Polymerization-Induced Phase Separation in Rubber-Toughened Amine-Cured Epoxy Resins: Tuning Morphology from the Nano- to Macro-scale
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99 GENERAL AND MISCELLANEOUS↗
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Rubber-toughened cyanate composites - Properties and toughening mechanism
Earlier work by Young et al. (1990) has shown that Dow experimental cyanate ester resin XU71787.02 is readily toughenable by rubber. A particularly effective rubber for this purpose is an experimental core-shell rubber which toughens the polymer by inducing shear yielding. This paper describes an investigation into the toughening mechanism in the corresponding carbon-fiber composite systems and the effect of fibers on composite properties. Resin-fiber interfacial shear strengths have been successfully correlated to the compressive strengths after impact and other key properties of composites based on rubber-toughened cyanate and several carbon fibers. The differences in the properties are explained by the difference in the functioning of the rubber particles during the fracture process.
Yang, P. C.↗
Polyfunctional epoxies. I - Rubber-toughened brominated and nonbrominated formulations for graphite composites. II - Nonrubber versus rubber-toughened brominated formulations for graphite composites
A new trifunctional epoxy resin, Tris-(hydroxyphenyl) methane triglycidyl ether, is compared to a state-of-the-art tetraglycidyl 4,4'-diaminodiphenyl methane (TGDDM), in graphite composites. Rubber-toughened brominated formulations of the epoxy resin are compared to nonbrominated ones in terms of their mechanical performance, environmental stability, thermochemical behavior, and flame retardancy. It is shown that the new resin performs almost the same way as the TGDDM does, but has improved glass transition temperature and environmental properties. Brominated polymeric additives (BPA) of different molecular weights are tested as a Br source to flame retardant graphite epoxy composites. The optimal molecular weight of the BPA and its polymeric backbone length are derived and compared with a 10 percent rubber-toughened formulation of the epoxy resin. Results indicate that when the Br content in the graphite composite is increased without the use of rubber, the mechanical properties improved. The use of BPAs as tougheners for graphite composites is also considered.
Nir, Z.↗
Toughening materials: enhancing resistance to fracture
It has been said that ‘God invented plasticity, but the Devil invented fracture!’ Both mechanisms represent the two prime modes of structural failure, respectively, plastic collapse and the rupture/breaking of a component, but the concept of developing materials with enhanced resistance to fracture can be difficult. This is because fracture resistance invariably involves a compromise—between strength and ductility, between strength and toughness—fundamentally leading to a ‘conflict’ between nano-/micro-structural damage and the mechanisms of toughening. Here, we examine the two major classes of such toughening: (i) intrinsic toughening, which occurs ahead of a crack tip and is motivated by plasticity—this is the principal mode of fracture resistance in ductile materials, and (ii) extrinsic toughening, which occurs at, or in the wake of, a crack tip and is associated with crack-tip shielding—this is generally the sole mode of fracture resistance in brittle materials. We briefly examine how these distinct mechanistic processes have been used to toughen synthetic materials—intrinsically in gradient materials and in multiple principal-element metallic alloys with the example of metallic glasses and high-entropy alloys, and extrinsically in ceramics with the example of ceramic-matrix composites—in comparison to Nature which has been especially adept in creating biological/natural materials which are toughened by one or both mechanistic classes, despite often consisting of constituents with meagre mechanical properties. The success of Nature has been driven by its ability to cultivate the development of materials with multiple length-scale hierarchical structures that display ingenious gradients and structural adaptability, a philosophy which we need to emulate and more importantly learn to synthesize to make structural materials of the future with unprecedented combinations of mechanical properties.
