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 electromagnetic-thermal-mechanical (EMTM) model. The developed multiphysics model reveals that the metal powder specimen's runaway does not result from its intrinsic material properties, but results from the resonance phenomenon thermally activated by the surrounding tooling material. The EMTM simulation predicts with a very good accuracy the microwave repartition and the resulting densification and powder specimen's shape distortions observed experimentally. The comparison of the microwave and conventional sintering kinetics indicates an important acceleration of the sintering behavior under microwave heating. The developed sintering approach has a potential of the implementation for time-effective mass production of small metal parts.
The microwave sintering homogeneity of large and complex shape specimens is analyzed. A new approach enabling the fabrication of complex shapes ceramics via 3D printing and microwave sintering is presented. The use of a dental microwave cavity is shown to enable a substantial level of densification of complex shape components while restricting the grain growth. The homogeneity of the processed samples during microwave sintering is studied by an electromagnetic-thermal-mechanical simulation. The realistic densification behavior, that phenomenologically takes into account the microwave effect, i…
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 …
The present work reports the effect of Ta on densification and microstructure evolution during non-isothermal and spark plasma sintering of nanocrystalline W. Nanocrystalline W-5wt.%Ta alloy powder was synthesized using mechanical alloying. The nanocrystalline powder was characterized thoroughly using X-ray diffraction line profile analysis. Furthermore, the shrinkage behavior of nanocrystalline powder was investigated during non-isothermal sintering using dilatometry. Subsequently, the alloy powder was consolidated using spark plasma sintering up to 1600 °C. The role of Ta on stabilizing the …
The present work reports the role of different atomic mobility induced localized pore evolution on densification during spark plasma sintering of nanocrystalline W-Mo alloy powder. The shrinkage (or expansion) behavior of cold compacted milled powders was studied using dilatometry during non-isothermal sintering up to 1600 °C. Subsequently, the milled powders were densified to ~95% relative density using spark plasma sintering up to 1600 °C. The enhanced localized Joule heating due to dynamically evolved porous structure could be attributed for the densification during spark plasma sintering.
In this work, sintered polycrystalline cubic boron nitride (cBN) compacts, with titanium carbonitride (TiC0.7N0.3) and titanium nitride (TiN), respectively, as binders, were prepared at temperature of 1450°C and pressure of 5.5 GPa during 3 minutes, and the influence of binders on the plastic deformation of cBN powder due to the sintering process was experimentally investigated by X-ray diffraction (XRD) analysis. It was shown that the sintered compact with titanium carbonitride as a binder displays more intense plastic deformation of cBN grains than that with titanium nitride binder. This res…
The thermoelectric properties of AlMgB14-based materials prepared by spark plasma sintering were investigated. Al, Mg, and B powder were used as raw material powders. The raw powders were mixed using a V-shaped mixer, and then the mixture was sintered at 1673 K or 1773K. The mixture ratio of raw powders was varied around stoichiometric ratio of AlMgB14. X-ray diffraction patterns of samples showed that all samples consist of AlMgB14 and some by-products, MgAl2O4, B2O and AlB12. The Seebeck coefficient of the samples exhibited significant change depending on the varying mixture ratio. One sampl…
Selective laser sintering (SLS) of single component metal powders is a rapid prototyping technology in which a high-energy laser beam scans, melts, shrinks and consolidates metal powders with single component. For better understanding physical mechanisms during laser sintering of single-component metal particles, a temperature transforming model with the consideration of shrinkage and convective flows is introduced to analyze the thermal/fluid behaviors in selective laser sintering of single powder layer. The model is also applied to investigate the sintering of powders on top of existing sint…
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 …
The effect of sintering temperatures (Ts) on the structural and magnetic properties of Ni0.6Zn0.4Fe2O4 (NZFO) ferrites synthesized by conventional double sintering method has been reported. The samples are sintered at 1200, 1250 and 1300 °C. The X-ray diffraction (XRD) analysis reveals the formation of a single phase cubic spinel structure of the sample. The magnetic parameters such as saturation magnetization, Ms; coercive field, Hc; remanent magnetization, Mr and Bohr magneton, μB are determined and well compared with reported values. The obtained values are found to be 71.94 emu/gm and 1.2 …
A novel and sustainable method to develop non-equiatomic CoCrFeNiMox high entropy alloys via spark plasma sintering using commercial commodity powders and evaluation of its mechanical behaviour
