Advances in Inorganic Synthesis

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Dear Colleagues,

Recent progress in inorganic chemistry would have been impossible without new and advanced methods of inorganic synthesis. New compounds have been synthesized and crystals grown thanks to the application of new techniques and ideas. Among them are multiagent chemical transport, deep eutectic synthesis, reactions in ionic liquids, nanoscale reactions, cryo-synthesis, and spark plasma sintering, to name a few. With new approaches, new compounds and materials appear, which were impossible to synthesize by using traditional routines. Coupled to new and advanced analytical techniques, advanced inorganic synthesis ensures a fascinating and exciting development of inorganic chemistry into a modern yet traditional branch of science. We invite scientists to contribute research papers, reviews, and communications to the topical collection entitled “Adcances in Inorganic Synthesis”. Contributions on any topic related to inorganic synthesis are welcome.

Prof. Dr. Andrei V. Shevelkov
Prof. Dr. Maxim N. Sokolov
Topic Editors

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Participating Journals

Journal Name	Impact Factor	CiteScore	Launched Year	First Decision (median)	APC
Catalysts catalysts	3.8	6.8	2011	12.9 Days	CHF 2200	Submit
Crystals crystals	2.4	4.2	2011	10.8 Days	CHF 2100	Submit
Inorganics inorganics	3.1	2.8	2013	14.7 Days	CHF 2700	Submit
Materials materials	3.1	5.8	2008	15.5 Days	CHF 2600	Submit
Molecules molecules	4.2	7.4	1996	15.1 Days	CHF 2700	Submit
Solids solids	2.4	3.4	2020	20.5 Days	CHF 1000	Submit

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14 pages, 5878 KiB  

Open AccessArticle

Study on Synthesis of CSH Gel and Its Immobilization of Heavy Metals

by Kunqian Zhu, Lijuan Wang, Libing Liao, Yunlong Bai and Jing Hu

Crystals 2024, 14(10), 864; https://doi.org/10.3390/cryst14100864 - 30 Sep 2024

Viewed by 471

Abstract

Calcium silicate hydrate (CSH) gel is the most important hydration product of cement. It influences the mechanical properties of resulting materials and plays an important role in the adsorption and immobilization of heavy metal ions. Research in the structure of CSH gel and [...] Read more.

Calcium silicate hydrate (CSH) gel is the most important hydration product of cement. It influences the mechanical properties of resulting materials and plays an important role in the adsorption and immobilization of heavy metal ions. Research in the structure of CSH gel and its ability for heavy metal immobilization enables the development of tailored cement-based materials, a feature that holds significant future potential. In this study, CSH gel was synthesized under different pH and Ca/Si conditions. Structural and morphological changes in CSH gel were investigated using modern technologies. The results revealed that both pH and Ca/Si ratios were important factors influencing the structure of CSH gel. During the formation of CSH, both Cr³⁺ and Pb²⁺ can be incorporated into CSH gel, and promoting the formation of calcium hydroxide Cr³⁺ can also replace Si⁴⁺ in the Si-O bond. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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17 pages, 7911 KiB  

Open AccessFeature PaperArticle

Precursor-Based Syntheses of Mo(C,N,O)_x, Molybdenum Carbide, Nitride, and Oxide Applying a Microjet Reactor

by Mana Abdirahman Mohamed, Oliver Janka, Susanne Harling and Guido Kickelbick

Solids 2024, 5(3), 443-459; https://doi.org/10.3390/solids5030030 - 4 Sep 2024

Viewed by 741

Abstract

Composite materials such as molybdenum carbides, nitrides, oxides, and mixed anionic compounds like Mo(C,N,O)_x embedded in carbonaceous matrix exhibit promising potential as anode materials for lithium batteries, with a preference for fine-grained morphologies. In this study, we present a novel synthetic approach [...] Read more.

