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At least 55 records · Page 3

Development of test methodology for dynamic mechanical analysis instrumentation

Dynamic mechanical analysis instrumentation was used for the development of specific test methodology in the determination of engineering parameters of selected materials, esp. plastics and elastomers, over a broad range of temperature with selected environment. The methodology for routine procedures was established with specific attention given to sample geometry, sample size, and mounting techniques. The basic software of the duPont 1090 thermal analyzer was used for data reduction which simplify the theoretical interpretation. Clamps were developed which allowed 'relative' damping during the cure cycle to be measured for the fiber-glass supported resin. The correlation of fracture energy 'toughness' (or impact strength) with the low temperature (glassy) relaxation responses for a 'rubber-modified' epoxy system was negative in result because the low-temperature dispersion mode (-80 C) of the modifier coincided with that of the epoxy matrix, making quantitative comparison unrealistic.

Allen, V. R.↗

Solvent Resistant Thermoplastic Composite Matrices

The following approaches improved the solvent resistance and raised the Tg of thermoplastics: end-capping aligomers with ethynyl groups; incorporating ethynyl groups pendent along the polymer chain; and correcting polymers containing pendent ethynyl groups with a low molecular weight diethynyl compound. The following conclusions were reached: (1) film and composite properties off an ethynyl-terminated sulfone were better than those of UDEL (trademark); (2) fracture energy of an ethynyl-terminated sulfone was lower than that of UDEL (trademark); (3) residual palladium in the cured ethynyl-terminated sulfone lower the thermooxidative stability of the cured resin; (4) the properties of a phenoxy resin were altered considerably by placing pendent ethynyl groups along the polymer chain; and (5) property trade-offs must be considered when thermoplastics are modified via reactant groups.

Hergenrother, P. M.↗

The width-tapered double cantilever beam for interlaminar fracture testing

The width-tapered double-cantilever-beam (WTDCB) specimen configuration used to determine the Mode-I interlaminar fracture energy (IFE) of composites has special advantages for routine development work and for quality-assurance purposes. These advantages come primarily from the simplicity of testing and the fact that the specimen is designed for constant change in compliance with crack length, so that the computation of Mode-I IFE is independent of crack length. In this paper, a simplified technique for fabrication and testing WTDCB specimens is described. Also presented are the effects of fiber orientation and specimen dimensions, a comparison of data obtained using the WTDCB specimens and other specimen geometries, and comparison of data obtained at different laboratories. It is concluded that the WTDCB gives interlaminar Mode-I IFE essentially equal to other type specimens, and that it can be used for rapid screening in resin-development work and for quality assurance of composite materials.

Bascom, W. D.↗

Polyimide of Modified Melt Flow and Toughness

Linear aromatic polyphenylene ether sulfideimide (BDSDA/APB) polymer molded, used as resin, and cast into thin films. In effort to improve further both use properties and amenability to process BDSDA/APB, molecular weight of polymer varied by variations in percentage of end capping. Effect of end capping BDSDA/APB determined by measurement of polymer melt viscosity and fracture-energy values for different number average synthesized molecular weights.

St. Clair, T. L.↗

Polyphenylquinoxalines Containing Alkylenedioxy Groups

New polyphenylquinoxalines (PPQ's) prepared from reaction of novel bis(alpha-diketones) with aromatic bis(o-diamines). Contain alkylenedioxy groups in repeating units. Lower glass-transition temperatures and melt viscosities and better processability than all-aromatic PPQ's. Tensile strength, modulus, elongation, adhesive strength, fracture energy, and solvent resistance of new polymers comparable with properties of known PPQ's. Useful as adhesives, coatings, films, and molded products, particularly for aerospace applications.

Hergenrother, Paul M.↗

A microscopy study of composite delamination

Double cantilever beam specimens of carbon fiber-epoxy composites were tested for interlaminar fracture energy. While still under load, the specimens were potted in a clear epoxy polymer. The potted specimens were cut longitudinally into sections 0.6 mm (0.025 in.) or less in thickness and examined using reflection and transmission light microscopy. Massive fiber bridging was observed especially at the crack tip.

