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The results are described of the final stage of the research involving the role of anions in the behavior of magnesium oxide, as well as the continued efforts of the fracture behavior of silicon nitride materials. These efforts, particularly the first, are further sub-divided in subsections describing individual types of behavior of materials.
Various properties of ceramic materials were investigated. Magnesium oxide and the role of anion impurities were investigated together with the slow crack growth in silicon nitride-silicon carbide ceramics. The oxide program involved development of fabrication techniques for anion doped materials and evaluation of the role of these anions in the hot pressing response, grain boundary diffusion of nickel doped material, grain boundary microhardness, and grain growth. The carbide-nitride work employed commercial materials and the research involved evaluation of a recently reported technique for study of slow crack growth and the development of data for these commercial materials.
The first study area involved magnesium oxide and the role of anion impurities, while the second area was directed toward slow crack growth in silicon nitride-silicon carbide ceramics. The oxide program involved development of fabrication techniques for anion doped materials and evaluation of the role of these anions in the hot pressing response, grain boundary diffusion of nickel doped material, grain boundary microhardness, and grain growth.
The utilization of local resources for the construction and operation of a lunar base can significantly reduce the cost of transporting materials and supplies from Earth. The feasibility of processing lunar regolith to form construction materials and structural components is investigated. A preliminary review of potential processing methods such as sintering, hot-pressing, liquification, and cast basalt techniques, was completed. The processing method proposed is a variation on the cast basalt technique. It involves liquification of the regolith at 1200-1300 C, casting the liquid into a form, and controlled cooling. While the process temperature is higher than that for sintering or hot-pressing (1000-1100 C), this method is expected to yield a true engineering material with low variability in properties, high strength, and the potential to form large structural components. A scenario for this processing method was integrated with a design for a representative lunar base structure and potential construction techniques. The lunar shelter design is for a modular, segmented, pressurized, hemispherical dome which could serve as habitation and laboratory space. Based on this design, estimates of requirements for power, processing equipment, and construction equipment were made. This proposed combination of material processing method, structural design, and support requirements will help to establish the feasibility of lunar base construction using indigenous materials. Future work will refine the steps of the processing method. Specific areas where more information is needed are: furnace characteristics in vacuum; heat transfer during liquification; viscosity, pouring and forming behavior of molten regolith; design of high temperature forms; heat transfer during cooling; recrystallization of basalt; and refinement of estimates of elastic moduli, compressive and tensile strength, thermal expansion coefficient, thermal conductivity, and heat capacity. The preliminary design of the lunar shelter showed us that joining is a critical technology needed for building a structure from large segments. The problem of joining is important to the design of any structure that is not completely prefabricated. It is especially important when the structure is subjected to tensile loading by an internal pressure. For a lunar shelter constructed from large segments the joints between these large segments must be strong, and they must permit automated construction. With a cast basalt building material which is brittle, there is the additional problem of connecting the joint with the material and avoiding stress concentration that would cause failure. Thus, a well-defined project which we intend to pursue during this coming year is the design of joints for cast basalt structural elements.
The existing methods of assessing the fracture toughness of materials exhibiting semi-brittle fracture are critically reviewed. The methods concern the Crack Growth Resistance (R-curve), the Crack Opening Displacement (COD), and the J-integral. An analysis of the shortcomings of the methods described makes it possible to formulate a new definition of fracture toughness appropriate to semi-brittle fracture. An improved simple experimental method for measuring fracture toughness for semi-brittle fracture is proposed which takes into account both crack growth and plastic nonlinear effects at crack front. The proposed method is shown to be free of the theoretical and experimental discrepancies encountered in the R-curve, COD, and J-integral methods.
A generalized reliability model was developed for use in the design of structural components made from brittle, homogeneous anisotropic materials such as single crystals. The model is based on the Weibull distribution and incorporates a variable strength distribution and any equivalent stress failure criteria. In addition to the reliability model, an energy based failure criterion for elastically anisotropic materials was formulated. The model is different from typical Weibull-based models in that it accounts for strength anisotropy arising from fracture toughness anisotropy and thereby allows for strength and reliability predictions of brittle, anisotropic single crystals subjected to multiaxial stresses. The model is also applicable to elastically isotropic materials exhibiting strength anisotropy due to an anisotropic distribution of flaws. In order to develop and experimentally verify the model, the uniaxial and biaxial strengths of a single crystal nickel aluminide were measured. The uniaxial strengths of the <100> and <110> crystal directions were measured in three and four-point flexure. The biaxial strength was measured by subjecting <100> plates to a uniform pressure in a test apparatus that was developed and experimentally verified. The biaxial strengths of the single crystal plates were estimated by extending and verifying the displacement solution for a circular, anisotropic plate to the case of a variable radius and thickness. The best correlation between the experimental strength data and the model predictions occurred when an anisotropic stress analysis was combined with the normal stress criterion and the strength parameters associated with the <110> crystal direction.
