Thermal properties of zirconium diboride ceramics

This presentation will focus on the thermal conductivity of zirconium diboride ceramics. Previous reports of thermal conductivity values for ZrB2 vary from as low as about 30 W/m•K to over 100 W/m•K without any direct evidence to identify the reasons for the variations. Our group systematically investigated the effects of transition metal impurities, which led to the discovery that the size of the dissolved impurity species was directly related to the decrease in thermal conductivity. Analysis of the electron contribution to thermal conductivity utilizing the Wiedemann-Franz methodology led to the conclusion that both the phonon and electron contributions were affected by dissolved metallic impurities. Further, the effects of some transition metals including Ti and Y were masked by other impurities in ceramics produced from commercial ZrB2 powders. Please click Additional Files below to see the full abstract

Mechanical properties of zirconium diboride ceramics

This presentation will focus on the mechanical properties of zirconium diboride ceramics. Diboride ceramics offer a combination of properties that include high elastic modulus, hardness, strength, and moderate fracture toughness to elevated temperatures. However, like all structural ceramics, their mechanical properties are controlled by microstructure wherein grain size, dispersion and size of second phases, and impurities limit their potential use at elevated temperatures, particularly for proposed extreme environment applications at temperatures exceeding 2000°C. As an example, the flexure strength of nearly phase pure ZrB2 ranges from 300 to \u3e600 MPa at room temperature but retains a strength of \u3e300 MPa at temperatures \u3e1500°C. Further, the fracture toughness of ZrB2 ceramics is generally low, typically in the range of 3 to 4 MPa-m1/2, at both room and elevated temperatures. Please click Additional Files below to see the full abstract

Freeform Extrusion of High Solids Loading Ceramic Slurries, Part II: Extrusion Process Control

Part I of this paper provided a detailed description of a novel fabrication machine for high solids loading ceramic slurry extrusion and presented an empirical model of the ceramic extrusion process, with ram velocity as the input and extrusion force as the output. A constant force is desirable in freeform extrusion processes as it correlates with a constant material deposition rate and, thus, good part quality. The experimental results in Part I demonstrated that a constant ram velocity will produce a transient extrusion force. In some instances the extrusion force increased until ram motor skipping occurred. Further, process disturbances, such as air bubble release and nozzle clogging that cause sudden changes in extrusion force, were often present. In this paper a feedback controller for the ceramic extrusion process is designed and experimentally implemented. The controller intelligently adjusts the ram motor velocity to maintain a constant extrusion force. Since there is tremendous variability in the extrusion process characteristics, an on-off controller is utilized in this paper. Comparisons are made between parts fabricated with and without the feedback control. It is demonstrated that the use of the feedback control reduces the effect of process disturbances (i.e., air bubble release and nozzle clogging) and dramatically improves part quality.Mechanical Engineerin

Freeform Extrusion of High Solids Loading Ceramic Slurries, Part I: Extrusion Process Modeling

A novel solid freeform fabrication method has been developed for the manufacture of ceramic-based components in an environmentally friendly fashion. The method is based on the extrusion of ceramic slurries using water as the binding media. Aluminum oxide (Al2O3) is currently being used as the part material and solids loading as high as 60 vol. % has been achieved. This paper describes a manufacturing machine that has been developed for the extrusion of high solids loading ceramic slurries. A critical component of the machine is the deposition system, which consists of a syringe, a plunger, a ram actuated by a motor that forces the plunger down to extrude material, and a load cell to measure the extrusion force. An empirical, dynamic model of the ceramic extrusion process, where the input is the commanded ram velocity and the output is the extrusion force, is developed. Several experiments are conducted and empirical modeling techniques are utilized to construct the dynamic model. The results demonstrate that the ceramic extrusion process has a very slow dynamic response, as compared to other non-compressible fluids such as water. A substantial amount of variation exists in the ceramic extrusion process, most notably in the transient dynamics, and a constant ram velocity may either produce a relatively constant steady-state extrusion force or it may cause the extrusion force to steadily increase until the ram motor skips. The ceramic extrusion process is also subjected to significant disturbances such as air bubble release, which causes a dramatic decrease in the extrusion force, and nozzle clogging, which causes the extrusion force to slowly increase until the clog is released or the ram motor skips.Mechanical Engineerin

Mechanical andthermal properties of Zeta phase tantalum carbide atelevated temperatures

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Aqueous-Based Extrusion Fabrication of Ceramics on Demand

