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School of Materials Science and Engineering

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College of Engineering

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Now showing 1 - 10 of 54

Developing a high temperature, oxidation resistant molybdenum-silica composite

(Georgia Institute of Technology, 2015-10-27) Daloz, William

A new powder processing approach to produce oxidation resistant molybdenum alloys for high temperature use has been developed. Oxidation protection is provided by fine dispersion of silica glass particles within a molybdenum matrix. As the molybdenum oxidizes, the glass is exposed and melts to form a self-healing protective oxide coating. Additionally, homogeneously dispersed Mo5SiB2 and/or Mo2B provide boria upon oxidation which reduces glass viscosity and allows flowing glass to coat the surface while remaining solid internally. This is similar to the oxidation protection used in Mo-3Si-1B (wt%) systems; however embedding the glass directly into the Mo matrix and eliminating the Mo3Si (A15) phase provides the same volume of glass at lower volume fractions of brittle phases and also without embrittling Si impurities in solution in Mo. Additionally the glass composition can be tailored for different applications and different temperatures beyond that achievable in Mo-Si-B based systems. A variety of microstructures, compositions and additional components for improved oxidation protection are also explored, and mechanisms of the oxidation protection are discussed.
Fabrication, strength and oxidation of molybdenum-silicon-boron alloys from reaction synthesis

(Georgia Institute of Technology, 2009-04-06) Middlemas, Michael Robert

Mo-Si-B alloys are a leading candidate for the next generation of jet turbine engine blades and have the potential to raise operating temperatures by 300-400°C. The alloys of interest are a three-phase mixture of the molybdenum solid solution (Moss) and two intermetallic phases, Mo3Si (A15) and Mo5SiB2 (T2). A novel powder metallurgical method was developed which uses the reaction of molybdenum, silicon nitride (Si3N4) and boron nitride (BN) powders to synthesize a fine dispersion of intermetallics in a Moss matrix. The covalent nitrides are stable in oxidizing environments up to 1000ºC, allowing for fine particle processing. The process developed uses standard powder processing techniques to create Mo-Si-B alloys in a less complex and expensive manner than previously demonstrated. This powder metallurgy approach yields a fine dispersion of intermetallics in the Moss matrix with average grain sizes of 2-4μm. Densities up to 95% of theoretical were attained from pressureless sintering at 1600°C and full theoretical density was achieved by hot-isostatic pressing (HIP). Sintering and HIPing at 1300°C reduced the grain sizes of all three phases by over a factor of two. Microstructure examination by electron back-scatter diffraction imaging was used to precisely define the location of the phases and to measure the volume fractions and grain size distributions. Microstructural quantification techniques including two-point correlation functions were used to quantify microstructural features and correlate the BN reactant powder size and morphology to the distribution of the intermetallic phases. High-temperature tensile tests were conducted and yield strengths of 580MPa at 1100°C and 480MPa at 1200°C were measured for the Mo-2Si-1Bwt.% alloy. The yield strength of the Mo-3Si-1Bwt.% alloy was 680MPa at 1100°C and 420MPa at 1300°C. A review of the pertinent literature reveals that these are among the highest yield strengths measured for these compositions. The oxidation resistance in air at 1000 and 1100°C was examined. The protective borosilicate surface layer formed quickly due to the close spacing of intermetallic particles and pre-oxidation treatment was developed to further limit the transient oxidation behavior. An oxidation model was developed which factors in the different stages of oxidation to predict compositions that minimize oxidation.
Extension of the master sintering curve for constant heating rate modeling

