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A special issue of Ceramics (ISSN 2571-6131).

Deadline for manuscript submissions: closed (30 November 2020) | Viewed by 68135

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Special Issue Editors

Dr. Manuel Belmonte

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Guest Editor

Institute of Ceramics and Glass (ICV-CSIC) Campus Cantoblanco, c/Kelsen 5, 28049 Madrid, Spain
Interests: development of ceramic/carbon nanostructure (graphene or nanotube) composites; 3D printing of porous materials; densification by spark plasma sintering; tribological, mechanical, and thermal properties

Dr. Claude Estournes

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Guest Editor

CNRS Resarch Director at CIRIMAT, Université de Toulouse, CNRS, Université Toulouse 3 - Paul Sabatier, 118 Route de Narbonne, 31062 Toulouse, CEDEX 9, France
Interests: synthesis, preparation, and densification of materials (with nano and microscales, composite, multilayered system, ceramic, metal, polymer, glass etc.) by spark plasma sintering; development of novel, specific, and multifunctional architectures (FGM, micro- and mesoporous composite structure, sandwiches) to tailor specific properties; studies of densification mechanisms and finite element modeling; electrothermal, mechanical, and microstructural (ETMM) of the SPS process for the elaboration of parts with complex shapes
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Prof. Dr. Angel L. Ortiz

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Department of Mechanical, Energy and Materials Engineering, University of Extremadura, 06006 Badajoz, Spain
Interests: ceramics; ceramic composites; ceramic thin-films and coatings; processing and sintering; mechanical properties; tribology; X-ray diffraction theory and methods; microstructural characterization; severe plastic deformation
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Dr. Koji Morita

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National Institute for Materials Science Tsukuba, Tsukuba, Japan
Interests: structural ceramics; creep; superplasticity; sintering; spark-plasma-sintering (SPS); transparent ceramics

Special Issue Information

Dear Colleagues,

In recent decades, spark plasma sintering (SPS) and field-assisted sintering technology (FAST), which are both pressure-assisted pulsed direct current sintering processes belonging to electric current activated/assisted sintering (ECAS) techniques, have allowed hundreds of research laboratories and companies around the world to step forward to develop new materials with improved performance that could not have been manufactured using common sintering techniques. Among them, multifunctional nanomaterials with negligible grain growth and/or phase transformation at reduced temperatures, complex composites including novel fillers such as carbon nanotubes or graphene, or graded materials stand out. In addition, important efforts have been carried out to elucidate the mass transfer mechanisms occurring within the materials during the SPS process, also modeling the physical parameters that govern this sintering technique. Scaling up to manufacture larger specimens and tooling to produce dense complex parts has also been investigated.

This Special Issue is focused on novel research activities that closely combine the use of the SPS/FAST technique to produce new ceramic-based materials with improved properties (mechanical, electrical, thermal, tribological, etc.) for emerging applications. Theoretical studies and reviews will also be covered, and the Guest Editors encourage scientists investigating these topics to contribute to this Special Issue.

Dr. Manuel Belmonte
Dr. Claude Estournes
Prof. Dr. Angel L. Ortiz
Dr. Koji Morita

Guest Editors

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Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Ceramics is an international peer-reviewed open access quarterly journal published by MDPI.

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Keywords

Spark plasma sintering (SPS), HP-SPS, Flash-SPS
Field-assisted sintering technology (FAST)
Ceramics and nanoceramics
Ceramic composites and nanocomposites
Functionally-graded materials
Multimaterials
Mechanical/Tribological properties of SPSed ceramics
Functional properties of SPSed ceramics
Sintering mechanisms
Modeling

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Published Papers (13 papers)

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Research

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39 pages, 24639 KiB

Open AccessArticle

Progress of Spark Plasma Sintering (SPS) Method, Systems, Ceramics Applications and Industrialization

by Masao Tokita

Ceramics 2021, 4(2), 160-198; https://doi.org/10.3390/ceramics4020014 - 25 Apr 2021

