Editorial

9 pages, 233 KiB

Open AccessEditorial

10th Anniversary of Inorganics: Inorganic Materials

by Roberto Nisticò, Hicham Idriss, Luciano Carlos, Eleonora Aneggi and Torben R. Jensen

Inorganics 2024, 12(3), 62; https://doi.org/10.3390/inorganics12030062 - 20 Feb 2024

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To celebrate the 10th anniversary of the journal Inorganics, the “Inorganic Materials” section launched this Special Issue entitled “10th Anniversary of Inorganics: Inorganic Materials”, which collected 25 interesting papers (i [...] Full article

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19 pages, 3030 KiB

Open AccessArticle

ZnO–Doped CaO Binary Core–Shell Catalysts for Biodiesel Production via Mexican Palm Oil Transesterification

by M. G. Arenas-Quevedo, M. E. Manríquez, J. A. Wang, O. Elizalde-Solís, J. González-García, A. Zúñiga-Moreno and L. F. Chen

Inorganics 2024, 12(2), 51; https://doi.org/10.3390/inorganics12020051 - 03 Feb 2024

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Abstract

This work investigates biodiesel production via transesterification of Mexican palm oil with methanol catalyzed by binary solid base core–shell catalysts with improved catalytic stability. A series of CaO–ZnO mixed solids were prepared using an inexpensive co–precipitation method by varying ZnO content from 5 [...] Read more.

This work investigates biodiesel production via transesterification of Mexican palm oil with methanol catalyzed by binary solid base core–shell catalysts with improved catalytic stability. A series of CaO–ZnO mixed solids were prepared using an inexpensive co–precipitation method by varying ZnO content from 5 to 20 mol%. Several factors, such as surface basicity, ZnO content, phase compositions, and thermal treatment of the catalysts, were all proven to be crucial for the production of biodiesel with good quality. Thermal treatment could effectively remove the surface adsorbed water and impurities and improved the catalytic activity. The addition of ZnO to CaO significantly enhanced the catalysts’ stability; however, it led to lower surface basicity and slightly diminished catalytic activity. ZnO doping inhibited the formation of surface Ca(OH)₂ and promoted the formation of Ca–Zn–O or CaZn₂(OH)₆ phase as the core and a surface CaCO₃ shell, which effectively decreased Ca²⁺ leaching by approximately 74% in methanol and 65% in a methanol–glycerol (4:1) mixture. A combined method of separation and purification for obtaining clean biodiesel with high quality was proposed. The biodiesel obtained under the control conditions exhibited properties which satisfied the corresponding standards well. Full article

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14 pages, 5358 KiB

Open AccessArticle

Preparation of Environmentally Friendly BiVO₄@SiO₂ Encapsulated Yellow Pigment with Remarkable Thermal and Chemical Stability

by Renhua Chen, Xiaozhen Zhang, Rui Tao, Yuhua Jiang, Huafeng Liu and Lanlan Cheng

Inorganics 2024, 12(1), 17; https://doi.org/10.3390/inorganics12010017 - 30 Dec 2023

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Abstract

The preparation of environmentally friendly inorganic encapsulated pigments with a bright color and sufficient stability provides an effective strategy for expanding their applications in plastic, paint, glass, and ceramic decoration. The challenges facing the use of such pigments include the formation of a [...] Read more.

The preparation of environmentally friendly inorganic encapsulated pigments with a bright color and sufficient stability provides an effective strategy for expanding their applications in plastic, paint, glass, and ceramic decoration. The challenges facing the use of such pigments include the formation of a dense protective coating with the required endurance, the relatively weak color of the encapsulated pigments, and the preferable inclusion particle size. Environmentally friendly BiVO₄ is regarded as a very promising pigment for multiple coloring applications due to its brilliant yellow color with high saturation. However, its poor thermal and chemical stability greatly limit the application of BiVO₄. Herein, we report a sol–gel method to synthesize inorganic BiVO₄@SiO₂ yellow pigment with a core–shell structure. By controlling the synthesis conditions, including the particle size and dispersion of BiVO₄ and the calcination temperature, a BiVO₄@SiO₂ encapsulated pigment with excellent chromatic properties was achieved. The obtained environmentally friendly BiVO₄@SiO₂ pigment with encapsulation modification has a comparable color-rendering performance to BiVO₄, and it has a high thermal stability at 700 °C, excellent acid resistance, and good compatibility in plastics. The present research is expected to expand the application of yellow BiVO₄ pigment in harsh environments. Full article

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17 pages, 5717 KiB

Open AccessArticle

Modification of Graphite/SiO₂ Film Electrodes with Hybrid Organic–Inorganic Perovskites for the Detection of Vasoconstrictor Bisartan 4-Butyl-Ν,Ν-bis{[2-(2H-tetrazol-5-yl)biphenyl-4-yl]methyl}imidazolium Bromide

by Georgios Papathanidis, Anna Ioannou, Alexandros Spyrou, Aggeliki Mandrapylia, Konstantinos Kelaidonis, John Matsoukas, Ioannis Koutselas and Emmanuel Topoglidis

Inorganics 2023, 11(12), 485; https://doi.org/10.3390/inorganics11120485 - 18 Dec 2023

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Abstract

In the present work, a hybrid organic–inorganic semiconductor (HOIS) has been used to modify the surface of a graphite paste/silica (G–SiO₂) film electrode on a conducting glass substrate to fabricate a promising, sensitive voltammetric sensor for the vasoconstrictor bisartan BV6, which [...] Read more.

