Quasi-instantaneous materials processing technology via high-intensity electrical nano pulsing.

Despite many efforts, the outcomes obtained with field-assisted processing of materials still rely on long-term coupling with other electroless processes. This conceals the efficacy and the intrinsic contributions of electric current. A new device utilizing electrical nano pulsing (ENP) has been designed and constructed to bring quasi-instantaneous modifications to the micro- and nano-structure in materials. Featuring ultra-high intensity (~ 1011 A/m2) and ultra-short duration (< 1 µs), the ENP technology activates non-equilibrium structural evolutions at nanometer spatial scale and nanosecond temporal scale. Several examples are provided to demonstrate its utility far outpacing any conventional materials processing technology. The ENP technology gives a practical tool for exploring the intrinsic mechanism of electric-field effects and a pathway towards the rapid industrial manufacturing of materials with unique properties.

Growing recyclable and healable piezoelectric composites in 3D printed bioinspired structure for protective wearable sensor.

Bionic multifunctional structural materials that are lightweight, strong, and perceptible have shown great promise in sports, medicine, and aerospace applications. However, smart monitoring devices with integrated mechanical protection and piezoelectric induction are limited. Herein, we report a strategy to grow the recyclable and healable piezoelectric Rochelle salt crystals in 3D-printed cuttlebone-inspired structures to form a new composite for reinforcement smart monitoring devices. In addition to its remarkable mechanical and piezoelectric performance, the growth mechanisms, the recyclability, the sensitivity, and repairability of the 3D-printed Rochelle salt cuttlebone composite were studied. Furthermore, the versatility of composite has been explored and applied as smart sensor armor for football players and fall alarm knee pads, focusing on incorporated mechanical reinforcement and electrical self-sensing capabilities with data collection of the magnitude and distribution of impact forces, which offers new ideas for the design of next-generation smart monitoring electronics in sports, military, aerospace, and biomedical engineering.

Additive manufacturing of titanium-based alloys- A review of methods, properties, challenges, and prospects.

The development of materials for biomedical, aerospace, and automobile industries has been a significant area of research in recent years. Various metallic materials, including steels, cast iron, nickel-based alloys, and other metals with exceptional mechanical properties, have been reportedly utilized for fabrication in these industries. However, titanium and its alloys have proven to be outstanding due to their enhanced properties. The ß-titanium alloys with reduced modulus compared with the human bone have found more usage in the biomedical industry. In contrast, the α and α+ß titanium alloys are more utilized to fabricate parts in the automobile and aerospace industries due to their relatively lightweight. Amongst the numerous additive manufacturing (AM) techniques, selective laser and electron beam melting techniques are frequently used for the fabrication of metallic components due to the full densification and high dimensional accuracy they offer. This paper reviews and discusses the different types of AM techniques, attention is also drawn to the properties and challenges associated with additively manufactured titanium -based alloys. The outcome from this study shows that 3D printed titanium and titanium-alloys exhibit huge prospects for various applications in the medical and aerospace industries. Also, laser-assisted 3D technologies were found to be the most effective AM method for achieving enhanced or near-full densification.

Proportional Integral Derivative Control in Spark Plasma Sintering Simulations.

The prediction of microstructure evolution and densification behavior during the spark plasma sintering (SPS) process largely depends on accurate temperature regulation. A loop feedback control algorithm called proportional integral derivative (PID) control is a practical simulation tool, but its coefficients are often determined by an inefficient "trial and error" method. This paper is devoted to proposing a numerical method based on the principles of variable coefficients to construct an optimal linear PID controller in SPS electro-thermal simulations. Different types of temperature profiles were applied to evaluate the feasibility of the proposed method. Simulation results showed that, for temperature profiles conventionally used in SPS cycles, the PID output keeps pace with the desired profile. Characterized by an imperfect time delay and overshoot/undershoot, the constructed PID controller needs further advancement to provide a more satisfactory temperature regulation for non-continuous temperature profiles. The first step towards a numerical rule for the optimal PID controller design was undertaken in this work. It is expected to provide a valuable reference for the advanced electro-thermal modeling of SPS.

Simultaneous Spark Plasma Sintering of Multiple Complex Shapes.

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 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 developed process is studied by electro-thermal-mechanical (ETM) simulation. The ETM simulation reveals that homogeneous densification conditions can be attained by inserting an alumina powder at the sample/punches interfaces, enabling the energy efficient heating and the thermal confinement of the nickel powder. Finally, the feasibility of the fabrication of the two near net shape gears with a very homogeneous microstructure is demonstrated.

Fabrication of Porous Materials by Spark Plasma Sintering: A Review.

