Li-intercalation behaviour of vanadium oxide thin film prepared by thermal oxidation of vanadium metal

In order to produce thin films of crystalline V₂O₅, vanadium metal was thermally oxidised at 500 °C under oxygen pressures between 250 and 1000 mbar for 1-5 min. The oxide films were characterised by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), X-ray diffraction (XRD) and Rutherford backscattering spectrometry (RBS). The lithium intercalation performance of the oxide films was investigated by cyclic voltammetry (CV), chronopotentiometry and electrochemical impedance spectroscopy (EIS). It was shown that the composition, the crystallinity and the related lithium intercalation properties of the thin oxide films were critically dependent on the oxidation conditions. The formation of crystalline V₂O₅ films was stimulated by higher oxygen pressure and longer oxidation time. Exposure for 5 min at 750 mbar O₂ at 500 °C resulted in a surface oxide film composed of V₂O_5, and consisting of crystallites up to 200 nm in lateral size. The thickness of the layer was about 100 nm. This V₂O₅ oxide film was found to have good cycling performance in a potential window between 3.8 and 2.8 V, with a stable capacity of 117 ± 10 mAh/g at an applied current density of 3.4 μA/cm². The diffusion coefficients corresponding to the two plateaus at 3.4 and 3.2 V were determined from the impedance measurements to (5.2 and 3.0) × 10⁻¹³ cm² s⁻¹, respectively. Beneath the V₂O₅ layer, lower oxides (mainly VO₂) were found close to the metal. At lower oxygen pressure and shorter exposure times, the oxide films were less crystalline and the amount of V⁴⁺ increased in the surface oxide film, as revealed by XPS. At intermediate oxygen pressures and exposure times a mixture of crystalline V₂O₅ and V₆O₁₃ was found in the oxide film.     

双标记1-氨基乙内酰脲盐酸盐-(2-~(13)C,~(15)N_3)的合成

以氨基脲盐酸盐-(2-13C,15 N3)为原料,经与苯甲醛缩合,在乙醇钠催化作用下,与氯乙酸乙酯缩合环化制得1-苯亚甲基氨基乙内酰脲,最后盐酸水解,制得1-氨基乙内酰脲盐酸盐-(2-13 C,15 N3)。合成路线优势在于反应条件温和,产物总收率高于65%。产品经IR、HPLC、NMR和MS表征结果表明:化学纯度>98.4%,13C同位素丰度>98%,15 N同位素丰度>99%。     

玉米秸秆木质素降解过程的CP/MAS 13CNMR和SEM表征

利用黄孢原毛平革菌对玉米秸秆木质素进行降解处理,通过CP/MAS 13 CNMR和SEM研究降解过程中木质素的结构变化。CP/MAS 13 CNMR结果表明:玉米秸秆木质素降解过程中,作为木质素结构单元主要连接方式的β-O-4键基本上没有被降解;木质素单位苯环的甲氧基含量稍有增加;S/G值降低,推断反应过程中紫丁香基优先参与反应。SEM结果表明:降解后的木质素空穴增多且增大、颗粒物质减少,主要是由于酶解木质素中大量碳水化合物的降解所致;比木质素更容易降解的纤维素和半纤维素也存在于样品中。CP/MAS 13 CNMR为木质纤维原料结构的定性和初步定量提供了可能,是传统定量表征手段的有力补充,具有一定的研究意义。     

利用振动检测诊断双螺杆压缩机故障

定期对海上关键设备进行振动检测,发现双螺杆压缩机的振动烈度超标。利用频谱分析,诊断设备故障原因,并在检修中进行了修正。     

Fate of coagulant species and conformational effects during the aggregation of a model of a humic substance with Al13 polycations

