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Ceramics
Volume 5
Issue 3
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Ceramics, Volume 5, Issue 3 (September 2022) – 26 articles

Cover Story (view full-size image): The exposure of ceramic films to a high-temperature environment limits the substrate choice. We are proposing a photonic sintering (flash lamp annealing—FLA) method to sinter ceramic films on substrates with softening points much lower than those of ceramic materials. We are solving the main obstacle to the FLA of ceramic films—low light absorption in the visible range—by adding colored pigments to the precursor alumina or zirconia. To investigate the most effective pigment for sintering we admixed 5 vol% of red (α-Fe2O3), brown ((Fe,Mn)2O3), yellow (α-FeOOH), and black (Fe3O4) pigments to the alumina slurry. The highest absorption has an alumina layer colored by red α-Fe2O3 nanoparticles. A thin alumina film on glass and a zirconia coating on flexible metal foil were obtained by FLA in 7 seconds. View this paper
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13 pages, 2772 KiB  
Article
Electrical Conductivity of Thin Film SrTi0.8Fe0.2O3−δ-Supported Sr0.98Zr0.95Y0.05O3−δ Electrolyte
by Adelya Khaliullina, Aleksander Pankratov and Liliya Dunyushkina
Ceramics 2022, 5(3), 601-613; https://doi.org/10.3390/ceramics5030045 - 17 Sep 2022
Viewed by 2354
Abstract
Thin films of Sr0.98Zr0.95Y0.05O3−δ (SZY) electrolyte were grown on porous supporting SrTi0.8Fe0.2O3−δ electrodes by the chemical solution deposition method from a low-viscous solution of inorganic salts. The films were characterized by [...] Read more.
Thin films of Sr0.98Zr0.95Y0.05O3−δ (SZY) electrolyte were grown on porous supporting SrTi0.8Fe0.2O3−δ electrodes by the chemical solution deposition method from a low-viscous solution of inorganic salts. The films were characterized by X-ray diffraction and scanning electron microscopy. The gas-tightness of the films was evaluated using the differential-pressure method. The across-plane electrical conductivity of 1 mm thick SZY film was measured by impedance spectroscopy and compared to that of a massive ceramic sample. The revealed difference in electrical properties of the film and massive SZY samples indicates that diffusional interaction between the film and the substrate influences the performance of the supported electrolyte. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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8 pages, 1283 KiB  
Article
Modelling the Mechanical Properties of Hydroxyapatite Scaffolds Produced by Digital Light Processing-Based Vat Photopolymerization
by Francesco Baino, Martin Schwentenwein and Enrica Verné
Ceramics 2022, 5(3), 593-600; https://doi.org/10.3390/ceramics5030044 - 16 Sep 2022
Cited by 8 | Viewed by 2697
Abstract
Porosity is a key feature in dictating the overall performance of biomedical scaffolds, with special relevance to mechanical properties. Usually, compressive strength and elastic modulus are the main parameters used to determine the potential mechanical suitability of porous scaffolds for bone repair. However, [...] Read more.
Porosity is a key feature in dictating the overall performance of biomedical scaffolds, with special relevance to mechanical properties. Usually, compressive strength and elastic modulus are the main parameters used to determine the potential mechanical suitability of porous scaffolds for bone repair. However, their assessment may not be so easy from an experimental viewpoint and, especially if the porosity is high, so reliable for brittle bioceramic foams. Hence, assessing the relationship between porosity and mechanical properties based only on the constitutive parameters of the solid material is a challenging and important task to predict the scaffold performance for optimization during design. In this work, a set of equations was used to predict the compressive strength and elastic modulus of bone-like hydroxyapatite scaffolds produced by digital light processing-based vat photopolymerization (total porosity about 80 vol.%). The compressive strength was found to depend on total porosity, following a power-law approximation. The relationship between porosity and elastic modulus was well fitted by second-order power law, with relative density and computational models obtained by numerical simulations. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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18 pages, 4290 KiB  
Article
Sol–Gel Synthesis of Iron-Doped Sepiolite as a Novel Humidity-Sensing Material
by Ahmed Sabry Afify, Mehran Dadkhah and Jean-Marc Tulliani
Ceramics 2022, 5(3), 575-592; https://doi.org/10.3390/ceramics5030043 - 15 Sep 2022
Cited by 4 | Viewed by 1848
Abstract
Nowadays, humidity sensors are attracting a great deal of attention, and there are many studies focusing on enhancing their performances. Nevertheless, their fabrication through facile methods at reasonable cost is a significant factor. In this article, a new magnesium silicate nanopowder was successfully [...] Read more.
