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Keywords = microextrusion printing

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18 pages, 12812 KB  
Article
Semi-Theoretical Modeling and Experimental Validation of the Extrusion Swell Ratio of Highly Concentrated Silver Paste in Micro-Extrusion
by Zhijie Huang, Shixiong Wu, Zhichao Yuan, Zeyu Wang, Cuimin Sun and Hui You
Micromachines 2026, 17(7), 855; https://doi.org/10.3390/mi17070855 - 17 Jul 2026
Viewed by 316
Abstract
In micro-extrusion and direct ink writing, the nozzle outlet diameter is often used to estimate the deposited line width or free-filament diameter. However, highly loaded conductive silver pastes may exhibit pronounced extrusion swell after leaving the nozzle, resulting in a filament diameter larger [...] Read more.
In micro-extrusion and direct ink writing, the nozzle outlet diameter is often used to estimate the deposited line width or free-filament diameter. However, highly loaded conductive silver pastes may exhibit pronounced extrusion swell after leaving the nozzle, resulting in a filament diameter larger than the nozzle inner diameter. To quantify this deviation, this study proposes a single-parameter semi-theoretical correction model based on radial force balance at the nozzle exit, integrating Herschel–Bulkley yield stress–shear-thinning rheology with a finite-deformation description. The exit radial stress is derived from pressure-driven circular tube flow, while the post-exit radial expansion is balanced against atmospheric constraint. A comprehensive correction force constant, C, is introduced to account for wall-induced energy dissipation, particle-structure rearrangement, residual elastic recovery, and model simplifications. After calibration using a transition-swelling nozzle, C was determined as 1.03 × 10−2 N. The model was applied to six nozzle diameters and four nozzle length–pressure conditions. For Nozzles 1–4 with significant swelling, the mean absolute percentage error was 5.31%, while the overall error for all six nozzles was 11.84%, mainly due to overestimation for the nearly non-swelling Nozzle 6. For varying nozzle lengths, the error was 5.20%, and both experimental and predicted swell ratios decreased with increasing effective nozzle length. The model provides a semi-theoretical tool for estimating free-filament dimensions and analyzing nozzle-length effects, primarily under pronounced-swell conditions. Its predictive capability becomes limited as the swell ratio approaches unity, where additional corrections for wall slip, relaxation, and the zero-swell boundary are required. Full article
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43 pages, 3884 KB  
Review
Advanced Layer Fabrication Technologies in Solid Oxide Fuel Cells: From Traditional Methods to Additive and Thin-Film Strategies
by Serikzhan Opakhai, Asset Kabyshev, Marzhan Kubenova, Zhassulan Zeinulla, Bakytbek Mauyey and Saira Sakhabayeva
Nanoenergy Adv. 2026, 6(1), 2; https://doi.org/10.3390/nanoenergyadv6010002 - 25 Dec 2025
Cited by 3 | Viewed by 2785
Abstract
This review examines modern approaches to layer formation in solid oxide fuel cells (SOFCs), focusing on traditional, thin-film, and additive manufacturing methods. A systematic comparison of technologies, including slip casting, screen printing, CVD, PLD, ALD, HiPIMS, inkjet, aerosol, and microextrusion printing, is provided. [...] Read more.