(Georgia Institute of Technology, 2008-01-15) McCoy, Tammy Michelle

The purpose of this work is to extend the functionality of the Master Sintering Curve (MSC) such that it can be used as a practical tool for predicting sintering schemes that combine both a constant heating rate and an isothermal hold. Rather than just being able to predict a final density for the object of interest, the extension to the MSC will actually be able to model a sintering run from start to finish. Because the Johnson model does not incorporate this capability, the work presented is an extension of what has already been shown in literature to be a valuable resource in many sintering situations. A predicted sintering curve that incorporates a combination of constant heating rate and an isothermal hold is more indicative of what is found in real-life sintering operations. This research offers the possibility of predicting the sintering schedule for a material, thereby having advanced information about the extent of sintering, the time schedule for sintering, and the sintering temperature with a high degree of accuracy and repeatability. The research conducted in this thesis focuses on the development of a working model for predicting the sintering schedules of several stabilized zirconia powders having the compositions YSZ (HSY8), 10Sc1CeSZ, 10Sc1YSZ, and 11ScSZ1A. The compositions of the four powders are first verified using x-ray diffraction (XRD) and the particle size and surface area are verified using a particle size analyzer and BET analysis, respectively. The sintering studies were conducted on powder compacts using a double pushrod dilatometer. Density measurements are obtained both geometrically and using the Archimedes method. Each of the four powders is pressed into 1/4 inch diameter pellets using a manual press with no additives, such as a binder or lubricant. Using a double push-rod dilatometer, shrinkage data for the pellets is obtained over several different heating rates. The shrinkage data is then converted to reflect the change in relative density of the pellets based on the green density and the theoretical density of each of the compositions. The Master Sintering Curve (MSC) model is then utilized to generate data that can be utilized to predict the final density of the respective powder over a range of heating rates. The Elton Master Sintering Curve Extension (EMSCE) is developed to extend the functionality of the MSC tool. The parameters generated from the original MSC are used in tandem with the solution to a specific closed integral (discussed in document) over a set range of temperatures. The EMSCE is used to generate a set of sintering curves having both constant heating rate and isothermal hold portions. The EMSCE extends the usefulness of the MSC by allowing this generation of a complete sintering schedule rather than just being able to predict the final relative density of a given material. The EMSCE is verified by generating a set of curves having both constant heating rate and an isothermal hold for the heat-treatment. The modeled curves are verified experimentally and a comparison of the model and experimental results are given for a selected composition. Porosity within the final product can hinder the product from sintering to full density. It is shown that some of the compositions studied did not sinter to full density because of the presence of large porosity that could not be eliminated in a reasonable amount of time. A statistical analysis of the volume fraction of porosity is completed to show the significance of the presence in the final product. The reason this is relevant to the MSC is that the model does not take into account the presence of porosity and assumes that the samples sinter to full density. When this does not happen, the model actually under-predicts the final density of the material.
Flexural Testing of Molybdenum-Silicon-Boron Alloys Reacted from Molybdenum, Silicon Nitride, and Boron Nitride

(Georgia Institute of Technology, 2007-05-16) Rockett, Chris H.

MoSiB alloys show promise as the next-generation turbine blade material due to their high-temperature strength and oxidation resistance afforded by a protective borosilicate surface layer. Powder processing and reactive synthesis of these alloys has proven to be a viable method and offers several advantages over conventional melt processing routes. Microstructures obtained have well-dispersed intermetallics in a continuous matrix of molybdenum solid-solution (Mo-ss). However, bend testing of pure Mo and Mo-ss samples has shown that, while the powder processing route can produce ductile Mo metal, the hardening effect of Si and B in solid-solution renders the matrix brittle. Testing at elevated temperatures (200°C) was performed in order to determine the ductile-to-brittle transition temperature of the metal as an indication of ductility. Methods of ductilizing the Mo-ss matrix such as annealing and alloying additions have been investigated.
Processing of a Hybrid Solid Oxide Fuel Cell Platform

(Georgia Institute of Technology, 2006-01-09) Oh, Raymond H.

Solid oxide fuel cell platforms consisting of alternating cellular layers of yttria-stabilized zirconia electrolyte and Fe-Ni metallic interconnects (Fe45Ni, Fe47.5Ni, Fe50Ni) were produced through the co-extrusion of two particulate pastes. Subsequent thermal treatment in a hydrogen atmosphere was used to reduce iron and nickel oxides and co-sinter the entire structure. Issues surrounding this process include the constrained sintering of the layers and the evolution of residual stress between the dense, fired layers. Sintering curves for individual components of the layers were measured by dilatometry to ascertain each materials impact on overall sintering mismatch. X-ray diffraction, scanning electron microscopy and weight loss were utilized to examine phase evolution within the Fe-Ni alloys during reduction. YSZ powders densified above ~1050C and shrinkage was rapid above the sintering temperature. Shrinkage of the interconnect occurred in two stages: reduction and the initial stages of sintering concluded around ~600C, plateauing shortly and continuing at ~900C as pore removal and grain growth ensued simultaneously. Constrained sintering resulted in the formation of remnant porosity within the interconnect layers. Interconnect compositions were chosen in efforts to minimize disparities in thermal expansion with the electrolyte. Residual strains on the surfaces of the layers were measured by x-ray diffraction. Corresponding stresses were calculated using the sin2y method. Grain growth within the interconnect prohibited random planes to be measured so stress measurements were confined to the ceramic layers. Various material properties such as thermal expansion were collected and employed in a modified finite element model to estimate residual stresses in the platform. A method for determining a crucial parameter, the zero stress temperature was outlined and incorporated. Modeled values were found to agree well with XRD values, providing indirect confirmation of the zero stress temperature calculations. Discrepancies were attributed to microcracks found within the layer that arose due to residual stress values surpassing the tensile strength of the zirconia.
A Nitride-Based Reaction for the Formation of a Three-Phase Molybdenum-Silicon-Boron Intermetallic Alloy