Nowadays, humidity sensors are attracting a great deal of attention, and there are many studies focusing on enhancing their performances. Nevertheless, their fabrication through facile methods at reasonable cost is a significant factor. In this article, a new magnesium silicate nanopowder was successfully synthesized using a simple and low-cost sol–gel method. Subsequently, modified sepiolite was achieved by the substitution of iron ions in the synthesized nanopowders. The specimens were then characterized by X-ray diffraction, field emission–scanning electron microscopy, X-ray photoelectron spectroscopy, thermogravimetric–differential thermal analysis, infrared spectroscopy, and nitrogen adsorption. Furthermore, humidity sensors were manufactured by screen printing the prepared powders on alumina substrates with interdigitated Pt electrodes. The results showed that the fabricated sensors with modified sepiolite exhibited interesting characteristics for humidity detection. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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13 pages, 35314 KiB  
Article
Fabrication of Complex Three-Dimensional Structures of Mica through Digital Light Processing-Based Additive Manufacturing
by Sinuo Zhang, Imam Akbar Sutejo, Jeehwan Kim, Yeong-Jin Choi, Chang Woo Gal and Hui-suk Yun
Ceramics 2022, 5(3), 562-574; https://doi.org/10.3390/ceramics5030042 - 8 Sep 2022
Cited by 7 | Viewed by 2945
Abstract
Mica is a group of clay minerals that are frequently used to fabricate electrical and thermal insulators and as adsorbents for the treatment of cationic pollutants. However, conventional subtractive manufacturing has the drawback of poor three-dimensional (3D) shape control, which limits its application. [...] Read more.
Mica is a group of clay minerals that are frequently used to fabricate electrical and thermal insulators and as adsorbents for the treatment of cationic pollutants. However, conventional subtractive manufacturing has the drawback of poor three-dimensional (3D) shape control, which limits its application. In this study, we propose digital light processing (DLP)-based additive manufacturing (AM) as one of the most effective ways to address this drawback. Two major challenges for the ceramic DLP process are the production of a homogeneous and stable slurry with the required rheological properties and the maintenance of printing precision. The mica green body was fabricated using a 53 vol.% solid loading slurry through DLP, which exhibited good dimensional resolution under an exposure energy dose of 10 mJ/cm2. The precise, complex 3D structure was maintained without any defects after debinding and sintering at 1000 °C. The use of ceramic AM to overcome the shape-control limitations of mica demonstrated in this study offers great potential for expanding the applications of mica. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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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 - 5 Sep 2022
Cited by 7 | Viewed by 2704
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, 3809 KiB  
Article
Influence of Porosity on R-Curve Behaviour of Tetragonal Stabilized Zirconia
by Dino N. Boccaccini, Vanesa Gil, Jonas Gurauskis, Rosa I. Merino, Andrea Pellacani, Cecilia Mortalò, Stefano Soprani, Marcello Romagnoli and Maria Cannio
Ceramics 2022, 5(3), 533-549; https://doi.org/10.3390/ceramics5030040 - 5 Sep 2022
Viewed by 2140
Abstract
Y2O3 at 3% mol partially stabilized Zr2O3 (3YSZ) porous specimens with variable open porosity, from fully dense up to ~47%, and their potential use as anode supports for new solid oxide cell designs were fabricated by tape [...] Read more.
