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Solution Blow Spinning of Polymeric Nano-Composite Fibers for Personal Protective Equipment

Published: March 18th, 2021



1Material Measurement Laboratory, National Institute of Standards and Technology, 2Theiss Research, 3Department of Chemical Engineering, Texas Tech University

The primary goal of this study is to describe a protocol to prepare polymeric fiber mats with consistent morphology via solution blow spinning (SBS). We aim to use SBS to develop novel, tunable, flexible polymeric fiber nanocomposites for various applications, including protective materials, by incorporating nanoparticles in a polymer-elastomer matrix.

Light-weight, protective armor systems typically consist of high modulus (>109 MPa) and high-strength polymeric fibers held in place with an elastic resin material (binder) to form a non-woven, unidirectional laminate. While significant efforts have focused on improving the mechanical properties of the high-strength fibers, little work has been undertaken to improve the properties of the binder materials. To improve the performance of these elastomeric polymer binders, a relatively new and simple fabrication process, known as solution blow spinning, was used. This technique is capable of producing sheets or webs of fibers with average diameters ranging from the nanoscale to the microscale. To achieve this, a solution blow spinning (SBS) apparatus has been designed and built in the laboratory to fabricate non-woven fiber mats from polymer elastomer solutions.

In this study, a commonly used binder material, a styrene-butadiene-styrene block-co-polymer dissolved in tetrahydrofuran, was used to produce nanocomposite fiber mats by adding metallic nanoparticles (NPs), such as iron oxide NPs, that were encapsulated with silicon oil and thus incorporated in the fibers formed via the SBS process. The protocol described in this work will discuss the effects of the various critical parameters involved in the SBS process, including the polymer molar mass, the selection of the thermodynamically appropriate solvent, the polymer concentration in solution, and the carrier gas pressure to assist others in performing similar experiments, as well as provide guidance to optimize the configuration of the experimental setup. The structural integrity and morphology of the resultant non-woven fiber mats were examined using scanning electron microscopy (SEM) and elemental X-ray analysis via energy-dispersive X-ray spectroscopy (EDS). The goal of this study is to evaluate the effects of the various experimental parameters and material selections to optimize the structure and morphology of the SBS fiber mats.

Many light-weight, ballistic, protective armor systems are currently constructed using high-modulus and high-strength polymeric fibers, such as oriented, ultra-high molar mass polyethylene fibers or aramids, which provide outstanding ballistic resistance1,2. These fibers are used in combination with an elastic resin material (binder) that can penetrate to the filament level and secure the fibers in a 0°/90° configuration to form a non-woven, unidirectional laminate. The percentage of the polymer elastomer resin (binder) should not exceed 13% of the total weight of the unidirectional laminate to maint....

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NOTE: Details related to the equipment, instrumentation, and chemicals used in this section can be found in the Table of Materials. This entire protocol should first be reviewed and approved by the institutional safety department/personnel to ensure procedures and processes specific to the institution are adhered to.

1. Preparation of polymer solution using the appropriate solvent

NOTE: Consult manufacturer/supplier safety data sheets and the institut.......

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In this study, non-woven fiber mats consisting of poly(styrene-butadiene-styrene) fibers in the nano- and micro-scale, were synthesized with and without the presence of iron oxide NPs. To form fibers, the SBS parameters must be carefully selected for the polymer/solvent system used. The molar mass of the dissolved polymer and the solution concentration are critical in controlling the morphology of the structures produced by the SBS process. In this study, a poly(styrene-butadiene-styrene) block-co-polymer (styrene 30 wt........

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The method described herein provides a protocol for producing polymer elastomer nanocomposite fiber mats via a relatively new technique known as solution blow spinning. This technique allows the fabrication of fibers in the nanoscale and has several advantages over other well-established techniques, such as the electrospinning process, as it can be carried out under atmospheric pressure and room temperature27. Furthermore, SBS is not highly susceptible to local environmental changes (temperature o.......

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The authors would like to acknowledge Mr. Dwight D. Barry for his important contributions for fabrication of the solution blow spinning apparatus. Zois Tsinas and Ran Tao would like to acknowledge funding from the National Institute of Standards and Technology under Awards # 70NANB20H007 and # 70NANB15H112, respectively.


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Name Company Catalog Number Comments
45 MM Toolmaker Vise Tormach Inc. 32547 To secure substrate onto the collector
ARES-G2 Rheometer TA Instruments 401000.501 Rheometer
Branson Ultrasonics M Series - Ultrasonic Cleaning Bath Fisher Scientific 15-336-100 To disperse nanoparticles
Cadence Science Micro-Mate Interchangeable Syringe Fisher Scientific 14-825-2A Glass Syringe 5mL in 1/5mL, Luer Lock Tip
Chemical hood Any company
Corning - Disposable Pasteur Glass Pipette Sigma Aldrich CLS7095D5X-200EA Non-Sterile
DWK Life Sciences Wheaton - Glass Scintillation Vial Fisher Scientific 03-341-25G 20 mL with cap
FEI Quanta 200 Scanning Electron Microscope (SEM) FEI For imaging samples
Iron Oxide Nanopowder/Nanoparticles US Research Nanomaterials, inc. US3320 Fe3O4, 98%, 20-3- nm, Silicon oil Coated
KD Scientific Legato 100 Single-Syringe Pump Sigma Aldrich Z401358-1EA Single syringe infusion pump
Master Airbrush - Model S68 TCP Global MAS S68 Nozzle/needle diameter: 0.35 mm
Mettler Toledo AB265-S/FACT Scale Cole-Parmer Scientific EW-11333-14 For weighing polymer and  Nanoparticles
N2 Gas Regulator Any company
Nanoenclosure Any company
Optical Microscopy Glass Slides Fisher Scientific 12-550-A3 Used as a substrate for fiber mat deposition
OSP Slotted Bob, 33 mm TA Instruments 402796.902 Bob, upper geometry
OSP Slotted Double Gap Cup, 34 mm TA Instruments 402782.901 Double wall cup, lower geometry
Oxford BenchMate Digital Vortex Mixer Pipette VM-D Rated up to 4,200 rpm, for mixing solutions
Oxford Benchmate Tube Roller Pipette OTR-24DR Sample mixer/rotator
Polystyrene-block-polybutadiene-block-polystyrene Sigma Aldrich 432490-1KG styrene 30 wt. %, Mw ~ 185,000 g/mol
SEM Pin Stub Specimen Mount Ted Pella Inc. 16119 18 mm diameter x 8 mm height
Spatula VWR 82027-532 To load test materials
Tetrahydrofuran (THF) Fisher Scientific T425-1 solvent, HPLC grade
TRIOS TA Instruments v4.3.1.39215 Rheometer software

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