New horizon in mechanochemistry—high-temperature,high-pressure mechanical synthesis in a planetary ball mill—with magnesium hydride synthesis as an example

A new route of materials synthesis, namely, high-temperature, high-pressure reactive planetary ball milling (HTPRM), is presented. HTPRM allows for the mechanosynthesis of materials at fully controlled temperatures of up to 450 °C and pressures of up to 100 bar of hydrogen. As an example of this application, a successful synthesis of magnesium hydride is presented. The synthesis was performed at controlled temperatures (room temperature (RT), 100, 150, 200, 250, 300, and 325 °C) while milling in a planetary ball mill under hydrogen pressure ($>$50 bar). Very mild milling conditions (250 rpm) were applied for a total milling time of 2 h, and a milling vial with a relatively small diameter (φ = 53 mm, V = ～0.06 dm³) was used. The effect of different temperatures on the synthesis kinetics and outcome were examined. The particle morphology, phase composition, reaction yield, and particle size were measured and analysed by scanning electron microscopy, X-ray diffraction, differential scanning calorimetry (DSC) techniques. The obtained results showed that increasing the temperature of the process significantly improved the reaction rate, which suggested the great potential of this technique for the mechanochemical synthesis of materials.     

Polyetherimide-LaNi5 composite films for hydrogen storage applications

This study investigates the preparation of polyetherimide (PEI) – LaNi₅ composites films for hydrogen storage. Prior to the polymer addition, LaNi₅ was ball-milled at different conditions (250, 350, and 450 RPM) and annealed at 500 °C for 1 h under vacuum. The composites were produced with BM-LaNi₅-350 (PEI/LaNi₅-350) and annealed BM-LaNi₅-350 (PEI/LaNi₅-350-TT). Membranes were successfully produced through solvent casting assisted by an ultrasonic bath. The particles dispersion and the film morphology did not change after hydrogenation cycles. In the H₂ sorption experiments at 43 °C and 20 bar, the films stored H₂ without incubation time; both samples reached a capacity of ~0.6 wt%. The H₂ sorption kinetics of PEI/LaNi₅-350 was comparable to that of BM-LaNi₅-350, whereas PEI/LaNi₅-350-TT presented significantly slower kinetics. LaNi₅ oxidation was hindered by PEI, showing that it can be explored to improve metal hydrides air resistance. The results demonstrated that PEI films filled with LaNi₅ are promising materials for hydrogen storage.     

Effect of Ni/tubular g-C3N4 on hydrogen storage properties of MgH2

Additive doping is one of the effective methods to overcome the shortcomings of MgH₂ on the aspect of relatively high operating temperatures and slow desorption kinetics. In this paper, hollow g-C₃N₄ (TCN) tubes with a diameter of 2 μm are synthesized through the hydrothermal and high-temperature pyrolysis methods, and then nickel is chemically reduced onto TCN to form Ni/TCN composite at 278 K. Ni/TCN is then introduced into the MgH₂/Mg system by means of hydriding combustion and ball milling. The MgH₂–Ni/TCN composite starts to release hydrogen at 535 K, which is 116 K lower than the as-milled MgH₂ (651 K). The MgH₂–Ni/TCN composite absorbs 5.24 wt% H₂ within 3500 s at 423 K, and takes up 3.56 wt% H₂ within 3500 s, even at a temperature as low as 373 K. The apparent activation energy (E_a) of the MgH₂ decreases from 161.1 to 82.6 kJ/mol by the addition of Ni/TCN. Moreover, the MgH₂–Ni/TCN sample shows excellent cycle stability, with a dehydrogenation capacity retention rate of 98.0% after 10 cycles. The carbon material enhances sorption kinetics by dispersing and stabilizating MgH₂. Otherwise, the phase transformation between Mg₂NiH₄ and Mg₂NiH_0.3 accelerates the re/dehydrogenation reaction of the composite.     

