Ceramic Materials Commons^™

A Novel Extrusion-Based Additive Manufacturing Process For Ceramic Parts, Amir Ghazanfari, Wenbin Li, Ming-Chuan Leu, Greg Hilmas

Mechanical and Aerospace Engineering Faculty Research & Creative Works

An extrusion-based additive manufacturing process, called the Ceramic On-Demand Extrusion (CODE) process, for producing three-dimensional ceramic components with near theoretical density is introduced in this paper. In this process, an aqueous paste of ceramic particles with a very low binder content ( < 1 vol%) is extruded through a moving nozzle at room temperature. After a layer is deposited, it is surrounded by oil (to a level just below the top surface of most recent layer) to preclude non-uniform evaporation from the sides. Infrared radiation is then used to partially, and uniformly, dry the just-deposited layer so that the yield stress of the paste increases and the part maintains its shape. The same procedure is repeated for every layer until part fabrication is completed. Several sample parts for various applications were produced using this process and their properties were obtained. The results indicate that the proposed method enables fabrication of large, dense ceramic parts with complex geometries.

3d Printing Of A Polymer Bioactive Glass Composite For Bone Repair, Caroline Murphy, Krishna C. R. Kolan, M. Long, Ming-Chuan Leu, Julie A. Semon, D. E. Day

Mechanical and Aerospace Engineering Faculty Research & Creative Works

A major limitation of synthetic bone repair is insufficient vascularization of the interior region of the scaffold. In this study, we investigated the 3D printing of adipose derived mesenchymal stem cells (AD-MSCs) with polycaprolactone (PCL)/bioactive glass composite in a single process. This offered a three-dimensional environment for complex and dynamic interactions that govern the cell’s behavior in vivo. Borate based bioactive (13-93B3) glass of different concentrations (10 to 50 weight %) was added to a mixture of PCL and organic solvent to make an extrudable paste. AD-MSCs suspended in Matrigel was extruded as droplets using a second syringe. Scaffolds measuring …

Designed Extrudate For Additive Manufacturing Of Zirconium Diboride By Ceramic On-Demand Extrusion, Devin Mcmillen, Wenbin Li, Ming-Chuan Leu, Greg Hilmas, Jeremy Lee Watts

Mechanical and Aerospace Engineering Faculty Research & Creative Works

This work describes a process by which zirconium diboride (ZrB2) parts may be fabricated using the Ceramic On-Demand Extrusion (CODE) process. An oxide-carbide-nitride system consisting of ceramic powders and pre-ceramic organics, designed to yield ZrB₂ after reaction sintering, has been developed to produce an aqueous-based extrudate for subsequent processing in the CODE system. Pressurelessly sintered test specimens containing 1 wt% PVA binder achieve high relative density ≥ 99%. The viscoelastic response of the extrudate was characterized via spindle rheometry with a small sample adapter. Batches with 1 wt% PVA and 0.5 wt% Methocel show strong shear thinning characteristic, under …

Novel Extrusion-Based Additive Manufacturing Process For Ceramic Parts, Amir Ghazanfari, Wenbin Li, Ming-Chuan Leu, Greg Hilmas

Mechanical and Aerospace Engineering Faculty Research & Creative Works

An extrusion-based additive manufacturing process, called the Ceramic On-Demand Extrusion (CODE) process, for producing three-dimensional ceramic components with near theoretical density is introduced in this paper. In this process, an aqueous paste of ceramic particles with a very low binder content (< 1 vol%) is extruded through a moving nozzle at room temperature. After a layer is deposited, it is surrounded by oil (to a level just below the top surface of most recent layer) to preclude non-uniform evaporation from the sides. Infrared radiation is then used to partially, and uniformly, dry the just-deposited layer so that the yield stress of the paste increases and the part maintains its shape. The same procedure is repeated for every layer until part fabrication is completed. Several sample parts for various applications were produced using this process and their properties were obtained. The results indicate that the proposed method enables fabrication of large, dense ceramic parts with complex geometries.

