膜流动电位测试中Ag-AgCl电极的制备及稳定性研究

膜的动电特性研究中,往往采用流动电位方法。该方法中,Ag-Ag Cl测试电极的质量是影响测试准确性的关键要素。本文采用正交试验设计和方差分析,着重考察电解法制备Ag-Ag Cl电极过程中,电流强度(I)、氯化时间(t)、电解质溶液浓度(CHCl)、电极来源(n)、烘烤温度(T)、活化电极溶液浓度(CKCl)等因素对Ag-Ag Cl电极稳定性的影响。得到Ag-Ag Cl电极的最优制备参数为:电流密度3.0m A/cm2,氯化时间50min,盐酸浓度0.1mol·L-1,烘烤温度120℃,活化电极溶液(KCl)浓度0.001mol·L-1;最显著影响因素为电极来源,显著影响因素为氯化时间和烘烤温度。对最优条件组合下制备的AgAg Cl电极,进行了稳定性实验,结果表明:制备的电极具有较好的稳定性,24h内电极电位漂移量小于0.10mv,7天内电极电位漂移量小于0.2mv;在聚偏氟乙烯中空纤维超滤膜流动电位测试中,流动电位与流动压差具有良好的线性和可重复性,回归曲线R20.99,变化规律符合Helmholtz-Smoluehowski公式,可以较好满足膜的流动电位测试要求。     

镁掺杂氧化铈整体式催化剂催化CO2和CH3OH直接合成碳酸二甲酯

采用共沉淀法成功地合成了不同Mg掺杂量的Ce_1-xMg_xO₂(x=0.05、0.10、0.15、0.20)固溶体催化材料,并运用透射电子显微镜(TEM)、X射线衍射(XRD)、氮气吸附-脱附测试、拉曼光谱、X射线光电子能谱(XPS)、CO₂程序升温脱附(CO₂-TPD)等技术对这些材料进行了表征。结果发现,通过调控CeO₂晶格中Mg的含量,可以调控所制备的Ce_1-xMg_xO₂催化材料的粒径、比表面积、表面缺陷等。其中Ce_0.90Mg_0.10O₂展现了最佳的表面性质,具有最小的平均粒径(约5.8 nm),最大的比表面积(约136 m2·g^-1)以及最高的表面氧含量(31.98%)。将Ce_1-xMg_xO₂催化材料涂覆在堇青石蜂窝陶瓷上制成整体催化剂,考察其对CO₂和CH₃OH直接合成碳酸二甲酯的催化性能。在140℃、2.4 MPa、反应2 h的条件下,Ce_0.90Mg_0.10O₂整体催化剂上碳酸二甲酯的收率高达20.21%,催化效果明显优于CeO₂和其余的Ce_1-xMg_xO₂(x=0.05、0.15、0.20)催化材料。     

Pseudomorphic growth of a single element quasiperiodic ultrathin film on a quasicrystal substrate

An ultrathin film with a periodic interlayer spacing was grown by the deposition of Cu atoms on the fivefold surface of the icosahedral Al70Pd21Mn9 quasicrystal. For coverages from 5 to 25 monolayers, a distinctive quasiperiodic low-energy electron diffraction pattern is observed. Scanning tunneling microscopy images show that the in-plane structure comprises rows having separations of S=4.5+/-0.2 A and L=7.3+/-0.3 A, whose ratio equals tau=1.618... within experimental error. The sequences of such row separations form segments of terms of the Fibonacci sequence, indicative of the formation of a pseudomorphic Cu film.     

Surface layer self diffusion in icosahedral Al-Pd-Mn quasicrystals

The self diffusion of Mn and Pd in a single grain icosahedral Al_69.9Pd_20.5Mn_9.6 quasicrystal has been determined by low energy ion scattering (LEIS). The diffusion was determined by depositing different elements (Pd, Mn) on the surface and measuring the rate of change in surface composition as a function of temperature by LEIS. The surface composition was monitored over the temperature range of 355-575 K for Mn and 440-745 K for Pd and compared to model calculations to allow the activation energy for diffusion to be determined. Activation energies of 0.20 ± 0.01 eV for Mn and 0.64 ± 0.03 eV for Pd have then been measured for self diffusion in i-Al-Pd-Mn, respectively. No deviation from Arrhenius behavior was detected in the temperature range covered by the present experiments. From the low values of activation energy we propose that this range of diffusion is phason related, reflecting the specific nature of the icosahedral structure.     

Step structure on the fivefold Al-Pd-Mn quasicrystal surface, and on related surfaces

We compare step morphologies on surfaces of Al-rich metallic alloys, both quasicrystalline and crystalline. We present evidence that the large-scale step structure observed on Al-rich quasicrystals after quenching to room temperature reflects equilibrium structure at an elevated temperature. These steps are relatively rough, i.e., have high diffusivity, compared to those on crystalline surfaces. For the fivefold quasicrystal surface, step diffusivity increases as step height decreases, but this trend is not obeyed in a broader comparison between quasicrystals and crystals. On a shorter scale, the steps on Al-rich alloys tend to exhibit local facets (short linear segments), with different facet lengths, a feature which could develop during quenching to room temperature. Facets are shortest and most difficult to identify for the fivefold quasicrystal surface.     

4-氨基-7-硝基苯并-2-氧杂-1,3-二唑类衍生物的合成及其对汞离子的识别研究

以4-氯-7-硝基苯并-2-氧杂-1,3-二唑、乙二胺和溴乙酸乙酯等为原料,合成4-氨基-7-硝基苯并-2-氧杂-1,3-二唑类衍生物(NBD-OEt),通过IR、NMR和MS对其进行结构表征。研究NBD-OEt的吸收光谱和荧光光谱性质,探讨其在H2O/EtOH(60/40, V/V) pH 7.40的HEPES缓冲体系中对Hg₂ 的响应,以及NBD-OEt与Hg₂ 的结合模式。结果表明, 随Hg₂ 的不断加入可诱使NBD-OEt在476nm的吸收峰红移至514nm,并有两个等吸收点(347nm、482nm);其荧光发射峰由536nm红移至559nm,且在525nm出现等发射点;通过Job plot法测定NBD-OEt与Hg₂ 以1:1的计量比结合。     

Analysis of ultrasonic guided waves propagating in long bones and cortical thickness based on time-frequency methods

The ultrasonic signals in long bones contain multiple guided modes which are mutual superposed.The velocities of guided waves in long bones are very sensitive to cortical thickness (CTh).In this paper,Hilbert-Huang transform(HHT) was proposed to analyze multi-mode guided waves,which can decompose superposed waves into many independent modes.Then the group velocity of each mode was obtained at corresponding frequency,which was compared with the results of short time Fourier transform(STFT).The CTh was also obtained by comparing with the theoretical calculation.The results showed that the experimental determined thickness was in agreement with the actual CTh,indicating that measuring the velocity of the guided mode can be used to estimate the CTh.The HHT is an effective method to identify multimode guided waves.     

Lost heat capacity and entropy in the helical magnet MnSi

The heat capacity of MnSi at B = 0 and B = 4 T was measured in the temperature range 2.5-100 K. To analyze the data, calculations of the phonon spectrum and phonon density of states in MnSi were performed. The calculated phonon frequencies were confirmed by means of inelastic neutron scattering. The analysis of the data suggests the existence of negative contributions to the heat capacity and entropy of MnSi at T > T(c) that may imply a specific ordering in the spin subsystem in the paramagnetic phase of MnSi.