A new method of characterizing equivalent strain for equal channel angular processing

In order to establish the quantitative relationship between equivalent strain and the performance index of the deformed material within the range of certain passes for equal channel angular processing （ECAP）, a new approach to characterize the equivalent strain was proposed. The results show that there exists better accordance between mechanical property （such as hardness or strength） and equivalent strain after rolling and ECAP in a certain range of deformation amount, and Gauss equation can be satisfied among the equivalent strain and the mechanical properties for ECAP. Through regression analysis on the data of hardness and strength after the deformation, a more generalized expression of equivalent strain for ECAP is proposed as：ε=k0exp[-（k1M-k2）^2], where M is the strength or hardness of the material, k1 is the modified coefficient （k1∈ （0, 1））, ko and k2 are two parameters dependent on the critical strain and mechanical property that reaches saturation state for the material, respectively. In this expression the equivalent strain for ECAP is characterized novelly through the mechanical parameter relating to material property rather than the classical geometry equation.

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 and characterization of layered Li(Ni_(1/3)Mn_(1/3)Co_(1/3))O_2 cathode materials by spray-drying method

Spherical Li(Ni_(1/3)Mn_(1/3)Co_(1/3))O_2 was prepared via the homogenous precursors produced by solution spray-drying method. The precursors were sintered at different temperatures between 600 and 1 000 ℃ for 10 h. The impacts of different sintering temperatures on the structure and electrochemical performances of Li(Ni_(1/3)Mn_(1/3)Co_(1/3))O_2 were compared by means of X-ray diffractometry(XRD), scanning electron microscopy(SEM), and charge/discharge test as cathode materials for lithium ion batteries. The experimental results show that the spherical morphology of the spray-dried powers maintains during the subsequent heat treatment and the specific capacity increases with rising sintering temperature. When the sintering temperature rises up to 900 ℃ , Li(Ni_(1/3)Mn_(1/3)Co_(1/3))O_2 attains a reversible capacity of 153 mA·h/g between 3.00 and 4.35 V at 0.2C rate with excellent cyclability.

A review of in-situ high-temperature characterizations for understanding the processes in metallurgical engineering

For the rational manipulation of the production quality of high-temperature metallurgical engineering,there are many challenges in understanding the processes involved because of the black box chemical/electrochemical reactors.To overcome this issue,various in-situ characterization methods have been recently developed to analyze the interactions between the composition,microstructure,and solid-liquid interface of high-temperature electrochemical electrodes and molten salts.In this review,recent progress of in-situ hightemperature characterization techniques is discussed to summarize the advances in understanding the processes in metallurgical engineering.In-situ high-temperature technologies and analytical methods mainly include synchrotron X-ray diffraction(s-XRD),laser scanning confocal microscopy,and X-ray computed microtomography(X-rayμ-CT),which are important platforms for analyzing the structure and morphology of the electrodes to reveal the complexity and variability of their interfaces.In addition,laser-induced breakdown spectroscopy,high-temperature Raman spectroscopy,and ultraviolet-visible absorption spectroscopy provide microscale characterizations of the composition and structure of molten salts.More importantly,the combination of X-rayμ-CT and s-XRD techniques enables the investigation of the chemical reaction mechanisms at the two-phase interface.Therefore,these in-situ methods are essential for analyzing the chemical/electrochemical kinetics of high-temperature reaction processes and establishing the theoretical principles for the efficient and stable operation of chemical/electrochemical metallurgical processes.

In-situ Characterization of Non-aqueous Nano-dispersion Systems by Freeze-etching TEM and Comparative Study with Laser Scattering Method

In-situ characterization of non-aqueous nano-dispersion systems（NANDS） by freeze-etching transmission electron microscope（FETEM） was reported.To improve just-for-once successive rate of specimen preparation and get good characterization results,an improving specimen preparation method of freezing etching was developed.Size,distribution and morphology of NANDS were directly visualized.Some information of particle dispersion feature and particle density can also be obtained.Reproductivity of the FETEM characterization is excellent.Comparing with laser scattering method,which is liable to give positive error especially for small size particle anchoring disperser,FETEM characterization can give more accurate measurement of particle size.Moreover,FETEM can give dispersion feature of nanoparticle in non-aqueous medium.

