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NASA NTRS1998

Test Standard Developed for Determining the Slow Crack Growth of Advanced Ceramics at Ambient Temperature

The service life of structural ceramic components is often limited by the process of slow crack growth. Therefore, it is important to develop an appropriate testing methodology for accurately determining the slow crack growth design parameters necessary for component life prediction. In addition, an appropriate test methodology can be used to determine the influences of component processing variables and composition on the slow crack growth and strength behavior of newly developed materials, thus allowing the component process to be tailored and optimized to specific needs. At the NASA Lewis Research Center, work to develop a standard test method to determine the slow crack growth parameters of advanced ceramics was initiated by the authors in early 1994 in the C 28 (Advanced Ceramics) committee of the American Society for Testing and Materials (ASTM). After about 2 years of required balloting, the draft written by the authors was approved and established as a new ASTM test standard: ASTM C 1368-97, Standard Test Method for Determination of Slow Crack Growth Parameters of Advanced Ceramics by Constant Stress-Rate Flexural Testing at Ambient Temperature. Briefly, the test method uses constant stress-rate testing to determine strengths as a function of stress rate at ambient temperature. Strengths are measured in a routine manner at four or more stress rates by applying constant displacement or loading rates. The slow crack growth parameters required for design are then estimated from a relationship between strength and stress rate. This new standard will be published in the Annual Book of ASTM Standards, Vol. 15.01, in 1998. Currently, a companion draft ASTM standard for determination of the slow crack growth parameters of advanced ceramics at elevated temperatures is being prepared by the authors and will be presented to the committee by the middle of 1998. Consequently, Lewis will maintain an active leadership role in advanced ceramics standardization within ASTM. In addition, the authors have been and are involved with several international standardization organizations including the Versailles Project on Advanced Materials and Standards (VAMAS), the International Energy Agency (IEA), and the International Organization for Standardization (ISO). The associated standardization activities involve fracture toughness, strength, elastic modulus, and the machining of advanced ceramics.

Choi, Sung R.↗

NASA NTRS2020

Experimental Reexamination of Transverse Tensile Strength for IM7/8552 Tape-Laminate Composites

Due to the observed dependence of transverse-tensile strength, YT, on test geometry and specimen size, there is no consensus regarding a test method that can uniquely measure YT. This study reexamines characterization of YT by comparing results from established flexure tests with results from a new tensile test that exhibits consistent failure in the gage region. Additionally, the effects of surface preparation and direction of transverse fracture are investigated. Results show that YT is inversely proportional to specimen volume and surface roughness, and is insensitive to direction of transverse fracture. The relationship between specimen volume and YT is adequately captured by Weibull strength-scaling theory, except at the tails of the YT distributions. However, specimens exhibited microcracking prior to failure, which violates the “weak-link” assumptions of the Weibull theory. These findings highlight the challenges of using deterministic YT values in progressive damage analysis.

Arndt, Caitlin M.↗

DOE OSTI2022

Development of Quantum Computing Interconnect Based on Aerosol Jet Printing and Electrochemical Deposition of Rhenium

The electrodeposition of rhenium on to a metal seed layer on flexible substrates is presented as a means to creating superconducting flexible cable connectors in an enabling plug-and-play approach for quantum computing. Cryogenic quantum electronics are currently connected using masses of stainless-steel coaxial cables that are bulky, rigid - both in form and design - and lead to significant joule heating, thermal noise, and cross talk. Here, we present an unprecedented approach to integrate an aerosol jet printed (AJP) metal seed layer with rhenium electrodeposition on a flexible substrate in the advancement of superconducting interconnect technologies. Silver and gold were printed using the ‘Nanojet’ aerosol jet printer on Kapton films. Adhesion of gold was found to be far superior to that of silver and adhesion on roughened Kapton surpassed that of its smooth counterpart. Electrodeposition of rhenium was successful on both silver and gold and an amorphous Re film was confirmed by XRD. Results for both materials are presented however due to the poor adhesion of silver to Kapton it was ruled out as a viable candidate. Composite materials were characterized by profilometry, EDS, XRD and FIBSEM. Electrical measurements of the composite at ambient temperature showed a critical temperature (T c ), where the resistance drops to 0, of 5.8 K, well above 4.2 K, the temperature of liquid helium. Stress-strain tests of the Ag-Re and Au-Re composites on roughened and smooth Kapton were completed. Cyclic flexure testing (200 cycles) to 1.25% strain showed smooth Kapton samples reach a stress of ~16 MPa, while Kapton roughened with sandpaper, reaches ~20MPa of stress for the same 1.25% strain.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Maturing ceramic am and establishing a qualification framework at los alamos national laboratory

We successfully produced specimens made from porcelain resin (Tethon3D) in three different orientations (Z=45mm, Z=4mm and Z=3mm) without any cracks or delamination, both before and after post-processing. Four-point flexural tests were conducted on these specimens. Among the three orientations, specimens printed in the Z=4mm direction showed the best flexural strength, followed by Z=3mm and Z=45mm.

