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.

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.

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.

Comparison of the interface reaction behaviors of CaO–V_(2)O_(5) and MnO_(2)–V_(2)O_(5) solid-state systems based on the diffusion couple method

The formation mechanism of calcium vanadate and manganese vanadate and the difference between calcium and manganese in the reaction with vanadium are basic issues in the calcification roasting and manganese roasting process with vanadium slag.In this work,CaO–V_(2)O_(5) and MnO_(2)–V_(2)O_(5) diffusion couples were prepared and roasted for different time periods to illustrate and compare the diffusion reaction mechanisms.Then,the changes in the diffusion product and diffusion coefficient were investigated and calculated based on scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS) analysis.Results show that with the extension of the roasting time,the diffusion reaction gradually proceeds among the CaO–V_(2)O_(5) and MnO_(2)–V_(2)O_(5) diffusion couples.The regional boundaries of calcium and vanadium are easily identifiable for the CaO–V_(2)O_(5) diffusion couple.Meanwhile,for the MnO_(2)–V_(2)O_(5) diffusion couple,MnO_(2) gradually decomposes to form Mn_(2)O_(3),and vanadium diffuses into the interior of Mn_(2)O_(3).Only a part of vanadium combines with manganese to form the diffusion production layer.CaV_(2)O_(6) and MnV_(2)O_(6) are the interfacial reaction products of the CaO–V_(2)O_(5) and MnO_(2)–V_(2)O_(5) diffusion couples,respectively,whose thicknesses are 39.85 and 32.13μm when roasted for 16 h.After 16 h,both diffusion couples reach the reaction equilibrium due to the limitation of diffusion.The diffusion coefficient of the CaO–V_(2)O_(5) diffusion couple is higher than that of the MnO_(2)–V_(2)O_(5) diffusion couple for the same roasting time,and the diffusion reaction between vanadium and calcium is easier than that between vanadium and manganese.

A review of ^(17)O isotopic labeling techniques for solid-state NMR structural studies of metal oxides in lithium-ion batteries

Recent advances in utilizing ^(17)O isotopic labeling methods for solid-state nuclear magnetic resonance(NMR)investigations of metal oxides for lithium-ion batteries have yielded extensive insights into their structural and dynamic details.Herein,we commence with a brief introduction to recent research on lithium-ion battery oxide materials studied using ^(17)O solid-state NMR spectroscopy.Then we delve into a review of ^(17)O isotopic labeling methods for tagging oxygen sites in both the bulk and surfaces of metal oxides.At last,the unresolved problems and the future research directions for advancing the ^(17)O labeling technique are discussed.

Synthesis, Characterization and Optical Morphology of ZnO Nanoparticles

The ZnO molecule plays an important role in the industry due to it special features, anti-corrosion anti-bacterial properties, as well as due to its low electrical conductivity and heat resistance. In these experimental researches, the sol-gel method was chosen, which enables control of nucleation, aging and growth of particles in the solution. ZnO synthesis was prepared utilizing chemical method with Zinc acetate dyhidrate and NaOH with the appropriate methanol solvent and heating (60˚C). The methods used in identification and characterization are FTIR, UV/VIS, OPTICAL MICROSCOPY, SEM and XRD. The FTIR spectra of synthesized ZnO with corresponding ones show characteristic bands at the corresponding wavelengths, which confirm the presence of ZnO nanoparticles. SEM characterization of ZnO shows the morphology of needle-shaped nanoparticles. XRD spectar in this research by chemical method indicates the particle size of 17.76 nm.

Solriamfetol impurities:Synthesis,characterization,and analytical method(UPLC-UV)validation

Given that impurities may affect the quality and safety of drug products,impurity identification and profiling is an integral part of drug quality control and is particularly important for newly developed medications such as solriamfetol,which is used to treat excessive daytime sleepiness.Although the highperformance liquid chromatography analysis of commercial solriamfetol has revealed the presence of several impurities,their synthesis,structure elucidation,and chromatographic determination have not been reported yet.To bridge this gap,we herein identified,synthesized,and isolated eight processrelated solriamfetol impurities,characterized them using spectroscopic and chromatographic techniques,and proposed plausible mechanisms of their formation.Moreover,we developed and validated a prompt impurity analysis method based on ultrahigh-performance liquid chromatography with UV detection,revealing that its selectivity,linearity,accuracy,precision,and quantitation limit meet the acceptance criteria of method validation stipulated by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use.Thus,the developed method was concluded to be suitable for the routine analysis of solriamfetol substances.

Synthesis strategies of covalent organic frameworks: An overview from nonconventional heating methods and reaction media

Covalent organic frameworks(COFs), as an emerging class of porous crystalline materials constructed by covalent links between the building monomers, have gained tremendous attention. Over the past 15 years, COFs have made rapid progress and substantial development in the chemistry and materials fields. However, the synthesis of COFs has been dominated by solvothermal methods for a long time and it usually involves high temperature, high pressure and toxic organic solvents, which created many challenges for environmental considerations. Recently,the exploration of new approaches for facile fabrication of COFs has aroused extensive interest. Hence, in this review, we comprehensively describe the synthetic strategies of COFs from the aspects of nonconventional heating methods and reaction media. In addition, the advantages,limitations and properties of the preparation methods are compared. Finally, we outline the main challenges and development prospects of the synthesis of COFs in the future and propose some possible solutions.

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.

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.

Mechanical densification synthesis of single-crystalline Ni-rich cathode for high-energy lithium-ion batteries

The intergranular microcracking in polycrystalline Ni-rich cathode particle is led by anisotropic volume change and stress corrosion along grain boundary,accelerating battery performance decay.Herein,we have suggested a simple but advanced solid-state method that ensures both uniform transition metal distribution and single-crystalline morphology for Ni-rich cathode synthesis without sophisticated coprecipitation.Pelletization-assisted mechanical densification(PAMD)process on solid-state precursor mixture enables the dynamic mass transfer through the increased solid-solid contact area which facilitates the grain growth during sintering process,readily forming micro-sized single-crystalline particle.Furthermore,the improved chemical reactivity by a combination of capillary effect and vacancyassisted diffusion provides homogeneous element distribution within each primary particle.As a result,single-crystalline Ni-rich cathode with PAMD process has eliminated a potential evolution of intergranular cracking,thus achieving superior energy retention capability of 85%over 150 cycles compared to polycrystalline Ni-rich particle even after high-pressure calendering process(corresponding to electrode density of~3.6 g cm^(-3))and high cut-off voltage cycling.This work provides a concrete perspective on developing facile synthetic route of micron-sized single-crystalline Ni-rich cathode materials for high energy density lithium-ion batteries(LIBs).

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.