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DOE OSTI2026

Microfibril orientation and compositional heterogeneity in fiber and vessel cell walls of poplar xylem studied by AFM-IR and SFG spectroscopy

Understanding the structural organization of cellulose microfibrils (CMFs) within individual plant cell walls is essential for connecting cell wall architecture to its mechanical and physiological functions. However, due to the complex hierarchical structure and nanoscale heterogeneity of cell walls, it remains technically challenging to resolve detailed compositional and orientational information at subcellular levels of individual cell walls. This study investigates the internal 3D structure, chemical composition, and sublayer organization of fiber and vessel cell walls in the xylem tissue of a two-year-old field-grown hybrid poplar tree (Populus alba × P. glandulosa) using photothermal atomic force microscopy coupled with infrared spectroscopy (AFM-IR) and sum frequency generation (SFG) hyperspectral microscopy. AFM-IR provided nanoscale chemical imaging, revealing localized compositional heterogeneity, including variations between adjacent cell walls and transitional layers beyond the traditional S1, S2, and S3 sublayers. SFG microscopy revealed that CMFs in fiber walls are highly aligned along the stem axis, consistent with their role in mechanical support, while vessel cell walls exhibited slightly tilted CMFs, reflecting their function in hydraulic transport. Together, these results offer new insights into cell-type-specific CMF organization and compositional gradients in hybrid poplar xylem. These findings highlight the structural and chemical complexity of secondary cell walls in woody plants and demonstrate the value of AFM-IR and SFG spectroscopy in elucidating plant cell wall architecture.

60 APPLIED LIFE SCIENCES↗

NASA NTRS1980

Graphite fiber surface treatment to improve char retention and increase fiber clumping

Composites containing carbon and graphite fibers can release fibers into the atmosphere during a fire. This release can potentially cause failure in some types of electrical equipment. Reduced fiber dispersion during and after combustion will reduce risks. Epoxidized char forming systems were synthesized which will react with commercially available surface treated carbon fiber. Fibers modified with these char formers retained adhesion in a specific epoxy matrix resin. Small scale combustion testing indicates that using these char former modified fibers in laminates will help to reduce the dispersement of fibers resulting from exposure to fire without sacrificing resin to fiber adhesion.

Paul, J. T., Jr.↗

NASA NTRS1989

The use of curvilinear fiber format in composite structure design

This paper investigates the gains in structural efficiency that can be achieved by aligning the fibers in some or all of the layers in a laminate with the principal stress directions in those layers. The name curvilinear fiber format is given to this idea. The problem studied is a plate with a central circular hole subjected to a uniaxial tensile load. An iteration scheme is used to find the fiber directions at each point in the laminate. Two failure criteria are used to evaluate the tensile load capacity of the plates with a curvilinear format, and for comparison, counterpart plates with a conventional straightline fiber format. The curvilinear designs for improved tensile capacity are then checked for buckling resistance. It is concluded that gains in efficiency can be realized with the curvilinear format.

Hyer, M. W.↗

NASA NTRS1998

Method of Manufacturing Carbon Fiber Reinforced Carbon Composite Valves

A method for forming a carbon composite valve for internal combustion engines is discussed. The process includes the steps of braiding carbon fiber into a rope thereby forming a cylindrically shaped valve stem portion and continuing to braid said fiber while introducing into the braiding carbon fiber rope a carbon matrix plug having an outer surface in a net shape of a valve head thereby forming a valve head portion. The said carbon matrix plug acting as a mandrel over which said carbon fiber rope is braided, said carbon fiber rope and carbon matrix plug forming a valve head portion suitable for mating with a valve seat; cutting said braided carbon valve stem portion at one end to form a valve tip and cutting said braided carbon fiber after said valve head portion to form a valve face and thus provide a composite valve preform; and densifying said preform by embedding the braided carbon in a matrix of carbon to convert said valve stem portion to a valve stem and said valve head portion to a valve head thereby providing said composite valve.

Rivers, H. Kevin↗

NASA NTRS1978

Fiber reinforced PMR polyimide composites

Commercially obtained PMR-15 polyimide prepregs with S-glass and graphite fiber reinforcements were evaluated along with in-house prepared glass and graphite cloth PMR 2 materials. A novel autoclave approach was conceived and used to demonstrate that both the PMR systems respond to 1.4 MPa (200 psi) autoclave pressures to produce void free composites equivalent to die molded laminates. Isothermal gravimetric analysis and subsequent mechanical property tests indicated that the PMR 2 system was significantly superior in thermo-oxidative stability, and that S-glass reinforcements may contribute to the accelerated degradation of composites at 316 C (600 F) when compared to graphite fiber reinforced composites. Fully reversed bending fatigue experiments were conducted with a type of fixture unused for organic matrix composites. These studies indicated that the graphite fiber composites were clearly superior in fatigue resistance to the glass fiber reinforced material and that PMR matrix composite systems yield performance of the same order as composite materials employing other families of matrices.

