A Green and Facile Solid-state Synthesis Method for the Preparation of Diazenecarboxamide Azo Compounds with Potassium Ferricyanide and Sodium Hydroxide System

Eleven new-typed azo compounds were synthesized in good yields by dehydrogenating the corresponding aryl substituted semicarbazides using potassium ferricyanide and sodium hydroxide system under solid-state conditions.

Synthesis methods and powder quality of titanium monocarbide

Titanium monocarbide(TiC),which is the most stable titanium-based carbide,has attracted considerable interest in the fields of energy,catalysis,and structural materials due to its excellent properties.Synthesis of high-quality TiC powders with low cost and high efficiency is crucial for industrial applications;however major challenges face its realization.Herein,the methods for synthesizing TiC powders based on a reaction system are reviewed.This analysis is focused on the underlying mechanisms by which synthesis methods affect the quality of powders.Notably,strategies for improving the synthesis of highquality powders are analyzed from the perspective of enhancing heat and mass transfer processes.Furthermore,the critical issues,challenges,and development trends of the synthesis technology and application of high-quality TiC powder are discussed.

An Efficient Solid-State Synthesis of N-Aryl-2-phenyldiazenecarboxamides

A new and ancient solid-state reaction using K3Fe(CN)(6)/KOII to oxidize diaryl semicarbazides for preparing azo compounds has been reported. Nine N-aryl-2-phenyl-diazenecarboxamides have been synthesized in excellent yields with simple instrument.

Multiscale strain alleviation of Ni-rich cathode guided by in situ environmental transmission electron microscopy during the solid-state synthesis

Ni-rich layered oxides are one of the most promising cathode materials for Li-ion batteries due to their high energy density.However,the chemomechanical breakdown and capacity degradation associated with the anisotropic lattice evolution during lithiation/delithiation hinders its practical application.Herein,by utilizing the in situ environmental transmission electron microscopy(ETEM),we provide a real time nanoscale characterization of high temperature solid-state synthesis of LiNi_(0.8)CO_(0.1)Mn_(0.1)O_(2)(NCM811) cathode,and unprecedentedly reveal the strain/stress formation and morphological evolution mechanism of primary/second ary particles,as well as their influence on electrochemical performance.We show that stress inhomogeneity during solid-state synthesis will lead to both primary/secondary particle pulverization and new grain boundary initiation,which are detrimental to cathode cycling stability and rate performance.Aiming to alleviate this multiscale strain during solid-state synthesis,we introduced a calcination scheme that effectively relieves the stress during the synthesis,thus mitigating the primary/secondary particle crack and the detrimental grain boundaries formation,which in turn improves the cathode structural integrity and Li-ion transport kinetics for long-life and high-rate electrochemical performance.This work remarkably advances the fundamental understanding on mechanochemical properties of transition metal oxide cathode with solid-state synthesis and provides a unified guide for optimization the Ni-rich oxide cathode.

Sustainable solid-state synthesis of uniformly distributed PdAg alloy nanoparticles for electrocatalytic hydrogen oxidation and evolution

New sustainable syntheses based on solid-state strategies have sparked enormous attention and provided novel routes for the synthesis of supported metallic alloy nanocatalysts(SMACs).Despite considerable recent progress in this field,most of the developed methods suffer from either complex operations or poorly controlled morphology,which seriously limits their practical applications.Here,we have developed a sustainable strategy for the synthesis of PdAg alloy nanoparticles(NPs)with an ultrafine size and good dispersion on various carbon matrices by directly grinding the precursors in an agate mortar at room temperature.Interestingly,no solvents or organic reagents are used in the synthesis procedure.This simple and green synthesis procedure provides alloy NPs with clean surfaces and thus an abundance of accessible active sites.Based on the combination of this property and the synergistic and alloy effects between Pd and Ag atoms,which endow the NPs with high intrinsic activity,the PdAg/C samples exhibit excellent activities as electrocatalysts for both the hydrogen oxidation and evolution reactions(HOR and HER)in a basic medium.Pd9Ag1/C showed the highest activity in the HOR with the largest j0,m value of 26.5 A g Pd^–1 and j0,s value of 0.033 mA cmPd^–2,as well as in the HER,with the lowest overpotential of 68 mV at 10 mA cm^–2.As this synthetic method can be easily adapted to other systems,the present scalable solid-state strategy may open opportunity for the general synthesis of a wide range of well-defined SMACs for diverse applications.