Composite materials such as molybdenum carbides, nitrides, oxides, and mixed anionic compounds like Mo(C,N,O)_x embedded in carbonaceous matrix exhibit promising potential as anode materials for lithium batteries, with a preference for fine-grained morphologies. In this study, we present a novel synthetic approach involving an inorganic–organic hybrid precursor precipitated from aqueous solutions of ammonium heptamolybdate and one of two organic species: 1,8-diaminonaphthalene (1,8-DAN) or hexamethylenediamine (HMD). The precipitation reaction can be carried out in a beaker and in a continuous process using a microjet reactor. This enables the synthesis of precursor material on the gram scale within minutes. The pyrolysis of these precursors yields mixtures of Mo(C,N,O)_x, MoO₂, Mo₂C, Mo₂N, and Mo, with the choice of organic compound significantly influencing the resulting phases and the excess carbon content in the pyrolyzed product. Notably, the pyrolysis process maintains the size and morphology of the micro- to nanometer-sized starting materials. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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16 pages, 4292 KiB  

Open AccessArticle

Recovery of Zinc and Rhenium for the Production of Zinc Perrhenates

by Katarzyna Leszczyńska-Sejda, Joanna Malarz, Dorota Kopyto, Karolina Goc, Alicja Grzybek, Mateusz Ciszewski, Arkadiusz Palmowski, Grzegorz Benke and Karolina Pianowska

Crystals 2024, 14(8), 725; https://doi.org/10.3390/cryst14080725 - 14 Aug 2024

Viewed by 677

Abstract

This study outlines findings from an investigation into the development of a hydrometallurgical process for manufacturing various forms of zinc perrhenate, entirely from waste from recycling and from the Zn–Pb industry. Scraps of Re-bearing Ni-based superalloys and acidic waste, circulating zinc solutions generated [...] Read more.

This study outlines findings from an investigation into the development of a hydrometallurgical process for manufacturing various forms of zinc perrhenate, entirely from waste from recycling and from the Zn–Pb industry. Scraps of Re-bearing Ni-based superalloys and acidic waste, circulating zinc solutions generated during the production of Zn by the electrolytic method and which contain >45 g/dm³ of Zn, Na, Mn, and Mg, were used in the research. In the publication, the conditions for the production of three types of zinc perrhenate, i.e., Zn(ReO₄)₂·4H₂O, Zn(ReO₄)_2, and Zn(ReO₄)₂·2H₂O, are presented. As a result of the analysis of the obtained results, it was concluded that to obtain the above-mentioned forms of zinc perrhenate, zinc carbonate can be used, precipitated from acidic, waste, and multi-component solutions after their prior neutralization to pH 4.0 and partial purification from Mn, Mg, and Na using metallurgical zinc oxide. Zinc carbonate should be precipitated using Na₂CO₃ at pH 6.3 and subsequently purified from other impurities, i.e., Mg, Na, and Mn, using aqueous ammonia solutions. As a result, zinc carbonate was obtained, which was used in a reaction with an aqueous solution of HReO₄ to produce zinc perrhenate. The precipitated forms of Zn(ReO₄)₂ were obtained by appropriately drying the crude and hydrated Zn(ReO₄)₂ to obtain its tetrahydrate, dihydrate, and anhydrous forms, respectively, using drying temperatures of 55, 135, and 185 °C. The developed technology has been submitted for a patent and is an example of a technology founded on the principles of sustainable development, with a particular emphasis on the minimalization of loss of rhenium and zinc at all stages of its realization. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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11 pages, 13409 KiB  

Open AccessArticle

Heterojunctions of Mercury Selenide Quantum Dots and Halide Perovskites with High Lattice Matching and Their Photodetection Properties

by Chengye Yu, Yufeng Shan, Jiaqi Zhu, Dingyue Sun, Xiaohong Zheng, Na Zhang, Jingshan Hou, Yongzheng Fang, Ning Dai and Yufeng Liu

Materials 2024, 17(8), 1864; https://doi.org/10.3390/ma17081864 - 18 Apr 2024

Viewed by 1174

Abstract

Heterojunction semiconductors have been extensively applied in various optoelectronic devices due to their unique carrier transport characteristics. However, it is still a challenge to construct heterojunctions based on colloidal quantum dots (CQDs) due to stress and lattice mismatch. Herein, HgSe/CsPbBr_xI_3−x [...] Read more.

