Direct observation of microstructural fracture dynamics in carbon fiber reinforced plastics via in situ transmission electron microscopy
Graphical abstract
Introduction
Remarkable mechanical properties of carbon fiber reinforced plastics (CFRPs) have been demonstrated by various strength and fracture tests to obtain relating various physical quantities, such as specific strength, specific stiffness, and fracture length [[1], [2], [3], [4], [5], [6], [7], [8]]. The fracture of CFRPs, which represents the reliability of CFRPs as structural materials, has been investigated using various methods, and the obtained results have been utilized in their material designs [5,[9], [10], [11], [12], [13], [14], [15], [16], [17], [18], [19]]. The examples of the methods are X-ray computer tomography [[20], [21], [22]], the digital image correlation [23], and scanning electron microscopy [16]. In these studies, observations were performed before and after fracture with spatial resolutions on the micrometer order of magnitude; the fracture dynamics was not directly observed. As a result, the fracture processes and mechanisms have been speculated on the basis of the observed results before and after fracture. One of the most effective methods to evaluate fracture in CFRPs is to observe in situ the localized microstructural dynamics in crack generation and propagation, although the method is a state-of-the-art technology. In situ transmission electron microscopy (TEM) allows us to observe such fracture dynamics, as demonstrated for that in isolated carbon fibers [24]. In particular, the atomic resolution of TEM provides a clue to the elucidation of the atomistic fracture processes in CFRPs [25]. Since the fracture and the other mechanical properties of CFRPs are affected by the adhesive strength of fiber/resin interfaces, the fiber surfaces are coated by sizing agents [1,15,16,[26], [27], [28], [29], [30], [31], [32], [33], [34], [35], [36], [37], [38], [39], [40], [41], [42], [43], [44], [45], [46]]. Thus, it is important to clarify the relationship between fracture features and the variations in the interface structures by sizing treatments. In this study, the fracture of CFRPs during off-axis tensile deformation tests was directly observed by in situ TEM. This observation resulted in the quantitative analyses of the influence of a sizing treatment on fracture.
Section snippets
Materials and sample preparation for TEM
The original materials of CFRPs used in this study were provided by NIPPON STEEL Chemical & Material Co., Ltd. The CFRPs were prepared along with following processes. A mixed solution of bisphenol A (BPA) type epoxy and cyclohexylamine was used as the resin matrix. The carbon fibers produced by the combustion of polyacrylonitrile fibers (TORAY T700SC-12000-50C), in which graphitic layered structures align along the fiber direction, were used for reinforcement. Two types of CFRPs were prepared:
Unsized CFRPs
- (1)
Crack propagation along the fiber/resin interfaces
Fig. 2 shows a TEM image of an unsized CFRP before a tensile test. Parts of the fiber/resin interfaces were sufficiently thinned and could be successfully observed by TEM. Fig. 3 shows a time-sequence series of the TEM images of the region indicated by the broken-line red frame in Fig. 2 during the tensile test (see Movie 1 in Supplementary materials). As shown in Fig. 3(a–c), a crack propagated along a fiber/resin interface by application of a
The crack propagation paths
In both unsized and sized CFRPs, the resin matrix was exfoliated from the fibers during tensile deformation, and the resin fragments remained discretely on fiber surfaces. The external shape of the residual resin fragments corresponds to the trajectory of the crack propagation path inside the resin matrix. Based on the observation of the change in the crack propagation path (Fig. 7), the propagation processes are explained as shown in Fig. 14. A crack propagates at a fiber/resin interface when
Conclusions
The microscopic fracture process in CFRPs, i.e., the crack propagation and relating structural variation, was observed in situ by TEM. The crack propagated alternatively along the fiber/resin interfaces and inside the resin matrix, regardless of the sizing treatment. The sizing treatment leads to the increase in the average size of the residual resin fragments and to the decrease in the coverage factor on the fiber surfaces after tensile fracture.
The results of this study revealed
CRediT authorship contribution statement
Tatsuhiro Ishikawa: Investigation, Formal analysis, Visualization, Writing - original draft. Manabu Tezura: Investigation, Writing - review & editing. Tokushi Kizuka: Conceptualization, Methodology, Investigation, Visualization, Writing - original draft, Supervision, Project administration, Funding acquisition.
Declaration of competing interest
The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Acknowledgments
We thank NIPPON STEEL Chemical & Material Co., Ltd. for providing CFRP samples and their information. The authors acknowledge the members within their laboratory for cooperation with a part of the experiment, especially, TEM observation. This study was partly supported by Cross-Ministerial Strategic Innovation Promotion Program (Unit D66, Innovative Measurement and Analysis for Structural Materials).
References (49)
The carbon fibre/epoxy interface—a review
Compos. Sci. Technol.
(1991)Measurement of the static compressive strength of carbon-fibre/epoxy laminates
Compos. Sci. Technol.
(1991)- et al.