In the present work, a hybrid organic–inorganic semiconductor (HOIS) has been used to modify the surface of a graphite paste/silica (G–SiO₂) film electrode on a conducting glass substrate to fabricate a promising, sensitive voltammetric sensor for the vasoconstrictor bisartan BV6, which could possibly treat hypertension and COVID-19. The HOIS exhibits exceptional optoelectronic properties with promising applications not only in light-emitting diodes, lasers, or photovoltaics but also for the development of voltammetric sensors due to the ability of the immobilized HOIS lattice to interact with ions. This study involves the synthesis and characterization of an HOIS and its attachment on the surface of a G–SiO₂ film electrode in order to develop a nanocomposite, simple, sensitive with a fast-response, low-cost voltammetric sensor for BV6. The modified HOIS electrode was characterized using X-ray diffraction, scanning electron microscopy, and optical and photoluminescence spectroscopy, and its electrochemical behavior was examined using cyclic voltammetry. Under optimal conditions, the modified G–SiO₂ film electrode exhibited a higher electrocatalytic activity towards the oxidation of BV6 compared to a bare graphite paste electrode. The results showed that the peak current was proportional to BV6 concentration with a linear response range from 0 to 65 × 10⁻⁶ (coefficient of determination, 0.9767) and with a low detection limit of 1.5 × 10⁻⁶ M (S/N = 3), estimated based on the area under a voltammogram, while it was 3.5 × 10⁻⁶ for peak-based analysis. The sensor demonstrated good stability and reproducibility and was found to be appropriate for the determination of drug compounds such as BV6. Full article

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12 pages, 5086 KiB

Open AccessArticle

Alternative Synthesis of MCM-41 Using Inexpensive Precursors for CO₂ Capture

by Guillermo D. Aquino, M. Sergio Moreno, Cristian M. Piqueras, Germán P. Benedictto and Andrea M. Pereyra

Inorganics 2023, 11(12), 480; https://doi.org/10.3390/inorganics11120480 - 14 Dec 2023

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Abstract

We explore the use of industrial sources of silicon and surfactant for obtaining low-cost MCM-41 materials and evaluate their performances as CO₂ adsorbents. All of them presented a high specific surface area with different structural characteristics and textural properties. Interestingly, the MCM-41 [...] Read more.

We explore the use of industrial sources of silicon and surfactant for obtaining low-cost MCM-41 materials and evaluate their performances as CO₂ adsorbents. All of them presented a high specific surface area with different structural characteristics and textural properties. Interestingly, the MCM-41 manufactured with the most economical reagents presented a S_BET of 1602 m²·g⁻¹. The template was removed by using thermal treatments in an air atmosphere or a washing process. Preservation of silanol groups proved to be more effective under washing or mild thermal treatment conditions with the advantage of their lower cost and environmental benefit. Surface reactivity against CO₂ was enhanced by anchoring APTS to silanol groups through wet grafting. All amino-functionalized materials showed a performance as CO₂ adsorbents comparable to those reported in the literature, reaching values close to 30 cm³·g⁻¹ at 25 °C and 760 mmHg. Samples with a higher concentration of silanol groups showed better performance. Our studies indicate that adsorbed CO₂ is retained at least up to 50 °C, and the CO₂ is chemisorbed on the silica modified with amine groups. The chemisorbed gas at very low pressures points to the potential use of these materials for CO₂ storage. Full article

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20 pages, 4281 KiB

Open AccessArticle

Combination of Multiple Operando and In-Situ Characterization Techniques in a Single Cluster System for Atomic Layer Deposition: Unraveling the Early Stages of Growth of Ultrathin Al₂O₃ Films on Metallic Ti Substrates

by Carlos Morales, Ali Mahmoodinezhad, Rudi Tschammer, Julia Kosto, Carlos Alvarado Chavarin, Markus Andreas Schubert, Christian Wenger, Karsten Henkel and Jan Ingo Flege

Inorganics 2023, 11(12), 477; https://doi.org/10.3390/inorganics11120477 - 14 Dec 2023

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Abstract

This work presents a new ultra-high vacuum cluster tool to perform systematic studies of the early growth stages of atomic layer deposited (ALD) ultrathin films following a surface science approach. By combining operando (spectroscopic ellipsometry and quadrupole mass spectrometry) and in situ (X-ray [...] Read more.

This work presents a new ultra-high vacuum cluster tool to perform systematic studies of the early growth stages of atomic layer deposited (ALD) ultrathin films following a surface science approach. By combining operando (spectroscopic ellipsometry and quadrupole mass spectrometry) and in situ (X-ray photoelectron spectroscopy) characterization techniques, the cluster allows us to follow the evolution of substrate, film, and reaction intermediates as a function of the total number of ALD cycles, as well as perform a constant diagnosis and evaluation of the ALD process, detecting possible malfunctions that could affect the growth, reproducibility, and conclusions derived from data analysis. The homemade ALD reactor allows the use of multiple precursors and oxidants and its operation under pump and flow-type modes. To illustrate our experimental approach, we revisit the well-known thermal ALD growth of Al₂O₃ using trimethylaluminum and water. We deeply discuss the role of the metallic Ti thin film substrate at room temperature and 200 °C, highlighting the differences between the heterodeposition (<10 cycles) and the homodeposition (>10 cycles) growth regimes at both conditions. This surface science approach will benefit our understanding of the ALD process, paving the way toward more efficient and controllable manufacturing processes. Full article

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15 pages, 2263 KiB

Open AccessArticle

Microwave-Mediated Synthesis and Characterization of Ca(OH)₂ Nanoparticles Destined for Geraniol Encapsulation

by Panagiota Tryfon, Nathalie N. Kamou, Stefanos Mourdikoudis, George Vourlias, Urania Menkissoglu-Spiroudi and Catherine Dendrinou-Samara

Inorganics 2023, 11(12), 470; https://doi.org/10.3390/inorganics11120470 - 02 Dec 2023

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Abstract

Nanotechnology presents promising opportunities for enhancing pest management strategies, particularly in protecting active ingredients to prolong their shelf life and effectiveness. Among different approaches, the combination of inorganic nanoparticles with active ingredients such as the main constituents of natural essential oils in one [...] Read more.

