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Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods...
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Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II)

A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Inorganic Crystalline Materials".

Deadline for manuscript submissions: closed (31 December 2022) | Viewed by 38725

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editors

Dr. Aleksej Zarkov

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Guest Editor
Institute of Chemistry, Faculty of Chemistry and Geosciences, Vilnius University, Naugarduko 24, LT-03225 Vilnius, Lithuania
Interests: functional inorganic materials; mixed metal oxides; inorganic biomaterials; nanomaterials; thin films; ceramics
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Aivaras Kareiva

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Guest Editor
Institute of Chemistry, Vilnius University, LT-03225 Vilnius, Lithuania
Interests: multifunctional metal oxides; catalysts; microstructure; physical properties; nanoparticles; nanoclusters; nanocomposites; solid-state chemistry
Special Issues, Collections and Topics in MDPI journals
Dr. Loreta Tamasauskaite-Tamasiunaite

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Guest Editor
Department of Catalysis, Center for Physical Sciences and Technology, Saulėtekio Ave. 3, Vilnius, Lithuania
Interests: nanoparticles; composites; metals; multifunctional materials; catalysts; fuel cells
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Functional inorganic materials are an indispensable part of innovative technologies, which are essential to the development of many fields of industry. The use of new materials, nanostructures, or multicomponent composites with specific chemical or physical properties promotes technological progress in electronics, optoelectronics, catalysis, biomedicine, and many other areas that are concerned with plenty of aspects of human life. Due to the broad and diverse range of potential applications of functional inorganic materials, the development of superior synthesis pathways, reliable characterization, and a deep understanding of the structure–property relationships in materials are rightfully considered to be fundamentally important scientific issues. Only synergetic efforts of scientists dealing with the synthesis, functionalization, and characterization of materials will lead to the development of future technologies.

The scope of this Special Issue of Crystals, entitled “Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volumn II)”, includes but is not limited to the preparation routes, characterization, and application of functional inorganic materials, as well as hybrid materials that are important in the fields of electronics, optics, and biomedicine, among others. We would like to invite you to submit your work in the form of an original research article or a review paper related to the investigation of bulk materials, nanomaterials, or thin films.

Dr. Aleksej Zarkov
Dr. Aivaras Kareiva
Dr. Loreta Tamasauskaite-Tamasiunaite
Guest Editors

Manuscript Submission Information

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

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2100 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • multifunctional materials
  • magnetic materials
  • ferroelectric materials
  • piezoelectric materials
  • optical materials
  • processing routes
  • ceramics

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Editorial

Jump to: Research

4 pages, 184 KiB  
Editorial
Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II)
by Aleksej Zarkov, Aivaras Kareiva and Loreta Tamasauskaite-Tamasiunaite
Crystals 2023, 13(2), 324; https://doi.org/10.3390/cryst13020324 - 15 Feb 2023
Cited by 1 | Viewed by 1294
Abstract
Functional inorganic materials are an indispensable part of innovative technologies, which are essential for development in many fields of industry [...] Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))