Y2O3 at 3% mol partially stabilized Zr2O3 (3YSZ) porous specimens with variable open porosity, from fully dense up to ~47%, and their potential use as anode supports for new solid oxide cell designs were fabricated by tape casting. The stiffness, strength and fracture properties were measured to investigate the influence of porosity on mechanical properties. The evolution of Young’s modulus and characteristic strength was evaluated by ball-on-ring tests. The variation of critical plane stress Mode I stress intensity factor with porosity has also been investigated and modelled from the results obtained from fracture mechanics testing. R-curve behaviour was observed in dense 3YSZ specimens and in porous 3YSZ compositions. The width of the transformation zone after fracture mechanics testing and the variation with porosity were investigated. The phases existing in the fracture zone were determined and quantified by Raman spectroscopy. It was found that the width of the transformation zone increased with increasing porosity. A new general R-curve model for 3YSZ based on the McMeeking–Evans equation is presented, which can be used to predict the behaviour of the R-curve as a function of porosity, simply by knowing the properties of the dense material and introducing in this equation porosity-dependent laws on the key properties that affect fracture toughness. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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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 8 | Viewed by 2721
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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17 pages, 3383 KiB  
Article
Synthesis and Optical Characteristics of Gd0.96Eu0.01Sm0.01Tb0.01Er0.01Nb0.9Ta0.1O4 Ceramic Solid Solutions Prepared under Different Temperature Conditions
by Mikhail Palatnikov, Olga Shcherbina, Maxim Smirnov, Sofja Masloboeva, Vadim Efremov and Konstantin Andryushin
Ceramics 2022, 5(3), 499-515; https://doi.org/10.3390/ceramics5030038 - 26 Aug 2022
Cited by 1 | Viewed by 1862
Abstract
Fine powders of mixed gadolinium tantalum niobates doped with Eu, Sm, Tb, and Er were synthesized. Ceramic samples of polycomponent solid solutions of Gd0.96Eu0.01Sm0.01Tb0.01Er0.01Nb0.9Ta0.1O4 were obtained from synthesized [...] Read more.
Fine powders of mixed gadolinium tantalum niobates doped with Eu, Sm, Tb, and Er were synthesized. Ceramic samples of polycomponent solid solutions of Gd0.96Eu0.01Sm0.01Tb0.01Er0.01Nb0.9Ta0.1O4 were obtained from synthesized powders using conventional sintering technology. The phase composition and phase structure characteristics of the Gd0.96Eu0.01Sm0.01Tb0.01Er0.01Nb0.9Ta0.1O4 ceramic phases were determined by XRD. The effect of ceramic sintering temperature on the physical characteristics of Gd0.96Eu0.01Sm0.01Tb0.01Er0.01Nb0.9Ta0.1O4 solid solutions is shown. The morphological features of the microstructure of the Gd0.96Eu0.01Sm0.01Tb0.01Er0.01Nb0.9Ta0.1O4 ceramics were studied in relation to its mechanical characteristics. At the same time, the strength characteristics (Young’s modulus, microhardness) and the critical stress intensity factor for mode I KIC were evaluated for the first time for the synthesized compounds. Photoluminescence and cathodoluminescence were studied in the visible region. The study confirms the potential application of Gd0.96Eu0.01Sm0.01Tb0.01Er0.01Nb0.9Ta0.1O4 ceramic solid solutions as scintillators and radioluminescent light sources. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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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 4 | Viewed by 6612
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, 3570 KiB  
Article
Manufacturing and Thermal Shock Characterization of Porous Yttria Stabilized Zirconia for Hydrogen Energy Systems
by M. Faisal Riyad, Mohammadreza Mahmoudi and Majid Minary-Jolandan
Ceramics 2022, 5(3), 472-483; https://doi.org/10.3390/ceramics5030036 - 22 Aug 2022
Cited by 6 | Viewed by 3404
Abstract
Porous yttriastabilized zirconia (YSZ), in a composite with NiO, is widely used as a cermet electrode in solid oxide fuel cells (SOFCs) and solid oxide electrolysis cells (SOECs). Given cycles of high temperature in these energy devices, mechanical integrity of the porous YSZ [...] Read more.