Cited by 169 | Viewed by 14644

Abstract

The spark plasma sintering (SPS) method is of great interest to the powder and powder metallurgy industry and material researchers of academia for both product manufacturing and advanced material research and development. Today in Japan, a number of SPS products for different industries have already been realized. Today’s fifth-generation SPS systems are capable of producing parts of increasing size, offering improved functionality, reproducibility, productivity, and cost. For instance, pure nano-Tungsten Carbide WC powder (no additives) is fully densified with a nano-grain-sized structure for glass lens application in the optics industry. The SPS is now moving from scientific academia and/or R&D proto-type materials level usage to practical industry use product stage utilizing in the field of electronics, automotive, mold and die, cutting tools, fine ceramics, clean energy, biomaterials industries, and others. This paper reviews and introduces the peculiar phenomenon of SPS and the progress of SPS technology, method, development of SPS systems, and its industrial product applications. Full article

(This article belongs to the Special Issue Spark Plasma Sintering Technology)

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13 pages, 3822 KiB

Open AccessArticle

Ultrasonic Characterization of Nanoparticle-Based Ceramics Fabricated by Spark-Plasma Sintering

by Hanuš Seiner, Michaela Janovská, Martin Koller, Petr Sedlák, Kateřina Seinerová, Archana Loganathan and Arvind Agarwal

Ceramics 2021, 4(2), 135-147; https://doi.org/10.3390/ceramics4020012 - 29 Mar 2021

Viewed by 3236

Abstract

Resonant ultrasound spectroscopy was used to determine elastic constants and internal friction parameters of bulk nanoparticle-based ceramic materials compacted by spark plasma sintering. Boron nitride-based and boron carbon nitride-based materials were studied, and the results were compared with similar bulk materials prepared from graphene nanoplatelets. The results showed that such nanoparticle-based materials can be strongly anisotropic, and can have very different elastic constants depending on the nanoparticles used. From the temperature dependence of the internal friction parameters, the activation energy for sliding of the individual monolayers along each other was determined for each material. Very similar values of the activation energy were obtained for boron nitride, boron carbon nitride, and graphene, ranging from 15 to 17 kJ/mol. Full article

(This article belongs to the Special Issue Spark Plasma Sintering Technology)

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13 pages, 5972 KiB

Open AccessArticle

Fabrication and Characterization of Quinary High Entropy-Ultra-High Temperature Diborides

by Simone Barbarossa, Roberto Orrù, Valeria Cannillo, Antonio Iacomini, Sebastiano Garroni, Massimiliano Murgia and Giacomo Cao

Ceramics 2021, 4(2), 108-120; https://doi.org/10.3390/ceramics4020010 - 25 Mar 2021

Cited by 17 | Viewed by 3270

Abstract

Due to their inherent chemical complexity and their refractory nature, the obtainment of highly dense and single-phase high entropy (HE) diborides represents a very hard target to achieve. In this framework, homogeneous (Hf_0.2Nb_0.2Ta_0.2Mo_0.2Ti_0.2)B₂, (Hf_0.2Zr_0.2Ta_0.2Mo_0.2Ti_0.2)B₂, and (Hf_0.2Zr_0.2Nb_0.2Mo_0.2Ti_0.2)B₂ ceramics with high relative densities (97.4, 96.5, and 98.2%, respectively) were successfully produced by spark plasma sintering (SPS) using powders prepared by self-propagating high-temperature synthesis (SHS). Although the latter technique did not lead to the complete conversion of initial precursors into the prescribed HE phases, such a goal was fully reached after SPS (1950 °C/20 min/20 MPa). The three HE products showed similar and, in some cases, even better mechanical properties compared to ceramics with the same nominal composition attained using alternative processing methods. Superior Vickers hardness and elastic modulus values were found for the (Hf_0.2Nb_0.2Ta_0.2Mo_0.2Ti_0.2)B₂ and the (Hf_0.2Zr_0.2Ta_0.2Mo_0.2Ti_0.2)B₂ systems, i.e., 28.1 GPa/538.5 GPa and 28.08 GPa/498.1 GPa, respectively, in spite of the correspondingly higher residual porosities (1.2 and 2.2 vol.%, respectively). In contrast, the third ceramic, not containing tantalum, displayed lower values of these two properties (25.1 GPa/404.5 GPa). However, the corresponding fracture toughness (8.84 MPa m^1/2) was relatively higher. This fact can be likely ascribed to the smaller residual porosity (0.3 vol.%) of the sintered material. Full article

