Ceramic Processing and Sintering

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

Deadline for manuscript submissions: closed (15 November 2022) | Viewed by 55990

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Laboratory of Composite Ceramic Materials, A. A. Baikov Institute of Metallurgy and Materials Science (IMET), Russian Academy of Sciences, 119334 Moscow, Russia
Interests: synthesis; nanoparticles; bioceramic; calcium phosphates; magnesium phosphates; additive manufacturing; zirconia; alumina
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Department of Mechanical Engineering, San Diego State University, San Diego, CA 92182, USA
Interests: advanced processing of powder materials; field assisted sintering; sintering-assisted additive manufacturing; numerical and experimental methods in materials science
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

This Special Issue is dedicated to recent advances in ceramic processing and sintering. Ceramic materials are characterized by unique properties and applied in infinite aspects of human life, from dentistry to aerospace production. The development of the design, composition, synthesis, formation, and sintering of functional ceramics and the investigation of the processing–structure–property relationship open broad opportunities for creating new and improved materials. Potential topics in this Special Issue include, but are not limited to, modern approaches of obtaining powders; product formation, including additive manufacturing methods and ceramic injection molding technology; heat treatment, including hot isostatic pressing; and spark plasma sintering and post-processing operations. Studies incorporating innovative technology approaches of all ceramic types are welcome, including original articles, communications, and reviews.

Dr. Margarita A. Goldberg
Dr. Elisa Torresani
Guest Editors

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Keywords

  • powder preparation
  • novel forming technologies
  • additive manufacturing
  • ceramic injection molding
  • sintering additives
  • hot isostatic pressing
  • spark plasma sintering
  • pulse electric current sintering
  • post-processing
  • thermal stability
  • phase transformation
  • phase equilibrium
  • microstructure
  • processing–structure–property relationships
  • phsyical–chemical properties
  • mechanical properties
  • biomedical properties
  • characterization techniques

Published Papers (23 papers)

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21 pages, 13391 KiB  
Article
Spark Plasma Sintering of Ceramics Based on Solid Solutions of Na1+2xZr2−xCox(PO4)3 Phosphates: Thermal Expansion and Mechanical Properties Research
by A. A. Aleksandrov, A. I. Orlova, D. O. Savinykh, M. S. Boldin, S. A. Khainakov, A. A. Murashov, A. A. Popov, G. V. Shcherbak, S. Garcia-Granda, A. V. Nokhrin, V. N. Chuvil’deev and N. Yu. Tabachkova
Ceramics 2023, 6(1), 278-298; https://doi.org/10.3390/ceramics6010017 - 16 Jan 2023
Viewed by 2006
Abstract
The structure, microstructure, coefficient of thermal expansion (CTE), and mechanical properties of Na1+2xZr2−xCox(PO4)3 ceramics (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) were studied. Na1+2xZr2−xCox(PO4)3 [...] Read more.
The structure, microstructure, coefficient of thermal expansion (CTE), and mechanical properties of Na1+2xZr2−xCox(PO4)3 ceramics (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) were studied. Na1+2xZr2−xCox(PO4)3 submicron powders with the NaZr2(PO4)3 structure (NZP, kosnarite type) were obtained by the solid-phase method. The starting reagents (NaNO3, ZrOCl2·8H2O, NH4H2PO4, CoCl2·6H2O, ethanol) were mixed with the addition of ethyl alcohol. The resulting mixtures were annealed at 600 °C (20 h) and 700 °C (20 h). The obtained phosphates crystallized in the expected structure of the NaZr2(PO4)3 type (trigonal system, space group R3¯c). Thermal expansion of the powders was studied with high-temperature X-ray diffraction at temperatures ranging from 25 to 700 °C. CTEs were calculated, and their dependence on the cobalt content was analyzed. Na1+2xZr2−xCox(PO4)3 ceramics with high relative density (93.67–99.70%) were obtained by Spark Plasma Sintering (SPS). Ceramics poor in cobalt (x = 0.1) were found to have a high relative density (98.87%) and a uniform fine-grained microstructure with a grain size of 0.5–1 µm. Bigger cobalt content leads to a smaller relative density of ceramics. During the sintering of ceramics with high cobalt content, anomalous grain growth was observed. The powder compaction rate was shown to be determined by creep and diffusion intensity in the Na1+2xZr2−xCox(PO4)3 crystal lattice. SPS activation energy in ceramics increased as the cobalt content grew. The microhardness and fracture toughness of ceramics did not depend on their cobalt content. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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16 pages, 7653 KiB  
Article
Structure, Mechanical and Luminescent Properties of Solid Solution (Y0.96Eu0.01Sm0.01Tb0.01Er0.01)Nb0.7Ta0.3O4
by Mikhail Palatnikov, Olga Shcherbina, Maxim Smirnov, Sofja Masloboeva and Vadim Efremov
Ceramics 2023, 6(1), 86-101; https://doi.org/10.3390/ceramics6010007 - 09 Jan 2023
Viewed by 1541
Abstract
Ceramic samples of polycomponent solid solution (Y0.96Eu0.01Sm0.01Tb0.01Er0.01)Nb0.7Ta0.3O4 have been prepared by sol–gel synthesis from fine powders obtained using nitrate solutions of rare earth elements REE and coprecipitated hydroxides [...] Read more.