Charactering and optimizing cathode electrolytes interface for advanced rechargeable batteries:Promises and challenges

With the advancement of secondary batteries,interfacial properties of electrode materials have been recognized as essential factors to their electrochemical performance.However,the majority of investigations are devoted into advanced electrode materials synthesis,while there is insufficient attention paid to regulate their interfaces.In this regard,the solid electrolyte interphase(SEI)at anode part has been studied for 40 years,already achieving remarkable outcomes on improving the stability of anode candidates.Unfortunately,the study on the cathode electrolyte interfaces(CEI)remains in infancy,which constitutes a potential restriction to the capacity contribution,stability and safety of cathodes.In fact,the native CEI generally possesses unfavorable characteristics against structural and compositional stability that requires demanding optimization strategies.Meanwhile,an in-depth understanding of the CEI is of great significance to guide the optimization principles in terms of composition,structure,growth mechanism,and electrochemical properties.In this literature,recent progress and advances of the CEI characterization methods and optimization protocols are summarized,and meanwhile the mutually-reinforced mechanisms between detection and modification are explained.The criteria and the potential development of the CEI characterization are proposed with insights of novel optimization directions.

Screening,Preparation,Characterization and Solubility of Polymorphic Forms of Ethinyl Estradiol

Ethinyl estradiol（EE） as a contraceptive,（17α）-19-nopregna-1,3,5-（10）-trien-20-yne-3,17-diol（formula： C（20）H（24）O2, molecular weight： 296.4, CAS number： 57-63-6）, is known to have different pseudo-polymorphic forms. Some EE polymorphs have been synthesized by means of physical or chemical methods, characterized by X-ray powder diffraction（XRPD）, thermogravimetric（TG）, differential scanning calorimetry（DSC） and IR spectra. Dissolution profile was tested by high performance liquid chromatography（HPLC）. Meanwhile, the crystal structure of the new EE solvate（formamide） was characterized by single-crystal X-ray structure analysis（SXRD）. The results confirmed that EE existed polymorphism. Five crystal forms of EE were presented and two of them were reported firstly. Furthermore, five polymorphs＇ dissolution curves were drawn and they could be identified by several analysis methods. Our study on polymorphs of EE could provide a variety of crystal material composition, preparation methods and solubility.

Effect of Preparation Methods of Bi_(2)O_(3) Nanoparticles on their Photocatalytic Activity

Bi 2O 3 nanoparticles were prepared by means of ammonia precipitation, polyol mediated methods and microemulsion chemical method. The structure and properties of the as-prepared nanoparticles, having been submitted to a heat-treatment test at 750 ℃, were characterized by means of XRD, BET, XPS and UV-Vis absorption techniques. The photocatalytic oxidation reactions of benzene, toluene and xylene were used as the model reaction to measure the photocatalytic activity of Bi 2O 3 nanoparticles, respectively. The results show that the crystallite size of Bi 2O 3 prepared with different methods and calcined at 750 ℃ were 50.6, 38.5 and 31.5 nm, respectively. The photocatalytic activity of Bi 2O 3 nanoparticles prepared with the microemulsion chemical method was higher than that of the particles prepared with the polyol mediated method; and that of the particles prepared with the micromulsion chemical method was the highest among the three. The degradation rates of the three pollutants xylene, toluene and benzene decreased in sequence.

Preparation of calcium stannate by modified wet chemical method

A modified wet chemical route for low-temperature synthesis of the calcium stannate CaSnO3, a potentialmaterial for dielectric applications is reported. Firstly, a precursor CaSn(OH)6 was prepared using tin tetrachloride,calcium chloride and sodium hydroxide at room temperature. Then the precursor was annealed at relatively low tem-perature of 600 ℃ to obtain CaSnO3. The phase identification, thermal behavior and surface morphology of the sam-ples were characterized by element analysis, X-ray diffraction (XRD), thermo-gravimetric (TG) analysis and deriva-tive thermo-gravimetric (DTG) analysis, Fourier transform infrared spectroscopy (FTIR) and scanning electron mi-croscopy (SEM) in detail. The results show that CaSnO3 obtained by this method possesses a cubic perovskitestructure with average grain size of 5 μm.

Preparation and Characterization of CeO_2 Superfine Powder

The CeO_2 superfine powder was prepared by the co-precipitation method, using the industrial grade Ce_2(CO_3)_3 and NH_4HCO_3 as starting material and precipitating reagent, respectively. The precipitated precursons and the calcinated products were characterized by the thermogravimetric analysis/thermoanalysis (TGA/DTA), X-ray diffraction analysis (XRD) and transmission electron microscopy (TEM). The results show that using NH_4HCO_3 as a precipitating reagent, the precipitate decomposed full as it was heated to 360 ℃. The CeO_2 superfine powder formed by calcinating the precipitate belongs to a cubic CaF_2-type structure and has the first mean particle diameter 140 nm and second mean particle diameter 630 nm. The CeO_2 powder particles aggregate and grow with raising the calcination temperature.