(This article belongs to the Special Issue Spark Plasma Sintering Technology)

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11 pages, 2252 KiB

Open AccessArticle

Overview of Spark Plasma Texturing of Functional Ceramics

by Jacques G. NOUDEM and Yiteng XING

Ceramics 2021, 4(1), 97-107; https://doi.org/10.3390/ceramics4010009 - 15 Mar 2021

Cited by 6 | Viewed by 3095

Abstract

This work reports the progress in the preparation of superconducting and thermoelectric lamellar compounds processed by the unconventional Spark Plasma Sintering (SPS). The SPS equipment was modified with the aim of obtaining the textured and dense superconductor Bi₂Sr₂Ca₂Cu₃O_10,p-type oxide thermoelectric bulk as Ca₃Co₄O₉ and Ca_3-xAg_xCo₄O₉/Ag composites respectively. The new process is referred to as Spark Plasma Texturing (SPT). During SPT, the bulk material can freely deform. As a result, inter-grain preferential crystallographic orientation is created. The series of sintered and textured samples using the same Ag content were processed respectively. From the results, we can evidence: (i) the magnetic and/or structural transition around 350 °C, for both series of samples. (ii) The electrical resistivity (ρ) decreases with increasing Ag-substituted or Ag-added. (iii) The Seebeck coefficient (S) of the textured series is higher than that of the sintered series. In the case of the Ag-substituted, S, decreases with Ag content. The optimized composite is found to be Ca_2.6Ag_0.4Co₄O₉/8wt% Ag. We can note the remarkable reduction of ρ, and the improvement of power factor values up to 360 μW.m⁻¹.K⁻².The superconducting properties of single phased Bi₂Sr₂Ca₂Cu₃O₁₀ (Bi2223) consolidated using SPS and SPT will also be discussed. Full article

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14 pages, 3682 KiB

Open AccessArticle

Effect of the Heating Rate on the Spark-Plasma-Sintering (SPS) of Transparent Y₂O₃ Ceramics: Microstructural Evolution, Mechanical and Optical Properties

by Lihong Liu, Koji Morita, Tohru S. Suzuki and Byung-Nam Kim

Ceramics 2021, 4(1), 56-69; https://doi.org/10.3390/ceramics4010006 - 17 Feb 2021

Cited by 7 | Viewed by 4035

Abstract

High strength transparent Y₂O₃ ceramics were fabricated from commercial powders using spark plasma sintering (SPS) technique by optimizing the heating rate. The heating rate significantly influenced the microstructures and the optical/mechanical properties of the Y₂O₃ ceramics. Grain growth was limited accordingly with increasing the heating rate. The ball milling process of the commercial Y₂O₃ powders is likely to further enhance the sinterability during the SPS processing. The dense Y₂O₃ ceramics, which were sintered by SPS with 100 °C/min, showed good transmittance range from visible to near infrared (IR). For a high heating rate of 100 °C/min, the in-line transmittance at a visible wavelength of 700 nm was 66%, whereas for a slow heating rate of 10 °C/min, it reduced to 46%. The hardness H_v tends to increase with increasing the heating rate and rigorously followed the Hall–Petch relationship; that is, it is enhanced with a reduction of the grain size. The toughness K_IC, on the other hand, is less sensitive to both the heating rate and the grain size, and takes a similar value. This research highlighted that the high heating rate SPS processing can fabricate fully dense fine-grained Y₂O₃ ceramics with the excellent optical and mechanical properties. Full article