36 MATERIALS SCIENCE↗

DOE OSTI2022

In-situ imaging of flexure-induced fracture in tape-laminate composites using high-resolution X-ray computed tomography

Here, this study presents development of an in-situ flexure test for imaging progressive inter- and intralaminar fracture in tape-laminate composites using X-ray computed tomography (CT). The intent of this test is to provide detailed experimental observations of ply-level damage that can be used to validate existing, and develop new, progressive damage analysis (PDA) tools. The test consists of a vertically mounted specimen which is flexed using two eccentric compressive loads using an in-situ uniaxial load stage. The flexure specimen contains a starter notch mid-span which promotes initiation of composite failure within the X-ray field of view. Specimens with two different laminate stacking sequences were tested, imaged, analyzed. For a quasi-isotropic laminate with large angle changes between adjacent plies, there was near simultaneous growth of transverse cracks and delaminations below the midplane of the laminate. For a laminate with small angles between adjacent plies, there was extensive formation of transverse crack networks which penetrated the laminate thickness without delamination growth. In addition to imaging fracture, the X-ray CT data from both specimen types were used to quantify the variability in thickness and analyze the local orientation of individual plies. Overall, the proposed test and the image-data analysis methodology provided an important insight into the fracture processes in tape laminates and highlights the inherent ply-level geometrical variabilities that should be accounted for in PDA simulations.

42 ENGINEERING↗

NASA NTRS2004

Plate Deformation Behavior of Polymer Matrix Composite-Ti Honeycomb-Metal Sandwiches for Pressurized Propulsion Component Applications

THe objectives are: 1. To experimentally validate bi-axial plate flexural performance of PMC-Ti H/C-A286 sandwich panels for the internally pressurized RBCC combustion chamber support structure. 2. To explore ASTM 2-D plate flexure test (D 6416) to simulate the internal pressure loading and to correlate the results with analytical and FE modeling based on 2-D flexure properties.

Bertelsen, William D.↗

DOE OSTI2022

Evaluating the Lightning Strike Damage Tolerance for CFRP Composite Laminates Containing Conductive Nanofillers

Conductive nanofillers, such as carbon nanotube, graphene nanoplatelets, and carbon black particles (with diameters in nanometers) have been shown to enhance the electrical conductivity of fiber reinforced polymer matrix composites in many existing studies. The motivation is primarily for lightning strike protection, electromagnetic interference shielding, de-icing, and the manufacturing of lightweight electronic components. Here, we evaluate the lightning strike damage tolerance of carbon fiber reinforced polymer (CFRP) matrix composite laminates containing conductive nanofillers with varying weight fractions, including carbon black (CB), carbon nanotubes (CNT), and a mix of CB and CNT, through simulated lightning strike tests, followed by both non-destructive ultrasonic inspection and destructive sectioning to characterize the damage inflicted by the simulated lightning strike. Three-point flexural tests are performed to evaluate the residual strength retained by all CFRP specimens. Results show that lightning strike damage experienced varying levels of reduction for CFRP composite specimens containing conductive fillers in comparison to the baseline specimen without fillers. Notably, the delamination only penetrated to the interface between the 1st and 2nd layer for the specimen with 0.25 wt.% CNT in comparison to the baseline CFRP specimen for which the delamination penetrated to the interface between the 5th and 6th layer. Moreover, the retention of the flexural modulus increased from 26.5% to a maximum of 95.0% for the specimen with 0.25 wt.% hybrid CB and CNT. Yet, we show that using our chosen conductive fillers cannot fully eliminate lightning strike damage. Additionally, adding conductive fillers could compromise the flexural properties. We provide discussions on future recommendations on using conductive fillers for the lightning strike protection of CFRP composites.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Vertical z-axis discontinuous carbon fibers for improved lightning strike performance of continuous fiber-reinforced polymer composites