This review examines modern approaches to layer formation in solid oxide fuel cells (SOFCs), focusing on traditional, thin-film, and additive manufacturing methods. A systematic comparison of technologies, including slip casting, screen printing, CVD, PLD, ALD, HiPIMS, inkjet, aerosol, and microextrusion printing, is provided. It is shown that traditional methods remain technologically robust but are limited in their capabilities for miniaturization and interfacial architecture design. Modern thin-film and additive approaches provide high spatial accuracy, improved ion-electron characteristics, and flexibility in the design of multilayer structures; however, they require addressing issues related to scalability, ink stability, interfacial compatibility, and reproducibility. Particular attention is paid to interfacial engineering methods, such as functionally graded layers, nanostructured infiltration, and temperature-controlled 3D printing. Key challenges are discussed, including thermal instability of materials, the limited gas impermeability of ultra-thin electrolytes, and degradation during long-term operation. Development prospects lie in the integration of hybrid methods, the digitalization of deposition processes, and the implementation of intelligent control of printing parameters. The presented analysis forms the basis for further research into the scalable and highly efficient production of next-generation SOFCs designed for low-temperature operation and long-term operation in future energy systems. Full article
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13 pages, 3616 KB  
Article
Double-Network Hydrogel 3D BioPrinting Biocompatible with Fibroblast Cells for Tissue Engineering Applications
by Immacolata Greco, Hatim Machrafi and Carlo S. Iorio
Gels 2024, 10(11), 684; https://doi.org/10.3390/gels10110684 - 23 Oct 2024
Cited by 15 | Viewed by 3279
Abstract
The present study examines the formulation of a biocompatible hydrogel bioink for 3D bioprinting, integrating poly(ethylene glycol) diacrylate (PEGDA) and sodium alginate (SA) using a double-network approach. These materials were chosen for their synergistic qualities, with PEGDA contributing to mechanical integrity and SA [...] Read more.
The present study examines the formulation of a biocompatible hydrogel bioink for 3D bioprinting, integrating poly(ethylene glycol) diacrylate (PEGDA) and sodium alginate (SA) using a double-network approach. These materials were chosen for their synergistic qualities, with PEGDA contributing to mechanical integrity and SA ensuring biocompatibility. Fibroblast cells were included in the bioink and printed with a Reg4Life bioprinter employing micro-extrusion technology. The optimisation of printing parameters included needle size and flow velocities. This led to precise structure development and yielded results with a negligible deviation in printed angles and better control of line widths. The rheological characteristics of the bioink were evaluated, demonstrating appropriate viscosity and shear-thinning behaviour for efficient extrusion. The mechanical characterisation revealed an average compressive modulus of 0.38 MPa, suitable for tissue engineering applications. The printability of the bioink was further confirmed through the evaluations of morphology and diffusion rates, confirming structural integrity. Biocompatibility assessments demonstrated a high cell viability rate of 82.65% following 48 h of incubation, supporting the bioink’s suitability for facilitating cell survival. This study introduced a reliable technique for producing tissue-engineered scaffolds that exhibit outstanding mechanical characteristics and cell viability, highlighting the promise of PEGDA–SA hydrogels in bioprinting applications. Full article
(This article belongs to the Special Issue Composite Hydrogels for Biomedical Applications)
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16 pages, 7588 KB  
Article
Three-Dimensional-Bioprinted Non-Small Cell Lung Cancer Models in a Mouse Phantom for Radiotherapy Research
by Yikun Mei, Elena Lakotsenina, Marie Wegner, Timon Hehne, Dieter Krause, Dani Hakimeh, Dongwei Wu, Elisabeth Schültke, Franziska Hausmann, Jens Kurreck and Beatrice Tolksdorf
Int. J. Mol. Sci. 2024, 25(19), 10268; https://doi.org/10.3390/ijms251910268 - 24 Sep 2024
Cited by 6 | Viewed by 3128
Abstract
Lung cancer continues to have one of the highest morbidity and mortality rates of any cancer. Although radiochemotherapy, in combination with immunotherapy, has significantly improved overall survival, new treatment options are urgently needed. However, preclinical radiotherapy testing is often performed in animal models, [...] Read more.
