Direct microwave heating of 3Y-ZrO 2 is studied at frequency of 2.45 GHz. Different conditions of input power, sample position and size are tested. For the first time, the experimentally known instability of microwave sintering is explained coupling the effective medium approximation and finite-element method. We show how the material dielectric permittivity imaginary part which increases with temperature and relative density encourages high hot spot phenomena. It is shown that the sample location has a great impact on the
Aiiso Yufeng Li Family Department of Chemical and Nano Engineering, Program in Materials Science and Engineering, University of California San Diego（加州大学圣地亚哥分校艾依索·于峰李家族化学与纳米工程系材料科学与工程项目）
Direct and hybrid microwave sintering of 3Y-ZrO 2 are comparatively studied at frequency of 2.45 GHz. Using the continuum theory of sintering, a fully coupled electromagnetic-thermalmechanical (EMTM) finite element simulation is carried out to predict powder samples deformation during their microwave processing. Direct and hybrid heating configurations are computationally tested using advanced heat transfer simulation tools including the surface to surface thermal radiation boundary conditions and a numeric proportional-integral-derivative (PID) regulation. The developed modeling framework sho…
The reliability of perovskite material LSCF to be used as cathode parts in solid oxide fuel cells also relies on its mechanical properties. Adequate surface conditions are desired when the as-sintered porous thin films are subjected to nanoindentation for mechanical property determination. In this study, extensive cracks and considerable surface roughness were found in the LSCF films after sintering at high temperatures. This would significantly scatter the nanoindentation data and result in unreliable measurements. Various attempts including the comparison of film deposition methods, drying a…
This study aimed to develop a contamination free porous titanium scaffold by a plasma activated sintering within an originally developed TiN coated graphite mold. The surface of porous titanium sheet with or without a coated graphite mold was characterized. The cell adhesion property of porous titanium sheet was also evaluated in this study. The peak of TiC was detected on the titanium sheet processed with the graphite mold without a TiN coating. Since the titanium fiber elements were directly in contact with the carbon graphite mold during processing, surface contamination was unavoidable eve…
The mechanism of rapid and selective heating of magnetic metal oxides under the magnetic field of microwaves which continues beyond the Curie temperature $ T_{c} $ is identified by using the Heisenberg model. Monte Carlo calculations based on the energy principle show that such heating is caused by non-resonant response of electron spins in the unfilled 3d shell to the wave magnetic field. Small spin reorientation thus generated leads to a large internal energy change through the exchange interactions between spins, which becomes maximal around $ T_{c} $ for magnetite $ {\rm Fe}_{3}{\rm O}_{4}…
The modeling of powder compaction process, such as spark plasma sintering (SPS), requires the determination of the visco-plastic deformation behavior of the particle material including the viscosity moduli. The establishment of these parameters usually entails a long and difficult experimental campaign which in particular involves several hot isostatic pressing tests. A more straightforward method based on the coupled sinter-forging and die compaction tests, which can be easily carried out in a regular SPS device, is presented. Compared to classical creep mechanism studies, this comprehensive …
A perturbation analysis has been conducted to evaluate the generation of hotspots inside an electrical loaded ceramic sample, which is assumed to have an Arrhenius-type conductivity. The results identified a critical size, above which a small temperature perturbations will be magnified and hotspots will be generated. It provides an estimate for the largest sample size suitable for flash sintering, beyond which hotspots are likely to form, resulting in inhomogeneous heating and sintering.