Effective lightning strike protection for critical aerospace and wind applications requires high electrical conductivity to dissipate current efficiently. However, polymer matrix composites face a challenge due to their inherently insulating nature. While conventional carbon fiber-reinforced composites (CFRP) exhibit electrical conductivity in the planar direction, achieving through-thickness conductivity remains an ongoing challenge. In this work, we have undertaken the fabrication of CFRP interleaved with vertically oriented carbon fibers (Z-fiber) to impart higher electrical conductivity along the thickness direction. Two Z-fiber composite variations are prepared: Z-1 with a single layer of Z-fiber and Z-5 with five interleaved layers and compared with no Z-fiber layer (Z-0) composite. The composite panels were subjected to lab-scale lightning strike tests with a current magnitude of 100 kA. To emulate real-world service conditions, an aerospace-grade paint coating was applied to the composite laminates. Comparative analysis shows Z-1 reduces damage diameter to ∼22 mm compared to Z-0 (∼26 mm), while Z-5 exhibits the least damage (∼16.7 mm), confirmed by optical microscopy. Z-5 demonstrates nine times higher through-thickness electrical conductivity than Z-0, reducing electrical anisotropy substantially. Thermal-electric finite element damage modeling predicts surface damage within 6% of experimental values for both Z-0 and Z-5 composites. Flexural tests post-lightning reveal Z-5 retains 66% flexural strength and 86% modulus, significantly better than Z-0, which retains less than 40% for both properties. This study highlights the efficacy of Z-fiber composites in lightning strike protection, offering improved through-thickness conductivity and mechanical property retention.

36 MATERIALS SCIENCE↗

NASA NTRS1986

Strength and microstructure of Si3N4 sintered with ZrO2 additions

Densities greater than 99 percent of theoretical were obtained with stabilized ZrO2 additions to Si3N4. Material sintered at 2140 C under 2.5 MPa nitrogen overpressure with 3.8, 9.9, and 13.4 wt pct ZrO2 had a predominantaly equiaxed grain size ranging from 0.2 to 7.0 microns. At 1370 C, the latter composition exhibited a flexural strength of about 487 MPa, equal to that of a finer-grain-size, hot-pressed Si3N4 + ZrO2 material having excellent high-temperature static fatigue properties. Transmission electron microscopy of the sintered Si3N4 revealed a glassy grain-boundary phase at all three ZrO2 levels and partially crystalline triple points for the 9.9 and 13.4 wt pct ZrO2-containing materials. Slow crack growth was observed for 1370 C flexure tests and correlated with nonlinear load deflection traces for stresses greater than 503 MPa. The crystallization of the grain-boundary glass is insterpreted as beneficial to the attainment of high (1370 C) flexural strength.

Sanders, W. A.↗

DOE OSTI2021

Large-scale additive manufacturing of self-heating molds

Large-scale material extrusion additive manufacturing technology is becoming the new mainstream technology for scaled-up composite mold and die applications. This paradigm shift in composite processing technology is primarily driven by out-of-autoclave tooling applications, in which fiber reinforced composite molds with scaled-up sizes and embedded heating elements are attractive. The present research describes the design, manufacturing, and testing of self-heating composite molds fabricated via a large-scale pellet extrusion 3D printing machine with an integrated wire co-extrusion tool. Polycarbonate (PC) composites reinforced with carbon fiber (PC/CF; 20 wt.%) and glass fiber (PC/GF; 20 wt.%) were used to fabricate mold parts. Joule heating thermal test results showed that uniform temperatures (~100 °C) were achieved for both PC/CF and PC/GF mold surfaces, using a custom-made feedback control power supply and infrared thermography. Mechanical characterizations, including tensile and flexural testing were performed on the wire-embedded and un-wired PC/CF and PC/GF base specimens to investigate the impact of the fiber reinforcement as well as the embedded wires. In the direction of extrusion, the ultimate tensile stress of PC/CF was 105 MPa, and that of PC/GF was 73 MPa, while the neat PC value was 64 MPa. Inner-bead voids and interfacial gaps were observed and characterized via optical and scanning electron microscopy. The embedded wires and inner bead impacted the mechanical properties of the composites. Furthermore, the stiffness of the wire-embedded mold was still satisfactory, proving that the technology can be used to fabricate additively manufactured out-of-oven/autoclave molds.

36 MATERIALS SCIENCE↗

NASA NTRS1998

Crack Branching and Fracture Mirror Data of Glasses and Advanced Ceramics

The fracture mirror and crack branching constants were determined from three glasses and nine advanced ceramics tested under various loading and specimen configurations in an attempt to use the constants as a data base for fractography. The ratios of fracture mirror or crack branching constant to fracture toughness were found to be approximately two for most ceramic materials tested. A demonstration of how to use the two constants as a tool for verifying stress measurements was presented for silicon nitride disk specimens subjected to high-temperature, constant stress-rate biaxial flexure testing.