苏通GIL运输专用机具动力电池类型探讨

GIL运输专用机具是为安全、可靠、高效地完成苏通GIL综合管廊工程GIL单元的运输任务而研制的专用机具,其中动力电池系统设计是整机设计的重点之一。通过对各种常见动力电池优缺点的分析,并结合苏通GIL运输专用机具对动力电池的需求分析,确定了动力电池系统的技术路线,为苏通GIL运输专用机具的研制提供了坚实的基础。     

氢化物原子荧光光谱法测定酱油中微量铅的方法研究

建立了一种快速、高效的QuEChERS-高效液相色谱-质谱联用法（QuEChERS-HPLC-MS/MS）测定谷类杂粮制品中脱氧雪腐镰刀菌烯醇（DON）、3-乙酰脱氧雪腐镰刀菌烯醇（3-ADON）、15-乙酰脱氧雪腐镰刀菌烯醇（15-ADON）和玉米赤霉烯酮（ZON）共4种真菌毒素。样品前处理采用乙腈-水溶剂提取，经Florisil+C18+无水硫酸镁净化后检测。以0.10%甲酸-乙腈作为流动相，在质谱检测器的多反应监测模式下进行分析。结果表明，4种真菌毒素在各自的线性范围内线性关系良好，相关系数R2均大于0.999，回收率在85.1%～102.0%，相对标准偏差（RSD）为2.11%～6.22%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点，适用于谷类杂粮制品中DON、3-ADON、15-ADON 和ZON的分析和定量检测。     

Effect of Stoichiometry on Properties of Rare-Earth-Based Hydrogen Storage Alloy for Nickel-Metal Hydride Secondary Battery

Effect of stoichiometry on microstructures, electrochemical properties and PCT characteristics of the alloys MI(Ni0.71Co0.15-Al0.06Mn0.08)x (MI=Lanthanum-rich Michmetal, x=4.6~5.2) have been investigated. The lattice constants a, c, and cellvolumes of non-stoichiometric alloys are bigger than those of the stoichiometric alloy. With the increasing stoichiometry x,the value of a decreases, and the value of c and cell volume increases except for those of the stoichiometric alloy; the plateaupressure of PCT curve, discharge capacity and cycling stability all increase. The alloy with x=5.2 shows the highest dischargecapacity and the best cycling stability among the studied alloys.     

Effect of Synergistic Anticorrosion Treatments on Cycling Stability of Mg-Based Hydrogen Storage Electrode

In this paper, any two of the three anticorrosion agents, that is emulsifier (OP-10), soluble glass (Na2O·nSiO2) and glycerin (C3H8O3), were treated simultaneously on the surface of amorphous (a-) MgNi+5% Ml2Mg17 (Ml denotes the lanthanum-rich mish metal) electrode and the electrolyte. Effect of the synergistic anticorrosion treatment on charging/discharging cycle stability of the electrode was investigated. Contrasted with single treatment method, the cycling stability of the electrodes was further improved. The desirable synergistic anticorrosion method was that the electrode was treated by the soluble glass, and that OP-10 was added into the electrolyte. The cyclic voltammogram (CV) results of the electrode show clearly that the anticorrosion agent can change the electrochemical activity and mechanism of the electrode. The concentration of the anticorrosion agent in the electrolyte treated by the synergistic anticorrosion method was also investigated. The appropriate concentration of the anticorrosion agents in the electrolyte is 0.143%.     

直流法测量钯氢化物电极电阻时的阻值偏移

讨论了直流法在线测量钯氢化物电极电阻时的电化学效应，计算了电解液的共导、测量电流与电解电流引起的浓差电池效应以及电极作为集流体引起的电阻贡献。结果表明：当电极具有高的长度与半径比值、粗糙的表面、高的溶液电导以及大的电解电流时容易引起显著的附加电阻。     

H原子对固态合金化颗粒表面成份分布影响的研究

本文研究了氢化物ＴｉＨ２对Ｆｅ＋Ｔｉ机械合金化非晶储氢合金的表面成份偏聚和性能的影响。应用Ｘ射线光电子谱（ＸＰＳ）和俄歇电子谱（ＡＥＳ）对样品表面由表及里逐层测量成份分布。同时应用热重分析方法研究了样品氧化性能和产物。研究结果表明，在机械合金化过程中，Ｈ原子不仅能使ＦｅＴｉ非晶化，同时促使表面产生明显的Ｆｅ原子偏聚。表面Ｆｅ／Ｔｉ原子比接近７。非晶ＦｅＴｉ（Ｈ）相的氧化分两个阶段进行，Ｔｉ原子首先氧化（８３３Ｋ），随后Ｆｅ原子氧化（８９０Ｋ）。     

Ni|MH二次电池负极用贮氢合金的研究发展

本文详细综述了近年Ni MH二次电池负极用贮氢合金的研究发展概况。依次阐述了AB5、AB2与Ni Ni基、V Ti基固溶体合金以及Mg Ni合金的电化学性能。讨论了改善电化学性能的一些方法 ,同时给出目前一些研究成果