Research

Jump to: Editorial

11 pages, 3393 KiB  
Article
Solvothermal Synthesis of Calcium Hydroxyapatite via Hydrolysis of Alpha-Tricalcium Phosphate in the Presence of Different Organic Additives
by Rasa Karalkeviciene, Eva Raudonyte-Svirbutaviciene, Aleksej Zarkov, Jen-Chang Yang, Anatoli I. Popov and Aivaras Kareiva
Crystals 2023, 13(2), 265; https://doi.org/10.3390/cryst13020265 - 3 Feb 2023
Cited by 13 | Viewed by 2312
Abstract
In this study, the effects of sodium lauryl sulfate and various amino acids (DL-aspartic acid, dodecanedioic acid, and suberic acid) on the formation of calcium-deficient hydroxyapatite via hydrolysis of α-tricalcium phosphate (α-TCP) were investigated; moreover, a combined effect of these additives and ethylene [...] Read more.
In this study, the effects of sodium lauryl sulfate and various amino acids (DL-aspartic acid, dodecanedioic acid, and suberic acid) on the formation of calcium-deficient hydroxyapatite via hydrolysis of α-tricalcium phosphate (α-TCP) were investigated; moreover, a combined effect of these additives and ethylene glycol as a synthesis medium was also estimated. The hydrolysis reaction was performed in solutions containing different concentrations of additives in aqueous and mixed aqueous–organic media under solvothermal conditions. It was demonstrated that the nature and the concentration of organic additives influence the phase purity and morphology of the final product. Higher concentrations of sodium lauryl sulfate and dodecanedioic acid induced the formation of impurities in addition to hydroxyapatite, while aspartic and suberic acid did not affect the phase purity. The morphology of the samples varied from plate- to rod-like depending on the concentrations of specific organic additive. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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15 pages, 5313 KiB  
Article
Synthetic Conditions for Obtaining Different Types of Amine-Holding Silica Particles and Their Sorption Behavior
by Inna Melnyk, Veronika Tomina and Nataliya Stolyarchuk
Crystals 2023, 13(2), 190; https://doi.org/10.3390/cryst13020190 - 21 Jan 2023
Cited by 2 | Viewed by 2229
Abstract
The Stöber version of a sol-gel method of co-condensation of two alkoxysilanes (structuring tetraethoxysilane (TEOS) and functionalising N-containing silane) in an ammonia medium was used for the one-pot synthesis of spherical silica particles with ≡Si(CH2)3NH2, ≡Si(CH2 [...] Read more.
The Stöber version of a sol-gel method of co-condensation of two alkoxysilanes (structuring tetraethoxysilane (TEOS) and functionalising N-containing silane) in an ammonia medium was used for the one-pot synthesis of spherical silica particles with ≡Si(CH2)3NH2, ≡Si(CH2)3NH(CH2)2NH2, and ≡[Si(CH2)3NH]2 functional groups with available groups content of 1.3–2.3 mmol/g. The materials were researched by a range of methods, including SEM, TEM, IR spectroscopy, 13C, and 29Si solid-state NMR spectroscopy, acid-base titration, and thermal analysis to identify the peculiarities of the morphology, functional groups content, composition, and thermal resistance of the surface layers in the synthesised samples. The type of N-containing silane was shown to affect the structure and properties of the synthesised spherical particles. The silane with the simplest, 3-aminopropyl, functional group caused the formation of nonporous material composed of large 600–800 nm spherical microparticles. Meanwhile, the complication of functional groups enhanced the emergence of small 15 nm primary particles and the origination of porosity, generated by the slits between particles and particle agglomerates. Thereafter, the sorption properties of the synthesised hybrid materials for nickel(II) and copper(II)ions, and bovine serum albumin (BSA) were also found to be dependent on the structure of the materials and the type of incorporated functional group. The maximal static sorption capacity values towards the targeted adsorbates were shown by the samples with 3-aminopropyl groups (1.27 mmol Ni/g), diamine groups (1.09 mmol Cu/g), and secondary amine groups (204.6 mg BSA/g). The conducted research opens up the prospects of directed one-pot synthesis of amino-functionalised hybrid organosilica materials for different applications. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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14 pages, 4206 KiB  
Article
Hydrothermal Synthesis of Well-Defined Red-Emitting Eu-Doped GdPO4 Nanophosphors and Investigation of Their Morphology and Optical Properties
by Egle Ezerskyte, Aleksej Zarkov, Vaidas Klimkevicius and Arturas Katelnikovas
Crystals 2023, 13(2), 174; https://doi.org/10.3390/cryst13020174 - 19 Jan 2023
Cited by 6 | Viewed by 1847
Abstract
Rare-earth-doped GdPO4 nanoparticles have recently attracted much scientific interest due to the simultaneous optical and magnetic properties of these materials and their possible application in bio-imaging. Herein, we report the hydrothermal synthesis of GdPO4:Eu3+ nanoparticles by varying different synthesis [...] Read more.
