Manufacturing and Processing of Advanced Ceramic Materials: On-Demand Advanced Manufacturing Process of Ceramics
Sponsored by: ACerS Manufacturing Division
Program Organizers: Bai Cui, University of Nebraska Lincoln; James Hemrick, Oak Ridge National Laboratory; Mike Alexander, Allied Mineral Products; Eric Faierson, Iowa State University; Keith DeCarlo, Blasch Precision Ceramics
Friday 8:00 AM
October 22, 2021
Room: On-Demand Room 4
Location: MS&T On Demand
Session Chair: Tatsuki Ohji, National Institute of Advanced Industrial Science and Technology ; Bai Cui, University of Nebraska-Lincoln
Invited
The Future of Manufacturing in Energy-intensive Industries: William Lee1; Michael Rushton1; Simon Middleburgh1; Phylis Makurunje1; 1Bangor University
Production of steel and other metals, glass, refractories, cement and other ceramics, uses much energy and generates high volumes of CO2 either in process or to reach the high temperatures necessary. With the push for Net Zero by 2050 Governments’ are looking closely at these energy-intensive industries and legislation will follow to ensure compliance with this global need. We examine technical options to achieve reductions in CO2 emissions including use of thermal management via multi-sensor monitoring and single location control. We examine low-temperature manufacturing routes such as cold sintering, focused energy routes such as Additive Layer Manufacture, and novel routes for nuclear fuel production. Use of hydrogen as a fuel and in processes e.g. in steelmaking will be discussed along with potential to develop Clean Energy Industrial Parks using low carbon nuclear power generated by small modular and micro-reactors. Finally, we consider the potential for manufacturing in extra-terrestrial applications.
Invited
Making Pre-stressed Ceramics with High Strength and High Damage Tolerance: Yiwang Bao1; Fenghua Kuang1; Yi Sun2; Yueming Li2; Detian Wan1; Zongyang Shen2; Delong Ma1; Lingfeng He3; 1China Building Materials Academy; 2Jingdezhen Ceramic Institute; 3Idaho National Laboratory
High strength and high damage-tolerance are critical for the reliability and durability of ceramic components. In the past decades, various strengthening mechanisms or processes, such as dispersion strengthening, minimizing grain size and porosity, reduction of crystal anisotropy and localized stresses, functionally grading glass/ceramic/glass structures, introduction of compressive stress in the surface layer by quenching or laser shock etc., have been proposed to enhance the mechanical properties of ceramics and obtained great achievements. However, large-scale and economical fabrication technology is still a goal for applications. We propose a simple method to prepare pre-stressed ceramics with high strength and high damage tolerance. Residual surface compressive stress is generated in ceramic components by pressureless sintering of a green bulk coated with a thin layer of low coefficient of thermal expansion. This method is simple and economical and has potential for reinforcement of structural ceramics, building ceramics, refractories, and bioceramics.
Invited
Progress of Silicon Nitride: Processing, Structure and Property: Tatsuki Ohji1; You Zhou1; Hiroyuki Miyazaki1; Hideki Hyuga1; Kiyoshi Hirao1; 1National Institute of Advanced Industrial Science and Technology
Silicon nitride is one of the most widely used engineering ceramics for a variety of structural applications because of their excellent mechanical and thermal properties. During the last four decades, a great deal of research effort has been devoted for tailoring the microstructures through innovative processing routes and enhancing the properties, leading to tremendous progress of silicon nitride. This paper gives an overview on such progress of silicon nitride, focusing on the processing-structure-property relationship, with some examples of how a unique processing route generates a novel microstructure, which brings enhanced properties in turn. The paper also focuses on the recent developments and applications of silicon nitride ceramics, including high thermal conductivity substrates for next-generation power devices, which are subjected to harsh temperature cycling conditions between -50 and 250ºC and large internal residual stress arising due to thermal expansion mismatch with metal parts, requiring substantial thermal fatigue resistance.
Invited
Issues Related to the Manufacturing and Processing of Refractory Ceramic Materials: James Hemrick1; 1Oak Ridge National Laboratory
Although refractory ceramic products are often viewed as merely “dirt in a bag”, these materials are in actuality highly engineered systems. Through a combination of chemical composition, microstructure, and thermo-physical properties; these complex ceramics can be designed and produced to improve the energy efficiency and decrease the environmental impact of the various industrial processes that our manufacturing-based society is dependent upon. This talk will explore how the proper design and production of refractory ceramic technology can lead to a more sustainable industrial footprint and preserve our resources and environment while maintaining our modern standard of living.