Nanotechnology presents promising opportunities for enhancing pest management strategies, particularly in protecting active ingredients to prolong their shelf life and effectiveness. Among different approaches, the combination of inorganic nanoparticles with active ingredients such as the main constituents of natural essential oils in one nanoarchitecture is challenging. In this study, hydrophobic calcium hydroxide nanoparticles coated with oleylamime [Ca(OH)₂@OAm NPs] were synthesized using microwave-assisted synthesis. These primary NPs were physicochemically characterized and subsequently utilized to prepare nanocapsules (NCs) either alone (Ca NCs) and/or in combination with geraniol at different ratios of Ca(OH)₂@OAm NPs and geraniol, i.e. 1:1 (CaGer1 NCs), 1:2 (CaGer2 NCs), and 1:3 (CaGer3 NCs), respectively. Among the formulations, the CaGer2 NCs demonstrated higher encapsulation efficiency (EE) and loading capacity (LC) of 95% and 20%, correspondingly. They exhibited a hydrodynamic size of 306 nm, a ζ-potential of −35 mV, and a monodisperse distribution. Release kinetics of geraniol from CaGer2 NCs indicated a pH-dependent slow release over 96 h at both 25 °C and 35 °C. In vitro antifungal assay against B. cinerea revealed a concentration-dependent activity, and the EC₅₀ values for Ca(OH)₂@OAm NPs, Ca NCs, and CaGer2 NCs were estimated to be 654 µg/mL, 395 µg/mL, and 507 µg/mL, respectively. These results underscore the potential of Ca-based nanoformulations to control plant pathogens, suggesting that while Ca NCs showcase potent antifungal attributes, the different architectures/structures play a critical role in the antifungal effectiveness of the nanoformulations that have to be explored further. Full article

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15 pages, 5332 KiB

Open AccessArticle

Gd₂O₃ Doped UO₂(s) Corrosion in the Presence of Silicate and Calcium under Alkaline Conditions

by Sonia García-Gómez, Javier Giménez, Ignasi Casas, Jordi Llorca and Joan De Pablo

Inorganics 2023, 11(12), 469; https://doi.org/10.3390/inorganics11120469 - 01 Dec 2023

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Abstract

The anodic reactivity of UO₂ and UO₂ doped with Gd₂O₃ was investigated by electrochemical methods in slightly alkaline conditions in the presence of silicate and calcium. At the end of the experiments, the electrodes were analysed by X-ray [...] Read more.

The anodic reactivity of UO₂ and UO₂ doped with Gd₂O₃ was investigated by electrochemical methods in slightly alkaline conditions in the presence of silicate and calcium. At the end of the experiments, the electrodes were analysed by X-ray photoelectron spectroscopy to determine the oxidation state of the uranium on the surface. The experiments showed that the increase in gadolinia doping level led to a reduction in the reactivity of UO₂, this effect being more marked at the highest doping level studied (10 wt.% Gd₂O₃). This behaviour could be attributed to the formation of dopant-vacancy clusters (Gd^III-Ov), which could limit the accommodation of excess O²⁻ into the UO₂ lattice. In addition, the presence of Ca²⁺ and SiO₃²⁻ decreased the anodic dissolution of UO₂. In summary, the Gd₂O₃ doping in presence of silicate and calcium was found to strongly decrease the oxidative dissolution of UO₂, which is a beneficial situation regarding the long-term management of spent nuclear fuel in a repository. Full article

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14 pages, 1995 KiB

Open AccessArticle

Photocatalytic Degradation of Emerging Contaminants with N-Doped TiO₂ Using Simulated Sunlight in Real Water Matrices

by Elisa Gaggero, Arianna Giovagnoni, Alessia Zollo, Paola Calza and Maria Cristina Paganini

Inorganics 2023, 11(11), 439; https://doi.org/10.3390/inorganics11110439 - 17 Nov 2023

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Abstract

In the present work, the photodegradation performances of N-doped TiO₂ photocatalysts with enhanced absorption of visible light were exploited for the abatement of some representative contaminants of emerging concern (CECs). Pristine TiO₂ and N-TiO₂ were synthesized using hydrothermal (HT) and [...] Read more.

In the present work, the photodegradation performances of N-doped TiO₂ photocatalysts with enhanced absorption of visible light were exploited for the abatement of some representative contaminants of emerging concern (CECs). Pristine TiO₂ and N-TiO₂ were synthesized using hydrothermal (HT) and sol–gel (SG) routes, they were characterized using XRD and UV-Vis spectroscopy, and their band gaps were determined via analysis in diffuse reflectance. Their photodegradation efficiency was tested on a mixture of recalcitrant organic pollutants, namely, benzotriazole, diclofenac, sulfamethoxazole, and bisphenol A, using a solar simulator lamp with two different cut-off filters (λ > 340 nm and λ > 400 nm). The evaluation of the photocatalytic performances was initially carried out in spiked ultrapure water and subsequently in aqueous matrices of increasing complexity such as Po River water and water coming from an aquaculture plant. The exclusive utilization of visible light (λ > 400 nm) highlighted the advantage of introducing the dopant into the TiO₂ photocatalyst since this modification allows for the material to be responsive to visible light, which is not sufficient in the case of pristine TiO₂ and the higher efficiency of materials obtained via the sol–gel route. Thanks to the doping, improved performance was obtained in both ultrapure water and real water matrices, indicating the potential of the doped material for future applications in the field. Full article

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12 pages, 2430 KiB

Open AccessArticle

Incorporation of Antimony Ions in Heptaisobutyl Polyhedral Oligomeric Silsesquioxanes

by Stefano Marchesi, Chiara Bisio, Fabio Carniato and Enrico Boccaleri

Inorganics 2023, 11(11), 426; https://doi.org/10.3390/inorganics11110426 - 30 Oct 2023

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Abstract

The direct incorporation of Sb(V) ions into a polycondensed silsesquioxane network based on heptaisobutyl POSS units (Sb(V)-POSSs) through a corner-capping reaction is reported for the first time in this work. As a reference sample, a completely condensed monomeric Sb(III)-POSS was prepared using a [...] Read more.