(Georgia Institute of Technology, 2005-07-18) Middlemas, Michael Robert

The alloy Mo-3Si-1B (wt%) may have the fracture toughness and oxidation resistance required for use as jet turbine engine blades. Mo-3Si-1B (wt%) forms a three-phase mixture of and #945;-Moss, A15 (Mo3Si) and T2 (Mo5SiB2). It has been observed that at high-temperatures, the A15 and T2 intermetallics form a oxidation resistant borosilicate glass coating. To achieve the proper combination of mechanical and thermal properties, the material must have a molybdenum matrix with a fine dispersion of intermetallics to produce a continuous protective layer. In this project, reactive sintering of molybdenum, Si3N4 and BN powders was used to create a semi-continuous molybdenum matrix with a fine dispersion of the A15 and T2 intermetallics. Sintering of the materials was further enhanced by the use of submicron-sized reactants. X-ray diffraction analysis was used verify the desired phases were formed. It was determined that formation of the A15 intermetallic phases begins as low as 1200?nd formation of T2 begins at 1300? The reactions are complete by 1400? Samples with bulk densities as high as 95% of theoretical were produced. Scanning electron microscopy images reveal a microstructure with dispersed intermetallics in a semi-continuous molybdenum matrix with grain sizes on the order of 1-4 and #956;m. It was found that by varying parameters such as mixing method and heating rates, it is possible to engineer the final microstructure, changing the level of dispersion of the intermetallics and continuity of the matrix.
Dynamic and Quasi-Static Mechanical Properties of Fe-Ni Alloy Honeycomb

(Georgia Institute of Technology, 2004-04-12) Clark, Justin Lewis

Several metal honeycombs, termed Linear Cellular Alloys (LCAs), were fabricated via a paste extrusion process and thermal treatment. Two Fe-Ni based alloy compositions were evaluated. Maraging steel and Super Invar were chosen for their compatibility with the process and the wide range of properties they afforded. Cell wall material was characterized and compared to wrought alloy specifications. The bulk alloy was found to compare well with the more conventionally produced wrought product when porosity was taken into account. The presence of extrusion defects and raw material impurities were shown to degrade properties with respect to wrought alloys. The performance of LCAs was investigated for several alloys and cell morphologies. The results showed that out-of-plane properties exceeded model predictions and in-plane properties fell short due to missing cell walls and similar defects. Strength was shown to outperform several existing cellular metals by as much as an order of magnitude in some instances. Energy absorption of these materials was shown to exceed 150 J/cc at strains of 50% for high strength alloys. Finally, the suitability of LCAs as an energetic capsule was investigated. The investigation found that the LCAs added significant static strength and as much as three to five times improvement in the dynamic strength of the system. More importantly, it was shown that the pressures achieved with the LCA capsule were significantly higher than the energetic material could achieve alone. High pressures, approaching 3 GPa, coupled with the fragmentation of the capsule during impact increased the likelihood of initiation and propagation of the energetic reaction. This multi-functional aspect of the LCA makes it a suitable capsule material.
The hydrogen reduction of iron and chromium oxides

(Georgia Institute of Technology, 2003-05) Nadler, Jason Hayes
The influence of honeycomb dies on paste extrusion mechanics

(Georgia Institute of Technology, 2002-05) Oh, Raymond H.
Paste mechanics for fine extrusion

(Georgia Institute of Technology, 2001-12) Hurysz, Kevin Michael