Ba_2SbGaS_5 : Solid-state Synthesis, Crystal and Electronic Structures, and Property Characterization

Single crystal of Ba2SbGaSs has been synthesized by the high temperature solidstate reaction method. The compound crystallizes in the orthorhombic space group Pnma with a = 12.177（4）, b = 8.880（3）, c = 8.982（3） A, V= 971.4（6） A3, Z = 4, De = 4.284 g/cm3,μ = 14.487 mm-1, F（000） - 1096, the final R = 0.0171 and wR = 0.0384 for all data. The structure comprises an infinite one-dimensional 1∞[SbGaS5]4- anionic chain constructed from the GaS4 tetrahedra and the SbS5 polyhedra via sharing edge alternately. The paralleled 1∞[SbGaS5]4anionic chains engage with each other and form the two-dimensional Sb-Ga-S layer perpendicular to a-axis with the isolated Ba2＋ cations arranged between layers. The IR spectrum and the UV-Vis spectrum have been investigated. Also, the first-principles band structure and density of states calculations indicate that the compound belongs to indirect semiconductor with the band gap of 2.1 eV, which is supported by the UV-Vis diffuse reflectance results.

Carbon Nitride Nanowire Bundle and Tubes:Solid-state Synthesis,Characterization and Photoluminescent Properties

Graphite-like carbon nitride nanowire bundles were synthesized from melamine via the solid state thermolysis at relatively low temperature（400℃）.Hexagonal carbon nitride tubes were prepared for the first time by heating the nanowire bundles at 550 ℃ in argon atmosphere.The forming process of tubes and transformation of the molecular structures from s-triazine rings to tri-s-triazine units were analyzed.The blue and yellow-green emission photoluminescent（PL） properties of the products were investigated in detail,and the reasons for the differences of PL properties between the bundles and tubes were discussed.

Solid-State Synthesis of Metastable Ytterbium (II) Oxide

Due to its electron configuration (Xe) 4 f14 6 s2, Ytterbium (Yb) could form divalent oxide, YbO. In this study, the solid-state synthesis of metastable YbO was investigated by the oxidation of Yb metal at normal pressure using two experimental conditions: 1) heat treatment of Yb metal under Ar gas atmosphere with metal carbonate as an oxygen source;and 2) heat treatment of Yb metal under the continuous gas flow condition using various gas atmospheres. Products were identified using the powder X-ray diffraction and scanning electron microscope. It was found that almost single phase YbO was obtained in the experimental condition 1) using the molar ratio of Ca-CO3/Yb = 0.4. Thermodynamic calculations suggested that the YbO formation be controlled not by thermodynamics but by kinetics, and further that the evaporation of Yb metal in the BN crucible played a key role for the formation of the meta-stable YbO.

Study on Component Synthesis Active Vibration Suppression Method Using Zero-placement Technique

The component synthesis active vibration suppression method （CSVS） can be applied to suppress the vibration of flexible systems. By this method, several same or similar time-varying components are arranged according to certain rules along the time axis. The synthesized command can suppress the arbitrary unwanted vibration harmonic while achieving the desired rigid body motion. The number of the components increases rapidly when the number of harmonic vibration is growing. In this article, the CSVS based on zero-placement technique is used to construct the synthesized command to suppress the multi-harmonics simultaneously in the discrete domain. The nature of zero-placement method is to put enough zeros to cancel system poles at necessary points. The designed synthesized command has equal time intervals between each component and which is much easier to be implemented. Using this method, the number of components increases linearly with the increasing of the number of being suppressed harmonics. For the spacecraft with flexible appendages, CSVS based on zero-placement is used to design the time optimal large angle maneuver control strategy. Simulations have verified the validity and superiority of the proposed approach.

