R-Curve Measurements of silicon nitride glass ceramic and PZT.
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Grutzik, Scott Joseph↗
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Thermal Equation of State of α Silicon Nitride
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99 GENERAL AND MISCELLANEOUS↗
Fracture mechanics
The application of fracture mechanics to the design of ceramic structures will require the precise measurement of crack growth and fracture resistance of these materials over their entire range of anticipated service temperatures and standardized test methods for making such measurements. The development of a standard test for measuring the plane strain fracture toughness is sought. Stress intensity factor coefficients were determined for three varieties of chevron-notch specimens, and fracture toughness measurements were made on silicon nitrides, silicon carbides, and aluminum oxides to assess the performance of each specimen variety. It was determined that silicon nitride and silicon carbides have flat crack growth resistance curves, but aluminum oxide does not. Additionally, batch-to-batch differences were noticed for the aluminum oxide. Experiments are continuing to explain the rising crack growth resistance and batch-to-batch variations for the aluminum oxide.
Shannon, John L., Jr.↗
Molecular Dynamics Simulations of Silicon Carbide, Boron Nitride and Silicon for Ceramic Matrix Composite Applications
A comprehensive computational molecular dynamics study is presented for crystalline α-SiC (6H, 4H, and 2H SiC), β-SiC (3C SiC), layered boron nitride, amorphous boron nitride and silicon, the constituent materials for high-temperature SiC/SiC compositions. Large-scale Atomic/Molecular Parallel Simulator software package was used. The Tersoff Potential force field was utilized to evaluate their mechanical characteristics of most of the materials, and the Reax force field was used to model silicon when the Tersoff Potential did not provide accurate results. Their mechanical behaviors were evaluated at a strain rate of 10(exp 7)/s and the results agree with the experimental data in the literature. The results are foundational for linking constituent behavior to composite performance, particularly when test data is unavailable or suspect.
Aluko, Olanrewaju↗
Neutral but Impactful: Gallium Cluster-Induced Nanopores from Beam-Blanked Gallium Ion Sources
Neutral atoms originating from liquid metal ion sources are an often-overlooked source of contamination and damage in focused ion beam microscopy. Beyond ions and single atoms, these sources also generate atom clusters. While most studies have investigated charged clusters, here we demonstrate that neutral clusters are also formed. These neutral clusters bypass the electrostatic beam blanking system, allowing them to impinge on samples even when the ion beam is blanked. We investigate this phenomenon using thin (≤20 nm) freestanding membranes of hexagonal boron nitride, silicon, and silicon nitride as targets. Randomly dispersed nanopores that form upon neutral cluster exposure are revealed. The average nanopore diameter is ∼2 nm with a narrow size distribution, suggesting that the atom clusters have a preferred size. Various electron microscopy techniques are used to characterize the nanopores, including high-resolution transmission electron microscopy, multislice ptychography, and electron energy-loss spectroscopy. Finally, we show how electron irradiation in the transmission electron microscope can be used to both remove any amorphous material that may clog the pores and to controllably grow the pores to specific sizes. Tunable nanopores such as these are interesting for nanofluidic applications requiring size-selective membranes.
Byrne, Dana O↗
Materials review for improved automotive gas turbine engine
The potential role of superalloys, refractory alloys, and ceramics in the hottest sections of engines operating with turbine inlet temperatures as high as 1370 C is examined. The convential superalloys, directionally solidified eutectics, oxide dispersion strenghened alloys, and tungsten fiber reinforced superalloys are reviewed and compared on the basis of maximum turbine blade temperature capability. Improved high temperature protective coatings and special fabrication techniques for these advanced alloys are discussed. Chromium, columbium, molybdenum, tantalum, and tungsten alloys are also reviewed. Molbdenum alloys are found to be the most suitable for mass produced turbine wheels. Various forms and fabrication processes for silicon nitride, silicon carbide, and SIALON's are investigated for use in highstress and medium stress high temperature environments.
Belleau, C.↗
Testing of ceramic gas turbine components under service-like conditions
The German firm MTU, Munich, West Germany, is developing gas turbine components made of special ceramics (silicon nitride, silicon carbide) which can withstand temperatures up to 1600 K. Various components such as the combustor and turbine wheel are being developed. Various preliminary tests of components are discussed.
