BiVO4的添加对Nd0.2Ce0.8O1.9电解质微观结构和性能的影响

采用溶胶凝胶法制备BiVO₄（BV）和Nd_0.2Ce_0.8O_1.9（NDC）粉末,研究BV的加入对NDC电解质结构、形貌及电性能的影响。实验结果表明,NDC-5BV电解质的微观结构更致密,700℃时总电导率（σ_t）提高至3.35×10^-2 S·cm^-1,极化电阻（R_p）降低34%以上。单电池在700℃时的最大功率密度（MPD）为514 mW·cm^-2,开路电压（OCV）在70 h内可以保持良好的长期稳定性。     

服役温度对多壁碳纳米管/Li1.18Ni0.15Co0.15Mn0.52O2复合正极材料性能的影响

通过煅烧的方式制得多壁碳纳米管(MWCNT)质量分数为3%的MWCNT/Li1.18Ni0.15Co0.15Mn0.52O2锂离子电池复合正极材料,并测试了复合正极材料在不同服役温度环境下的电化学性能:-20和60℃下服役时,其放电容量分别高达169、303 mAh·g^-1,且展示出良好的倍率性能和循环稳定性。结合电化学阻抗测试结果可知,MWCNT均匀附着在层状粒子的表面,有效减少了电解液对电极材料的侵蚀,阻碍了表面膜的生成,同时提高了材料的电子电导率。     

离子对UIO-66-2OH光催化性能的影响

实际废水中存在的离子会对有机污染物的光催化降解产生影响。以ZrCl₄和2,5-二羟基对苯二甲酸为原料,通过水热合成法成功制备了金属有机骨架材料UIO-66-2OH。通过红外（IR）、X射线粉末衍射（XRD）、X射线光电子能谱（XPS）和扫描电子显微镜（SEM）对UIO-66-2OH的结构进行表征。利用水中常见的金属阳离子和无机阴离子,探索UIO-66-2OH的光催化性能。研究发现,金属阳离子Fe³⁺和无机阴离子HCO₃^-、CO₃^2-可以加快光催化降解的速度。然而,金属离子Na⁺、K⁺、Ca²⁺、Mg²⁺、Cu²⁺和无机阴离子Cl^-、SO₄^2-、PO₄^3-会抑制光催化性能,且离子价态越高,抑制效果越明显。     

水性颜料体系无树脂色浆的制备与应用

中性墨水属于热力学上不稳定的颜料悬浮体系,选择低黏度、高稳定性的色浆是保证墨水体系分散稳定性的重要手段之一。基于此,以颜料炭黑和酞菁蓝为着色剂,配合超分散剂(EK43)与协同增效剂(BM10),制备了两款适用于中性墨水体系的无树脂色浆。首次从色浆粒径与体系分散稳定性角度出发,确定了EK43、BM10用量以及最佳研磨时间,并对其理化性能、稳定性与书写性能进行分析测试。结果表明:在黑色浆中添加质量分数10.0%的EK43、2.5%的BM10,研磨时间为90 min;在蓝色浆中添加质量分数8.0%的EK43、2.0%的BM10,研磨时间为120 min时,两种色浆的粒径与分散稳定性均达到最佳。所制备的无树脂色浆颜料固含量高、黏度较低、储存稳定性好、着色力强,以其调配的中性墨水书写性能良好,且具有较好的离心稳定性和耐热稳定性。     

A Triple Crosslinking Design toward Epoxy Vitrimers and Carbon Fiber Composites of High Performance and Multi-shape Memory

It remains a challenge to use a simple approach to fabricate a multi-shape memory material with high mechanical performances. Here,we report a triple crosslinking design to construct a multi-shape memory epoxy vitrimer(MSMEV), which exhibits high mechanical properties,multi-shape memory property and malleability. The triple crosslinking network is formed by reacting diglycidyl ether of bisphenol F(DGEBF) with4-aminophenyl disulfide, γ-aminopropyltriethoxysilane(APTS) and poly(propylene glycol) bis(2-aminopropyl ether)(D2000). The triple crosslinking manifests triple functions: the disulfide bonds and the silyl ether linkages enable malleability of the epoxy network; the silyl ether linkages impart the network with high heterogeneity and broaden the glass transition region, leading to multi-shape memory property; a small amount of D2000 increases the modulus difference between the glassy and rubbery states, thereby improving the shape fixity ratio. Meanwhile,the high crosslinking density and rigid structure provide the MSMEV with high tensile strength and Young's modulus. Moreover, integrating carbon fibers and MSMEV results in shape memory composites. The superior mechanical properties of the composites and the recyclability of carbon fiber derived from the dissolvability of MSMEV make the composites hold great promise as structural materials in varied applications.     

酰胺修饰杂化硅胶整体柱的制备及其在莱克多巴胺检测中的应用

以氧化琼脂糖（AG）和四甲氧基硅烷（TMOS）为前驱体,通过溶胶－凝胶法制备 AG/SiO2整体柱,利 用酰胺化反应对整体柱进行酰胺基团修饰。通过X射线光电子能谱（XPS）、傅里叶变换红外光谱（FTIR）、N2 吸附－脱附和扫描电镜（SEM）等表征手段对所制备材料的结构和形貌进行分析。结果显示酰胺基团被成功修 饰至整体柱,该材料具有良好的通透性及较大的比表面积。以其为固相微萃取介质对羊肉中的莱克多巴胺进 行萃取富集,在优化的样品前处理条件下,采用基质添加标准曲线法,结合高效液相色谱－紫外（HPLC－ UV）检测,建立了羊肉中痕量莱克多巴胺的分析方法。该方法在 1. 94～1 170 ng/g范围内线性良好,相关系 数（r 2 ）为 0. 993 1,检出限（LOD）和定量下限（LOQ）分别为0. 618、1. 94 ng/g,3个不同加标水平下样品的平均回 收率为86. 6%～103%,相对标准偏差（RSD,n = 5）为4. 8%～7. 3%。该方法具有检出限低、回收率高、样品用 量少等特点,可用于羊肉中痕量莱克多巴胺的灵敏检测。     