This work investigates a method for pre-screening material systems for Selective Laser Sintering (SLS) using a combination of Revolution Powder Analysis (RPA) and machine learning. To develop this method, nylon was mixed with alumina or carbon fibers in different wt.% to form material systems with varying flowability. The materials were measured in a custom RPA device and the results compared with as-spread layer density and surface roughness. Machine learning was used to attempt classification of all powders for each method. Ultimately, it was found that the RPA method is able to reliably cla…
DC flash sintering of both pure and 0.5 mol. % Bi2O3-doped ZnO at a relatively high activating field of 300 V/cm has been investigated. It is demonstrated that even high-purity ZnO single crystals can "flash" at 870C. In comparison, flash sintering occurs at a substantially lower onset temperature of 550C in ZnO powder specimens, indicating the important roles of surfaces and/or grain boundaries. A model has been developed to forecast the thermal runaway conditions and the predictions are in excellent agreements with the observed onset flash temperatures, attesting that the flash starts as a t…
Magnetic isotropic NdFeB powder is processed by the following additive manufacturing methods: (i) stereolithography (SLA), (ii) fused filament fabrication (FFF), and (iii) selective laser sintering (SLS). For the first time, a stereolithography based method is used to 3D print hard magnetic materials. FFF and SLA use a polymer matrix material as binder, SLS sinters the powder directly. All methods use the same hard magnetic NdFeB powder material. Complex magnets with small feature sizes in a superior surface quality can be printed with SLA. The magnetic properties for the processed samples are…
Spark plasma sintering (SPS) technique is applied in combination with hydrogen decrepitation process for the recycling of SmCo5 magnets. The SmCo5 magnets for recycling were first decrepitated by hydrogen gas of a pressure of 4 bar for 3 hours to produce decrepitated powder. This powder was then used to prepare isotropic sintered magnets using the SPS technique, by sintering at 800-1000 oC for 1 minute. Full densification of the SPS-ed magnets was possible at a temperature of 1000 oC. The sample sintered at 900 oC showed the best internal coercivity (jHc) of higher than 1500 kA/m with high rem…
Predicting the microstructure during selective laser sintering (SLS) is of great interests, which can compliment the current time and cost expensive trial-and-error principle with an efficient computational design tool. However, it still remains a great challenge to simulate the microstructure evolution during SLS due to the complex underlying physical phenomena. In this work, we present a three-dimensional finite element phase-field simulation of the SLS single scan, and revealed the process-microstructure relation. We use a thermodynamically consistent non-isothermal phase-field model includ…
One of the major barriers in adapting the existing EB-PBF process parameters to a new powder material system is controlling the preheating conditions such that every layer of powder results in enough partial sintering to create a coherent powder cake. To be able to understand the powder sintering process and adapt it to other materials, we must look at the degree of sintering and the effective thermal conductivity of the powder bed. An in-depth understanding of these characteristics will help tailor the preheating conditions and furthermore, make it easier to remove/de-powder intricate parts a…
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…
The size effect of the raw B powder on the MgB2 phase formation has been studied by the technique of in-situ high temperature resistivity (HT-rT) measurement. The onset temperature, Tonset, and the completion temperature, TPF, of the phase formation are determined directly during the ongoing thermal process. These two temperatures, Tonset and TPF of the sample synthesized using nanometer B and Mg powders (NanoB-MgB2) are 440 C and 490 C, respectively, the same as those of the sample using micrometer B and nanometer Mg powders (MicroB-MgB2). This indicates that the phase formation temperature o…
Nanocrystalline bulk materials are desirable for many applications as they combine mechanical strength and specific electronic transport properties. Our bottom up approach starts with tailored nanoparticles. Compaction and thermal treatment are crucial, but usually the final stage sintering is accompanied by rapid grain growth which spoils nanocristallinity. For electrically conducting nanoparticles, field activated sintering techniques overcome this problem. Small grain sizes have been maintained in spite of consolidation. Nevertheless, the underlying principles, which are of high practical i…
It is presented some technological parameters and physical characteristics of Fe - Ni - Al composite materials, fabricated by pressing with following sintering at a high temperature, and also shock-wave compacted using explosives. The comparison of materials properties fabricated using different technologies at equal precursor powders parameters (dimensions and shape of particles, a way of their mixing and density of filling) points on the difference of their phase compositions, metallographic and defect structure, porosity and some physical properties.