Current technology for producing in-situ structural materials on future missions to Mars or the moon relies heavily on energy-intensive sintering processes to produce solid bricks from regolith. This process requires heating the material up to temperatures in excess of 1000 C and results in solid regolith pieces with compressive strengths in the range of 14000 to 28000 psi, but are heavily dependent on the porosity of the final material and are brittle. This method is currently preferred over a low temperature cementation process to prevent consumption of precious water and other non-renewable materials. A high strength structural material with low energy requirements is still needed for future colonization of other planets. To fulfill these requirements, a nano-functionalization process has been developed to produce structural bricks from regolith simulant and shows promising mechanical strength results. Functionalization of granular silicate particles into alkoxides using a simple low temperature chemical process produces a high surface area zeolite particles that are held together via inter-particle oxygen bonding. Addition of water in the resulting zeolite particles produces a sol-gel reaction called "inorganic polymerization" which gives a strong solid material after a curing process at 60 C. The aqueous solution by-product of the reaction is currently being investigated for its reusability; an essential component of any ISRU technology. For this study, two batches of regolith bricks are synthesized from JSC-1A; the first batch from fresh solvents and chemicals, the second batch made from the water solution by-product of the first batch. This is done to determine the feasibility of recycling necessary components of the synthesis process, mainly water. Characterization including BET surface area, SEM, and EDS has been done on the regolith bricks as well as the constituent particles,. The specific surface area of 17.53 sq m/g (average) of the granular regolith material was obtained from nitrogen adsorption isotherm measurement. The size, shape and textures of regolith from SEM shows that the particles are 25-50 micrometers in size and mostly irregular in shape (Figure 1a). The elemental composition of regolith was identified from EDS analysis showed the presence of Si, Al, Fe, Na, Mg, Ca, Ti, O and C (see figure 1b). Each set of cylindrical brick samples were prepared by low energy process, and cured for 21 and 28 days, respectively to compare their compressive strength. Figure 1c, and d shows the JSC-1A brick and the compressive strength measurements. The results from the 21 day cured bricks (2 bricks) have been done and yielded an aver-age strength of 3050 psi, considerably higher than Portland cement mortars (Type IV and V). This promising technology provides the benefits of construction material similar to concrete, with a low complexity, low energy synthesis process and the likelihood of complete reusability of precious resources. Compressive strength using this method can be improved by increasing the surface area of the particles, using bi-modal particle size distribution, and adding certain additives to increase inter-particle forces.
Failure mechanisms of materials under very high strains experienced at and ahead of the crack tip such as formation, growth, and interaction of microvoids in ductile materials, microcracks in brittle solids or crazes in polymers and adhesives are represented by one-dimensional, nonlinear stress-strain relations possessing different ways by which the material loses capacity to carry load up to fracture or total separation. A double cantilever beam (DCB) type specimen is considered. The nonlinear material is confined to a thin strip between the two elastic beams loaded by a wedge. The problem is first modeled as a beam on a nonlinear foundation. The pertinent equation is solved numerically as a two-point boundary value problem for both the stationary and the quasi-stationay propagating crack. A finite element model is then used to model the problem in more detail in order to assess the adequacy of the beam model for the reduction of experimental data to determine in-situ properties of the thin interlayer.
Alternative insulating process forms flexible coat of uncured refractory insulating material on copper wire. Coated wire formed into coil or other complex shape. Wire-coating apparatus forms "green" coat on copper wire. After wire coiled, heating converts "green" coat to refractory electrical insulator. When cured to final brittle form, insulating material withstands temperatures above melting temperature of wire. Process used to make coils for motors, solenoids, and other electrical devices to be operated at high temperatures.
The subcritical growth of cracks from pre-existing flaws in ceramics can severely affect the structural reliability of a material. The ability to directly observe subcritical crack growth and rigorously analyze its influence on fracture behavior is important for an accurate assessment of material performance. A Mode I fracture specimen and loading method has been developed which permits the observation of stable, subcritical crack extension in monolithic and toughened ceramics. The test specimen and procedure has demonstrated its ability to generate and stably propagate sharp, through-thickness cracks in brittle high modulus materials. Crack growth for an aluminum oxide ceramic was observed to be continuously stable throughout testing. Conversely, the fracture behavior of a silicon nitride ceramic exhibited crack growth as a series of subcritical extensions which are interrupted by dynamic propagation. Dynamic initiation and arrest fracture resistance measurements for the silicon nitride averaged 67 and 48 J/sq m, respectively. The dynamic initiation event was observed to be sudden and explosive. Increments of subcritical crack growth contributed to a 40 percent increase in fracture resistance before dynamic initiation. Subcritical crack growth visibly marked the fracture surface with an increase in surface roughness. Increments of subcritical crack growth loosen ceramic material near the fracture surface and the fracture debris is easily removed by a replication technique. Fracture debris is viewed as evidence that both crack bridging and subsurface microcracking may be some of the mechanisms contributing to the increase in fracture resistance. A Statistical Fracture Mechanics model specifically developed to address subcritical crack growth and fracture reliability is used together with a damaged zone of material at the crack tip to model experimental results. A Monte Carlo simulation of the actual experiments was used to establish a set of modeling input parameters. It was demonstrated that a single critical parameter does not characterize the conditions required for dynamic initiation. Experimental measurements for critical crack lengths, and the energy release rates exhibit significant scatter. The resulting output of the model produces good agreement with both the average values and scatter of experimental measurements.