Ceramic samples of polycomponent solid solution (Y0.96Eu0.01Sm0.01Tb0.01Er0.01)Nb0.7Ta0.3O4 have been prepared by sol–gel synthesis from fine powders obtained using nitrate solutions of rare earth elements REE and coprecipitated hydroxides of niobium and tantalum. The structural state of the initial powders’ crystal lattice has been investigated. The morphological features of the microstructure of the ceramics samples have been studied in dependence of temperature regimes of their preparation. The ceramics’ strength characteristics (Young’s modulus) and the critical stress intensity factor of the mode I KIC have been estimated. Cathode- and photoluminescent properties of ceramic solid solutions (Y0.96Eu0.01Sm0.01Tb0.01Er0.01)Nb0.7Ta0.3O4 have been studied. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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17 pages, 4707 KiB  
Article
Microporous Ceramics Based on β-Tricalcium Phosphate
by Tatiana Safronova, Grigorii Grigorev, Tatiana Shatalova, Ilya Roslyakov, Vadim Platonov and Dinara Khayrutdinova
Ceramics 2022, 5(4), 1269-1285; https://doi.org/10.3390/ceramics5040090 - 12 Dec 2022
Viewed by 1633
Abstract
Microporous ceramic material, based on β-tricalcium phosphate β-Ca3(PO4)2 with grain size 2–5 μm, pore size smaller than 10 mm, and density 1.22 g/cm3 corresponding to ~40% of the theoretical density (3.07 g/cm3) of β-Ca3 [...] Read more.
Microporous ceramic material, based on β-tricalcium phosphate β-Ca3(PO4)2 with grain size 2–5 μm, pore size smaller than 10 mm, and density 1.22 g/cm3 corresponding to ~40% of the theoretical density (3.07 g/cm3) of β-Ca3(PO4)2, was obtained from a powder mixture with a given molar ratio Ca/P = 1.5 after firing at 1100 °C. A homogenized powder mixture of synthetic dicalcium hydrogen phosphates with the molar ratio Ca/P = 1 and calcium citrate tetrahydrate Ca3(C6H5O7)2·4H2O with the molar ratio Ca/P = ∞ was used for microporous ceramic preparation. The phase composition of calcium phosphate powder, synthesized from an aqueous solution of phosphoric acid H3PO4 and calcium carbonate CaCO3 powder, included brushite CaHPO4·2H2O as the predominant phase. Formation of β-tricalcium phosphate β-Ca3(PO4)2 during firing occurred due to the heterophase interaction of the products of thermal decomposition of the components of the starting powder mixture, namely, calcium pyrophosphate Ca2P2O7 and calcium oxide CaO. The formation of arch-like structures from β-tricalcium phosphate β-Ca3(PO4)2 grains, which were tightly sintered together, hindered the shrinkage of ceramics. The microporous ceramics obtained, based on β-tricalcium phosphate β-Ca3(PO4)2, can be recommended as a biocompatible and biodegradable material for treatment of bone defects and as a substrate for bone-cell cultivation. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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14 pages, 4810 KiB  
Article
Spark Plasma Sintering of Variable SiC α/β Ratio with Boron and Carbon Additions—Microstructure Transformation
by Marek Kostecki, Mateusz Petrus, Tomasz Płociński and Andrzej Roman Olszyna
Ceramics 2022, 5(4), 1255-1268; https://doi.org/10.3390/ceramics5040089 - 10 Dec 2022
Viewed by 1500
Abstract
This study investigated the possibility of obtaining dense silicon carbide sinters with the use of a spark plasma sintering (SPS) process by changing the composition of SiC α/β polymorphs in a starting powder mixture. Amorphous boron was used as the basic additive to [...] Read more.
This study investigated the possibility of obtaining dense silicon carbide sinters with the use of a spark plasma sintering (SPS) process by changing the composition of SiC α/β polymorphs in a starting powder mixture. Amorphous boron was used as the basic additive to activate the sintering processes. Some of the compositions were prepared with additional carbon in two different forms: multilayer graphene flakes and carbon black. The well-described effect of the β–α transition in the form of elongated lamellar grains in the sintered structure was confirmed. The obtained sinters were analyzed qualitatively and quantitatively in terms of the microstructure and density. The hardness and the participation of the polytypes in the sinter structures were examined. During the study, SPS sintering allowed us to obtain a material with a density close to the theoretical (relative density of 99.5% and hardness of 27 MPa) without the addition of carbon. It was found that the role of carbon was not limited to the activation of the sintering process. Additional effects accompanying its presence, depending on the initial α/β composition, included grain size reduction and an influence on the transformation kinetics. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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13 pages, 1590 KiB  
Article
Study of Tricalcium Phosphate Ceramics Doped with Gadolinium Ions with Various EPR Techniques
by Margarita A. Sadovnikova, Fadis F. Murzakhanov, Inna V. Fadeeva, Anna A. Forysenkova, Dina V. Deyneko, Georgy V. Mamin and Marat R. Gafurov
Ceramics 2022, 5(4), 1154-1166; https://doi.org/10.3390/ceramics5040081 - 01 Dec 2022
Cited by 3 | Viewed by 1766
Abstract
Tricalcium phosphate (TCP)-based materials, such as β-Ca3(PO4)2 doped with rare earth ions (RE), have shown applications as biomaterials, lighting emitting materials, scintillating materials, in vivo imaging probes, and thermoluminescent dosimeters. Their properties are found to be dependent on [...] Read more.