Lung cancer continues to have one of the highest morbidity and mortality rates of any cancer. Although radiochemotherapy, in combination with immunotherapy, has significantly improved overall survival, new treatment options are urgently needed. However, preclinical radiotherapy testing is often performed in animal models, which has several drawbacks, including species-specific differences and ethical concerns. To replace animal models, this study used a micro-extrusion bioprinting approach to generate a three-dimensional (3D) human lung cancer model consisting of lung tumor cells embedded in human primary lung fibroblasts for radiotherapy research. The models were placed in a mouse phantom, i.e., a 3D-printed mouse model made of materials that mimic the X-ray radiation attenuation rates found in mice. In radiotherapy experiments, the model demonstrated a selective cytotoxic effect of X-rays on tumor cells, consistent with findings in 2D cells. Furthermore, the analysis of metabolic activity, cell death, apoptosis, and DNA damage-induced γH2AX foci formation revealed different results in the 3D model inside the phantom compared to those observed in irradiated models without phantom and 2D cells. The proposed setup of the bioprinted 3D lung model inside the mouse phantom provides a physiologically relevant model system to study radiation effects. Full article
(This article belongs to the Section Molecular Oncology)
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15 pages, 4573 KB  
Article
Computational Fluid Dynamics Analysis and Empirical Evaluation of Carboxymethylcellulose/Alginate 3D Bioprinting Inks for Screw-Based Microextrusion
by Sungmin Lee, Minjae Son, Juo Lee, Iksong Byun, Jin-Woo Kim, Jungsil Kim and Hoon Seonwoo
Polymers 2024, 16(8), 1137; https://doi.org/10.3390/polym16081137 - 18 Apr 2024
Cited by 11 | Viewed by 3143
Abstract
Three-dimensional microextrusion bioprinting technology uses pneumatics, pistons, or screws to transfer and extrude bioinks containing biomaterials and cells to print biological tissues and organs. Computational fluid dynamics (CFD) analysis can simulate the flow characteristics of bioinks in a control volume, and the effect [...] Read more.
Three-dimensional microextrusion bioprinting technology uses pneumatics, pistons, or screws to transfer and extrude bioinks containing biomaterials and cells to print biological tissues and organs. Computational fluid dynamics (CFD) analysis can simulate the flow characteristics of bioinks in a control volume, and the effect on cell viability can be predicted by calculating the physical quantities. In this study, we developed an analysis system to predict the effect of a screw-based dispenser system (SDS) on cell viability in bioinks through rheological and CFD analyses. Furthermore, carboxymethylcellulose/alginate-based bioinks were used for the empirical evaluation of high-viscous bioinks. The viscosity of bioinks was determined by rheological measurement, and the viscosity coefficient for the CFD analysis was derived from a correlation equation by non-linear regression analysis. The mass flow rate derived from the analysis was successfully validated by comparison with that from the empirical evaluation. Finally, the cell viability was confirmed after bioprinting with bioinks containing C2C12 cells, suggesting that the developed SDS may be suitable for application in the field of bioengineering. Consequently, the developed bioink analysis system is applicable to a wide range of systems and materials, contributing to time and cost savings in the bioengineering industry. Full article
(This article belongs to the Special Issue Functional Alginate-Based Materials III)
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13 pages, 3110 KB  
Article
In Vitro Profile of Hydrocortisone Release from Three-Dimensionally Printed Paediatric Mini-Tablets
by Chrystalla Protopapa, Angeliki Siamidi, Siva Satyanarayana Kolipaka, Laura Andrade Junqueira, Dennis Douroumis and Marilena Vlachou
Pharmaceutics 2024, 16(3), 385; https://doi.org/10.3390/pharmaceutics16030385 - 11 Mar 2024
Cited by 17 | Viewed by 3978
Abstract
Three-dimensional (3D) printing is quickly being adopted in pharmaceutics due to the many advantages it offers, including treatment, adaptability, the reduction in waste and the accelerated development of new formulations. In this study, micro-extrusion printing was implemented for the production of modified-release hydrocortisone [...] Read more.
