Preparation Method Research Articles

Preparation of silicon foam supported CoMn catalysts and their catalytic performances in higher alcohol synthesis via syngas

A series of silicon foam supported CoMn catalysts were prepared using impregnation, precipitation, and hydrothermal methods. Combining the characterization techniques such as XRD, H2-TPR, N2 physical adsorption, TEM, and XPS, the effect of different catalyst preparation methods on the catalytic performance in the synthesis of higher alcohols from syngas was investigated. It is shown that there are Co2+(Co2C) and Co0 species on the surface of the catalyst. The active sites of Co2C-Co0 on the surface of the catalyst prepared by hydrothermal method have a good synergistic effect, which is conducive to the generation of alcohols. A higher proportion of Co2C also promotes the associative adsorption and insertion of CO, resulting in the highest alcohol selectivity. Under the reaction conditions of t=260 °C, p=5.0 MPa, GHSV=4500 h–1 and H2/CO(volume ratio)=2:1, the catalyst exhibited the best reaction performances with CO conversion of 11.1%, total alcohol selectivity of 34.7%, and C2+OH selectivity of 34.5%.

Formulation Design and Characterization of Nilotinib Polymeric Nanoparticles by Nanoprecipitation Technique for the Improved Drug Solubility and Dissolution Rate

Introduction: Nilotinib is a BCS class-IV poorly water-soluble kinase inhibitor drug, that was used for this study to prepare the polymeric nanoparticles by nanoprecipitation technique using Eudragit RL-100 and RS-100 as polymers, Killophore P-188 as a surfactant, and PEG 400 used as a non-volatile, and nontoxic solvent for the improvement of the drug solubility and dissolution rate. Method: The initial process and formulation variables are screened out based on the selected critical quality attributes such as drug release (%), particle size (nm), zeta potential (mV), and polydispersity index. The FT-IR and DSC studies reveal that the drug has no compatibility between the selected drug and the polymers and does not show any additional drug peaks after physical mixing and formulations. The prepared nanoparticles were further characterized to evaluate the particle size (nm), polydispersity index (PDI), zeta potential (mV), entrapment efficiency (%), and in-vitro drug release (%). From the in vitro drug release study, Eudragit RL-100 and Killophore P-188-based formulations showed optimum drug entrapment efficiency with improved drug solubility and dissolution rate in PEG 400 compared to Eudragit RS-100-based formulations. The accelerated stability data for the optimized formulation batch (F6) before and after storage conditions at 40±2 0C and 75±5% RH indicates that the optimized formulation (F6) is more stable for up to 6 months without changes in drug entrapment efficiency and in vitro dissolution rate. Dissolution kinetic data and diffusion exponent values suggested that optimized formulation followed the Higuchi model with a non-Fickian transport mechanism. Result: According to the results, the preparation method proposed in this study is the most suitable for generating polymeric nanoparticles of nilotinib for improved drug solubility and dissolution rate. Conclusion: The nilotinib-based polymeric nano-formulation proved a potential alternative for better drug release with an enhanced solubility rate.

Properties and characteristics of steam-exploded donkey bone powder and corresponding whole wheat cookies

Steam explosion was found to be the most effective preparation method for donkey bone powder, compared with non-treatment, autoclave and steam processing. And the effect of steam-exploded donkey bone powder (SEDBP) on the quality characteristics of whole wheat cookies was evaluated. Compared with untreated powder, particle size of SEDBP was reduced by 55.60 %, while oil- and water-holding capacity, water solubility and ABTS radical-scavenging rate significantly increased by 13.94 %, 26.86 %, 298.26 % and 91.47 %, respectively. Steam explosion enhanced protein digestibility from 32.17 % to 71.43 %, increased the Ca2+ release rate from 37.47 % to 47.82 %, and increased the release of 11 amino acids during digestion. SEDBP reduced the solvent retention capacity of flour blends and improved the color, hardness and spread ratio of whole wheat cookies. Cookies with 30 % SEDBP addition had better flavor, texture and scored the highest on overall acceptability. The results will help expand animal bone applications and develop nutrition-fortified foods.

