Visualization of the tensile fracture behaviors at adhesive interfaces between brass and sulfur-containing rubber studied by transmission electron microscopy

Shimizu, Kosuke; Miyata, Tomohiro; Nagao, Tomohiko; Kumagai, Akemi; Jinnai, Hiroshi

doi:10.1016/j.polymer.2019.121789

Cited by 19 publications

(15 citation statements)

References 30 publications

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“…The thin film was mounted on the cartridge of the tensile TEM holder. [ 26–31 ] Both edges of the sample specimen adhered to the tensile holder with epoxy glue. The cartridge had a ~30 μm gap or span length.…”

Section: Methodsmentioning

confidence: 99%

“…Microcrack growth and void formation in the composite sheets during tensile deformation were observed by real‐time transmission electron microscopy (TEM), without staining, and by using a specially designed holder. [ 26–31 ] Thus, the real‐time TEM technique was applied to TEMPO‐CNF‐containing rubber composite sheets, for the first time, to make clear the tensile deformation process and mechanism at the nanometer level in term of TEMPO‐CNF structures, their clusters, and the rubber/TEMPO‐CNF interfaces. The tensile deformation behavior of the two rubber/TEMPO‐CNF composites differed a little, because of the different morphologies, sizes, distributions, and structures of the TEMPO‐CNF/rubber clusters and TEMPO‐CNFs in the composites.…”

Section: Introductionmentioning

confidence: 99%

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Real‐time observation of microcrack growth in thin film microtomed from rubber/nanocellulose composite sheets, during tensile deformation

et al. 2022

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Rubber/nanocellulose composite sheets improve tensile properties compared with neat rubber sheets, when nanocellulose materials are suitably compounded with rubber matrices. First, two oven‐dried nanocellulose materials containing different additive components were prepared from nanocellulose/water dispersions, and the oven‐dried nanocellulose‐containing materials were compounded with rubber sheets under high shear forces by using a two‐roll mill. The tensile moduli and strength of the rubber/nanocellulose composite sheets were clearly better than those of the rubber sheet prepared without nanocellulose, while the elongations at break were similar. Thin films were cut from the rubber/nanocellulose composite sheets, and their real‐time tensile deformation processes were observed by transmission electron microscopy (TEM) to understand the time‐dependent patterns of crack propagation, void formations, and fusion between cracks and voids in the composites during tensile deformation. TEM observations showed that the composite sheets consisted of individual rubber/nanocellulose clusters. Voids initially formed inside the rubber/nanocellulose clusters, propagated to form cracks, fused with other voids or secondary cracks. There were slight differences between the crack‐propagation patterns of the two rubber composites, probably because of differences in the morphologies, sizes, distributions, and structures of the rubber/nanocellulose clusters, and surface chemical structures of individual nanocellulose elements between the composites.

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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Real‐time observation of microcrack growth in thin film microtomed from rubber/nanocellulose composite sheets, during tensile deformation

et al. 2022

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“…Because of the lack of appropriate means to observe rubber materials under deformation with TEM, few in situ nanoscale observations of these materials have been reported. Recently, a TEM holder was developed that enables the stretching of rubber materials during TEM observation, 20,59,60 with which nanoscale deformation behaviors in a silica nanoparticle‐filled rubber were successfully observed. It was observed that strain propagates along the network of silica aggregates.…”

Section: Introductionmentioning

confidence: 99%

Crack propagation behaviors in a nanoparticle‐filled rubber studied by in situ tensile electron microscopy

Watanabe

Miyata

Nagao

et al. 2021

Journal of Polymer Science

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Although fracture resistance is critical for rubber materials, the fracture mechanisms are poorly understood from a microscopic perspective. In this study, a crack propagation process in rubber with silica nanoparticles, which is commonly used to enhance the mechanical properties of rubber materials, was successfully observed in situ with nanoscale resolution using transmission electron microscopy (TEM). The consecutive time-sliced TEM images clarified that the crack tip propagated along the interfaces between the rubber matrix and aggregates of silica nanoparticles (rubber-aggregate interfaces). Moreover, the path and propagation rate of the crack were significantly affected by the heterogeneous distribution of the silica aggregates, which resulted in a "stickslip" propagation behavior of the crack tip. Detailed spatial strain analysis revealed that the local maximum principal strain (ε max ) around the crack tip was nonuniform. The crack tip propagated through regions with large ε max , delaminating the rubber-aggregate interfaces. This study successfully demonstrated that the heterogeneous distribution of nanoparticles significantly affects the fracture behavior of nanoparticle-filled rubbers.

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“…Electron microscopy is a powerful tool for directly observing the adhesive interfaces between the steel cord and rubber at a much higher spatial resolution. Chandra et al used scanning electron microscopy (SEM) equipped with energy-dispersive X-ray spectroscopy (EDX) to observe an adhesive interface and clarify the structure of the adhesive layer. , Transmission electron microscopy (TEM) was also used with EDX chemical composition analysis to examine the structure of adhesive interfaces. − Recently, Shimizu et al carried out a direct observation of fracture behavior of the adhesive interface formed between rubber and brass particles using a tensile holder for TEM . Although electron microscopy-based structural analysis directly measures the distribution of chemical compounds with high spatial resolution, the region analyzed is limited to a small area of the interfaces several micrometers across.…”

Section: Introductionmentioning

confidence: 99%

Degradation of a Metal–Polymer Interface Observed by Element-Specific Focused Ion Beam-Scanning Electron Microscopy

et al. 2020

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The degradation of a metal−polymer interface was studied in three dimensions using focused ion beam-scanning electron microscopy (FIB-SEM) with energy-dispersive X-ray spectroscopy. A brass-rubber interface, which is important for tires, was examined as an example of a metal-polymer interface. Brass-plated steel cords were embedded in rubber, which was then vulcanized. The brass-rubber interface was treated at 70 °C under 96% humidity for up to 14 days (a wet-heat aging treatment). FIB-SEM provided clear three-dimensional images of the adhesive layer consisting of brass (CuZn), Cu x S, and ZnO/ZnS between the steel cords and rubber. During degradation, Cu x S at the interfaces diffused into the rubber, resulting in the direct contact of bare steel with rubber. The lack of a substantial adhesive layer explained the degradation of mechanical properties after the wet−heat treatment. In addition, electron diffraction and electron energy loss spectroscopy revealed that the Cu 2 S crystals in the adhesive layer changed to crystal-like CuS during the degradation, which also caused a degradation of mechanical properties because a high Cu valence of x ≈ 2 in Cu x S leads to stronger adhesion than a valence of x = 1.

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Visualization of the tensile fracture behaviors at adhesive interfaces between brass and sulfur-containing rubber studied by transmission electron microscopy

Cited by 19 publications

References 30 publications

Real‐time observation of microcrack growth in thin film microtomed from rubber/nanocellulose composite sheets, during tensile deformation

Real‐time observation of microcrack growth in thin film microtomed from rubber/nanocellulose composite sheets, during tensile deformation

Crack propagation behaviors in a nanoparticle‐filled rubber studied by in situ tensile electron microscopy

Degradation of a Metal–Polymer Interface Observed by Element-Specific Focused Ion Beam-Scanning Electron Microscopy

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