Rare-earth-doped GdPO4 nanoparticles have recently attracted much scientific interest due to the simultaneous optical and magnetic properties of these materials and their possible application in bio-imaging. Herein, we report the hydrothermal synthesis of GdPO4:Eu3+ nanoparticles by varying different synthesis parameters: pH, <Gd>:<P> molar ratio, and Eu3+ concentration. It turned out that the Eu3+ content in the synthesized nanoparticles had little effect on particle shape and morphology. The synthesis media pH, however, has showed a pronounced impact on particle size and distribution, i.e., the nanoparticle length can be adjusted from hundreds to tens of nanometers by changing the pH from 2 to 11, respectively. Increasing the <Gd>:<P> molar ratio resulted in a decrease in nanoparticle length and an increase in its width. The temperature-dependent measurements in the 77–500 K range revealed that the GdPO4:50%Eu3+ sample maintains half of its emission intensity, even at room temperature (TQ1/2 = 291 ± 19 K). Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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17 pages, 3989 KiB  
Article
Wet Synthesis of Graphene-Polypyrrole Nanocomposites via Graphite Intercalation Compounds
by Gintarė Rimkutė, Gediminas Niaura, Rasa Pauliukaitė, Justina Gaidukevič and Jurgis Barkauskas
Crystals 2022, 12(12), 1793; https://doi.org/10.3390/cryst12121793 - 9 Dec 2022
Cited by 2 | Viewed by 1609
Abstract
Graphene-polypyrrole (GP) nanocomposites were synthesized by a wet-way protocol using a graphite bisulfate (GBS) precursor. Consequently, GBS, a type of graphite intercalation compound, was prepared in the presence of concentrated sulfuric acid in the presence of a potassium periodate oxidizer. Three different types [...] Read more.
Graphene-polypyrrole (GP) nanocomposites were synthesized by a wet-way protocol using a graphite bisulfate (GBS) precursor. Consequently, GBS, a type of graphite intercalation compound, was prepared in the presence of concentrated sulfuric acid in the presence of a potassium periodate oxidizer. Three different types of graphite precursor with particle sizes of <50 μm, ≥150, ≤830 μm, and ≤2000 μm were used for this purpose. It was found that in the Raman spectra of GBS samples, the characteristic D band, which is caused by defects in the graphene layer, disappears. Therefore, the proposed synthesis protocol of GBS could be considered as a prospective intermediate stage in the preparation of graphene with low defect concentration. In contrast to alkali metal intercalation, the intercalation process involving anions with a relatively complex structure (e.g., HSO4−), which has been much less studied and requires further research. On the basis of the results obtained, structural models of graphite intercalation compounds as well as GP nanocomposites were discussed. The most relevant areas of application for GP nanocomposites, including energy storage and (bio)sensing, were considered. This work contributes to the development of cost-effective, scalable, and highly efficient intercalation methods, which still remain a significant challenge. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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16 pages, 8829 KiB  
Article
Wet Chemical Synthesis and Characterization of Au Coatings on Meso- and Macroporous Si for Molecular Analysis by SERS Spectroscopy
by Siarhei Zavatski, Anatoli I. Popov, Andrey Chemenev, Alma Dauletbekova and Hanna Bandarenka
Crystals 2022, 12(11), 1656; https://doi.org/10.3390/cryst12111656 - 17 Nov 2022
Cited by 9 | Viewed by 2257
Abstract
Porous silicon (PS) is a promising material for nanostructure fabrication providing a precise control over its size, shape, and spatial distribution. This makes it an excellent candidate for constructing highly sensitive, reproducible, and low-cost platforms for surface enhanced Raman scattering (SERS) spectroscopy. In [...] Read more.
Porous silicon (PS) is a promising material for nanostructure fabrication providing a precise control over its size, shape, and spatial distribution. This makes it an excellent candidate for constructing highly sensitive, reproducible, and low-cost platforms for surface enhanced Raman scattering (SERS) spectroscopy. In this work, we connect the PS structural parameters with the morphology of the gold nanostructures fabricated on its surface, placing the emphasis on the SERS response. Two different types of PS are considered here, namely meso- and macro-PS. The former is prepared by Si electrochemical etching, applying three different current densities: 100 mA cm−2, 60 mA cm−2, and 30 mA cm−2, while the technological parameters for the latter are selected to mimic metal nanovoids’ (Me NVs) configuration. The gold-coated PS surfaces are produced via an electroless chemical deposition method for different time periods. By performing comprehensive structural, morphological, and optical characterization, we show the importance of the size and density of the PS pore openings, which govern the Au growth kinetics. The results presented in this work assure a simple yet flexible approach for the fabrication of large-area plasmonic gold nanostructures, which are not only suitable for advanced SERS spectroscopy studies but can also serve for a wider range of plasmonic applications. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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10 pages, 2787 KiB  
