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In This Article

  • Summary
  • Abstract
  • Introduction
  • Protocol
  • Representative Results
  • Discussion
  • Acknowledgements
  • Materials
  • References
  • Reprints and Permissions

Summary

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.

Abstract

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.

Introduction

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....

Protocol

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.......

Representative Results

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........

Discussion

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.......

Acknowledgements

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.

....

Materials

NameCompanyCatalog NumberComments
45 MM Toolmaker ViseTormach Inc.32547To secure substrate onto the collector
ARES-G2 RheometerTA Instruments401000.501Rheometer
Branson Ultrasonics M Series - Ultrasonic Cleaning BathFisher Scientific15-336-100To disperse nanoparticles
Cadence Science Micro-Mate Interchangeable SyringeFisher Scientific14-825-2AGlass Syringe 5mL in 1/5mL, Luer Lock Tip
Chemical hoodAny company
Corning - Disposable Pasteur Glass PipetteSigma AldrichCLS7095D5X-200EANon-Sterile
DWK Life Sciences Wheaton - Glass Scintillation VialFisher Scientific03-341-25G20 mL with cap
FEI Quanta 200 Scanning Electron Microscope (SEM)FEIFor imaging samples
Iron Oxide Nanopowder/NanoparticlesUS Research Nanomaterials, inc.US3320Fe3O4, 98%, 20-3- nm, Silicon oil Coated
KD Scientific Legato 100 Single-Syringe PumpSigma AldrichZ401358-1EASingle syringe infusion pump
Master Airbrush - Model S68TCP GlobalMAS S68Nozzle/needle diameter: 0.35 mm
Mettler Toledo AB265-S/FACT ScaleCole-Parmer ScientificEW-11333-14For weighing polymer and  Nanoparticles
N2 Gas RegulatorAny company
NanoenclosureAny company
Optical Microscopy Glass SlidesFisher Scientific12-550-A3Used as a substrate for fiber mat deposition
OSP Slotted Bob, 33 mmTA Instruments402796.902Bob, upper geometry
OSP Slotted Double Gap Cup, 34 mmTA Instruments402782.901Double wall cup, lower geometry
Oxford BenchMate Digital Vortex MixerPipetteVM-DRated up to 4,200 rpm, for mixing solutions
Oxford Benchmate Tube RollerPipetteOTR-24DRSample mixer/rotator
Polystyrene-block-polybutadiene-block-polystyreneSigma Aldrich432490-1KGstyrene 30 wt. %, Mw ~ 185,000 g/mol
SEM Pin Stub Specimen MountTed Pella Inc.1611918 mm diameter x 8 mm height
SpatulaVWR82027-532To load test materials
Tetrahydrofuran (THF)Fisher ScientificT425-1solvent, HPLC grade
TRIOSTA Instrumentsv4.3.1.39215Rheometer software

References

  1. Lee, B. L., et al. Penetration failure mechanisms of armor-grade fiber composites under impact. Journal of Composite Materials. 35 (18), 1605-1633 (2001).
  2. Prevorsek, D. C., Kwon, Y. D., Chin, H. B.

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