Heterojunction semiconductors have been extensively applied in various optoelectronic devices due to their unique carrier transport characteristics. However, it is still a challenge to construct heterojunctions based on colloidal quantum dots (CQDs) due to stress and lattice mismatch. Herein, HgSe/CsPbBr_xI_3−x heterojunctions with type I band alignment are acquired that are derived from minor lattice mismatch (~1.5%) via tuning the ratio of Br and I in halide perovskite. Meanwhile, HgSe CQDs with oleylamine ligands can been exchanged with a halide perovskite precursor, acquiring a smooth and compact quantum dot film. The photoconductive detector based on HgSe/CsPbBr_xI_3−x heterojunction presents a distinct photoelectric response under an incident light of 630 nm. The work provides a promising strategy to construct CQD-based heterojunctions, simultaneously achieving inorganic ligand exchange, which paves the way to obtain high-performance photodetectors based on CQD heterojunction films. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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13 pages, 4044 KiB  

Open AccessArticle

New Data on Crystal Phases in the System MgSO₄–OC(NH₂)₂–H₂O

by Rositsa Nikolova, Vladislav Kostov-Kytin, Nadia Petrova, Krasimir Kossev, Rositsa Titorenkova and Gergana Velyanova

Crystals 2024, 14(3), 227; https://doi.org/10.3390/cryst14030227 - 27 Feb 2024

Cited by 1 | Viewed by 1278

Abstract

Urea complexes of magnesium sulfate have been intensively studied due to their application in many areas of life, including agricultural chemistry, pharmacy, medicine, etc. The aim of this study is to add new knowledge about the trends and consistencies in the preparation procedures [...] Read more.

Urea complexes of magnesium sulfate have been intensively studied due to their application in many areas of life, including agricultural chemistry, pharmacy, medicine, etc. The aim of this study is to add new knowledge about the trends and consistencies in the preparation procedures of MgSO₄·nOC(NH₂)₂·mH₂O phases. A set of analytical methods was used to characterize their structure, thermal and spectroscopic properties. The conditions for obtaining the three complexes in pure form were specified and the crystal structures of MgSO₄·OC(NH₂)₂·2H₂O and MgSO₄·OC(NH₂)₂·3H₂O were determined. The spectroscopic data of the considered compounds were analysed with respect to their structural and chemical properties. Thermal analyses showed that both the melting point and the urea decomposition temperature depend on the OC(NH₂)₂: H₂O ratio in the octahedral environment of the magnesium ion in the studied structures. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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14 pages, 3787 KiB  

Open AccessArticle

Unveiling the Exceptional Performance of ZnO/Zn₂TiO₄ Nanocomposites

by Husnain Ahmad Abbasi, Maha M. Al Moneef, Jahanzeb Khan, Muhammad Hafeez, Muhammad Usman Hameed, Muhammad Abdullah Khan, Shabnam Shahida, Habib Ahmad Abbasi and Sook-Keng Chang

Catalysts 2024, 14(2), 156; https://doi.org/10.3390/catal14020156 - 19 Feb 2024

Cited by 3 | Viewed by 1758

Abstract

In this study, we engineered a sub-70 nm nanocomposite of ZnO/Zn₂TiO₄ using a low-temperature solution-phase method with titanium isopropoxide and zinc acetate as precursors, and isopropyl alcohol and water as solvents. The investigation focused on nanocomposite growth by varying precursor [...] Read more.