Spark plasma sintering (SPS), a sintering method that uses the action of pulsed direct current and pressure, has received a lot of attention due to its capability of exerting control over the microstructure of the sintered material and flexibility in terms of the heating rate and heating mode. Historically, SPS was developed in search of ways to preserve a fine-grained structure of the sintered material while eliminating porosity and reaching a high relative density. These goals have, therefore, been pursued in the majority of studies on the behavior of materials during SPS. Recently, the potential of SPS for the fabrication of porous materials has been recognized. This article is the first review to focus on the achievements in this area. The major approaches to the formation of porous materials by SPS are described: partial densification of powders (under low pressures, in pressureless sintering processes or at low temperatures), sintering of hollow particles/spheres, sintering of porous particles, and sintering with removable space holders or pore formers. In the case of conductive materials processed by SPS using the first approach, the formation of inter-particle contacts may be associated with local melting and non-conventional mechanisms of mass transfer. Studies of the morphology and microstructure of the inter-particle contacts as well as modeling of the processes occurring at the inter-particle contacts help gain insights into the physics of the initial stage of SPS. For pre-consolidated specimens, an SPS device can be used as a furnace to heat the materials at a high rate, which can also be beneficial for controlling the formation of porous structures. In sintering with space holders, SPS processing allows controlling the structure of the pore walls. In this article, using the literature data and our own research results, we have discussed the formation and structure of porous metals, intermetallics, ceramics, and carbon materials obtained by SPS.

Iron oxide-based nanostructured ceramics with tailored magnetic and mechanical properties: development of mechanically robust, bulk superparamagnetic materials.

Nanostructured iron-oxide based materials with tailored mechanical and magnetic behavior are produced in bulk form. By applying ultra-fast heating routines via spark plasma sintering (SPS) to supercrystalline pellets, materials with an enhanced combination of elastic modulus, hardness and saturation magnetization are achieved. Supercrystallinity - namely the arrangement of the constituent nanoparticles into periodic structures - is achieved through self-assembly of the organically-functionalized iron oxide nanoparticles. The optimization of the following SPS regime allows the control of organics' removal, necking, iron oxide phase transformations and nano-grain size retention, and thus the fine-tuning of both mechanical properties and magnetic response, up until the production of bulk mm-size superparamagnetic materials.

Fabrication of Titanium-Niobium-Zirconium-Tantalium Alloy (TNZT) Bioimplant Components with Controllable Porosity by Spark Plasma Sintering.

Spark Plasma Sintering (SPS) is used to fabricate Titanium-Niobium-Zirconium-Tantalum alloy (TNZT) powder-based bioimplant components with controllable porosity. The developed densification maps show the effects of final SPS temperature, pressure, holding time, and initial particle size on final sample relative density. Correlations between the final sample density and mechanical properties of the fabricated TNZT components are also investigated and microstructural analysis of the processed material is conducted. A densification model is proposed and used to calculate the TNZT alloy creep activation energy. The obtained experimental data can be utilized for the optimized fabrication of TNZT components with specific microstructural and mechanical properties suitable for biomedical applications.

All-Materials-Inclusive Flash Spark Plasma Sintering.

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 phenomenon is enabled by the combination of the electric current concentration around the sample and the confinement of the heat generated in this area by the lateral thermal contact resistance. The presented new method allows: extending flash sintering to nearly all materials, controlling sample shape by an added graphite die, and an energy efficient mass production of small and intermediate size objects. This approach represents also a potential venue for future investigations of flash sintering of complex shapes.

Flash (Ultra-Rapid) Spark-Plasma Sintering of Silicon Carbide.

A new ultra-rapid process of flash spark plasma sintering is developed. The idea of flash spark plasma sintering (or flash hot pressing - FHP) stems from the conducted theoretical analysis of the role of thermal runaway phenomena for material processing by flash sintering. The major purpose of the present study is to theoretically analyze the thermal runaway nature of flash sintering and to experimentally address the challenge of uncontrollable thermal conditions by the stabilization of the flash sintering process through the application of the external pressure. The effectiveness of the developed FHP technique is demonstrated by the few seconds-long consolidation of SiC powder in an industrial spark plasma sintering device. Specially designed sacrificial dies heat the pre-compacted SiC powder specimens to a critical temperature before applying any voltage to the powder volume and allowing the electrode-punches of the SPS device setup to contact the specimens and pass electric current through them under elevated temperatures. The experimental results demonstrate that flash sintering phenomena can be realized using conventional SPS devices. The usage of hybrid heating SPS devices is pointed out as the mainstream direction for the future studies and utilization of the new flash hot pressing (ultra-rapid spark plasma sintering) technique.

The Manufacturing of High Porosity Iron with an Ultra-Fine Microstructure via Free Pressureless Spark Plasma Sintering.

High porosity (>40 vol %) iron specimens with micro- and nanoscale isotropic pores were fabricated by carrying out free pressureless spark plasma sintering (FPSPS) of submicron hollow Fe-N powders at 750 °C. Ultra-fine porous microstructures are obtained by imposing high heating rates during the preparation process. This specially designed approach not only avoids the extra procedures of adding and removing space holders during the formation of porous structures, but also triggers the continued phase transitions of the Fe-N system at relatively lower processing temperatures. The compressive strength and energy absorption characteristics of the FPSPS processed specimens are examined here to be correspondingly improved as a result of the refined microstructure.

