Synthesis Of Inorganic Materials Research Articles

Chiral mesostructured SnO2 films with tunable optical activities

New strategies for tunable optical activities (OAs) are of fundamental importance in the advancement of science and technology. Here, we report hierarchically chiral mesostructured SnO2 films (CMSFs) deposited on FTO substrates via a symmetry breaking agent-inducing method. Three levels of chiral structures exist in the film, including tertiary plates helically arranged in fan-like form, secondary subplates helically stacked along [001] direction and primary nanosheets twisted along [100] direction. The thickness of plates was significantly increased with decreasing reactants concentration due to slower and preferential growth of plates along [001] direction. The increasing number of nanosheets results in enhancement and red shift of circular dichroism (CD) signals based on electron-transition absorption and reflection–based OA, which is in accordance with the circular Bragg resonance theory. Such novel chiral films with tunable OAs and morphologies may bring new ideas for design and synthesis of chiral inorganic materials with specific chirality and OA in the nanomaterial field.

Sonochemical synthesis of gum guar biopolymer stabilized copper oxide on exfoliated graphite: Application for enhanced electrochemical detection of H2O2 in milk and pharmaceutical samples

A novel and cost-effective synthesis of biopolymer-based organic and inorganic composite materials have received substantial attention in a broad range application including electroanalysis of small molecules. In this perspective, we report the synthesis of gum guar (guar) biopolymer stabilized cupric oxide decorated on exfoliated graphite (GR-guar/CuO) composite. Different physicochemical characterization methods were used to confirm the successful exfoliation of graphite and formation of the GR-guar/CuO composite. A simple sonochemical method has been used for the preparation of guar stabilized exfoliated graphite (GR-guar). The flower-like CuO on GR-guar and guar stabilized CuO (CuO-guar) composites were synthesized using a hydrothermal method. Cyclic voltammetric studies revealed that the GR-guar/CuO composite modified screen-printed carbon electrode (SPCE) had enhanced electro-reduction ability towards H2O2 than GR-guar and pristine graphite/CuO-guar modified SPCEs. Under optimized experimental conditions, the GR-guar/CuO composite modified electrode detects H2O2 in the response ranges from 0.02 to 1296.6 µM. The sensor shows a lower detection limit of 5.8 nM with high sensitivity. The as-prepared GR-guar/CuO composite sensor is highly reproducible and had excellent selectivity and practicality towards the detection of H2O2. Consequently, the fabricated sensor can be used for the accurate detection of H2O2 in real samples.

Designing Solid Materials from Their Solute State: A Shift in Paradigms toward a Holistic Approach in Functional Materials Chemistry.

"Non-classical" notions consider formation pathways of crystalline materials where larger species than monomeric chemical constituents, i.e., ions or single molecules, play crucial roles, which are not covered by the classical theories dating back to the 1870s and 1920s. Providing an outline of "non-classical" nucleation, we demonstrate that prenucleation clusters (PNCs) can lie on alternative pathways to phase separation, where the very event of demixing is primarily based on not the sizes of the species forming, as in the classical view, but their dynamics. Rationalizing, on the other hand, that precursors that can be analytically detected in pre-nucleation stages and that play a role in phase separation must be considered PNCs and cannot be explained by classical notions, we outline a variety of systems where PNCs are important. Indeed, in recent years, with the advent of "non-classical" theories, a primary focus of research concentrated on the fundamental understanding of oligomeric/polymeric and particulate species involved in nucleation and crystallization processes, respectively. At the same time, the near-to unfathomable potential of "non-classical" routes for the synthesis of inorganic functional materials slowly unfolds. An overview of recent developments in the fundamental and mechanistic understanding of "non-classical" nucleation and crystallization in this Perspective then allows us to map out the potential of cluster/particle-driven mineralization pathways to intrinsically tailor the properties of inorganic functional (hybrid) materials via structuration from the nano- to the mesoscale. This is of utter importance for the functionality and performance of materials, as it may even confer emergent properties such as self-healing. Biominerals-often formed via particle accretion mechanisms-demonstrate this impressively and thus can serve as a further source of inspiration how to exploit nonclassical crystallization routes for syntheses of structured and functional materials. These new avenues to synthetic approaches may finally provide a holistic material concept, in which fundamental chemistry and materials science synergistically alloy.