A model of a humic substance (MHS) obtained from auto-oxidation of catechol and glycine, was aggregated at pH 6 and 8 with Al(13) polycations. The fate of Al(13) coagulant species upon association with MHS functional groups was studied using solid state (27)Al Magic-angle spinning (MAS) NMR and CP-MAS (13)C NMR. Electrophoretic measurements and steady-state fluorescence spectroscopy with pyrene as a fluoroprobe, were combined to investigate structural re-organization of humic material with aluminum concentration. MAS (27)Al NMR revealed that the coagulant species are Al(13) polycations or oligomers of Al(13) units at both pHs. CP MAS (13)C spectra indicated that, at low Al concentration, hydrolyzed aluminum species bind selectively to carboxylic groups at pH 6 and to phenolic moieties at pH 8. At higher coagulant concentrations, the remaining functional groups also interact with hydrolyzed Al to yield similar CP MAS (13)C spectra in the optimum concentration range. Negative values of electrophoretic mobility were obtained at optimum coagulant concentrations even though an overall charge balance was achieved between MHS anionic charge and Al(13) cationic charge at pH 6. The polarity-sensitive fluorescence of pyrene revealed that the interaction of Al(13) coagulant species with MHS functional groups induces the formation of intramolecular hydrophobic microenvironments. Such structural changes were reversed upon further addition of Al(13) polycations.     

Reply to the alternative optimal growth controls

Sasaki (2002) argues that: (1) “the agglomeration effect in the (Lai and Yang 2002, (L-Y)) paper is different from the introduction of urban production in Sasaki (1998)”; and (2) the “treatment of public good in the (L-Y) paper is strange,” because the public good provided by owner-residents is only consumed by renter-residents. This reply shows that (1) the agglomeration effect in the L-Y model catches the key results of urban production presented in Sasaki's model; and (2) both renter and owner-residents consuming the public good have been developed in this reply. However, the major conclusions of the L-Y model are still hold. Received: February 2001/Accepted: September 2001     

核电用1Cr13厚壁管材内表面裂纹产生原因分析

分析了热轧后空冷产生的淬火效应、退火缓冷引起的回火脆性和轧制对裂纹生长方向的影响.不合理的热处理制度使材料发生马氏体相变和回火脆性,在冲击性冷轧后产生开裂.而轧制压扁造成的内表面切向拉应力是产生纵向裂纹的原因.     

高温短时退火LaFe_(13-x)Si_x合金的组织结构

采用XRD、SEM及EDS等手段研究了LaFe13-xSix(x=1.43,1.56,2.4)合金铸态及高温短时退火后的结构与显微组织,并通过振动样品磁强计研究了退火态合金的磁性能.结果表明:铸态LaFe11.57Si1.43和LaFe11.44Si1.56含有大量的α-Fe和LaFeSi相,显微组织呈典型的树枝晶状,LaFe11.44Si1.56还含有较多具有NaZn13型结构的相.铸态LaFe10.6Si2.4可直接得到具有NaZn13型结构的主相,组织呈胞状.在1350 ℃退火0.5 h并随炉冷却后,除含有少量α-Fe及LaFeSi杂相外,LaFe11.57Si1.43和LaFe11.44Si1.56主要以具有NaZn13型结构的相为主,其组织呈等轴晶状.磁性测量结果表明:随Si含量的增加,合金居里温度逐渐升高.     

3Cr13不锈钢低温双辉等离子渗铬

对3Cr13不锈钢在700 ℃进行低温等离子渗铬处理,并观察处理后试样的组织,进行了截面成分检测、硬度检测、X射线衍射物相分析以及电化学腐蚀性能测试.结果表明,表面覆盖4～5 μm 的铬沉积层后在沉积层的下边形成了一定区域的脱碳层,表面硬度达728 HV0.05;表层物相主要为Fe、Cr、Cr_(1.36)Fe_(0.52)及Cr_(23)C_6;在2.5%HCl溶液中耐腐蚀性能提高约6倍,抗点蚀能力有一定的增强,提高了耐晶间腐蚀的能力.     

3Cr13钢高温抗氧化性能的研究

3Cr13钢分别在500、650、800及950℃高温下进行氧化试验,采用SEM、XRD分析氧化表面的形貌、成分和物相,探究3Cr13钢的高温抗氧化性能.结果表明:500℃时,试样表面氧化物膜不完整,氧化物量几乎为0;温度高于570℃时,氧化物在试样表面形成完整的覆盖膜,氧化速度仍很缓慢;而温度为950℃且氧化时间较长时,试样表面氧化物迅速增多,试样氧化反应剧烈.