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Title: In-situ X-ray scattering study of isotactic polypropylene/graphene nanocomposites under shear during fused deposition modeling 3D printing

Journal Article · · Composites Science and Technology
 [1];  [1];  [1];  [1];  [2];  [3];  [3];  [1];  [1];  [4];  [1];  [1]
  1. Stony Brook Univ., NY (United States)
  2. Argonne National Lab. (ANL), Argonne, IL (United States)
  3. Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
  4. Hebrew Univ. of Jerusalem (Israel)

Complementary techniques were applied to characterize the structure property relationships of FDM printed isotactic polypropylene/graphene nanocomposites. Raman spectroscopy indicated that graphene was mostly exfoliated during the nozzle extrusion process. Rheological measurements of the viscosity indicated that the presence of graphene induced shear thinning during extrusion. Azimuthal scans of wide angle x-ray scattering indicate correlated thermal fluctuations of the graphene platelets which stops abruptly at the onset of transcrystallization, or templating of the iPP chains on the graphene. X-ray microbeam SAXS analysis show the formation of ‘shish-kebab’ structures at the core of the unfilled filaments, where the ‘kebab’ component vanishes at the fiber-fiber interface enabling interdiffusion. Weak lamellar structure, and a corresponding decrease in the storage modulus are observed with the addition of 5% graphene. The lamellar structure disappears entirely with the addition of 10% graphene, while the storage modulus is decreased by nearly 50%. Thermal imaging of heat flux dissipation across molded and printed samples shows no orientational effects in pure iPP despite differences in crystal structure. Thermal conductivity increases dramatically in the samples with 10% graphene, and strong orientational effects are observed where the thermal coefficients differ by 180% between samples printed parallel or perpendicular to the heat flux.

Research Organization:
Brookhaven National Lab. (BNL), Upton, NY (United States); AArgonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES); National Science Foundation (NSF); Casali Foundation Israel
Grant/Contract Number:
SC0012704; AC02-06CH11357
OSTI ID:
1643999
Alternate ID(s):
OSTI ID: 1774535; OSTI ID: 1777571
Report Number(s):
BNL-216194-2020-JAAM
Journal Information:
Composites Science and Technology, Vol. 196; ISSN 0266-3538
Publisher:
ElsevierCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 23 works
Citation information provided by
Web of Science

References (38)

Anisotropic material properties of fused deposition modeling ABS journal October 2002
Disentanglement effects on welding behaviour of polymer melts during the fused-filament-fabrication method for additive manufacturing journal August 2017
Weld formation during material extrusion additive manufacturing journal January 2017
Alignments and network of graphite fillers to improve thermal conductivity of epoxy-based composites journal October 2015
Thermal conductivity of polymer-based composites: Fundamentals and applications journal August 2016
High thermal conductivity of chain-oriented amorphous polythiophene journal March 2014
RTA-Treated Carbon Fiber/Copper Core/Shell Hybrid for Thermally Conductive Composites journal May 2014
Shear-induced crystallization of isotactic polypropylene within the oriented scaffold of noncrystalline ultrahigh molecular weight polyethylene journal September 2005
Shear-induced crystallization in isotactic polypropylene containing ultra-high molecular weight polyethylene oriented precursor domains journal April 2005
Shear-Enhanced Crystallization in Isotactic Polypropylene. 1. Correspondence between in Situ Rheo-Optics and ex Situ Structure Determination journal November 1999
Shear-enhanced crystallization in isotactic polypropylenePart 2. Analysis of the formation of the oriented “skin” journal December 2000
Shear-Enhanced Crystallization in Isotactic Polypropylene. In-Situ Synchrotron SAXS and WAXD journal November 2004
Combined effect of shear and fibrous fillers on orientation-induced crystallization in discontinuous aramid fiber/isotactic polypropylene composites journal January 2008
Shear-induced crystallization of isotactic polypropylene with different molecular weight distributions: in situ small- and wide-angle X-ray scattering studies journal June 2001
Restructuring of confined crystalline morphology in the drawing process of VGCF-iPP nanocomposite filaments journal October 2018
Network formation in polymer nanocomposites under shear journal January 2011
In Situ Time-Resolved X-ray Scattering Study of Isotactic Polypropylene in Additive Manufacturing journal September 2019
Preparation and Mechanical Properties of Polypropylene−Clay Hybrids journal October 1997
Mechanical properties of polypropylene composites: A review journal December 2011
Superior Thermal Conductivity of Single-Layer Graphene journal March 2008
The rise of graphene journal March 2007
Boron Nitride Nanomaterials for Thermal Management Applications journal February 2015
Carbon nanofiller networks- a comparative study of networks formed by branched versus linear carbon nanotubes in thermoplastic polyurethane journal June 2019
Shear-induced preferential alignment of carbon nanotubes resulted in anisotropic electrical conductivity of polymer composites journal November 2006
Comparison of filler percolation and mechanical properties in graphene and carbon nanotubes filled epoxy nanocomposites journal June 2013
Rheological Behavior of Filled Polymeric Systems I. Yield Stress and Shear‐Thinning Effects journal October 1988
Conductive polymer composites with carbonic fillers: Shear induced electrical behaviour journal March 2018
In Operando Monitoring of Dynamic Recovery in 3D-Printed Thermoset Nanocomposites by XPCS journal June 2019
Simultaneous in Situ X-ray Scattering and Infrared Imaging of Polymer Extrusion in Additive Manufacturing journal May 2019
Instrumentation for In situ/Operando X-ray Scattering Studies of Polymer Additive Manufacturing Processes journal March 2019
Synthesis and characterization of graphene: influence of synthesis variables journal January 2014
Melt rheological properties of nylon 6/multi-walled carbon nanotube composites journal September 2008
The spherulitic and lamellar morphology of melt-crystallized isotactic polypropylene journal May 1985
The thermo-mechanical response of PP nanocomposites at high graphene loading journal July 2015
Graphene Nanosheets and Shear Flow Induced Crystallization in Isotactic Polypropylene Nanocomposites journal April 2011
Polypropylene–graphene – a nanocomposite that can be converted into a meta-material at desired frequencies journal January 2014
Segmental Dynamics of Head-to-Head Polypropylene and Polyisobutylene in Their Blend and Pure Components journal September 2005
Unusual Rheological Behavior of Liquid Polybutadiene Rubber/Clay Nanocomposite Gels:  The Role of Polymer−Clay Interaction, Clay Exfoliation, and Clay Orientation and Disorientation journal September 2006