Cavano, P. J.↗

NASA NTRS2019

Automated Fiber Placement of Composite Wind Tunnel Blades: Process Planning and Manufacturing

The ability to accurately manufacture large complex shapes in a consistent and repeatable manner has led to Automated Fiber Placement (AFP) being the predominant mode of manufacturing for large composite aerospace structures today. Currently, AFP is being considered for medium- and small-scale parts. Composite wind tunnel blades have traditionally been fabricated by hand layup for pre-impregnated or dry fabrics with resin infusion. Though well proven, the traditional fabrication method is laborious and tedious, and hence expensive. The project described in this paper used the Integral Structural Assembly of Advanced Composites (ISAAC) facility at the NASA Langley Research Center to build a manufacturing demonstration unit (MDU) with a shape representative of a wind tunnel blade. This MDU is used to discuss tooling, process planning, and fabrication. Additionally, details of the generic manufacturing workflow are presented.

Harik, Ramy↗

DOE OSTI2020

Mechanical Characterization of High-Temperature Carbon Fiber-Polyphenylene Sulfide Composites for Large Area Extrusion Deposition Additive Manufacturing

Additive manufacturing (AM) is evolving from rapid prototyping to production of structural components. The widespread application of AM demands a high level of mechanical performance from these components, and it is therefore essential to improve feedstock material in order to meet these mechanical expectations. However, compared to traditional manufacturing techniques, the mechanical properties of AM materials and their resulting components are not well understood. In this study, we investigated the processability, microstructure, and mechanical performance of twin-screw compounded short carbon fiber reinforced polyphenylene sulfide (PPS) pellets as a feedstock material for big area AM (BAAM). The performance of the AM components was compared to that of traditional processing methods, namely injection molding (IM) and extrusion-compression molding (ECM). It was found that the AM composites exhibited 118% lower tensile strength and 55% lower tensile modulus when compared to traditional injection molding composite specimens; however, AM composites exhibited comparable properties to ECM composites. This response was attributed to highly aligned fibers in IM and AM samples. However, the AM composites contained porosity (15.5% volume), which reduced their mechanical properties in comparison to ECM composites. Finally, the IM process showed the maximum amount of fiber attrition with minimum porosity (0.007% volume), while the ECM process exhibited the least fiber attrition with 4.3% volume porosity.

36 MATERIALS SCIENCE↗

NASA NTRS2016

Time-Dependent Stress Rupture Strength Degradation of Hi-Nicalon Fiber-Reinforced Silicon Carbide Composites at Intermediate Temperatures

The stress rupture strength of silicon carbide fiber-reinforced silicon carbide composites with a boron nitride fiber coating decreases with time within the intermediate temperature range of 700 to 950 degree Celsius. Various theories have been proposed to explain the cause of the time-dependent stress rupture strength. The objective of this paper is to investigate the relative significance of the various theories for the time-dependent strength of silicon carbide fiber-reinforced silicon carbide composites. This is achieved through the development of a numerically based progressive failure analysis routine and through the application of the routine to simulate the composite stress rupture tests. The progressive failure routine is a time-marching routine with an iterative loop between a probability of fiber survival equation and a force equilibrium equation within each time step. Failure of the composite is assumed to initiate near a matrix crack and the progression of fiber failures occurs by global load sharing. The probability of survival equation is derived from consideration of the strength of ceramic fibers with randomly occurring and slow growing flaws as well as the mechanical interaction between the fibers and matrix near a matrix crack. The force equilibrium equation follows from the global load sharing presumption. The results of progressive failure analyses of the composite tests suggest that the relationship between time and stress-rupture strength is attributed almost entirely to the slow flaw growth within the fibers. Although other mechanisms may be present, they appear to have only a minor influence on the observed time-dependent behavior.

Progressive Failure Analysis↗

NASA NTRS2002

Characterization of C/SiC Ceramic Matrix Composites (CMCs) with Novel Interface Fiber Coatings

Ceramic Matrix Composites (CMCs) are attractive candidate materials in the aerospace industry due to their high specific strength, low density and higher temperature capabilities. The National Aeronautics and Space Administration (NASA) is pursuing the use of CMC components in advanced Reusable Launch Vehicle (RLV) propulsion applications. Carbon fiber-reinforced silicon carbide (C/SiQ is the primary material of interest for a variety of RLV propulsion applications. These composites offer high-strength carbon fibers and a high modulus, oxidation-resistant matrix. For comparison, two types of carbon fibers were processed with novel types of interface coatings (multilayer and pseudoporous). For RLV propulsion applications, environmental durability will be critical. The coatings show promise of protecting the carbon fibers from the oxidizing environment. The strengths and microstructures of these composite materials are presented.

