芒果玻璃化转变与状态图研究

研究了25℃下芒果的吸附等温线,实验数据采用GAB模型进行非线性拟合,结果表明芒果的吸附等温线呈'J'型,其单分子层干基含水率为0.107 g/g。芒果的状态图由冻结曲线、玻璃化转变温度曲线和最大冻结浓缩状态组成,其中冻结温度和玻璃化转变温度由差示扫描量热仪(DSC)测量得到。冻结温度和玻璃化转变温度的实验数据,分别采用Clausius-Clapeyron方程和Gordon-Taylor方程进行非线性拟合。实验结果显示,最大冻结浓缩状态时的固形物湿基质量分数为84%,在此状态下的玻璃化转变温度为-52.9℃。状态图的建立能够预测芒果贮藏过程的稳定性,并且能够提供最适干燥或冷冻加工条件。

Experimental investigation of crystallization process of nanofluid by DSC

A water-TiO2nanofluid with a weight fraction of 5% and an average particle size of 75 nm is used to investigate the effect of TiO2 nanoparticles on the crystallization and melting behaviors of deionized water by using differential scanning calorimetry（DSC）at four different cooling rates,3,5,7,9 ℃/min.The DSC experimental results show that the water-TiO2 nanofluid has a lower supercooling degree and a faster crystallization rate than the deionized water.With the increase in the cooling rate,the influence of the TiO2 nanoparticles on the supercooling degree of the deionized water becomes greater,but on the crystallization rate it turns lower.During the melting process,compared with the deionized water,the water-TiO2 nanofluid has a lower melting temperature,a less latent heat and a higher melting rate.

A Facile Route for Synthesis of LiFePO_4/C Cathode Material with Nano-sized Primary Particles

A facile and practical route was introduced to prepare LiFePO4/C cathode material with nano-sized primary particles and excellent electrochemical performance. LiH2PO4 was synthesized by using H3PO4 and LiOH as raw materials. Then, as-prepared LiH2PO4, reduced iron powder andα-D-glucose were ball-milled, dried and sin-tered to prepare LiFePO4/C. X-ray diffractometry was used to characterize LiH2PO4, ball-milled product and LiFePO4/C. Differential scanning calorimeter-thermo gravimetric analysis was applied to investigate possible reac-tions in sintering and find suitable temperature for LiFePO4 formation. Scanning electron microscopy was em-ployed for the morphology of LiFePO4/C. As-prepared LiH2PO4 is characterized to be in P21cn（33） space group, which reacts with reduced iron powder to form Li3PO4, Fe3（PO4）2 and H2 in ball-milling and sintering. The appro-priate temperature for LiFePO4/C synthesis is 541.3-976.7 ℃. LiFePO4/C prepared at 700 ℃ presents nano-sized primary particles forming aggregates. Charge-discharge examination indicates that as-prepared LiFePO4/C displays appreciable discharge capacities of 145 and 131 mA·h·g^-1 at 0.1 and 1 C respectively and excellent discharge ca-pacity retention.

Microstructure and dielectric properties of Ca-Al-B-Si-O glass/Al_2O_3 composites with various alkali oxides contents

The effects of alkali oxides （Na2O and K2O addition on both the sintering behavior and dielectric properties of Ca-AI-B-Si-O glass/Al2O3 composites were investigated by Fourier transform infrared spectroscopy （FTIR）, differential scanning calorimeter （DSC）, X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. The results show that the increasing amount of alkali oxides in the glass causes the decrease of [SiO4], which results in the decrease of the continuity of glass network, and leads to the decrease of the softening temperature Tf of the samples and the increasing trend of crystallization. And that deduces corresponding rise of densification, dielectric constant, dielectric loss of the low temperature co-fired ceramic （LTCC） materials and the decrease of its thermal conductivity. By contrast, the borosilicate glass/A1203 composites with 1.5% （mass fraction） alkali oxides sintered at 875 ℃ for 30 rain exhibit better properties of a bulk density of 2.79 g/cm3, a porosity of 0.48%, a 2 value of 2.28 W/（m.K）, a er value of 7.82 and a tand value of 9.1 × 10-4 （measured at 10 MHz）.