Siebmanns, W.↗
Ceramic technology for solar thermal receivers
The high-temperature capability, resistance to corrosive environments and non-strategic nature of ceramics have prompted applications in the solar thermal field whose advantages over metallic devices of comparable performance may begin to be assessed. It is shown by a survey of point-focusing receiver designs employing a variety of ceramic compositions and fabrication methods that the state-of-the-art in structural ceramics is not sufficiently advanced to fully realize the promised benefits of higher temperature capabilities at lower cost than metallic alternatives. The ceramics considered include alumina, berylia, magnesia, stabilized zirconia, fused silica, silicon nitride, silicon carbide, mullite and cordierite, processed by such methods as isostatic pressing, dry pressing, slip casting, extrusion, calendaring and injection molding.
Kudirka, A. A.↗
Breakway friction and dynamic friction/wear measurements of various ceramic materials from 25 C (75 F) to 650 C (1200 F)
This report describes the results of a program designed to evaluate the breakaway friction and dynamic friction/wear characteristics of materials having potential for use as load bearing components in a high-performance high-temperature heavy duty diesel engine. Ten candidate materials were selected, six of which were evaluated under all possible material combinations as both stationary as well as moving breakaway specimens. The remaining materials were evaluated either in the static mode against themselves and all other materials, or against themselves only. Experiments were performed at five temperatures up to 650 C (1200 F) and unit pressures of 700 kPa (100 lb/sq in.), 3500 kPa (500 lb/sq in.), and 7000 kPa (1000 lb/sq in.). Experimental results indicate that under dynamic conditions, four of the ten materials exhibited good to excellent friction/wear characteristics in various material combinations. These materials were: titanium carbide, silicon nitride, silicon carbide (reaction sintered), and Refel (SiC).
Boes, D. J.↗
Ceramic Parts for Turbines
Abilities of ceramics to serve as turbine blades, stator vanes, and other elements in hot-gas flow of rocket engines discussed in report. Ceramics prime candidates, because of resistance to heat, low density, and tolerance of hostile environments. Ceramics considered in report are silicon nitride, silicon carbide, and new generation of such ceramic composites as transformation-toughened zirconia and alumina and particulate- or whisker-reinforced matrices. Report predicts properly designed ceramic components viable in advanced high-temperature rocket engines and recommends future work.
Jones, R. D.↗
Thin film thermocouples for high temperature measurement on ceramic materials
Thin film thermocouples have been developed for use on metal parts in jet engines to 1000 C. However, advanced propulsion systems are being developed that will use ceramic materials and reach higher temperatures. The purpose of this work is to develop thin film thermocouples for use on ceramic materials. The thin film thermocouples are Pt13Rh/Pt fabricated by the sputtering process. Lead wires are attached using the parallel-gap welding process. The ceramic materials are silicon nitride, silicon carbide, aluminum oxide, and mullite. Both steady state and thermal cycling furnace tests were performed in the temperature range to 1500 C. High-heating-rate tests were performed in an arc lamp heat-flux-calibration facility. The fabrication of the thin film thermocouples is described. The thin film thermocouple output was compared to a reference wire thermocouple. Drift of the thin film thermocouples was determined, and causes of drift are discussed. The results of high-heating-rate tests up to 2500 C/sec are presented. The stability of the ceramic materials is examined. It is concluded that Pt13Rh/Pt thin film thermocouples are capable of meeting lifetime goals of 50 hours or more up to temperatures of 1500 C depending on the stability of the particular ceramic substrate.