Petko, Jeanne F.↗

NASA NTRS2000

Fabrication of Fiber-Reinforced Celsian Matrix Composites

A method has been developed for the fabrication of small diameter, multifilament tow fiber reinforced ceramic matrix composites. Its application has been successfully demonstrated for the Hi-Nicalon/celsian system. Strong and tough celsian matrix composites, reinforced with BN/SiC-coated Hi-Nicalon fibers, have been fabricated by infiltrating the fiber tows with the matrix slurry, winding the tows on a drum, cutting and stacking of the prepreg tapes in the desired orientation, and hot pressing. The monoclinic celsian phase in the matrix was produced in situ, during hot pressing, from the 0.75BaO-0.25SrO-Al2O3-2SiO2 mixed precursor synthesized by solid state reaction from metal oxides. Hot pressing resulted in almost fully dense fiber-reinforced composites. The unidirectional composites having approx. 42 vol% of fibers exhibited graceful failure with extensive fiber pullout in three-point bend tests at room temperature. Values of yield stress and strain were 435 +/- 35 MPa and 0.27 +/- 0.01 percent, respectively, and ultimate strengths of 900 +/- 60 MPa were observed. The Young's modulus of the composites was measured to be 165 +/- 5 GPa.

Bansal, Narottam P.↗

NASA NTRS2002

Characterization of C/SiC Ceramic Matrix Composites (CMCs) with Novel Interface Fiber Coatings

Ceramic Matrix Composites (CMCs) are attractive candidate aerospace materials due to their high specific strength, low density and high temperature capabilities. The National Aeronautics and Space Administration (NASA) is pursuing the use of CMC components in advanced Reusable Launch Vehicle (RLV) propulsion applications. Carbon fiber-reinforced silicon carbide (C/SiC) is the primary material of interest for a variety of RLV propulsion applications. These composites consist of high-strength carbon fibers and a high modulus, oxidation resistant matrix. For RLV propulsion applications, environmental durability will be critical. Two types of carbon fibers were processed with both standard (pyrolytic carbon) and novel (multilayer and pseudoporous) types of interface coatings as part of a study investigating various combinations of constituents. The benefit of protecting the composites with a surface sealant was also investigated. The strengths, durability in oxidizing environments, and microstructures of these developmental composite materials are presented. The novel interface coatings and the surface sealant show promise for protecting the carbon fibers from the oxidizing environment.

Petko, Jeanne F.↗

NASA NTRS1979

Elastic moduli of transversely isotropic graphite fibers and their composites

The paper demonstrates that it is possible to calculate the complete set of elastic mechanical properties for graphite-epoxy fiber-reinforced materials at any fiber-volume fraction by modifying equations previously developed to include transversely isotropic graphite-fiber properties. Experimental verification of the modified equations is demonstrated by using these equations to curve fit elastic-property data obtained ultrasonically over a range of fiber-volume fractions. Material systems under consideration are T300/5208, AS-3501 and Modomor II/LY558 graphite epoxy. Using the modified equations it is possible to extrapolate for fiber properties. From Modomor II/LY558 ultrasonic data, it is shown that five out of seven extrapolated graphite-fiber properties are consistent with the assumption that graphite fibers are transversely isotropic. Elastic properties for T300/5208 and AS-3501 are ultrasonically evaluated by propagating stress waves through six individual specimens cut at various angles from a block of unidirectional material. Particular attention is devoted to specimen dimensions. To demonstrate the need for accurately calculating or experimentally measuring all lamina elastic properties, a brief discussion is included on the effect that variations in lamina elastic properties have on calculating interlaminar stresses.

Kriz, R. D.↗

NASA NTRS2002

Structural Health Monitoring of Composite Materials Using Distributed Fiber Bragg Sensors

Health monitoring of polymer matrix composite materials using fiber optic Bragg grating (FBG) sensors is accomplished using a tunable IR (infrared) laser via transmission mode. Results are presented from experiments of composite structures with FBG's embedded at various orientations, and surface measurements of various cryogenic composite vessels.

Grant, Joseph↗

NASA NTRS1990

Finite element analysis and optimization of composite structures

Linearly elastic fiber reinforced composite discs and laminates in plane stress with variable local orientation and concentration of one or two fiber fields embedded in the matrix material, are considered. The thicknesses and the domain of the discs or laminates are assumed to be given, together with prescribed boundary conditions and in-plane loading along the edge. The problem under study consists in determining throughout the structural domain the optimum orientations and concentrations of the fiber fields in such a way as to maximize the integral stiffness of the composite disc or laminate under the seven loading. Minimization of the integral stiffness can also be performed. The optimization is performed subject to a prescribed bound on the total cost or weight of the composite that for given unit cost factors or specific weights determines the amounts of fiber and matrix materials in the structure. Examples are presented.