Article
Solvent-Induced Cobalt(II) Cyanoguanidine Bromides: Syntheses, Crystal Structure, Optical and Magnetic Properties
by Jing Zhang, Alex. J. Corkett, Jan van Leusen, Ulli Englert and Richard Dronskowski
Crystals 2022, 12(10), 1377; https://doi.org/10.3390/cryst12101377 - 28 Sep 2022
Cited by 3 | Viewed by 1771
Abstract
Two different phase-pure cobalt(II) cyanoguanidine bromide coordination compounds, Co(C2N4H4)2(H2O)4·2Br·2H2O (1) and Co3(C2N4H4)8(H2O)8·6Br ( [...] Read more.
Two different phase-pure cobalt(II) cyanoguanidine bromide coordination compounds, Co(C2N4H4)2(H2O)4·2Br·2H2O (1) and Co3(C2N4H4)8(H2O)8·6Br (2), were precipitated from aqueous and methanol solutions, respectively, and their structures were solved and refined from X-ray single-crystal data at 100 K. Both 1 and 2 crystallize in the triclinic system with space group P1¯. The structure of 1 consists of two crystallographically distinct isolated CoO4N2 octahedral units plus bromide anions and crystal water molecules, whereas 2 is built from both isolated octahedra and discrete binuclear cluster units made from edge-sharing octahedra. Diffuse reflectance spectra and IR analysis then go on to highlight optical and vibrational differences between these two compounds. The magnetic susceptibility of 1 is consistent with either isolated or very weakly interacting Co2+ centers whereas the magnetic susceptibility of 2 evidences the potential weak antiferromagnetic exchange interactions that may arise from superexchange within the binuclear clusters. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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12 pages, 4647 KiB  
Article
The Impact of Full-Scale Substitution of Ca2+ with Ni2+ Ions on Brushite’s Crystal Structure and Phase Composition
by Mazen Alshaaer, Khalil Issa, Ahmed S. Afify, Moustapha E. Moustapha, Abdulaziz A. Alanazi, Ammar Elsanousi and Talal F. Qahtan
Crystals 2022, 12(7), 940; https://doi.org/10.3390/cryst12070940 - 4 Jul 2022
Cited by 4 | Viewed by 2008
Abstract
Because the impact of the full-scale substitution of Ca2+ in brushite (CaHPO4·2H2O) with Ni2+ ions has never been systematically explored, it is the focus of this investigation, as it holds potential for use in CaxNi [...] Read more.
Because the impact of the full-scale substitution of Ca2+ in brushite (CaHPO4·2H2O) with Ni2+ ions has never been systematically explored, it is the focus of this investigation, as it holds potential for use in CaxNi1−xHPO4·nH2O production. These biomaterials have many beneficial characteristics that can be modified to suit diverse applications, including bone tissue regeneration and pharmaceutics. For the present study, NaH2PO4·2H2O, Ca(NO3)2·4H2O, and Ni(NO3)2·6H2O were used in various molar concentrations to obtain the required starting solutions. Previous studies have shown that adding Ni ions in the initial solution below 20% results in the precipitation of monophasic brushite with slight changes in the crystal structure. However, this study confirms that when the Ni ions substitution increases to 20%, a mixture of phases from both brushite and hexaaquanickel(II) hydrogenphosphate monohydrate HNiP (Ni(H2O)6·HPO4·H2O) is formed. The results confirm that the full replacement (100%) of Ca ions by Ni ions results in a monophasic compound solely comprising orthorhombic HNiP nanocrystals. Therefore, a novel technique of HNiP synthesis using the precipitation method is introduced in this research work. These materials are subsequently analyzed utilizing powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). The obtained results confirm that the material microstructure is controlled by the Ni/Ca ratio in the starting solution and can be modified to obtain the desired characteristics of phases and crystals. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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16 pages, 4018 KiB  
Article
Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid
by Gintare Rimkute, Mantvydas Gudaitis, Jurgis Barkauskas, Aleksej Zarkov, Gediminas Niaura and Justina Gaidukevic
Crystals 2022, 12(3), 421; https://doi.org/10.3390/cryst12030421 - 18 Mar 2022
Cited by 12 | Viewed by 4001
Abstract
In this work, graphite intercalation compounds (GICs) were synthesized using three different oxidizers: (NH4)2S2O8, K2S2O8, and CrO3 with and without P2O5 as a water-binding agent. [...] Read more.
