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Composites: Processing and Fabrication Methodologies of Nonoxide Ceramic Composites. Processing HfB2 Composites for Use in Extreme Environments

HfB2 and ZrB2 composites containing SiC are known to have good thermal shock and configurational stability at elevated temperatures. These are promising ultra-high temperature ceramics (UHTCs) for use on the sharp leading edges of next generation space vehicles. Sharp leading edges on these vehicles will need to: withstand repeated exposures to temperatures > 2200 C in oxidizing environments; have good thermal shock and ablation resistance; and withstand the mechanical stress of launch and reentry. The HfB2/SiC composite is currently undergoing processing improvements in an effort to better the performance of a material that has been studied for approx. 35 years. The potential for HfB2/SiC composites to meet the requirements of hypersonic flight depends on controlling processing techniques. This presentation will focus on understanding processing steps now being undertaken to optimize the material properties of HfB2/SiC composites at NASA Ames Research Center. Correlation between processing techniques and microstructure will be shown. Preliminary oxidation studies will also be discussed.

Gusman, Michael I.

Composite materials. Volume 3 - Engineering applications of composites. Volume 4 - Metallic matrix composites. Volume 8 - Structural design and analysis, Part 2

This volume discusses a vaety of applications of both low- and high-cost composite materials in a number of selected engineering fields. The text stresses the use of fiber-reinforced composites, along with interesting material systems used in the electrical and nuclear industries. As to technology transfer, a similarity is noted between many of the reasons responsible for the utilization of composites and those problems requiring urgent solution, such as mechanized fabrication processes and design for production. Features topics include road transportation, rail transportation, civil aircraft, space vehicles, builing industry, chemical plants, and appliances and equipment. The laminate orientation code devised by Air Force materials laboratory is included. Individual items are announced in this issue.

Noton, B. R.

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.

A Groundmass Composition for EET 79001A Using a Novel Microprobe Technique for Estimating Bulk Compositions. Lithology A as an Impact Melt?

Petrologic investigation of the shergottites has been hampered by the fact that most of these meteorites are partial cumulates. Two lines of inquiry have been used to evaluate the compositions of parental liquids: (i) perform melting experiments at different pressures and temperatures until the compositions of cumulate crystal cores are reproduced [e.g., 1]; and (ii) use point-counting techniques to reconstruct the compositions of intercumulus liquids [e.g., 2]. The second of these methods is hampered by the approximate nature of the technique. In effect, element maps are used to construct mineral modes; and average mineral compositions are then converted into bulk compositions. This method works well when the mineral phases are homogeneous [3]. However, when minerals are zoned, with narrow rims contributing disproportionately to the mineral volume, this method becomes problematic. Decisions need to be made about the average composition of the various zones within crystals. And, further, the proportions of those zones also need to be defined. We have developed a new microprobe technique to see whether the point-count method of determining intercumulus liquid composition is realistic. In our technique, the approximating decisions of earlier methods are unnecessary because each pixel of our x-ray maps is turned into a complete eleven-element quantitative analysis. The success or failure of our technique can then be determined by experimentation. As discussed earlier, experiments on our point-count composition can then be used to see whether experimental liquidus phases successfully reproduce natural mineral compositions. Regardless of our ultimate outcome in retrieving shergottite parent liquids, we believe our pixel-bypixel analysis technique represents a giant step forward in documenting thin-section modes and compositions. For a third time, we have analyzed the groundmass composition of EET 79001, 68 [Eg]. The first estimate of Eg was made by [4] and later modified by [5], to take phase diagram considerations into account. The Eg composition of [4] was too olivine normative to be the true Eg composition, because the ,68 groundmass contains no forsteritic olivine. A later mapping by [2] basically reconfirmed the modifications of [5]. However, even the modified composition of [5] has olivine on the liquidus for ~50 C before low-Ca pyroxene appears [6].

Jones, John H.