Konvencionalni i napredni adjuvansi u formulacijama vakcina - mineralni adsorbenti, nanočestični nosači i sistemi tipa mikroigala

In the era of modern vaccinology, limited immunogenicity of the most commonly used antigens has enforced the use of various adjuvants in vaccine formulations to achieve desired immune response. Aluminum-containing adjuvants have been, historically, the most widely used mineral immunostimulants, generally regarded as safe to use in human vaccines. The great academic progress in inorganic (nano)materials synthesis, structure control and functionalization design has led to a growing interest in innovative adjuvants such as clays, mesoporous silica nanoparticles, zinc oxide, iron oxide and iron hydroxide nanoparticles, etc. On the other hand, there has been an intention to use specific nanoparticulated antigen delivery systems, such as nanoemulsions, in order to protect antigens from premature proteolytic degradation and/or to improve antigen immunogenicity by facilitating antigen uptake and processing by antigen presenting cells. Simultaneously, numerous research efforts have been focused on the development of innovative technologies for antigen delivery into the skin (such as microneedles), with the aim to improve vaccine efficacy alongside with enhanced patient adherence, particularly in children population (noninvasive or minimally invasive administration). Therefore, this review deals with each of these approaches in more detail, with the special emphasis on examples of their use in vaccine formulations as well as on the factors influencing their efficacy and safety.

Cesium Oleate Precursor Preparation for Lead Halide Perovskite Nanocrystal Synthesis: The Influence of Excess Oleic Acid on Achieving Solubility, Conversion, and Reproducibility

In the colloidal synthesis of inorganic perovskite materials, cesium oleate (CsOL) is the most commonly used Cs precursor. Yet, despite its ubiquitous use in literature, CsOL has been observed to be insoluble at room temperature and leads to surprisingly inconsistent results in CsPbX3 nanocrystal synthesis, depending on the Cs salt from which the precursor is derived. We show that under the conditions used in most reports, the amount of oleic acid (OA) added, while stoichiometrically sufficient, still leads to incomplete conversion of the Cs salts to CsOL. This results in a mixture of Cs sources being present during the reaction, causing decreased homogeneity and reproducibility. When a 1:5 Cs:OA ratio is used, complete conversion is readily obtained, even under mild conditions, resulting in a precursor solution that is soluble at room temperature and yields identical synthetic results, regardless of the initial Cs source. Furthermore, 1H nuclear magnetic resonance (NMR) of solutions prepared using varyin...

Inorganic Nanomaterials for Restoration of Cultural Heritage: Synthesis Approaches towards Nanoconsolidants for Stone and Wall Paintings.

The synthesis of inorganic nanostructured materials for the consolidation of stone and wall paintings is reviewed. To begin, a description of the methods most commonly used to prepare nanoconsolidants is provided, particularly in the frame of colloid chemistry. Some concepts of the carbonation mechanism as well as the transport properties of some of these materials are addressed. An overview of the synthesis methods together with some of the application particularities of the distinct consolidants are presented thereafter. Furthermore, the requisites for efficient consolidants and some drawbacks of the nanoconsolidants are discussed.

Recent progress in the synthesis of inorganic particulate materials using microfluidics

Abstract Microfluidic systems have unique advantages originating from the miniaturization of real chemical processes. On this basis, the synthesis of inorganic materials, including micro- and nanomaterials, can be used to develop useful features, such as a uniform particle size distribution, morphology control, online monitoring, etc. In this review, we introduce and discuss the recent progress in the preparation of inorganic materials, mainly microfluidics systems. Furthermore, utilizing microfluidic devices, we present the basic principles and representative shape of microfluidic systems. In addition, the synthesis of various inorganic material particles using microfluidic systems, such as metal nanoparticles, metal oxide nanoparticles, semiconductor nanoparticles, organic-inorganic hybrid particles, surface functionalized particles, core-shell particles, and traditional porous materials, is introduced. Finally, we propose the future prospects of microfluidics in the synthesis of noble inorganic materials.

Crafting Inorganic Materials for Use in Energy Capture and Storage.

Harnessing solar energy effectively by the judicious use of photoactive inorganic/hybrid structures has become a pivotal requirement in the pursuit of environmentally benign technologies. The synthesis of new inorganic materials whose stoichiometry, structure, and activity can be tuned while maintaining a high level of architectural homogeneity and the successful evaluation of each material as a viable component in specific energy-capture- and storage-based applications are being presented here. Two of our current projects are detailed, involving (i) new 1D-structured hybrid perovskite that is a more temporally and thermally stable analogue of the oft-cited methylammonium lead iodide and (ii) a new electroactive material that can function not only as a conventional electrode in a battery but also, because of the material's inherent photoactivity, as a component in solar batteries. Hence, the concept that energy capture and energy storage can be coupled in a single device is also being detailed.