Type Synthesis of 4-DOF Parallel Kinematic Mechanisms Based on Grassmann Line Geometry and Atlas Method

Many methods are proposed to deal with the type synthesis of parallel kinematic mechanisms（PKMs）, but most of them are less intuitive to some extent. Thus, to propose a concise and intuitive type synthesis method for engineering application is a very challenging issue, which should be further studied in the field. Grassmann line geometry, which can investigate the dimensions of spatial line-clusters in a concise way, is taken as the mathematic foundation. Atlas method is introduced to visually describe the degrees of freedom（DOFs） and constraints of a mechanism, and the dual rule is brought in to realize the mutual conversion of the freedom-space and constraint-space. Consequently, a systematic method based on Grassmann line geometry and Atlas method is generated and the entire type synthesis process is presented. Three type 4-DOF PKMs, i.e., 1T3R, 2T2R and 3T1R（T： translational DOF; R： rotational DOF）, are classified according to the different combinations of the translational DOFs and rotational DOFs. The type synthesis of 4-DOF PKMs is carried out and the possible configurations are thoroughly investigated. Some new PKMs with useful functions are generated during this procedure. The type synthesis method based on Grassmann line geometry and Atlas method is intuitive and concise, and can reduce the complexity of the PKMs＇ type synthesis. Moreover, this method can provide theoretical guidance for other PKMs＇ type synthesis and engineering application. A novel type synthesis method is proposed, which solves the existing methods＇ problems in terms of complicated, not intuitive and unsuitable for practical application.

Synthesis and Characterization of Y-Doped Mesoporous CeO_2 Using A Chemical Precipitation Method

Using cetyltrimethylammonium bromide （CTAB） as the template agent, cerium nitrate as the cerium resource, yttrium nitrate as the yttrium resource, and ammonium carbonate as the precipitating agent, mesoporous CeO2 powders doped with different yttrium contents were successfully synthesized using a chemical precipitation method, under an alkalescent condition. Properties of the obtained samples were characterized and analyzed with X-ray diffraction （XRD）, energy dispersive analysis of X-rays （EDAX）, transmission electron microscopy （TEM）, infrared （IR） absorbance, and the BET method. For the prepared samples with 20% （molar ratio） Y-doped content, a BET specific surface area of 106. 6 m^2 · g^- 1, with an average pore size of3~27 nm were obtained. XRD patterns showed that the doped samples were with a cubic fluorite structure. TEM micrographs revealed that the doped samples showed a spherical morphology with a diameter ranging from 20 to 30 nm and a round pore shape. IR results indicated that the Ce-O-Ce vibration intensity decreased as the Y-doped content increased. N2 adsorption-desorption isotherms showed that the samples possessed typical mesopore characteristics. The average pore size of the samples decreased alter mesoporous CeO2 was doped with yttrium, and the average pore size decreased largely as the Y-doped content increased.

Synthesis methods of functionalized nanoparticles:a review

With the recent advancement in nanotechnology,nanoparticles(NPs)offer an ample variety of smart functions than conventional materials in various aspects.As compared to larger particles,NPs possess unique characteristics and excellent abilities,such as low toxicity,chemical stability,surface functionality,and biocompatibility.These advantageous properties allow them to be widely utilized in many applications,including biomedical applications,energy applications,IT applications,and industrial applications.In order to fulfill the increasing demands of NP applications,existing NP synthesis methods need to be improved based on the requirements of different applications to further their usage.A comprehensive understanding of the relationships between synthesis parameters and properties of NPs can help us better fine-tune them with designed properties and minimal toxicity.This review paper will discuss the commonly used synthesis methods of functionalized NPs,as well as future directions and challenges to develop various synthesis methods further.

Synthesis of potassium hexatitanate whiskers using hydrothermal method

High quality potassium hexatitanate whiskers were hydrothermally synthesized in one step under moderate temperature and pressure conditions. Effects of the titanium source and reaction conditions on the hydrothermal reaction rate, product phase component, and morphology of whiskers were investigated. The results show that the reactivity of hydrated titania, anatase TiO2, and rutile TiO2 with KOH decreases in turn, and with hydrated titania as titanium source, it is difficult to obtain potassium hexatitanate whiskers with good morphology. In contrast, uniform potassium hexatitanate whiskers with a length of 10-20 μm and a diameter of 200-700 nm were obtained using anatase TiO2 as titanium source. The investigation demonstrates that the initial KOH concentration, annealing temperature and time, molar ratio of K2O/TiO2, etc. significantly affect the morphology of the as-synthesized whiskers. The optimized synthesis condition is as follows： anatase as a titanium source 10 wt.% KOH solution; annealing temperature and time of 300℃ and 5 h, respectively; K2O/TiO2 molar ratio of 5, etc. A rhombic potassium hexatitanate was prepared under the optimum condition and the whisker grew along the [110] direction. The reaction mechanism was discussed.