Tricalcium phosphate (TCP)-based materials, such as β-Ca3(PO4)2 doped with rare earth ions (RE), have shown applications as biomaterials, lighting emitting materials, scintillating materials, in vivo imaging probes, and thermoluminescent dosimeters. Their properties are found to be dependent on the distribution of RE3+ on Ca2+ sites that can be controlled by pulsed electron paramagnetic resonance (EPR) and electron spin echo envelop modulation (ESEEM) experiments. The main spectroscopic parameters (spin Hamiltonian values) of Gd3+ and nitrogen impurity centers are quantitatively determined (g-factor, the fine structure parameters D and E, the hyperfine constants A) as well as dynamic characteristics: spin–lattice T1 and spin–spin T2 relaxation times. Based on the analysis of the EPR datasets, the interatomic distance between Gd3+ and 31P was estimated in the dipole–dipole approximation. Two structurally nonequivalent Gd3+ positions in the β-TCP structure have been identified. The obtained valuable results demonstrate applicability of modern EPR techniques to characterize Gd-TCP systems despite the powder structure of the material and high electron spin S = 7/2 of Gd3+ ions. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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10 pages, 3329 KiB  
Article
A Rapid Sintering Method for Cerium Nitride Pellet: A Uranium Mononitride Surrogate
by Logan Joyce and Yi Xie
Ceramics 2022, 5(4), 1009-1018; https://doi.org/10.3390/ceramics5040072 - 18 Nov 2022
Cited by 1 | Viewed by 1980
Abstract
Uranium mononitride (UN) is a candidate fuel material for light water reactors with higher uranium (U) loading and thermal conductivity than uranium dioxide (UO2). However, the sintering of UN pellets is challenging as the UN powder particles oxidize rapidly at high [...] Read more.
Uranium mononitride (UN) is a candidate fuel material for light water reactors with higher uranium (U) loading and thermal conductivity than uranium dioxide (UO2). However, the sintering of UN pellets is challenging as the UN powder particles oxidize rapidly at high temperatures unless the oxygen concentration is extremely low. Oxidation during sintering either reduces the relative density of the sintered UN pellet or disintegrates the sintered UN pellet to powder. To address this problem, the present work developed a rapid sintering method for producing highly densified UN surrogate pellets with minimal oxidation. Cerium nitride (CeN) is used as a surrogate for UN to reduce radiation hazards. With the custom-developed fast-heating system, the sintering process was completed within 150 s. The sintering atmosphere was flowing nitrogen (N2). The sintered CeN pellet density was 95% of the theoretical density (TD) or higher. The microstructure was uniform with a 10–25 µm grain size as demonstrated by scanning electron microscopy (SEM) and contained trivial levels of oxides as demonstrated by X-ray diffraction (XRD). The resultant pellets indicate that the rapid sintering method is a promising method to make UN fuel pellets with equivalent or higher density to pellets made by conventional sintering methods, while also being more efficient in time and costs. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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16 pages, 2955 KiB  
Article
Microstructural Characteristics of 3Y-TZP Ceramics and Their Effects on the Flexural Strength
by Manuel Fellipe Rodrigues Pais Alves, Leonardo Queiroz Bueno de Campos, Bruno Galvão Simba, Cosme Roberto Moreira da Silva, Kurt Strecker and Claudinei dos Santos
Ceramics 2022, 5(4), 798-813; https://doi.org/10.3390/ceramics5040058 - 17 Oct 2022
Cited by 10 | Viewed by 2087
Abstract
This work evaluates the effects of grain growth and tetragonality of the t-ZrO2 phase on the mechanical properties of 3Y-TZP ceramics. Samples were sintered at 1475 °C for 2 h, and at 1600 °C for 2, 12, or 24 h. After sintering, [...] Read more.
This work evaluates the effects of grain growth and tetragonality of the t-ZrO2 phase on the mechanical properties of 3Y-TZP ceramics. Samples were sintered at 1475 °C for 2 h, and at 1600 °C for 2, 12, or 24 h. After sintering, the tetragonal ZrO2 polytypes t and t′ were observed under all sintering conditions, while a residual content of monoclinic ZrO2 was detected in samples sintered at 1600 °C for 24 h. The average grain size was found to vary from 0.65 ± 0.10 to 2.20 ± 0.35 μm. Moreover, zirconia ceramics sintered at 1475 °C for 2 h exhibit higher flexural strength (1210 ± 85 MPa), while samples sintered at 1600 °C for 24 h exhibit the lowest flexural strength (910 ± 90 MPa). These results were related to the progressive formation of Y3+-rich grains (t′-ZrO2) due to the grain boundary segregation-induced phase (GBSIPT) mechanism. Due to the high stabilizer concentration in the solid solution, these grains present lower tetragonality, being highly stable at room temperature. Consequently, the observed strength reduction of samples sintered at 1600 °C for 24 h is related to the presence of the t′-ZrO2 phase, which is less prompt to the phase transformation toughening process, limiting shielding zones’ effectiveness at the crack tip. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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12 pages, 2873 KiB  
Article
Composite Ceramics in the Na2O–CaO–SiO2–P2O5 System Obtained from Pastes including Hydroxyapatite and an Aqueous Solution of Sodium Silicate
by Maksim Kaimonov, Tatiana Safronova, Tatiana Shatalova, Yaroslav Filippov, Irina Tikhomirova and Nikollay Sergeev
Ceramics 2022, 5(3), 550-561; https://doi.org/10.3390/ceramics5030041 - 05 Sep 2022
Cited by 7 | Viewed by 2103
Abstract
The new approach to obtaining ceramic materials in the Na2O–CaO–SiO2–P2O5 system based on the binder—an aqueous solution of sodium silicate and filler—hydroxyapatite was shown in current research. After heat treatment at 500 °C and 700 °C, [...] Read more.
