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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Materials Chemistry".

Deadline for manuscript submissions: closed (31 October 2023) | Viewed by 33890

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Special Issue Editors

Dr. Yunchao Xie

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Guest Editor

Department of Mechanical and Aerospace Engineering, University of Missouri, Columbia, MO 65211, USA
Interests: machine learning; deep learning; advanced manufacturing; metal-organic frameworks; joule heating

Dr. Hongxing Dong

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Guest Editor

Key Laboratory of Materials for High-Power Laser, Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800, China
Interests: high-quality microcavity lasers; metamaterial for electromagnetic wave modulation

Dr. Chi Zhang

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Guest Editor

School of Physics and Optoelectronic Engineering, Hangzhou Institute for Advanced Study, University of Chinese Academy of Sciences, Hangzhou 310024, China
Interests: machine learning; laser processing; metamaterials
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Nanomaterials have emerged as a promising class of materials with a size of less than 100 nm in at least one dimension. Nanomaterials possess remarkable and interesting mechanical, electrical, optical, electrochemical, and magnetic properties due to their high aspect ratio, unique surface chemistry, and quantum-size effect. The development of nanomaterials is intimately linked to the development of synthesis methods. Hence, it is always an attractive research topic for academic and industry communities to update conventional methods or develop new synthesis methods with the aim to enhance the performance and property, increase yields, lower the energy consumption, reduce the amounts of raw resources used, etc. Over the past decade, many novel synthetic methods including carbothermal shock, Joule heating, and microwave heating have been widely investigated and achieved exciting research progress. Meanwhile, green synthesis such as ball milling and extrusion synthesis has also been developed to make the nanomaterial synthesis safer, energy efficient, and less toxic. In addition, the rapid development of robotics and machine learning has greatly powered the material synthesis method, making it more efficient and automatic.

This Special Issue is devoted to presenting the recent advances in various synthetic methods in nanomaterials. We welcome researchers to submit their findings in the following forms: original research articles, reviews, perspectives, short summaries, and communications.

Topics of this Special Issue include, but are not limited to, the following:

Green synthesis including ball milling and extruding synthesis;
Synthesis automation with the aid of robotics;
Machine-learning-guided synthesis optimization;
Conventional synthesis methods including soft/hard template, solvo-/hydro-thermal, sol-gel, micro-emulsion, etc.

Dr. Yunchao Xie
Dr. Hongxing Dong
Dr. Chi Zhang
Guest Editors

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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. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

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Keywords

far-from equilibrium synthesis
green chemistry
synthesis automation
machine learning
synthesis optimization

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Published Papers (10 papers)

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Research

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13 pages, 3687 KiB

Open AccessArticle

Effect of Tetrahedrally Coordinated Al on the Surface Acidity of Mg-Al Binary Mixed Oxides

by Vidya Chandrabose, Taeho Kim, Ji won Park, Sang-Yong Jung and Jae-Min Oh

Molecules 2023, 28(16), 6072; https://doi.org/10.3390/molecules28166072 - 15 Aug 2023

Cited by 3 | Viewed by 1516

Abstract

Metal oxides (MOs) having Mg and Al with Mg/Al ratios of 1, 2, 3, and 4 were synthesized via calcination of the layered double hydroxides (LDH). The X-ray diffraction analysis revealed that all the MO consisted of periclase (MgO) crystallite with comparable crystallinity regardless of the metal ratio. According to the ²⁷Al magic-angle spinning nuclear magnetic resonance, the phase transformation from LDH to MO upon calcination facilitated the evolution of the Al³⁺ ions with unsaturated coordination at the surface of MO. The specific surface area values of MOs were not significantly different from each other, ranging between 100 and 200 m²/g, suggesting that the metal ratio did not strongly influence the porous structure of MO. The temperature-dependent desorption of ammonia demonstrated that the Lewis acidity of the Al-rich MOs was the largest with an Mg/Al ratio of 1, attributed to the efficient exposure of the surface-active site Al³⁺-O²⁻ pairs. The acidity of heterogenous Al-rich MOs significantly increased with the exposed tetrahedral Al site on the surface and dramatically diminished when the molar ratio (Mg/Al) was over two. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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14 pages, 2498 KiB

Open AccessArticle

Usnic Acid-Loaded Magnetite Nanoparticles—A Comparative Study between Synthesis Methods

by Cristina Chircov, Alexandra Cătălina Bîrcă, Lorena Alexandra Dănciulescu, Ionela Andreea Neacșu, Ovidiu-Cristian Oprea, Roxana-Doina Trușcă and Ecaterina Andronescu

Molecules 2023, 28(13), 5198; https://doi.org/10.3390/molecules28135198 - 4 Jul 2023