In this work, graphite intercalation compounds (GICs) were synthesized using three different oxidizers: (NH4)2S2O8, K2S2O8, and CrO3 with and without P2O5 as a water-binding agent. Furthermore, the samples obtained were heat-treated at 800 °C. Specimens were characterized by optical microscopy, Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), and scanning electron microscopy (SEM). The correlation between different characteristic parameters of the Raman analysis has shown that the use of CrO3 results in a much higher structural disorder compared to the products obtained using persulfate oxidizers. Narrowing the correlation set revealed that minimal defect concentration can be reached by using K2S2O8, while the use of (NH4)2S2O8 causes a slightly higher concentration of defects. It was also established that the additional use of P2O5 can help to achieve more effective intercalation and has a positive effect on the formation of the stage I GIC phase. After heat treatment, the intercalated products mostly return to a graphite-like structure; however, the samples obtained with CrO3 stand out with the most significant changes in their surface morphology. Therefore, analysis suggests that GICs obtained using persulfate oxidizers and P2O5 could be a candidate to produce high-quality graphene or graphene oxide. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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18 pages, 2554 KiB  
Article
An Enhanced Oxidation of Formate on PtNi/Ni Foam Catalyst in an Alkaline Medium
by Antanas Nacys, Dijana Šimkūnaitė, Aldona Balčiūnaitė, Aušrinė Zabielaitė, Daina Upskuvienė, Benjaminas Šebeka, Vitalija Jasulaitienė, Vitalij Kovalevskij, Eugenijus Norkus and Loreta Tamašauskaitė-Tamašiūnaitė
Crystals 2022, 12(3), 362; https://doi.org/10.3390/cryst12030362 - 8 Mar 2022
Cited by 10 | Viewed by 3976
Abstract
In this study, a platinum-coated Ni foam catalyst (denoted PtNi/Ni foam) was investigated for the oxidation of the formate reaction (FOR) in an alkaline medium. The catalyst was fabricated via a two-step procedure, which involved an electroless deposition of the Ni layer using [...] Read more.
In this study, a platinum-coated Ni foam catalyst (denoted PtNi/Ni foam) was investigated for the oxidation of the formate reaction (FOR) in an alkaline medium. The catalyst was fabricated via a two-step procedure, which involved an electroless deposition of the Ni layer using sodium hypophosphite as a reducing agent and the subsequent electrodeposition of the platinum layer. The PtNi/Ni foam catalyst demonstrated enhanced electrocatalytic activity for the FOR in an alkaline medium compared to the Ni/Ni foam catalyst and pure Pt electrode. Moreover, the PtNi/Ni foam catalyst promoted the FOR at more negative potentials than the Pt electrode. This contributed to a significant negative shift in the onset potential, indicating the high activity of the catalyst. Notably, in alkaline media with the PtNi/Ni foam catalyst, the FOR proceeds via a direct pathway mechanism without significant accumulation of poisonous carbonaceous species on the PtNi/Ni foam catalyst. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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12 pages, 2891 KiB  
Article
Synthesis, Crystal Structure, and Hirshfeld Surface Analysis of Hexachloroplatinate and Tetraclorouranylate of 3-Carboxypyridinium—Halogen Bonds and π-Interactions vs. Hydrogen Bonds
by Anton Petrovich Novikov, Mikhail Alexandrovich Volkov, Alexey Vladimirovich Safonov and Mikhail Semenovich Grigoriev
Crystals 2022, 12(2), 271; https://doi.org/10.3390/cryst12020271 - 17 Feb 2022
Cited by 16 | Viewed by 2880
Abstract
This work aimed to synthesize new platinum and uranium compounds with nicotinic acid. In this article we describe the synthesis of two new anionic complexes (HNic)2[PtCl6] and (HNic)2[UO2Cl4] using wet chemistry methods. The [...] Read more.
This work aimed to synthesize new platinum and uranium compounds with nicotinic acid. In this article we describe the synthesis of two new anionic complexes (HNic)2[PtCl6] and (HNic)2[UO2Cl4] using wet chemistry methods. The structure of the obtained single crystals was established by single-crystal X-ray diffraction. The Hirshfeld surface analysis of the obtained complexes and their analogue (HNic)2[SiF6] was carried out for the analysis of intermolecular interactions. Hydrogen bonds (H···Hal/Hal···H and O···H/H···O) make the main contribution to intermolecular interactions in all compounds. Other important contacts in cations in all compounds are H···H, C···H/H···C and C···Hal/Hal···C; in anions H···Hal/Hal···H. The Pt-containing complex has a halogen-π interaction and halogen bonds, but Si-containing complex has a π–π staking interaction; these types of interactions are not observed in the U-containing compound. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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11 pages, 3819 KiB  
Article
Solvothermal Synthesis of Calcium-Deficient Hydroxyapatite via Hydrolysis of α-Tricalcium Phosphate in Different Aqueous-Organic Media
by Rasa Karalkeviciene, Eva Raudonyte-Svirbutaviciene, Justina Gaidukevic, Aleksej Zarkov and Aivaras Kareiva
Crystals 2022, 12(2), 253; https://doi.org/10.3390/cryst12020253 - 13 Feb 2022