Choi, Sung R.↗

NASA NTRS1980

Tests of graphite/polyimide sandwich panels in uniaxial edgewise compression

The local and general buckling behavior of graphite/polyimide sandwich panels simply supported along all four edges and loaded in uniaxial edgewise compression were investigated. Material properties of sandwich panel constituents (adhesive and facings) were determined from flatwise tension and sandwich beam flexure tests. Buckling specimens were 30.5 by 33 cm, had quasi-isotropic, symmetric facings, and a glass/polyimide honeycomb core. Core thicknesses were varied and three panels of each thickness were tested at room temperature to investigate failure modes and corresponding buckling loads. Specimens 0.635 cm thick failed by overall buckling at loads close to the analytically predicted buckling load; all other panels failed by face wrinkling. Results of the wrinkling tests indicated that several buckling formulas were unconservative and therefore not suitable for design purposes; a recommended wrinkling equation is presented.

Camarda, C. J.↗

NASA NTRS1995

Effects of through-the-thickness stitching on impact and interlaminar fracture properties of textile graphite/epoxy laminates

This study investigated the effects of through-the-thickness stitching on impact damage resistance, impact damage tolerance, and mode I and mode II fracture toughness of textile graphite/epoxy laminates. Uniweave resin-transfer-molded 48 ply graphite/epoxy (AS4/3501-6) laminates were stitched with Kevlar and glass yarns of different linear densities and stitch spacings. Delaminations were implanted during processing to simulate impact damage. Sublaminate buckling tests were performed to determine the effects of stitching on the compressive strength. The results showed outstanding improvements of up to 400 percent in the compression strength over the unstitched laminates. In impact and static indentation tests the onset of damage occurred at the same level, but the extent of damage was less in stitched laminates. Mode I fracture toughness of 24 ply Uniweave unidirectional (AS4/3501-6) stitched laminates was measured by conducting double-cantilever-beam tests. The critical strain energy release rate (G(sub Ic)) was found to be up to 30 times higher than the unstitched laminates. Mode II fracture toughness of the Uniweave laminates was measured by performing end-notched-flexure tests. Two new methods to compute the apparent G(sub IIc) are presented. The apparent G(sub IIc) was found to be at least 5-15 times higher for the stitched laminates.

Sharma, Suresh K.↗

NASA NTRS1992

Contact thermal shock test of ceramics

A novel quantitative thermal shock test of ceramics is described. The technique employs contact between a metal-cooling rod and hot disk-shaped specimen. In contrast with traditional techniques, the well-defined thermal boundary condition allows for accurate analyses of heat transfer, stress, and fracture. Uniform equibiaxial tensile stresses are induced in the center of the test specimen. Transient specimen temperature and acoustic emission are monitored continuously during the thermal stress cycle. The technique is demonstrated with soda-lime glass specimens. Experimental results are compared with theoretical predictions based on a finite-element method thermal stress analysis combined with a statistical model of fracture. Material strength parameters are determined using concentric ring flexure tests. Good agreement is found between experimental results and theoretical predictions of failure probability as a function of time and initial specimen temperature.

Rogers, W. P.↗

NASA NTRS1976

PMR polyimide/graphite fiber composite fan blades

Ultrahigh speed fan blades, designed in accordance with the requirements of an ultrahigh tip speed blade axial flow compressor, were fabricated from a high strength graphite fiber tow and a PMR polyimide resin. The PMR matrix was prepared by combining three monomeric reactants in methyl alcohol, and the solution was applied directly to the reinforcing fiber for subsequent in situ polymerization. Some of the molded blades were completely finished by secondary bonding of root pressure pads and an electroformed nickel leading edge sheath prior to final machining. The results of the spin testing of nine PMR fan blades are given. Prior to blade fabrication, heat resin tensile properties of the PMR resin were examined at four formulated molecular weight levels. Additionally, three formulated molecular weight levels were investigated in composite form with both a high modulus and a high strength fiber, both as-molded and postcured, in room temperature and 232 C transverse tensile, flexure and short beam shear. Mixed fiber orientation panels simulating potential blade constructions were also evaluated. Flexure tests, short beam shear tests, and tensile tests were conducted on these angle-plied laminates.