The direct incorporation of Sb(V) ions into a polycondensed silsesquioxane network based on heptaisobutyl POSS units (Sb(V)-POSSs) through a corner-capping reaction is reported for the first time in this work. As a reference sample, a completely condensed monomeric Sb(III)-POSS was prepared using a similar synthetic protocol. The chemical properties of both Sb-containing POSSs were investigated with different analytical and spectroscopic techniques. The analyses confirm the success of the corner-capping reaction for both samples and indicate that an Sb(V)-POSS sample is characterized by a heterogenous multimeric arrangement with an irregular organization of POSS cages linked to Sb(V) centers, and has a more complex structure with respect to the well-defined monomeric Sb(III)-POSS. Full article

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15 pages, 865 KiB

Open AccessArticle

Hydrazine Oxidation in Aqueous Solutions I: N₄H₆ Decomposition

by Martin Breza and Alena Manova

Inorganics 2023, 11(10), 413; https://doi.org/10.3390/inorganics11100413 - 18 Oct 2023

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Abstract

A mixture of nonlabeled (¹⁴N₂H₄) and ¹⁵N labeled hydrazine (¹⁵N₂H₄) in an aqueous solution is oxidized to ¹⁵N₂, ¹⁴N₂, and ¹⁴N¹⁵N [...] Read more.

A mixture of nonlabeled (¹⁴N₂H₄) and ¹⁵N labeled hydrazine (¹⁵N₂H₄) in an aqueous solution is oxidized to ¹⁵N₂, ¹⁴N₂, and ¹⁴N¹⁵N molecules, indicating the intermediate existence of the ¹⁴NH₂-¹⁴NH-¹⁵NH-¹⁵NH₂ with subsequent hydrogen transfers and splitting of side N-N bonds. The structures, thermodynamics and electron characteristics of various N₄H₆ molecules in aqueous solutions are investigated using theoretical treatment at the CCSD/cc-pVTZ level of theory to explain the crucial part of the hydrazine oxidation reaction. Most N₄H₆ structures in aqueous solutions are decomposed during geometry optimization. Splitting the bond between central nitrogen atoms is the most frequent method, but the breakaway of the side nitrogen is energetically the most preferred one. The N-N fissions are enabled by suitable hydrogen rearrangements. Gibbs free energy data indicate the dominant abundance of NH₃... N₂... NH₃ species. The side N atoms have very high negative charges, which should support hydrogen transfers in aqueous solutions. The only stable cyclo-(NH)₄…H₂ structure has a Gibbs energy that is too high and breaks the H₂ molecule. The remaining initial cyclic structures are split into hydrazine and HN≡NH or H₂N≡N species, and their relative abundance in aqueous solutions is vanishing. Full article

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11 pages, 3672 KiB

Open AccessArticle

Synthesis of Polystyrene@TiO₂ Core–Shell Particles and Their Photocatalytic Activity for the Decomposition of Methylene Blue

by Naoki Toyama, Tatsuya Takahashi, Norifumi Terui and Shigeki Furukawa

Inorganics 2023, 11(8), 343; https://doi.org/10.3390/inorganics11080343 - 21 Aug 2023

Cited by 1 | Viewed by 1003

Abstract

In this study, we investigated the preparation conditions of polystyrene (PS)@TiO₂ core–shell particles and their photocatalytic activity during the decomposition of methylene blue (MB). TiO₂ shells were formed on the surfaces of PS particles using the sol–gel method. Homogeneous PS@TiO₂ [...] Read more.

In this study, we investigated the preparation conditions of polystyrene (PS)@TiO₂ core–shell particles and their photocatalytic activity during the decomposition of methylene blue (MB). TiO₂ shells were formed on the surfaces of PS particles using the sol–gel method. Homogeneous PS@TiO₂ core–shell particles were obtained using an aqueous NH₃ solution as the promoter of the sol–gel reaction and stirred at room temperature. This investigation revealed that the temperature and amount of the sol–gel reaction promoter influenced the morphology of the PS@TiO₂ core–shell particles. The TiO₂ shell thickness of the PS@TiO₂ core–shell particles was approximately 5 nm, as observed using transmission electron microscopy. Additionally, Ti elements were detected on the surfaces of the PS@TiO₂ core–shell particles using energy-dispersive X-ray spectroscopy analysis. The PS@TiO₂ core–shell particles were used in MB decomposition to evaluate their photocatalytic activities. For comparison, we utilized commercial P25 and TiO₂ particles prepared using the sol–gel method. The results showed that the PS@TiO₂ core–shell particles exhibited higher activity than that of the compared samples. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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16 pages, 3423 KiB

Open AccessArticle

Hydrogen Incorporation in Ru_xTi_1−xO₂ Mixed Oxides Promotes Total Oxidation of Propane

by Wei Wang, Yu Wang, Phillip Timmer, Alexander Spriewald-Luciano, Tim Weber, Lorena Glatthaar, Yun Guo, Bernd M. Smarsly and Herbert Over

Inorganics 2023, 11(8), 330; https://doi.org/10.3390/inorganics11080330 - 07 Aug 2023

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Abstract

A rational synthetic approach is introduced to enable hydrogen insertion into oxides by forming a solid solution of a reducible oxide with a less reducible oxide as exemplified with RuO₂ and TiO₂ (Ru_x, a mixture of x% RuO₂ with (100−x)% [...] Read more.

A rational synthetic approach is introduced to enable hydrogen insertion into oxides by forming a solid solution of a reducible oxide with a less reducible oxide as exemplified with RuO₂ and TiO₂ (Ru_x, a mixture of x% RuO₂ with (100−x)% TiO₂). Hydrogen exposure at 250 °C to Ru_x (Ru_x_250R) results in substantial hydrogen incorporation accompanied by lattice strain that in turn induces pronounced activity variations. Here, we demonstrate that hydrogen incorporation in mixed oxides promotes the oxidation catalysis of propane combustion with Ru_60_250R being the catalytically most active catalyst. Full article

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11 pages, 3975 KiB

Open AccessCommunication

Binder-Free CoMn₂O₄ Nanoflower Particles/Graphene/Carbon Nanotube Composite Film for a High-Performance Lithium-Ion Battery

by Xin Tong, Bo Yang, Fei Li, Manqi Gu, Xinxing Zhan, Juan Tian, Shengyun Huang and Gang Wang

Inorganics 2023, 11(8), 314; https://doi.org/10.3390/inorganics11080314 - 25 Jul 2023

Cited by 1 | Viewed by 951

Abstract

Manganese-based bimetallic oxides show a high theoretical specific capacity, making them a potential next-generation lithium-ion battery anode material. However, as with metal oxide anode materials, aggregation, volume expansion, and poor conductivity are the main obstacles. In this manuscript, flexible CoMn₂O₄ [...] Read more.