Porous yttriastabilized zirconia (YSZ), in a composite with NiO, is widely used as a cermet electrode in solid oxide fuel cells (SOFCs) and solid oxide electrolysis cells (SOECs). Given cycles of high temperature in these energy devices, mechanical integrity of the porous YSZ is critical. Pore morphology, as well as properties of the ceramic, ultimately affect the mechanical properties of the cermet electrode. Here, we fabricated porous YSZ sheets via freezing of an aqueous slurry on a cold thermoelectric plate and quantified their flexural properties, both for as-fabricated samples and samples subjected to thermal shock at 200 °C to 500 °C. Results of this work have implications for the hydrogen economy and global decarbonization efforts, in particular for the manufacturing of SOFCs and SOECs. Full article
(This article belongs to the Special Issue Ceramics for Decarbonization of the Global Industry)
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13 pages, 3355 KiB  
Article
Effects of the Processing Technology of CVD-ZnSe, Cr2+:ZnSe, and Fe2+:ZnSe Polycrystalline Optical Elements on the Damage Threshold Induced by a Repetitively Pulsed Laser at 2.1 µm
by Nikolay Yudin, Oleg Antipov, Stanislav Balabanov, Ilya Eranov, Yuri Getmanovskiy and Elena Slyunko
Ceramics 2022, 5(3), 459-471; https://doi.org/10.3390/ceramics5030035 - 20 Aug 2022
Cited by 7 | Viewed by 2552
Abstract
Polycrystalline zinc selenide (ZnSe) and Cr2+ or Fe2+ doped ZnSe are key optical elements in mid-infrared laser systems. The laser-induced damage of the optical elements is the limiting factor for increasing the power and pulse energy of the lasers. In the [...] Read more.
Polycrystalline zinc selenide (ZnSe) and Cr2+ or Fe2+ doped ZnSe are key optical elements in mid-infrared laser systems. The laser-induced damage of the optical elements is the limiting factor for increasing the power and pulse energy of the lasers. In the present work, the optical damage of the ZnSe, Cr2+:ZnSe, and Fe2+:ZnSe samples induced by a repetitively pulsed Ho3+:YAG laser at 2091 nm was studied. The probability of the optical damage and the laser-induced damage threshold (LIDT) were determined for the samples manufactured using different processing techniques. The highest LIDT was found in ZnSe samples annealed in an argon atmosphere. It was also found that the samples annealed in a zinc atmosphere or with hot isostatic pressing resulted in a decrease in the LIDT. The Cr2+-doped ZnSe had the lowest LIDT at 2.1 µm compared to Fe2+-doped or undoped ZnSe. The LIDT fluence of all tested ZnSe samples decreased with the increase in the pulse repetition rate and the exposure duration. The results obtained may be used to improve the treatment procedures of ZnSe, Cr2+:ZnSe, and Fe2+:ZnSe polycrystals to further increase their LIDT. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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12 pages, 1681 KiB  
Article
Study of Radiation Damage Processes Caused by Hydrogen Embrittlement in Lithium Ceramics under High-Temperature Irradiation
by Dmitriy I. Shlimas, Artem L. Kozlovskiy, Maxim V. Zdorovets and Ainagul A. Khametova
Ceramics 2022, 5(3), 447-458; https://doi.org/10.3390/ceramics5030034 - 17 Aug 2022
Cited by 1 | Viewed by 1968
Abstract
The aim of this work is to study the hydrogenation processes in lithium-containing ceramics under high-temperature irradiation. Irradiation was carried out with protons with an energy of 1 MeV and fluences of 1015–1017 ion/cm2 at irradiation temperatures of 300–1000 [...] Read more.
