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DOE OSTI2024

Tough and circular glass fiber composites via a tailored dynamic boronic ester interface

Glass fiber reinforced polymer (GFRP) composites are valued for their strength and cost-effectiveness. However, traditional GFRPs often face challenges for end-of-life recycling due to their non-depolymerizable thermoset matrices, and long-term performance due to inadequate interfacial adhesion, which can lead to fiber–matrix delamination. Here, in this work, we have designed dynamic fiber–matrix interfaces to allow tough and closed-loop recyclable GFRPs by utilizing a vitrimer, derived from upcycled polystyrene-b-poly(ethylene-co-butylene)-b-polystyrene (SEBS) with boronic ester (S-Bpin) and amine-based diol crosslinker. The boronic ester groups in S-Bpin form dynamic covalent bonds with the naturally present hydroxyl groups on the unsized GF surface, which eliminates the need for fiber sizing and enables facile closed-loop recyclability of both the fibers and the vitrimer matrix. The resulting strong fiber–matrix interface, depicted by the Raman mapping, leads to a 552% increase in-plane shear toughness (6.2 ± 0.3 MJ m -3 ) and 27% ultimate tensile strength (361 ± 89.2 MPa) compared to those of the conventional epoxy-based matrix (0.95 ± 0.05 MJ m -3 and 264 ± 59.7 MPa, respectively). The network rearrangement through dynamic boronic ester exchange enables fast thermoformability and repairability of micro-cracks at elevated temperatures. Additionally, both the matrix and composite demonstrate strong adhesion to various surfaces including steel and glasses exhibiting ≥6 MPa lap shear strength, which expands their suitability for diverse industrial applications. The readily created dynamic interface between boronic ester functionalized vitrimer and neat GFs presents a promising strategy for developing closed-loop recyclable, multifunctional structural materials, offering a sustainable alternative to non-recyclable thermoset GFRPs and contributes to a circular economy in composite materials.

36 MATERIALS SCIENCE↗

NASA NTRS1990

Microstructure of a SiC/Ti-15-3 composite

A continuous SiC-fiber-reinforced titanium (Ti-15V-3Cr-3Sn-3A1) composite was metallographically examined. Several methods for examining composite materials were investigated and documented. Polishing techniques for this material are described. An interference layering method was developed to reveal the structure of the fiber, the reaction zone, and various phases within the matrix. Microprobe and TEM analyses were performed on the fiber-matrix interface. Detailed descriptions of the fiber distribution and the microstructure of the fiber and matrix are presented.

Lerch, B. A.↗

NASA NTRS1990

Elastic/plastic analyses of advanced composites investigating the use of the compliant layer concept in reducing residual stresses resulting from processing

High residual stresses within intermetallic and metal matrix composite systems can develop upon cooling from the processing temperature to room temperature due to the coefficient of thermal expansion (CTE) mismatch between the fiber and matrix. As a result, within certain composite systems, radial, circumferential, and/or longitudinal cracks have been observed to form at the fiber-matrix interface. The compliant layer concept (insertion of a compensating interface material between the fiber and matrix) was proposed to reduce or eliminate the residual stress buildup during cooling and thus minimize cracking. The viability of the proposed compliant layer concept is investigated both elastically and elastoplastically. A detailed parametric study was conducted using a unit cell model consisting of three concentric cylinders to determine the required character (i.e., thickness and material properties) of the compliant layer as well as its applicability. The unknown compliant layer mechanical properties were expressed as ratios of the corresponding temperature dependent Ti-24Al-11Nb (a/o) matrix properties. The fiber properties taken were those corresponding to SCS-6 (SiC). Results indicate that the compliant layer can be used to reduce, if not eliminate, radial and circumferential residual stresses within the fiber and matrix and therefore also reduce or eliminate the radial cracking. However, with this decrease in in-plane stresses, one obtains an increase in longitudinal stress, thus potentially initiating longitudinal cracking. Guidelines are given for the selection of a specific compliant material, given a perfectly bonded system.