Cited by 8 | Viewed by 3226
Abstract
In the present work, the effects of various organic solvents (solvent nature and fraction within the solution) and solvothermal conditions on the formation of calcium-deficient hydroxyapatite (CDHA) via hydrolysis of α-tricalcium phosphate (α-TCP) are investigated. The wet precipitation method is applied for α-TCP [...] Read more.
In the present work, the effects of various organic solvents (solvent nature and fraction within the solution) and solvothermal conditions on the formation of calcium-deficient hydroxyapatite (CDHA) via hydrolysis of α-tricalcium phosphate (α-TCP) are investigated. The wet precipitation method is applied for α-TCP synthesis, and the hydrolysis reaction is performed in solutions with different water-to-organic solvent ratios under solvothermal conditions at 120 °C for 3 h and at 200 °C for 5 h. Ethyl alcohol, isopropyl alcohol, and butyl alcohol did not inhibit the hydrolysis of α-TCP, while methyl alcohol and ethylene glycol have a more prominent inhibitory effect on the hydrolysis, hence the formation of single-phased CDHA. From all the solvents analysed, ethylene glycol has the highest impact on the sample morphology. Under certain water to ethylene glycol ratios and solvothermal conditions, samples containing a significant fraction of rods are obtained. However, samples prepared with ethylene glycol are characterised by a particularly low BET surface area. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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13 pages, 3689 KiB  
Article
Effect of Synthesis Method on Properties of Layered Double Hydroxides Containing Ni(III)
by Olga V. Nestroinaia, Irina G. Ryltsova and Olga E. Lebedeva
Crystals 2021, 11(11), 1429; https://doi.org/10.3390/cryst11111429 - 21 Nov 2021
Cited by 6 | Viewed by 2929
Abstract
Unstable oxidation state +3 of nickel can be stabilized in the structure of layered double hydroxides, the resulting crystallinity and properties being dependent on the synthesis method. Three different wet chemical methods (co-precipitation at variable pH, co-precipitation followed by hydrothermal treatment, co-precipitation with [...] Read more.
Unstable oxidation state +3 of nickel can be stabilized in the structure of layered double hydroxides, the resulting crystallinity and properties being dependent on the synthesis method. Three different wet chemical methods (co-precipitation at variable pH, co-precipitation followed by hydrothermal treatment, co-precipitation with microwave treatment) were used to synthesize Mg/Ni–Al layered double hydroxides containing triply charged nickel cations. Lattice parameters of the samples synthesized by various methods were found to differ from each other by about 1.5%. The most crystallized sample was obtained by hydrothermal synthesis. The oxidation state of nickel in the LDH samples was confirmed by XPS. TEM mapping gave evidence of the uniform distribution of nickel in all the samples. The LDHs’ reduction with hydrogen and thermal transformations of the phase composition and morphology of LDHs were studied in detail. The properties of the samples synthesized by the different methods were shown to be quite similar. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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14 pages, 5274 KiB  
Communication
Synthesis and Characterization of New Guanine Complexes of Pt(IV) and Pd(II) by X-ray Diffraction and Hirshfeld Surface Analysis
by Anton Petrovich Novikov, Mikhail Alexandrovich Volkov, Alexey Vladimirovich Safonov, Mikhail Semenovich Grigoriev and Evgeny Vladilenovich Abkhalimov
Crystals 2021, 11(11), 1417; https://doi.org/10.3390/cryst11111417 - 19 Nov 2021
Cited by 11 | Viewed by 2714
Abstract
The aim of the work was to synthesize new perspective compounds of palladium and platinum with nitrogenous bases (guanine), promising for use in biomedicine and catalysis. The article describes the synthesis of new [PdCl2(HGua)2]Cl2·H2O and [...] Read more.
The aim of the work was to synthesize new perspective compounds of palladium and platinum with nitrogenous bases (guanine), promising for use in biomedicine and catalysis. The article describes the synthesis of new [PdCl2(HGua)2]Cl2·H2O and [PtCl5(HGua)]·2H2O compounds using wet chemistry methods. The structure of the obtained single crystals was established by the method of single crystal X-ray diffraction. The complexes have an M-N bond, and the organic ligand is included in the first coordination sphere. The analysis of Hirshfeld surfaces for the obtained complexes and their analogues for the analysis of intermolecular interactions was carried out. In the palladium complex we obtained, π-halogen and π-stacking interactions were found; in analogues, such interactions were not found. π-halogen and halogen interactions were found in structure of platinum complex and its analogues. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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Graphical abstract