A large language model-powered literature review for high-angle annular dark field imaging

Abstract High-angle annular dark field (HAADF) imaging in scanning transmission electron microscopy (STEM) has become an indispensable tool in materials science due to its ability to offer sub-Å resolution and provide chemical information through Z-contrast. This study leverages large language models (LLMs) to conduct a comprehensive bibliometric analysis of a large amount of HAADF-related literature (more than 41000 papers). By using LLMs, specifically ChatGPT, we were able to extract detailed information on applications, sample preparation methods, instruments used, and study conclusions. The findings highlight the capability of LLMs to provide a new perspective into HAADF imaging, underscoring its increasingly important role in materials science. Moreover, the rich information extracted from these publications can be harnessed to develop AI models that enhance the automation and intelligence of electron microscopes.

Synthesis, characterization, and double shielding performance for ultraviolet and short-wave blue light of ceria-based materials

In order to extend the photo-shielding range of ceria from the ultraviolet (UV) region (≤ 400 nm) to the high-energy short-wave blue light (BL) region (400–450 nm), three groups of ceria-based materials, including ceria nanoparticles (nano-CeO2), cerium-oxygen-sulfur (Ce-O-S) composites and samarium-cerium-oxygen-sulfur (Sm-Ce-O-S) composites, were prepared from the perspectives of improving the preparation method, non-metal doping and metal/non-metal co-doping. Although the three groups of as-prepared samples have similar phase composition, morphology and pore structure, the Sm-Ce-O-S composites show remarkable double shielding performance for UV light and short-wave BL. Compared with nano-CeO2 and Ce-O-S composites, Sm-Ce-O-S composites that retains the characteristics of n-type semiconductor exhibits a greater degree of lattice distortion, higher concentrations of Ce3+ (41.17%) and oxygen vacancy (77.29%), and narrower band gap (2.71 eV). Through the comparison of the three groups of samples, the order of modification degree from high to low is as follows: metal/non-metal co-doping > non-metal doping > improving the preparation method. This paper provides experimental and theoretical support for breaking through the bottleneck of ceria in the fields of UV shielding agents and catalysts.

Role of CsBr in structure and properties of new cesium bromo-borate glasses

Glasses of enlarged chemical composition in the xCsBr-(100-x)B2O3 system, with x = 30–80 mol% have been prepared and studied for the first time. The hydrothermal preparation method is used to prepare fine powdered samples. The X-ray Diffraction (XRD), Fourier Transform Infrared spectra (FTIR) and 11B Nuclear Magnetic Resonance (11B NMR) are the tools used to study the structure of glasses. Even at the high CsBr concentration (30–60 mol%), XRD results revealed an amorphous structure characterized most of the examined compositions. But glasses enriched with CsBr (70 and 80 mol%) possess some ordered sub-structures impeded in the main amorphous network. 11B NMR and FTIR spectroscopy confirmed the presence of BO3 triangle as the major and dominant structural units. The four coordinated boron (BO4), on the other hand, can't be detected in the all analyzed compositions. An extremely low concentration from BBr4 tetrahedral groups (boron coupled with Br) is formed. The B-O bonds of planar BO3 triangles, which are the fundamental units, were involved in the production of amorphous clusters of the type Cs4B5O9]Br. Density (D) measurement and calculating molar volume (Vm), packing density and free volume(Vf) have been studied. The added CsBr can't play a role of modifier but it might be inserted interstitially between the borate structural units causing increasing of molar volume and free space in the glass network structure. The results based on transmission electron microscopy (TEM-EDP) and X-ray diffraction pattern (XRD) are in good agreement, indicating that the amorphous-clustered species are developed in the studied glasses.

Novel experimental method for rate-independent triaxial tests under partial drainage condition

A novel and yet simple technique for partially drained triaxial tests while preserving the assumptions of an element test is presented. The approach is based on the defined adjustment of the bulk modulus of a fluid system consisting of water and gas. Monotonic triaxial compression tests on Karlsruhe fine sand with different initial densities, sample preparation methods, loading rates and sample dimensions demonstrate the feasibility of the novel method. A drainage factor Df is introduced, which describes the current state of the drainage possibility. This drainage factor is subjected to changes during the experiment.