Fischer–Tropsch synthesis using Co and Co-Ru bifunctional nanocatalyst supported on carbon nanotube prepared via chemical reduction method

We used a chemical reduction method to synthesize the catalysts of cobalt(Co) and cobalt-ruthenium(Co-Ru) bifunctional supported on carbon nanotubes(CNTs) for Fischer–Tropsch synthesis(FTS) in a fixedbed reactor. These Co-Ru/CNTs catalysts were synthesized with various weight proportions of Ru/Co(0.1 to 0.4 wt%) with keeping a fixed amount of cobalt(10 wt%). Moreover, for comparison purpose, CNTs supported Co-and Co(Ru)-based catalysts at same loading as the above catalysts were prepared through impregnation method. We characterize the present catalysts through the various techniques such as Energy–dispersive X-ray(EDX), Transmission Electron Microscopy(TEM), Brunauer–Emmett–Teller(BET),Hydrogen-Temperature-Programmed Reduction(H_2-TPR), Hydrogen-Temperature-Programmed Desorption(H_2-TPD) and O_2 titration. Thus using the chemical reduction method, a narrow particle size distribution was obtained so that the small cobalt particles were confined inside the CNTs. The Co-based catalyst prepared by impregnation was compared with the Co-Ru catalysts at the same loading. The results demonstrated that the use of chemical reduction method led to decrease the average Co oxide cluster size to8.7 nm so that the reduction enhanced about 24% and stabilized an earlier time at the stream. Among the prepared catalysts, the results indicated that the Co-Ru/CNTs catalysts demonstrated high catalytic activity with the highest long-chain hydrocarbons(C_(5+)), selectivity up to 74.76%, which was higher than those we obtained by the Co-Ru/γ-Al_2O_3(61._20%), Co/CNTs(43.68%) and Co/γ-Al_2O_3(37.69%). At the same time, comparing with those catalyst synthesized by impregnation, the use of chemical reduction led to enhancement of the C_(5+) selectivity from 59.30% to 68.83% and increment in FTS rate about 11% for the Co-Ru/CNTs catalyst.

A New Method for Type Synthesis of 2R1T and 2T1R 3-DOF Redundant Actuated Parallel Mechanisms with Closed Loop Units

The current type synthesis of the redundant actuated parallel mechanisms is adding active-actuated kinematic branches on the basis of the traditional parallel mechanisms,or using screw theory to perform multiple getting intersection and union to complete type synthesis.The number of redundant parallel mechanisms obtained by these two methods is limited.In this paper,based on Grassmann line geometry and Atlas method,a novel and effective method for type synthesis of redundant actuated parallel mechanisms(PMs)with closed-loop units is proposed.Firstly,the degree of freedom(DOF)and constraint line graph of the moving platform are determined successively,and redundant lines are added in constraint line graph to obtain the redundant constraint line graph and their equivalent line graph,and a branch constraint allocation scheme is formulated based on the allocation criteria.Secondly,a scheme is selected and redundant lines are added in the branch chains DOF graph to construct the redundant actuated branch chains with closed-loop units.Finally,the branch chains that meet the requirements of branch chains configuration criteria and F&C(degree of freedom&constraint)line graph are assembled.In this paper,two types of 2 rotational and 1 translational(2R1T)redundant actuated parallel mechanisms and one type of 2 translational and 1 rotational(2T1R)redundant actuated parallel mechanisms with few branches and closed-loop units were taken as examples,and 238,92 and 15 new configurations were synthesized.All the mechanisms contain closed-loop units,and the mechanisms and the actuators both have good symmetry.Therefore,all the mechanisms have excellent comprehensive performance,in which the two rotational DOFs of the moving platform of 2R1T redundant actuated parallel mechanism can be independently controlled.The instantaneous analysis shows that all mechanisms are not instantaneous,which proves the feasibility and practicability of the method.