Electrical resistance measurement technique for detecting failure in CFRP materials at high strain rates
Compos. Sci. Technol.
(1994) Machining of composite materials
CIRP Ann.
(2002)- et al.
Statistical analysis of the tensile strength of GFRP, CFRP and hybrid composites
Thin-Walled Struct.
(2018) - et al.
Fatigue growth of matrix cracks in the transverse direction of CFRP laminates
Compos. Sci. Technol.
(2002) - et al.
Numerical investigation to prevent crack jumping in Double Cantilever Beam tests of multidirectional composite laminates
Compos. Sci. Technol.
(2011) - et al.
Characterization of crack propagation in mode I delamination of multidirectional CFRP laminates
Compos. Sci. Technol.
(2012) - et al.
Damage monitoring and analysis of composite laminates with an open hole and adhesively bonded repairs using digital image correlation
Compos. B Eng.
(2013) - et al.
Pseudo-ductility and damage suppression in thin ply CFRP angle-ply laminates
Compos. Part A Appl. Sci. Manuf.
(2015)
In-situ toughened CFRP composites by shear-calendar orientation and fiber-bundle filtration of PA microparticles at prepreg interlayer
Compos. Part A Appl. Sci. Manuf.
Tensile failure analysis and residual strength prediction of CFRP laminates with open hole
Compos. B Eng.
Failure modes and strength prediction of thin ply CFRP angle-ply laminates
Compos. Struct.
A modified Schapery theory to predict the progressive failure of CFRP
Compos. Struct.
A study of fracture of unidirectional composites using in situ high-resolution synchrotron X-ray microtomography
Compos. Sci. Technol.
In situ fibre fracture measurement in carbon–epoxy laminates using high resolution computed tomography
Compos. Sci. Technol.
Orientation-dependent tensile deformation and damage of a T700 carbon fiber/epoxy composite: a synchrotron-based study
Carbon
High strain rate characterisation of unidirectional carbon-epoxy IM7-8552 in transverse compression and in-plane shear using digital image correlation
Mech. Mater.
In situ transmission electron microscope tensile testing reveals structure–property relationships in carbon nanofibers
Carbon
Effect of γ-ray irradiation grafting on the carbon fibers and interfacial adhesion of epoxy composites
Compos. Sci. Technol.
Effect of the surface roughness on interfacial properties of carbon fibers reinforced epoxy resin composites
Appl. Surf. Sci.
Tagged and enhanced interface of carbon fiber/epoxy by doping sizing agent with upconversion luminescent nanoparticles
Mater. Lett.
Interface property of carbon fibers/epoxy resin composite improved by hydrogen peroxide in supercritical water
Mater. Lett.
Effects of bonding types of carbon fibers with branched polyethyleneimine on the interfacial microstructure and mechanical properties of carbon fiber/epoxy resin composites
Compos. Sci. Technol.
Cited by (9)
Revealing low temperature-mechanical coupling failure mechanisms in CFRP laminates with in-situ observations
2024, Journal of Materials Research and TechnologyEpoxy resins containing epoxy-modified polyrotaxanes
2023, PolymerAtomistic prediction on the degradation of vinylester-based composite under chloride and elevated temperature
2022, Composites Science and TechnologyCitation Excerpt :Observed in microscopic experiments, the interphase width increases under wet condition due to the debonding between glass additives and the polymer matrix [10]. Valuable information towards the effect of chloride and elevated temperature on the interfacial debonding has been provided by some microscopic experiments such as atomic force microscopy [11], scanning electron microscopy [12], and nanoindentation [13], but there are still limitations and challenges to be resolved. Practically, a complicated physical-chemical adsorption process is related to the formation of the interface between additive and polymer, resulting in a nanometer-sized interphase region, which comprehensive investigation requires to go down to atomistic scale [14].
Preparation of high-performance transparent glass-fiber reinforced composites based on refractive index-tunable epoxy-functionalized siloxane hybrid matrix
2021, Composites Science and TechnologyCitation Excerpt :Fiber reinforced polymer composites (FRPs) have been widely developed for automotive and electronics applications because of their promising characteristics such as structural reliability, light weight, mechanical strength, and cost-effectiveness [1–3].
Transmission electron microscopy of unidirectional carbon fiber reinforced plastics at on-axis tension
2020, MaterialiaCitation Excerpt :To investigate the separation dynamics, the microstructural analyses of the interfacial textures before and after the separation have been performed by, for example, transmission and scanning electron microscopy (TEM and SEM), scanning probe-type microscopy, and computational methods [8–27]. In particular, TEM is the only method that can directly observe the inner structures of CF/resin interfaces with a thickness of only several atoms, and has been applied for studies of CFRPs 28–[30]. Some of the present authors already applied in situ deformation TEM into the fracture of CFRPs during tensile deformation along the direction tilted by 45° from the fiber direction, and demonstrated that the microstructural dynamics of the CF/resin interfaces can be observed [30].