A novel Zr-based metallic glass composite and its plasticizing mechanism

A novel Zr-based metallic glass composite was prepared utilizing a die casting process in this study. This composite utilizes high-porosity open-pored foam metal as the second phase and takes advantage of the unique distribution characteristics of this phase to achieve structural characteristics resembling hard regions surrounded by soft regions. This facilitates the formation and interleaving of numerous shear bands during the deformation process of the composite, resulting in work-hardening capability and favorable compressive plasticity. The results indicate that the compressive strength of the metallic glass composites containing 2.72% foamed Ni and 3.71% foamed Cu respectively does not decrease significantly compared to single-phase metallic glass, while their compressive plasticity increases from 1.60 ± 0.46% to 12.21 ± 1.04% and 13.01 ± 1.15%, respectively. This study not only uncovers the preparation method and plasticizing mechanism of a novel metallic glass composite, but also offers a fresh perspective for the design of high-plasticity metallic glass composites.

Nickel sulfide nanorods encapsulated in Nitrogen-Doped carbon on nickel foam in situ derived from Saccharomycetes cerevisiae for the selective oxidation of biomass

The design and development of an efficient catalyst for the electrocatalytic oxidation reaction of 5-hydroxymethylfurfural (HMF) require a novel, cost-effective, environmentally friendly, and safe preparation method. In this study, we synthesized nickel sulfide nanorods encapsulated by nitrogen-doped carbon on a nickel foam substrate (Ni3S2@NC/NF), derived in situ from Saccharomyces cerevisiae. The utilization of a gas-phase route facilitated the binding of C, N and S elements to the NF substrate. The resulting Ni3S2@NC/NF catalyst exhibited excellent electrocatalytic performance in the HMF oxidation reaction (HMFOR), achieving a complete conversion of HMF, a selectivity of 95.6 % for 2,5-furandicarboxylic acid, and a Faraday efficiency of 88.9 % at a potential of 1.45 V. Moreover, in situ electrochemical impedance spectroscopy revealed an enhanced charge transfer rate for the Ni3S2@NC/NF catalyst during the interfacial HMFOR. Additionally, the catalyst demonstrated outstanding stability after five cycles of electrolysis. Therefore, this work provides a valuable guide for using microorganisms as sources of C, N, and S in the targeted synthesis of metallic electrocatalysts.

Development of a multifunctional bio-based insulation material with corncob and silica aerogel

Bio-based insulation materials with superior comprehensive properties are crucial to building energy conservation. This study aims to develop a multifunctional bio-based insulation material that integrates good insulation, mechanical strength, and waterproofing. In this work, using corncob as the raw material, foamed geopolymer as the binder, silica aerogel and silicone oil as additives, a novel bio-based insulation material was prepared. Moreover, the effect of corncob size, silica aerogel content and silicone oil content on the microstructure, density, thermal conductivity, compressive strength, water absorption, moisture absorption and water contact angle properties were discussed. The results showed that, a desirable bio-based insulation material with a corncob size of 20 mesh, silica aerogel/geopolymer mass ratio (A/G) being 1.71 %, silica aerogel/ silicone oil mass ratio (A/O) being 0.2, is recommended, of which the thermal conductivity is 0.111 W/(m.K) with the compressive strength being 2.2 MPa, the density being 350 kg/m3, the water absorption being 7.1 %, the moisture absorption being 9.4 % and the water contact angle being 133°. With a simple preparation process, low cost and low energy consumption, this bio-based insulation material has good application prospects in buildings. Meanwhile, the preparation method of bio-based insulation materials proposed in this study provides new ideas for the development of multifunctional insulation materials in the future.

Fabrication of conductive composite hydrogels with excellent pressure sensitivity via in situ polymerization of ternary DES

In this paper, choline chloride, acrylamide and urea were used to prepare deep eutectic solvent (DES), and CS and N-CNTs were used as fillers to prepare composite hydrogels through in-situ polymerization. Using FTIR and SEM characterization analysis, the results showed that the pressure sensitivity and conductivity of the composite hydrogel were significantly improved after adding CS and N-CNTs. When the filler content reaches the highest level, the pressure sensitivity increases by 13 times and the conductivity reaches 2.05 mS/cm, which is 14.7 times that of the hydrogel without filler. This study provides a preparation method for composite hydrogels with excellent conductive properties and pressure sensitivity.