Three-dimensional (3D) printing is quickly being adopted in pharmaceutics due to the many advantages it offers, including treatment, adaptability, the reduction in waste and the accelerated development of new formulations. In this study, micro-extrusion printing was implemented for the production of modified-release hydrocortisone (HCT) mini-tablets for paediatric patients. For the developed formulations, Gelucire® 44/14 and Precirol® ATO 5 were used as the main inks at three different ratios: 70%/30%, 60%/40% and 50%/50%, respectively. The printing parameters (temperature and pressure) were altered accordingly for each ratio to achieve printability. The printed mini-tablets exhibited excellent printing quality, featuring consistent layer thicknesses and smooth surfaces. Dissolution tests were performed, and the results indicated a successful modified release of HCT from the mini-tablets. In summary, micro-extrusion exhibited favourable processing abilities for powder blends, facilitating quick printing and the fabrication of potential personalized dosages. Full article
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24 pages, 7601 KB  
Review
A Review of the Preparation of Porous Fibers and Porous Parts by a Novel Micro-Extrusion Foaming Technique
by Zelin Wang, Hanyi Huang, Yushu Wang, Mengnan Zhou and Wentao Zhai
Materials 2024, 17(1), 172; https://doi.org/10.3390/ma17010172 - 28 Dec 2023
Cited by 11 | Viewed by 5010
Abstract
This review introduces an innovative technology termed “Micro-Extrusion Foaming (MEF)”, which amalgamates the merits of physical foaming and 3D printing. It presents a groundbreaking approach to producing porous polymer fibers and parts. Conventional methods for creating porous materials often encounter obstacles such as [...] Read more.
This review introduces an innovative technology termed “Micro-Extrusion Foaming (MEF)”, which amalgamates the merits of physical foaming and 3D printing. It presents a groundbreaking approach to producing porous polymer fibers and parts. Conventional methods for creating porous materials often encounter obstacles such as the extensive use of organic solvents, intricate processing, and suboptimal production efficiency. The MEF technique surmounts these challenges by initially saturating a polymer filament with compressed CO2 or N2, followed by cell nucleation and growth during the molten extrusion process. This technology offers manifold advantages, encompassing an adjustable pore size and porosity, environmental friendliness, high processing efficiency, and compatibility with diverse polymer materials. The review meticulously elucidates the principles and fabrication process integral to MEF, encompassing the creation of porous fibers through the elongational behavior of foamed melts and the generation of porous parts through the stacking of foamed melts. Furthermore, the review explores the varied applications of this technology across diverse fields and imparts insights for future directions and challenges. These include augmenting material performance, refining fabrication processes, and broadening the scope of applications. MEF technology holds immense potential in the realm of porous material preparation, heralding noteworthy advancements and innovations in manufacturing and materials science. Full article
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14 pages, 3514 KB  
Article
Experimental Validation of a Micro-Extrusion Set-Up with In-Line Rheometry for the Production and Monitoring of Filaments for 3D-Printing
by João Sousa, Paulo F. Teixeira, Loïc Hilliou and José A. Covas
Micromachines 2023, 14(8), 1496; https://doi.org/10.3390/mi14081496 - 26 Jul 2023
Cited by 3 | Viewed by 3069
Abstract
The main objective of this work is to validate an in-line micro-slit rheometer and a micro-extrusion line, both designed for the in-line monitoring and production of filaments for 3D printing using small amounts of material. The micro-filament extrusion line is first presented and [...] Read more.
