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At least 163 records · Page 9

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

Silicon Carbide (SiC) is a promising material for thermostructural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, Mo-B and TiCu. In this presentation, we report the microstructure of diffusion bonded SA-THX mainly with TiCu interlayers obtained by TEM observations, and the influence of metallic interlayers on the joint microstructure and microhardness will be discussed.

Ceramics↗

Morphology and the Strength of Intermolecular Contact in Protein Crystals

The strengths of intermolecular contacts (macrobonds) in four lysozyme crystals were estimated based on the strengths of individual intermolecular interatomic interaction pairs. The periodic bond chain of these macrobonds accounts for the morphology of protein crystals as shown previously. Further in this paper, the surface area of contact, polar coordinate representation of contact site, Coulombic contribution on the macrobond strength, and the surface energy of the crystal have been evaluated. Comparing location of intermolecular contacts in different polymorphic crystal modifications, we show that these contacts can form a wide variety of patches on the molecular surface. The patches are located practically everywhere on this surface except for the concave active site. The contacts frequently include water molecules, with specific intermolecular hydrogen-bonds on the background of non-specific attractive interactions. The strengths of macrobonds are also compared to those of other protein complex systems. Making use of the contact strengths and taking into account bond hydration we also estimated crystal-water interfacial energies for different crystal faces.

Matsuura, Yoshiki↗

The Effect of Interface Roughness and Oxide Film Thickness on the Inelastic Response of Thermal Barrier Coatings to Thermal Cycling

The effects of interfacial roughness and oxide film thickness on thermally-induced stresses in plasma-sprayed thermal barrier coatings subjected to thermal cycling are investigated using the recently developed higher-order theory for functionally graded materials. The higher-order theory is shown to be a viable alternative to the finite-element approach, capable of modeling different interfacial roughness architectures in the presence of an aluminum oxide layer and capturing the high stress gradients that occur at the top coat/bond coat interface. The oxide layer thickness is demonstrated to have a substantially greater effect on the evolution of residual stresses than local variations in interfacial roughness. Further, the location of delamination initiation in the top coat is predicted to change with increasing oxide layer thickness. This result can be used to optimize the thickness of a pre-oxidized layer introduced at the top coat/bond coat interface in order to enhance TBC durability as suggested by some researchers. The results of our investigation also support a recently proposed hypothesis regarding delamination initiation and propagation in the presence of an evolving bond coat oxidation, while pointing to the importance of interfacial roughness details and specimen geometry in modeling this phenomenon.

Pindera, Marek-Jerzy↗

Residual Stresses Modeled in Thermal Barrier Coatings

Thermal barrier coating (TBC) applications continue to increase as the need for greater engine efficiency in aircraft and land-based gas turbines increases. However, durability and reliability issues limit the benefits that can be derived from TBC's. A thorough understanding of the mechanisms that cause TBC failure is a key to increasing, as well as predicting, TBC durability. Oxidation of the bond coat has been repeatedly identified as one of the major factors affecting the durability of the ceramic top coat during service. However, the mechanisms by which oxidation facilitates TBC failure are poorly understood and require further characterization. In addition, researchers have suspected that other bond coat and top coat factors might influence TBC thermal fatigue life, both separately and through interactions with the mechanism of oxidation. These other factors include the bond coat coefficient of thermal expansion, the bond coat roughness, and the creep behavior of both the ceramic and bond coat layers. Although it is difficult to design an experiment to examine these factors unambiguously, it is possible to design a computer modeling "experiment" to examine the action and interaction of these factors, as well as to determine failure drivers for TBC's. Previous computer models have examined some of these factors separately to determine their effect on coating residual stresses, but none have examined all the factors concurrently. The purpose of this research, which was performed at DCT, Inc., in contract with the NASA Lewis Research Center, was to develop an inclusive finite element model to characterize the effects of oxidation on the residual stresses within the TBC system during thermal cycling as well as to examine the interaction of oxidation with the other factors affecting TBC life. The plasma sprayed, two-layer thermal barrier coating that was modeled incorporated a superalloy substrate, a NiCrAlY bond coat, and a ZrO2-8 wt % Y2O3 ceramic top coat. We examined the effect on stress during burner rig thermal cycling of the following independent variables: creep in the bond coat and top coat, oxidation, bond coat coefficient of thermal expansion, number of thermal cycles, and interfacial roughness. All these factors were suspected of influencing TBC failure. The model showed that all the material properties studied had a significant effect on the coating's residual stresses if the interface of the bond coat was rough. Bond coat expansion, bond coat oxidation, and bond coat creep had the highest effect on coating stresses, and these were highly interactive. The model also showed that the mechanism of stress generation during thermal cycling changed with the number of thermal cycles. Bond coat and top coat creep dominated stress generation during early thermal cycles, greatly increasing delamination stresses at the peaks of the bond coat. Therefore, creep is the prime driver for delamination cracking early in life, but cracking is limited to the bond coat peak region. Oxidation of the bond coat, on the other hand, tended to dominate stress generation during later cycles by greatly increasing delamination stresses over bond coat valleys. These results indicate that oxidation is the driver for the continued cracking necessary to cause ceramic layer spallation.