Robust nickel silicate catalysts with high Ni loading for CO2 methanation

CO₂ is the main component of greenhouse gases and also an important carbon source. The hydrogenation of CO₂ to methane using Ni-based catalysts can not only alleviate CO₂ emissions but also obtain useful fuels. However, Ni-based catalysts face one major problem of the sintering of Ni nanoparticles in the process of CO₂ methanation. Thus, this work has synthesized a series of efficient and robust nickel silicate catalysts (NiPS−X) with different nickel content derived from nickel phyllosilicate by the hydrothermal method. It was found that the Ni loading plays a critical role in the structure and catalytic performance of the NiPS−X catalysts. The catalytic performance gradually increases with the increase of Ni loading. In particular, the highly dispersed NiPS-1.6 catalyst with a high Ni loading of 34.3 wt% could obtain the CO₂ conversion greater than 80%, and the methane selectivity was close to 100% for 48 h at 330 °C and the GHSV of 40,000 mL g⁻¹ h⁻¹. The excellent catalytic property can be assigned to the high dispersion of Ni nanoparticles and the strong interaction between the active component and the carrier, which is derived from a unique layered silicate structure with lots of nickel phyllosilicate and a large number of Lewis acid sites.     

The mosaic structure design to improve the anchoring strength of SiOx@C@Graphite anode

Silicon oxide (SiO_x)-based anodes have aroused great interest as the most promising alternative anode in the practical application of high-performance lithium-ion batteries. However, the electrochemical performance is inhibited because of the large volume change, and the electrode structure deteriorates during the cycling process, which hinders their practical application. In this article, a novel fabrication method for the synthesis of high-performance SiO_x@C@Graphite composites is presented. SiO_x particles are anchored on the graphite surface by chemical vapor deposition and compression molding. This structure makes up the shortcomings of poor electrical conductivity and poor bonding strength between SiO_x and graphite particles. It is beneficial to form a stable solid electrolyte interface and helps to maintain the structural integrity of electrode materials. As a result, the synthetic SiO_x@C@Graphite anode shows a high reversible capacity (2698.8 mA h), excellent cycle stability (about 76.9% capacity retention for 500 cycles) and a superior rate ability. Our research hopes to provide a new idea for improving the bonding strength of the surface coating.     

Feasibility of ultra-high performance liquid and gas chromatography coupled to mass spectrometry for accurate determination of primary and secondary phthalate metabolites in urine samples

Phthalates (PAEs) are ubiquitous toxic chemical compounds. During the last few years, some phthalate metabolites (MPAEs) have been proposed as appropriate biomarkers in human urine samples to determine PAE human intake and exposure. So, it is necessary to have fast, easy, robust and validated analytical methods to determine selected MPAEs in urine human samples. Two different instrumental methods based on gas (GC) and ultra-high performance liquid (UHPLC) chromatography coupled to mass spectrometry (MS) have been optimized, characterized and validated for the simultaneous determination of nine primary and secondary phthalate metabolites in urine samples. Both instrumental methods have similar sensitivity (detection limits ranged from 0.03 to 8.89 pg μL⁻¹ and from 0.06 to 0.49 pg μL⁻¹ in GC–MS and UHPLC–MS², respectively), precision (repeatability, expressed as relative standard deviation, which was lower than 8.4% in both systems, except for 5OH-MEHP in the case of GC–MS) and accuracy. But some advantages of the UHPLC–MS² method, such as more selectivity and lower time in the chromatographic runs (6.8 min vs. 28.5 min), have caused the UHPLC–MS² method to be chosen to analyze the twenty one human urine samples from the general Spanish population. Regarding these samples, MEP showed the highest median concentration (68.6 μg L⁻¹), followed by MiBP (23.3 μg L⁻¹), 5cx-MEPP (22.5 μg L⁻¹) and MBP (19.3 μg L⁻¹). MMP (6.99 μg L⁻¹), 5oxo-MEHP (6.15 μg L⁻¹), 5OH-MEHP (5.30 μg L⁻¹) and MEHP (4.40 μg L⁻¹) showed intermediate levels. Finally, the lowest levels were found for MBzP (2.55 μg L⁻¹). These data are within the same order of magnitude as those found in other similar populations.     

Tutorial review on validation of liquid chromatography–mass spectrometry methods: Part I

This is the part I of a tutorial review intending to give an overview of the state of the art of method validation in liquid chromatography mass spectrometry (LC–MS) and discuss specific issues that arise with MS (and MS/MS) detection in LC (as opposed to the “conventional” detectors). The Part I briefly introduces the principles of operation of LC–MS (emphasizing the aspects important from the validation point of view, in particular the ionization process and ionization suppression/enhancement); reviews the main validation guideline documents and discusses in detail the following performance parameters: selectivity/specificity/identity, ruggedness/robustness, limit of detection, limit of quantification, decision limit and detection capability. With every method performance characteristic its essence and terminology are addressed, the current status of treating it is reviewed and recommendations are given, how to determine it, specifically in the case of LC–MS methods.