Cited by 2 | Viewed by 1640

Abstract

Since cancer is a continuously increasing concern for the general population, more efficient treatment alternatives ought to be developed. In this regard, a promising direction is represented by the use of magnetite nanoparticles (MNPs) to act both as a nanocarrier for the targeted release of antitumoral drugs and as hyperthermia agents. Thus, the present study focused on improving the control upon the outcome properties of MNPs by using two synthesis methods, namely the co-precipitation and microwave-assisted hydrothermal method, for the incorporation of usnic acid (UA), a natural lichen-derived metabolite with proven anticancer activity. The obtained UA-loaded MNPs were thoroughly characterized regarding their morpho-structural and physicochemical properties through X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), dynamic light scattering (DLS) and zeta potential, scanning electron microscopy (SEM), and vibrating sample magnetometry (VSM). Results demonstrated the formation of magnetite as the unique mineralogical phase through both types of synthesis, with increased uniformity regarding the drug loading efficiency, size, stability, and magnetic properties obtained through the microwave-assisted hydrothermal method. Furthermore, the cytotoxicity of the nanostructures against the HEK 293T cell line was investigated through the XTT assay, which further proved their potential for anticancer treatment applications. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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18 pages, 5666 KiB

Open AccessArticle

Fabrication of Enhanced UV Protective Cotton Fabric Using Activated Nano-Biocarbon Derived from Teff Hay Grafted by Polyaniline: RSM-Based Optimization and Characterization

by Kibebe Sahile, Esayas Alemayehu, Abebe Worku, Sundramurthy Venkatesa Prabhu and Bernd Lennartz

Molecules 2023, 28(13), 5142; https://doi.org/10.3390/molecules28135142 - 30 Jun 2023

Cited by 6 | Viewed by 1657

Abstract

In the present study, a hybrid cotton fabric with an enhanced ultraviolet (UV) shielding property was developed by coating with functionally activated nanocarbon (FACN) which was grafted by polyaniline (PANI) using in situ polymerization. In light of this, Teff hay biomass was used to establish the activated nanocarbon (ANC), that was subsequently given a surface functionalization using a silane coupling agent. Using the response surface (RSM) statistical analysis, the study was optimized for the weight percent of ANC and PANI with respect to the cotton fabric that was found to offer remarkable UV protection, with an ultraviolet protection factor (UPF) of 64.563, roughly 17 times more than that of primitive cotton (UPF = 3.7). The different characterization techniques, such as UV absorption, Fourier transform infrared (FTIR), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and thermal behavior studies were investigated. In addition, the basic textile properties on optimized hybrid material were found to be appreciably increased. The results suggested that activated FACN made from Teff hay could be an effective alternative organic source material for developing UV protective hybrid cotton fabrics. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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16 pages, 9470 KiB

Open AccessArticle

Correlation between Magnetic and Dielectric Response of CoFe₂O₄:Li¹⁺/Zn²⁺ Nanopowders Having Improved Structural and Morphological Properties

by Mahwish Afzia, Rafaqat Ali Khan, Bushra Ismail, Magdi E. A. Zaki, Talal M. Althagafi, Abdulaziz A. Alanazi and Afaq Ullah Khan

Molecules 2023, 28(6), 2824; https://doi.org/10.3390/molecules28062824 - 21 Mar 2023

Cited by 4 | Viewed by 2046

Abstract

The vast applicability of spinel cobalt ferrite due to its unique characteristics implies the need for further exploration of its properties. In this regard, structural modification at the O-site of spinel with Li¹⁺/Zn²⁺ was studied in detail for exploration of the correlation between structural, magnetic, and dielectric properties of the doped derivatives. The CTAB-assisted coprecipitation method was adopted for the synthesis of the desired compositions owing to its cost effectiveness and size controlling ability. Redistribution of cations at T- and O-sites resulted in the expansion of the crystal lattice, but no distortion of the cubic structure was observed, which further supports the flexible crystal structure of spinel for accommodating larger Li¹⁺/Zn²⁺ cations. Moreover, an XPS analysis confirmed the co-existence of the most stable oxidation states of Zn²⁺, Li¹⁺, Co²⁺, and Fe³⁺ ions with unstable Co³⁺ and Fe²⁺ ions as well, which induces the probability of hopping mechanisms to a certain extent and is a well-established behavior of cobalt ferrite nanoparticles. The experimental results showed that Li¹⁺/Zn²⁺ co-doped samples exhibit the best magnetic properties at dopant concentration x = 0.3. However, increasing the dopant content causes disturbance at both sites, resulting in decreasing magnetic parameters. It is quite evident from the results that dielectric parameters are closely associated with each other. Therefore, dopant content at x = 0.1 is considered the threshold value exhibiting the highest dielectric parameters, whereas any further increase would result in decreasing the dielectric parameters. The reduced dielectric properties and enhanced magnetic properties make the investigated samples a potential candidate for magnetic recording devices. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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13 pages, 3651 KiB