Thomsen, Jan↗

DOE OSTI2020

Structure and composition of blueberry fiber pectin and xyloglucan that bind anthocyanins during fruit puree processing

Blueberry is a well-known source of antioxidants and prebiotic dietary fiber yet the fate of these health-beneficial ingredients during fruit processing it is not understood. Detailed composition and structure of blueberry pomace (PF) remaining after commercial blueberry fruit puree processing, as well as the water soluble and water insoluble fractions, were determined. The PF was comprised of dietary fiber (60.8%) that was largely insoluble (46.2% vs. 14.6% soluble dietary fiber) pectin, xyloglucan, arabinoxylan and mannan polysaccharides, fructose (11.22%) and glucose (10.37%) free sugars, protein (9%), fat (5%), and anthocyanins (6444.5 μg/g). The most abundant anthocyanins detected in PF were malvidin 3-arabinoside and peonidin 3-glucoside and the pectin was determined to be methyl-esterified and acetylated rhamnogalacturonan I with a 4,5-unsaturated function at the non-reducing end based on oligosaccharide structural analysis. Blueberry PF xyloglucan oligosaccharide side chain structures included xylose, arabinose and galactose consistent with arabino-xyloglucan structure. Additionally, microwave-assisted extraction of blueberry PF (pH 2 for 10 min at 80 °C) was performed to more clearly elucidate pectin structure, and revealed a pectin polymer with high molar mass (1072 kDa) and viscosity that was dependent upon the molar mass. A random coil shape was confirmed for both the blueberry PF and microwave extracted blueberry pectin, which agreed with previous reports that flexible blueberry pectin contributes to strong anthocyanin binding. In summary, the blueberry pomace anthocyanin content was slightly higher than that reported for fresh whole blueberry fruit, which suggests that most blueberry anthocyanins adhered to the pomace fiber, and most likely the insoluble pectin, during and after processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2002

Investigation of Structural Properties of Carbon-Epoxy Composites Using Fiber-Bragg Gratings

Fiber Bragg-gratings are embedded in carbon-epoxy laminates as well as bonded on the surface of cylindrical structures fabricated out of such composites. Structural properties of such composites is investigated. The measurements include stress-strain relation in laminates and Poisson's ratio in several specimens with varying orientation of the optical fiber Bragg-sensor with respect to the carbon fiber in an epoxy matrix. Additionally, Bragg gratings are bonded on the surface of cylinders fabricated out of carbon-epoxy composites and longitudinal and hoop strain on the surface is measured.

Grant, J.↗

NASA NTRS1988

Continuous fiber ceramic matrix composites for heat engine components

High strength at elevated temperatures, low density, resistance to wear, and abundance of nonstrategic raw materials make structural ceramics attractive for advanced heat engine applications. Unfortunately, ceramics have a low fracture toughness and fail catastrophically because of overload, impact, and contact stresses. Ceramic matrix composites provide the means to achieve improved fracture toughness while retaining desirable characteristics, such as high strength and low density. Materials scientists and engineers are trying to develop the ideal fibers and matrices to achieve the optimum ceramic matrix composite properties. A need exists for the development of failure models for the design of ceramic matrix composite heat engine components. Phenomenological failure models are currently the most frequently used in industry, but they are deterministic and do not adequately describe ceramic matrix composite behavior. Semi-empirical models were proposed, which relate the failure of notched composite laminates to the stress a characteristic distance away from the notch. Shear lag models describe composite failure modes at the micromechanics level. The enhanced matrix cracking stress occurs at the same applied stress level predicted by the two models of steady state cracking. Finally, statistical models take into consideration the distribution in composite failure strength. The intent is to develop these models into computer algorithms for the failure analysis of ceramic matrix composites under monotonically increasing loads. The algorithms will be included in a postprocessor to general purpose finite element programs.

Tripp, David E.↗

NASA NTRS2002

Fracture Mechanisms For SiC Fibers And SiC/SiC Composites Under Stress-Rupture Conditions at High Temperatures

The successful application of SiC/SiC ceramic matrix composites as high-temperature structural materials depends strongly on maximizing the fracture or rupture life of the load-bearing fiber and matrix constituents. Using high-temperature data measured under stress-rupture test conditions, this study examines in a mechanistic manner the effects of various intrinsic and extrinsic factors on the creep and fracture behavior of a variety of SiC fiber types. It is shown that although some fiber types fracture during a large primary creep stage, the fiber creep rate just prior to fracture plays a key role in determining fiber rupture time (Monkman-Grant theory). If it is assumed that SiC matrices rupture in a similar manner as fibers with the same microstructures, one can develop simple mechanistic models to analyze and optimize the stress-rupture behavior of SiC/SiC composites for applied stresses that are initially below matrix cracking.

DiCarlo, James A.↗