36 MATERIALS SCIENCE↗
Toughening of Boron Carbide Composites by Hierarchical Microstructuring
Due to a unique combination of properties including high hardness, low density, chemical and thermal stability, semi-conductivity, and high neutron absorption, boron carbide (B4C) is a potential candidate for various applications involving extreme environment. However, B4C’s current application is limited because of its low fracture toughness. In this study, a hierarchical microstructure design with features including TiB2 grains and graphite platelets was used to toughen B4C by simultaneously utilizing multiple toughening mechanisms including crack deflection, bridging, and micro-crack toughening. Using field-assisted sintering technology (FAST), B4C composites with dense and hierarchical microstructure were fabricated. Previously, the fracture toughness of fabricated B4C composites was measured at micro-scale using micro-indentation to have up to 56% improvement. In this work, the B4C composites’ fracture toughness was characterized at macro-scale using four-point bending methods and compared with previous results obtained at micro-scale. Micromechanics modeling of fracture behaviors for B4C-TiB2 composites was also performed to evaluate the contributions from experimentally observed toughening mechanisms. From four-point bending tests, B4C composites reinforced with both TiB2 grains (~15 vol%) and graphite platelets (~8.7 vol%) exhibited the highest fracture toughness enhancement from 2.38 to 3.65 MPa∙m^(1/2). The measured values were lower than those obtained using micro-indentation but maintained the general trends. The discrepancy between the indentation and four-point bending test results originated from the complex deformation behaviors triggered by the high contact load during indentation tests. Through micromechanics modeling, introduced thermal residual stress due to thermal expansion mismatch between B4C and TiB2, and weak interphases at B4C-TiB2 boundaries were identified as the main causes for experimentally observed toughness enhancement. These results proved the effectiveness of hierarchical microstructure designs for B4C toughening and can provide reference for the future design of B4C composites with optimized microstructures for further fracture toughness enhancement.
composites↗
Toughening mechanism in elastomer-modified epoxy resins, part 2
The role of matrix ductility on the toughenability and toughening mechanism of elastomer-modified DGEBRA epoxies was investigated. Matrix ductility was varied by using epoxide resins of varying epoxide monomer molecular weights. These epoxide resins were cured using 4,4' diaminodiphenyl sulfone (DDS) and, in some cases, modified with 10% HYCAR(r)CTBN 1300X8. Fracture roughness values for the neat epoxies were found to be almost independent on the monomer molecular weight of the epoxide resin used. However, it was found that the fracture toughness of the elastomer-modified epoxies was very dependent upon the epoxide monomer molecular weight. Tensile dilatometry indicated that the toughening mechanism, when present, is similar to the mechanisms found for the piperidine cured epoxies in Part 1. SEM and OM corroborate this finding. Dynamic mechanical studies were conducted to shed light on the toughenability of the epoxies. The time-dependent small strain behavior of these epoxies were separated into their bulk and shear components. The bulk component is related to brittle fracture, whereas the shear component is related to yielding. It can be shown that the rates of shear and bulk strain energy buildup for a given stress are uniquely determined by the values of Poisson's ratio, nu. It was found that nu increases as the monomer molecular weight of the epoxide resin used increases. This increase in nu can be associated with the low temperature beta relaxation. The effect of increasing cross-link density is to shift the beta relaxation to higher temperatures and to decrease the magnitude of the beta relaxation. Thus, increasing cross-link density decreases nu and increases the tendency towards brittle fracture.
Yee, A. F.↗
Comparison of the compressive strengths for stitched and toughened composite systems
The compression strength of a stitched and a toughened matrix graphite/epoxy composite was determined and compared to a baseline unstitched untoughened composite. Two different layups with a variety of test lengths were tested under both ambient and hot/wet conditions. No significant difference in strength was seen for the different materials when the gage lengths of the specimens were long enough to lead to a buckling failure. For shorter specimens, a 30 percent reduction in strength from the baseline was seen due to stitching for both a 48-ply quasi-isotropic and a (0/45/0/-45/90/-45/0/45/0)s laminate. Analysis of the results suggested that the decrease in strength was due to increased fiber misalignment due to the stitches. An observed increasing strength with decreasing gage length, which was seen for all materials, was explained with a size effect model. The model assumed a random distribution of flaws (misaligned fibers). The toughened materials showed a small increase in strength over the baseline material for both laminates presumably due to the compensating effects of a more compliant matrix and straighter fibers in the toughened material. The hot/wet strength of the stitched and baseline material fell 30 percent below their ambient strengths for shorter, nonbuckling specimen, while the strength of the toughened matrix material only fell 20 percent. Video images of the failing specimen were recorded and showed local failures prior to global collapse of the specimen. These images support the theory of a random distribution of flaws controlling composite failure. Failed specimen appearance, however, seems to be a misleading indication of the cause of failure.