Cavano, P. J.↗

DOE OSTI2025

Multiscale Mechanical Characterization of Mineral-Reinforced Wood Cell Walls

Studying the multiscale mechanics of bio-based composites offers unique perspectives on underlying structure–property relations. Cellular materials, such as wood, are highly organized, hierarchical assemblies of load-bearing structural elements that respond to mechanical stimuli at the microscopic, mesoscopic and macroscopic scale. In this study, we modified oak wood with nanocrystalline ferrihydrite, a widespread ferric oxyhydroxide mineral, and characterized the resulting mechanical properties of the composite at various levels of organization. Ferrihydrite nanoparticles were deposited inside the wood cell wall by an in situ chemical reaction, resulting in increased stiffness and hardness of the functionalized secondary cell wall, as evidenced by region-specific nanoindentation tests under an electron microscope. Chemically modified and pristine wood samples were characterized by using atomic force microscopy in the bimodal frequency modulation mode, which produced topographical images from the cellular ultrastructure with high lateral resolution and localized nanomechanical information across distinct cell wall layers. In conclusion, despite mineral reinforcement at the cell wall level, the macroscopic fracture behavior examined through three-point flexural testing remained unchanged upon modification, as cell–cell adhesion could be impaired by harsh chemical conditions.

Cells↗

NASA NTRS1984

Methods for assessing the structural reliability of brittle materials

Failure from contact-induced surface flaws is considered along with controlled indentation flaws for construction of toughness and fatigue master maps, fatigue properties of ceramics with natural and controlled flaws, and a statistical analysis of size and stress state effects on the strength of an alumina ceramic. Attention is also given to dynamic and static fatigue of a machinable glass ceramic, the effect of multiregion crack growth on proof testing, and a fracture mechanics analysis of defect sizes. Other topics explored are related to the effect of temperature and humidity on delayed failure of optical glass fibers, subthreshold indentation flaws in the study of fatigue properties of ultrahigh-strength glass, the lifetime prediction for hot-pressed silicon nitride at high temperatures, static fatigue in high-performance ceramics, and requirements for flexure testing of brittle materials.

Freiman, S. W.↗

NASA NTRS2003

Characterization of a Ultra-high Temperature Ceramic Composite

Ultra-high temperature ceramics (UHTC) are of interest for hypersonic vehicle leading edge applications. Monolithic UHTCs are of concern because of their low fracture toughness and brittle behavior. UHTC composites (UHTCC) are being investigated as a possible approach to overcome these deficiencies. In this study a small sample of a UHTCC was evaluated by limited mechanical property tests, furnace oxidation exposures, and oxidation exposures in a flowing environment. The composite was prepared from a carbon fiber perform using ceramic particulates and a preceramic polymer. The as-received composite plate was non-uniform from front to back surface. Plate dimensions were 150 x 150 x 6 mm. The back surface had a fibrous, uniform appearance; XRD analysis revealed the presence of Sic and C. The front surface was smooth and non-uniform in appearance with evidence of a coarse grain structure produced by a liquid phase; XRD analysis revealed the presence of HfB2. Microcracks were present throughout the thickness as one might expect from a carbon fiber reinforced composite with attendant large thermal expansion mismatch between the matrix phases and the fibers. The HfB2 phase on the front surface was comparable in thickness to a fiber ply or about 0.6 mm, and surface microcracks were evident. Limited four point flexural tests were carried out at span to depth ratios of approximately 14 and 16 with markedly different results. Tests were run with the front or the back surface in tension. At the shorter span to depth failures occurred under a loading pin for both orientations. At a span to depth of 16 failures occurred in the center of the span with fracture clearly initiating from a tensile failure. Ultimate flexural strength, strain at ultimate stress, stress and strain at deviation from linear elastic behavior are reported. Strains at ultimate stress ranged from about 0.6 to 0.7 % for the back surface in tension, and 0.4 to 0.6 for the front surface in tension. At constant span to depth the strain at ultimate stress was about 0.2% greater for the back surface in tension and the ultimate strength was also higher. Strengths were in line with predictions from theory. Furnace oxidation studies were carried out at 1627 and 1927OC in a static furnace environment using ten minute cycles and one, five, and ten cycles. Limited oxidation studies were also carried out in a flowing oxyacetylene torch environment. Specimens were photographed, and weight and dimensional changes were determined. XRD and SEM characterizations were performed. Weight losses were attributed primarily to carbon fiber oxidation. The composite survived the torch test with little visible distress. Further details will be determined once metallographic studies are completed.

Levine, Stanley R.↗