Direct three-dimensional imaging of the fracture of fiber-reinforced plastic under uniaxial extension: Effect of adhesion between fibers and matrix

Saito, Hayate; Aoyanagi, Yuko; Mihara, Takaaki; Tanaka, Teruhisa; Higuchi, Takeshi; Morita, Hiroshi; Jinnai, Hiroshi

doi:10.1016/j.polymer.2017.01.072

Cited by 6 publications

(3 citation statements)

References 43 publications

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“…The biggest advantage of X-ray CT over LSCM is the strong penetrative power of the X-rays that allows it to be readily used for opaque materials. It has recently been used to observe dynamical processes in fiber-reinforced plastic under uniaxial extension in which the orientation of fibers and formation of voids were clearly imaged and correlated with mechanical properties . For extremely fine resolution, the atom probe field-ion microscope was developed to allow atom probe tomography with truly atomic scale precision, though few studies have applied this type of microscopy to polymers.…”

Section: Introductionmentioning

confidence: 99%

Three-Dimensional Visualization and Characterization of Polymeric Self-Assemblies by Transmission Electron Microtomography

et al. 2017

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* S Supporting Information CONSPECTUS: Self-assembling structures and their dynamical processes in polymeric systems have been investigated using three-dimensional transmission electron microscopy (3D-TEM). Block copolymers (BCPs) self-assemble into nanoscale periodic structures called microphase-separated structures, a deep understanding of which is important for creating nanomaterials with superior physical properties, such as high-performance membranes with well-defined pore size and high-density data storage media. Because microphase-separated structures have become increasingly complicated with advances in precision polymerization, characterizing these complex morphologies is becoming increasingly difficult. Thus, microscopes capable of obtaining 3D images are required. In this article, we demonstrate that 3D-TEM is an essential tool for studying BCP nanostructures, especially those self-assembled during dynamical processes and under confined conditions. The first example is a dynamical process called order−order transitions (OOTs). Upon changing temperature or pressure or applying an external field, such as a shear flow or electric field, BCP nanostructures transform from one type of structure to another. The OOTs are examined by freezing the specimens in the middle of the OOT and then observing the boundary structures between the preexisting and newly formed nanostructures in three-dimensions. In an OOT between the bicontinuous double gyroid and hexagonally packed cylindrical structures, two different types of epitaxial phase transition paths are found. Interestingly, the paths depend on the direction of the OOT. The second example is BCP self-assemblies under confinement that have been examined by 3D-TEM. A variety of intriguing and very complicated 3D morphologies can be formed even from the BCPs that self-assemble into simple nanostructures, such as lamellar and cylindrical structures in the bulk (in free space). Although 3D-TEM is becoming more frequently used for detailed morphological investigations, it is generally used to study static nanostructures. Although OOTs are dynamical processes, the actual experiment is done in the static state, through a detailed morphological study of a snapshot taken during the OOT. Developing time-dependent nanoscale 3D imaging has become a hot topic. Here, the two main problems preventing the development of in situ electron tomography for polymer materials are addressed. First, the staining protocol often used to enhance contrast for electrons is replaced by a new contrast enhancement based on chemical differences between polymers. In this case, no staining is necessary. Second, a new 3D reconstruction algorithm allows us to obtain a high-contrast, quantitative 3D image from fewer projections than is required for the conventional algorithm to achieve similar contrast, reducing the number of projections and thus the electron beam dose. Combining these two new developments is expected to open new doors to 3D in situ real-time structural observation of polymer materials.

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Section: Introductionmentioning

confidence: 99%

Three-Dimensional Visualization and Characterization of Polymeric Self-Assemblies by Transmission Electron Microtomography

et al. 2017

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“…Historically, laser-scanning confocal microscopy and X-ray computerized tomography are two imaging techniques commonly used in characterizing 3D structures of soft materials. The former was first introduced by Jinnai et al in the mid-1990s, to resolve the morphology of bicontinuous polymer mixtures, − and the latter has been reported in imaging fiber-reinforced or porous polymers. , While both imaging techniques allow 3D visualization, their spatial resolutions are traditionally limited to micrometer-scale with the recent innovation of pushing it to 7 nm in resolving NP lattices and multimaterial frameworks, still far below that of electron beam-based methods (0.1–0.3 nm for TEM and 0.5–1 nm for SEM) . On the other hand, field ion microscopy was introduced in 1951, which resolved individual atoms in 1955, evolved into a 3D imaging technique called atom probe tomography (APT) in 1980s. − While APT offers a high resolution below 0.15 nm on composition, it has a few drawbacks; the most prominent one is that APT is a destructive technique. − Apart from consuming the specimen during analysis, APT also has limited sample size and requires special sample preparation methods such as FIB-milling and chemical fixation, which may interact with samples and introduce unwanted artifacts …”

Section: Electron Tomography Of the 3d Structure Morphology And Compo...mentioning

confidence: 99%

“…114−116 and the latter has been reported in imaging fiber-reinforced or porous polymers. 117,118 While both imaging techniques allow 3D visualization, their spatial resolutions are traditionally limited to micrometer-scale with the recent innovation of pushing it to 7 nm in resolving NP lattices and multimaterial frameworks, 119 still far below that of electron beam-based methods (0.1−0.3 nm for TEM and 0.5−1 nm for SEM). 120 On the other hand, field ion microscopy was introduced in 1951, which resolved individual atoms in 1955, evolved into a 3D imaging technique called atom probe tomography (APT) in 1980s.…”

Section: Electron Tomography Of the 3d Structure Morphology And Compo...mentioning

confidence: 99%

Electron Microscopy Studies of Soft Nanomaterials

et al. 2023

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This review highlights recent efforts on applying electron microscopy (EM) to soft (including biological) nanomaterials. We will show how developments of both the hardware and software of EM have enabled new insights into the formation, assembly, and functioning (e.g., energy conversion and storage, phonon/photon modulation) of these materials by providing shape, size, phase, structural, and chemical information at the nanometer or higher spatial resolution. Specifically, we first discuss standard real-space two-dimensional imaging and analytical techniques which are offered conveniently by microscopes without special holders or advanced beam technology. The discussion is then extended to recent advancements, including visualizing three-dimensional morphology of soft nanomaterials using electron tomography and its variations, identifying local structure and strain by electron diffraction, and recording motions and transformation by in situ EM. On these advancements, we cover state-of-the-art technologies designed for overcoming the technical barriers for EM to characterize soft materials as well as representative application examples. The even more recent integration of machine learning and its impacts on EM are also discussed in detail. With our perspectives of future opportunities offered at the end, we expect this review to inspire and stimulate more efforts in developing and utilizing EM-based characterization methods for soft nanomaterials at the atomic to nanometer length scales in academic research and industrial applications.

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In-situ 3D fracture propagation of short carbon fiber reinforced polymer composites

Wang

Pei

et al. 2019

Composites Science and Technology

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Direct three-dimensional imaging of the fracture of fiber-reinforced plastic under uniaxial extension: Effect of adhesion between fibers and matrix

Cited by 6 publications

References 43 publications

Three-Dimensional Visualization and Characterization of Polymeric Self-Assemblies by Transmission Electron Microtomography

Three-Dimensional Visualization and Characterization of Polymeric Self-Assemblies by Transmission Electron Microtomography

Electron Microscopy Studies of Soft Nanomaterials

In-situ 3D fracture propagation of short carbon fiber reinforced polymer composites

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