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14 pages, 1190 KiB

Open AccessArticle

Micro/Nano Indentation Testing of Spark Plasma Sintered Al₂O₃ + ZrO₂ + cBN Ceramics

by Richard Sedlák, Michal Ivor, Piotr Klimczyk, Piotr Wyzga, Marcin Podsiadlo, Marek Vojtko and Ján Dusza

Ceramics 2021, 4(1), 40-53; https://doi.org/10.3390/ceramics4010004 - 22 Jan 2021

Cited by 6 | Viewed by 3198

Abstract

Al₂O₃ + 30 vol% ZrO₂ matrix composites with 20 and 30 vol% cBN have been prepared with the optimized processing route, using spark plasma sintering (SPS) at temperatures of 1400 °C and 1250 °C. The influence of cBN addition on the microstructure characteristics, micro/nanohardness, elastic modulus, and crack-extension resistance of the composites and their constitutions have been investigated using scanning electron microscopy (SEM), statistical analyses of the individual grain size and micro/nanoindentation methods. The matrix consists of alumina and zirconia grains with grain sizes/diameter of approximately 220 and 160 nm with approximately 1.9 μm cBN grains in the Al₂O₃ + ZrO₂ + cBN composites. The microhardness is slightly increasing with cBN addition from 16.2 to 17.1 GPa and the crack-extension resistance from 3.72 to 4.29 MPa.m^1/2. The toughening mechanisms are in the form of crack deflection, crack branching, and crack bridging. The nanohardness and indentation modulus of the matrix are approximately 30 and 420 GPa, and the cBN grains 70 and 777 GPa, respectively. Full article

(This article belongs to the Special Issue Spark Plasma Sintering Technology)

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8 pages, 5139 KiB

Open AccessArticle

In Situ Graded Ceramic/Reduced Graphene Oxide Composites Manufactured by Spark Plasma Sintering

by Cristina Ramírez, Pilar Miranzo, Maria Isabel Osendi and Manuel Belmonte

Ceramics 2021, 4(1), 12-19; https://doi.org/10.3390/ceramics4010002 - 29 Dec 2020

Cited by 2 | Viewed by 3024

Abstract

The present work merges two key strategies for the manufacturing of advanced ceramics, in particular, the development of functionally graded materials (FGMs) and the addition of graphene-based fillers into a ceramic matrix. A silicon nitride/reduced graphene oxide FGM composite is produced, in one step, from a single powder composition using the spark plasma sintering (SPS) technique with an asymmetric setting of the punches and die to create a continuous temperature gradient along the cross section of the powder compact. A deep microstructural and mechanical characterization has been done across the specimen thickness. The FGM composite exhibits bottom-top gradients in both the matrix grain size (150% increase) and α-phase content (89→1%). The FGM bottom surface is 10% harder than the top one and, on the other hand, the latter is 15% tougher. The presence of reduced graphene oxide sheets homogeneously distributed within the ceramic composite reduces the mechanical gradients compared to the monolithic silicon nitride FGM, although allows reaching a maximum long-crack toughness value of 9.4 MPa·m^1/2. In addition, these graphene-based fillers turn the insulating ceramics into an electrical conductor material. Full article

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12 pages, 2209 KiB

Open AccessArticle

Dense MgB₂ Ceramics by Ultrahigh Pressure Field-Assisted Sintering

by Mythili Prakasam, Felix Balima, Jacques Noudem and Alain Largeteau

Ceramics 2020, 3(4), 521-532; https://doi.org/10.3390/ceramics3040042 - 21 Dec 2020