Reeder, James R.↗
Comparison of the Compressive Strengths for Stitched and Toughened Composite Systems
The compression strength of a stitched and a toughened matrix graphite/epoxy composite was determined and compared to a baseline unstitched untoughened composite. Two different layups with a variety of test lengths were tested under both ambient and hot/wet conditions. No significant difference in strength was seen for the different materials when the gage lengths of the specimens were long enough to lead to a buckling failure. For shorter specimens, a 30% reduction in strength from the baseline was seen due to stitching for both a 48-ply quasi-isotropic and a (0/45/0/-45/90/-45/0/45/0)s laminate. Analysis of the results suggested that the decrease in strength was due to increased fiber misalignment due to the stitches. An observed increasing strength with decreasing gage length, which was seen for all materials, was explained with a size effect model. The model assumed a random distribution of flaws (misaligned fibers). The toughened material showed a small increase in strength over the baseline material for both laminates presumably due to the compensating effects of a more compliant matrix and straighter fibers in the toughened material. The hot/wet strength of the stitched and baseline material fell 30% below their ambient strengths for shorter, non-buckling specimen, while the strength of the toughened matrix material only fell 20%. Video images of the failing specimen were recorded and showed local failures prior to global collapse of the specimen. These images support the theory of a random distribution of flaws controlling composite failure. Failed specimen appearance however, seems to be a misleading indication of the cause of failure.
Reeder, James R.↗
Nanotubular Toughening Inclusions
Conventional toughening agents are typically rubbery materials or small molecular weight molecules, which mostly sacrifice the intrinsic properties of a matrix such as modulus, strength, and thermal stability as side effects. On the other hand, high modulus inclusions tend to reinforce elastic modulus very efficiently, but not the strength very well. For example, mechanical reinforcement with inorganic inclusions often degrades the composite toughness, encountering a frequent catastrophic brittle failure triggered by minute chips and cracks. Thus, toughening generally conflicts with mechanical reinforcement. Carbon nanotubes have been used as efficient reinforcing agents in various applications due to their combination of extraordinary mechanical, electrical, and thermal properties. Moreover, nanotubes can elongate more than 20% without yielding or breaking, and absorb significant amounts of energy during deformation, which enables them to also be an efficient toughening agent, as well as excellent reinforcing inclusion. Accordingly, an improved toughening method is provided by incorporating nanotubular inclusions into a host matrix, such as thermoset and thermoplastic polymers or ceramics without detrimental effects on the matrix's intrinsic physical properties.
Park, Cheol↗
Nanotubular Toughening Inclusions
Conventional toughening agents are typically rubbery materials or small molecular weight molecules, which mostly sacrifice the intrinsic properties of a matrix such as modulus, strength, and thermal stability as side effects. On the other hand, high modulus inclusions tend to reinforce elastic modulus very efficiently, but not the strength very well. For example, mechanical reinforcement with inorganic inclusions often degrades the composite toughness, encountering a frequent catastrophic brittle failure triggered by minute chips and cracks. Thus, toughening generally conflicts with mechanical reinforcement. Carbon nanotubes have been used as efficient reinforcing agents in various applications due to their combination of extraordinary mechanical, electrical, and thermal properties. Moreover, nanotubes can elongate more than 20% without yielding or breaking, and absorb significant amounts of energy during deformation, which enables them to also be an efficient toughening agent, as well as excellent reinforcing inclusion. Accordingly, an improved toughening method is provided by incorporating nanotubular inclusions into a host matrix, such as thermoset and thermoplastic polymers or ceramics without detrimental effects on the intrinsic physical properties of the matrix.