The new approach to obtaining ceramic materials in the Na2O–CaO–SiO2–P2O5 system based on the binder—an aqueous solution of sodium silicate and filler—hydroxyapatite was shown in current research. After heat treatment at 500 °C and 700 °C, the ceramic samples included non-reacted hydroxyapatite Ca10(PO4)6(OH)2, β-rhenanite β-NaCaPO4 and sodium calcium silicophosphate Na2Ca4(PO4)2SiO4. An increase in temperature to 900 °C and 1100 °C allowed to obtain ceramic materials with the following phases: devitrite Na2Ca3Si6O16, β-rhenanite β-NaCaPO4, β-wollastonite β-CaSiO3, and silicon dioxide SiO2. The strength of ceramic samples rose with increasing temperature from ≈7.0 MPa (bending) and ≈7.2 MPa (compression) at 500 °C to ≈9.5 MPa (bending) and ≈31.6 MPa (compression) at 1100 °C. At the same time, the apparent density decreased from 1.71 g/cm3 to 1.15 g/cm3. The top of the compressive strength equal to 31.6 MPa was observed when the apparent density was 1.15 g/cm3. Obtained ceramics consisted of biocompatible phases, widely studied in the literature; thus, it confirms the possibility of using an aqueous solution of sodium silicate in medical materials science. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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17 pages, 6632 KiB  
Article
Biocompatibility of Ceramic Materials in Ca2P2O7–Ca(PO3)2 System Obtained via Heat Treatment of Cement-Salt Stone
by Otabek Toshev, Tatiana Safronova, Maksim Kaimonov, Tatiana Shatalova, Elena Klimashina, Yulia Lukina, Konstantin Malyutin and Sergey Sivkov
Ceramics 2022, 5(3), 516-532; https://doi.org/10.3390/ceramics5030039 - 27 Aug 2022
Cited by 6 | Viewed by 2187
Abstract
Biocompatibility of ceramic materials in Ca2P2O7-Ca(PO3)2 system was investigated using different methods, including in vitro and in vivo tests. Ceramic materials in the Ca2P2O7-Ca(PO3)2 system [...] Read more.
Biocompatibility of ceramic materials in Ca2P2O7-Ca(PO3)2 system was investigated using different methods, including in vitro and in vivo tests. Ceramic materials in the Ca2P2O7-Ca(PO3)2 system were obtained by annealing cement-salt stone based on powder mixtures of calcium citrate tet-rahydrate Ca3(C6H5O7)2·4H2O and monocalcium phosphate monohydrate (MCPM) Ca(H2PO4)2·H2O. The phase composition of cement-salt stone included brushite, monetite as a result of chemical reaction of starting components after adding of water. The presence of citric acid as by-product of chemical reaction, leads to increase the setting time of the cement-salt stone. Highly concentrated aqueous suspensions based on calcium citrate and MCPM powders providing content of calcium polyphosphate Ca(PO3)2 up to 20 wt % in ceramics were used for designing bioresorbable materials. The presence of an excess of monocalcium phosphate monohydrate makes it possible to reduce the annealing temperature of ceramics, which is associated with the formation of a lower melting phase of Ca(PO3)2. In vivo tests shown that obtained ceramic materials can be recommended for regenerative treatments for bone defects. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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15 pages, 8608 KiB  
Article
Inorganic Powders Prepared from Fish Scales
by Tatiana Safronova, Viktor Vorobyov, Natalia Kildeeva, Tatiana Shatalova, Otabek Toshev, Yaroslav Filippov, Artem Dmitrienko, Olga Gavlina, Olga Chernega, Elena Nizhnikova, Marat Akhmedov, Elena Kukueva and Konstantin Lyssenko
Ceramics 2022, 5(3), 484-498; https://doi.org/10.3390/ceramics5030037 - 26 Aug 2022
Cited by 3 | Viewed by 5240
Abstract
A mixture of abramis brama (freshwater bream), carassius carassius (crucian carp), and sander lucioperca (pike perch) scales was used for the preparation of fish scale powder containing constituents of organic and inorganic nature. The mixture of the mentioned fish scales was washed, dried, [...] Read more.
A mixture of abramis brama (freshwater bream), carassius carassius (crucian carp), and sander lucioperca (pike perch) scales was used for the preparation of fish scale powder containing constituents of organic and inorganic nature. The mixture of the mentioned fish scales was washed, dried, and ground for the preparation of fish scale powder. Vibration sieving was used to prepare fish scale powder enriched with inorganic components. According to thermal analysis data, this fish scale powder enriched with inorganic components included about 36.5 wt.% components removed when heating, primarily those of organic nature, and 63.5 wt.% mineral components. Inorganic powders consisting of hydroxyapatite and magnesium whitlockite were obtained via heat treatment of this fish scale powder at 800–1000 °C. Particles of these inorganic powders consisted of sintered grains with dimensions less than 100 nm after heat treatment at 800 °C, less than 200 nm after heat treatment at 900 °C, and 100–1000 nm after heat treatment at 1000 °C. Fish scale powder enriched with inorganic components as well as heat-treated inorganic powders consisting of hydroxyapatite and magnesium whitlockite can be recommended for the production of different materials, such as ceramics or composites. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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12 pages, 3103 KiB  
Article
Powders Based on Ca2P2O7-CaCO3-H2O System as Model Objects for the Development of Bioceramics
by Kristina Peranidze, Tatiana V. Safronova, Yaroslav Filippov, Gilyana Kazakova, Tatiana Shatalova and Julietta V. Rau
Ceramics 2022, 5(3), 423-434; https://doi.org/10.3390/ceramics5030032 - 13 Aug 2022
Cited by 3 | Viewed by 2049
Abstract
Nanoscale powders of hydrated Ca2P2O7, CaCO3, and a product of mixed-anionic composition containing P2O74− and CO32− anions were synthesized from aqueous solutions of Ca(CH3COO)2, pyrophosphoric [...] Read more.
