Structure Development in Polymers during Fused Filament Fabrication (FFF): An in Situ Small- and Wide-Angle X-ray Scattering Study Using Synchrotron Radiation

Microstructure formation in individual layers during fused filament fabrication (FFF) of a Π-shaped multilayer single-walled polymer sample was studied by simultaneous measurement of small- and wide-angle X-ray scattering (SAXS and WAXS, respectively) methods employing synchrotron radiation. We investigated individual layers and the welding zone between individual layers. As a model material, we used isotactic polypropylene (iPP), which is a commodity semicrystalline polymer and has a strong potential as a feedstock material for additive manufacturing. The layers were deposited by an FFF three-dimensional (3D) printer that was custom-built to fit into the synchrotron beamline. WAXS data were utilized to determine the temperature of the irradiated volume. The polymer microstructure was characterized in terms of crystallinity and long-spacing. Avrami analysis indicates that the crystallization behavior of iPP in thin layers is rather similar to that observed in quiescent crystallization of bulk iPP, suggest...

[1]  M. Avrami Kinetics of Phase Change. I General Theory , 1939 .

[2]  D. J. Blundell,et al.  The morphology of poly(aryl-ether-ether-ketone) , 1983 .

[3]  V. Varriale,et al.  Temperature dependence of the thermodynamic stability of the two crystalline α forms of isotactic polypropylene , 1990 .

[4]  Simultaneous measurements of small angle X-ray scattering, wide angle X-ray scattering and heat exchange during crystallization and melting of polymers , 1993 .

[5]  D. Lacks,et al.  Temperature Dependence of Structural and Mechanical Properties of Isotactic Polypropylene , 1995 .

[6]  J. Schultz Effect of specimen thickness on crystallization rate , 1996 .

[7]  A. Nogales,et al.  Structure Development during Shear Flow-Induced Crystallization of i-PP: In-Situ Small-Angle X-ray Scattering Study , 2000 .

[8]  B. Hsiao,et al.  Probing the Early Stages of Melt Crystallization in Polypropylene by Simultaneous Small- and Wide-Angle X-ray Scattering and Laser Light Scattering , 2000 .

[9]  T. Ezquerra,et al.  Crystallization of 2-propanol studied by neutron diffraction and dielectric spectroscopy in real-time , 2002 .

[10]  P. Olmsted,et al.  Early Stages of Crystallization in Isotactic Polypropylene , 2003 .

[11]  A. Nogales,et al.  In-Situ Simultaneous Small- and Wide-Angle X-ray Scattering Study of Poly(ether ester) during Cold Drawing , 2003 .

[12]  A. Vaughan,et al.  Anisotropic crystallization in polypropylene induced by deformation of a nucleating agent network , 2003 .

[13]  W. H. Jeu,et al.  Shear-Induced Crystallization of Poly(butylene terephthalate): A Real-Time Small-Angle X-ray Scattering Study , 2004 .

[14]  A. Nogales,et al.  Order and segmental mobility during polymer crystallization : Poly (butylene isophthalate) , 2006 .

[15]  A. Nogales,et al.  Influence of Shear on the Templated Crystallization of Poly(butylene terephthalate)/Single Wall Carbon Nanotube Nanocomposites , 2008 .

[16]  A. Hiltner,et al.  Ultra‐Small‐Angle X‐Ray Scattering Study of PET/PC Nanolayers and Comparison to AFM Results , 2008 .

[17]  G. Strobl,et al.  The Physics of Polymers , 2009 .

[18]  Hermann Seitz,et al.  A review on 3D micro-additive manufacturing technologies , 2012, The International Journal of Advanced Manufacturing Technology.

[19]  J. Rieger,et al.  Effect of processing parameters on the morphology development during extrusion of polyethylene tape : an in-line small-angle X-ray scattering (SAXS) study , 2013 .

[20]  A. Ryan,et al.  The interaction between fundamental and industrial research and experimental developments in the field of polymer crystallization , 2016 .

[21]  C. Kenel,et al.  Combined in situ synchrotron micro X-ray diffraction and high-speed imaging on rapidly heated and solidified Ti-48Al under additive manufacturing conditions , 2016 .

[22]  K. Migler,et al.  Infrared thermography of welding zones produced by polymer extrusion additive manufacturing. , 2016, Additive manufacturing.

[23]  Chelsea S Davis,et al.  Mechanical strength of welding zones produced by material extrusion additive manufacturing. , 2017, Additive manufacturing.

[24]  K. Migler,et al.  Effect of processing conditions on crystallization kinetics during materials extrusion additive manufacturing. , 2018, Polymer.

[25]  Michael F Toney,et al.  An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes. , 2018, The Review of scientific instruments.

[26]  Richard S. Graham,et al.  Modelling flow-enhanced crystallisation during fused filament fabrication of semi-crystalline polymer melts , 2018, Additive Manufacturing.

[27]  Sri Hinduja,et al.  Structural Evolution of PCL during Melt Extrusion 3D Printing , 2018 .

[28]  J. A. Sethian,et al.  Instrumentation for In situ/Operando X-ray Scattering Studies of Polymer Additive Manufacturing Processes , 2019, Synchrotron Radiation News.