In this study, we engineered a sub-70 nm nanocomposite of ZnO/Zn₂TiO₄ using a low-temperature solution-phase method with titanium isopropoxide and zinc acetate as precursors, and isopropyl alcohol and water as solvents. The investigation focused on nanocomposite growth by varying precursor and surfactant concentrations and their efficiency within different pH ranges. All three ZnO/Zn₂TiO₄ nanocomposites exhibited hexagonal wurtzite ZnO and Zn₂TiO₄ structures. The crystallite size in these nanocomposites ranged from 39.50 nm to 62.67 nm for ZnO and 21.24 nm to 26.15 nm for Zn₂TiO₄. Morphological observations using FESEM revealed the formation of dispersed cotton packet-like nanocomposites with sizes ranging from 18 to 350 nm. FTIR analysis showed peaks indicative of Ti–O and Zn–O bond formation, and EDX spectrum confirmed the presence of Ti, O, and Zn. UV spectrums and photocatalytic investigations confirmed the successful formation of ZnO/Zn₂TiO₄ nanocomposites with notable photocatalytic degradation efficiency for methylene blue dye under various conditions. These findings suggest the potential applicability of the synthesized nanocomposites for environmental pollutant degradation. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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17 pages, 9238 KiB  

Open AccessArticle

Influence of the La_0.2Sr_0.7Ti_0.95Ni_0.05O₃ (LSTN) Synthesis Method on SOFC Anode Performance

by Moran Dahan, Ludmila Fadeev, Hagay Hayun, Michael Gozin, Yaniv Gelbstein and Brian A. Rosen

Catalysts 2024, 14(1), 79; https://doi.org/10.3390/catal14010079 - 18 Jan 2024

Cited by 1 | Viewed by 1641

Abstract

Solid oxide fuel cells are characterized by a high efficiency for converting chemical energy into electricity and fuel flexibility. This research work focuses on developing durable and efficient anodes for solid oxide fuel cells (SOFCs) based on exsolving nickel from the perovskite structure. [...] Read more.

Solid oxide fuel cells are characterized by a high efficiency for converting chemical energy into electricity and fuel flexibility. This research work focuses on developing durable and efficient anodes for solid oxide fuel cells (SOFCs) based on exsolving nickel from the perovskite structure. A-site-deficient La- and Ni-doped strontium titanates (La_0.2Sr_0.7Ti_0.95Ni_0.05O_3−δ, LSTN) were synthesized using four different techniques and mixed with Ce_0.8Gd_0.2O_2−δ (GDC) to form the SOFC anode. The synthesis routes of interest for comparison included solid-state, sol-gel, hydrothermal, and co-precipitation methods. LSTN powders were characterized via XRD, SEM, TPR, BET and XPS. In situ XRD during reduction was measured and the reduced powders were analyzed using TEM. The impact of synthesis route on SOFC performance was investigated. All samples were highly durable when kept at 0.5 V for 48 h at 800 °C with H₂ fuel. Interestingly, the best performance was observed for the cell with the LSTN anode prepared via co-precipitation, while the conventional solid-state synthesis method only achieved the second-best results. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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18 pages, 7025 KiB  

Open AccessArticle

A New Method of Obtaining High Purity Nickel(II) Perrhenate from Waste

by Katarzyna Leszczyńska-Sejda, Grzegorz Benke, Dorota Kopyto, Joanna Malarz, Mateusz Ciszewski and Karolina Goc

Crystals 2023, 13(10), 1465; https://doi.org/10.3390/cryst13101465 - 7 Oct 2023

Cited by 1 | Viewed by 1664

Abstract

The article presents a new method of producing anhydrous nickel(II) perrhenate of high purity, entirely from waste from the national Cu industry. This method consists mainly of the reaction of water-washed nickel(II) oxide (obtained by purification in a mixture of alcohols, and subsequent [...] Read more.

The article presents a new method of producing anhydrous nickel(II) perrhenate of high purity, entirely from waste from the national Cu industry. This method consists mainly of the reaction of water-washed nickel(II) oxide (obtained by purification in a mixture of alcohols, and subsequent roasting of the Ni-containing sulfate semi-finished products (NSP) at 1200 °C) with perrhenic acid (obtained using the ion exchange method). After the dissolution of nickel(II) oxide in the acid (at a temperature in the range of 60–80 °C) and obtaining a pH of 5–8, the solution is sent to evaporate to dryness, also at a temperature not exceeding 80 °C. The obtained crude nickel(II) perrhenate is washed with methanol and subsequently dried at 160 °C to obtain its anhydrous form, with the following composition: 10.5% of Ni; 66.6% of Re; <5 ppm of Bi, As, Zn and Cu; <10 ppm Co, Mg, Fe, K, Pb, Na, Ca and Mo. Importantly, this composition allows for the use of the compound for the production of superalloys and catalysts. A patent application and a technological scheme were prepared for the developed method. It consists of seven technological operations, including six based on processes in the field of hydrometallurgy, and one in the field of pyrometallurgy (roasting). Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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11 pages, 12506 KiB  