The aim of this work is to study the hydrogenation processes in lithium-containing ceramics under high-temperature irradiation. Irradiation was carried out with protons with an energy of 1 MeV and fluences of 1015–1017 ion/cm2 at irradiation temperatures of 300–1000 K. The choice of irradiation conditions is due to the possibility of simulation of the radiation damage accumulation processes in the near-surface layer of Li2TiO3 ceramics, as well as establishing the dependences of changes in structural parameters during temperature heating of samples during irradiation. It has been established that at irradiation fluences of 1015–1016 ion/cm2, the formation of dislocation defects is observed, the density of which has a pronounced dependence on the irradiation temperature. At irradiation fluence above 5 × 1016 ion/cm2, an increase in the crystal structure deformation is observed, due to swelling processes as a result of implanted hydrogen accumulation in the near-surface layer structure. At the same time, an increase in the irradiation temperature leads to a decrease in the swelling value, which is due to the accelerated migration of implanted hydrogen in the near-surface layer and its release through the existing pores. Results of mechanical tests showed that the swelling of the crystal structure and its deformation leads to embrittlement and a partial decrease in the strength of the near-surface layer. The obtained research results will further allow us to evaluate the resistance of lithium ceramics to the processes of hydrogenation and destruction as a result of the formation of gas-filled cavities in the structure of the near-surface layer. Full article
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12 pages, 1698 KiB  
Article
Kinetics of the Synthesis of Aluminum Boride by the Self-Propagating High-Temperature Synthesis Method
by Sestager Khusainovich Aknazarov, Alibek Zhumabekovich Mutushev, Juan Maria Gonzalez-Leal, Olga Stepanovna Bairakova, Olga Yuryevna Golovchenko, Natalia Yuryevna Golovchenko and Elena Alexandrovna Ponomareva
Ceramics 2022, 5(3), 435-446; https://doi.org/10.3390/ceramics5030033 - 15 Aug 2022
Cited by 4 | Viewed by 2090
Abstract
The influence of certain factors on the kinetics of the process of obtaining aluminum borides (burning rate, ingot formation, and phase separation) was investigated. In this study, we report the registration of diboride using the SHS protocol. The synthesis of aluminum diboride from [...] Read more.
The influence of certain factors on the kinetics of the process of obtaining aluminum borides (burning rate, ingot formation, and phase separation) was investigated. In this study, we report the registration of diboride using the SHS protocol. The synthesis of aluminum diboride from boric anhydride occurred by the aluminothermic method. The initial components were boron trioxide and aluminum in the form of powders. Researchers paid special attention to the degree of grinding of the charge fluxing substances. The influence this had on the rate of development of the degree of charge concentration was studied. To calculate the degree of charge, a composition was chosen according to the speed obtained from a number of experiments where melting was carried out with the following charge densities in g/cm3: 0.80; 1.08; 1.18; 1.74. The method of melting was ignition from above. The experimental results allowed us to conclude that the nature of the change in the combustion rate of the system, where there was an excess of the reducing agent in the charge, is the same. An increase in the combustion rate, where there was an excess of aluminum of up to 20%, was likely due to the fact that the reaction area of the charge components increased. In addition, an increase in speed can be explained by a decrease in heat losses due to a reduction in the melting time. With an increase in excess aluminum above 20% of the stoichiometry, the observed decrease in the combustion rate can be explained by a decrease in the specific heat of the process due to the melting of the excess aluminum, which played the role of a ballast. Full article
(This article belongs to the Special Issue Geopolymers and Ceramics)
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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 5 | Viewed by 2677
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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19 pages, 8347 KiB  
Article
Possibilities of Mechanochemical Synthesis of Apatites with Different Ca/P Ratios
by Marina V. Chaikina, Natalia V. Bulina, Olga B. Vinokurova, Konstantin B. Gerasimov, Igor Yu. Prosanov, Nikolay B. Kompankov, Olga B. Lapina, Evgeniy S. Papulovskiy, Arcady V. Ishchenko and Svetlana V. Makarova
Ceramics 2022, 5(3), 404-422; https://doi.org/10.3390/ceramics5030031 - 3 Aug 2022
Cited by 21 | Viewed by 2820
Abstract
Apatite is widely used in medicine as a biomaterial for bone tissue restoration. Properties of apatite depend on its composition, including the Ca/P ratio. This paper shows what range of Ca/P ratio can be attained in apatite by the mechanochemical method of synthesis, [...] Read more.