Effects of Fiber Coating Composition on Mechanical Behavior of Silicon Carbide Fiber-Reinforced Celsian Composites

Celsian matrix composites reinforced with Hi-Nicalon fibers, precoated with a dual layer of BN/SiC by chemical vapor deposition in two separate batches, were fabricated. Mechanical properties of the composites were measured in three-point flexure. Despite supposedly identical processing, the composite panels fabricated with fibers coated in two batches exhibited substantially different mechanical behavior. The first matrix cracking stresses (sigma(sub mc)) of the composites reinforced with fibers coated in batch 1 and batch 2 were 436 and 122 MPa, respectively. This large difference in sigma(sub mc) 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 values of 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, 904 and 759 MPa, 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.

Thermo-Oxidative Stability of Graphite/PMR-15 Composites: Effect of Fiber Surface Modification on Composite Shear Properties

Experiments were conducted to establish a correlation between the weight loss of a polyimide (PMR- 15) matrix and graphite fibers and the in-plane shear properties of their unidirectional composites subjected to different isothermal aging times up to 1000 hr at 316 C. The role of fiber surface treatment on the composite degradation during the thermo-oxidative aging was investigated by using A4 graphite fibers with three surface modifications: untreated (AU-4), surface treated (AS-4), and surface treated and sized with an epoxy-compatible sizing (AS-4G). The weight loss of the matrix fibers, and composites was determined during the aging. The effect of thermal aging was seen in all the fiber samples in terms of weight loss and reduction in fiber diameter. Calculated values of weight loss fluxes for different surfaces of rectangular unidirectional composite plates showed that the largest weight loss occurred at those cut surfaces where fibers were perpendicular to the surface. Consequently, the largest amount of damage was also noted on these cut surfaces. Optical observation of the neat matrix and composite plates subjected to different aging times revealed that the degradation (such as matrix microcracking and void growth) occurred in a thin surface layer near the specimen edges. The in-plane shear modulus of the composites was unaffected by the fiber surface treatment and the thermal aging. The shear strength of the composites with the untreated fibers was the lowest and it decreased with aging. A fracture surface examination of the composites with untreated fibers suggested that the weak interface allowed the oxidation reaction to proceed along the interface and thus expose the inner material to further oxidation. The results indicated that the fiber-matrix interface affected the composite degradation process during its thermal aging and that the the weak interface accelerated the composite degradation.

Madhukar, Madhu S.

Impetus of composite mechanics on test methods for fiber composites

Significant contributions of the three major areas of composite mechanics to the development of test methods are illustrated with selected examples. The areas of composite mechanics include composite micromechanics, composite macromechanics, and laminate theory. The examples can be considered to be representative of the contribution of composite mechanics to the development of composite test methods. The specific examples describe contributions such as criteria for selecting resin matrices for improved composite strength, the 10 deg off-axis tensile test, procedures for configuring hybrids, and the concept of 'reduced bending rigidities'. The pertinent composite mechanics equations associated with each contribution are given and supplemented by tabular and/or graphical data which illustrate the significance of the contribution.

Chamis, C. C.

Effect of Composite Fabrication on the Strength of Single Crystal Al2O3 Fibers in Two Fe-Base Alloy Composites

Continuous single-crystal Al2O3 fibers have been incorporated into a variety of metal and intermetallic matrices and the results have consistently indicated that the fiber strength had been reduced by 32 to 50% during processing. Two iron-based alloys, FeNiCoCrAl and FeAlVCMn, were chosen as matrices for Al2O3 fiber reinforced metal matrix composites (MMC) with the goal of maintaining Al2O3 fiber strength after composite processing. The feasibility of Al2O3/FeNiCoCrAl and Al2O3/FeAlVCMn composite systems for high temperature applications were assessed in terms of fiber-matrix chemical compatibility, interfacial bond strength, and composite tensile properties. The strength of etched-out fibers was significantly improved by choosing matrices containing less reactive elements. The ultimate tensile strength (UTS) values of the composites could generally be predicted with existing models using the strength of etched-out fibers. However, the UTS of the composites were less than desired due to a low fiber Weibull modulus. Acoustic emission analysis during tensile testing was a useful tool for determining the efficiency of the fibers in the composite and for determining the failure mechanism of the composites.

Draper, Susan L.