Strontium ferrite powders prepared from oily cold rolling mill sludge by solid-state reaction method

Oily cold rolling mill （CRM） sludge is one of the pollutants emitted by iron and steel plants. Recycling oily CRM sludge can not only reduce pollution but also bring social and environmental benefits. In this study, using oily CRM sludge as sources of iron oxide, the strontium ferrite powders were synthesized in multiple steps including vacuum distillation, magnetic separation, oxidizing roasting, and solidstate reaction. The optimal technological conditions of vacuum distillation and oxidizing roasting were studied carefully. To consider the effects of Fe203/ SrCO3 tool ratio, calcination temperature, milling time and calcination time on magnetic properties of prepared strontium ferrite powders, the orthogonal experimental method was adopted. The maximum saturation magneti- zation （62.6 mA-m2.g-1） of the synthesized strontium ferrite powders was achieved at the Fe203/SrCO3 mol ratio of 6, 5 h milling time, 1250 ~C calcination temperature, and 1 h calcination time. Strontium ferrite powders syn- thesis method not only provides a cheap, high quality raw material for the production of strontium ferrite powders, but also effectively prevents the environmental pollution.

Adding Sub-chain Method for Structural Synthesis of Planar Closed Kinematic Chains

For at least the past five decades,structural synthesis has been used as a main means of finding better mechanisms with some predefined function.In structural synthesis,isomorphism identification is still a problem unsolved well,and to solve this problem is very significant to the design of new mechanisms.According to the given degree of freedom（DOF） and link connection property of planar closed chain mechanisms,vertex assortment is obtained.For solving the isomorphism problem,a method of the adding sub-chains is proposed with the detailed steps and algorithms in the synthesizing process.Employing this method,the identification code and formation code of every topological structure are achieved,therefore many isomorphic structures could be eliminated in time during structural synthesis by comparing those codes among different topological graphs,resulting in the improvement of synthesizing efficiency and accuracy,and the approach for eliminating rigid sub-chains in and after the synthesizing process is also presented.Some examples are given,including how to add sub-chains,how to detect simple rigid sub-chains and how to obtain identification codes and formulation codes et al.Using the adding sub-chain method,the relative information of some common topological graphs is given in the form of table.The comparison result is coincident with many literatures,so the correctness of the adding sub-chain method is convinced.This method will greatly improve the synthesizing efficiency and accuracy,and has a good potential for application.

Synthesis of Codon-optimized Human Interleukin-18 Gene by Combination of Chemical and Enzymatic Method

According to the amino acid sequence and codon preference of E. coli, the human interleukin-18（IL-18） gene was optimized to avoid the rare codons. The total length of the synthesized gene is 571 bp; 18 oligonucleotides, DNA fragments were designed and synthesized by the phosphoramidite four-step chemical method. The whole DNA sequence was synthesized by a one-step total gene synthesis method, and then inserted in pUC18 vector. Five positive clones identified by blue-white colony screening were sent to Shanghai Sangon Biological Engineering Technology and Service Co., Ltd. for sequencing. The sequencing result shows that one clone contained the complete correct gene in all the five positive clones.

Synthesis of mesoporous carbon as electrode material for supercapacitor by modified template method

The pore structures and electrochemical performances of mesoporous carbons prepared by silica sol template method as electrode material for supercapacitor were investigated. The mean pore size and mass specific capacitance of the mesoporous carbons increase with the increase of mass ratio of silica sol to carbon source （glucose）. A modified template method, combining silica sol template method and ZnCl2 chemical activation method, was proposed to improve the mass specific capacitance of the mesoporous carbon with an improved BET surface area. The correlation of rate capability and pore structure was studied by constant current discharge and electrochemical impedance spectroscopy. A commercially available microporous carbon was used for comparison. The result shows that mesoporous carbon with a larger pore size displays a higher rate capability. Mesoporous carbon synthesized by modified template method has both high mass specific capacitance and good rate capability.