Electrospinning is one of the leading techniques for fiber development. Still, one of the biggest challenges of the technique is to control the nanofiber morphology without many trial-and-error tests. In this study, it is demonstrated that via design of experiments (DoE), response surface methodology (RSM) and machine learning regressions (MLR) it is possible to predict the beads-on-string size, size distribution and bead density in electrospun poly(vinylidene fluoride) (PVDF) mats with a small number of tests. PVDF concentration, dimethylacetamide/acetone ratio, tip-to-collector voltage and distance were the parameters considered for the design. The results show good agreement between the experimental and modeled data. It was found that concentration and solvent ratio play the main roles in minimizing bead size and number, distance tends to reduce them, and voltage does not play a significant role. As an evaluation of the potential of the method, bead-free fibers were obtained through the predicted parameter values. Comparison of the performance of the two methods is presented for the first time in electrospinning research. Response surface methodology resulted much faster, but MLR achieved a lower error and better generalization abilities. This approach and the availability of the MLR script used in this work may help other groups implement it in their research and find information hidden in the data while improving model prediction performance.
Electrospinning allows the fabrication of polymeric nonwovens with a wide variety of inclusions in the micro-nanofibers. However, the electrospinning of microparticle-filled polymer solutions is still limited in particle size, density, and concentration, mainly due to suspension instability during the electrospinning process, so it is not commonly investigated despite the vast number of possible applications. In this study, a simple and effective novel rotation device was developed to prevent the settling of microparticles in the polymer solution during electrospinning. The stability of polyvinyl alcohol and polyvinylidene fluoride (PVDF) solutions with indium microparticles (IMPs) of (42 ± 7) μm diameter was evaluated using LASER transmittance inside a syringe, both static and rotating for 24 h. While the static suspensions completely settled at 7 min and 9 h, respectively, depending on solution viscosity, the rotating suspensions remained stable throughout the experiment. The number and distribution of IMPs in PVDF electrospun mats were determined by optic microscopy and a novel x-ray imaging mapping method, showing 165% more IMPs in the mat obtained with the rotating syringe device. A simple analysis of the theoretical background of settling and rotating suspensions was included to understand the working mechanism of the device. Also, the electrospinning of solutions with high loadings of IMPs (up to 400% w/w PVDF) was accomplished. The simplicity and outstanding efficiency of the device shown in this work may serve as a solution to technical difficulties and as an encouragement to future research in microparticle-filled solution electrospinning.
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