Freborg, A. M.↗

Reducing the Resistance of Conductive-Adhesive Bonds

Current pulses lower resistance of silver-filled epoxies. Capacitive discharge reduces interfacial resistance between aluminum surfaces joined with silver-filled epoxy. Technique offers noninvasive solution to problem of attaching grounding brackets to aluminum honeycomb structures.

Guertin, L. J.↗

Ultrasonic study of adhesive bond quality at a steel-to-rubber interface by using quadrature phase detection techniques

The quadrature phase detection technique was used to simultaneously monitor the phase and amplitude of a toneburst signal normally reflected from an adhesively bonded steel-to-rubber interface. The measured phase was found to show a positive shift for all bonded samples with respect to the disbonded state - the phase shift being larger for samples with weaker bonds, as manifested by smaller values of applied tensile loads at failure. A model calculation, which incorporates the concept of interfacial strength into the usual problem of wave propagation in multilayered media, was used to deduce a bond-quality parameter from an experimentally measured phase shift. This bond-quality parameter was found to be correlated with the tensile strength of the adhesive bonds at failure loads.

Smith, A. C.↗

Adherent Al2O3 scales formed on undoped NiCrAl alloys

Changes in the spalling behavior of Al2O3 scales formed on an undoped NiCrAl alloy are described. Two samples of Ni-15Cr-13Al (wt pct), one a control and the other sanded, were subjected to 25 oxidation cycles. It is observed that adherent scales formed on the sanded sample; however, the control sample had speckled, spalled scales. The data reveal that the adherent scales are caused by repeated removal of surface layers after each oxidation cycle. It is determined that interfacial segregation of sulfur influences spallation and sulfur removal increases bonding. The effect of moisture on scale adhesions is investigated.

Smialek, James L.↗

Predictions of the critical strain for matrix cracking of ceramic matrix composites

The critical strain for matrix cracking of ceramic matrix composites has been studied; emphasis is placed on the effects of the fiber/matrix debonding length and interfacial debonding energy. Based on a modified shear-lag model, stresses in the fiber and matrix have been found for both the bonded and debonded regions. An energy-balance approach, based upon the stress field, is then adopted to evaluate the critical strain for matrix cracking. From the general equation for the critical strain, close form solutions have been deduced for two limiting cases: complete debonding and perfect bonding. Numerical solutions are given for the cases of nonzero debonding energy and partial fiber debonding. The results show that the interfacial debonding energy, which has been ignored by most of the investigators, is an important factor in determining both the critical strain and the debonding length.

Kuo, Wen-Shyong↗

Investigation of interfacial shear strength in SiC/Si3N4 composites

A fiber push-out technique was used to determine fiber/matrix interfacial shear strength (ISS) for silicon carbide fiber reinforced reaction-bonded silicon nitride (SiC/RBSN) composites in the as-fabricated condition and after consolidation by hot isostatic pressing (HIPing). In situ video microscopy and acoustic emission detection greatly aided the interpretation of push-out load/displacement curves.

Eldridge, J. I.↗

Adhesive bond evaluation using phase sensitive detection techniques

Quadrature phase detection techniques have been used to monitor the amplitude and phase of a toneburst ultrasonic wave normally reflected from adhesively-bonded steel/rubber interface. The measured phase change values of the reflected signals were found to correlate with variations in sample preparation. It was determined that measured phase shift changes were larger for samples with weaker bonds as manifested by smaller measured values of the applied tensile loads at failure. A model calculation which incorporates the concept of interfacial strength into the usual problem of wave propagation in multi-layered isotropic elastic media was used to deduce a bond-quality parameter from an experimentally measured phase shift.