Critical role of phase-dependent properties in modeling photothermal sintering of LiCoO2 cathodes
Empa - Swiss Federal Laboratories for Materials Science and Technology（瑞士联邦材料科学与技术研究院）；National Centre for Computational Design and Discovery of Novel Materials MARVEL, Empa（MARVEL新型材料计算设计与发现国家中心，瑞士联邦材料科学与技术研究院）；Univ. Grenoble Alpes, CEA, Leti（格勒诺布尔阿尔卑斯大学，法国原子能和替代能源委员会，电子学和信息技术实验室）
In this paper, a 3 Dimensional dynamic model of a perforated rectangular metal hydride tank is presented. The metal hydride tank consists of powder LaNi5 and the tubes are organized in the geometry of the rectangular in order to simulate the flux of the ambient air through the reactor, which affect hardly both the hydriding and the dehydriding reaction. A simulating study is made by solving simultaneously the energy, mass and momentum differential equations of conservation by using Comsol Multiphysics (version 4.2) software. The simulation results show great agreement with the experimental dat…
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…
Microwave Pressing is a promising way to reduce microwave sintering temperatures and stabilize microwave powder materials processing. A multi-physics simulation was conducted of the regulated pressure-assisted microwave cavity. This simulation took into consideration resonance phenomena and the nonlinear temperature-dependent material parameters of zirconia. The intrinsic behaviors of microwave systems and zirconia make the regulation of the microwave pressing difficult. However, the same phenomena can be used to activate flash sintering. Flash microwave sintering uses high electric fields of …
Recent investigations have shown that highly oxygen defective cerium oxides generate non-classical electrostriction that is superior to lead-based ferroelectrics. In this work, we report the effect of field-assisted spark plasma sintering (SPS) on electro-chemo-mechanical properties on Ca-doped ceria (CDC). Nanometric powders of ca. 10 nm are rapidly consolidated to form polycrystalline nanostructures with a high degree of crystalline disorder. Remarkably, the resultant material demonstrates a large electromechanical strain without a frequency-related relaxation effect. We conclude that electr…
We prepared Li0.5Mn0.5Fe2O4 ferrite through chemical reaction in highly acidic solution and subsequent sintering of chemical routed powder at temperatures > 800 0C. Surface morphology showed plastoferrite character for sintering temperature > 1000 0C. Mechanical softening of metal-oxygen bonds at higher measurement temperatures stimulated delocalization of charge carriers, which were strongly localized in A and B sites of the spinel structure at lower temperatures. The charge delocalization process has activated semiconductor to metallic transition in ac conductivity curves, obeyed by Jonscher…
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…
Nanocrystalline metals and ceramics with <100 nm grain sizes and superior properties (e.g., mechanical strength, hardness, fracture toughness and stored dielectric energy) are of great interest. Much has been discussed about achieving nano grains, but little is known about maintaining grain-size uniformity that is critical for material reliability. An especially intriguing question is whether it is possible to achieve a size distribution narrower than what Hillert[1] theoretically predicted for normal grain growth, a possibility suggested, for growth with a higher growth exponent, by the gener…
Combined Thermal Expansion and Hydrolytic Stability Study of Lanthanide Vanadates LnVO4 and CaLnZr(VO4)3 (Ln = La, Nd, Sm, Eu, Gd, Dy, Yb) with Zircon and Monazite Structures
Nanocrystalline metal alloys show great potential as structural materials, but are often only available in small volumes such as thin films or powders. However, recent research has suggested that dopant segregation and grain boundary structural transitions between states known as complexions can dramatically alter grain size stability and potentially enable activated sintering. In this study, we explore strategic consolidation routes for mechanically alloyed Cu-4 at.% Zr powders to capture the effects of amorphous complexion formation on the densification of bulk nanostructured metals. We obse…
A multiphysics modeling approach for heat conduction in metal hydride powders is presented, including particle shape distribution, size distribution, granular packing structure, and effective thermal conductivity. A statistical geometric model is presented that replicates features of particle size and shape distributions observed experimentally that result from cyclic hydride decreptitation. The quasi-static dense packing of a sample set of these particles is simulated via energy-based structural optimization methods. These particles jam (i.e., solidify) at a density (solid volume fraction) of…
Commercial nuclear power plants extensively rely on fission energy from uranium dioxide (UO2) fuel pellets that provide thermal energy; consequently, generating carbon-free power in current generation reactors. UO2 fuel incurs damage and fractures during operation due to large thermal gradients that develop across the fuel pellet during normal operation. The underlying mechanisms by which these processes take place are still poorly understood. This work is a part of our combined experimental and computational effort for quantifying the UO2 fuel fracture behavior induced by thermal shock. In th…
Titanium diboride (TiB2) is a low-density refractory material belonging to the family of ultra-high temperature ceramics (UHTCs). This paper reports on the production and microstructural and optical characterization of nearly fully dense TiB2, with particular interest to its potential utilization as novel thermal solar absorber. Monolithic bulk samples are produced starting from elemental reactants by a two-step method consisting of the Self-propagating High-temperature Synthesis (SHS) followed by the Spark Plasma Sintering (SPS) of the resulting powders. The surface of obtained samples has-be…