Properties Of Partially Stabilized Zirconia Components Fabricated By The Ceramic On-Demand Extrusion Process, Wenbin Li, Amir Ghazanfari, Devin Mcmillen, Ming-Chuan Leu, Greg Hilmas, Jeremy Lee Watts

Mechanical and Aerospace Engineering Faculty Research & Creative Works

The Ceramic On-Demand Extrusion (CODE) process is a novel additive manufacturing process for fabricating dense ceramic components from aqueous pastes of high solids loading. In this study, 3 mol% Y₂O₃ stabilized tetragonal zirconia polycrystal (3Y-TZP) parts were fabricated using the CODE process. The parts were then dried in a humidity controlled environmental chamber and sintered under atmospheric pressure. Mechanical properties of the sintered parts were examined using ASTM standard test techniques, including density, Young’s modulus, flexural strength, Weibull modulus, fracture toughness and Vickers hardness. The microstructure was analyzed, and grain size was measured using scanning electron microscopy. …

Design And Testing Of A Top Mask Projection Ceramic Stereolithography System For Ceramic Part Manufacturing, Dylan Robert De Caussin

Master's Theses

Ceramic manufacturing is an expensive process with long lead times between

the initial design and final manufactured part. This limits the use of ceramic as a viable material unless there is a large project budget or high production volume associated with the part. Ceramic stereolithography is an alternative to producing low cost parts through the mixing of a photo curable resin and ceramic particles. This is an additive manufacturing process in which each layer is built upon the previous to produce a green body that can be sintered for a fully dense ceramic part.

This thesis introduces a new approach …

Properties Of Partially Stabilized Zirconia Components Fabricated By The Ceramic On-Demand Extrusion Process, Wenbin Li, Amir Ghazanfari, Devin Mcmillen, Ming Leu, Gregory Hilmas, Jeremy Watts

Faculty Publications, Mechanical Engineering

The Ceramic On-Demand Extrusion (CODE) process is a novel additive manufacturing process for fabricating dense ceramic components from aqueous pastes of high solids loading. In this study, 3 mol% Y2O3 stabilized tetragonal zirconia polycrystal (3Y-TZP) parts were fabricated using the CODE process. The parts were then dried in a humidity controlled environmental chamber and sintered under atmospheric pressure. Mechanical properties of the sintered parts were examined using ASTM standard test techniques, including density, Young’s modulus, flexural strength, Weibull modulus, fracture toughness and Vickers hardness. The microstructure was analyzed, and grain size was measured using scanning electron microscopy. The results compared …

A Novel Extrusion-Based Additive Manufacturing Process For Ceramic Parts, Amir Ghazanfari, Wenbin Li, Ming Leu, Gregory Hilmas

Faculty Publications, Mechanical Engineering

An extrusion-based additive manufacturing process, called the Ceramic On-Demand Extrusion (CODE) process, for producing three-dimensional ceramic components with near theoretical density is introduced in this paper. In this process, an aqueous paste of ceramic particles with a very low binder content (<1 vol%) is extruded through a moving nozzle at room temperature. After a layer is deposited, it is surrounded by oil (to a level just below the top surface of most recent layer) to preclude non-uniform evaporation from the sides. Infrared radiation is then used to partially, and uniformly, dry the just-deposited layer so that the yield stress of the paste increases and the part maintains its shape. The same procedure is repeated for every layer until part fabrication is completed. Several sample parts for various applications were produced using this process and their properties were obtained. The results indicate that the proposed method enables fabrication of large, dense ceramic parts with complex geometries.

Effects Of Temperature On Aqueous Freeform Extrusion Fabrication, Jie Li, Ming-Chuan Leu, Greg Hilmas

Mechanical and Aerospace Engineering Faculty Research & Creative Works

An experimental study was conducted to investigate the effect of temperature on ceramic parts produced by paste extrusion based additive manufacturing followed by sintering. A computer-controlled gantry system equipped with a piston extruder was used to extrude aqueous alumina paste. The system includes a temperature control subsystem that allows for freeform extrusion fabrication inside a low-temperature (<0°C) chamber. It can also be used for fabricating parts on a hot plate at ambient or higher temperatures (≥20°C). Test specimens were fabricated from aqueous aluminum pastes at -20°C in the low-temperature chamber and also on the hot plate at 40°C. The minimum angles achievable by these two processes for part fabrication, without use of support material, were compared. Also compared were the relative density and mechanical properties of the parts obtained after sintering. Microstructures were examined via scanning electron microscopy in order to obtain a deeper understanding of the effect of fabrication temperature.

