Review Article

A Review of In Situ Mechanical Characterization of Polymer Nanocomposites: Prospect and Challenges

[+] Author and Article Information
Samit Roy

Department of Aerospace Engineering and
University of Alabama,
Tuscaloosa, AL 35487-0280

John Ryan, Samantha Webster

Air Force Research Laboratory,
Wright-Patterson Air Force Base, OH 45433-7750

Dhriti Nepal

Air Force Research Laboratory,
Wright-Patterson Air Force Base, OH 45433-7750
e-mail: dhriti.nepal.1@us.af.mil

1Corresponding author.

Manuscript received January 17, 2017; final manuscript received October 19, 2017; published online November 15, 2017. Editor: Harry Dankowicz.

Appl. Mech. Rev 69(5), 050802 (Nov 15, 2017) (18 pages) Paper No: AMR-17-1005; doi: 10.1115/1.4038257 History: Received January 17, 2017; Revised October 19, 2017

Mechanics at the nanoscale is radically different from mechanics at the macroscale. Atomistic simulations have revealed this important fact, and experiments are being performed to support it. Specifically, in situ testing is being performed by researchers using different approaches with different material systems to interrogate the material at the nanoscale and prove or disprove many of the proposed models. This paper attempts to provide a fairly comprehensive review of the in situ testing that is being performed at the nanoscale, together with a brief description of the models that in situ testing are being used to verify. This review paper intends to primarily provide a broad snapshot of in situ testing of different nanocarbon-based polymeric nanocomposite materials.

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Grahic Jump Location
Fig. 1

(a) Representative stress–strain curve showing a brittle failure (e.g., epoxy) and a ductile failure (e.g., nanocomposite). (b) Schematic showing intrinsic and extrinsic toughening mechanisms. The intrinsic mechanism promotes plasticity ahead of the crack tip and typically acts at the micron scale, whereas the latter shields the crack tip from local stresses, acting at larger length scales along the crack-face created behind the crack tip. (Reproduced with permission from Wegst et al. [17]. Copyright 2015 by Nature.) (c) Schematic illustrating a variety of fracture mechanics information, both qualitative and quantitative, that can be obtained by XRD. (Reproduced with permission from Withers [19]. Copyright 2015 by The Royal Society.)

Grahic Jump Location
Fig. 2

(a) Stress concentration in plate of decreasing thickness, where the plate on the far right is of critical length h*. Stress is normalized to the theoretical strength σth and the thickness of the plate is normalized to h*. (Reproduced with permission from Gao et al. [31]. Copyright 2003 by Proceedings of the National Academy of Sciences.) At large thicknesses (h/,h* = 20, 200), the fracture strength σf is significantly reduced from the theoretical strength, σth, of the material by the stress concentration at the crack tip. As the plate thickness approaches the critical thickness h* (h/h* = 1), the strength approaches the theoretical strength and the stress concentration vanishes due to a nanoscale phenomenon. (b) Critical energy release rate in a nanoscale specimen of width, W, calculated with continuum mechanics (left graph). It shows that conventional fracture mechanics breaks down below a critical singular field size. Discrete fracture mechanics (right graph) was developed by taking account of the discrete nature of interatomic bonds, and it can handle fracture even below the critical size by predicting a constant value of critical energy release rate as a function of specimen width. (Reproduced with permission from Shimada et al. [27] and Tang et al. [43]. Copyright 2015 by PubMed Central and 2013 by Elsevier.)

Grahic Jump Location
Fig. 3

(a) A comprehensive map of the dependence of fracture toughness of different types of nanoparticles/epoxy nanocomposites on particle loading. (Reproduced with permission from Domun et al. [48]. Copyright 2015 by Royal Society of Chemistry.) (b) A plot showing a compilation of results for KIC from various research groups for varying weight percentages of graphene. (Reproduced with permission from Jia et al. [12], Rafiee et al. [13], Tang et al. [43], and Bortz et al. [44], Chandrasekaran [45], and Kumar et al. [46]. Copyright 2014 by American Chemical Society, 2009 by American Chemical Society, 2013 by Elsevier, 2012 by American Chemical Society, 2014 by Elsevier, 2015 by Elsevier.) The inset figures show different failure mechanism observed on SEM images of the fracture surfaces. Left top: evidence of crack pinning in GNP sheets. (Reproduced with permission from Bortz et al. [44]. Copyright 2012 by American Chemical Society.) Left middle: examples of crack pinning failure, dotted line indicates crack propagation direction. (Reproduced with permission from Chandrasekaran et al. [45]. Copyright 2014 by Elsevier.) Left bottom: graphene platelet pull-out seen in 0.1 wt % GNP fracture surface. (Reproduced with permission from Kumar et al. [46]. Copyright 2015 by Elsevier.) Right bottom: circle showing GNP sheet in TEM, and pink square showing SEM of a 5.0 wt % GNP graphene/epoxy composite indicating epoxy-coated GNP protruding out of the fracture surface. Inset shows the wavy edge structure of the GNP. (Reproduced with permission from Rafiee et al. [13]. Copyright 2009 by American Chemical Society.) Right top: circle: SEM image of graphene form (GF), and square: GF/epoxy composites with 0.1 wt % GF. White arrow indicates crack propagation direction. (Reproduced with permission from Jia et al. [12]. Copyright 2014 by American Chemical Society.) Right middle: 0.2 wt % highly dispersed GNP/epoxy showing the crack growth direction. (Reproduced with permission from Tang et al. [43]. Copyright 2013 by Elsevier.)

