火花放电原子发射光谱类型标准化校正方式的探讨

在国内,火花放电原子发射光谱分析广泛使用类型标准化进行方法校正。在国外,标准和文献中鲜见使用此方法的相关论述。类型标准化主要采用平移校正和转动校正两种方式,哪种方式更加合理也鲜见报道。国外设备类型标准化的默认设置优先采用转动校正方式,相关国内标准对最优校正方式的规定尚不明确,此默认设置的合理性有待探讨。实验选用低合金钢20CrNi2Mo、R407标准样品和不锈钢317L、0Cr18Ni9标准样品,引用国内相关标准,以正确度临界差为评判依据,模拟类型标准化样品和待测样品“十分接近”和“接近”两种情况下平移校正和转动校正的数据正确度。经数据统计分析,平移校正分析结果均满足要求,转动校正结果在“接近”情况下部分元素不满足要求。结合相关国家标准中元素含量范围和精密度数据进行分析,通过计算允许最大偏倚量并制作曲线图方式展开分析,得出如下结论:在满足文中类型标准化控制要点前提下,分析设置更适合于采用平移校正方式。     

Formation of single-crystalline BaTiO3 nanorods from glycolate by tuning the supersaturation conditions

We have studied peculiarities in the formation of single-crystalline barium titanate (BaTiO₃) nanorods from a glycolate-mediated complex via a single-step hydrothermal process under different supersaturation (S_R) conditions. X-ray diffraction (XRD) showed the formation of pure BaTiO₃ with an S_R of above 19. The tetragonality for the BaTiO₃ (c/a) reached 1.013 at S_R = 19–29 and dropped to 1.010 for S_R = 39. According to the transmission electron microscopy (TEM) and XRD analyses, the rod-shaped particles exhibited single crystallinity and crystal growth along the [001] plane. With scanning electron microscopy (SEM), the morphological evolution from a plate-shaped intermediate precursor (S_R = 6–9) to a rod-shaped product with an aspect ratio of 6–9 (S_R = 19–29), and to non-polar material with an irregular structure (S_R = 39), was observed. The negative slope, linear dependence of the particles’ width and length on the supersaturation level in the range S_R = 19–39 was established for the first time. The replacement of the prevailing crystallization mechanism from in-situ topotactic transformation into dissolution-precipitation above S_R = 19 was observed. It was shown that with a simple regulation of the S_R, the structural and morphological characteristics of the obtained BaTiO₃ nanoparticle can be effectively tuned.     

In Vivo Albumin-Binding of a C-Functionalized Cyclam Platform for 64Cu-PET/CT Imaging in Breast Cancer Model

An improved glucose-chelator-albumin bioconjugate (GluCAB) derivative, GluCAB-2^Mal, has been synthesized and studied for in vivo ⁶⁴Cu-PET/CT imaging in breast cancer mice models together with its first-generation analogue GluCAB-1^Mal. The radioligand works on the principle of tumor targeting through the enhanced permeability and retention (EPR) effect with a supportive role played by glucose metabolism. [⁶⁴Cu]Cu-GluCAB-2^Mal (99 % RCP) exhibited high serum stability with immediate binding to serum proteins. In vivo experiments for comparison between tumor targeting of [⁶⁴Cu]Cu-GluCAB-2^Mal and previous-generation [⁶⁴Cu]Cu-GluCAB-1^Mal encompassed microPET/CT imaging and biodistribution analysis in an allograft E0771 breast cancer mouse model. Tumor uptake of [⁶⁴Cu]Cu-GluCAB-2^Mal was clearly evident with twice as much accumulation as compared to its predecessor and a tumor/muscle ratio of up to 5 after 24 h. Further comparison indicated a decrease in liver accumulation for [⁶⁴Cu]Cu-Glu-CAB-2^Mal.     

[2.2]Paracyclophane-Based TCN-201 Analogs as GluN2A-Selective NMDA Receptor Antagonists

Recent studies have shown the involvement of GluN2A subunit-containing NMDA receptors in various neurological and pathological disorders. In the X-ray crystal structure, TCN-201 ( 1 ) and analogous pyrazine derivatives 2 and 3 adopt a U-shape (hairpin) conformation within the binding site formed by the ligand binding domains of the GluN1 and GluN2A subunits. In order to mimic the resulting π/π-interactions of two aromatic rings in the binding site, a [2.2]paracyclophane system was designed to lock these aromatic rings in a parallel orientation. Acylation of [2.2]paracyclophane ( 5 ) with oxalyl chloride and chloroacetyl chloride and subsequent transformations led to the oxalamide 7 , triazole 10 and benzamides 12 . The GluN2A inhibitory activities of the paracyclophane derivatives were tested with two-electrode voltage clamp electrophysiology using Xenopus laevis oocytes expressing selectively functional NMDA receptors with GluN2A subunit. The o-iodobenzamide 12 b with the highest similarity to TCN-201 showed the highest GuN2A inhibitory activity of this series of compounds. At a concentration of 10 μM, 12 b reached 36 % of the inhibitory activity of TCN-201 ( 1 ). This result indicates that the [2.2]paracyclophane system is well accepted by the TCN-201 binding site.     