Open AccessArticle

Exploring Relaxation Phenomenon in Cu-Substituted Ba₂NiWO₆ Double Perovskites

by Shahid M. Ramay, Mohammed H. Aldosary, Ghulam M. Mustafa, Sadaf Saba, Shahid Atiq, Sikandar Aftab and M. A. Ebdah

Crystals 2023, 13(4), 625; https://doi.org/10.3390/cryst13040625 - 5 Apr 2023

Cited by 1 | Viewed by 1578

Abstract

Double perovskites are an emerging class of functional materials with a great deal of durability perspective owing to their inherent flexibility in cation coordination selection. Here, we synthesized pristine and Cu²⁺-doped Ba₂NiWO₆ utilizing the solid-state reaction route to [...] Read more.

Double perovskites are an emerging class of functional materials with a great deal of durability perspective owing to their inherent flexibility in cation coordination selection. Here, we synthesized pristine and Cu²⁺-doped Ba₂NiWO₆ utilizing the solid-state reaction route to investigate their structural, morphological, and dielectric behavior. Structural examination revealed the development of a cubic crystal structure for both compositions, and Cu²⁺ integration in Ba₂NiWO₆ decreases the crystallite size. The spherical-shaped grains shrink in size and start agglomeration with Cu²⁺ incorporation. The incorporation of Cu²⁺ reduces the grain size, leads to accumulation of space charges at the grain boundaries, and thus, facilitates growth in the space charge polarization. This increases the dielectric constant of the material, thus making these compositions viable for advanced miniaturized electronic devices. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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18 pages, 8410 KiB  

Open AccessArticle

Copper Ferrite Nanoparticles Synthesized Using Anion-Exchange Resin: Influence of Synthesis Parameters on the Cubic Phase Stability

by Svetlana Saikova, Aleksandr Pavlikov, Denis Karpov, Aleksandr Samoilo, Sergey Kirik, Mikhail Volochaev, Tatyana Trofimova, Dmitry Velikanov and Artem Kuklin

Materials 2023, 16(6), 2318; https://doi.org/10.3390/ma16062318 - 14 Mar 2023

Cited by 6 | Viewed by 2326

Abstract

Copper ferrite is of great interest to researchers as a material with unique magnetic, optical, catalytic, and structural properties. In particular, the magnetic properties of this material are structurally sensitive and can be tuned by changing the distribution of Cu and Fe cations [...] Read more.

Copper ferrite is of great interest to researchers as a material with unique magnetic, optical, catalytic, and structural properties. In particular, the magnetic properties of this material are structurally sensitive and can be tuned by changing the distribution of Cu and Fe cations in octahedral and tetrahedral positions by controlling the synthesis parameters. In this study, we propose a new, simple, and convenient method for the synthesis of copper ferrite nanoparticles using a strongly basic anion-exchange resin in the OH form. The effect and possible mechanism of polysaccharide addition on the elemental composition, yield, and particle size of CuFe₂O₄ are investigated and discussed. It is shown that anion-exchange resin precipitation leads to a mixture of unstable cubic (c-CuFe₂O₄) phases at standard temperature and stable tetragonal (t-CuFe₂O₄) phases. The effect of reaction conditions on the stability of c-CuFe₂O₄ is studied by temperature-dependent XRD measurements and discussed in terms of cation distribution, cooperative Jahn–Teller distortion, and Cu²⁺ and oxygen vacancies in the copper ferrite lattice. The observed differences in the values of the saturation magnetization and coercivity of the prepared samples are explained in terms of variations in the particle size and structural properties of copper ferrite. Full article

(This article belongs to the Topic Advances in Inorganic Synthesis)

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