ZnCl2-assisted Synthesis of ZnSe Polycrystal

A chemical-assisted element direct-reaction method is developed to synthesize ZnSe compound semiconductor material at a relatively low temperature (～1000 C). ZnSe polycrystal was obtained in the closed-tube systems with Zn-Se, Zn-Se-Zn(NH3)2Cl2, Zn-Se-NH4Cl and Zn-Se-ZnCl2. The as-synthesized samples were tested by X-ray diffraction (XRD), thermogravimetric analysis (TGA) and analyzed by thermodynamic numerical method. The results demonstrate that the synthesis efficiency is higher than 99.96% for Zn-Se-ZnCl2 system at around 1000 C for 3 weeks. It also exhibits that not only temperature, but also low apparent ratio of volume and surface area of the source materials and higher ZnCl2 content are required to achieve high synthesis efficiency. A SeCl transporting reaction synthesis process is proposed based on the thermodynamic analysis.     

Facile synthesis of carbon coated LiFePO4 nanocomposite with excellent electrochemical performance through in situ formed lithium stearate pyrolysis route

Carbon coated LiFePO₄ (LiFePO₄/C) nanocomposite is successfully synthesized at a comparatively low temperature (400 °C) via a pyrolysis process of in situ formed lithium stearate. The obtained products are characterized by X-ray diffraction, electron microscopy, thermogravimetry, infrared and X-ray photoelectron spectroscopy. Experimental results indicate that the in situ formed lithium stearate can decompose at ∼290 °C, which is beneficial for the formation of carbon coating and reduction of Fe³⁺ species, and then the crystallized LiFePO₄/C nanocomposite can be formed at 400 °C without other intermediate products. As cathode material of Li-ion battery, the obtained LiFePO₄/C nanocomposite exhibits a good rate and cycling performance with a high discharge capacity of ∼160 mAh g⁻¹ (>94% theoretical capacity of LiFePO₄) at a current density of 1 C (170 mA g⁻¹), and ∼96% of its initial capacity can be retained after 200 charging/discharging cycles. Even at a high current density (10 C), the LiFePO₄/C nanocomposite still presents a discharge capacity as high as ∼100 mAh g⁻¹. The excellent electrochemical performances of the present LiFePO₄/C nanocomposite mainly originate from the good crystallinity, small particles and enhanced electronic conductivity of the materials coated and linked by carbon layers.     

铝酸钠溶液深度脱硅

叙述了硅在铝酸钠溶液中的存在状态，指出了在碱法生产氧化铝过程中铝酸钠溶液深度脱硅的重要性。介绍了铝酸钠溶液深度脱硅研究现状，讨论了Ca（OH）2、C3AH6（立方水合铝酸钙）、C4AHn（六方水合铝酸钙）、HCAC（水合碳铝酸钙）、HSAC（水合硫铝酸钙）等含钙化合物深度脱硅机理。在此基础上指出了铝酸钠溶液脱硅的研究方向。     

Evaluation of different screening methods to understand the dissolution behaviors of amorphous solid dispersions

Objective: The objectives of the current study were to understand the dissolution behaviors of amorphous solid dispersions (ASD) using different screening methods and their correlation to the dissolution of formulated products.

Materials and methods: A poorly soluble compound, compound E, was used as a model compound. ASDs were prepared with HPMC, Kollidon VA64 and Eudragit EPO using hot-melt extrusion. Different techniques including precipitation, powder, capsule and compact dissolution and the dissolution of formulated products were conducted in USP simulated gastric fluid using a USP II dissolution apparatus.

Results and discussions: It was found that a precipitation study could generally predict powder, capsule and compact dissolution. Yet, it was recommended to run the dissolution at a higher paddle speed or for a longer duration to improve the predictability. It was also recommended to run powder, capsule and compact dissolution at both slow and high speeds to gain insights into wetting, dispersion and the dissolution of a system. Sometimes, capsule or compact dissolution could not be predicted by precipitation or powder dissolution due to plug formation. In this case, properly designed dosage forms were needed to break up this plug to optimize the dissolution profiles. On the contrary, formulations and dissolution conditions would have minimal effects on the dissolution profiles of a fast-dissolving solid dispersion.