Freeform Extrusion Fabrication Of Titanium Fiber Reinforced Bioactive Glass Scaffolds, Albin Thomas, Krishna C. R. Kolan, Ming-Chuan Leu, Greg Hilmas

Mechanical and Aerospace Engineering Faculty Research & Creative Works

Although implants made with bioactive glass have shown promising results for bone repair, their application in repairing load-bearing long bones is limited due to their low fracture toughness and fairly fast degradation response in vivo. In this paper, we describe our investigation of freeform extrusion fabrication of silicate based 13-93 bioactive glass scaffolds reinforced with titanium fibers. A composite paste was prepared with 13-93 bioactive glass filled with titanium fibers (~16 µm in diameter and aspect ratio of ~250) having a volume fraction of 0.4 vol. %. This paste was then extruded to fabricate scaffolds with an extrudate diameter …

Methods Of Extrusion On Demand For High Solids Loading Ceramic Paste In Freeform Extrusion Fabrication, Wenbin Li, Amir Ghazanfari, Ming Leu, Robert Landers

Faculty Publications, Mechanical Engineering

Fabrication of highly dense parts with complex geometry by paste-extrusion-based solid freeform fabrication processes requires a precise control of the extrusion flow rate to dispense material on demand, which is often referred as Extrusion-On-Demand (EOD). The extrusion process for aqueous ceramic pastes is complex and difficult to control due to their non-Newtonian behavior, compressibility and inhomogeneity. In this study, three methods of EOD (based on ram extruder, needle valve, and auger valve) are introduced and investigated for the extrusion of high solids loading (i.e., >50%, volumetric) aqueous alumina paste. Optimal extrusion process parameters for these methods are determined through printing …

Microstructure Development Of Granular System During Compaction, Chen Shang, Marcial Gonzalez

The Summer Undergraduate Research Fellowship (SURF) Symposium

Granular materials is the second most manipulated material in the industry today. They are easy to transport and more and more newly developed materials cannot stand the process of traditional casting, like energetic materials and bio-materials, but will survive the powder compaction process. Having a better understanding of the microstructure development of granular systems during compaction process, especially for particles that will heavily deform under loading, will give an insight of how to better process the powders to produce materials with overall better performance comparing to bulk materials. The main theory and mechanism applied are Hertz law and nonlocal contact …

In Vitro Assessment Of Laser Sintered Bioactive Glass Scaffolds With Different Pore Geometries, Krishna C. R. Kolan, Albin Thomas, Ming-Chuan Leu, Greg Hilmas

Mechanical and Aerospace Engineering Faculty Research & Creative Works

The pore geometry of bioactive glass scaffolds intended for use in bone repair or replacement is one of the most important parameters that could determine the rate of bone regeneration. The pore geometry would also affect the mechanical properties of the scaffolds and their rate of degradation. Scaffolds with five different architectures, having ~50% porosity, were fabricated with silicate (13–93) and borate (13–93B3) based bioactive glasses using a laser sintering process. An established, late-osteoblasts/early-osteocytes cell line was used to perform cell proliferation tests on the scaffolds. The results indicated that the cells proliferate significantly more on the scaffolds which mimic …

Effect Of Architecture And Porosity On Mechanical Properties Of Borate Glass Scaffolds Made By Selective Laser Sintering, Krishna C. R. Kolan, Ming-Chuan Leu, Greg Hilmas, Taylor Comte

Mechanical and Aerospace Engineering Faculty Research & Creative Works

The porosity and architecture of bone scaffolds, intended for use in bone repair or replacement, are two of the most important parameters in the field of bone tissue engineering. The two parameters not only affect the mechanical properties of the scaffolds but also aid in determining the amount of bone regeneration after implantation. Scaffolds with five different architectures and four porosity levels were fabricated using borate bioactive glass (13-93B3) using the selective laser sintering (SLS) process. The pore size of the scaffolds varied from 400 to 1300 μm. The compressive strength of the scaffolds varied from 1.7 to 15.5 MPa …

Effect Of Particle Size, Binder Content And Heat Treatment On Mechanical Properties Of 13-93 Bioactive Glass Scaffolds, Krishna C. R. Kolan, Ming-Chuan Leu, Greg Hilmas, Mariano Garcia Velez

Mechanical and Aerospace Engineering Faculty Research & Creative Works

Particle size, binder content and the post-processing schedule are important parameters that affect the microstructure, and, hence, the mechanical properties of parts produced using the indirect selective laser sintering process. 13-93 bioactive glass, with mean particle sizes ranging from 10 μm to 44 μm, is mixed with different amounts of stearic acid binder to fabricate green scaffolds. Through the design of the post-processing schedule, the time required for postprocessing the green scaffolds is reduced from the initial 80 hrs to 12 hrs. The compressive strength varies from 41 MPa for a part with~60% porosity to 157 MPa for a part …

Freeze Extrusion Fabrication Of 13-93 Bioactive Glass Scaffolds For Bone Repair, Tieshu Huang, Nikhil D. Doiphode, M. N. Rahaman, Ming-Chuan Leu, B. Sonny Bal, D. E. Day

