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

Abstract

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.

Authors:
 [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)
Publication Date:
Research Org.:
Brookhaven National Lab. (BNL), Upton, NY (United States); AArgonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES); National Science Foundation (NSF); Casali Foundation Israel
OSTI Identifier:
1643999
Alternate Identifier(s):
OSTI ID: 1774535; OSTI ID: 1777571
Report Number(s):
BNL-216194-2020-JAAM
Journal ID: ISSN 0266-3538
Grant/Contract Number:  
SC0012704; AC02-06CH11357
Resource Type:
Accepted Manuscript
Journal Name:
Composites Science and Technology
Additional Journal Information:
Journal Volume: 196; Journal ID: ISSN 0266-3538
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE

Citation Formats

Shmueli, Yuval, Lin, Yu-Chung, Zuo, Xianghao, Guo, Yichen, Lee, Sungsik, Freychet, Guillaume, Zhernenkov, Mikhail, Kim, Taejin, Tannenbaum, Rina, Marom, Gad, Gersappe, Dilip, and Rafailovich, Miriam H. In-situ X-ray scattering study of isotactic polypropylene/graphene nanocomposites under shear during fused deposition modeling 3D printing. United States: N. p., 2020. Web. doi:10.1016/j.compscitech.2020.108227.
Shmueli, Yuval, Lin, Yu-Chung, Zuo, Xianghao, Guo, Yichen, Lee, Sungsik, Freychet, Guillaume, Zhernenkov, Mikhail, Kim, Taejin, Tannenbaum, Rina, Marom, Gad, Gersappe, Dilip, & Rafailovich, Miriam H. In-situ X-ray scattering study of isotactic polypropylene/graphene nanocomposites under shear during fused deposition modeling 3D printing. United States. https://doi.org/10.1016/j.compscitech.2020.108227
Shmueli, Yuval, Lin, Yu-Chung, Zuo, Xianghao, Guo, Yichen, Lee, Sungsik, Freychet, Guillaume, Zhernenkov, Mikhail, Kim, Taejin, Tannenbaum, Rina, Marom, Gad, Gersappe, Dilip, and Rafailovich, Miriam H. Fri . "In-situ X-ray scattering study of isotactic polypropylene/graphene nanocomposites under shear during fused deposition modeling 3D printing". United States. https://doi.org/10.1016/j.compscitech.2020.108227. https://www.osti.gov/servlets/purl/1643999.
@article{osti_1643999,
title = {In-situ X-ray scattering study of isotactic polypropylene/graphene nanocomposites under shear during fused deposition modeling 3D printing},
author = {Shmueli, Yuval and Lin, Yu-Chung and Zuo, Xianghao and Guo, Yichen and Lee, Sungsik and Freychet, Guillaume and Zhernenkov, Mikhail and Kim, Taejin and Tannenbaum, Rina and Marom, Gad and Gersappe, Dilip and Rafailovich, Miriam H.},
abstractNote = {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.},
doi = {10.1016/j.compscitech.2020.108227},
journal = {Composites Science and Technology},
number = ,
volume = 196,
place = {United States},
year = {Fri May 15 00:00:00 EDT 2020},
month = {Fri May 15 00:00:00 EDT 2020}
}

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Works referenced in this record:

Anisotropic material properties of fused deposition modeling ABS
journal, October 2002


Weld formation during material extrusion additive manufacturing
journal, January 2017

  • Seppala, Jonathan E.; Hoon Han, Seung; Hillgartner, Kaitlyn E.
  • Soft Matter, Vol. 13, Issue 38
  • DOI: 10.1039/C7SM00950J

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

  • Singh, Virendra; Bougher, Thomas L.; Weathers, Annie
  • Nature Nanotechnology, Vol. 9, Issue 5
  • DOI: 10.1038/nnano.2014.44

RTA-Treated Carbon Fiber/Copper Core/Shell Hybrid for Thermally Conductive Composites
journal, May 2014

  • Yu, Seunggun; Park, Bo-In; Park, Cheolmin
  • ACS Applied Materials & Interfaces, Vol. 6, Issue 10
  • DOI: 10.1021/am500871b