Present State in the Development of Aerogel and Xerogel and their Applications for Wastewater Treatment: A Review

Abstract: This comprehensive analysis investigates the current state of development and emerging applications of aerogels and xerogels in wastewater treatment. Aerogels and xerogels, which are characterized by their distinctive porosity architectures and extraordinary material qualities (low density and high surface area), have received much interest in recent years for their potential to transform the field of wastewater treatment. In this study, we present a complete overview of the synthesis processes and structural properties of these materials, highlighting current advancements and innovations. As adsorbents, catalysts, thermal insulation materials, or drug delivery matrices, they have been employed in a number of different disciplines. Aerogels and xerogels have demonstrated their adsorption capability by effectively collecting a wide spectrum of pollutants contained in wastewater. These include the removal of potentially hazardous and deleterious components such as metal ions and organic dyes, which are prevalent in wastewater streams, as well as other organic compounds. Our analysis not only covers the synthesis and applications of aerogels and xerogels, but it also highlights eco-friendly synthesis alternatives, in line with the growing demand for sustainable material preparation methods. Against the backdrop of rising global water concerns, this analysis highlights the promising potential of these materials to play a crucial role in providing sustainable wastewater treatment solutions, thereby establishing a critical future goal.

Preparation and Molecular Dynamic Simulation of Superfine CL-20/TNT Cocrystal Based on the Opposite Spray Method.

In view of the current problems of slow crystallization rate, varying grain sizes, complex process conditions, and low safety in the preparation of CL-20/TNT cocrystal explosives in the laboratory, an opposite spray crystallization method is provided to quickly prepare ultrafine explosive cocrystal particles. CL-20/TNT cocrystal explosive was prepared using this method, and the obtained cocrystal samples were characterized by electron microscopy morphology, differential thermal analysis, infrared spectroscopy, and X-ray diffraction analysis. The effects of spray temperature, feed ratio, and preparation method on the formation of explosive cocrystal were studied, and the process conditions of the pneumatic atomization spray crystallization method were optimized. The crystal plane binding energy and molecular interaction forces between CL-20 and TNT were obtained through molecular dynamic simulation, and the optimal binding crystal plane and cocrystal mechanism were analyzed. The theoretical calculation temperature of the binding energy was preliminarily explored in relation to the preparation process temperature of cocrystal explosives. The mechanical sensitivity of ultrafine CL-20/TNT cocrystal samples was tested. The results showed that choosing acetone as the cosolvent, a spraying temperature of 30 °C, and a feeding ratio of 1:1 was beneficial for the formation and growth of cocrystal. The prepared CL-20/TNT cocrystal has a particle size of approximately 10 μm. The grain size is small, and the crystallization rate is fast. The impact and friction sensitivity of ultrafine CL-20/TNT cocrystal samples were significantly reduced. The experimental process conditions are simple and easy to control, and the safety of the preparation process is high, providing certain technical support for the preparation of high-quality cocrystal explosives.

A preparation method for microstructure of flexible pressure sensors based on origami craft

With the development of flexible pressure sensors, an increasing number of microstructures and their preparation methods have been developed. However, how to reduce the cost and complexity of microstructure preparation while ensuring sensors’ performance and microstructure diversity remains a significant challenge. This paper explores the feasibility and diversity of origami craft in the microstructure preparation. Based on origami craft, various different microstructures, such as linear, cross, wrinkle and wave, could be prepared using low-cost silicone paper as mold material and simple steps. Due to the diversity of origami craft in microstructure preparation, our sensors with different microstructures also have their own advantage interval of pressure detection (0–4.4 kPa: the sensitivities of piezoresistive sensors with linear and cross microstructures are So = -0.31 kPa−1, St = -0.34 kPa−1; 4.4–13.3 kPa: the sensitivity of the piezoresistive sensor with wave microstructure is Swa = -0.028 kPa−1), some of the sensors have rapid response times, excellent response characteristics, repeatability, and hysteresis. Sensors designed for low-pressure applications can detect pressures as low as 22 Pa. Additionally, it was observed that they possess significant potential in human motion environments, office environments, and equipment testing environments. This indicates that origami craft offers excellent diversity and feasibility in the preparation of sensor microstructures.