Materials Science and Engineering Faculty Research & Creative Works

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 …

Selective Laser Sintering Of 13-93 Bioactive Glass, Krishna C. R. Kolan, Ming-Chuan Leu, Greg Hilmas, Mariano Garcia Velez

Mechanical and Aerospace Engineering Faculty Research & Creative Works

Bioactive glasses are more promising than biopolymers in fabricating scaffolds for bone tissue repair because they convert to hydroxyapatite, when implanted in vivo. Both direct and indirect selective laser sintering (SLS) methods of 13-93 bioactive glass were considered in this research to study the feasibility of fabricating scaffolds for bone repair applications. Stearic acid was used as the binder in the indirect method to fabricate the scaffolds. The green scaffolds underwent binder burnout and sintering at various soaking conditions between 675⁰C and 700⁰C, achieving a maximum compressive strength of 23.6 MPa, which is higher than that of the human cancellous …

Freeform Fabrication Of Zirconium Diboride Parts Using Selective Laser Sintering, Ming-Chuan Leu, Erik B. Adamek, Tieshu Huang, Greg Hilmas, Fatih Dogan

Mechanical and Aerospace Engineering Faculty Research & Creative Works

Using the Selective Laser Sintering (SLS) process, both flexural test bars and 3D fuel injector components have been fabricated with zirconium diboride (ZrB₂) powder. Stearic acid was selected as the binder. Values of SLS process parameters were chosen such that the green parts could be built with sharp geometrical features and that the sintered parts could have good mechanical properties. After binder burnout and sintering, the SLS fabricated ZrB₂ test bars achieved 80% theoretical density, and the average flexural strength of the sintered samples was 195 MPa. These values demonstrate the feasibility of the SLS process for …

Aqueous-Based Extrusion Fabrication Of Ceramics On Demand, Michael S. Mason, Tieshu Huang, Robert G. Landers, Ming-Chuan Leu, Greg Hilmas, Michael W. Hayes

Mechanical and Aerospace Engineering Faculty Research & Creative Works

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 extrusion process on demand. Design pros and cons are examined and a comparison between two material reservoir designs is made. Tests were conducted to determine the optimal deposition parameters for starting and stopping of the extrudate on demand. The collected test data is used to create a process model that describes the relationship between ram velocity and material extrusion rate. …

Freeform Extrusion Of High Solids Loading Ceramic Slurries, Part I: Extrusion Process Modeling, Michael S. Mason, Tieshu Huang, Robert G. Landers, Ming-Chuan Leu, Greg Hilmas

Mechanical and Aerospace Engineering Faculty Research & Creative Works

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 novel 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, …

Freeze-Spray Processing Of Layered Ceramic Composites, Qiang Fu, Oratai Jongprateep, Ashlee Abbott, Fatih Dogan

Materials Science and Engineering Faculty Research & Creative Works

Thermal gradients and associated stresses are critical in designing with ceramic composites having low thermal conductivity. In order to reduce the stresses from thermal gradients, compositional gradients are employed in designing of composite structures. This study addresses development of freeze-spray process to fabricate layered ceramic structures with controlled layer thickness and microstructural development. The composites were processed by spraying of ceramic slurries with low binder content and relatively high solids loadings (up to 40 vol%) on a cooled substrate. The frozen parts were freeze-dried and sintered at elevated temperatures. The relationship between microstructural development and thermal expansion behavior of Al …

Recent Developments In Extrusion Freeform Fabrication (Eff) Utilizing Non-Aqueous Gel Casting Formulations, Greg Hilmas, John L. Lombardi, Robert A. Hoffman, Kevin Stuffle

Materials Science and Engineering Faculty Research & Creative Works

Extrusion Freeform Fabrication (EFF) was shown to be an extremely versatile method for fabricating Functionally Graded Materials (FGMs) The approach is inexpensive and potentially feasible for grading between any thermodynamically compatible ceramic-metal, ceramic-ceramic, or metal-metal material combination. Several material systems were investigated in this study including alumina-304 stainless steel, zirconia-304 stainless steel, alumina-Inconel 625, zirconiaInconel625, alumina-nickel aluminide, zirconia-nickel aluminide, titanium carbide-InconeI625, titanium diboride-nickel aluminide, and tungsten carbide-nickel aluminide. A controlled gradient was demonstrated between the end members for all of the above compositions. The FGMs were hot pressed to achieve near theoretical densities, providing flexural strengths as high as 1000 …