Preparation and characterization of Pt-WO_3/C catalysts for direct ethanol fuel cells

Three co-impregnation/chemical reduction methods in acidic solutions of pH 〈 1,including ethylene glycol （EG）,NaBH4,and HCOOH,were compared for Pt-WO3/C catalysts.Pt-WO3/C catalysts containing 10 wt.% and 20 wt.% platinum per carbon were prepared by the three methods; their morphology and electrocatalytic activities were characterized.The 20 wt.% Pt-WO3/C catalyst prepared by the co-impregnation/EG method presented the optimal dispersion with an average particle size of 4.6 nm and subsequently the best electrocatalytic activity,and so,it was further characterized.Its anodic peak current density for ethanol oxidation from linear sweep voltammetry （LSV） is 7.9 mA·cm^-2,which is 1.4 and 5.2 times as high as those of the catalysts prepared by co-impregnation/NaBH4 and co-impregnation/ HCOOH reduction methods,2.1 times as high as that of the 10 wt.% Pt-WO3/C catalyst prepared by co-impregnation/EG method,respectively.

A Noveland Simple Creep Testing Method and Its Use in Measuring the Creep of Solder

A simple creep testing method is presented which involves using coiled specimens. With this method, a single experiment can give all the data required for a plot of strain rate versus stress. The value of the stress-expo-nent of room temperature steady-state creep a Pb-61. 5wt %Sn solder was measured in this way to be 1. 06,aselected from a diffusion creep mechanism.

Characterization of interfaces: Lessons from the past for the future of perovskite solar cells

A photovoltaic technology historically goes through two major steps to evolve into a mature technology. The first step involves advances in materials and is usually accompanied by the rapid improvement of power conversion efficiency. The second step focuses on interfaces and is usually accompanied by significant stability improvement. As an emerging generation of photovoltaic technology, perovskite solar cells are transitioning to the second step of their development when a significant focus shifts toward interface studies and engineering. While various interface engineering strategies have been developed, interfacial characterization is crucial to show the effectiveness of interfacial modification. Here, we review the characterization techniques that have been utilized in studying interface properties in perovskite solar cells. We first summarize the main roles of interfaces in perovskite solar cells, and then we discuss some typical characterization methodologies for morphological, optical,and electrical studies of interfaces. Successful experiences and existing problems are analyzed when discussing some commonly used methods. We then analyze the challenges and provide an outlook for further development of interfacial characterizations. This review aims to evoke strengthened research devotion on novel and persuasive interfacial engineering.

A Comparative Study of the Phase Distribution in Carbon-Silica Hybrid Fillers for Rubber Obtained by Different Methods

Different types of carbon-silica fillers were prepared via pyrolysis-cum-water vapor of waste green tires tread and impregnation method. Dual phase fillers have been characterized by energy dispersive X-ray (EDX) spectroscopy in a scanning transmission electron microscope (STEM) or STEM-EDX. Phase distribution in hybrid fillers for rubber was investigated. The results achieved show that the conditions of obtaining influence the distribution and the location of the phases in the carbon-silica hybrid fillers as well as their most essential characteristics including specific area, oil absorption number, iodine adsorption number, ash content and others.

New approaches to identification and characterization of tioconazole in raw material and in pharmaceutical dosage forms

Tioconazole(TCZ), a broad-spectrum antifungal agent, has significant activity against Candida albicans and other Candida species, and therefore, it is indicated for the topical treatment of superficial mycoses.The main goal of this work is to report an exhaustive identification and characterization procedure to improve and facilitate the online quality control and continuous process monitoring of TCZ in bulk material and loaded in two different dosage forms: ovules and nail lacquer. The methodologies were based on thermal(differential scanning calorimetry(DSC), melting point, and thermogravimetry(TG)),spectroscopic(ultraviolet(UV), Raman, near infrared(NIR), infrared spectroscopy coupled to attenuated total reflectance(FTIR-ATR), and nuclear magnetic resonance(NMR)), microscopic and X-ray diffraction(XRD). The TCZ bulk powder showed a high crystallinity, as observed by XRD, with a particles size distribution(3–95 mm) resolved by microscopic measurements. TCZ melting point(82.8 °C) and a degradation peak centered at 297.8 °C were obtained by DSC and DTG, respectively. An unambiguous structure elucidation of TCZ was obtained by mono-and two-dimensional1 H and13 C NMR spectral data analysis. The FTIR-ATR, Raman and NIR spectra of both the raw material and the commercial products were analyzed and their characteristic bands were tabulated. The best methods for TCZ identification in ovules were DSC, TG, XRD, NIR and Raman, while NIR and FTIR-ATR were the most appropriate techniques to analyze it in the nail lacquer. DSC, TG, DRX, Raman, FTIR-ATR and NIR spectroscopy are effective techniques to be used in online process analysis, because they do not require sample preparation, and they are considerably sensitive to analyze complex samples.