Nanoscale powders of hydrated Ca2P2O7, CaCO3, and a product of mixed-anionic composition containing P2O74− and CO32− anions were synthesized from aqueous solutions of Ca(CH3COO)2, pyrophosphoric acid (H4P2O7), and/or (NH4)2CO3. Pyrophosphoric acid was previously obtained on the basis of the ion exchange process from Na4P2O7 solution and H+-cationite resin for further introduction into the reactions as an anionic precursor. The phase composition of powders after the syntheses was represented by bioresorbable phases of X-ray amorphous hydrated Ca2P2O7 phase, calcite and vaterite polymorphs of CaCO3. Based on synthesized powders, simple cylindrical constructions were prepared via mechanical pressing and fired in the temperature range of 600–800 °C. Surface morphology observation showed the presence of bimodal porosity with pore sizes up to 200 nm and 2 μm, which is likely to ensure tight particle packing and roughness of the sample surface required for the differentiation of osteogenic cells. Thus, the prepared ceramic samples can be further examined as model objects for bone tissue repair. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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15 pages, 5949 KiB  
Article
Oxidation Resistance of γ-TiAl Based Alloys Modified by C, Si and Y2O3 Microdopants
by Pavel A. Loginov, Georgy M. Markov, Nataliya V. Shvyndina, Gleb V. Smirnov and Evgeny A. Levashov
Ceramics 2022, 5(3), 389-403; https://doi.org/10.3390/ceramics5030030 - 02 Aug 2022
Cited by 1 | Viewed by 1724
Abstract
This work aimed to study the oxidation resistance of γ-TiAl based alloy, doped with small concentrations of carbon, silicon, and yttrium oxide in air at 800 and 1100 °C for 30 h. The TNM-B1 alloy samples were produced via high-energy ball milling, self-propagating [...] Read more.
This work aimed to study the oxidation resistance of γ-TiAl based alloy, doped with small concentrations of carbon, silicon, and yttrium oxide in air at 800 and 1100 °C for 30 h. The TNM-B1 alloy samples were produced via high-energy ball milling, self-propagating high-temperature synthesis, and hot isostatic pressing techniques. The microstructure, oxidation kinetics at 800–1100 °C, scale structure, and oxidation mechanism were studied. The oxidation of alloys modified with carbon and silicon at 1100 °C was characterized by the formation of a three-layer coating. The Y2O3 modified alloy performed the greatest oxidation resistance at 1100 °C and promoted the formation of a dense Al2O3 interlayer. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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17 pages, 8195 KiB  
Article
Ti/Cu/Kovar Multilayer Interlayer PTLP Diffusion Bonding Si3N4/Ht250
by Deku Zhang, Lian Zhang, Ning Zhou, Kehong Wang and Xiaopeng Li
Ceramics 2022, 5(3), 372-388; https://doi.org/10.3390/ceramics5030029 - 31 Jul 2022
Viewed by 1866
Abstract
In this paper, partial transient liquid phase (PTLP) diffusion bonding between Si3N4 ceramics and Ht250 cast iron was carried out by using an Ti/Cu/Kovar/Cu/Ti interlayer. The effects of the heating temperature and holding time on the microstructure, formation mechanism, and [...] Read more.
In this paper, partial transient liquid phase (PTLP) diffusion bonding between Si3N4 ceramics and Ht250 cast iron was carried out by using an Ti/Cu/Kovar/Cu/Ti interlayer. The effects of the heating temperature and holding time on the microstructure, formation mechanism, and mechanical properties of Si3N4/Ht250 cast iron joints were studied. The results show that the maximum shear strength of the joint is 112 MPa when the welding temperature is 1000 °C and the holding time is 1 h. In addition, the problems of Ti/Cu/Ti intermetallic compound formation and Cu/Si3N4 ceramic residual thermal stress in the joint can be effectively alleviated. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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10 pages, 4174 KiB  
Article
Synthesis and Thermal Behaviour of Calcium Alkyl Phosphates as Bioceramic Precursors
by Andrey Tikhonov and Valery Putlayev
Ceramics 2022, 5(3), 362-371; https://doi.org/10.3390/ceramics5030028 - 29 Jul 2022
Cited by 1 | Viewed by 1483
Abstract
Powders of alkyl phosphoric acids and calcium alkyl phosphates with various alkyl chains (butyl, octyl, and dodecyl) have been synthesized. The resulting powders were characterized by X-ray phase analysis, electron microscopy, and thermal analysis. It was shown that the calcium alkyl phosphates correspond [...] Read more.
Powders of alkyl phosphoric acids and calcium alkyl phosphates with various alkyl chains (butyl, octyl, and dodecyl) have been synthesized. The resulting powders were characterized by X-ray phase analysis, electron microscopy, and thermal analysis. It was shown that the calcium alkyl phosphates correspond to the composition of acid salts of calcium alkyl phosphates Ca(RPO4H)2, data on which are not presented in the literature. The thermal behaviour of calcium alkyl phosphates can be described as a complex phase transformation into biphasic calcium phosphate mixture (of Ca2P2O7 and Ca3(PO4)2) with the increase of the Ca to P ratio in comparison to initial materials. The powders thermally treated in the range of 400–600 °C could be recommended as single precursors of biphasic bioceramics. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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11 pages, 2425 KiB  
Article
Photonic Sintering of Oxide Ceramic Films: Effect of Colored FexOy Nanoparticle Pigments
by Evgeniia Gilshtein, Stefan Pfeiffer, Severin Siegrist, Vitor Vlnieska, Thomas Graule and Yaroslav E. Romanyuk
Ceramics 2022, 5(3), 351-361; https://doi.org/10.3390/ceramics5030027 - 28 Jul 2022
Cited by 2 | Viewed by 2812
Abstract
Alumina and zirconia thin films modified with colored nano-FexOy pigments were sintered by the flash-lamp-annealing method. We selected a nano α-Al2O3 and micron α-Al2O3 bimodal mixture as the base precursor material, and we doped [...] Read more.