Open AccessArticle

The Strengthened Photocatalytic NO_x Removal of Composites Bi₄O₅Br₂/BiPO₄: The Efficient Regulation of Interface Carriers by Integrating a Wide-Bandgap Ornament

by Fei Chang, Zhuoli Shi, Yibo Lei, Zhongyuan Zhao, Yingfei Qi, Penghong Yin and Shengwen Chen

Molecules 2022, 27(23), 8474; https://doi.org/10.3390/molecules27238474 - 2 Dec 2022

Cited by 6 | Viewed by 1460

Abstract

A series of binary composites Bi₄O₅Br₂/BiPO₄ (PBX) was fabricated through a simple mechanical ball milling protocol. Relevant microstructural, morphological, and optical properties were thoroughly analyzed via various techniques. The integration of both components was confirmed to produce heterojunction domains at the phase boundaries. Upon exposure to visible light irradiation, the as-achieved PBX series possessed the reinforced photocatalytic NO_x removal efficiencies and the weakened generation of toxic intermediate NO₂ in comparison to both bare components, chiefly attributed to the efficient transport and separation of carriers and boosted production of superoxide radicals (·O₂⁻) through the combination of a wide-bandgap ornament BiPO₄ as an electron acceptor. In particular, the composite PB5 with the optimal phase composition exhibited the highest NO_x removal of 40% with the lowest NO₂ formation of 40 ppb among all tested candidates. According to the band structures’ estimation and reactive species’ detection, a reasonable mechanism was ultimately proposed to describe the migration of charge carriers and the enhancement of photocatalytic performance. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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Review

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35 pages, 3869 KiB

Open AccessReview

Optimized DOX Drug Deliveries via Chitosan-Mediated Nanoparticles and Stimuli Responses in Cancer Chemotherapy: A Review

by HafizMuhammad Imran, Yixin Tang, Siyuan Wang, Xiuzhang Yan, Chang Liu, Lei Guo, Erlei Wang and Caina Xu

Molecules 2024, 29(1), 31; https://doi.org/10.3390/molecules29010031 - 20 Dec 2023

Cited by 3 | Viewed by 2608

Abstract

Chitosan nanoparticles (NPs) serve as useful multidrug delivery carriers in cancer chemotherapy. Chitosan has considerable potential in drug delivery systems (DDSs) for targeting tumor cells. Doxorubicin (DOX) has limited application due to its resistance and lack of specificity. Chitosan NPs have been used for DOX delivery because of their biocompatibility, biodegradability, drug encapsulation efficiency, and target specificity. In this review, various types of chitosan derivatives are discussed in DDSs to enhance the effectiveness of cancer treatments. Modified chitosan–DOX NP drug deliveries with other compounds also increase the penetration and efficiency of DOX against tumor cells. We also highlight the endogenous stimuli (pH, redox, enzyme) and exogenous stimuli (light, magnetic, ultrasound), and their positive effect on DOX drug delivery via chitosan NPs. Our study sheds light on the importance of chitosan NPs for DOX drug delivery in cancer treatment and may inspire the development of more effective approaches for cancer chemotherapy. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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16 pages, 4775 KiB

Open AccessReview

Dynamic Metal Nanoclusters: A Review on Accurate Crystal Structures

by Xiang Liu, Fan Peng, Gao Li and Kai Diao

Molecules 2023, 28(14), 5306; https://doi.org/10.3390/molecules28145306 - 10 Jul 2023

Cited by 2 | Viewed by 1968

Abstract

Dynamic metal nanoclusters have garnered widespread attention due to their unique properties and potential applications in various fields. Researchers have been dedicated to developing new synthesis methods and strategies to control the morphologies, compositions, and structures of metal nanoclusters. Through optimized synthesis methods, it is possible to prepare clusters with precise sizes and shapes, providing a solid foundation for subsequent research. Accurate determination of their crystal structures is crucial for understanding their behavior and designing custom functional materials. Dynamic metal nanoclusters also demonstrate potential applications in catalysis and optoelectronics. By manipulating the sizes, compositions, and surface structures of the clusters, efficient catalysts and optoelectronic materials can be designed and synthesized for various chemical reactions and energy conversion processes. This review summarizes the research progress in the synthesis methods, crystal structure characterization, and potential applications of dynamic metal nanoclusters. Various nanoclusters composed of different metal elements are introduced, and their potential applications in catalysis, optics, electronics, and energy storage are discussed. Additionally, the important role of dynamic metal nanoclusters in materials science and nanotechnology is explored, along with an overview of the future directions and challenges in this field. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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38 pages, 7550 KiB