Metal matrix composite micromechanics: In-situ behavior influence on composite properties

Recent efforts in computational mechanics methods for simulating the nonlinear behavior of metal matrix composites have culminated in the implementation of the Metal Matrix Composite Analyzer (METCAN) computer code. In METCAN material nonlinearity is treated at the constituent (fiber, matrix, and interphase) level where the current material model describes a time-temperature-stress dependency of the constituent properties in a material behavior space. The composite properties are synthesized from the constituent instantaneous properties by virtue of composite micromechanics and macromechanics models. The behavior of metal matrix composites depends on fabrication process variables, in situ fiber and matrix properties, bonding between the fiber and matrix, and/or the properties of an interphase between the fiber and matrix. Specifically, the influence of in situ matrix strength and the interphase degradation on the unidirectional composite stress-strain behavior is examined. These types of studies provide insight into micromechanical behavior that may be helpful in resolving discrepancies between experimentally observed composite behavior and predicted response.

Murthy, P. L. N.

NASA GEOS Composition Forecast Modeling System GEOS-CF v1.0: Stratospheric Composition

The NASA Goddard Earth Observing System (GEOS) Composition Forecast (GEOS-29CF) provides recent estimates and five-day forecasts of atmospheric composition to the public in near-real time. To do this, the GEOS Earth system model is coupled with the GEOS-Chem tropospheric-stratospheric unified chemistry extension (UCX) to represent composition from the surface to the top of the GEOS atmosphere (0.01 hPa). The GEOS-CF system is described, including updates made to the GEOS-Chem UCX mechanism within GEOS-CF for improved representation of stratospheric chemistry. Comparisons are made against balloon, lidar and satellite observations for stratospheric composition, including measurements of ozone (O3) and important nitrogen and chlorine species related to stratospheric O3recovery. The GEOS-CF nudges the stratospheric O3towards the GEOS Forward Processing (GEOS FP) assimilated O3product; as a result the stratospheric O3in the GEOS-CF historical estimate agrees well with observations. During abnormal dynamical and chemical environments such as the 2020 polar vortexes, the GEOS-CF O3forecasts are more realistic than GEOS FP O3forecasts because of the inclusion of the complex GEOS-Chem UCX stratospheric chemistry. Overall, the spatial patterns of the GEOS-CF simulated concentrations of stratospheric composition agree well with satellite observations. However, there are notable biases – such as low NOx and HNO3 in the polar regions and generally low HCl throughout the stratosphere – and future improvements to the chemistry mechanism and emissions are discussed. GEOS-CF is a new tool for the research community and instrument teams observing trace gases in the stratosphere and troposphere, providing near-real-time three-dimensional gridded information on atmospheric composition.

GEOS-CF

A creep model for metallic composites based on matrix testing: Application to Kanthal composites

An anisotropic creep model is formulated for metallic composites with strong fibers and low to moderate fiber volume percent (less than 40 percent). The idealization admits no creep in the local fiber direction and assumes equal creep strength in longitudinal and transverse shear. Identification of the matrix behavior with that of the isotropic limit of the theory permits characterization of the composite through uniaxial creep tests on the matrix material. Constant and step-wise creep tests are required as a data base. The model provides an upper bound on the transverse creep strength of a composite having strong fibers embedded in a particular matrix material. Comparison of the measured transverse strength with the upper bound gives an assessment of the integrity of the composite. Application is made to a Kanthal composite, a model high-temperature composite system. Predictions are made of the creep response of fiber reinforced Kanthal tubes under interior pressure.

Binienda, W. K.

Integrated mechanics for the passive damping of polymer-matrix composites and composite structures

Some recent developments on integrated damping mechanics for unidirectional composites, laminates, and composite structures are reviewed. Simplified damping micromechanics relate the damping of on-axis and off-axis composites to constituent properties, fiber volume ratio, fiber orientation, temperature, and moisture. Laminate and structural damping mechanics for thin composites are summarized. Discrete layer damping mechanics for thick laminates, including the effects of interlaminar shear damping, are developed and semianalytical predictions of modal damping in thick simply supported specialty composite plates are presented. Applications show the advantages of the unified mechanics, and illustrate the effect of fiber volume ratio, fiber orientation, structural geometry, and temperature on the damping. Additional damping properties for composite plates of various laminations, aspect ratios, fiber content, and temperature illustrate the merits and ranges of applicability of each theory (thin or thick laminates).