In this paper we show how reliable measurements on porous ceramic films can be made by appropriate nanoindentation experiments and analysis. Room-temperature mechanical properties of the mixed-conducting perovskite material LSCF6428 were investigated by nanoindentation of porous bulk samples and porous films sintered at temperatures from 900-1200C. A spherical indenter was used so that the contact area was much greater than the scale of the porous microstructure. The elastic modulus of the bulk samples was found to increase from 33.8-174.3 GPa and hardness from 0.64-5.32 GPa as the porosity de…
Flash sintering phenomena are predominantly associated with ceramics due to thermal runaway of their electric conductivity noticeably represented in materials such as zirconia or silicon carbide. Because of their high electric conductivity, flash sintering of metals is nearly inexistent. In this work, an original metal powder flash sintering method based on a microwave approach is presented. Within the developed approach, an unusually fast (60 s) thermal and sintering runaway of Ti-6Al-4V powder is experimentally revealed under microwave illumination. This phenomenon is simulated based on an e…
A new flash (ultra-rapid) spark plasma sintering method applicable to various materials systems, regardless of their electrical resistivity, is developed. A number of powders ranging from metals to electrically insulative ceramics have been successfully densified resulting in homogeneous microstructures within sintering times of 8-35 s. A finite element simulation reveals that the developed method, providing an extraordinary fast and homogeneous heating concentrated in the sample's volume and punches, is applicable to all the different samples tested. The utilized uniquely controllable flash p…
This work addresses the two great challenges of the spark plasma sintering (SPS) process: the sintering of complex shapes and the simultaneous production of multiple parts. A new controllable interface method is employed to concurrently consolidate two nickel gear shapes by SPS. A graphite deformable sub-mold is specifically designed for the mutual densification of the both complex parts in a unique 40 mm powder deformation space. An energy efficient SPS configuration is developed to allow the sintering of a large-scale powder assembly under electric current lower than 900 A. The stability of …
A mathematical model is presented for the Joule heating that occurs in a ceramic powder compact during the process of flash sintering. The ceramic is assumed to have an electrical conductivity that increases with temperature, and this leads to the possibility of runaway heating that could facilitate and explain the rapid sintering seen in experiments. We consider reduced models that are sufficiently simple to enable concrete conclusions to be drawn about the mathematical nature of their solutions. In particular we discuss how different local and non-local reaction terms, which arise from speci…
The General Thermodynamic Theory of Sintering, formulated by the author in 1998 is given. This theory is applied to the problem of swelling of materials under conditions of radiation. Driving forces, caused by the presence of the evolution of heat in the volume of a sample (electric contact, hf, inductive heating or penetrating radiation, e.g., neutrons could be the sources of the heat in the bulk of a sample) are considered. The influence of these driving forces on sintering, structure and properties is discussed. The role of mobile and immobile dislocations, grain boundaries, and pores is re…
An energy efficient spark plasma sintering method enabling the densification of large size samples assisted by very low electric current levels is developed. In this method, the electric current is concentrated in the graphite foils around the sample. High energy dissipation is then achieved in this area enabling the heating and full densification of large (alumina) parts ({Ø} 40 mm) at relatively low currents (800 A). The electrothermal mechanical simulation reveals that the electric current needed to heat the large samples is 70 % lower in the energy efficient configuration compared to the t…
Analyzing porous (nano)materials by the atom probe tomography has been notoriously difficult. The electrostatic pressure intensifies stress at voids which results in premature failure of the specimen, and the electrostatic field distribution near voids lead to aberrations that are difficult to predict. Here we propose a new encapsulating method for a porous sample using a low-melting-point Bi-In-Sn alloy, known as Fields metal. As a model porous sample, we used single-crystalline wustite following direct hydrogen-reduced into iron. The complete encapsulation is performed using in-situ heating …
The novel phototunable photonic structures based on electrochemically etched silicon filled with four photochromic azobenzene-containing compounds, bent-shaped low molar mass substance and side-chain polymethacrylates and copolyacrylate, were prepared and their photooptical properties were studied. It was found that irradiation of these composites with polarized blue light results in spectral changes in photonic band gap (split of the cavity mode) associated with cooperative photoorientation of azobenzene moieties inside silicon pores in direction perpendicular to the polarization plane of the…
Graphite is a unique material for high temperature applications and will likely become increasingly important as we attempt to electrify industrial applications. However, high-quality graphite can be expensive, limiting the cost-competitiveness of high-quality graphite technologies. Here, we investigate the thermal properties of low-cost, low-quality, macro-porous graphite to determine the tradeoff between cost and thermal performance. We use laser flash analysis (LFA) to measure the thermal diffusivity of graphite at high temperatures. However, due to the large pores in the graphite samples p…