Smith, Alphonso C.↗

Investigation of interfacial shear strength in SiC/Si3N4 composites

A fiber push-out technique was used to determine fiber/matrix interfacial shear strength (ISS) for silicon carbide fiber reinforced reaction-bonded silicon nitride (SiC/RBSN) composites in the as-fabricated condition and after consolidation by hot isostatic pressing (HIPing). In situ video microscopy and acoustic emission detection greatly aided the interpretation of push-out load/displacement curves.

Eldridge, J. I.↗

X ray attenuation measurements for high-temperature materials characterization and in-situ monitoring of damage accumulation

The scope of this dissertation is to develop and apply x ray attenuation measurement systems that are capable of: (1) characterizing density variations in high-temperature materials, e.g., monolithic ceramics, ceramic and intermetallic matrix composites, and (2) noninvasively monitoring damage accumulation and failure sequences in ceramic matrix composites under room temperature tensile testing. This dissertation results in the development of: (1) a point scan digital radiography system, and (2) an in-situ x ray material testing system. Radiographic evaluation before, during, and after loading shows the effect of preexisting volume flaws on the fracture behavior of composites. Results show that x ray film radiography can monitor damage accumulation during tensile loading. Matrix cracking, fiber matrix debonding, fiber bridging, and fiber pullout are imaged throughout the tensile loading of the specimens. Further in-situ radiography is found to be a practical technique for estimating interfacial shear strength between the silicon carbide fibers and the reaction bonded silicon nitride matrix. It is concluded that pretest, in-situ, and post test x ray imaging can provide for greater understanding of ceramic matrix composite mechanical behavior.

Baaklini, George Y.↗

Sulfur Impurities and the Microstructure of Alumina Scales

The relationship between the microstructure of alumina scales, adhesion, and sulfur content was examined through a series of nickel alloys oxidized in 1100 to 1200 deg. C cyclic or isothermal exposures in air. In cyclic tests of undoped NiCrAl, adhesion was produced when the sulfur content was reduced, without any change in scale microstructure. Although interfacial voids were not observed in cyclic tests of NiCrAl, they were promoted by long-term isothermal exposures, by sulfur doping, and in most exposures of NiAl. Two single crystal superalloys, PWA 1480 and Rene' N5, were also tested, either in the as-received condition or after the sulfur content had been reduced to less than 1 ppmw by hydrogen annealing. The unannealed alloys always exhibited spalling to bare metal, but interfacial voids were not observed consistently. Desulfurized PWA 1480 and Rene' N5 exhibited remarkable adhesion and no voidage for either isothermal or cyclic exposures. The most consistent microstructural feature was that, for the cases where voids did form, the scale undersides exhibited corresponding areas with ridged oxide grain boundaries. Voids were not required for spallation nor were other microstructural features essential for adhesion. These observations are consistent with the model whereby scale spallation is controlled primarily by interfacial sulfur segregation and the consequent degradation of oxide-metal bonding.

Smialek, James L.↗

Normal Gravity Testing of a Microchannel Phase Separator for In Situ Resource Utilization

A microchannel separator, with 2.7 millimeters as the smallest dimension, was tested, and a pore throat structure captured and removed liquid from a gas-liquid stream. The microchannel device was tested over a of gas and liquid flow rates ranging from 0.0005 up to 0. 14 volume fraction of liquid. Four liquids were tested with air. The biggest factor affecting the throughput is the capacity of liquid flow through the pore throat, which is dictated by permeability, liquid viscosity, flow area, pore throat thickness, and pressure difference across the pore throat. Typically, complete separation of gas and liquid fractions was lost when the liquid flow rate reached about 40 to 60% of the pore throat capacity. However, this could occur over a range of 10 to 90% utilization of pore throat capacity. Breakthrough occurs in the microchannel phase separator at conditions similar to the annular to plug flow transition of two-phase microgravity pipe flow implying that operating in the proper flow regime is crucial. Analysis indicates that the Bond number did not affect performance, supporting the premise that hydrodynamic, interfacial, and capillary forces are more important than gravity. However, the relative importance of gravity is better discerned through testing under reduced gravity conditions.