Comparison of Microstructural Evolution of Hydroxyapatite Powder Sintered by Microwave, SPS and Conventional Sintering: Anne Leriche1; Pierre Lefeuvre1; Vedi Dupont2; Diana Vitiello3; Hamza Karouiti3; Anthony Thuault1; David Smith3; Stéphane Hocquet2; 1UPHF - LMCPA; 2BCRC; 3IRCER Limoges
For recent years, new sintering techniques were developed such as microwave sintering, spark plasma sintering and cold sintering. Microwave sintering and SPS techniques can be used to sinter ceramics at a faster rate with reduced grain growth. The hypothesis backing this study is that this behavior difference might be explained by different mechanisms occurring at the first step of sintering. A two-step sintering process was applied to a sub-micrometer sized pure hydroxyapatite. The first step involved either conventional heat treatment, microwave or spark plasma techniques to achieve partially densified (~70% theoretical density) ceramics for microstructural analysis. Then in the second step the samples were fully densified by conventional sintering. Differences in grain size were observed after the first step of sintering and were maintained after the second sintering step leading to denser ceramics compared to those obtained by uniquely conventional sintering.
Luminescence Thermometry - Striving a Breakthrough: Eugeniusz Zych1; Paulina Bolek1; Małgorzata Sójka1; Dagmara Kulesza1; Joanna Trojan-Piegza1; 1University of Wroclaw
For the last dozen or so years, the number of publications on luminescence thermometry has been growing steadily and rapidly. In the meantime, this field has split into several parallel research directions due to different requirements they set. For medical and biological applications, sensitivity is a prime concern, but within a limited temperature range, while space research, aviation or thermal imaging of electronics require a wider measuring range and can be satisfied with a lower sensitivity. We will critically discuss possible expectations from luminescent thermometers. We will pay a special attention to luminescent thermometers, which could operate in a wide range, offering a relatively high sensitivity. Physics puts clear limitations here. Can we undertake a kind of game here that will turn limitations into opportunities? We will be discussing this challenge during our presentation. This research was supported by the Polish National Centre (NCN) under the grant # UMO-2018/29/B/ST5/00420.
Leveraging Computational Thermodynamics for Guiding SiC-ZrC Chemical Vapor Deposition Process Development: Benjamin Lamm1; Jian Peng2; Jake McMurray2; Dongwon Shin2; David Mitchell2; 1Oak Ridge National Laboratory; 2Materials Science and Technology Division, Oak Ridge National Laboratory
The codeposition of SiC-ZrC using CVD is of interest for application as high temperature materials. Computational thermodynamics was used to explore the potential CVD processing space with regards to pressure and temperature for a given set of precursor gases. The Zr process gas was generated via chlorination of solid metal pieces. Coupling thermodynamic calculations with experimental CVD can reduce the required number of CVD runs to achieve optimum deposition by refining experimental conditions prior to experimentation. Thermodynamics also offers insight into mechanistic decomposition and deposition behavior, potential for process impurities, and coating properties. A custom thermodynamic database developed at ORNL was used to model the cold-wall CVD process to identify an optimum region of temperature, pressure, and gas precursor ratios for deposition of the desired species. Representative characterization demonstrating the synergy between the model and the coating composition will be presented.Research sponsored by the Laboratory Directed Research and Development Program of Oak Ridge National Laboratory, managed by UT-Battelle, LLC for the US Department of Energy under contract DE-AC05-00OR22725.
Selective Laser Sintering of Hexagonal Barium Titanate Ceramics: Xiang Zhang1; Fei Wang1; Zhipeng Wu1; Yongfeng Lu1; Yan Chen2; Michael Nastasi3; Bai Cui1; 1University of Nebraska-Lincoln; 2Oak Ridge National Laboratory; 3Texas A&M University
A direct selective laser sintering (SLS) process was combined with a laser preheating procedure to decrease the temperature gradient and thermal stress, which was demonstrated as a promising approach for additive manufacturing of BaTiO3 ceramics. The phase compositions in BaTiO3 ceramics fabricated by SLS were investigated by X-ray and neutron diffractions. SLS resulted in the formation of the high-temperature phase, h-BaTiO3, which was retained at room temperature possibly due to the high cooling rate. A dense hexagonal h-BaTiO3 layer was formed on the surface and extended to a depth of 500 μm, with a relative density of higher than 97% and absence of pores or microcracks. The grain boundaries of SLSed h-BaTiO3 ceramics consist of a Ti-rich secondary phase. Compared with that of the pressureless sintered t-BaTiO3 ceramics, the Vickers hardness of SLSed h-BaTiO3 was 70% higher.