Manganese-based bimetallic oxides show a high theoretical specific capacity, making them a potential next-generation lithium-ion battery anode material. However, as with metal oxide anode materials, aggregation, volume expansion, and poor conductivity are the main obstacles. In this manuscript, flexible CoMn₂O₄/graphene/carbon nanotube films were successfully prepared through a facile filtration strategy and a subsequent thermal treatment process. When used as anodes for lithium batteries, these films can be pressed onto nickel foam without other conductive additives and binders, which simplifies the manufacturing process. When used as an anode in the lithium-ion battery, CoMn₂O₄/GR/CNT film exhibits a high discharge capacity of 881 mAh g⁻¹ after 55 cycles. This value is ~2 times higher than the discharge capacity of CoMn₂O₄. The three-dimensional GR/CNT carrier effectively dispersed CoMn₂O₄, preventing its aggregation and alleviating the problem of volume expansion. Full article

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18 pages, 6285 KiB

Open AccessArticle

The Mechanical Properties of Geopolymers from Different Raw Materials and the Effect of Recycled Gypsum

by Henna Korhonen, Juha Timonen, Sari Suvanto, Pipsa Hirva, Kirsi Mononen and Sirpa Jääskeläinen

Inorganics 2023, 11(7), 298; https://doi.org/10.3390/inorganics11070298 - 14 Jul 2023

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Abstract

Geopolymers are amorphous inorganic polymers that are mainly used in the construction industry as an environmentally friendly alternative to ordinary cement. This study compared selected mechanical properties (setting time, shrinkage, strength) of geopolymer specimens made from different main raw materials, mainly at room [...] Read more.

Geopolymers are amorphous inorganic polymers that are mainly used in the construction industry as an environmentally friendly alternative to ordinary cement. This study compared selected mechanical properties (setting time, shrinkage, strength) of geopolymer specimens made from different main raw materials, mainly at room temperature, and investigated the effects of recycled gypsum on these. A structural analysis of the specimens was conducted with XRD and SEM. Also, the leaching of aluminium, silicon, and calcium from the specimens was investigated. According to this study, raw materials have a significant impact on the properties of geopolymers. Recycled gypsum affected the setting time of the geopolymers, but the effect was not the same for all specimens. It increased the setting time of specimens made from calcium-rich raw materials, for example, and the ground-granulated blast furnace slag specimens hardened as fast as ordinary Portland cement (about 300 min), but the addition of gypsum decreased it to 1300 min. Gypsum-containing specimens, based on Ca-deficient metakaolin or fly ash, hardened even faster than OPC, in 100–150 min. Recycled gypsum significantly reduced the plastic shrinkage of most of the 28 d specimens to lower values than those achieved for OPC (0.07%). The only exceptions were the fly-ash-based specimens. However, gypsum had no effect on the drying shrinkage, which accounted for a larger proportion of the total shrinkage in most specimens. Therefore, it had no significant effect on the total shrinkage of the geopolymer specimens. The reducing effect of gypsum on the plastic shrinkage of geopolymers was attributed to ettringite, which was observed in all gypsum-containing specimens analysed with XRD. In this study, recycled gypsum decreased the compressive strength of the specimens, which could be prevented by using a finer gypsum powder. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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13 pages, 2183 KiB

Open AccessArticle

Method for Decontamination of Toxic Aluminochrome Catalyst Sludge by Reduction of Hexavalent Chromium

by Igor Pyagay, Olga Zubkova, Margarita Zubakina and Viktor Sizyakov

Inorganics 2023, 11(7), 284; https://doi.org/10.3390/inorganics11070284 - 30 Jun 2023

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Abstract

The article is devoted to the neutralization of the harmful effects of aluminochrome catalyst sludge. Catalyst sludge is a waste product from petrochemical production and poses a serious threat to the environment and humans because of the toxic hexavalent chromium it contains. The [...] Read more.

The article is devoted to the neutralization of the harmful effects of aluminochrome catalyst sludge. Catalyst sludge is a waste product from petrochemical production and poses a serious threat to the environment and humans because of the toxic hexavalent chromium it contains. The emissions of Russian petrochemical enterprises’ alumochrome sludge is 10,000–12,000 tons per year. In this paper, research related to the possibility of reducing the harmful effects of sludge by converting hexavalent chromium to a less dangerous trivalent state is presented. The reduction of hexavalent chromium was carried out with different reagents: Na₂SO₃, FeSO₄, Na₂S₂O₃, and Na₂S₂O₅. Then, a comparative analysis was carried out, and sodium metabisulfite was chosen as the most preferred reagent. The peculiarity of the reducing method was carrying out the reaction in a neutral medium, pH = 7.0. The reduction was carried out in the temperature range of 60–85 °C and under standard conditions. The maximum recovery efficiency of chromium from the catalyst sludge (100%) was achieved at 85 °C and 10 min. This method did not involve the use of concentrated sulfuric acid, as in a number of common techniques, or additional reagents for the precipitation of chromium in the form of hydroxide. Full article

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12 pages, 1133 KiB

Open AccessArticle

Superoxide Radical Formed on the TiO₂ Surface Produced from Ti(OiPr)₄ Exposed to H₂O₂/KOH

by Rimma I. Samoilova and Sergei A. Dikanov

Inorganics 2023, 11(7), 274; https://doi.org/10.3390/inorganics11070274 - 27 Jun 2023

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Abstract

In this study, the superoxide radical O₂^•− formed by treating Ti(OR)₄ (R = iPr, nBu) with H₂O₂ in the presence of KOH was detected in the EPR spectra. The g-tensor of this radical differs from the typical [...] Read more.