Silver-substituted (Ag1-xCux)2ZnSnS4 solar cells from aprotic molecular inks

To battle the high open-circuit voltage deficit (V_OC,def) in kesterite (Cu₂ZnSnS₄ or CZTS) solar cells, a current field of research relates to point defect engineering by cation substitution. For example, by partly replacing Cu with an element of a larger ionic radius, such as Ag, the degree of Cu/Zn disorder decreases, and likewise does the associated band tailing. In this paper, solution-processed (Ag_1-xCu_x)₂ZnSnS₄ (ACZTS) samples are prepared through the aprotic molecular ink approach using DMSO as the solvent. The successful incorporation of silver into the CZTS lattice is demonstrated with relatively high silver concentrations, namely Ag/(Ag+Cu) ratios of 13% and 26%. The best device was made with 13% Ag/(Ag+Cu) and had an efficiency of 4.9%. The samples are compared to the pure CZTS sample in terms of microstructure, phase distribution, photoluminescence, and device performance. In the XRD patterns, a decrease in the lattice parameter c/a ratio is observed for ACZTS, as well as significant peak splitting with Ag addition for several of the characteristic kesterite XRD reflections. In addition to the improvement in efficiency, other advantageous effects of Ag-incorporation include enhanced grain growth and an increased band gap. A too high concentration of Ag leads to the formation of secondary phases such as SnS and Ag₂S as detected by XRD.     

Study of Pb-based and Pb-free perovskite solar cells using Cu-doped Ni1-xO thin films as hole transport material

SCAPS solar cell simulation program was applied to model an inverted structure of perovskite solar cells using Cu-doped Ni_1-xO thin films as hole transport layer. The Cu-doped Ni_1-xO film were made by co-sputtering deposition under different deposition conditions. By increasing the amount of the Cu-dopant, the film crystallinity enhanced whereas the bandgap energy decreased. The transmittance of the thin films decreased significantly by increasing the sputtering power of copper. High quality, uniform, compact, and pin-hole free films with low surface roughness were achieved. The structural, chemical, surface morphology, optical, electrical, and electronic properties of the Cu doped Ni_1-xO films were used as input parameters in the simulation of Pb-based (MAPbI_3-xCl_x) and Pb-free (MAGeI₃) perovskite solar cells. Simulation results showed that the performance of both Pb-based and Pb-free perovskite solar cell devices significantly enhanced with Cu-doped Ni_1-xO film. The highest power conversion efficiency (PCE) for the Pb-free perovskite solar cell is 8.9% which is lower than the highest PCE of 17.5% for the Pb-based perovskite solar cell.     

渗流作用下新型装配重力式挡土墙有限元分析

为研究渗流作用下新型装配重力式挡土墙应力变化及墙体排水通道对墙后土体固结的影响,采用ABAQUS进行有限元分析,有限元分析结果与模型试验结果相吻合,证明该模型的合理性。在此基础上研究渗流作用下墙体应力变化趋势及墙体排水通道对墙后土体固结效果的影响。研究结果表明:横向排水通道对墙后土体固结效果的影响优于纵向排水通道对土体固结效果的影响,墙体底部横向排水通道的影响作用最显著;渗流作用下墙体应力由上往下呈先增大后减小的趋势,墙体下部所受最大水平剪应力最大。     

Effect of metallurgical evolution during post-weld aging treatment on localised corrosion of resistance spot welding joints of A286 superalloy

The combined effect of resistance spot welding and precipitation hardening on the localised corrosion of A286 superalloy is studied. The specimens tested by double loop electrochemical potentiokinetic reactivation were welded in the solution treated condition, and then subjected to different precipitation hardening treatments. For both base metal and weld nugget, the maximum localised corrosion is reached when η phase is clearly observable. The fact that the localised corrosion resistance of weld nugget is different from that shown by base metal may be explained by the segregation of Ni and Ti towards the interdendritic region of weld nugget (studied by using scanning electron microscope/energy dispersive X-ray analysis).