Lignin-Based Composite Film and Its Application for Agricultural Mulching.

Agricultural mulching is an important input for modern agricultural production and plays an important role in guaranteeing food security worldwide. At present, polyethylene (PE) mulching is still commonly used in agricultural production in most countries around the world, which is non-biodegradable, and years of mulching have caused serious agricultural white pollution. Lignin is one of the three major components of plant cell walls, and it is also the main renewable natural aromatic compounds in nature. Lignin-based composite film materials are green, biodegradable, and show good prospects for development in the field of agricultural mulch. This paper introduces the types, structure, and application status of lignin, summarizes the preparation of lignin-based composite film materials and its latest research progress, focuses on the types, preparation methods, and application examples of lignin-based agricultural mulching, and looks forward to the future development prospects of lignin-based agricultural mulching.

Optimisation of pulsed laser deposited Ba1-xKxBiO3 thin films with tunable superconducting properties by control of K doping level, x

The mid-TC superconductor Ba1-XKXBiO3 (BKBO) exhibits different superconducting mechanisms depending on x, in the range ∼ 0.35–0.65. The optimal doping for the highest TC is reported to be around x = 0.4. To understand more about the dependence of the superconducting mechanism on x, high quality and reproducible epitaxial films with controlled x are needed. This has been challenging owing to the volatility of K and (to a lesser extent) Bi. In this work, we use pulsed laser deposition (PLD) with several novel process steps to achieve high-quality films in a reproducible way. These include a modified method for target preparation, a low NO2 growth pressure, and precise positioning of substrates in the PLD plume. Optimum TC films (32 K onset) were grown from an x = 0.4 target, i.e. with no excess K, as is normally used. Stable, higher K content films (made from an x = 0.45 target), were also grown. These x = 0.45 films had a lower TC (22.5 K onset), as expected for (K) overdoped films, with very high upper critical field, HC2 (0 K), and irreversibility field, Hirr (0 K), values, from linear extrapolation, of ∼ 31.7 T and ∼ 28.8 T, respectively. The growth methodology demonstrated in this work is highly beneficial for fundamental mechanistic studies of this complex superconductor on which there is renewed interest, and where controlled compositions and crystalline quality are currently limited.

Bowel preparation with linaclotide and 1 L polyethylene glycol plus ascorbic acid prior to colonoscopy in chronic constipated patients

Background and Aims Information on effective bowel preparation (BP) methods for patients with constipation is limited. We recently reported the efficacy of 1 L polyethylene glycol plus ascorbic acid (PEG-Asc) combined with senna for BP; however, this regimen was insufficient in patients with constipation. We hypothesized that the addition of linaclotide, which is approved for the treatment of chronic constipation, to 1 L PEG-Asc would yield results superior to those of senna in patients with constipation. Methods This was a retrospective, single-center study that included outpatients with constipation who underwent BP prior to colonoscopy between March and December 2019 (receiving 1 L PEG-Asc with 24 mg senna) and between January and October 2020 (receiving 1 L PEG-Asc with 500 mg linaclotide). Results A total of 543 patients with constipation were included, of whom 269 received linaclotide and 274 received senna. The rate of inadequate BP was significantly lower (11% vs 20%, p < 0.01) and the adenoma detection rate was significantly higher (54% vs 45%, p = 0.04) in the linaclotide group than in the senna group. Multivariate analysis revealed that the linaclotide regimen significantly reduced the risk of inadequate BP (odds ratio = 0.36, 95% confidence interval = 0.21–0.60, p < 0.01). Conclusions The linaclotide regimen significantly increased BP efficacy and the adenoma detection rate compared with the senna regimen without reducing tolerability and is therefore a promising new option for BP in patients with constipation.