Alumina and zirconia thin films modified with colored nano-FexOy pigments were sintered by the flash-lamp-annealing method. We selected a nano α-Al2O3 and micron α-Al2O3 bimodal mixture as the base precursor material, and we doped it with 5 vol% of FexOy red/brown/black/yellow pigments. The coatings were deposited from nanoparticle dispersions both on glass and on flexible metal foil. The characteristics of the thin films obtained with the use of various additives were compared, including the surface morphologies, optical properties, crystallinities, and structures. Flash lamp annealing was applied with the maximum total energy density of 130 J/cm2 and an overall annealing time of 7 s. Based on the simulated temperature profiles and electron-microscopy results, a maximum annealing temperature of 1850 °C was reached for the red Al2O3: Fe2O3 ceramic film. The results show that red α-Fe2O3 pigments allow for the achievement of maximum layer absorption, which is effective for flash lamp sintering. It was also possible to use the selected red α-Fe2O3 particles for the flash-lamp-assisted sintering of ZrO2 on a 30 µm-thin flexible stainless-steel substrate. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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21 pages, 8693 KiB  
Article
Chemically Bound Resorbable Ceramics as an Antibiotic Delivery System in the Treatment of Purulent–Septic Inflammation of Bone Tissue
by Yuliya Lukina, Yuriy Panov, Ludmila Panova, Aleksandr Senyagin, Leonid Bionyshev-Abramov, Natalya Serejnikova, Aleksey Kireynov, Sergey Sivkov, Nikolay Gavryushenko, Dmitriiy Smolentsev, Otabek Toshev, Dmitriy Lemenovsky and Dmitriy Krutko
Ceramics 2022, 5(3), 330-350; https://doi.org/10.3390/ceramics5030026 - 27 Jul 2022
Cited by 2 | Viewed by 1775
Abstract
Local drug delivery systems are an effective approach in the treatment of purulent–septic inflammation of bone tissue. Chemically bonded multiphase ceramics based on calcium-deficient carbonate-substituted hydroxyapatite combine resorbability, osteoconductivity, and the possibility of volumetric incorporation of antibiotics. Macroporosity is regulated by the concentration [...] Read more.
Local drug delivery systems are an effective approach in the treatment of purulent–septic inflammation of bone tissue. Chemically bonded multiphase ceramics based on calcium-deficient carbonate-substituted hydroxyapatite combine resorbability, osteoconductivity, and the possibility of volumetric incorporation of antibiotics. Macroporosity is regulated by the concentration of polyethylene glycol granules introduced into the initial powder composition, followed by their extraction. The selected conditions for the consolidation of the ceramic matrix and the extraction of PEG granules retain the activity of vancomycin, which is confirmed by the results of microbiological studies. The concentration of vancomycin and the porosity affect the local concentration and release of the antibiotic. The incorporation method provides a prolonged release of the antibiotic for up to 31 days. In vivo experiments with bone implantation have shown that chemically bound macroporous ceramics with incorporated vancomycin are a therapeutically effective carrier of the substance during the healing of bone defects in conditions of surrounding purulent–septic inflammation, and can be considered as a carrier for local antibacterial therapy, at the site of implantation. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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12 pages, 2777 KiB  
Article
Incorporation of Manganese (II) in Beta-Tricalcium Phosphate from EPR and ENDOR Measurements for Powders
by Fadis F. Murzakhanov, Anna A. Forysenkova, Inna V. Fadeeva, Georgy V. Mamin and Marat R. Gafurov
Ceramics 2022, 5(3), 318-329; https://doi.org/10.3390/ceramics5030025 - 26 Jul 2022
Cited by 1 | Viewed by 1814
Abstract
Powders of β-tricalcium phosphate (β-TCP, Ca3PO4) doped with manganese (Mn2+) are comprehensively analyzed with electron paramagnetic resonance (EPR) and electron-nuclear double resonance (ENDOR) techniques. The modeling of the spectra permitted to calculate the values of zero-field splitting [...] Read more.
Powders of β-tricalcium phosphate (β-TCP, Ca3PO4) doped with manganese (Mn2+) are comprehensively analyzed with electron paramagnetic resonance (EPR) and electron-nuclear double resonance (ENDOR) techniques. The modeling of the spectra permitted to calculate the values of zero-field splitting (B20 = −904 MHz; B40 = −1.41 MHz and B43 = 195.2 MHz) and explain the origin of the low-field hyperfine structures as the allowed spin transitions of fine structure. Three structurally inequivalent positions for Mn2+ in the β-TCP crystal lattice are identified and their g-factors and hyperfine constants are quantified. The obtained results can serve as fundamental background to the study of structurally disordered matrices with high spin (S ≥ 1) impurities which are important for catalytic systems. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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13 pages, 5626 KiB  
Article
FIB and Wedge Polishing Sample Preparation for TEM Analysis of Sol-Gel Derived Perovskite Thin Films
by Jorge Sanz-Mateo, Marco Deluca, Bernhard Sartory, Federica Benes and Daniel Kiener
Ceramics 2022, 5(3), 288-300; https://doi.org/10.3390/ceramics5030023 - 20 Jul 2022
Cited by 1 | Viewed by 3129
Abstract
In ceramic thin films, choosing an appropriate sample preparation method for transmission electron microscopy (TEM) analyses is of paramount importance to avoid preparation-induced damage and retain nanoscale features that require investigation. Here we compare two methods of TEM thin film sample preparation, namely [...] Read more.