Zirconium Carbide Produced by Spark Plasma Sintering and Hot Pressing: Densification Kinetics, Grain Growth, and Thermal Properties.

Spark plasma sintering (SPS) has been employed to consolidate a micron-sized zirconium carbide (ZrC) powder. ZrC pellets with a variety of relative densities are obtained under different processing parameters. The densification kinetics of ZrC powders subjected to conventional hot pressing and SPS are comparatively studied by applying similar heating and loading profiles. Due to the lack of electric current assistance, the conventional hot pressing appears to impose lower strain rate sensitivity and higher activation energy values than those which correspond to the SPS processing. A finite element simulation is used to analyze the temperature evolution within the volume of ZrC specimens subjected to SPS. The control mechanism for grain growth during the final SPS stage is studied via a recently modified model, in which the grain growth rate dependence on porosity is incorporated. The constant pressure specific heat and thermal conductivity of the SPS-processed ZrC are determined to be higher than those reported for the hot-pressed ZrC and the benefits of applying SPS are indicated accordingly.

Spark Plasma Sintering of Commercial Zirconium Carbide Powders: Densification Behavior and Mechanical Properties.

Commercial zirconium carbide (ZrC) powder is consolidated by Spark Plasma Sintering (SPS). Processing temperatures range from 1650 to 2100 °C. Specimens with various density levels are obtained when performing single-die SPS at different temperatures. Besides the single-die tooling setup, a double-die tooling setup is employed to largely increase the actual applied pressure to achieve higher densification in a shorter processing time. In order to describe the densification mechanism of ZrC powder under SPS conditions, a power-law creep constitutive equation is utilized, whose coefficients are determined by the inverse regression of the obtained experimental data. The densification of the selected ZrC powder is shown to be likely associated with grain boundary sliding and dislocation glide controlled creep. Transverse rupture strength and microhardness of sintered specimens are measured to be up to 380 MPa and 24 GPa, respectively. Mechanical properties are correlated with specimens' average grain size and relative density to elucidate the co-factor dependencies.

Microstructure Investigation of 13Cr-2Mo ODS Steel Components Obtained by High Voltage Electric Discharge Compaction Technique.

Refractory oxide dispersion strengthened 13Cr-2Mo steel powder was successfully consolidated to near theoretical density using high voltage electric discharge compaction. Cylindrical samples with relative density from 90% to 97% and dimensions of 10 mm in diameter and 10-15 mm in height were obtained. Consolidation conditions such as pressure and voltage were varied in some ranges to determine the optimal compaction regime. Three different concentrations of yttria were used to identify its effect on the properties of the samples. It is shown that the utilized ultra-rapid consolidation process in combination with high transmitted energy allows obtaining high density compacts, retaining the initial structure with minimal grain growth. The experimental results indicate some heterogeneity of the structure which may occur in the external layers of the tested samples due to various thermal and electromagnetic in-processing effects. The choice of the optimal parameters of the consolidation enables obtaining samples of acceptable quality.

Outside Mainstream Electronic Databases: Review of Studies Conducted in the USSR and Post-Soviet Countries on Electric Current-Assisted Consolidation of Powder Materials.

This paper reviews research articles published in the former USSR and post-soviet countries on the consolidation of powder materials using electric current that passes through the powder sample and/or a conductive die-punch set-up. Having been published in Russian, many of the reviewed papers are not included in the mainstream electronic databases of the scientific articles and thus are not known to the scientific community. The present review is aimed at filling this information gap. In the paper, the electric current-assisted sintering techniques based on high- and low-voltage approaches are presented. The main results of the theoretical modeling of the processes of electromagnetic field-assisted consolidation of powder materials are discussed. Sintering experiments and related equipment are described and the major experimental results are analyzed. Sintering conditions required to achieve the desired properties of the sintered materials are provided for selected material systems. Tooling materials used in the electric current-assisted consolidation set-ups are also described.

Localized Overheating Phenomena and Optimization of Spark-Plasma Sintering Tooling Design.

The present paper shows the application of a three-dimensional coupled electrical, thermal, mechanical finite element macro-scale modeling framework of Spark Plasma Sintering (SPS) to an actual problem of SPS tooling overheating, encountered during SPS experimentation. The overheating phenomenon is analyzed by varying the geometry of the tooling that exhibits the problem, namely by modeling various tooling configurations involving sequences of disk-shape spacers with step-wise increasing radii. The analysis is conducted by means of finite element simulations, intended to obtain temperature spatial distributions in the graphite press-forms, including punches, dies, and spacers; to identify the temperature peaks and their respective timing, and to propose a more suitable SPS tooling configuration with the avoidance of the overheating as a final aim. Electric currents-based Joule heating, heat transfer, mechanical conditions, and densification are imbedded in the model, utilizing the finite-element software COMSOL™, which possesses a distinguishing ability of coupling multiple physics. Thereby the implementation of a finite element method applicable to a broad range of SPS procedures is carried out, together with the more specific optimization of the SPS tooling design when dealing with excessive heating phenomena.