TeGrotenhuis, Ward E.↗

Engine materials characterization and damage monitoring by using x ray technologies

X ray attenuation measurement systems that are capable of characterizing density variations in monolithic ceramics and damage due to processing and/or mechanical testing in ceramic and intermetallic matrix composites are developed and applied. Noninvasive monitoring of damage accumulation and failure sequences in ceramic matrix composites is used during room-temperature tensile testing. This work resulted in the development of a point-scan digital radiography system and an in situ x ray material testing system. The former is used to characterize silicon carbide and silicon nitride specimens, and the latter is used to image the failure behavior of silicon-carbide-fiber-reinforced, reaction-bonded silicon nitride matrix composites. State-of-the-art x ray computed tomography is investigated to determine its capabilities and limitations in characterizing density variations of subscale engine components (e.g., a silicon carbide rotor, a silicon nitride blade, and a silicon-carbide-fiber-reinforced beta titanium matrix rod, rotor, and ring). Microfocus radiography, conventional radiography, scanning acoustic microscopy, and metallography are used to substantiate the x ray computed tomography findings. Point-scan digital radiography is a viable technique for characterizing density variations in monolithic ceramic specimens. But it is very limited and time consuming in characterizing ceramic matrix composites. Precise x ray attenuation measurements, reflecting minute density variations, are achieved by photon counting and by using microcollimators at the source and the detector. X ray computed tomography is found to be a unique x ray attenuation measurement technique capable of providing cross-sectional spatial density information in monolithic ceramics and metal matrix composites. X ray computed tomography is proven to accelerate generic composite component development. Radiographic evaluation before, during, and after loading shows the effect of preexisting volume flaws on the fracture behavior of composites. Results from one-, three-, five-, and eight-ply ceramic composite specimens show that x ray film radiography can monitor damage accumulation during tensile loading. Matrix cracking, fiber-matrix debonding, fiber bridging, and fiber pullout are imaged throughout the tensile loading of the specimens. In situ film radiography is found to be a practical technique for estimating interfacial shear strength between the silicon carbide fibers and the reaction-bonded silicon nitride matrix. It is concluded that pretest, in situ, and post-test x ray imaging can provide greater understanding of ceramic matrix composite mechanical behavior.

Baaklini, George Y.↗

Bonding by Hydroxide-Catalyzed Hydration and Dehydration

A simple, inexpensive method for bonding solid objects exploits hydroxide-catalyzed hydration and dehydration to form silicate-like networks in thin surface and interfacial layers between the objects. The method can be practiced at room temperature or over a wide range of temperatures. The method was developed especially to enable the formation of precise, reliable bonds between precise optical components. The bonds thus formed exhibit the precision and transparency of bonds formed by the conventional optical-contact method and the strength and reliability of high-temperature frit bonds. The method also lends itself to numerous non-optical applications in which there are requirements for precise bonds and/or requirements for bonds, whether precise or imprecise, that can reliably withstand severe environmental conditions. Categories of such non-optical applications include forming composite materials, coating substrates, forming laminate structures, and preparing objects of defined geometry and composition. The method is applicable to materials that either (1) can form silicate-like networks in the sense that they have silicate-like molecular structures that are extensible into silicate-like networks or (2) can be chemically linked to silicate-like networks by means of hydroxide-catalyzed hydration and dehydration. When hydrated, a material of either type features surface hydroxyl (-OH) groups. In this method, a silicate-like network that bonds two substrates can be formed either by a bonding material alone or by the bonding material together with material from either or both of the substrates. Typically, an aqueous hydroxide bonding solution is dispensed and allowed to flow between the mating surfaces by capillary action. If the surface figures of the substrates do not match precisely, bonding could be improved by including a filling material in the bonding solution. Preferably, the filling material should include at least one ingredient that can be hydrated to have exposed hydroxyl groups and that can be chemically linked, by hydroxide catalysis, to a silicate-like network. The silicate-like network could be generated in situ from the filling material and/or substrate material, or could be originally present in the bonding material.

Gwo, Dz-Hung↗

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

Ceramics↗