Aqueous-Based Extrusion Fabrication is an additive manufacturing technique that extrudes ceramic slurries of high solids loading layer by layer for part fabrication. The material reservoir in a previously developed system has been modified to allow for starting and stopping of the extrusion process on demand. Design pros and cons are examined and a comparison between two material reservoir designs is made. Tests are conducted to determine the optimal deposition parameters for starting and stopping the extrudate on demand. The collected test data is used for the development of a deposition strategy that improves material deposition consistency, including reduced material buildup at sharp corners. Example parts are fabricated using the deposition strategy and hardware design.Mechanical Engineerin

Mechanical properties of borothermally synthesized ZrB2

Mechanical properties of borothermally synthesized, highly pure ZrB2 were tested at room and elevated temperatures. Commercially available ZrB2 powder typically contains 1 to 4 wt % hafnium which has been shown to lower thermal properties of dense ZrB2 ceramics. Further, commercial grade ZrB2 contains other impurities (0.6 wt% O, 0.11 wt% N, 0.04 wt% Fe and others) which are also known to decrease its high-temperature mechanical strength. Purer grades of zirconia and boron powders, containing \u3c 75 ppm hafnium and \u3c0.5 wt% of other metal impurities, were reacted to produce ZrB2 for room and elevated temperature mechanical property studies. The zirconia and boron powders were reacted at 1000°C in a graphite vacuum furnace for two hours. The synthesized ZrB2 powder was then rinsed with methanol to remove boria from its surfaces, sieved with a #45 mesh, and hot pressed to near full density with 32 MPa applied pressure in a flowing argon atmosphere at 2100°C. The hot pressed billets were machined to ASTM standard test bars with the flexure surface polished to 1 um. Young’s modulus, Vickers Hardness, fracture toughness, and four-point bend strength were measured, and the results will be discussed

Effects of transition metals on thermal properties of ZrB2

Nominally phase pure zirconium diboride ceramics were synthesized to study their intrinsic thermal properties. Ceramics for this study were synthesized by reaction hot pressing of reactor grade ZrH2 and B to minimize impurities commonly found in commercial powders such as the natural abundance (1-4 wt%) of Hf. Starting powders contained \u3c200 ppm Hf. Previous results showed that Hf impurities present in quantities comparable to commercial powders masked the effect of other transition metal additions. For example, additions of 3 at% Ti and Y had no apparent effect on thermal conductivity of ceramics produced from commercial ZrB2. Lowering the Hf content to 0.4 at% increased thermal conductivity from ~90 W/m•K for ZrB2 ceramics prepared from commercial powders to ~100 W/m•K for low-Hf content ZrB2 at 25 °C. Lowering the Hf content also increased the thermal conductivity at 2000°C from ~70 W/m•K to ~80 W/m•K. For the low Hf ZrB2, adding 3 at% TiB2 decreased thermal conductivity ~15 W/m•K at 25°C while adding 3 at% MoB2 decreased thermal conductivity ~45 W/m•K at 25°C. For the present study, transition metals such as Hf, Ti, Y, Ta, and W were added individually to nominally phase pure ZrB2 to study the effects on thermal diffusivity, thermal conductivity and heat capacity at temperatures from 25°C to 2000°C. These properties will be compared to values obtained for ceramics prepared from commercial ZrB2 powders, which contained the natural abundance of Hf. Most previous reports have relied on heat capacity values from the NIST-JANAF thermodynamic tables to calculate thermal conductivity of ZrB2 ceramics. However, the heat capacity of ZrB2 with low Hf content was approximately 10% greater than widely accepted values. Due to this difference, heat capacity will be measured for each composition, and these values will be used to calculate thermal conductivity. The intrinsic thermal properties of ZrB2will be discussed as well as the effect of transition metal additions on the thermal properties of ZrB2 with low and naturally abundant quantities of Hf

Method and Apparatus for Fabricating Ceramic and Metal Components via Additive Manufacturing with Uniform Layered Radiation Drying

A freeform extrusion fabrication process for producing three - dimensional ceramic, metal and functionally gradient composite objects, including the steps of filling a plurality of paste sources with a respective plurality of aqueous paste compositions, operationally connecting respective syringes containing respective aqueous paste compositions to a mix ing chamber, moving a first aqueous paste composition from a first respective paste source into the mixing chamber, moving a second aqueous paste composition from a second respective paste source into the mixing chamber, mixing the first and second aqueous paste compositions to define a first admixture having a first admixture composition, extruding the first admixture onto a surface to define an extruded layer having a first admixture composition, surrounding the sides of the extruded layer with an oil bath, radiatively drying the extruded layer

Influence of Nb coating on the oxidation behavior of ZrB2

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