The long-term behavior of notched graphite-fiber-reinforced composite laminates with brittle or tough matrix materials and different fiber architectures was investigated using damage measurements and stiffness change, residual strength, and life data. The fiber/matrix materials included T300/5208, AS4/3501-6, AS4/1808, AS4/PEEK, and C3000/PMR-15 matrices and unidirectional tape and woven cloth fiber architectures. Results of damage evaluation and of residual strength measurements during the fatigue damage development showed that the long-term behavior and damage tolerance are controlled by a number of interacting factors such as the matrix toughness, fiber architecture, loading levels, and damage types and distributions.
An experiment was conducted to verify the results of mathematical models which predict the stresses and displacements of fibers and the amount of damage growth in a center-notched lamina as a function of the applied remote stress and the matrix and fiber material properties. A brittle lacquer coating was used to detect the yielding in the matrix while X-ray techniques were used to determine the number of broken fibers in the laminate. The notched strengths and the amounts of damage found in the specimens agree well with those predicted by the mathematical model. It is shown that the amount of damage and the crack opening displacement does not depend strongly on the number of plies in the laminate for a given notch width. By heat-treating certain laminates to increase the yield stress of the alumina matrix, the effect of different matrix properties on the fracture behavior was investigated. The stronger matrix is shown to weaken the notched laminate by decreasing the amount of matrix damage, thereby making the laminate more notch sensitive.
An experimental investigation of the fracture behavior of unidirectional boron/aluminum composite laminates was conducted in order to verify the results of mathematical models. These models predict the fiber stresses and displacements and the amount of damage growth in a center-notched lamina as a function of the applied remote stress and the matrix and fiber material properties. A brittle lacquer coating was used to detect the yielding in the matrix while X-ray techniques were used to determine the number of broken fibers in the laminate. The notched strengths and the amounts of damage found in the specimens agreed well with those predicted by the models. It was shown that for thin laminates the amount of damage and the fiber displacements do not depend strongly on the number of plies for a given notch width.
A series of rig calibration and high temperature tests simulating gas path seal erosion in turbine engines were performed at three impingement angles and at three downstream locations. Plasma sprayed, yttria stablized zirconia specimens were tested. Steady state erosion curves presented for 19 test specimens indicate a brittle type of material erosion despite scanning electron microscopy evidence of plastic deformation. Steady state erosion results were not sensitive to downstream location but were sensitive to impingement angle. At difference downstream locations specimen surface temperature varied from 1250 to 1600 C (2280 to 2900 F) and particle velocity varied from 260 to 320 m/s (850 to 1050 ft/s). The mass ratio of combustion products to erosive grit material was typically 240.
A series of rig calibration and high temperature tests simulating gas path seal erosion in turbine engines were performed at three impingement angles and at three downstream locations. Plasma sprayed, yttria stabilized zirconia specimens were tested. Steady state erosion curves presented for 19 test specimens indicate a brittle type of material erosion despite scanning electron microscopy evidence of plastic deformation. Steady state erosion results were not sensitive to downstream location but were sensitive to impingement angle. At different downstream locations specimen surface temperature varied from 1250 to 1600 C (2280 to 2900 F) and particle velocity varied from 260 to 320 m/s (850 to 1050 ft/s). The mass ratio of combustion products to erosive grit material was typically 240.
For technological applications of high T(sub c) superconductors, it will be necessary to overcome the inherent problem of brittleness, to develop materials with high current carrying capacity, and to devise ways of joining superconductors with other materials. These issues will be addressed in the context of superconducting films on metallic wires. These composite systems are expected to produce flexible wires with desirable properties.
An investigation was performed to study impact induced damage in small-diameter struts made of a composite material with a brittle matrix system. The major focus is on characterizing the impact behavior associated with the barely visible damage. An experimental procedure including ultrasonic inspection, instrumented impact testing, and delamination buckling and residual strength measurements is presented. From the ultrasonic inspection, it is found that for the strut specimens under investigation, the impact energy level for barely visible damage threshold is above that of the internal damage threshold. A 60- to 65-percent reduction in compressive strength was typical for struts subjected to the barely visible impact damage threshold.
An analytical calibration of the Stable Poisson Loaded (SPL) specimen is presented. The specimen configuration is similar to the ASTM E-561 compact-tension specimen with displacement controlled wedge loading used for R-Curve determination. The crack mouth opening displacements (CMOD's) are produced by the diametral expansion of an axially compressed cylindrical pin located in the wake of a machined notch. Due to the unusual loading configuration, a three-dimensional finite element analysis was performed with gap elements simulating the contact between the pin and specimen. In this report, stress intensity factors, CMOD's, and crack displacement profiles are reported for different crack lengths and different contacting conditions. It was concluded that the computed stress intensity factor decreases sharply with increasing crack length, thus making the SPL specimen configuration attractive for fracture testing of brittle, high modulus materials.