Bascom, W. D.↗

Stress corrosion study of PH13-8Mo stainless steel using the Slow Strain Rate Technique

The need for a fast and reliable method to study stress corrosion in metals has caused increased interest in the Slow Strain Rate Technique (SSRT) during the last few decades. PH13-8MoH950 and H1000 round tensile specimens were studied by this method. Percent reduction-in-area, time-to-failure, elongation at fracture, and fracture energy were used to express the loss in ductility, which has been used to indicate susceptibility to stress corrosion cracking (SCC). Results from a 3.5 percent salt solution (corrosive medium) were compared to those in air (inert medium). A tendency to early failure was found when testing in the vicinity of 1.0 x 10(-6) mm/mm/sec in the 3.5 percent salt solution. PH13-8Mo H1000 was found to be less likely to suffer SCC than PH13-8Mo H950. This program showed that the SSRT is promising for the SCC characterization of metals and results can be obtained in much shorter times (18 hr for PH steels) than those required using conventional techniques.

Torres, Pablo D.↗

Adhesive properties of a semi-crystalline polyimide

Adhesive and film properties of a new semi-crystalline polyimide, designated LARC-CPI, having a glass transition temperature of 222 C and a crystalline melt temperature of 350 C are presented. The films exhibited excellent resistance to solvents and strong base. Compact tension specimens from LARC-CPI moldings displayed a fracture energy of 37.8 lb/sq in. Titanium tensile shear specimens gave strengths of 6250 psi initially at 25 C, 7120 psi at 25 C after 1000 hours at 232 C, 2800 psi at 232 C after annealing for 5 hours at 300 C, and 3670 psi at 232 C after 100 hours at 316 C in air.

Hergenrother, P. M.↗

Improving processing and toughness of a high performance composite matrix through an interpenetrating polymer network. VI

The use of a semiinterpenetrating polymer network (SIPN) of the high-performance polyimide NR-150B2 to reduce brittleness and improve processability in the highly crosslinked acetylene-terminated polyimides Thermid LR-600, AL-600, MC-600, and FA-700 is described. The theoretical basis of the SIPN process is reviewed; the preparation and characterization of the neat SIPN resins and unidirectional graphite-fiber composites are explained; and the results are presented in extensive tables, graphs, and micrographs and discussed in detail. Significant increases in fracture energy were observed with SIPN, from 93 J/sq m for unmodified LR-600 to 283-603 J/sq m for the SIPN materials; the room-temperature flexural strength of the unidirectional composites also increased, from 1344 MPa for an unmodified MC-600 composite to 2020-1751 MPa for the SIPN composites. The potential applicability of SIPN-based composites to aerospace structures and electronic components is indicated.

Pater, Ruth H.↗

Push-out tests on a new silicon carbide/reaction-bonded silicon carbide ceramic matrix composite

Fiber push-out tests have been performed on a ceramic matrix composite consisting of carborundum-sintered SiC fibers, with a BN coating, embedded in a reaction-bonded SiC matrix. Analysis of the push-out data, utilizing the most complete theory presently available, shows that one of the fiber/coating/matrix interfaces has a low fracture energy (one-tenth that of the fiber) and a moderate sliding resistance of about 8 MPa. The debonded sliding interface shows some continuous but minor abrasion, which appears to increase the sliding resistance, but overall the system exhibits very clean smooth sliding. The tensile response of a full-scale composite is then modeled using data obtained here and known fiber strengths to demonstrate the good composite behavior predicted for this material.

Curtin, William A.↗

A design of experiments test to define critical spray cleaning parameters for Brulin 815 GD and Jettacin cleaners

Experimental design testing was conducted to identify critical parameters of an aqueous spray process intended for cleaning solid rocket motor metal components (steel and aluminum). A two-level, six-parameter, fractional factorial matrix was constructed and conducted for two cleaners, Brulin 815 GD and Diversey Jettacin. The matrix parameters included cleaner temperature and concentration, wash density, wash pressure, rinse pressure, and dishwasher type. Other spray parameters: nozzle stand-off, rinse water temperature, wash and rinse time, dry conditions, and type of rinse water (deionized) were held constant. Matrix response testing utilized discriminating bond specimens (fracture energy and tensile adhesion strength) which represent critical production bond lines. Overall, Jettacin spray cleaning was insensitive to the range of conditions tested for all parameters and exhibited bond strengths significantly above the TCA test baseline for all bond lines tested. Brulin 815 was sensitive to cleaning temperature, but produced bond strengths above the TCA test baseline even at the lower temperatures. Ultimately, the experimental design database was utilized to recommend process parameter settings for future aqueous spray cleaning characterization work.