Apatite is widely used in medicine as a biomaterial for bone tissue restoration. Properties of apatite depend on its composition, including the Ca/P ratio. This paper shows what range of Ca/P ratio can be attained in apatite by the mechanochemical method of synthesis, providing fast formation of a single-phase product. The synthesis was carried out from a reaction mixture of CaHPO4 and CaO at different Ca/P ratios in the range of 1.17–2.10. The products were studied by PXRD, FTIR and NMR spectroscopy, HRTEM, and STA. In mixtures with a low initial Ca/P ratio (1.17–1.48), directly in the mill, the formation of calcium orthophosphate with whitlockite structure containing an HPO42− group and structural water is shown for the first time. This phosphate has structure similar to that of whitlockites of hydrothermal origin and differs from high-temperature β-tricalcium phosphate that has composition Ca3(PO4)3. A series of samples of apatite was obtained with varied composition, which depends on the initial Ca/P ratio. At Ca/P < 1.67, the formation of two types of calcium-deficient apatite was documented. At Ca/P > 1.67, the existence of two types of calcium-rich apatite is confirmed. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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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 - 2 Aug 2022
Cited by 1 | Viewed by 2231
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
Cited by 1 | Viewed by 2358
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 1911
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 3582
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 3 | Viewed by 2193
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 2222
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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17 pages, 4352 KiB  
Article
Calcium Silicate Hydrate Cation-Exchanger from Paper Recycling Ash and Waste Container Glass
by Andrew P. Hurt, Aimee A. Coleman, Haosen Ma, Qiu Li and Nichola J. Coleman
Ceramics 2022, 5(3), 301-317; https://doi.org/10.3390/ceramics5030024 - 22 Jul 2022
Cited by 1 | Viewed by 2828
Abstract
Synthetic 11 Å tobermorite (Ca5Si6O16(OH)2.4H2O) and its Al-substituted analogue are layer-lattice ion-exchangers with potential applications in nuclear and hazardous wastewater treatment. The present study reports the facile one-pot hydrothermal synthesis of an Al-tobermorite-rich [...] Read more.
Synthetic 11 Å tobermorite (Ca5Si6O16(OH)2.4H2O) and its Al-substituted analogue are layer-lattice ion-exchangers with potential applications in nuclear and hazardous wastewater treatment. The present study reports the facile one-pot hydrothermal synthesis of an Al-tobermorite-rich cation-exchanger from a combination of paper recycling ash, post-consumer container glass, and lime, with compositional ratios of [Ca]/[Si + Al] = 0.81 and [Al]/[Si + Al] = 0.18. The reaction products were characterized by powder X-ray diffraction analysis, 29Si magic angle spinning nuclear magnetic resonance spectroscopy, and scanning electron microscopy. Hydrothermal processing in 4 M NaOH(aq) at 100 °C for 7 days yielded an Al-tobermorite-rich product that also contained katoite (Ca3Al2SiO12H8), portlandite (Ca(OH)2), calcite (CaCO3), and amorphous silicate gel. The hydrothermal product was found to have a Cs+ cation exchange capacity of 59 ± 4 meq 100 g−1 and selective Cs+ distribution coefficients (Kd) of 574 ± 13 and 658 ± 34 cm3 g−1 from solutions with molar ratios [Cs+]:[Na+] and [Cs+]:[Ca2+] of 1:100. In a batch sorption study at 20 °C, the uptakes of Pb2+, Cd2+, and Cs+ were determined to be 1.78 ± 0.04, 0.65 ± 0.06, and 0.36 ± 0.03 mmol g−1, respectively. The kinetics of Pb2+, Cd2+, and Cs+ removal were described by the pseudo-second-order rate model, which gave respective rate constants (k2) of 0.010, 0.027, and 1.635 g mmol−1 min−1, and corresponding correlation coefficients (R2) of 0.997, 0.996, and 0.999. The metal ion sorption properties of the tobermorite-rich product compared favorably with those of other waste-derived tobermorites reported in the literature. Potential strategies to improve the yield, crystallinity, and sorption characteristics of the product are discussed. Full article
(This article belongs to the Special Issue Geopolymers and Ceramics)
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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 2 | Viewed by 4097
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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7 pages, 2769 KiB  
Article
Thermoelectric Properties of Si-Doped In2Se3 Polycrystalline Alloys
by Okmin Park, Se Woong Lee and Sang-il Kim
Ceramics 2022, 5(3), 281-287; https://doi.org/10.3390/ceramics5030022 - 9 Jul 2022
Cited by 3 | Viewed by 2284
Abstract
Post-metal chalcogenides, including InSe, In2Se3, and In4Se3, have attracted considerable attention as potential thermoelectric materials because of their intrinsically low thermal conductivity, which is attributed to their layered structure with weak van der Waals bonds. [...] Read more.