Open AccessReview

Nanotechnology–General Aspects: A Chemical Reduction Approach to the Synthesis of Nanoparticles

by Paulina Szczyglewska, Agnieszka Feliczak-Guzik and Izabela Nowak

Molecules 2023, 28(13), 4932; https://doi.org/10.3390/molecules28134932 - 22 Jun 2023

Cited by 49 | Viewed by 13327

Abstract

The role of nanotechnology is increasingly important in our society. Through it, scientists are acquiring the ability to understand the structure and properties of materials and manipulate them at the scale of atoms and molecules. Nanomaterials are at the forefront of the rapidly growing field of nanotechnology. The synthesis of nanostructured materials, especially metallic nanoparticles, has attracted tremendous interest over the past decade due to their unique properties, making these materials excellent and indispensable in many areas of human activity. These special properties can be attributed to the small size and large specific surface area of nanoparticles, which are very different from those of bulk materials. Nanoparticles of different sizes and shapes are needed for many applications, so a variety of protocols are required to produce monodisperse nanoparticles with controlled morphology. The purpose of this review is firstly to introduce the reader to the basic aspects related to the field of nanotechnology and, secondly, to discuss metallic nanoparticles in greater detail. This article explains the basic concepts of nanotechnology, introduces methods for synthesizing nanoparticles, and describes their types, properties, and possible applications. Of many methods proposed for the synthesis of metal nanoparticles, a chemical reduction is usually preferred because it is easy to perform, cost-effective, efficient, and also allows control of the structural parameters through optimization of the synthesis conditions. Therefore, a chemical reduction method is discussed in more detail—each factor needed for the synthesis of nanoparticles by chemical reduction is described in detail, i.e., metal precursors, solvents, reducing agents, and stabilizers. The methods that are used to characterize nanomaterials are described. Finally, based on the available literature collection, it is shown how changing the synthesis parameters/methods affects the final characteristics of nanoparticles. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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24 pages, 5216 KiB

Open AccessReview

Synthesis and Application of Porous Carbon Nanomaterials from Pomelo Peels: A Review

by Zixuan Liu, Qizheng Yang, Lei Cao, Shuo Li, Xiangchen Zeng, Wenbo Zhou and Cheng Zhang

Molecules 2023, 28(11), 4429; https://doi.org/10.3390/molecules28114429 - 30 May 2023

Cited by 14 | Viewed by 3544

Abstract

Advanced carbon nanomaterials have been widely applied in various fields such as microelectronics, energy storage, catalysis, adsorption, biomedical engineering, and material strengthening. With the increasing demand for porous carbon nanomaterials, many studies have explored obtaining porous carbon nanomaterials from biomass, which is highly abundant. Pomelo peel, a type of biomass rich in cellulose and lignin, has been widely upgraded into porous carbon nanomaterials with large yield and significant applications. Here, we systematically review the recent progress in pyrolysis, activation, and applications of synthesizing porous carbon nanomaterials from waste pomelo peels. Moreover, we provide a perspective on the remaining challenges and potential future research directions. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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28 pages, 5341 KiB

Open AccessReview

Review of Recent Developments in the Fabrication of ZnO/CdS Heterostructure Photocatalysts for Degradation of Organic Pollutants and Hydrogen Production

by Santhosh Kumar Nadikatla, Vinod Babu Chintada, Thirumala Rao Gurugubelli and Ravindranadh Koutavarapu

Molecules 2023, 28(11), 4277; https://doi.org/10.3390/molecules28114277 - 23 May 2023

Cited by 16 | Viewed by 3063

Abstract

Researchers have recently paid a lot of attention to semiconductor photocatalysts, especially ZnO-based heterostructures. Due to its availability, robustness, and biocompatibility, ZnO is a widely researched material in the fields of photocatalysis and energy storage. It is also environmentally beneficial. However, the wide bandgap energy and quick recombination of the photoinduced electron–hole pairs of ZnO limit its practical utility. To address these issues, many techniques have been used, such as the doping of metal ions and the creation of binary or ternary composites. Recent studies showed that ZnO/CdS heterostructures outperformed bare ZnO and CdS nanostructures in terms of photocatalytic performance when exposed to visible light. This review largely concentrated on the ZnO/CdS heterostructure production process and its possible applications including the degradation of organic pollutants and hydrogen evaluation. The importance of synthesis techniques such as bandgap engineering and controlled morphology was highlighted. In addition, the prospective uses of ZnO/CdS heterostructures in the realm of photocatalysis and the conceivable photodegradation mechanism were examined. Lastly, ZnO/CdS heterostructures’ challenges and prospects for the future have been discussed. Full article

(This article belongs to the Special Issue Recent Advances in Nanomaterial Synthesis)

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