Holanda, Raymond↗
Development of thin film thermocouples on ceramic materials for advanced propulsion system applications
Thin film thermocouples were developed for use on metal parts in jet engines to 1000 C. However, advanced propulsion systems are being developed that will use ceramic materials and reach higher temperatures. The purpose is to develop thin film thermocouples for use on ceramic materials. The new thin film thermocouples are Pt13Rh/Pt fabricated by the sputtering process. Lead wires are attached using the parallel-gap welding process. The ceramic materials tested are silicon nitride, silicon carbide, aluminum oxide, and mullite. Both steady state and thermal cycling furnace tests were performed in the temperature range to 1500 C. High-heating-rate tests were performed in an arc lamp heat-flux-calibration facility. The fabrication of the thin film thermocouples is described. The thin film thermocouple output was compared to a reference wire thermocouple. Drift of the thin film thermocouples was determined, and causes of drift are discussed. The results of high heating rate tests up to 2500 C/sec are presented. The stability of the ceramic materials is examined. It is concluded that Pt13Rh/Pt thin film thermocouples are capable of meeting lifetime goals of 50 hr or more up to temperatures of 1500 C depending on the stability of the particular ceramic substrate.
Holanda, Raymond↗
Fracture Toughness in Advanced Monolithic Ceramics - SEPB Versus SEVENB Methods
Fracture toughness of a total of 13 advanced monolithic ceramics including silicon nitrides, silicon carbide, aluminas, and glass ceramic was determined at ambient temperature by using both single edge precracked beam (SEPB) and single edge v-notched beam (SEVNB) methods. Relatively good agreement in fracture toughness between the two methods was observed for advanced ceramics with flat R-curves; whereas, poor agreement in fracture toughness was seen for materials with rising R-curves. The discrepancy in fracture toughness between the two methods was due to stable crack growth with crack closure forces acting in the wake region of cracks even in SEVNB test specimens. The effect of discrepancy in fracture toughness was analyzed in terms of microstructural feature (grain size and shape), toughening exponent, and stable crack growth determined using back-face strain gaging.
Choi, S. R.↗
Assessments of Fracture Toughness of Monolithic Ceramics-SEPB Versus SEVNB Methods
Fracture toughness of a total of 13 advanced monolithic ceramics including silicon nitrides, silicon carbide, aluminas, and glass ceramic was determined at ambient temperature by using both single edge precracked beam (SEPB) and single edge v-notched beam (SEVNB) methods. Relatively good agreement in fracture toughness between the two methods was observed for advanced ceramics with flat R-curves; whereas, poor agreement in fracture toughness was seen for materials with rising R-curves. The discrepancy in fracture toughness between the two methods was due to stable crack growth with crack closure forces acting in the wake region of cracks even in SEVNB test specimens. The effect of discrepancy in fracture toughness was analyzed in terms of microstructural feature (grain size and shape), toughening exponent in R-curve, and stable crack growth determined using back-face strain gaging.
Choi, Sung R.↗
Development of Thin Film Thermocouples on Ceramic Materials for Advanced Propulsion System Applications
Thin film thermocouples have been developed for use on metal parts in jet engines to 1000 c. However, advanced propulsion systems are being developed that will use ceramic materials and reach higher temperatures. The purpose of this work is to develop thin film thermocouples for use on ceramic materials. The new thin film thermocouples are Pt13Rh/Pt fabricated by the sputtering process. Lead wires are attached using the parallel-gap welding process. The ceramic materials tested are silicon nitride, silicon carbide, aluminum oxide, and mullite. Both steady state and thermal cycling furnace tests were performed in the temperature range to 1500 C. High-heating-rate tests were performed in an arc lamp heat-flux-calibration facility. The fabrication of the thin film thermocouples is described. The thin film thermocouple output was compared to a reference wire thermocouple. Drift of the thin film thermocouples was determined, and causes of drift are discussed. The results of high heating rate tests up to 2500 C/sec are presented. The stability of the ceramic materials is examined. It is concluded that Pt13Rh/Pt thin film thermocouples are capable of meeting lifetime goals of 50 hours or more up to temperature of 1500 C depending on the stability of the particular ceramic substrate.