Arnold, Steven M.↗

NASA NTRS1992

Reduction of Thermal Residual Stresses in Advanced Metallic Composites Based upon a Compensating/Compliant Layer Concept

High residual stresses within metal and intermetallic matrix composite systems can develop upon cooling from the processing temperature to room temperature due to the coefficient of thermal expansion (CTE) mismatch between the fiber and matrix. As a result, within certain composite systems, radial, circumferential, and/or longitudinal cracks have been observed to form at the fiber-matrix interface region. The compliant layer concept (insertion of a compensating interface material between the fiber and matrix) has been proposed to reduce or eliminate the residual stress buildup during cooling, and thus minimize cracking. The present study investigates elastic-plastically the viability of the proposed compliant layer concept. A detailed parametric study was conducted utilizing a unit cell model consisting of three concentric cylinders to determine the required character (i.e., thickness and mechanical properties) of the compliant layer as well as its applicability. The unknown compliant layer mechanical properties were expressed as ratios of the corresponding temperature dependent Ti-24Al-11Nb (a/o) matrix properties. The fiber properties taken were those corresponding to SCS-6 (SiC). Results indicated that the compliant layer can be used to reduce, if not eliminate, radial and circumferential residual stresses within the fiber and matrix and therefore also reduce or eliminate the radial cracking. However, with this decrease in in-plane stresses, one obtains an increase in longitudinal stress, thus potentially initiating longitudinal cracking. Guidelines are given for the selection of a specific compensating/ compliant material, given a perfectly bonded system.

S. M. Arnold↗

NASA NTRS1993

Interface considerations in Al2O3/NiAl composite

The fiber-matrix interface requirements in an Al2O3/NiAl composite were examined from theoretical considerations. Several factors that influence the interface bonding requirements were analyzed. These include: (1) residual stresses due to fiber-matrix coefficient of thermal expansion (CTE) mismatch; (2) matrix cracking stress at room temperature; (3) fracture toughness at room temperature; (4) load transfer from the matrix to the fiber and ultimate tensile strength at the use temperature; and (5) creep resistance at high temperature. A relatively weak fiber-matrix bond, with an interfacial shear strength of approximately 15-20 MPa, might be sufficient for attaining the desired mechanical properties in the fiber direction at the use temperature. A weak fiber-matrix bond is also beneficial for increasing the fracture toughness of the composite at room temperature. In contrast, a strong fiber-matrix bond is required to withstand some of the residual stresses resulting from the fiber-matrix CTE mismatch, which are not likely to be reduced significantly by interface coatings. A relatively strong bond is also beneficial in increasing the matrix cracking stress at room temperature. Various interface coating options to accommodate the conflicting bonding requirements were reviewed. One viable coating option is to incorporate a thick, ductile interface layer well bonded to both the fiber and the matrix.

Misra, Ajay K.↗

NASA NTRS1990

Isothermal and nonisothermal fatigue behavior of a metal matrix composite

The isothermal and nonisothermal fatigue resistance of a metal matrix composite (MMC) consisting of Ti-15V-3Cr-3Al-3Sn (Ti-15-3) matrix reinforced by 33 vol pct continuous SiC fibers was investigated. The fibers were nominally oriented parallel to the specimen axis. Isothermal fatigue tests were performed in air at 300 and 550 C. The MMC had good isothermal fatigue resistance at low cyclic stress, with fatigue cracks initiating from fiber-matrix interfaces and foil laminations. At high cyclic stresses, stress relaxation in the matrix reduced isothermal composite fatigue resistance at 550 C. Nonisothermal fatigue loading substantially degraded composite fatigue resistnce. This degradation was produced by a thermomechanical fatigue damage mechanism associated with the fiber-matrix interfaces.