The main objective of this work is to validate an in-line micro-slit rheometer and a micro-extrusion line, both designed for the in-line monitoring and production of filaments for 3D printing using small amounts of material. The micro-filament extrusion line is first presented and its operational window is assessed. The throughputs ranged between 0.045 kg/h and 0.15 kg/h with a maximum 3% error and with a melt temperature control within 1 °C under the processing conditions tested for an average residence time of about 3 min. The rheological micro slit is then presented and assessed using low-density polyethylene (LDPE) and cyclic olefin copolymer (COC). The excellent matching between the in-line micro-rheological data and the data measured with off-line rotational and capillary rheometers validate the in-line micro-slit rheometer. However, it is shown that the COC does not follow the Cox–Merz rule. The COC filaments produced with the micro-extrusion line were successfully used in the 3D printing of specimens for tensile testing. The quality of both filaments (less than 6% variation in diameter along the filament’s length) and printed specimens validated the whole micro-set-up, which was eventually used to deliver a rheological mapping of COC printability. Full article
(This article belongs to the Special Issue 3D Printing Technology and Its Applications)
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18 pages, 20802 KB  
Article
Hydrothermal Synthesis of Nickel Oxide and Its Application in the Additive Manufacturing of Planar Nanostructures
by Darya A. Dudorova, Tatiana L. Simonenko, Nikolay P. Simonenko, Philipp Yu. Gorobtsov, Ivan A. Volkov, Elizaveta P. Simonenko and Nikolay T. Kuznetsov
Molecules 2023, 28(6), 2515; https://doi.org/10.3390/molecules28062515 - 9 Mar 2023
Cited by 19 | Viewed by 6590
Abstract
The hydrothermal synthesis of nickel oxide in the presence of triethanolamine was studied. Furthermore, the relationship between the synthesis conditions, thermal behavior, crystal structure features, phase composition and microstructure of semi-products, and the target oxide nanopowders was established. The thermal behavior of the [...] Read more.
The hydrothermal synthesis of nickel oxide in the presence of triethanolamine was studied. Furthermore, the relationship between the synthesis conditions, thermal behavior, crystal structure features, phase composition and microstructure of semi-products, and the target oxide nanopowders was established. The thermal behavior of the semi-products was studied using a simultaneous thermal analysis (in particular, using one that involved thermogravimetric analysis and differential scanning calorimetry, TGA/DSC). An X-ray diffraction (XRD) analysis revealed that varying the triethanolamine and nickel chloride concentration in the reaction system can govern the formation of α- and β-Ni(OH)2-based semi-products that contain Ni(HCO3)2 or Ni2(CO3)(OH)2 as additional components. The set of functional groups in the powders was determined using a Fourier-transform infrared (FTIR) spectroscopy analysis. Using microextrusion printing, a composite NiO—(CeO2)0.80(Sm2O3)0.20 anode film was fabricated. Using XRD, scanning electron microscopy (SEM), and atomic force microscopy (AFM) analyses, it was demonstrated that the crystal structure, dispersity, and microstructure character of the obtained material correspond to the initial nanopowders. Using Kelvin probe force microscopy (KPFM) and scanning capacitance microscopy (SCM), the local electrophysical properties of the printed composite film were examined. The value of its conductivity was evaluated using the four-probe method on a direct current in the temperature range of 300–650 °C. The activation energy for the 500–650 °C region, which is of most interest in the context of intermediate-temperature SOFCs working temperatures, has been estimated. Full article
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16 pages, 6918 KB  
Article
Gene-Expression Analysis of Human Fibroblasts Affected by 3D-Printed Carboxylated Nanocellulose Constructs
by Jennifer Rosendahl, Chiara Zarna, Joakim Håkansson and Gary Chinga-Carrasco
Bioengineering 2023, 10(1), 121; https://doi.org/10.3390/bioengineering10010121 - 16 Jan 2023
Cited by 9 | Viewed by 3853
Abstract
Three-dimensional (3D) printing has emerged as a highly valuable tool to manufacture porous constructs. This has major advantages in, for example, tissue engineering, in which 3D scaffolds provide a microenvironment with adequate porosity for cell growth and migration as a simulation of tissue [...] Read more.