Holanda, R.↗
Thermo-Elastic Analysis of Internally Cooled Structures Using a Higher Order Theory
This paper presents the results of a study on the thermomechanical behavior of internally cooled silicon nitride structures. Silicon nitride is under consideration for elevated temperature aerospace engine applications. and techniques for lowering the operating temperature of structures composed of this material are under development. Lowering the operating temperature provides a large payoff in terms of fatigue life and may be accomplished through the use of thermal barrier coatings (TBC's) and the novel concept of included cooling channels. Herein, an in-depth study is performed on the behavior of a flame-impinged silicon nitride plate with a TBC and internal channels cooled by forced air. The analysis is performed using the higher order theory for functionally graded materials (HOTFGM), which has been developed through NASA Glenn Research Center funding over the past several years. HOTFGM was chosen over the traditional finite element approach as a prelude to an examination of functionally graded silicon nitride structures for which HOTFGM is ideally suited. To accommodate the analysis requirement% of the internally cooled plate problem, two crucial enhancements were made to the two-dimensional Cartesian-based version of HOTFGM. namely, incorporation of internal boundary capabilities and incorporation of convective boundary conditions. Results indicate the viability and large benefits of cooling the plate via forced air through cooling channels. Furthermore, cooling can positively impact the stress and displacement fields present in the plate, yielding an additional payoff in terms of fatigue life. Finally, a spin-off capability resulted from inclusion of internal boundaries within HOTFGM; the ability to simulate the thermo-elastic response of structures with curved surfaces. This new capability is demonstrated, and through comparison with an analytical solution, shown to be viable and accurate.
Arnold, Steven M.↗
Improving the toughness of refractory compounds
Composition and processing studies were conducted on silicon nitride and silicon carbide materials. Charpy mode impact testing to 2415 F established the effectiveness of higher purity silicon nitride powder sources in reducing the scatter of measurements and in improving short time bend strengths as well as bend stress rupture properties. Stabilized zirconia additions in particular were observed to dramatically enhance low and high temperature bend strengths and stress rupture properties for all grades of silicon nitride powder. Silicon carbide samples showed relatively poor impact resistance, although the maxima in stress rupture behavior was exhibited by this material.
Vasilos, T.↗
New Oxide Ceramic Developed for Superior High-Temperature Wear Resistance
Ceramics, for the most part, do not have inherently good tribological properties. For example friction coefficients in excess of 0.7 have been reported for silicon nitride sliding on silicon nitride or on bearing steel (ref. 1). High friction is always accompanied by considerable wear. Despite their inherently poor tribological properties, the high strength and high toughness of silicon nitride (Si3N4) ceramics has led to their successful use in tribological applications (refs. 1 to 4). The upper temperature limit for the application of Si3N4 as wear-resistant material is limited by reaction with the tribological environment (ref. 3). Silicon nitride is known to produce a thin silicon dioxide film with easy shear capability that results in low friction and low wear in a moist environment (ref. 5). At elevated temperatures, the removal of the reaction product that acts as lubricant causes the friction coefficient to increase and, consequently, the wear performance to become poor. New materials are sought that will have wear resistance superior to that of Si3N4 at elevated temperatures and in harsh environments. A new class of oxide ceramic materials has been developed with potential for excellent high-temperature wear resistance. The new material consists of a multicomponent oxide with a two-phase microstructure, in which the wear resistance of the mixed oxide is significantly higher than that of the individual constituents. This is attributed to the strong constraining effects provided by the interlocking microstructures at different length scales, to the large aspect ratio of the phases, to the strong interphase bonding, and to the residual stresses. Fretting wear tests were conducted by rubbing the new ceramic material against boron carbide (B4C). The new ceramic material produced a wear track groove on B4C, suggesting significantly higher wear resistance for the oxide ceramic. The new material did not suffer from any microstructural degradation after the wear test. The wear rate of the new ceramic material at 600 C was determined to be on the order of 10-10 mm3/N-m, which is 3 to 5 orders of magnitude lower than that for the current state-of-theart wear-resistant materials (Si3N4and B4C). The friction coefficient of the new ceramic materials is on the order of 0.4, which is significantly lower than that of silicon nitride. This new class of oxide materials has shown considerable potential for applications requiring high wear resistance at high temperatures and in harsh environments. New understanding of the wear behavior of ceramic materials is emerging as a result of the surprisingly high wear resistance of two-phase oxide ceramics. There is excellent potential for further improvements in the wear resistance of oxide ceramics through optimizing the microstructure and altering the crystallographic properties of specific oxide materials as a second phase to reduce the coefficient of friction at elevated temperatures.
Sayir, Ali↗