In this study, the superoxide radical O₂^•− formed by treating Ti(OR)₄ (R = iPr, nBu) with H₂O₂ in the presence of KOH was detected in the EPR spectra. The g-tensor of this radical differs from the typical values reported for a superoxide on various TiO₂ surfaces. On the other hand, similar g-tensor components g_||(zz = 2.10 ± 0.01, g_⊥ = 2.005 ± 0.003 assigned to the O₂^•− were previously observed for radicals in aqueous solutions in the presence of K₂O, alkaline solutions of DMSO, and water/DMSO mixtures. A common factor in all these systems is the presence of alkali ions. However, there was no structural support for the possible interaction of alkali ions with a superoxide in these systems. The use of multifrequency pulsed EPR techniques in this work revealed the stabilization of the O₂^•− near the K⁺ ion and its involvement in a strong hydrogen bond with the surface. These findings are consistent with the features previously reported for superoxides on a Na pre-covered MgO surface. Interactions with a closely located ²³Na and a strongly coupled ¹H proton were also seen in the HYSCORE spectra but assigned to two different superoxides with various g_zz values presented in the sample. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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12 pages, 1520 KiB

Open AccessArticle

Basalt-Fiber-Reinforced Phosphorus Building Gypsum Composite Materials (BRPGCs): An Analysis on Their Working Performance and Mechanical Properties

by Lei Wu, Zhong Tao, Ronggui Huang, Zhiqi Zhang, Jinjin Shen and Weijie Xu

Inorganics 2023, 11(6), 254; https://doi.org/10.3390/inorganics11060254 - 09 Jun 2023

Viewed by 934

Abstract

The preparation of fiber-reinforced phosphorus building gypsum composite materials (FRPGCs) is an important approach to enlarge the utilization of phosphogypsum resources. Through reinforcing phosphorus building gypsum (PBG) with basalt fiber (BF), this article probes into the effects of the length and fiber content [...] Read more.

The preparation of fiber-reinforced phosphorus building gypsum composite materials (FRPGCs) is an important approach to enlarge the utilization of phosphogypsum resources. Through reinforcing phosphorus building gypsum (PBG) with basalt fiber (BF), this article probes into the effects of the length and fiber content of BF on the working performance and mechanical properties of basalt-fiber-reinforced phosphorus building gypsum composite materials (BRPGCs) and accesses the toughness of BRPGCs under bending loads using residual strength. The results showed that the addition of BF could significantly promote the mechanical properties of BRPGCs. However, due to the adverse effect of fibers on the working performance of BRPGCs, the fiber content was constrained. After adding 1.2% of 6 mm BF, the bending strength and compressive strength of FRPGCs reached maximum values of 10.98 MPa and 29.83 MPa, respectively. Under a bending load, BRPGCs exhibited an apparent ductile behavior. The P-δ curve presented five stages, with an evident phase of strength stability after cracking. A larger fiber content was conducive to the toughness of BRPGCs. When 1.6% of 6 mm BF was added, the residual strength of FRPGCs could reach 6.77 MPa. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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11 pages, 4029 KiB

Open AccessArticle

Hydrogen Storage Properties of Economical Graphene Materials Modified by Non-Precious Metal Nickel and Low-Content Palladium

by Yiwen Chen, Habibullah, Guanghui Xia, Chaonan Jin, Yao Wang, Yigang Yan, Yungui Chen, Xiufang Gong, Yuqiu Lai and Chaoling Wu

Inorganics 2023, 11(6), 251; https://doi.org/10.3390/inorganics11060251 - 08 Jun 2023

Cited by 3 | Viewed by 1764

Abstract

Ni/Pd co-modified graphene hydrogen storage materials were successfully prepared by a solvothermal method using NiCl₂·6H₂O and Pd(OAc)₂ and reduced graphene oxide (rGO). By adjusting the hydrothermal temperature, Pd–Ni is successfully alloyed, and the size of the obtained nanoparticles [...] Read more.

Ni/Pd co-modified graphene hydrogen storage materials were successfully prepared by a solvothermal method using NiCl₂·6H₂O and Pd(OAc)₂ and reduced graphene oxide (rGO). By adjusting the hydrothermal temperature, Pd–Ni is successfully alloyed, and the size of the obtained nanoparticles is uniform. The electronic structure of Pd was changed by alloying, and the center of the D-band moved down, which promoted the adsorption of hydrogen. The NiPd-rGO-180 sample, in which 180 represents the solvothermal temperature in centigrade (°C), has the highest hydrogen storage capacity of 2.65 wt% at a moderate condition (RT/4MPa). The excellent hydrogen storage performance benefits from the synergistic hydrogen spillover effect of Pd–Ni bimetal. The calculated hydrogen adsorption energies of Ni₂Pd₂-rGO are within the ideal range (−0.20 to −0.60 eV) of hydrogen ads/desorption; however, the introduction of substrate defects and the cluster orientation alter the hydrogen adsorption energy. This work provides an effective reference for the design and optimization of carbon-based hydrogen storage materials. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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11 pages, 12876 KiB

Open AccessArticle

Continuous and Intermittent Planetary Ball Milling Effects on the Alloying of a Bismuth Antimony Telluride Powder Mixture

by Georgios Samourgkanidis and Theodora Kyratsi

Inorganics 2023, 11(5), 221; https://doi.org/10.3390/inorganics11050221 - 20 May 2023

Cited by 2 | Viewed by 1177

Abstract

This study investigates the effects of continuous and in-steps mechanical alloying of a bismuth antimony telluride powder mixture (Bi

_{0.4}

Sb

_{1.6}

Te

_{3.0}

) via the mechanical planetary ball milling (PBM) process as a function of milling time and powder mixture amount. [...] Read more.