Gabb, T. P.↗

NASA NTRS2016

InSitu SEM Investigation of Microstructural Damage Evolution and Strain Relaxation in a Melt Infiltrated SiC/SiC Composite

With CMC components poised to complete flight certification in turbine engines on commercial aircraft within the near future, there are many efforts within the aerospace community to model the mechanical and environmental degradation of CMCs. Direct observations of damage evolution are needed to support these modeling efforts and provide quantitative measures of damage parameters used in the various models. This study was performed to characterize the damage evolution during tensile loading of a melt infiltrated (MI) silicon carbide reinforced silicon carbide (SiC/SiC) composite. A SiC/SiC tensile coupon was loaded to a maximum global stress of 30 ksi in a tensile fixture within an SEM while observations were made at 5 ksi increments. Both traditional image analysis and DIC (digital image correlation) were used to quantify damage evolution. With the DIC analysis, microscale damage was observed at the fiber-matrix interfaces at stresses as low as 5 ksi. First matrix cracking took place between 20 and 25 ksi, accompanied by an observable relaxation in strain near matrix cracks. Matrix crack opening measurements at the maximum load ranged from 200 nm to 1.5 m. Crack opening along the fiber-matrix interface was also characterized as a function of load and angular position relative to the loading axis. This characterization was funded by NASA GRC and was performed to support NASA GRC modeling of SiC/SiC environmental degradation

testing↗

NASA NTRS1990

Metal matrix composites microfracture: Computational simulation

Fiber/matrix fracture and fiber-matrix interface debonding in a metal matrix composite (MMC) are computationally simulated. These simulations are part of a research activity to develop computational methods for microfracture, microfracture propagation and fracture toughness of the metal matrix composites. The three-dimensional finite element model used in the simulation consists of a group of nine unidirectional fibers in three by three unit cell array of SiC/Ti15 metal matrix composite with a fiber volume ration of 0.35. This computational procedure is used to predict the fracture process and establish the hierarchy of fracture modes based on strain energy release rate. It is also used to predict stress redistribution to surrounding matrix-fibers due to initial and progressive fracture of fiber/matrix and due to debonding of fiber-matrix interface. Microfracture results for various loading cases such as longitudinal, transverse, shear and bending are presented and discussed. Step-by-step procedures are outlined to evaluate composite microfracture for a given composite system.

Mital, Subodh K.↗

NASA NTRS1990

Metal matrix composites microfracture - Computational simulation

Mital, S. K.↗

DOE OSTI2026

Uncertainty quantification for competing failure mechanisms in unidirectionally reinforced carbon–carbon composites

Microstructure-informed finite element models play a key role in the carbon–carbon composite design process. Variability in manufacturing process parameters and experimental limitations introduce model parameter uncertainty. This study quantifies the effect of model parameter uncertainty on transverse tensile fracture behavior and proposes a methodology to predict the failure mode based on competing microscale damage mechanisms. Finite element simulations incorporate fiber–matrix interface debonding with cohesive zones and matrix damage with a smeared crack band approach in a unidirectional carbon–carbon composite. Results from a variance-based global sensitivity analysis identifies interfacial and matrix damage parameters as the primary source of variability in fracture behavior. Sobol’ indices indicate that matrix and cohesive zone strengths contribute 94% of the variance in the effective ultimate stress. A local analysis elucidates the relationship between these constituent strength parameters and failure mode by estimating the probability of cohesive, matrix, and mixed-mode dominated failure. Based on the results for 4000 simulations, 93% exhibit mixed-mode or interfacial dominated failure, which underscores the crucial role of fiber–matrix interface debonding in the transverse tensile failure of carbon–carbon composites. These uncertainty quantification results facilitate more efficient model calibration and provide a framework for microstructure-informed failure predictions in the face of manufacturing-induced uncertainty.

36 MATERIALS SCIENCE↗

NASA NTRS1999

Effects of Fiber/Matrix Interface and its Composition on Mechanical Properties of Hi-Nicalon/Celsian Composites