Chemical Vapor Deposition of Zirconium-silicon-carbon Compositions: David Mitchell1; Benjamin Lamm1; Michael Lance1; Kevin Cooley1; Ercan Cakmak1; Todd Groff1; 1Oak Ridge National Laboratory
Chemical vapor deposition (CVD) was employed to fabricate materials with zirconium, silicon and carbon in the microstructure. CVD enables incorporation of multiple elements into a microstructure by delivering gaseous precursors to a heated substrate surface in the reaction chamber. A cold-wall CVD system was used to deposit coatings onto a graphite susceptor disk, heated via radiofrequency (RF) field. The precursor gas containing zirconium was created via chlorinating metal pieces to form a zirconium chloride gas. The microstructure of the deposited materials was evaluated using metallography and scanning electron microscopy. The chemistry and phases present were investigated via x-ray diffraction and Raman microscopy with chemometric principal component analysis. Analysis shows the CVD processing method was successful in depositing multiphase refractory metal-ceramic materials.Research sponsored by the Laboratory Directed Research and Development Program of Oak Ridge National Laboratory, managed by UT-Battelle, LLC for the US Department of Energy under contract DE-AC05-00OR22725.
A Novel Room-temperature Synthesis Technique for Producing High-density Electroceramic Composites: Evan Smith1; Rick Ubic1; 1Boise State University
Room-temperature fabrication represents a major technological leap in ceramic processing techniques. This procedure has the potential to save a significant amount of energy because it avoids use of the high temperatures needed for conventional ceramic sintering techniques. In this work, a novel approach is taken to achieve high densities (>90%) in ceramic compacts at room temperature. The electroceramic filler material (BaxSr1-xTiO3 or PbZr1-yTiyO3) is mixed with an aqueous solution of a dielectric binder material (e.g. Li2MoO4) and pressed in a cylindrical die under high pressure and high vacuum using a vacuum-assisted uniaxial press. The die is then immersed in a bath sonicator for various times, after which it is pressed again. A major advantage of this technique is that it uses a relatively small amount of binder material (~15vol%); thus, the electroceramic filler material is the dominant phase in the resultant composite pellets.
Aqueous Colloidal Processing of WC Based Materials with Alternative Metals as Sintering Aids or Binder: Antonio Javier Sanchez-Herencia1; Macarena Garcia-Ayala1; Begoña Ferrari1; Jose Ygnacio Pastor2; 1Institute for Ceramic and Glass; 2ETSI Caminos-UPM
Severe environments require of new materials designs where the properties of the compounds can be exploited in an effective manner. This work presents the use of aqueous slurries of WC with nanosized nickel and with metallic tungsten as a valid method to achieve a high dispersion of the phase and promote the manufacture of dense composites. By controlling the media conditions using an anionic dispersant slurries of WC with 5vol% of Nickel and with metallic W has been formulated. Dispersion conditions have been optimized in terms of dispersant and total solid contents with rheological measurements.WC with 5 vol% of Nickel has been sintered with high density through a liquid-phase sintering process. These CerMets show a good mechanical properties with high hardness and toughness. In the case of using metallic tungsten, only a WC/W2C composite is obtained after sintering by SPS.
Spark Plasma Joining of HfB2-ZrB2-SiC Composites Using Ni as a Filler: Shipra Bajpai1; Alok Bhadauria1; T. Venkateswaran2; Sudhanshu Singh1; Kantesh Balani1; 1Indian Institute of Technology Kanpur; 2Vikram Sarabhai Space Centre/ISRO
Real-life applications of Ultra-high temperature ceramics require them to be joined into the final complex shapes. Herein, pre-sintered HfB2-ZrB2-SiC (HZS) composite was diffusion bonded by spark plasma joining (1100 °C, 18 MPa) with pure Ni powder interlayer. The interfacial microstructure evolution and its effect on the hardness were investigated. Microstructure and phase analysis shows that Ni reacted preferentially with SiC and formed Ni2Si phase that leads to a large interaction layer (~ 200 µm) and smaller Ni joint layer (~ 40 µm). Uniform micro-hardness of 16 GPa was obtained at HZS composite, interaction layer, and Ni joint region, owing to good bonding, no apparent cracking, and compositional homogeneity at the interface. Modulus distribution and wear mechanism were also investigated by dynamic modulus mapping and micro-scratch testing, which demonstrates spark plasma joining as a useful approach to produce complex components without compromising mechanical and tribological properties across the joint.
Pressureless Sintered SiC Formed via Thermoplastic Fugitive Binders for High-temperature Applications: Rodrigo Orta Guerra1; Olivia Brandt1; Rodney Trice1; Jeffrey Youngblood1; 1Purdue University
Silicon carbide (SiC) has been identified as an ideal candidate material for high temperature applications due to its good strength, excellent resistance to corrosion and oxidation. Commercial applications require the capability to manufacture complex shapes at low cost and high sintered densities for mechanical integrity. SiC mixed with thermoplastics offers an alternative to mold and extrude ceramics at temperatures below 150°C. In this study, the effect of different loading volumes of SiC on a thermoplastic blend composed of Poly-(Isobutyl Methacrylate), Polyethylene Glycol, Heavy Mineral Oil and Ethylene Ethyl Acrylate was investigated to determine physical and mechanical properties after binder removal and sintering.