This study investigates the effects of continuous and in-steps mechanical alloying of a bismuth antimony telluride powder mixture (Bi

_{0.4}

Sb

_{1.6}

Te

_{3.0}

) via the mechanical planetary ball milling (PBM) process as a function of milling time and powder mixture amount. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the phase, composition, and morphology of the alloy. The alloyed powder with the optimum PBM conditions was then hot pressed (HP), and its thermoelectric properties were further investigated. The results on the alloying of the powder mixture showed that due to the high agglomeration tendency of BST during the PBM process, a significant deviation occurs in the development of a single-phase state over time when the powder mixture is milled continuously and in-steps. ’In-steps’ refers to the procedure of interrupting the PBM process and detaching the agglomerated powder adhering to the inner walls of the vessel. This task was repeated every hour and a half of the PBM process for a total of 12 h, and the results were compared with those of the 12 h continuous PBM process of the same mixture. In addition, the procedure was repeated with different amounts of mixture (100 g and 150 g) to determine the most efficient method of producing the material as a function of time. As for the thermoelectric profile of the powder, the data showed results in direct agreement with those in the literature. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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17 pages, 6317 KiB

Open AccessArticle

Tetragonal Nanosized Zirconia: Hydrothermal Synthesis and Its Performance as a Promising Ceramic Reinforcement

by Shikai Liu, Jialin Wang, Yingxin Chen, Zhijian Song, Bibo Han, Haocheng Wu, Taihang Zhang and Meng Liu

Inorganics 2023, 11(5), 217; https://doi.org/10.3390/inorganics11050217 - 17 May 2023

Cited by 4 | Viewed by 1171

Abstract

In this study, we produced zirconia nanoparticles with a pure tetragonal phase, good dispersion, and an average particle size of approximately 7.3 nm using the modified hydrothermal method. Zirconium oxychloride (ZrOCl₂-8H₂O) was used as zirconium source, while propanetriol was [...] Read more.

In this study, we produced zirconia nanoparticles with a pure tetragonal phase, good dispersion, and an average particle size of approximately 7.3 nm using the modified hydrothermal method. Zirconium oxychloride (ZrOCl₂-8H₂O) was used as zirconium source, while propanetriol was used as an additive. The influence of propanetriol content, sonication time, hydrothermal temperature, and type of dispersant on the physical phase and dispersibility of zirconia nanoparticles was investigated. Monoclinic zirconia was found to completely transform into a tetragonal structure when the mass fraction of glycerol was increased to 5 wt%. With the increase in the mechanical stirring time under ultrasonic conditions, the size distribution range of the prepared particles became narrower and then wider, and the particle size became first smaller and then larger. Ultrasonic and mechanical stirring for 5 min had the best effect. When comparing the effects of different dispersants (PEG8000, PVP, and CTAB), it was found that the average particle size of zirconia nanoparticles prepared with 0.5 wt% PVP was the smallest. Furthermore, by adding different concentrations of pure tetragonal phase nanozirconia to 3Y-ZrO₂ as reinforcement additives, the bending strength of the prepared ceramics increased first and then decreased with increasing addition amounts. When the amount of addition was 1 wt% and the ceramic was calcined at 1600 °C, the flexural strength of the ceramic increased significantly, which was about 1.6 times that of the unadded ceramic. The results are expected to provide a reference for the reinforcement of high-purity zirconia ceramics. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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10 pages, 2550 KiB

Open AccessArticle

Enhanced Thermal Stability of Sputtered TiN Thin Films for Their Applications as Diffusion Barriers against Copper Interconnect

by Abdullah Aljaafari, Faheem Ahmed, Nagih M. Shaalan, Shalendra Kumar and Abdullah Alsulami

Inorganics 2023, 11(5), 204; https://doi.org/10.3390/inorganics11050204 - 09 May 2023

Cited by 1 | Viewed by 1629

Abstract

In this work, the deposition of titanium nitride (TiN) thin film using direct current (DC) sputtering technique and its application as diffusion barriers against copper interconnect was presented. The deposited film was analyzed by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), [...] Read more.

In this work, the deposition of titanium nitride (TiN) thin film using direct current (DC) sputtering technique and its application as diffusion barriers against copper interconnect was presented. The deposited film was analyzed by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS) techniques. XRD patterns showed the face-centered cubic (FCC) structure for the TiN/SiO₂/Si film, having (111) and (200) peaks and TiN (111), Cu(111), and Cu(200) peaks for Cu/TiN/SiO₂/Si film. FESEM images revealed that the grains were homogeneously dispersed on the surface of the TiN film, having a finite size. XPS study showed that Ti2p doublet with peaks centered at 455.1 eV and 461.0 eV for TiN film was observed. Furthermore, the stoichiometry of the deposited TiN film was found to be 0.98. The sheet resistance of the TiN film was analyzed by using a four-point probe method, and the resistivity was calculated to be 11 μΩ cm. For the utilization, TiN film were tested for diffusion barrier performance against Cu interconnect. The results exhibited that TiN film has excellent performance in diffusion barrier for copper metallization up to a temperature of 700 °C. However, at a higher annealing temperature of 800 °C, the formation of Cu₃Si and TiSi₂ compounds were evident. Thus, stoichiometric TiN film with high thermal stability and low resistivity produced in this study could be applied for the fabrication of microelectronic devices. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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Review

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16 pages, 728 KiB

Open AccessReview

Emerging Nanomaterials Biosensors in Breathalyzers for Detection of COVID-19: Future Prospects

by Saravanan Rajendrasozhan, Subuhi Sherwani, Faheem Ahmed, Nagih Shaalan, Abdulmohsen Alsukaibi, Khalid Al-Motair and Mohd Wajid Ali Khan

Inorganics 2023, 11(12), 483; https://doi.org/10.3390/inorganics11120483 - 18 Dec 2023

Cited by 1 | Viewed by 1418

Abstract

In recent times, the global landscape of disease detection and monitoring has been profoundly influenced by the convergence of nanotechnology and biosensing techniques. Biosensors have enormous potential to monitor human health, with flexible or wearable variants, through monitoring of biomarkers in clinical and [...] Read more.