Titration Method Validation of Live Vaccines against Infectious Bursal Disease

Validating a method of analysis goes through different steps, which aims at testing the normality of measurements distribution, estimating the uncertainty of the components of a measurement （i.e., accuracy and correctness）, and finally, define the control tests of non degradation of the method performances. This paper outlines the steps for validating a biological method of analysis. It involves the construction of an experimental design, a statistical model, and the preparation of an interne laboratory reference material （pilot vaccine）. The latter is used to study the impact of deviation and variation factors, in order to, optimize the analytical method, to evaluate the bias （random error）, and to calculate the uncertainty of measurement, and make the control charts. This method is applied in the titration of live viral vaccines of Gumboro disease on chicken＇s embryos fibroblasts. The experimental results show that potential influence factors related to the titration method had no significant influence on the obtained results. Taking into account these results, an operating mode has been elaborated. The finalized method proved to be faithful to standard deviation of repeatability and reproducibility of 0.21 and 0.22, respectively, with a confidence level of 95%. The calculated uncertainty of measurement is equal to 0.2, which represents the average error level of a titer. A homogeneous stock of interne laboratory reference vaccine （MRIL）, with an average titer of 5.9 log DIT 50, was produced and the control chart set in away to provide the laboratory with an important tool of control and monitoring of the viral titers evolution in time, as well as, the mastery of the validated titration method performances.

Towards Reliability-Enhanced Mechanical Characterization of Non-Crimp Fabrics: How to Compare Two Force-Displacement Curves against a Null Material Hypothesis

Detailed characterization of fabric reinforcements is necessary to ensure the quality of manufactured composite parts, and subsequently to prevent structural failure during service. A lack of consensus and standardization exists in selecting test methods for the mechanical characterization of fabrics. Moreover, in reality, during any experimentation there are sources of uncertainties which may result in inconsistencies in the interpretation of data and the comparison of different testing methods. The aim of this article is to show how simple statistical data analysis methods may be used to enhance the characterization of composite fabrics under individual and combined loading modes while accounting for inherent material/test uncertainties. Results using a typical glass non-crimp fabric (NCF) show that, statistically, there are significant differences between the warp and weft direction responses of a presumably balanced NCF under all deformation modes, with weft yarns being generally stiffer. Moreover, the statistical significance of warp-weft couplings under both simultaneous and sequential biaxial-shear loading modes became statistically evident, when compared to a pure biaxial deformation.

风化煤腐植酸的提取应用研究进展

风化煤含氧量高、发热量低使其失去了作为燃料的价值,作为煤炭资源衍生而来的矿产资源,没有发挥出最大经济价值。但是,风化煤富含腐植酸,可以制备高附加值腐植酸,进而应用于工业、农业等领域。基于风化煤的化学性质和特点,简单介绍了风化煤腐植酸的结构表征方法,对风化煤的预处理方法及碱溶酸析法、催化法、微生物溶解法、絮凝法、序贯溶解法等腐植酸提取方法进行了综述,介绍了风化煤腐植酸的应用研究进展,并提出了风化煤腐植酸提取新工艺的研究方向,为推动风化煤资源的高附加值利用奠定了基础。

Selective separation, detection of zotepine and mass spectral characterization of degradants by LC–MS/MS/QTOF

A simple, precise, accurate stability-indicating gradient reversed-phase high-performance liquid chromatographic （RP-HPLC） method was developed for the quantitative determination of zotepine （ZTP） in bulk and pharmaceutical dosage forms in the presence of its degradation products （DPs）. The method was developed using Phenomenex C18 column （250 mm ~ 4.6 mm i.d., 5 mm） with a mobile phase containing a gradient mixture of solvents, A （0.05%trifluoroacetic acid （TFA）, pH ？ 3.0） and B （acetonitrile）. The eluted compounds were monitored at 254 nm;the run time was within 20.0 min, in which ZTP and its DPs were well separated, with a resolution of 41.5. The stress testing of ZTP was carried out under acidic, alkaline, neutral hydrolysis, oxidative, photolytic and thermal stress conditions. ZTP was found to degrade significantly in acidic, photolytic, thermal and oxidative stress conditions and remain stable in basic and neutral conditions. The developed method was validated with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness as per ICH guidelines. This method was also suitable for the assay determination of ZTP in pharmaceutical dosage forms. The DPs were characterized by LC-MS/MS and their fragmentation pathways were proposed.

An Effective Method of Synthesis and Purification of Organic Nonlinear Salt

A novel organic nonlinear material 4-dimethylamino-N-methyl-4-stilbazolium tosylate which was designed to have a donor/π-conjugated/acceptor structure was synthesized via an effective method.By this method,we have raised yields of every step.Red product with metal luster surface is obtained after repeated purification.The purification process was effective and less-product-lost.Nuclear magnetic resonance study and FTIR were performed to identify the molecular.