Keen, Jill M.↗

Structure-Property Relationships of Bismaleimides

The purpose of this research was to control and systematically vary the network topology of bismaleimides through cure temperature and chemistry (addition of various coreactants) and subsequently attempt to determine structure-mechanical property relationships. Characterization of the bismaleimide structures by dielectric, rheological, and thermal analyses, and density measurements was subsequently correlated with mechanical properties such as modulus, yield strength, fracture energy, and stress relaxation. The model material used in this investigation was 4,4'-BismaleiMidodIphenyl methane (BMI). BMI was coreacted with either 4,4'-Methylene Dianiline (MDA), o,o'-diallyl bisphenol A (DABA) from Ciba Geigy, or Diamino Diphenyl Sulfone (DDS). Three cure paths were employed: a low- temperature cure of 140 C where chain extension should predominate, a high-temperature cure of 220 C where both chain extension and crosslinking should occur simultaneously, and a low-temperature (140 C) cure followed immediately by a high-temperature (220 C) cure where the chain extension reaction or amine addition precedes BMI homopolymerization or crosslinking. Samples of cured and postcured PMR-15 were also tested to determine the effects of postcuring on the mechanical properties. The low-temperature cure condition of BMI/MDA exhibited the highest modulus values for a given mole fraction of BMI with the modulus decreasing with decreasing concentration of BMI. The higher elastic modulus is the result of steric hindrance by unreacted BMI molecules in the glassy state. The moduli values for the high- and low/high-temperature cure conditions of BMI/MDA decreased as the amount of diamine increased. All the moduli values mimic the yield strength and density trends. For the high-temperature cure condition, the room- temperature modulus remained constant with decreasing mole fraction of BMT for the BMI/DABA and BMI/DDS systems. Postcuring PMR-15 increases the modulus over that of the cured material even though density values of cured and postcured PMR were essentially the same. Preliminary results of a continuous and intermittent stress relaxation experiment for BMI:MDA in a 2:1 molar ratio indicate that crosslinking is occurring when the sample is in the undeformed state. Computer simulation of properties such as density, glass transition temperature, and modulus for the low- temperature cure conditions of BMI/MDA and BMI/DABA were completed. The computer modeling was used to help further understand and confirm the structure characterization results. The simulations correctly predicted the trends of these properties versus mole fraction BMI and were extended to other BMI/diamine systems.

Tenteris-Noebe, Anita D.↗

Solid Freeform Fabrication of Continuous Fiber Reinforced Composites for Propulsion Applications

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500'C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible- manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. This is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths With carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites-, they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP process.

Vaidyanathan, R.↗

Solid Free-Form Fabrication of Continuous Fiber Reinforced Composites for Propulsion Application

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500 C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible-manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. M is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths with carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites; they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP processes.

Vaidyanathan, R.↗

Accelerated Strength Testing of Thermoplastic Composites

Constant ramp strength tests on unidirectional thermoplastic composite specimens oriented in the 90 deg. direction were conducted at constant temperatures ranging from 149 C to 232 C. Ramp rates spanning 5 orders of magnitude were tested so that failures occurred in the range from 0.5 sec. to 24 hrs. (0.5 to 100,000 MPa/sec). Below 204 C, time-temperature superposition held allowing strength at longer times to be estimated from strength tests at shorter times but higher temperatures. The data indicated that a 50% drop in strength might be expected for this material when the test time is increased by 9 orders of magnitude. The shift factors derived from compliance data applied well to the strength results. To explain the link between compliance and strength, a viscoelastic fracture model was investigated. The model, which used compliance as input, was found to fit the strength data only if the critical fracture energy was allowed to vary with temperature reduced stress rate. This variation in the critical parameter severely limits its use in developing a robust time-dependent strength model. The significance of this research is therefore seen as providing both the indication that a more versatile acceleration method for strength can be developed and the evidence that such a method is needed.