Bioactive Polysaccharides from Gracilaria lemaneiformis: Preparation, Structures, and Therapeutic Insights.

Gracilaria lamaneiformis, a red seaweed, is an abundant source of bioactive polysaccharides with significant health-promoting properties. Nevertheless, the broad application of G. lamaneiformis in the nutraceutical and pharmaceutical sectors remains constrained due to the absence of comprehensive data. This review provides a detailed examination of the preparation methods, structural characteristics, and biological activities of G. lamaneiformis polysaccharides (GLPs). We explore both conventional and advanced extraction techniques, highlighting the efficiency and yield improvements achieved through methods such as microwave-, ultrasonic-, and enzyme-assisted extraction. The structural elucidation of GLPs using modern analytical techniques, including high-performance liquid chromatography, gas chromatography, and nuclear magnetic resonance spectroscopy, is discussed, providing comprehensive insights into their molecular composition and configuration. Furthermore, we critically evaluate the diverse biological activities of GLPs, including their antioxidant, anti-inflammatory, antitumor, and gut microbiota modulation properties. This review underscores the therapeutic potential of GLPs and suggests future research directions to fully harness their health benefits.

Total organic carbon quantification in soils and sediments: Performance test of a modified sample preparation method

The total organic carbon (TOC) concentration of particulate samples is a key parameter to characterize soils and sediments. To demonstrate the applicability and reliability of a modified sample preparation method for the direct measurement of TOC contents in suspended particulate samples, we analyzed five certified reference materials (CRMs) with varying TOC concentrations using a Shimadzu TOC-L CPH analyzer. Measured values were calibrated with a multi-point curve that cover the full range of the expected TOC concentrations and the results were validated using statistical values and measures. The method validation reveals that the measurements are accurate and precise for CRMs from marine and soil contexts, but show a low accuracy for the CRM containing polycyclic aromatic hydrocarbons (PAHs). This demonstrates the applicability and reliability of the modified preparation method for direct TOC determination of suspended particulate samples. Therefore, it is relevant for a broader community, beyond geosciences, and for users employing devices of other manufacturers to analyze TOC in suspended particulate samples.•Modified preparation method uses reduced sample weights and yields accurate and precise results.•Cost-efficient and environmentally friendly alternative: reduces waste by saving acid and ultrapure water.•Avoids incomplete dissolution of dolomite by heating acidified samples.

A Comprehensive Review on Co-Crystals: Transforming Drug Delivery with Enhanced Solubility and Bioavailability

Poor solubility and bioavailability of various drug compounds are the biggest challenges faced by researchers and industrialists, hindering their therapeutic efficacy. Researchers have developed a versatile approach to enhance the solubility and bioavailability of the drug i.e., co-crystallization. Pharmaceutical co-crystals are solid, crystalline materials consisting of API and co-formers that have supramolecular chemistry with one another. Co-crystallization helps in enhancing a drug’s physico-chemical properties, such as bioavailability, solubility and dissolution, preserving its therapeutic effect. The API and co-former in co-crystals are bound to each other via hydrogen bonding, π-stacking, and Van der Waals forces. Several methods to prepare co-crystals, such as solvent evaporation method, grinding method, cooling crystallization method, etc, and various research reports, including all the methods of preparation are discussed in this review article. Conventional marketed products and patents on co-crystals are also included. Data has been gathered, and relevant literature reports have been examined utilizing a variety of search engines, including Google Scholar, ScienceDirect, Pubmed, and Google patents. After reviewing the literature, the researchers found that the cocrystallization method is one the simplest method to enhance drug bioavailability and solubility. Moreover, it enhances the pharmacokinetics parameters, pharmacodynamics properties, and melting point of the drug. In this review article, the researchers have compiled the recent literature reports on enhanced drug solubility via co-crystallization method. The researchers concluded that this review article can help other researchers by providing them with recent literature on this article and can compare the various methods of enhancing drug solubility and bioavailability. It also consists of compiled data of patents and marketed formulations prepared by the co-crystallization technique. Thus, co-crystallization could be established as a versatile approach for enhancing drug solubility and bioavailability.