Three-dimensional (3D) printing has emerged as a highly valuable tool to manufacture porous constructs. This has major advantages in, for example, tissue engineering, in which 3D scaffolds provide a microenvironment with adequate porosity for cell growth and migration as a simulation of tissue regeneration. In this study, we assessed the suitability of three cellulose nanofibrils (CNF) that were obtained through 2,2,6,6-tetramethylpyperidine-1-oxyl (TEMPO)-mediated oxidation. The CNFs were obtained by applying three levels of carboxylation, i.e., 2.5, 3.8, and 6.0 mmol sodium hypochlorite (NaClO) per gram of cellulose. The CNFs exhibited different nanofibrillation levels, affecting the corresponding viscosity and 3D printability of the CNF gels (0.6 wt%). The scaffolds were manufactured by micro-extrusion and the nanomechanical properties were assessed with nanoindentation. Importantly, fibroblasts were grown on the scaffolds and the expression levels of the marker genes, which are relevant for wound healing and proliferation, were assessed in order to reveal the effect of the 3D-scaffold microenvironment of the cells. Full article
(This article belongs to the Special Issue Biopolymers and Nano-Objects Applications in Bioengineering)
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17 pages, 19940 KB  
Article
The Ti0.2V1.8C MXene Ink-Prepared Chemiresistor: From Theory to Tests with Humidity versus VOCs
by Nikolay P. Simonenko, Olga E. Glukhova, Ilya A. Plugin, Dmitry A. Kolosov, Ilya A. Nagornov, Tatiana L. Simonenko, Alexey S. Varezhnikov, Elizaveta P. Simonenko, Victor V. Sysoev and Nikolay T. Kuznetsov
Chemosensors 2023, 11(1), 7; https://doi.org/10.3390/chemosensors11010007 - 22 Dec 2022
Cited by 31 | Viewed by 3611
Abstract
The 2D structure of MXenes attracts wide research attention toward an application of these materials in gas sensors. These structures are extremely sensitive to minor variations in their composition, which are employed for tuning their functional properties. Here, we consider the partially substituted [...] Read more.
The 2D structure of MXenes attracts wide research attention toward an application of these materials in gas sensors. These structures are extremely sensitive to minor variations in their composition, which are employed for tuning their functional properties. Here, we consider the partially substituted MXenes of the composition of TixV2-xC, where x = 0.2, via quantum chemical calculations, and test their chemiresistive characteristics as a receptor component of the planar-type sensor and on-chip multisensor array. We thoroughly discuss the synthesis process of Ti0.2V1.8AlC MAX-phase and the corresponding MXenes, to prepare functional inks and, furthermore, deposit the films by microextrusion printing over an array of planar multi-electrode structures at the surface of a pen-sized chip. The crystal structure of the obtained materials is evaluated via X-ray diffraction analysis. The developed chip has been exposed upon few gaseous analytes, of alcohol VOCs, NH3, and H2O, of a 500–16,000 ppm concentration, at room temperature to ensure that we could observe the positive chemiresistive effect matured from resistance enhancing, with up to 10% vs. water vapors. The calculations carried in the framework of the density-functional theory for V2C, Ti2C, and Ti0.2V1.8C crystals ensured that the variations in their electronic structure were almost consistent with the experiment fundings: the most prominent effect is observed in relation to the H2O vapors. Therefore, these Ti0.2V1.8C structures could be considered for applying them in room temperature-operated hygrometers. Full article
(This article belongs to the Section Materials for Chemical Sensing)
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14 pages, 4533 KB  
Article
Microextrusion Printing of Multilayer Hierarchically Organized Planar Nanostructures Based on NiO, (CeO2)0.8(Sm2O3)0.2 and La0.6Sr0.4Co0.2Fe0.8O3−δ
by Tatiana L. Simonenko, Nikolay P. Simonenko, Philipp Yu. Gorobtsov, Elizaveta P. Simonenko and Nikolay T. Kuznetsov
Micromachines 2023, 14(1), 3; https://doi.org/10.3390/mi14010003 - 20 Dec 2022
Cited by 9 | Viewed by 2979
Abstract
In this paper, NiO, La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) and (CeO2)0.8(Sm2O3)0.2 (SDC) nanopowders with different microstructures were obtained using hydrothermal and glycol–citrate methods. The microstructural features of the [...] Read more.