To evaluate the effects of fiber coatings on composite mechanical properties. unidirectional celsian matrix composites reinforced with uncoated Hi-Nicalon fibers and those precoated with a dual BN/SiC layer in two separate batches (batch 1 and batch 2) were tested in three-point flexure. The uncoated-fiber reinforced composites showed catastrophic failure with strength of 210+/-35 MPa and a flat fracture surface. In contrast, composites reinforced with coated fibers exhibited graceful failure with extensive fiber pullout and showed significantly higher ultimate strengths, 904 and 759 MPa for the batch 1 and 2 coatings. respectively. Fiber push-in tests and microscopic examination indicated no chemical reaction at the uncoated or coated fiber-matrix interfaces that might be responsible for fiber strength degradation. Instead, the low strength of composite with uncoated fibers was due to degradation of the fiber strength from mechanical damage during composite processing. Despite identical processing, the first matrix cracking stresses (Sigma(sub mc)) of the composites reinforced with fibers coated in batch 1 and batch 2 were quite different, 436 and 122 MPa, respectively. The large difference in Sigma(sub mc) of the coated-fiber composites was attributed to differences in fiber sliding stresses (Tau(sub friction)), 121.2+/-48.7 and 10.4+/-3.1 MPa, respectively. for the two composites as determined by the fiber push-in method. Such a large difference in Tau(sub friction). for the two composites was found to be due to the difference in the compositions of the interface coatings. Scanning Auger microprobe analysis revealed the presence of carbon layers between the fiber and BN. and also between the BN and SiC coatings in the composite showing lower Tau(sub friction). This resulted in lower Sigma(sub mc) in agreement with the ACK theory. The ultimate strengths of the two composites depended mainly on the fiber volume fraction and were not significantly effected by Tau(sub friction) values, as expected. The poor reproducibility of the fiber coating composition between the two batches was judged to be the primary source of the large differences in performance of the two composites.

Bansal, Narottam P.↗

NASA NTRS1994

ASTM and VAMAS activities in titanium matrix composites test methods development

Titanium matrix composites (TMC's) are being considered for a number of aerospace applications ranging from high performance engine components to airframe structures in areas that require high stiffness to weight ratios at temperatures up to 400 C. TMC's exhibit unique mechanical behavior due to fiber-matrix interface failures, matrix cracks bridged by fibers, thermo-viscoplastic behavior of the matrix at elevated temperatures, and the development of significant thermal residual stresses in the composite due to fabrication. Standard testing methodology must be developed to reflect the uniqueness of this type of material systems. The purpose of this paper is to review the current activities in ASTM and Versailles Project on Advanced Materials and Standards (VAMAS) that are directed toward the development of standard test methodology for titanium matrix composites.

Johnson, W. S.↗

NASA NTRS1992

Interfacial stress state present in a 'thin-slice' fibre push-out test

An analysis of the stress distributions along the fiber-matrix interface in a 'thin-slice' fiber push-out test is presented for selected test geometries. For the small specimen thicknesses often required to displace large-diameter fibers with high interfacial shear strengths, finite element analysis indicates that large bending stresses may be present. The magnitude of these stresses and their spatial distribution can be very sensitive to the test configuration. For certain test geometries, the specimen configuration itself may alter the interfacial failure process from one which initiates due to a maximum in shear stress near the top surface adjacent to the indentor, to one which involves mixed mode crack growth up from the bottom surface and/or yielding within the matrix near the interface.

Kallas, M. N.↗

NASA NTRS1987

Study of the mechanical behavior of a 2-D carbon-carbon composite

The out-of-plane fracture of a 2-D carbon-carbon composite was observed and characterized to gain an understanding of the factors influencing the stress distribution in such a laminate. Finite element analyses of a two-ply carbon-carbon composite under in-plane, out-of-plane, and thermal loading were performed. Under in-plane loading all components of stress were strong functions of geometry. Additionally, large thermal stresses were predicted. Out-of-plane tensile tests revealed that failure was interlaminar, and that cracks propagated along the fiber-matrix interface. An elasticity solution was utilized to analyze an orthotropic fiber in an isotropic matrix under uniform thermal load. The analysis reveals that the stress distributions in a transversely orthotropic fiber are radically different than those predicted assuming the fiber to be transversely isotropic.