Effect of ZrO_2 Crystalline Phase on the Performance of Ni-B/ZrO_2 Catalyst for the CO Selective Methanation

Amorphous Ni-B/ZrO2 catalysts were prepared by coprecipitation-chemical reduction with KBH4 aqueous solution,and various crystalline phase ZrO2(amorphous-ZrO2,tetragonal-ZrO2 and monoclinic-ZrO2) supported Ni-B catalysts were obtained by thermal treatment in 5%H2-N2 stream at different temperature.The effect of ZrO2 polymorphs and the treatment temperature on the catalytic performance for the CO selective methanation were investigated,and the catalysts were characterized by N2 physisorption,Powder X-ray diffraction(XRD), Temperature-Programmed Desorption(CO-TPD and H2-TPD),and Differential Scanning Calorimeter(DSC).The treatment temperature affected strongly the crystalline structure of ZrO2,and the CO methanation activity and selectivity of the Ni-B/ZrO2 catalysts were significantly influenced by the crystalline phase of ZrO2.Of the three forms of ZrO2 polymorphs(amorphou-ZrO2,tetragonal-ZrO2 and monoclinic-ZrO2),the amorphous-ZrO2 supported nickle catalyst showed highest CO methanation activity,attributing in large part to the largest specific surface area and the optimum CO/H2 absorption intensity of the Ni-B/amorphous-ZrO2 catalyst.

Research on thermal decomposition of 1,3,5-trinitro-1,3,5-triazinane based on differential scanning calorimetry

In order to test the thermal decomposition of 1,3,5-trinitro-1,3,5-triazinane(RDX),the linear temperature rise experiment of RDX was carried out by differential scanning calorimeter under different heating rate conditions.The kinetic calculation of RDX thermal decomposition curve was carried out by Kissinger and Ozawa methods,respectively,and the thermal analysis software was used to calculate the parameters such as self-accelerating decomposition temperature.The results show that the initial decomposition temperature range,decomposition peak temperature range,and decomposition completion temperature range of RDX are 208.4-214.2,225.7-239.3 and 234.0-252.4℃,respectively,and the average decomposition enthalpy is 362.9 J·g^-1.Kissinger method was used to calculate the DSC experimental data of RDX,the apparent activation energy obtained is 190.8 kJ·mol^-1,which is coincident with the results calculated by Ozawa method at the end of the reaction,indicating that the apparent activation energy calculated by the two methods is relatively accurate.When the packaging mass values are 1.0,2.0 and 5.0 kg,respectively,the self-accelerating decomposition temperatures are 97.0,93.0 and 87.0℃,respectively,indicating that with the increase of packaging mass,the self-accelerating decomposition temperature gradually decreases,and the risk increases accordingly.

Thermal behavior and mass spectrometry analysis of N-methyl-N-nitroso-p-toluenesulfonamide

The effect of temperature on the functional groups transition of N-methyl-N-nitroso-p-toluenesulfonamide （Diazald） and thermal decomposition were investigated by Fourier Transform Infrared Spectroscopy （FT-IR） and Differential Scanning Calorimeter （DSC）. The results showed that the functional groups transition of Diazald was temperature dependent, and thermal decomposition of Diazald was accelerated above 47.7℃. The HPLC-ESI-MS method was used for Diazald analysis, which indicated the strong hydrogen bonding between Diazald and water and instability of the NO group.

Physicochemical Characterization and Solubility Enhancement Studies of Mebendazole Solid Dispersions in Solvent Mixtures

Abstract： The objective was to obtain solid dispersion to improve the dissolution rate, solubility and oral absorption of MB （mebendazole）, poor water-soluble drugs. The new formulation was characterized by DSC （differential scanning calorimetry）, PXRD （powder X-ray diffraction）, FT-1R （fourier transform infrared spectroscopy） and STEM （scanning transmission electron microscopy） methods. Solid dispersions of MB with polyvinylpyrrolidone K-30 （PVP K30） were prepared by solvent evaporation method. The solubility of MB （original powder） and that of the solid dispersions was measured at 25℃ in ethanol-water. The aqueous solubility of MB was favoured by the presence of the polymer in solvent mixtures. Combination of solid dispersions with co-solvents increased the water solubility of MB in a larger extent that each method separately. Solubility parameter （o） was used to relate to solubility profiles. MB and the solid dispersions show a solubility curve with a single peak at 51 = 30.78 MPav2. Solid state characterizations indicated that the solid dispersion exist an amorphous material entrapped in polymer matrix getting highest improvement in wettability and solubility.