In ceramic thin films, choosing an appropriate sample preparation method for transmission electron microscopy (TEM) analyses is of paramount importance to avoid preparation-induced damage and retain nanoscale features that require investigation. Here we compare two methods of TEM thin film sample preparation, namely conventional wedge polishing and focused ion beam (FIB) based lift out preparation applied to ferroelectric barium titanate (BaTiO3, BT) thin films made by chemical solution deposition (CSD). The aim of the work is to determine the pros and cons of each method considering not only the quality of the TEM specimen, but also aspects such as availability, ease of use, and affordability. Besides some limitations on the selection of visualized area due to thickness constraints on the FIB-made sample, both methods offer the capability to prepare samples with very comparable quality, as indicated by achieving the same thickness, a largely agreeing microstructure, no secondary phases on the diffraction pattern, and good atomic resolution. This last observation is especially important in the current context of material science, where more nanoscale phenomena are becoming the subject of study. The wedge polishing method, however, is deemed more affordable in terms of instrumentation, as it only requires a tripod polisher, a polishing wheel, and a precision ion polishing system, whereas the lift out method requires a scanning electron microscope (SEM) equipped with an FIB system. We believe that this work serves groups working on ferroelectric thin films in preparing TEM samples in a more effective and uncomplicated manner, facilitating progress in understanding this fascinating class of materials. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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12 pages, 5951 KiB  
Article
Investigation of Targeted Process Control for Adjusting the Macrostructure of Freeze Foams Using In Situ Computed Tomography
by Johanna Maier, Vinzenz Geske, David Werner, Thomas Behnisch, Matthias Ahlhelm, Tassilo Moritz, Alexander Michaelis and Maik Gude
Ceramics 2022, 5(3), 269-280; https://doi.org/10.3390/ceramics5030021 - 07 Jul 2022
Cited by 2 | Viewed by 1716
Abstract
Freeze foams are novel and innovative cellular structures that are based on a direct foaming process and that can be manufactured using any material that can be processed by powder technology. The foam formation process is characterized by the highly complex interaction of [...] Read more.
Freeze foams are novel and innovative cellular structures that are based on a direct foaming process and that can be manufactured using any material that can be processed by powder technology. The foam formation process is characterized by the highly complex interaction of various process and material parameters that were chosen empirically and that have so far been difficult to reproduce. To allow properties to be specifically tailored towards certain applications, it is necessary to examine the phenomena observed during foam formation as well as the impact of the process and material parameters on the structural constitution to deduce guidelines for manufacturing and quality assessment (e.g., mechanical strength, cell and pore sizes, pore size distribution). The variety of possible applications are a result of the wide spectrum of initial suspensions and especially the foam structure properties derived from process parameters such as the cell geometry, pore size distribution, fraction of open and closed porosity, and the textures of the cell struts. Due to earlier findings, the focus of this paper focuses on adjusting and tailoring the macrostructure (homogenization of the pore sizes and their distribution inside foam cells) to create load- and application-adapted ceramic foams. To this end, an experiment was designed using previously identified pore and characteristic influencers (air and water content, temperature of the suspension, pressure reduction rate) as influencing parameters. Their interconnected impacts on selected target values were examined during the freeze foaming process using an in situ freeze foaming device inside an X-ray. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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12 pages, 2853 KiB  
Article
Powder Mixture for the Production of Microporous Ceramics Based on Hydroxyapatite
by Tatiana Safronova, Stepan Chichulin, Tatiana Shatalova and Yaroslav Filippov
Ceramics 2022, 5(1), 108-119; https://doi.org/10.3390/ceramics5010010 - 18 Feb 2022
Cited by 2 | Viewed by 3345
Abstract
Powder mixtures with a given molar ratio of Ca/P = 1.67 were prepared under mechanical activation conditions from hydroxyapatite powder Ca10(PO4)6(OH)2 and a 1M aqueous solution of oxalic acid H2C2O4 at [...] Read more.
Powder mixtures with a given molar ratio of Ca/P = 1.67 were prepared under mechanical activation conditions from hydroxyapatite powder Ca10(PO4)6(OH)2 and a 1M aqueous solution of oxalic acid H2C2O4 at a molar ratio of Ca10(PO4)6(OH)2/H2C2O4 = 1:4. The phase composition of obtained powder mixture included brushite (calcium hydrophosphate dihydrate) CaHPO4·2H2O, calcium oxalate monohydrate CaC2O4·H2O in form of whewellite and weddellite, and some quantity of quasi-amorphous phase. This powder mixture was used to produce microporous monophase ceramics based on hydroxyapatite Ca10(PO4)6(OH)2 with apparent density of 1.25 g/cm3 after firing at 1200 °C. Microporosity of sintered ceramics was formed due to the presence of particles with plate-like morphology, restraining shrinkage during sintering. Microporous ceramics based on hydroxyapatite Ca10(PO4)6(OH)2 with the roughness of the surface as a consequence of the created microporosity can be recommended as a biocompatible material for bone defects treatment and as a substrate for bone cell cultivation. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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20 pages, 8554 KiB  
Article
Sinterability, Mechanical Properties and Wear Behavior of Ti3SiC2 and Cr2AlC MAX Phases
by Eduardo Tabares, Michael Kitzmantel, Erich Neubauer, Antonia Jimenez-Morales and Sophia A. Tsipas
Ceramics 2022, 5(1), 55-74; https://doi.org/10.3390/ceramics5010006 - 31 Jan 2022
Cited by 7 | Viewed by 2940
Abstract
MAX phases are a promising family of materials for several demanding, high-temperature applications and severe conditions. Their combination of metallic and ceramic properties makes MAX phases great candidates to be applied in energy production processes, such as high temperature heat exchangers for catalytic [...] Read more.