In recent times, the global landscape of disease detection and monitoring has been profoundly influenced by the convergence of nanotechnology and biosensing techniques. Biosensors have enormous potential to monitor human health, with flexible or wearable variants, through monitoring of biomarkers in clinical and biological behaviors and applications related to health and disease, with increasing biorecognition, sensitivity, selectivity, and accuracy. The emergence of nanomaterial-based biosensors has ushered in a new era of rapid and sensitive diagnostic tools, offering unparalleled capabilities in the realm of disease identification. Even after the declaration of the end of the COVID-19 pandemic, the demand for efficient and accessible diagnostic methodologies has grown exponentially. In response, the integration of nanomaterial biosensors into breathalyzer devices has gained considerable attention as a promising avenue for low-cost, non-invasive, and early detection of COVID-19. This review delves into the forefront of scientific advancements, exploring the potential of emerging nanomaterial biosensors within breathalyzers to revolutionize the landscape of COVID-19 detection, providing a comprehensive overview of their principles, applications, and implications. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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41 pages, 12406 KiB

Open AccessReview

Integration of CO₂ Capture and Conversion by Employing Metal Oxides as Dual Function Materials: Recent Development and Future Outlook

by Wei Jie Tan and Poernomo Gunawan

Inorganics 2023, 11(12), 464; https://doi.org/10.3390/inorganics11120464 - 30 Nov 2023

Viewed by 1582

Abstract

To mitigate the effect of CO₂ on climate change, significant efforts have been made in the past few decades to capture CO₂, which can then be further sequestered or converted into value-added compounds, such as methanol and hydrocarbons, by using [...] Read more.

To mitigate the effect of CO₂ on climate change, significant efforts have been made in the past few decades to capture CO₂, which can then be further sequestered or converted into value-added compounds, such as methanol and hydrocarbons, by using thermochemical or electrocatalytic processes. However, CO₂ capture and conversion have primarily been studied independently, resulting in individual processes that are highly energy-intensive and less economically viable due to high capital and operation costs. To enhance the overall process efficiency, integrating CO₂ capture and conversion into a single system offers an opportunity for a more streamlined process that can reduce energy and capital costs. This strategy can be achieved by employing dual function materials (DFMs), which possess the unique capability to simultaneously adsorb and convert CO₂. These materials combine basic metal oxides with active metal catalytic sites that enable both sorption and conversion functions. In this review paper, we focus on the recent strategies that utilize mixed metal oxides as DFMs. Their material design and characteristics, reaction mechanisms, as well as performance and limitations will be discussed. We will also address the challenges associated with this integrated system and attempt to provide insights for future research endeavors. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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55 pages, 2623 KiB

Open AccessReview

How to Address Flame-Retardant Technology on Cotton Fabrics by Using Functional Inorganic Sol–Gel Precursors and Nanofillers: Flammability Insights, Research Advances, and Sustainability Challenges

by Valentina Trovato, Silvia Sfameni, Rim Ben Debabis, Giulia Rando, Giuseppe Rosace, Giulio Malucelli and Maria Rosaria Plutino

Inorganics 2023, 11(7), 306; https://doi.org/10.3390/inorganics11070306 - 18 Jul 2023

Cited by 1 | Viewed by 2575

Abstract

Over the past decade, inorganic fillers and sol–gel-based flame-retardant technologies for textile treatments have gained increasing research interest as useful alternatives to hazardous chemicals previously employed in textile coating and finishing. This review presents the current state of the art of inorganic flame-retardant [...] Read more.

Over the past decade, inorganic fillers and sol–gel-based flame-retardant technologies for textile treatments have gained increasing research interest as useful alternatives to hazardous chemicals previously employed in textile coating and finishing. This review presents the current state of the art of inorganic flame-retardant technology for cotton fabrics to scientists and researchers. Combustion mechanism and flammability, as well as the thermal behavior of neat cotton samples, are first introduced. The main section is focused on assessing the effect of inorganic and sol–gel-based systems on the final flame-retardant properties of cotton fabrics, emphasizing their fire safety characteristics. When compared to organic flame-retardant solutions, inorganic functional fillers have been shown to be more environmentally friendly and pollution-free since they do not emit compounds that are hazardous to ecosystems and humans when burned. Finally, some perspectives and recent advanced research addressing the potential synergism derived from the use of inorganic flame retardants with other environmentally suitable molecules toward a sustainable flame-retardant technological approach are reviewed. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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22 pages, 3297 KiB

Open AccessReview

Nanomaterials Used in the Preparation of Personal Protective Equipment (PPE) in the Fight against SARS-CoV-2

by Pierantonio De Luca, Janos B.Nagy and Anastasia Macario

Inorganics 2023, 11(7), 294; https://doi.org/10.3390/inorganics11070294 - 12 Jul 2023

Cited by 1 | Viewed by 1536

Abstract

Following the well-known pandemic, declared on 30 January 2020 by the World Health Organization, the request for new global strategies for the prevention and mitigation of the spread of the infection has come to the attention of the scientific community. Nanotechnology has often [...] Read more.

Following the well-known pandemic, declared on 30 January 2020 by the World Health Organization, the request for new global strategies for the prevention and mitigation of the spread of the infection has come to the attention of the scientific community. Nanotechnology has often managed to provide solutions, effective responses, and valid strategies to support the fight against SARS-CoV-2. This work reports a collection of information on nanomaterials that have been used to counter the spread of the SARS-CoV-2 virus. In particular, the objective of this work was to illustrate the strategies that have made it possible to use the particular properties of nanomaterials, for the production of personal protective equipment (DIP) for the defense against the SARS-CoV-2 virus. Full article

(This article belongs to the Special Issue 10th Anniversary of Inorganics: Inorganic Materials)

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