Estimation of the desorption energy of dichloromethane and water in MIL-53 by DSC and ab-initio calculations

Desorption energies of dichloromethane （CH2C12） and water （H20） in a metal-organic framework, MIL-53（A1）, were investi- gated by the combination of experimental （differential scanning calorimeter, DSC） and computational （ab-initio calculations） methods. The differences of desorption energy and natural log of the frequency factor of CH2C12 and H20 in MIL-53（A1） were analyzed by a thermo active process using DSC measurements. The interaction energy of guest molecules with MIL-53（A1）, which corresponds to the desorption in the thermal active process, was explored using ab-initio calculation. As a result of the difference in the interaction energies of H20 and CH2C12 in MIL-53（A1）, the site near the p2-OH groups has two potential wells Both experimentally and computationally, MIL-53 presents the preferential adsorption of CH2C12 than H20.

Intermetallic phase formation and evolution during homogenization and solution in Al-Zn-Mg-Cu alloys

The effects of major alloy element contents of Zn, Mg, Cu in Al-Zn-Mg-Cu alloys on the formation and evolution of intermetallic phases during casting, homogenization and solution treatment have been investigated through using X-ray diffraction, scanning electron microscopy and differential scanning calorimetry. Experimental results showed that a relatively higher Zn content with lower Mg and Cu contents was beneficial to the formation of MgZn2 phase instead of the A12CuMg phase, which resulted in the unicity of the intermetallics in the A1 matrix, and that the MgZn2 phase was easier for diffusion and dissolution during homogenization and solution than the Al2CuMg phase. Additionally, the results of the first-principles calculations gave support for explaining the experimental phenomena. A larger absolute value of formation enthalpy and a smaller value of binding energy of the MgZn2 phase, as compared with the Al2CuMg phase, give it priority to precipitate during casting and make it easier to re-dissolve during homogenization and solution treatment. What＇s more, higher elastic constants with severe anisotropy of Young＇s modulus make undissolved blocks of AI^CuMg phase act as crack initiation, which degrade the perfor- mance of the materials.

High-zirconium bulk metallic glasses with high strength and large ductility

In this paper, high-zirconium Zr66＋2xAl9-x（Ni1/3Cu2/3）25-x （x=0,1,2 at.%） bulk metallic glasses with high strength and large duc- tility were fabricated by copper mould casting. The effects of zirconium content on the glass-forming ability （GFA）, thermal properties and mechanical properties were investigated using X-ray diffractometer （XRD）, differential scanning calorimeter （DSC）, and mechanical testing system in compressive and three-point bending modes, respectively. The high-zirconium BMGs show the critical diameters of 3-5 ram, the supercooled liquid region ranging from 70 K to 99 K, and the yield strength of over 1700 MPa. The Zr70Al7（Ni1/3Cu2/3）23 BMG exhibits a large compressive plastic strain up to 21% and a high notch toughness value of 60.6 MPa m1/2. The increase in Zr content results in the decrease in GFA and thermostability, and in the improvement of plasticity under compressive and three-point bending conditions. The superior plasticity of high-zirconium BMGs is at- tributed to their high Poisson＇s ratio and small elastic modulus ratioμl/B.

Hierarchical aging pathways and signatures of thermodynamic transition in molecular glasses

When a liquid is supercooled,its structural equilibration timeτeqincreases sharply approaching the glass transition temperature Tg,below which it is kinetically arrested in the out of equilibrium glassy state.Upon annealing below Tg,such glassy state relaxes toward the equilibrium state.There is growing evidence that such relaxation process is quite complex,influenced by the complexity of the potential energy landscape.Here we report the observation of a hierarchical aging pathway in the process of the glass-to-supercooled liquid transition in various molecular glass forming systems.Differential scanning calorimetry reveals that the glassy state upon annealing below Tgfirstly enters a transient metastable supercooled liquid state with slightly higher enthalpies than that of the equilibrium supercooled liquid state when extrapolated to below Tg.This observation is also confirmed by structural measurements via Raman scattering.The dynamics of the transient metastable-to-stable supercooled liquid transition exhibits characteristics of thermodynamic transition at spinodal temperature Tspslightly above Tg,leading to anomalous behaviors such as the appearance of a transition-like behavior in the plot of fragility measurements.These observations imply that the free energy landscape of the supercooled liquid develops complexity with qualitative changes approaching Tgand could have strong influence on the process of the glass transition.