MAX phases are a promising family of materials for several demanding, high-temperature applications and severe conditions. Their combination of metallic and ceramic properties makes MAX phases great candidates to be applied in energy production processes, such as high temperature heat exchangers for catalytic devices. For their successful application, however, the effect of the processing method on properties such as wear and mechanical behavior needs to be further established. In this work, the mechanical and wear properties of self-synthesized Ti3SiC2 and Cr2AlC MAX phase powders consolidated by different powder metallurgy routes are evaluated. Uniaxial pressing and sintering, cold isostatic pressing and sintering and hot pressing were explored as processing routes, and samples were characterized by analyzing microstructure, phase constitution and porosity. Wear behavior was studied by reciprocating-sliding tests, evaluating the wear rate by the loss of material and the wear mechanism. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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24 pages, 6750 KiB  
Article
Synthesis and Characterization of Novel Calcium-Silicate Nanobioceramics with Magnesium: Effect of Heat Treatment on Biological, Physical and Chemical Properties
by Konstantina Kazeli, Ioannis Tsamesidis, Anna Theocharidou, Lamprini Malletzidou, Jonathan Rhoades, Georgia K. Pouroutzidou, Eleni Likotrafiti, Konstantinos Chrissafis, Theodoros Lialiaris, Lambrini Papadopoulou, Eleana Kontonasaki and Evgenia Lymperaki
Ceramics 2021, 4(4), 628-651; https://doi.org/10.3390/ceramics4040045 - 27 Nov 2021
Cited by 6 | Viewed by 4086
Abstract
Glass-ceramic nanopowder with a composition of 55SiO2-35CaO-10MgO (mol %) was synthesized by the sol–gel method and was heat treated at three temperatures (T1 = 835 °C, T2 = 1000 °C, T3 = 1100 °C) in order to obtain different materials (C1, [...] Read more.
Glass-ceramic nanopowder with a composition of 55SiO2-35CaO-10MgO (mol %) was synthesized by the sol–gel method and was heat treated at three temperatures (T1 = 835 °C, T2 = 1000 °C, T3 = 1100 °C) in order to obtain different materials (C1, C2, C3, respectively) varying in crystal structure. Bioactivity and oxidative stress were evaluated in simulated body fluid (SBF) for various time periods (up to 10 days). The structure of the synthesized materials and their apatite-forming ability were investigated by X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy and Energy Dispersive Spectroscopy (SEM/EDS). The antibacterial properties of the synthesized materials were evaluated against three Gram-positive and four Gram-negative bacterial strains and their biocompatibility was verified on a primary cell line of human gingival fibroblasts (HGFs) by the MTT (3-[4, 5-dimethylthiazol-2-yl]-2, 5 diphenyl tetrazolium bromide) assay. The crystallization of the materials was increased by sintering temperature. Heat treatment did not inhibit the bioactive behavior of the materials as apatite formation started after 3 days in SBF. C2, C3 showed some indications of apatite forming even from the first day. Regarding cell viability, a variety of biological behaviors, concerning both dose and time points, was observed between the positive control and the tested materials by both the MTT assay and oxidative stress analysis. In conclusion, the nanobioceramic materials of this study possess a multitude of attractive physicochemical and biological properties that make them suitable candidates for bone regeneration applications, fillers in nanocomposite scaffolds, or as grafts in bone cavities and periodontal lesions. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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8 pages, 2135 KiB  
Perspective
Synthesis of Ceramic Reinforcements in Metallic Matrices during Spark Plasma Sintering: Consideration of Reactant/Matrix Mutual Chemistry
by Dina V. Dudina, Tomila M. Vidyuk and Michail A. Korchagin
Ceramics 2021, 4(4), 592-599; https://doi.org/10.3390/ceramics4040042 - 22 Oct 2021
Cited by 3 | Viewed by 2319
Abstract
Metal–ceramic composites are obtained via ex-situ or in-situ routes. The in-situ route implies the synthesis of reinforcement in the presence of a matrix and is often regarded as providing more flexibility to the microstructure design of composites than the ex-situ route. Spark plasma [...] Read more.
Metal–ceramic composites are obtained via ex-situ or in-situ routes. The in-situ route implies the synthesis of reinforcement in the presence of a matrix and is often regarded as providing more flexibility to the microstructure design of composites than the ex-situ route. Spark plasma sintering (SPS) is an advanced sintering method that allows fast consolidation of various powder materials up to full or nearly full density. In reactive SPS, the synthesis and consolidation are combined in a single processing step, which corresponds to the in-situ route. In this article, we discuss the peculiarities of synthesis of ceramic reinforcements in metallic matrices during SPS with a particular consideration of reactant/matrix mutual chemistry. The formation of carbide reinforcements in Cu, Al, and Ni matrices is given attention with examples elaborated in the authors’ own research. Factors determining the suitability of reactive SPS for manufacturing of composites from a matrix/reactants system and features of the structural evolution of the reaction mixture during sintering are discussed. Full article
(This article belongs to the Special Issue Ceramic Processing and Sintering)
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