Cited by 10 | Viewed by 3250

Abstract

Magnesium diboride (MgB₂) ceramics, due to their impressive transition temperature of 39 K for superconductivity, have been widely investigated. The possibility to obtain highly dense MgB₂ ceramics with fine microstructure and grain boundaries acting as pinning sites by novel high-pressure-assisted spark plasma sintering (HP-SPS) is reported in this article. HP-SPS was employed to reach 100% density in MgB₂ ceramics, and high pressure was utilized in the consolidation of MgB₂. An increase in pressure helped in stabilizing the MgB₂ phase above thermal decomposition, thus avoiding the formation of non-superconducting phases such as MgO and MgB₄. Pressure allowed strengthening of the covalent bond (condensation effect) to increase the thermal stability of MgB₂. HP-SPS yielded high mechanical hardness in MgB₂ (1488 HV). For better electrical connectivity, which leads to large magnetic moments in high density samples were obtained with the beneficial effect of high applied pressure (1.7–5 GPa) at high temperature (>1000 °C). The combination of the SPS process and high pressure ensured retention of the homogeneous fine microstructure required to obtain high current density and high hardness. Full article

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14 pages, 6663 KiB

Open AccessArticle

Effect of High Pressure Spark Plasma Sintering on the Densification of a Nb-Doped TiO₂ Nanopowder

by Alexandre Verchère, Sandrine Cottrino, Gilbert Fantozzi, Shashank Mishra, Thomas Gaudisson, Nicholas Blanchard, Stéphane Pailhès, Stéphane Daniele and Sylvie Le Floch

Ceramics 2020, 3(4), 507-520; https://doi.org/10.3390/ceramics3040041 - 4 Dec 2020

Cited by 7 | Viewed by 3255

Abstract

Sintering under pressure by means of the spark plasma sintering (SPS) technique is a common route to reduce the sintering temperature and to achieve ceramics with a fine-grained microstructure. In this work, high-density bulk TiO₂ was sintered by high pressure SPS. It is shown that by applying high pressure during the SPS process (76 to 400 MPa), densification and phase transition start at lower temperature and are accelerated. Thus, it is possible to dissociate the two densification steps (anatase then rutile) and the transition phase during the sintering cycle. Regardless of the applied pressure, grain growth occurs during the final stage of the sintering process. However, twinning of the grains induced by the phase transition is enhanced under high pressure resulting in a reduction in the crystallite size. Full article

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13 pages, 7446 KiB

Open AccessArticle

Effect of SiC on Microstructure, Phase Evolution, and Mechanical Properties of Spark-Plasma-Sintered High-Entropy Ceramic Composite

by Hanzhu Zhang and Farid Akhtar

Ceramics 2020, 3(3), 359-371; https://doi.org/10.3390/ceramics3030032 - 18 Sep 2020

Cited by 22 | Viewed by 4696

Abstract

Ultra-high temperature ceramic composites have been widely investigated due to their improved sinterability and superior mechanical properties compared to monolithic ceramics. In this work, high-entropy boron-carbide ceramic/SiC composites with different SiC content were synthesized from multicomponent carbides HfC, Mo₂C, TaC, TiC, B₄C, and SiC in spark plasma sintering (SPS) from 1600 °C to 2000 °C. It was found that the SiC addition tailors the phase formation and mechanical properties of the high-entropy ceramic (HEC) composites. The microhardness and fracture toughness of the HEC composites sintered at 2000 °C were improved from 20.3 GPa and 3.14 MPa·m^1/2 to 26.9 GPa and 5.95 MPa·m^1/2, with increasing SiC content from HEC-(SiC)0 (0 vol. %) to HEC-(SiC)3.0 (37 vol. %). The addition of SiC (37 vol. %) to the carbide precursors resulted in the formation of two high-entropy ceramic phases with two different crystal structures, face-centered cubic (FCC) structure, and hexagonal structure. The volume fraction ratio between the hexagonal and FCC high-entropy phases increased from 0.36 to 0.76 when SiC volume fraction was increased in the composites from HEC-(SiC)0 to HEC-(SiC)3.0, suggesting the stabilization of the hexagonal high-entropy phase over the FCC phase with SiC addition. Full article