Shear-induced crystallization of isotactic polypropylene within the oriented scaffold of noncrystalline ultrahigh molecular weight polyethylene
journal, September 2005


Shear-Enhanced Crystallization in Isotactic Polypropylene. 1. Correspondence between in Situ Rheo-Optics and ex Situ Structure Determination
journal, November 1999

  • Kumaraswamy, Guruswamy; Issaian, Ani M.; Kornfield, Julia A.
  • Macromolecules, Vol. 32, Issue 22
  • DOI: 10.1021/ma990772j

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

  • Kumaraswamy, Guruswamy; Verma, Ravi K.; Kornfield, Julia A.
  • Macromolecules, Vol. 37, Issue 24
  • DOI: 10.1021/ma035840n

Network formation in polymer nanocomposites under shear
journal, January 2011

  • Jaber, Eihab; Luo, Haobin; Li, Wentao
  • Soft Matter, Vol. 7, Issue 8
  • DOI: 10.1039/c0sm00990c

In Situ Time-Resolved X-ray Scattering Study of Isotactic Polypropylene in Additive Manufacturing
journal, September 2019

  • Shmueli, Yuval; Lin, Yu-Chung; Lee, Sungsik
  • ACS Applied Materials & Interfaces, Vol. 11, Issue 40
  • DOI: 10.1021/acsami.9b12908

Preparation and Mechanical Properties of Polypropylene−Clay Hybrids
journal, October 1997

  • Kawasumi, Masaya; Hasegawa, Naoki; Kato, Makoto
  • Macromolecules, Vol. 30, Issue 20
  • DOI: 10.1021/ma961786h

Mechanical properties of polypropylene composites: A review
journal, December 2011

  • Shubhra, Quazi TH; Alam, Akmm; Quaiyyum, Ma
  • Journal of Thermoplastic Composite Materials, Vol. 26, Issue 3
  • DOI: 10.1177/0892705711428659

Superior Thermal Conductivity of Single-Layer Graphene
journal, March 2008

  • Balandin, Alexander A.; Ghosh, Suchismita; Bao, Wenzhong
  • Nano Letters, Vol. 8, Issue 3, p. 902-907
  • DOI: 10.1021/nl0731872

The rise of graphene
journal, March 2007

  • Geim, A. K.; Novoselov, K. S.
  • Nature Materials, Vol. 6, Issue 3, p. 183-191
  • DOI: 10.1038/nmat1849

Boron Nitride Nanomaterials for Thermal Management Applications
journal, February 2015


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

  • Poslinski, A. J.; Ryan, M. E.; Gupta, R. K.
  • Journal of Rheology, Vol. 32, Issue 7
  • DOI: 10.1122/1.549987

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

  • Shmueli, Yuval; Jiang, Jiaolong; Zhou, Yuchen
  • ACS Applied Polymer Materials, Vol. 1, Issue 6
  • DOI: 10.1021/acsapm.9b00328

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

  • Lavin-Lopez, M. P.; Valverde, J. L.; Cuevas, M. C.
  • Physical Chemistry Chemical Physics, Vol. 16, Issue 7
  • DOI: 10.1039/c3cp54832e

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

  • Xu, Jia-Zhuang; Chen, Chen; Wang, Yan
  • Macromolecules, Vol. 44, Issue 8
  • DOI: 10.1021/ma1028104

Polypropylene–graphene – a nanocomposite that can be converted into a meta-material at desired frequencies
journal, January 2014

  • Perumal Ramasamy, Radha; Yang, Kai; Rafailovich, Miriam H.
  • RSC Adv., Vol. 4, Issue 85
  • DOI: 10.1039/C4RA05814C

Segmental Dynamics of Head-to-Head Polypropylene and Polyisobutylene in Their Blend and Pure Components
journal, September 2005

  • Krygier, Ernest; Lin, Guoxing; Mendes, Jessica
  • Macromolecules, Vol. 38, Issue 18
  • DOI: 10.1021/ma048224f