Leibniz‐Institute for Catalysis (LIKAT): From Basic Research to Practical Applications

Leibniz‐Institute for Catalysis (LIKAT): From Basic Research to Practical Applications

A zeolitic vanadotungstate family with structural diversity and ultrahigh porosity for catalysis

Design of the structure and composition of crystalline microporous inorganic oxides is of great importance in catalysis. Developing new zeolites is one approach towards this design because of the tunable pore system and high thermal stability. Zeolites are limited to main group elements, which limits their applications in redox catalysis. Another promising choice is zeolitic transition metal oxides providing both porosity and redox activity, thereby further expanding the diversity of porous materials. However, the examples of zeolitic transition metal oxides are rare. Here, we report a new class of zeolitic vanadotungstates with tunable frameworks exhibiting a large porosity and redox activity. The assembly of [W4O16]8− units with VO2+ forms two isomeric porous frameworks. Owing to the complex redox properties and open porosity, the vanadotungstates efficiently catalyse the selective reduction of NO by NH3. This finding provides an opportunity for design and synthesis of inorganic multifunctional materials for future catalytic applications.

Pseudomonas fluorescensAK Lipase Immobilization on MCM-48-Type Mesoporous Support in the Presence of Ionic Liquid

Abstract Pseudomonas fluorescens AK lipase was in situ immobilized on MCM-48-type mesoporous material employing the ionic liquid 1-hexadecyl-3-methylimidazolium chloride as a template for the inorganic material synthesis and also as an additive in the enzyme immobilization for lipase as a catalyst in chemical reactions—making it possible to reuse it. Storage stability, operational, and the potential for application in ester synthesis studies were performed. The support synthesis and AK lipase immobilization processes were efficient, presenting a 664% esterification yield and a 578 U/g enzymatic activity with 4 continuous reuse cycles, in addition to a conversion to the ester synthesis of ethyl and geranyl oleates of 14 and 18%, respectively. Thus, the results presented demonstrate the potential of using this mesoporous material in the enzymatic immobilization process.

Microfluidic approaches for the design of functional materials

Microfluidic systems, including microreactors, can precisely control an entire process and provide advantages, such as rapid mixing, fast heat and mass transfer due to miniaturization. Above all, the advantage of being easy to design and fabricate is the most attractive for the purposes of researchers. In the past two decades, it has become a research topic of great interest in the field of synthesis of chemicals and materials, due to these unique advantages. Furthermore, in recent years, studies are actively underway to design, construct, and compose the elements and functions of microfluidic devices for designing and synthesizing materials for specific applications or purposes. In this review, we will discuss the principles and forms of basic microfluidic devices, and discuss how microfluidic devices are used in the synthesis of polymeric and inorganic materials, particularly functional materials. Finally, we will present how microfluidic systems will be used in future materials research.

Nano-Sized Inorganic Energy-Materials by the Low-Temperature Molecular Precursor Approach.

The low-temperature synthesis of inorganic materials and their interfaces at the atomic and molecular level provides numerous opportunities for the design and improvement of inorganic materials in heterogeneous catalysis for sustainable chemical energy conversion or other energy-saving areas. Using suitable molecular precursors for functional inorganic nanomaterial synthesis allows for facile control over uniform particle size distribution, stoichiometry, and leads to desired chemical and physical properties. This Minireview outlines some advantages of the molecular precursor approach in light of selected recent developments of molecule-to-nanomaterials synthesis for renewable energy applications, relevant for the oxygen evolution reaction (OER), hydrogen evolution reaction (HER), and overall water-splitting.

Survey of new materials by solid state synthesis under external fields: high-pressure synthesis and microwave processing of inorganic materials

Survey of new materials by solid state synthesis under external fields: high-pressure synthesis and microwave processing of inorganic materials

3D‐Printed Microfluidic Devices for Materials Science

AbstractMicrofluidics (MFs) has emerged as a valuable and in some cases, unique platform for the synthesis and assembly of inorganic and polymeric materials. 3D printing enables time‐, labor‐, and cost‐efficient prototyping of MF devices, their durability during operation, and the ability to implement complex designs, however the applications of 3D‐printed MF devices in materials science are still in their infancy. Here, the synthesis and assembly of a diverse range of materials, including spraying‐based synthesis of inorganic NPs and conductive filaments, extrusion‐based fabrication of hydrogel fibers and sheets, and the preparation of composite solid films are reported. The properties are examined and potential applications of these materials are shown, the advantages of material fabrication in 3D‐printed MF devices are highlighted, and the directions for their further development are identified.