In this paper, NiO, La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) and (CeO2)0.8(Sm2O3)0.2 (SDC) nanopowders with different microstructures were obtained using hydrothermal and glycol–citrate methods. The microstructural features of the powders were examined using scanning electron microscopy (SEM). The obtained oxide powders were used to form functional inks for the sequential microextrusion printing of NiO-SDC, SDC and LSCF-SDC coatings with resulting three-layer structures of (NiO-SDC)/SDC/(LSCF-SDC) composition. The crystal structures of these layers were studied using an X-ray diffraction analysis, and the microstructures were studied using atomic force microscopy. Scanning capacitance microscopy was employed to build maps of capacitance gradient distribution over the surface of the oxide layers, and Kelvin probe force microscopy was utilized to map surface potential distribution and to estimate the work function values of the studied oxide layers. Using SEM and an energy-dispersive X-ray microanalysis, the cross-sectional area of the formed three-layer structure was analyzed—the interfacial boundary and the chemical element distribution over the surface of the cross-section were investigated. Using impedance spectroscopy, the temperature dependence of the electrical conductivity was also determined for the printed three-layer nanostructure. Full article
(This article belongs to the Special Issue Advanced Micro- and Nano-Manufacturing Technologies)
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16 pages, 6288 KB  
Article
Atmospheric Pressure Solvothermal Synthesis of Nanoscale SnO2 and Its Application in Microextrusion Printing of a Thick-Film Chemosensor Material for Effective Ethanol Detection
by Nikita A. Fisenko, Ivan A. Solomatov, Nikolay P. Simonenko, Artem S. Mokrushin, Philipp Yu. Gorobtsov, Tatiana L. Simonenko, Ivan A. Volkov, Elizaveta P. Simonenko and Nikolay T. Kuznetsov
Sensors 2022, 22(24), 9800; https://doi.org/10.3390/s22249800 - 14 Dec 2022
Cited by 8 | Viewed by 4118
Abstract
The atmospheric pressure solvothermal (APS) synthesis of nanocrystalline SnO2 (average size of coherent scattering regions (CSR)—7.5 ± 0.6 nm) using tin acetylacetonate as a precursor was studied. The resulting nanopowder was used as a functional ink component in microextrusion printing of a [...] Read more.
The atmospheric pressure solvothermal (APS) synthesis of nanocrystalline SnO2 (average size of coherent scattering regions (CSR)—7.5 ± 0.6 nm) using tin acetylacetonate as a precursor was studied. The resulting nanopowder was used as a functional ink component in microextrusion printing of a tin dioxide thick film on the surface of a Pt/Al2O3/Pt chip. Synchronous thermal analysis shows that the resulting semiproduct is transformed completely into tin dioxide nanopowder at 400 °C within 1 h. The SnO2 powder and the resulting film were shown to have a cassiterite-type structure according to X-ray diffraction analysis, and IR spectroscopy was used to establish the set of functional groups in the material composition. The microstructural features of the tin dioxide powder were analyzed using scanning (SEM) and transmission (TEM) electron microscopy: the average size of the oxide powder particles was 8.2 ± 0.7 nm. Various atomic force microscopy (AFM) techniques were employed to investigate the topography of the oxide film and to build maps of surface capacitance and potential distribution. The temperature dependence of the electrical conductivity of the printed SnO2 film was studied using impedance spectroscopy. The chemosensory properties of the formed material when detecting H2, CO, NH3, C6H6, C3H6O and C2H5OH, including at varying humidity, were also examined. It was demonstrated that the obtained SnO2 film has an increased sensitivity (the sensory response value was 1.4–63.5) and selectivity for detection of 4–100 ppm C2H5OH at an operating temperature of 200 °C. Full article
(This article belongs to the Collection Gas Sensors)
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16 pages, 3804 KB  
Article
Synthesis of ((CeO2)0.8(Sm2O3)0.2)@NiO Core-Shell Type Nanostructures and Microextrusion Printing of a Composite Anode Based on Them
by Tatiana L. Simonenko, Nikolay P. Simonenko, Philipp Yu. Gorobtsov, Oleg Yu. Grafov, Elizaveta P. Simonenko and Nikolay T. Kuznetsov
Materials 2022, 15(24), 8918; https://doi.org/10.3390/ma15248918 - 13 Dec 2022
Cited by 6 | Viewed by 2733
Abstract
The process of the hydrothermal synthesis of hierarchically organized nanomaterials with the core-shell structure with the composition ((CeO2)0.8(Sm2O3)0.2)@NiO was studied, and the prospects for their application in the formation of planar composite structures [...] Read more.
