were highly dispersed over carbon nanofibers, and the average particle size was 9.02 nm. The Mo ratio plays a crucial role in enhancing the electrochemical performance, and Ni0.6Mo0.4/CNFs showed higher electrocatalytic activity than other samples. The maximum current density of Ni0.6Mo0.4/CNFs was 10 and 43.89 mA/cm2 for the methanol oxidation at 0.45 and 0.75 V vs. Ag/AgCl, respectively, and the onset potential was 0.31 V. The synergistic effect between Ni and Mo NPs and the morphology and structure of substrate (CNFs) were responsible for its electrochemical performance.