Park, Cheol↗
Large scale polymer toughening of two-dimensional materials revealed by in situ TEM fracture tests and multiscale simulations
Two-dimensional (2D) materials offer significant potential for applications in energy-harvesting devices, batteries, sensors, and transistors. However, their intrinsic brittleness makes them prone to mechanical failure, limiting their practical use. In this work, we perform in situ transmission electron microscopy (TEM) fracture tests on monolayer MoSe2 and uncover an extrinsic toughening effect induced by an ultrathin adsorbed polystyrene adlayer. This adlayer substantially enhances the fracture resistance of the 2D flakes. Through a combination of molecular dynamics simulations and finite element analysis, we elucidate the molecular mechanism behind this toughening effect. Further, it arises from the active crack-bridging behavior of entangled polymer chains and the formation of a fracture process zone that stabilizes crack propagation and increases the energy required for crack extension. The proposed toughening mechanism offers a pathway to improving the mechanical reliability of 2D material-based devices by mitigating the risk of sudden failure.
2D materials↗
Toughening Brittle Bio‐P3HB with Synthetic P3HB of Engineered Stereomicrostructures
Abstract Poly(3‐hydroxybutyrate) (P3HB), a biologically produced, biodegradable natural polyester, exhibits excellent thermal and barrier properties but suffers from mechanical brittleness, largely limiting its applications. Here we report a mono‐material product design strategy to toughen stereoperfect, brittle bio or synthetic P3HB by blending it with stereomicrostructurally engineered P3HB. Through tacticity ([ mm ] from 0 to 100 %) and molecular weight ( M n to 788 kDa) tuning, high‐performance synthetic P3HB materials with tensile strength to ≈30 MPa, fracture strain to ≈800 %, and toughness to 126 MJ m −3 (>110× tougher than bio‐P3HB) have been produced. Physical blending of the brittle P3HB with such P3HB in 10 to 90 wt % dramatically enhances its ductility from ≈5 % to 95–450 % and optical clarity from 19 % to 85 % visible light transmittance while maintaining desirably high elastic modulus (>1 GPa), tensile strength (>35 MPa), and melting temperature (160–170 °C). This P3HB‐toughening‐P3HB methodology departs from the traditional approach of incorporating chemically distinct components to toughen P3HB, which hinders chemical or mechanical recycling, highlighting the potential of the mono‐material product design solely based on biodegradable P3HB to deliver P3HB materials with diverse performance properties.
Zhang, Zhen↗
Toughening Brittle Bio‐P3HB with Synthetic P3HB of Engineered Stereomicrostructures
Abstract Poly(3‐hydroxybutyrate) (P3HB), a biologically produced, biodegradable natural polyester, exhibits excellent thermal and barrier properties but suffers from mechanical brittleness, largely limiting its applications. Here we report a mono‐material product design strategy to toughen stereoperfect, brittle bio or synthetic P3HB by blending it with stereomicrostructurally engineered P3HB. Through tacticity ([ mm ] from 0 to 100 %) and molecular weight ( M n to 788 kDa) tuning, high‐performance synthetic P3HB materials with tensile strength to ≈30 MPa, fracture strain to ≈800 %, and toughness to 126 MJ m −3 (>110× tougher than bio‐P3HB) have been produced. Physical blending of the brittle P3HB with such P3HB in 10 to 90 wt % dramatically enhances its ductility from ≈5 % to 95–450 % and optical clarity from 19 % to 85 % visible light transmittance while maintaining desirably high elastic modulus (>1 GPa), tensile strength (>35 MPa), and melting temperature (160–170 °C). This P3HB‐toughening‐P3HB methodology departs from the traditional approach of incorporating chemically distinct components to toughen P3HB, which hinders chemical or mechanical recycling, highlighting the potential of the mono‐material product design solely based on biodegradable P3HB to deliver P3HB materials with diverse performance properties.