The process of the hydrothermal synthesis of hierarchically organized nanomaterials with the core-shell structure with the composition ((CeO2)0.8(Sm2O3)0.2)@NiO was studied, and the prospects for their application in the formation of planar composite structures using microextrusion printing were shown. The hydrothermal synthesis conditions of the (CeO2)0.8(Sm2O3)0.2 nanospheres were determined, and the approach to their surface modification by growing the NiO shell with the formation of core-shell structures equally distributed between the larger nickel(II) oxide nanosheets was developed. The resulting nanopowder was used as a functional ink component in the microextrusion printing of the corresponding composite coating. The microstructure of the powders and the oxide coating was studied by scanning (SEM) and transmission electron microscopy (TEM), the crystal structure was explored by X-ray diffraction analysis (XRD), the set of functional groups in the powders was studied by Fourier-transform infrared spectroscopy (FTIR) spectroscopy, and their thermal behavior in an air flow by synchronous thermal analysis (TGA/DSC). The electronic state of the chemical elements in the resulting coating was studied using X-ray photoelectron spectroscopy (XPS). The surface topography and local electrophysical properties of the composite coating were studied using atomic force microscopy (AFM) and Kelvin probe force microscopy (KPFM). Using impedance spectroscopy, the temperature dependence of the specific electrical conductivity of the obtained composite coating was estimated. Full article
(This article belongs to the Special Issue Dynamic Behavior of Ceramic Composites and Composite Structures)
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16 pages, 5756 KB  
Article
Microextrusion Printing of Hierarchically Structured Thick V2O5 Film with Independent from Humidity Sensing Response to Benzene
by Philipp Yu. Gorobtsov, Artem S. Mokrushin, Tatiana L. Simonenko, Nikolay P. Simonenko, Elizaveta P. Simonenko and Nikolay T. Kuznetsov
Materials 2022, 15(21), 7837; https://doi.org/10.3390/ma15217837 - 7 Nov 2022
Cited by 14 | Viewed by 3122
Abstract
The process of V2O5 oxide by the combination of sol-gel technique and hydrothermal treatment using heteroligand [VO(C5H7O2)2–x(C4H9O)x] precursor was studied. Using thermal analysis, X-ray powder diffraction [...] Read more.
The process of V2O5 oxide by the combination of sol-gel technique and hydrothermal treatment using heteroligand [VO(C5H7O2)2–x(C4H9O)x] precursor was studied. Using thermal analysis, X-ray powder diffraction (XRD) and infra-red spectroscopy (IR), it was found that the resulting product was VO2(B), which after calcining at 300 °C (1 h), oxidized to orthorhombic V2O5. Scanning electron microscopy (SEM) results for V2O5 powder showed that it consisted of nanosheets (~50 nm long and ~10 nm thick) assembled in slightly spherical hierarchic structures (diameter ~200 nm). VO2 powder dispersion was used as functional ink for microextrusion printing of oxide film. After calcining the film at 300 °C (30 min), it was found that it oxidized to V2O5, with SEM and atomic force microscopy (AFM) results showing that the film structure retained the hierarchic structure of the powder. Using Kelvin probe force microscopy (KPFM), the work function value for V2O5 film in ambient conditions was calculated (4.81 eV), indicating a high amount of deficiencies in the sample. V2O5 film exhibited selective response upon sensing benzene, with response value invariable under changing humidity. Studies of the electrical conductivity of the film revealed increased resistance due to high film porosity, with conductivity activation energy being 0.26 eV. Full article
(This article belongs to the Section Materials Chemistry)
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