Conclusions: Different techniques are available to select the right polymers to optimize dissolution behaviors. However, it is important to understand the merits and limitations of each technique in order to optimize the formulations for amorphous solid dispersions.     

Alumina‐Supported CoFe Alloy Catalysts Derived from Layered‐Double‐Hydroxide Nanosheets for Efficient Photothermal CO2 Hydrogenation to Hydrocarbons

A series of novel CoFe‐based catalysts are successfully fabricated by hydrogen reduction of CoFeAl layered‐double‐hydroxide (LDH) nanosheets at 300–700 °C. The chemical composition and morphology of the reaction products (denoted herein as CoFe‐x) are highly dependent on the reduction temperature (x). CO₂ hydrogenation experiments are conducted on the CoFe‐x catalysts under UV–vis excitation. With increasing LDH‐nanosheet reduction temperature, the CoFe‐x catalysts show a progressive selectivity shift from CO to CH₄, and eventually to high‐value hydrocarbons (C₂₊). CoFe‐650 shows remarkable selectivity toward hydrocarbons (60% CH₄, 35% C₂₊). X‐ray absorption fine structure, high‐resolution transmission electron microscopy, Mössbauer spectroscopy, and density functional theory calculations demonstrate that alumina‐supported CoFe‐alloy nanoparticles are responsible for the high selectivity of CoFe‐650 for C₂₊ hydrocarbons, also allowing exploitation of photothermal effects. This study demonstrates a vibrant new catalyst platform for harnessing clean, abundant solar‐energy to produce valuable chemicals and fuels from CO₂.     

Optimization of single mode fibre sensors to detect organic vapours

The construction of single mode optical fibre (SMF) sensors to handle with volatile organic compounds (VOCs), has been optimized to operate at the third telecommunication window (1550 nm). The main motivation is to take advantage of the photonic devices used in telecommunication systems that makes easier sensors multiplexing. Moreover, the low transmission attenuation at that wavelength offers the possibility of remote sensing. The sensing materials used suffer reversible structural alterations in the presence of VOC, such as colour change, which are detectable with a photonic system. Following the Electrostatic Self Assembly method (ESAm), a nanostructure is constructed onto cleaved ended SMF, which is doped with a sensing material. The fabrication of this type of sensors was focused on multimode fibres (MMF) and in the visible spectral range (VIS) so far. The implementation has been adapted to SMF and to operate around 1550 nm, specifically, by easing the adsorption of the VOCs molecules. It has been observed that the sensing material affects the morphology of the nanostructures as well and so, to the sensors response. The devices implemented show a potential use in the identification of single and complex mixtures of VOCs.     

Thiogenistein—Antioxidant Chemistry,Antitumor Activity,and Structure Elucidation of New Oxidation Products

Isoflavonoids such as genistein (GE) are well known antioxidants. The predictive biological activity of structurally new compounds such as thiogenistein (TGE)–a new analogue of GE–becomes an interesting way to design new drug candidates with promising properties. Two oxidation strategies were used to characterize TGE oxidation products: the first in solution and the second on the 2D surface of the Au electrode as a self-assembling TGE monolayer. The structure elucidation of products generated by different oxidation strategies was performed. The electrospray ionization mass spectrometry (ESI-MS) was used for identifying the product of electrochemical and hydrogen peroxide oxidation in the solution. Fourier transform infrared spectroscopy (FT-IR) with the ATR mode was used to identify a product after hydrogen peroxide treatment of TGE on the 2D surface. The density functional theory was used to support the experimental results for the estimation of antioxidant activity of TGE as well as for the molecular modeling of oxidation products. The biological studies were performed simultaneously to assess the suitability of TGE for antioxidant and antitumor properties. It was found that TGE was characterized by a high cytotoxic activity toward human breast cancer cells. The research was also carried out on mice macrophages, disclosing that TGE neutralized the production of the LPS-induced reactive oxygen species (ROS) and exhibits ABTS (2,2′-azino-bis-3-(ethylbenzothiazoline-6-sulphonic acid) radical scavenging ability. In the presented study, we identified the main oxidation products of TGE generated under different environmental conditions. The electroactive centers of TGE were identified and its oxidation mechanisms were proposed. TGE redox properties can be related to its various pharmacological activities. Our new thiolated analogue of genistein neutralizes the LPS-induced ROS production better than GE. Additionally, TGE shows a high cytotoxic activity against human breast cancer cells. The viability of MCF-7 (estrogen-positive cells) drops two times after a 72-h incubation with 12.5 μM TGE (viability 53.86%) compared to genistein (viability 94.46%).     

