The surface carboxyl group of carbonaceous microspheres effects on the synthesis and structure of SiOC ceramics

In this study, C/SiOC and C/SiO₂ composites were prepared by using carbonaceous microspheres with different surface functional groups. Carbonaceous microspheres based on hydrothermal reaction of glucose contains hydroxyl group, while the surface carboxyl group increases after NaOH etching. The hydroxyl group increases the oxygen-enriched structural units of SiOC ceramics, and the C spheres are closely enwrapped in SiOC matrix after pyrolysis at 900 °C. However, the interfacial reaction of surface carboxyl with Si–OH results in the formation of cristobalite SiO₂, and C spheres are not only encased inside the SiOC matrix, but also dispersed outside of SiOC ceramics. After removal of C via calcination at 500 °C for 5 h, C/SiOC and C/SiO₂ composites are transformed into amorphous SiO₂ and cristobalite SiO₂, respectively. The thermogravimetric analysis indicates the oxidation resistance of SiOC is superior to that of C and SiO₂.     

Chitosan Microspheres as Carriers for pH‐Indicating Species in Corrosion Sensing

Chitosan microspheres containing bromocresol green, cresol red, and phenolphthalein for corrosion detection, through pH change, are synthesized in order to be used in protective coatings for aluminium alloys. Microspheres containing corrosion detection species are characterized morphologically (SEM) and physico‐chemically (FTIR, TGA). Release studies (UV–vis) are performed in corrosion‐promoting conditions (pH, NaCl), and detection studies by immersion in media associated with corrosion activity while microspheres' sensing activity is evaluated visually. Electrochemical characterization of AA2024 substrates in the presence of chitosan spheres is performed to understand material performance, and a color change is observed as a result of local pH increase in cathodic areas when corrosion takes place. These findings can be correlated with the results from release studies and seem a promising approach for corrosion sensing purposes, not only because pH increase is possible to detect due to corrosion, but also because chitosan is considered an environmentally friendly material.     

Platinum nanoparticles anchored on aminated silica@PEDOT-PSS hybrid for enhanced methanol oxidation electrocatalysis

Direct methanol fuel cell (DMFC) with near-zero pollution emission, large energy density, and low operating temperature provides a beneficial and sustainable way for alleviating fossil energy crisis and ecological pollution issues. In this work, a systematic protocol was explored for the design of novel electrocatalyst based on PEDOT-PSS coated amino-functionalized SiO₂ microspheres (SiO₂–NH₂@PEDOT-PSS) support, and then Pt nano-particles (NPs) were uniformly anchored for the anodic process of DMFCs. Characterization techniques, e.g. X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed that the dispersity and homogeneity of Pt NPs on the surface of SiO₂–NH₂@PEDOT-PSS were markedly improved due to PEDOT-PSS modification, and the distribution of Pt NPs was in a smaller mean-size ~2.8 nm. Subsequently, X-ray photoelectron spectroscopy (XPS) study exposed fast electron shift phenomenon from SiO₂–NH₂@PEDOT-PSS support to Pt NPs in the catalyst. The various electrochemical tests such as cyclic voltammetry (CV), chronoamperometry (CA) and impedance spectroscopy (EIS) revealed that the prepared Pt/SiO₂–NH₂@PEDOT-PSS catalyst presented higher electrocatalytic efficacy, excellent durability with improved CO-tolerance towards methanol oxidation reaction rather than commercial Pt/C catalyst. These distinctive physical and chemical features of designed catalyst raise the spirit to design an efficient electrocatalyst based on Pt/SiO₂–NH₂@PEDOT-PSS in DMFC applications.     

中低温煤焦油基炭微球的制备

通过馏分切割、温和加氢相结合对中低温煤焦油进行精制处理，精制后的原料采用分级热聚制备中间相炭微球。考察了精制处理条件对原料性质、中间相炭微球宏观外貌及微晶结构的影响。采用FTIR、GC-MS、族组成、元素分析对原料进行表征，采用SEM、XRD对中间相炭微球进行表征。结果表明：中低温煤焦油中300～430℃馏分油是制备中间相炭微球的较佳馏分。300～430℃馏分油中正庚烷可溶物（HS）质量分数高达84.76%，吡啶不溶物（PI）质量分数低至0.23%，杂原子含量低，芳烃化合物的环数为2～4环。300～430℃馏分油在T_H=350℃、p=8MPa、t=1.5h、剂油比1∶40（质量比）的条件下温和加氢得到的精制原料，经420℃热聚6h得制备的中间相炭微球宏观外貌、微晶结构较好。中低温煤焦油基炭微球的粒径范围为5～15μm，小球表面光滑，微观结构为地球仪型，经1450℃高温煅烧后，石墨化度达到12.33%。     