Saravanos, D. A.

The Effect of Compositional Tailoring on the Thermal Expansion and Tribological Properties of PS300: A Solid Lubricant Composite Coating

This paper describes a research program in which the goal is to alter the thermal expansion coefficient of a composite solid lubricant coating, PS300, by compositional tailoring. PS300 is a plasma sprayed coating consisting of chrome oxide, silver and barium fluoride/calcium fluoride eutectic in NiCr binder. By adjusting the composition, the thermal expansion coefficient can be altered, and hence chosen, to more closely match a selected substrate preventing coating spallation at extreme temperatures. Thermal expansion coefficients (CTE) for a variety of compositions were measured from 25 to 800 C using a commercial dilatometer. The CTE's ranged from 7.0 to 13 x lO(exp -6)/deg C depending on the binder content. Subsequent tribological testing of a modified composition indicated that friction and wear properties were relatively insensitive to compositional tailoring.

DellaCorte, C.

Method for Forming Fiber Reinforced Composite Bodies with Graded Composition and Stress Zones

A near-net, complex shaped ceramic fiber reinforced silicon carbide based composite bodies with graded compositions and stress zones is disclosed. To provide the composite a fiber preform is first fabricated and an interphase is applied by chemical vapor infiltration, sol-gel or polymer processes. This first body is further infiltrated with a polymer mixture containing carbon, and/or silicon carbide, and additional oxide, carbide, or nitride phases forming a second body. One side of the second body is spray coated or infiltrated with slurries containing high thermal expansion and oxidation resistant. crack sealant phases and the other side of this second body is coated with low expansion phase materials to form a third body. This third body consisting of porous carbonaceous matrix surrounding the previously applied interphase materials, is then infiltrated with molten silicon or molten silicon-refractory metal alloys to form a fourth body. The resulting fourth body comprises dense composites consisting of fibers with the desired interphase which are surrounded by silicon carbide and other second phases materials at the outer and inner surfaces comprising material of silicon, germanium, refractory metal suicides, borides, carbides, oxides, and combinations thereof The resulting composite fourth body has different compositional patterns from one side to the other.

Singh, Mrityunjay

Torque Limit for Bolted Joint for Composites: TTTC Properties of Laminated Composites - Part A

The existing design code for torque limit of bolted joints for composites at Marshall Space Flight Center is MSFC-STD-486B, which was originally developed in 1960s for metallic materials. The theoretical basis for this code was a simplified mechanics analysis, which takes into account only the bolt, nut and washers, but not the structural members to be connected. The assumption was that metallic materials would not fail due to the bearing stress at the contact area between washer and the mechanical member. This is true for metallic materials; but for composite materials the results could be completely different. Unlike most metallic materials, laminated composite materials have superior mechanical properties (such as modulus and strength) in the in-plane direction, but not in the out-of-plane, or through-the-thickness (TTT) direction. During the torquing, TTT properties (particularly compressive modulus and compressive strength) play a dominant role in composite failure. Because of this concern, structural design engineers at Marshall are currently using a compromised empirical approach: using 50% of the torque value for composite members. Companies like Boeing is using a similar approach. An initial study was conducted last summer on this topic to develop theoretical model(s) that takes into consideration of composite members. Two simplified models were developed based on stress failure criterion and strain failure criterion, respective. However, these models could not be used to predict the torque limit because of the unavailability of material data, specifically, through-the-thickness compression (TTTC) modulus and strength. Therefore, the task for this summer is to experimentally determine the TTTC properties. Due to the time limitation, only one material has been tested: IM7/8552 with [0 degrees,plus or minus 45 degrees, 90 degree ] configuration. This report focuses the test results and their significance, while the experimentation will be described in a separate report by Mr. Kris Kostreva.