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11 pages, 45578 KiB

Open AccessArticle

Manufacturing of Continuous Carbon Fiber Reinforced Aluminum by Spark Plasma Sintering

by Miguel Jiménez, Felix Ott, Frank Kern and Rainer Gadow

Ceramics 2020, 3(3), 265-275; https://doi.org/10.3390/ceramics3030024 - 30 Jun 2020

Cited by 1 | Viewed by 3517

Abstract

In the field of metal matrix composites (MMC), spark plasma sintering (SPS) technique has been used so far for the manufacture of particle, whisker and short-fiber reinforced alloys. In this work, SPS technique is employed for the first time to produce continuous fiber reinforced light metals. For this purpose, metal matrix composite prepregs with aluminum as a surface coating on carbon fiber textiles are manufactured by twin arc wire spraying and subsequently consolidated by SPS in the semi-solid temperature range of the alloy. Shear thinning rheological behavior of the metal alloy at temperatures between solidus and liquidus enables the infiltration of fiber rovings under reduced forming loads. SPS offered a better controlled and more efficient heat transfer in the green body and faster consolidation cycles in comparison with alternative densification methods. Fully densified samples with no porosity proved the suitability of SPS for densification of MMC with a remarkable stiffness increase in comparison with samples densified by thixoforging, an alternative consolidation method. However, the pulse activated sintering process leads to a quite strong fiber/matrix adhesion with evidence of aluminum carbide formation. Full article

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Review

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20 pages, 5426 KiB

Open AccessReview

Unconventional Materials Processing Using Spark Plasma Sintering

by Ambreen Nisar, Cheng Zhang, Benjamin Boesl and Arvind Agarwal

Ceramics 2021, 4(1), 20-39; https://doi.org/10.3390/ceramics4010003 - 8 Jan 2021

Cited by 26 | Viewed by 8861

Abstract

Spark plasma sintering (SPS) has gained recognition in the last 20 years for its rapid densification of hard-to-sinter conventional and advanced materials, including metals, ceramics, polymers, and composites. Herein, we describe the unconventional usages of the SPS technique developed in the field. The potential of various new modifications in the SPS technique, from pressureless to the integration of a novel gas quenching system to extrusion, has led to SPS’ evolution into a completely new manufacturing tool. The SPS technique’s modifications have broadened its usability from merely a densification tool to the fabrication of complex-shaped components, advanced functional materials, functionally gradient materials, interconnected materials, and porous filter materials for real-life applications. The broader application achieved by modification of the SPS technique can provide an alternative to conventional powder metallurgy methods as a scalable manufacturing process. The future challenges and opportunities in this emerging research field have also been identified and presented. Full article

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18 pages, 4201 KiB

Open AccessReview

Spark Plasma Sintering of Ceramics: From Modeling to Practice

by Michael Stuer, Paul Bowen and Zhe Zhao

Ceramics 2020, 3(4), 476-493; https://doi.org/10.3390/ceramics3040039 - 17 Nov 2020

Cited by 16 | Viewed by 6556

Abstract

Summarizing the work of nearly a decade of research on spark plasma sintering (SPS), a review is given on the specificities and key factors to be considered in SPS of ceramic materials, based on the authors’ own research. Alumina is used primarily as a model material throughout the review. Intrinsic inhomogeneities linked to SPS and operational parameters, which depend on the generation of atomistic scale defects, are discussed in detail to explain regularly observed inhomogeneities reported in literature. Adopting an engineering approach to overcome these inherent issues, a successful processing path is laid out towards the mastering of SPS in a wide range of research and industrial settings. Full article

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