11 pages, 3404 KiB  
Article
Preparation and Characterization of Tubelike g-C3N4/Ag3PO4 Heterojunction with Enhanced Visible-Light Photocatalytic Activity
by Xin Yan, Yuanyuan Wang, Bingbing Kang, Zhuo Li and Yanhui Niu
Crystals 2021, 11(11), 1373; https://doi.org/10.3390/cryst11111373 - 11 Nov 2021
Cited by 12 | Viewed by 1920
Abstract
Water pollution caused by dye wastewater is a potential threat to human health. Using photocatalysis technology to deal with dye wastewater has the advantages of strong purification and no secondary pollution, so it is greatly significant to look for new visible-light photocatalysts with [...] Read more.
Water pollution caused by dye wastewater is a potential threat to human health. Using photocatalysis technology to deal with dye wastewater has the advantages of strong purification and no secondary pollution, so it is greatly significant to look for new visible-light photocatalysts with high photocatalytic ability for dye wastewater degradation. Semiconductor photocatalyst silver phosphate (Ag3PO4) has high quantum efficiency and photocatalytic degradation activity. However, Ag3PO4 is prone to photoelectron corrosion and becomes unstable during photocatalysis, which severely limits its application in this field. In this study, a tubelike g-C3N4/Ag3PO4 heterojunction was constructed by the chemical precipitation method. An Ag3PO4 nanoparticle was loaded onto the surface of the tubelike g-C3N4, forming close contact. The photocatalytic activity of the photocatalyst was evaluated by the degradation of RhB under visible-light irradiation. The tubelike g-C3N4/Ag3PO4-5% heterojunction exhibited optimal photocatalytic performance. In an optimal process, the degradation rate of the RhB is 90% under visible-light irradiation for 40 min. The recycling experiment showed that there was no apparent decrease in the activity of tubelike g-C3N4/Ag3PO4-5% heterojunction after five consecutive runs. A possible Z-type mechanism is proposed to explain the high activity and stability of the heterojunction. Full article
(This article belongs to the Special Issue Advances in Functional Inorganic Materials Prepared by Wet Chemical Methods (Volume II))
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