Grahic Jump Location
Fig. 4

(a) Schematic showing different crack mechanism on GNP composite proposed by Chandrasekaran et al. (Reproduced with permission from Chandrasekaran et al. [45]. Copright 2014 by Elsevier.) (a) The crack either deflects or bifurcates and goes around the graphene particle when the crack front meets the surface of the graphene sheets. (b) Height difference created between crack planes as the crack continues to propagate in between intercalated graphene sheets where shearing between the graphene layers is expected to occur. (d) A crack penetration between GNP layers creating a “dimple-type” fracture surface. (b) Experimental results (SEM) of fractured surfaces showing increased roughness with the addition of GNP, (a) baseline, (b) 0.1 wt %, and (c) 0.5 wt % GNP (b) Series of 10 μm SEM images displaying fracture surfaces of (a) epoxy, (b) 0.1 wt % GNP, and (c) 0.5% GNP. (Reproduced with permission from Kumar et al. [46]. Copyright 2015 by Elsevier.) (c) Three-dimensional (3D) schematic of shear failure in matrix due to a difference in height of fracture planes.

Grahic Jump Location
Fig. 5

A series of SEM images displaying various failure mechanisms: crack pinning failure observed within an epoxy/GNP nanocomposite (left) by Chandrasekaran (Reproduced with permission from Chandrasekaran et al. [45]. Copyright 2014 by Elsevier.), by Park (Reproduced with permission from Park et al. [49]. Copyright 2015 by Wiley.) for fracture in graphene nanosheets/epoxy (center), and by Bortz (Reproduced with permission from Bortz et al. [44]. Copyright 2012 by American Chemical Society.) for fracture in graphene oxide/epoxy (right).

Grahic Jump Location
Fig. 6

In situ nano-indentation of a polymer in TEM. (a) Schematic of the testing device (left), SEM of sample fabricated with a focused ion beam (right). (b) Characteristic TEM images show the development of a deformation zone at different time. (c) A plot showing results of the polymer surface displacement (nm), indenter displacement and the deformation zone size as a function of time. (Reproduced with permission from Zhou et al. [58]. Copyright 2006 by American Institute of Physics.)

Grahic Jump Location
Fig. 7

(a) (a) SEM image showing a graphene film suspended. (b) Morphology seen by TEM on a suspended graphene sample with polymer residue (discontinuous) where the fast Fourier transform diffraction pattern is shown in the inset. (b) In situ SEM tensile testing with a microdevice (a), SEM images ((b) and (c)) showing graphene before and after tensile testing, respectively. Note focused ion beam milled central precrack in (b). (d) Engineering stress–strain plots of the precracked graphene samples. (Reproduced with permission from Zhang et al. [41]. Copyright 2014 by Nature.)

Grahic Jump Location
Fig. 8

In situ nano-indentation study of polyvinyl alcohol/clay nanocomposite. (a) SEM image showing cantilever beam and conical probe prior to the experiment, in which the appropriate sample dimensions are prepared by etching using a focused ion beam. (b) Correlation of the experimental data to crack initiation and fracture. (c) Fracture surface morphology of the tensile zone. (Reproduced with permission from Allison et al. [63]. Copyright 2014 by Elsevier.)

Grahic Jump Location
Fig. 9

(a) (a) The hierarchical structure of natural nacre (red abalone shell), (b) SEM image of natural nacre, and (c) bio-mimetic brick-and-mortar nacre composite. (b) Snapshots from in situ (three-point bending) AFM studies on the bio-mimetic nacre, showing deformation at different loads by optical microscopic image and AFM images. The results were combined to get DIC using kinematic displacement field. (Reproduced with permission from Espinosa et al. [119]. Copyright 2011 by Nature.)

Grahic Jump Location
Fig. 10

(a) Nacre material under 0% tension, with arrows indicating the direction of applied tension. (b)–(f) Differential tensile strain percentages of 1%, 2%, 3%, 4%, 5%, respectively. (g) General schematic of grain rotation within an aragonite platelet showing (a) nanograins under no mechanical stress and (b) grain rotation and biopolymer expansion under mechanical loading. (Reproduced with permission from Li et al. [57]. Copyright 2006 by American Chemical Society.)

Grahic Jump Location
Fig. 11

(a) Crack length effect at the nanoscale leading to a brittle to ductile transition. (b) Schematic of crack propagation and damage evolution in the presence of GNP, (a) at the mesoscale and (b) magnified view at the nanoscale.

Grahic Jump Location
Fig. 12

Effect of nanoparticle size on mode I fracture toughness in GO/epoxy nanocomposite as a function of filler content. (Reproduced with permission from Wang et al. [135]. Copyright 2013 by Elsevier.)



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