Development Calcium Doped La(Cr0.2Co0.2Fe0.2Mn0.2Ni0.2)O3 High Entropy Perovskite Oxides: Sai Ram Gajjala1; Rasit Koc1; 1Southern Illinois University
Calcium (0-30mol%) doped La(Cr0.2Co0.2Fe0.2Mn0.2Ni0.2)O3 High Entropy Perovskite Oxide (HEPO) materials are synthesized by the polymerizable precursor method (1). The impact of calcium doping at various levels on the unit cell, sintering, and electrical conductivity is studied. The electrical conductivity of the present materials is due to a p-type small polaron mechanism (2). X-ray Diffraction (XRD) was used to investigate the phase purity. Energy Dispersive X-Ray Spectroscopy (EDX) was utilized to evaluate the uniformity of the elements in the materials. A Scanning Electron Microscope (SEM) was used to investigate the sintering conditions further. The four-probe AC method was used for conductivity measurements. To analyze the surface characteristics and valence states of transition metals, X-ray Photoelectron Spectroscopy (XPS) was used.
Mechanical Properties of La2Zr2O7/ ZrO2 Composites Prepared by Coating of ZrO2 Sol: Bong-Gu Kim1; Hyun-Hee Choi2; GuanLin Lyu2; JangHyeok Pyeon1; Jung-Hun Son2; SeungCheol Yang1; Yeon-Gill Jung1; 1Department of Materials Convergence and System Engineering of Changwon National University; 2Changwon national university
ZrO2 with 7–8wt% yttria (YSZ) is widely used as a thermal barrier coating (TBC) material owing to its high coefficient of thermal expansion (CTE) and low thermal conductivity. However, YSZ shows poor sintering resistance and phase stability, limiting its operating temperature to 1200℃. Even though La2Zr2O7 (LZO) is a promising material for the TBC with better phase stability and lower thermal conductivity than YSZ, it shortens the thermal cycle performance of TBC owing to its low fracture toughness and CTE. Therefore, the LZO/ZrO2 composite power was prepared to make up for the weak points of LZO. The ZrO2 sol was uniformly coated on the LZO powder, depending on processing parameters, and the composite improved the mechanical properties and CTE values compared to LZO. It was verified that the LZO/ZrO2 composite powder could be employed as a new feedstock for TBC that complements the shortcomings of LZO and YSZ.
Dispersion Studies of Alumina Toughened Zirconia Powders for Direct Ink Writing Applications: Berfu Goeksel1; Erin Koos1; Bart Van Meerbeek1; Jozef Vleugels1; Annabel Braem1; 1KU Leuven
Nanoparticles tend to agglomerate due to adhesive Van der Waals forces. To overcome these adhesive forces and break down agglomerates, polyelectrolytes are a good choice as dispersant. They provide electrosteric stabilization which is a combination of purely electrostatic repulsion and polymeric repulsion. To obtain the desired dispersion, the interaction of the ceramic powder with dispersant and optimum dispersant amount should be carefully examined. Therefore, three commercial dispersants are evaluated with the aim of finding the best dispersant and the optimum dispersant amount for 20 wt% alumina toughened zirconia powder (TZ-3YS-20A & TZ-3Y-20A, TOSOH, Japan). The studied anionic dispersants, Darvan CN, Darvan 821A, and Dolapix CE 64 are all completely water-soluble. The optimum dispersant content is studied in the range of 0.25-1.50 "mg" ⁄"m" ^"2". Based on the visual inspection, sedimentation rate, rheology tests, and zeta potential measurements, the best dispersant and optimum amount are reported for alumina toughened zirconia powders.
Analysis of Crystal Structure in Calcium and Strontium Hexaborides with Lithium Dopants: Alan Hirales1; Olivia Graeve1; 1University of California San Diego
We present the structural behavior of two solid solutions, Cax-1LixB6 and Srx-1LixB6 (x = 0, 0.1, 0.3, 0.5), and show their evolution as the experimental concentration, x, is increased. The powders were synthesized by combustion synthesis, acid-washed with HCl, and characterized using X-ray diffraction (XRD), electron energy-loss spectroscopy (EELS), electron diffraction, and transmission and scanning electron microscopy (TEM and SEM, respectively). Electron micrographs mostly show cubic morphologies with a particle size range from ~100 nm to 1 µm, while XRD analyses demonstrate single solid solution phases. EELS results suggest a homogeneous distribution of Li ions across the cubic nanoparticles. Finally, TEM along with electron diffraction show that the structures possess a high degree of crystallinity, with minimal misalignments and changes in crystallite orientation.