Avery, W. B.↗

NASA NTRS2019

Computational Micromechanics Model for the Analysis of Fiber Kinking in Unidirectional FRP

A computational micromechanics (CMM) model is developed to analyze fiber kinking, which is a failure mechanism that takes place in fiber-reinforced composites when they are loaded under longitudinal compression. The CMM model consists of a single AS4 carbon fiber with an initial misalignment embedded in an 8552 polymer matrix. The deformation of the model is governed by periodic boundary conditions (PBC). The relatively simple CMM model enables the evaluation of the role played by initial misalignment of the fiber, shear yielding of the matrix and fiber-matrix debonding. A novel microscale experimental technique devoted to the characterization of the longitudinal compressive strength of the fibers, X(sup f)(sub c) , was developed. By exercising the model and comparing it with several existing models in the literature, the nonlinear shear response of the composite lamina was shown to play a fundamental role not only in the prediction of the compressive strength X(sub c), but also during the post-peak regime in terms of residual stress σ(sub r) and fiber rotation φ. Finally, the influence of the fiber-matrix interface damage (not considered in most other fiber kinking models) on the fiber kinking phenomenon was assessed through a parametric study.

Polymer-matrix composites (PMC)↗

DOE OSTI2023

The combined effect of temperature and seawater on the compression properties of carbon fiber vinyl ester composites for sandwich structures

For naval applications, composite sandwich structures are of significant interest, and are often manufactured using thin (2 to 4 mm) composite facings made from carbon or glass fiber reinforcement, attached to a thick (25 to 50 mm) section of PVC cellular foam or balsa wood-based core materials using a suitable polymeric resin. In the present study, we focus on the hygrothermal effect on the fiber-dominated compression properties of carbon fiber reinforced vinyl ester resin based polymeric composite (CF/VE), used as “skin” for a polymeric composite sandwich material. Hygrothermal conditioning is achieved by saturating samples in simulated seawater at 40°C. Compression properties are evaluated for coupons extracted along warp and fill undergoing- no conditioning, conditioning till saturation (up to 6 months), and long-term conditioning (2 years). Sea-water saturation yields in up to 12% drop in compression strength with a further 3–4% drop resulting from long-term conditioning. No statistically significant modulus degradation is noticed due to short or long-term hygrothermal exposure. The failure mechanism of the warp extracted coupon, which fails in a splitting failure mode originating due to the delamination between the 0/90 interface, or the fill extracted coupon, which fails due to the instability caused by tow micro-buckling, remains unchanged due to combined exposure (short or long-term) of seawater and temperature. The loss in strength is attributed to the degradation of the fiber-matrix interface, which is validated via conducting single fiber push-in tests with a nominal diameter of 7 micron for conditioned and unconditioned coupons.

Engineering↗

DOE OSTI2022

An Engineered Multifunctional Composite for Passive Sensing, Power Harvesting, and In Situ Damage Identification with Enhanced Mechanical Performance

A multifunctional fiber-reinforced composite with passive self-sensing, energy-harvesting, and damage detection capabilities is presented. In this work, barium titanate piezoelectric microparticles are deposited on basalt fibers by a scalable, low-cost, environmentally friendly continuous feed-through process. The resulting composite derives a superior interlaminar shear strength from the microparticle-modified fiber–matrix interfaces. The composite also demonstrates passive self-sensing capabilities that produce electrical signals proportional to various dynamic loading events. Vibration and strain-controlled experiments are performed on composite beams to quantify the sensitivity and power output as a function of input acceleration and strain. Furthermore, these composite-generated electrical signals are used to identify in situ damage initiation for structural health monitoring to inform composite damage prior to structural failure. In brief, this truly multifunctional composite simultaneously displays a sensitivity of 0.5–2.6 mV g -1 at a resolution of 0.045–0.20g (g = gravitational acceleration), energy harvesting in the range of nW cc -1 , and prediction of early damage by exhibiting 0.017–1.17 mV peaks in voltage–time history profiles while assuring ≈20% improved interlaminar shear strength.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1993

Effect of thermal cycling on interface bonding requirements in Al2O3 fiber-reinforced superalloy composites

CTE (coefficient of thermal expansion) mismatch-induced stresses as they affect the fiber-matrix bond integrity of Al2O3 fiber-reinforced superalloy composites are examined. Of the three individual stress components, only the radial stress directly affects the integrity of the fiber-matrix interface. It is noted that a compressive radial stress leads to a clamping action on the fiber and is therefore beneficial to the integrity of the fiber-matrix bond. A radial tensile stress, on the other hand, can cause debonding of the fiber from the matrix for a weak fiber-matrix bond.

Misra, Ajay K.↗