Chemistry↗
Tailoring the Toughening Effects in Two-Dimensional Nanomaterial-Reinforced Ceramic Matrix Composites
Abstract Ceramic matrix composites (CMCs) reinforced by two-dimensional (2D) nanomaterials have shown extraordinary load-carrying capacities, even in the harsh environments required by emerging applications. Their exceptional mechanical performance, especially fracture toughness, primarily arises from their heterogeneous microstructures. The deliberate dispersion of 2D reinforcements enables toughening mechanisms that are extrinsic to the matrix and thus endows the composites with substantial resistance to catastrophic failure. However, the incomplete understanding of the fracture behavior of such nanocomposites, especially the complex energy dissipation process of the matrix/reinforcement interface, limits the development of stronger and tougher CMCs. To overcome these limitations, we investigate crack deflection and energy dissipation in nanocomposites using an extended cohesive shear-lag model. This new model accounts for interfacial debonding and friction, which critically control the toughening of nanocomposites. Our analysis provides mechanistic insights for optimizing the toughening effects of CMCs.
Mechanics↗
The Effect of Cross-Link Density on the Toughening Mechanism of Elastomer-Modified Epoxies
A DGEBA epoxide resin (EPON 828) was elastomer modified by using three different carboxyl terminated butadiene acrylonitrile copolymers. The fracture toughness of these elastomer modified epoxies was measured in terms of the critical strain energy release rate, G sub IC. The toughening mechanism was elucidated using a tensile dilatometry technique. A plot of volume strain versus longitudinal strain often reveals the types of micromechanical deformations occurring in the uniaxial tensile specimen up to yield. Several microscopy techniques were employed to corroborate the tensile dilatometry results. The role of matrix ductility on the toughening mechanism of elastomer modified epoxies was investigated. By reducing the cross link density with various equivalent weight epoxide resins. Fracture toughness was again measured in terms of G sub IC. The characterization of the toughening mechanism was performed using a uniaxial tensile dilatometry technique and corroborated using various microscopy techniques.
Pearson, R. A.↗
Transformation toughened ceramics for the heavy duty diesel engine technology program, phase 2
The objective of this program is to develop an insulating structural ceramic for application in a heavy duty adiabatic diesel engine. The approach is to employ transformation toughening (TT) by additions of zirconia-hafnia solid solution (ZHSS). The feasibility of using ZHSS as a toughening agent in mullite and alumina has been demonstrated in Phase 1 of this work. Based on Phase 1 results, a decision was made to concentrate the Phase 2 effort on process optimization of the TT mullite. A strong factor in that decision was the low thermal conductivity and high thermal shock resistance of the mullite. Results of the Phase 2 effort indicate that optimum toughening of mullite by additions of ZHSS is difficult to achieve due to apparent sensitivity to morphology. The 48 ksi room temperature modulus-of-rupture (MOR) achieved in selected specimens is approximately 50% of the original strength target. The MOR deteriorated to 34 ksi at 800 C.
Musikant, S.↗
Toughening mechanisms in elastomer-modified epoxies. I - Mechanical studies. II - Microscopy studies
Tensile dilatometry at constant displacement rates is presently used to ascertain whether voiding, crazing or shear banding are the deformation mechanisms at work in the toughening of brittle epoxies through the addition of an elastomeric phase. The results obtained for epoxies toughened by various levels of several types of carbonyl-terminated butadiene nitrile liquid rubber indicate that, at low strain rates, the rubber particles simply enhance shear deformation; at sufficiently high strain rates, the particles cavitate and promote further shear deformation. Examinations of these materials are conducted by means of SEM, TEM, and optical microscopy in the second part of this study. Toughening is hypothesized to involve cavitation's relieving of triaxial tension at the crack tip, as well as shear band formation, which creates a plastic zone.
Yee, A. F.↗
Toughened composites; Proceedings of the Symposium, Houston, TX, Mar. 13-15, 1985
The papers presented in this volume provide an overview of current research aimed at the development of tougher high-performance continuous graphite fiber composites for aerospace applications. Topics discussed include toughened composites selection criteria, micromechanisms of fracture in toughened graphite/epoxy laminates, the characterization of edge delamination growth in laminates under fatigue loading, and rate effects on delamination fracture toughness of a toughened graphite/epoxy. Papers are also presented on the development of residual thermal stresses in amorphous and semicrystalline thermoplastic matrix composites, structural property improvements through hybridized composites, and screening of advanced matrix resin systems in high performance aircraft.
Johnston, Norman J.↗