Zhao, Yi

Application of Pi Preform Composite Joints in Fabrication of NASA Composite Crew Module Demonstration Structure

This paper will describe unique and extensive use of pre-woven and impregnated pi cross-sections in fabrication of a carbon composite demonstration structure for the Composite Crew Module (CCM) Program. The program is managed by the NASA Safety and Engineering Center with participants from ten NASA Centers and AFRL. Multiple aerospace contractors are participating in the design development, tooling and fabrication effort as well. The goal of the program is to develop an agency wide design team for composite habitable spacecraft. The specific goals for this development project are: a) To gain hands on experience in design, building and testing a composite crew module. b) To validate key assumptions by resolving composite spacecraft design details through fabrication and testing of hardware. This paper will focus on the design and fabrication issues supporting selection of the Lockheed Martin patented Pi pre-form to provide sound composite joints a numerous locations in the structure. This abstract is based on Preliminary Design data. The final design will continue to evolve through the fall of 2007 with fabrication mostly completed by conference date.

Higgins, John E.

Voluntary Consensus Organization Standards for Nondestructive Evaluation of Thin-Walled Metallic Liners and Composite Overwraps in Composite Overwrapped Pressure Vessels

NASA fracture control requirements outlined in NASA-STD-5009 and NASA-STD-5014 are predicated on the availability and use of sensitive nondestructive evaluation (NDE) methods that can detect and monitor defects, thereby providing data that can be used to predict failure or reduce the risk of failure in fracture critical components. However, in the case of composite materials and components, including composite overwrapped pressure vessels (COPVs), the effect of defects is poorly understood, the NDE methods used to evaluate locate and size defects are typically at lower technical readiness level than analogous NDE methods used for metals, and demonstration studies to verify the probability of detection (POD) are generally lacking or unavailable. These factors together make failure prediction of fracture critical composite materials and components based on size, quantity, or orientation of defects nearly impossible. Also, when inspecting metal liners in as-manufactured COPVs, sensitivity is lost and only the inner surface of the liner is accessible. Also, NDE of COPVs as applied during manufacturing varies significantly from manufacturer to manufacturer and has not yet been standardized. Although requirements exist to perform NDE immediately after manufacturing to establish initial integrity of the parts, procedural detail for NDE of composites is still nonexistent or under development. For example, in practice, only a visual inspection of COPVs is performed during manufacturing and service, leaving in question whether defects of concern, for example, bridging, overwrap winding anomalies, impact damage below visible threshold, out-of-family strain growth, and liner buckling have been adequately detected and monitored. To address these shortcomings, in 2005 the NASA Nondestructive Evaluation Working Group (NNWG) began funding work to develop and adopt standards for nondestructive evaluation of aerospace composites in collaboration with the American Society for Testing and Materials (ASTM) Committee E07 on Nondestructive Testing. Similarly, in 2006 the NASA Engineering and Safety Center (NESC) recommended that nondestructive evaluation methods that can predict composite failure in COPVs should be developed and verified, and integrated into the damage control plan for these vessels

Waller, Jess

Structural CNT Composites Part II: Assessment of CNT Yarns as Reinforcement for Composite Overwrapped Pressure Vessels

Carbon nanotubes (CNTs) are one-dimensional nanomaterials with outstanding electrical and thermal conductivities and mechanical properties. This combination of properties offers routes to enable lightweight structural aerospace components. Recent advances in the manufacturing of CNTs have made bulk forms such as yarns, tapes and sheets available in commercial quantities to permit the evaluation of these materials for aerospace use, where the superior tensile properties of CNT composites can be exploited in tension dominated applications such as composite overwrapped pressure vessels (COPVs). To investigate their utility in this application, aluminum rings were overwrapped with thermoset/CNT yarn composite and their mechanical properties measured. CNT composite overwrap characteristics such as processing method, CNT/resin ratio, and applied tension during CNT yarn winding were varied to determine their effects on the mechanical performance of the CNT composite overwrapped Al rings (CCOARs). Mechanical properties of the CCOARs were measured under static and cyclic loads at room, elevated, and cryogenic temperatures to evaluate their mechanical performance relative to bare Al rings. At room temperature, the breaking load of CCOARs with a 10.8% additional weight due to the CNT yarn/thermoset overwrap increased by over 200% compared to the bare Al ring. The quality of the wound CNT composites was also investigated using x-ray computed tomography.

Kim, Jae-Woo