Fabrication of zinc‐loaded hollow glass microspheres (HGMs) for hydrogen storage

The greatest challenge for a feasible hydrogen economy lies on the production of pure hydrogen and the materials for its storage with controlled release at ambient conditions. Hydrogen with its great abundance, high energy density and clean exhaust is a promising candidate to meet the current global challenges of fossil fuel depletion and green house gases emissions. Extensive research on hollow glass microspheres (HGMs) for hydrogen storage is being carried out world‐wide, but the right material for hydrogen storage is yet underway. But many other characteristics, such as the poor thermal conductivity etc. of the HGMs, restrict the hydrogen storage capacity. In this work, we have attempted to increase the thermal conductivity of HGMs by ZnO doping. The HGMs with Zn weight percentage from 0 to 10 were prepared by flame spheroidization of amber‐colored glass powder impregnated with the required amount of zinc acetate. The prepared HGMs samples were characterized using field emission‐scanning electron microscope (FE‐SEM), environmental SEM (ESEM), high‐resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy and X‐ray diffraction (XRD) techniques. The deposition of ZnO on the microsphere walls was observed using FE‐SEM, ESEM and HRTEM which was further confirmed using the XRD and ultraviolet–visible absorption data. The hydrogen storage studies done on these samples at 200 °C and 10‐bar pressure for 5 h showed that the hydrogen storage increased when the Zn percentage in the sample increased from 0 to 2%. The percentage of zinc beyond 2, in the microspheres, showed a decline in the hydrogen storage capacity. The closure of the nanopores due to the ZnO nanocrystal deposition on the microsphere surface reduced the hydrogen storage capacity. The hydrogen storage capacity of HAZn2 was found 3.26 wt% for 10‐bar pressure at 200 °C. Copyright © 2015 John Wiley & Sons, Ltd.     

Study of physicochemical properties of flutamide-loaded Ocimum basilicum microspheres with ex vivo mucoadhesion and in vitro drug release

Drug which shows extensive first pass effect is difficult task that, needs to be solved by formulators in the pharmaceutical science. The low oral bioavailability (49%) of flutamide may be due to poor wettability, low aqueous solubility and extensive first pass effect. The aim of present investigation was to prepare flutamide loaded microspheres and incorporate it into suppositories for rectal delivery to avoid first pass effect and enhance residence time. Flutamide loaded mucoadhesive microspheres of Ocimum Basilicum mucilage (OBM) were prepared using spray drying and characterized by percent production yield, encapsulation efficiency, particle size, zeta potential, polydispersity index, DSC, SEM, XRPD, in vitro drug release and stability studies. Moreover, ex vivo mucoadhesion was investigated using falling liquid film technique to determine the adhesion of microspheres to sheep rectal mucosa. The microspheres had nearly spherical shape and size about 2.53?μm. The encapsulation efficiency and mucoadhesion of optimized formulation MBF10 were found to be 69.6?±?2.3% and 89.01?±?2.18%, respectively. Percent CDR of optimized flutamide loaded mucoadhesive microspheres was found to be 88.7?±?1.3 at 7?h. In conclusion, OBM microparticles based suppository could be used to deliver drug through rectal delivery.     

Feasible Preparation of a Thin‐Film Composite Nanofiltration (TFC NF) Membrane with Enhanced Skin–Substrate Adhesion and Compaction Resistance: In Situ Construction of Rigid–Flexible Polymer Composited Microspheres (CPs) in the Casting Solution

Novel microspheres (CPs) composited by rigid and flexible polymers are synthesized and embedded in the supporting membranes to enhance both the skin–substrate adhesion and compaction resistance of the thin‐film composite (TFC) nanofiltration membranes. The CPs are in situ formed in the casting solution after the rigid poly(p‐phenylene terephthamide) (PPTA) is produced in the flexible poly(m‐phenylene isophthalamide) (PMIA) solution. Then the PPTA/PMIA in situ blending membranes are prepared by using the NIPs method, and the TFC NF membranes are fabricated via interfacial polymerization on them. The CPs are characterized via polarizing microscopy and TEM. The surface morphology and chemical composition of the blended membranes are characterized by using FESEM, AFM, FTIR, and WCA, respectively. As the results show, the supporting membrane with higher PPTA content exhibits higher permeability, thermal stability, and compaction resistance. Moreover, the adhesion strength between the TFC functional layer and the supporting membrane is improved significantly. It is proposed that this improvement can be attributed to the CPs that are exposed on the top surface of the supporting membrane, which leads to a great enhancement because of the anchoring effect between the functional layer and the CPs.     

Compound surfactant-based emulsion method for the preparation of high-porosity alumina microspheres

Porous alumina microspheres have attracted significant attention owing to their high mechanical strength and excellent chemical and thermal stability. The emulsion method is considered as a simple and controllable method for the preparation of inorganic microspheres. However, preparing alumina microspheres with the emulsion method is challenging because the emulsification of the precursor is inhibited by the rapid hydrolysis of aluminum alkoxide. Herein, we report a new emulsion method for the preparation of high-porosity alumina microspheres using a combination of ionic and non-ionic surfactants; in this method, the compound surfactants act as a template agent to guide aluminum alkoxide to form a lamellar structure through self-assembly. The decomposition of the templating agent and transformation of the alumina crystal at a high temperature result in structural collapse and formation of lamellar pores. Compound surfactants increased the spheroidization rate of the emulsion from 47% to 63% after hydrolysis, whereas the particle size was decreased by almost half. Additionally, the morphology and porosity of the alumina microspheres were changed. With increasing anionic surfactant content, the porosity increased initially and then decreased. The porosity of the alumina microspheres reached a maximum value of 76% at the 1:1 mass ratio of the non-ionic to anionic surfactants. Heat treatment was found to change the size of lamellar pores, with the pore diameter reaching maximum value at 1300 °C. The compound surfactants also increased the compressive stress and specific surface area of the porous alumina microspheres.