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

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

Method for Fabricating Biocompatible Porous Titanium

A method for fabricating porous metal constructs (such as porous Ti constructs) which may be used as implants in bone repair is disclosed. The method employs a new saltbath sintering process coupled with conventional powder metallurgy technology which is capable of fabricating porous metal constructs with controlled porosity and pore size having a lower production cost than conventional powder metallurgy methods

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

Fusion Welding of Refractory Metals and ZrB2-SiC-ZrC Ceramics

Molybdenum and a molybdenum alloy were fusion welded to ZrB2-based ceramics to determine if the electrical and thermal properties of the metals and ceramics affected their weldability. Commercial ceramic powders were hot pressed, machined into coupons, and preheated to 1600 °C before joining the ceramics to commercial metals using plasma arc welding. Weldability varied as indicated by the range of porosity observed within the fusion zones. Measured thermal and electrical properties appeared to have little to no effect on the weldability of metal-ceramic welds despite the large range of values measured across each property. Differences in melting temperatures between metal and ceramic coupons did affect weldability by changing the weld penetration depth into ceramic coupons. Future studies on metal-ceramic welds are suggested to investigate the effect that work function, melt viscosity, wetting, or other properties have on weldability

Particle Migration in Large Cross-Section Ceramic On-Demand Extrusion Components

Ceramic On-Demand Extrusion (CODE) is a direct ink writing process which allows for the creation of near theoretically dense ceramic components with large cross-sections due to oil-assisted drying. Yttria-stabilized zirconia (YSZ) colloidal pastes (∼d50 ≲ 1 µm) were used in CODE to produce dense (multi-road infill and ≳ 98% relative density), large continuous volume (\u3e 1 cm3), and high fidelity (nozzle diameters ≲ 1 mm) structural ceramic components. However, many of these printed components underwent significant particle migration after forming. The reason for this particle migration defect was investigated using the coffee-ring effect for dilute solutions and rheological methods for dense suspensions. Modifications to the colloidal paste, such as changes in solids loading, pH, or surfactant concentration were explored as to their effectiveness to mitigate the defect. Ultimately, paste formulation and printing trade-offs are discussed with respect to the post-printing defect and as to general direct-write patterning

Freeze Extrusion Fabrication of 13-93 Bioactive Glass Scaffolds for Bone Repair

There is an increasing demand for synthetic scaffolds with the requisite biocompatibility, internal architecture, and mechanical properties for the bone repair and regeneration. In this work, scaffolds of a silicate bioactive glass (13-93) were prepared by a freeze extrusion fabrication (FEF) method and evaluated in vitro for potential applications in bone repair and regeneration. The process parameters for FEF production of scaffolds with the requisite microstructural characteristics, as well as the mechanical and cell culture response of the scaffolds were evaluated. After binder burnout and sintering (60 min at 700°C), the scaffolds consisted of a dense glass network with interpenetrating pores (porosity ≈ 50%; pore width = 100-500 μm). These scaffolds had a compressive strength of 140 ± 70 MPa, which is comparable to the strength of human cortical bone and far higher than the strengths of bioactive glass and ceramic scaffolds prepared by more conventional methods. The scaffolds also supported the proliferation of osteogenic MLO-A5 cells, indicating their biocompatibility. Potential application of these scaffolds in the repair and regeneration of load-bearing bones, such as segmental defects in long bones, is discussed

Fabricating Functionally Graded Materials by Ceramic On-Demand Extrusion with Dynamic Mixing

Ceramic On-Demand Extrusion (CODE) is an extrusion-based additive manufacturing process recently developed for fabricating dense, functional ceramic components. Presented in this paper is a further development of this process focusing on fabrication of functionally graded materials (FGM). A dynamic mixing mechanism was developed for mixing constituent ceramic pastes, and an extrusion control scheme was developed for fabricating specimens with desired material compositions graded in real time. FGM specimens with compositions graded between Al2O3 and ZrO2 were fabricated and ultimately densified by sintering to validate the effectiveness of the CODE process for FGM fabrication. Energy dispersive spectroscopy (EDS) was used to compare final compositions to the original material designs. The specimen’s hardness at different locations along the gradients was examined by micro-indentation tests. The dimensions of sintered specimens were measured, and the effects of material composition gradients on the distortions of sintered FGM specimens were analyze

Fabrication of ceramic components using freeze-form extrusion fabrication

A novel, environmentally friendly solid freeform fabrication method called Freeze-form Extrusion Fabrication (FEF) has been developed for the fabrication of high temperature and ultra-high temperature ceramic-based components. The method is based on deposition of ceramic pastes using water as the medium. The FEF system components and their interaction are examined, and the main process parameters affecting part geometry are defined. Three-dimensional (3D) shaped components have been fabricated by extrusion deposition of the ceramic paste in a layer-by-layer fashion. The feasibility of this process has been demonstrated by building components having a simple geometry, such as cylinders and solid or hollow cones. Hollow cones have also been fabricated to demonstrate the ability to build structures with sloped walls. Sintered samples have achieved 98% and 96% of their theoretical density for AI2O3 and ZrB2, respectively. The dispersion of ZrB2 particles in an aqueous medium was investigated. In aqueous systems, the surface of ZrB2 consists of a thin layer of ZrO2 that controls the surface chemistry and surface charge. Measurements showed that the ZrB2 had an isoelectric point of pH = 4.7 and a maximum zeta potential of -50 mV at pH = 9. Either an ionic ammonium polyacrylate or a nonionic alkoxylated polyether increased the zeta potential of ZrB2 by as much as 60 mV, to -110 mV. Viscosity measurements were used to optimize dispersant concentrations. High solids loading (~45 vol.% ZrB2) aqueous pastes were prepared. The pastes had viscosities of 40 - 50 Pa·s-1 ,which was acceptable for extrusion. The pastes were used to fabricate 3-D components from ZrB2. The microstructure of sintered ZrB2 consisted of equiaxed B4C with an average grain size of 4.3 μm and small equiaxed and large elongated ZrB2 grains with an average grain size of 40 μm. For longitude and transverse deposited samples, the elastic moduli were E = 435 and 417 GPa, the flexural strength σf = 353 and 230 MPa, and the Vickers’ hardness Hv = 18.74 and 18.50 GPa, respectively. The longitude deposited samples had an average fracture toughness of 3.09 MPa·m1/2. The ZrB2 component fabrication demonstrated the feasibility of using aqueous freeze-form extrusion fabrication technique --Abstract, page iv