Reeder, J. R.↗

Fracture in Phenolic Impregnated Carbon Ablator

The thermal protection materials used for spacecraft heat shields are subjected to various thermal-mechanical loads during an atmospheric entry which can threaten the structural integrity of the system. This paper discusses the development of a novel technique to understand the failure mechanisms inside thermal protection materials. The focus of research is Phenolic Impregnated Carbon Ablator (PICA). It has successfully flown on the Stardust spacecraft and is the TPS material chosen for the Mars Science Laboratory (MSL) and Dragon spacecraft. Although PICA has good thermal properties, structurally, it is a weak material. In order to thoroughly understand failure in PICA, fracture tests were performed on FiberForm* (precursor of PICA), virgin and charred PICA materials. Several samples of these materials were tested to investigate failure mechanisms at a microstructural scale. Stress-strain data were obtained simultaneously to estimate the fracture toughness. It was found that cracks initiated and grew in the FiberForm when a critical stress limit was reached such that the carbon fibers separated from the binder. However, both for virgin and charred PICA, crack initiation and growth occurred in the matrix (phenolic) phase. Both virgin and charred PICA showed greater strength values compared to FiberForm coupons, confirming that the presence of the porous matrix helps in absorbing the fracture energy.

Agrawal, Parul↗

Fracture in Phenolic Impregnated Carbon Ablator

The thermal protection materials used for spacecraft heat shields are subjected to various thermal-mechanical loads during an atmospheric reentry which can threaten the structural integrity of the system. This paper discusses the development of a novel technique to understand the failure mechanisms inside the thermal protection material, Phenolic Impregnated Carbon Ablator (PICA). PICA has successfully flown on the Stardust spacecraft and was the TPS material chosen for the Mars Science Laboratory (MSL), that will fly in 2011. Although PICA has good thermal properties, structurally, it is a weak material. To thoroughly understand failure in PICA, experiments were performed using FiberForm(Registered TradeMark) (precursor of PICA), virgin and furnace-charred PICA. Several small samples were tested inside an electron microscope to investigate the failure mechanisms. Micrographs were obtained before and after the failure in order to study crack initiation and growth. Videos were obtained to capture failure mechanisms in real time. Stress-strain data was obtained simultaneously for all the samples with the help of a data acquisition system, integrated to the mechanical stages. It was found that cracks initiated and grew in the FiberForm when a critical stress limit was reached such that the carbon fibers separated from the binder. However, both for virgin and charred PICA, crack initiation and growth occurred in the matrix (phenolic) phase. Both virgin and charred PICA showed greater strength values compared to FiberForm coupons, confirming that the presence of the porous matrix helps in absorbing the fracture energy.

Agrawal, Parul↗

Fracture in Phenolic Impregnated Carbon Ablator

This paper describes the development of a novel technique to understand the failure mechanisms inside thermal protection materials. The focus of this research is on the class of materials known as phenolic impregnated carbon ablators. It has successfully flown on the Stardust spacecraft and is the thermal protection system material chosen for the Mars Science Laboratory and SpaceX Dragon spacecraft. Although it has good thermal properties, structurally, it is a weak material. To understand failure mechanisms in carbon ablators, fracture tests were performed on FiberForm(Registered TradeMark) (precursor), virgin, and charred ablator materials. Several samples of these materials were tested to investigate failure mechanisms at a microstructural scale. Stress-strain data were obtained simultaneously to estimate the tensile strength and toughness. It was observed that cracks initiated and grew in the FiberForm when a critical stress limit was reached such that the carbon fibers separated from the binder. However, both for virgin and charred carbon ablators, crack initiation and growth occurred in the matrix (phenolic) phase. Both virgin and charred carbon ablators showed greater strength values compared with FiberForm samples, confirming that the presence of the porous matrix helps in absorbing the fracture energy.

Agrawal, Parul↗