Post-metal chalcogenides, including InSe, In2Se3, and In4Se3, have attracted considerable attention as potential thermoelectric materials because of their intrinsically low thermal conductivity, which is attributed to their layered structure with weak van der Waals bonds. In this study, we examined the electrical and thermoelectric properties of Si-doped In2Se3 (In2−xSixSe3, x = 0, 0.005, 0.01, 0.015, and 0.02) polycrystalline samples. Hexagonal α(2H)-In2Se3 phase was synthesized without any impurity, and gradual changes in the lattice parameters were observed with Si doping. Drastic changes were observed for the measured electrical and thermal transport properties at 450–500 K, due to the phase transition from α to β at 473 K. The highest power factors were achieved by the sample with x = 0.015 for both α and β phases, exhibiting the values of 0.137 and 0.0884 mW/mK2 at 450 and 750 K, respectively. The total thermal conductivities of the α phase samples decreased gradually with increasing Si doping content, which is attributed to the point defect phonon scattering by Si doping. The total thermal conductivities of the β phase samples significantly decreased compared to those of the α phase samples. Therefore, the sample with x = 0.015 (In1.985Si0.015Se3) showed the maximum thermoelectric figure of merit values of 0.100 and 0.154 at 450 and 750 K, which are enhanced by 152 and 48% compared with those of the undoped α- and β-In2Se3 samples, respectively. Full article
(This article belongs to the Special Issue Advances in Ceramics)
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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 - 7 Jul 2022
Cited by 2 | Viewed by 2006
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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16 pages, 5771 KiB  
Article
Smart Self-Sensing Piezoresistive Composite Materials for Structural Health Monitoring
by Relebohile George Qhobosheane, Monjur Morshed Rabby, Vamsee Vadlamudi, Kenneth Reifsnider and Rassel Raihan
Ceramics 2022, 5(3), 253-268; https://doi.org/10.3390/ceramics5030020 - 21 Jun 2022
Cited by 5 | Viewed by 2968
Abstract
The use of fiber-reinforced composite materials has widely spread in various sectors, including aerospace, defense, and civil industry. The assessment of these heterogeneous material systems is important for safer and risk-free applications and has contributed to the need for self-sensing composites. This work [...] Read more.
The use of fiber-reinforced composite materials has widely spread in various sectors, including aerospace, defense, and civil industry. The assessment of these heterogeneous material systems is important for safer and risk-free applications and has contributed to the need for self-sensing composites. This work is focused on the development of piezoresistive composites, the prediction of their performance and structural health monitoring (SHM). Additionally, this work unpacks the complexity of carbon nanotubes (CNTs) micro-fabrication and the development of piezoresistive and electromagnetic (EM) waves detection electrodes. Scanning electron microscopy (SEM) was used to characterize the CNTs structure and morphologies. The manufactured CNTs were incorporated in epoxy systems to fabricate glass fiber reinforced polymer (GFRP)-CNTs smart composites with piezoresistive properties. The detection of micro-damage onset and its progression was carried out in mode I, to evaluate the sensitivity of the smart composites to damage development. The change in electrical conductivity of the nanotubes-reinforced composite systems due to localized mechanical strains enabled crack propagation detection. The relationship between crack propagation, fracture toughness, and electrical resistivity of the smart composite was analyzed. Full article
(This article belongs to the Special Issue Innovative Processing Routes for Electroactive Materials)
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