Facile Microwave Assisted Synthesis of Silver Nanostars for Ultrasensitive Detection of Biological Analytes by SERS

We report a very simple, rapid and reproducible method for the fabrication of anisotropic silver nanostars (AgNS) that can be successfully used as highly efficient SERS substrates for different bioanalytes, even in the case of a near-infra-red (NIR) excitation laser. The nanostars have been synthesized using the chemical reduction of Ag⁺ ions by trisodium citrate. This is the first research reporting the synthesis of AgNS using only trisodium citrate as a reducing and stabilizing agent. The key elements of this original synthesis procedure are rapid hydrothermal synthesis of silver nanostars followed by a cooling down procedure by immersion in a water bath. The synthesis was performed in a sealed bottom flask homogenously heated and brought to a boil in a microwave oven. After 60 s, the colloidal solution was cooled down to room temperature by immersion in a water bath at 35 °C. The as-synthesized AgNS were washed by centrifugation and used for SERS analysis of test molecules (methylene blue) as well as biological analytes: pharmaceutical compounds with various Raman cross sections (doxorubicin, atenolol & metoprolol), cell lysates and amino acids (methionine & cysteine). UV-Vis absorption spectroscopy, (Scanning) Transmission Electron Microscopy ((S)TEM) and Atomic Force Microscopy (AFM) have been employed for investigating nanostars’ physical properties.     

SYNTHESIS OF AROMA COMPONENTS DURING THE SPONTANEOUS FERMENTATION OF LAMBIC AND GUEUZE

Lambic is a type of Belgian beer obtained by spontaneous fermentation of wort. The fermentation in casks takes almost two years, and after that period the beer may be re-fermented in bottles and is then called gueuze. To gain insight into the many microbiological transformations occurring during this process, a qualitative and quantitative study of several components formed over a two-year period was undertaken. It was found that lambic and gueuze are characterized by high contents of ethyl acetate, ethyl lactate, lactic acid and acetic acid. Two phases of fermentation may be distinguished: a primary phase lasting for about three months during which almost all the ethanol and higher alcohols are formed and a very long secondary phase during which lactic acid is formed first, followed by ethyl lactate. Some lower fatty acids, including all the acetic acid, are made at the very beginning of the first phase. An important part of the ethyl acetate is made during the first phase but the amounts increase slowly to high levels during the second phase. Unusually low amounts of isoamyl acetate are detected. Several components are above the reported threshold levels of taste and are thus probably involved in the genesis of the typical aroma of lambic and gueuze. These results will allow a further study of the relations between the components found and the microbial populations involved in the spontaneous fermentation inherent in the brewing of lambic and gueuze.     

钢中铈与锡相互作用的研究

 采用中频真空感应熔炼炉、X射线衍射仪、金相显微镜、电子探针、显微硬度计等实验分析方法,研究了稀土金属铈与低熔点金属锡在钢中的相互作用。结果表明,钢液中铈和锡浓度均较高的条件下,铸态试样中可析出化合物Ce3Sn7相,沿晶界分布。经奥氏体区高温退火处理,钢中的Ce3Sn7相化合为三元FeCe3Sn6相。退火状态下FeCe3Sn6相的显微硬度大于基体的显微硬度。FeCe3Sn6相在干燥器内稳定,在纯净水和酸性水溶液中不稳定。