A versatile expression vector for the growth and amplification of unmodified phage display polypeptides

Proteins and polypeptides represent nature's most complex and versatile polymer. They provide complicated shapes, diverse chemical functionalities, and tightly regulated and controlled sizes. Several disease states are related to the misfolding or overproduction of polypeptides and yet polypeptides are present in several therapeutic molecules. In addition to biological roles; short chain polypeptides have been shown to interact with and drive the bio-inspired synthesis or modification of inorganic materials. This paper outlines the development of a versatile cloning vector which allows for the expression of a short polypeptide by controlling the incorporation of a desired DNA coding insert. As a demonstration of the efficacy of the expression system, a solid binding polypeptide identified from M13 phage display was expressed and purified. The solid binding polypeptide was expressed as a soluble 6xHis-SUMO tagged construct. Expression was performed in E. coli using auto-induction followed by Ni-NTA affinity chromatography and ULP1 protease cleavage. Methodology demonstrates the production of greater than 8 mg of purified polypeptide per liter of E. coli culture. Isotopic labeling of the peptide is also demonstrated. The versatility of the designed cloning vector, use of the 6xHis-SUMO solubility partner, bacterial expression in auto-inducing media and the purification methodology make this expressionun vector a readily scalable and user-friendly system for the creation of desired peptide domains.

Call for papers: MWRM 2018

Abstract submissions are being accepted for the 2018 Midwest Regional Meeting, which will take place Oct. 21–23 at the Iowa State Center Scheman Building in Ames, Iowa. Symposia will highlight advances in all areas of chemical research, education, industry, and their intersections with diverse scientific and technological domains. In addition to 16 technical symposia and a poster session, the meeting will feature a plenary lecture, the Midwest Award Lecture, an award symposium, an undergraduate program, workshops, and an instrument exhibition. The symposium sessions include “Biological Applications of Mass Spectrometry,” “Bioanalysis: Sensing, Separations & Spectroscopy,” “Carbon Capture, Utilization & Storage,” “Physical Organic Chemistry,” “Catalysts for Organic Synthesis,” “Inorganic Chemistry for All,” “Materials for Energy,” “Materials for Biomedicine,” “Materials for Optical, Magnetic & Electronic Devices,” “Materials & Interfaces,” “Inorganic Materials Synthesis,” “Solid-State NMR Spectroscopy: Mat...

Thermodynamic limit for synthesis of metastable inorganic materials.

Realizing the growing number of possible or hypothesized metastable crystalline materials is extremely challenging. There is no rigorous metric to identify which compounds can or cannot be synthesized. We present a thermodynamic upper limit on the energy scale, above which the laboratory synthesis of a polymorph is highly unlikely. The limit is defined on the basis of the amorphous state, and we validate its utility by effectively classifying more than 700 polymorphs in 41 common inorganic material systems in the Materials Project for synthesizability. The amorphous limit is highly chemistry-dependent and is found to be in complete agreement with our knowledge of existing polymorphs in these 41 systems, whether made by the nature or in a laboratory. Quantifying the limits of metastability for realizable compounds, the approach is expected to find major applications in materials discovery.

Manipulation of matter by electric and magnetic fields: Toward novel synthesis and processing routes of inorganic materials

The use of external electric and magnetic fields for the synthesis and processing of inorganic materials such as metals and ceramics has seen renewed interest in recent years. Electromagnetic energy can be utilized in different ways to improve or accelerate phase formation and stabilization, chemical ordering, densification and coarsening of particle-based materials (pore elimination and grain growth), and mechanical deformation (plasticity and creep). In these new synthesis and processing routes, the resulting microstructures and macroscopic material behavior are determined by the interaction of the applied fields with defects such as single or clustered point defects, dislocation networks, and interfaces. Multiscale experimental investigations and modeling are necessary to unveil the mechanisms underlying this field-assisted manipulation of matter.

High phase-purity 1T'-MoS2- and 1T'-MoSe2-layered crystals.

Phase control plays an important role in the precise synthesis of inorganic materials, as the phase structure has a profound influence on properties such as conductivity and chemical stability. Phase-controlled preparation has been challenging for the metallic-phase group-VI transition metal dichalcogenides (the transition metals are Mo and W, and the chalcogens are S, Se and Te), which show better performance in electrocatalysis than their semiconducting counterparts. Here, we report the large-scale preparation of micrometre-sized metallic-phase 1T'-MoX2 (X = S, Se)-layered bulk crystals in high purity. We reveal that 1T'-MoS2 crystals feature a distorted octahedral coordination structure and are convertible to 2H-MoS2 following thermal annealing or laser irradiation. Electrochemical measurements show that the basal plane of 1T'-MoS2 is much more active than that of 2H-MoS2 for the electrocatalytic hydrogen evolution reaction in an acidic medium.