Abstract

Carbonized elastomer-based composites (CECs) possess a number of attractive features in terms of thermomechanical and electromechanical performance, durability in aggressive media and facile net-shape formability, but their relatively low ductility and strength limit their suitability for structural engineering applications. Prospective applications such as structural elements of micro-electro-mechanical systems MEMS can be envisaged since smaller principal dimensions reduce the susceptibility of components to residual stress accumulation during carbonization and to brittle fracture in general. We report the results of in situ in-SEM study of microdeformation and fracture behavior of CECs based on nitrile butadiene rubber (NBR) elastomeric matrices filled with carbon and silicon carbide. Nanostructured carbon composite materials were manufactured via compounding of elastomeric substance with carbon and SiC fillers using mixing rolling mill, vulcanization, and low-temperature carbonization. Double-edge notched tensile (DENT) specimens of vulcanized and carbonized elastomeric composites were subjected to in situ tensile testing in the chamber of the scanning electron microscope (SEM) Tescan Vega 3 using a Deben microtest 1 kN tensile stage. The series of acquired SEM images were analyzed by means of digital image correlation (DIC) using Ncorr open-source software to map the spatial distribution of strain. These maps were correlated with finite element modeling (FEM) simulations to refine the values of elastic moduli. Moreover, the elastic moduli were derived from unloading curve nanoindentation hardness measurements carried out using a NanoScan-4D tester and interpreted using the Oliver–Pharr method. Carbonization causes a significant increase of elastic moduli from 0.86 ± 0.07 GPa to 14.12 ± 1.20 GPa for the composite with graphite and carbon black fillers. Nanoindentation measurements yield somewhat lower values, namely, 0.25 ± 0.02 GPa and 9.83 ± 1.10 GPa before and after carbonization, respectively. The analysis of fractography images suggests that crack initiation, growth and propagation may occur both at the notch stress concentrator or relatively far from the notch. Possible causes of such response are discussed, namely, (1) residual stresses introduced by processing; (2) shape and size of fillers; and (3) the emanation and accumulation of gases in composites during carbonization.

Highlights

  • The formulation and use of carbonized elastomer-based composites (CECs) developed in the last decade due to the attractive perspective of reasonable cost net-shaped fabrication of carbon components for oil mining submersible pumps, brakes, current collectors, and other applications [1]

  • Taking into account the values of Young’s modulus for filler particulates (10–25, 250–650 and 350–450 GPa for graphite, carbon fibers and SiC, respectively), one can conclude that the simple additive rule of the mixture is not valid for elastic modulus and ultimate tensile strength of vulcanized CECs assuming that matrix-filler bonding is likely to be predominant factor governing their elastic and plastic behavior

  • Membrane-electrode blocks in fuel cells and MEMS are viewed as prospective fields for CECs requiring, a thorough characterization of their micro-deformation and fracture behavior

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Summary

Introduction

The formulation and use of carbonized elastomer-based composites (CECs) developed in the last decade due to the attractive perspective of reasonable cost net-shaped fabrication of carbon components for oil mining submersible pumps, brakes, current collectors, and other applications [1]. Brittleness reduces the suitability of CECs for structural engineering applications, promoting the search for functional applications, where mechanical performance does not represent the primary criterion. Use of hybrid microstructures and miniaturization of structural components seem to represent solutions where CECs can maximize the advantages of their performance. Fuel cell applications offer a good example of a functional application where CECs can offer overall benefit. Significant progress has been made in the development and implementation of one of the types of fuel cells, namely, redox batteries with an electrolyte based on vanadium salts

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