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Improving hydrogen storage thermodynamics and kinetics of Ce-Mg-Ni-based alloy by mechanical milling with TiF_(3)

Journal of Magnesium and Alloys 2024年第4期12卷 1593-1607页

作者： Hongwei Shang Wei zhang Xin Wei Yaqin Li Zeming Yuan Jun Li Yanghuan Zhang School of Mechanical and Electrical Engineering Chuzhou UniversityChuzhou 239000China Department of Functional Material Research Central Iron and Steel Research InstituteNo.76 Xueyuannan RoadHaidian DistrictBeijing 100081China Key Laboratory of Integrated Exploitation of Bayan-Obo Multi-Metal Resources Inner Mongolia University of Science and TechnologyBaotou 014010China China Rare Earth New Material(Weishan)Co. Ltd.Jining 277600China

Mg-based hydrides are too stable and the kinetics of hydrogen absorption and desorption is not satisfactory.An efficient way to improve these shortcomings is to employ reactive ball milling to synthesize the nanocomposite materials of Mg and additives.In this experiment,TiF_(3)was selected as an additive,and the mechanical milling method was employed to prepare the experimental alloys.The alloys used in this experiment were the as-cast Ce_(5)Mg_(85)Ni_(10),as-milled Ce_(5)Mg_(85)Ni_(10)and Ce_(5)Mg_(85)Ni_(10)+3 wt.%TiF3.The phase transformation,structural evolution,isothermal and non-isothermal hydrogenation and dehydrogenation performances of the alloys were inspected by XRD,SEM,TEM,Sievert apparatus,DSC and TGA.It revealed that nanocrystalline appeared in the as-milled samples.Compared with the as-cast alloy,ball milling made the particle dimension and grain size decrease dramatically and the defect density increase significantly.The addition of TiF_(3)made the surface of ball milling alloy particles markedly coarser and more irregular.Ball milling and adding TiF_(3)distinctly improved the activation and kinetics of the alloys.Moreover,ball milling along with TiF_(3)can decrease the onset dehydrogenation temperature of Mg-based hydrides and slightly ameliorate their thermodynamics.

关键词： Mg-based hydrides TiF_(3) Ball milling Thermodynamics Kinetics

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The variation of microstructures,spectral characteristics and catalysis effects of Fe^3+ and Zn^2+ co-doped CeO2 solid solutions

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Journal of Rare Earths 2020年第3期38卷 241-249页

作者： Guofang zhang Yiming Li Xin Zhao Jianyi Xu Yanghuan Zhang School of Material and Metallurgy Inner Mongolia University of Science and TechnologyBaotou 014010China

Fe^3+and Zn^2+ions were doped into the lattice of CeO2 via the hydrothermal method.The micro structure and spectra features were analyzed systemically.XRD results show that the solid solubility of Fe^3+and Zn^2+ions in Ce1-x(Fe0.5Zn0.5)xO2 can be identified as x=0.16.The cell volumes are decreased by increasing the doped content.The TEM graphs prove that the grain size of the sample is about 10 nm,and the EDS result indicates that the doped contents are in accordance with that of the theory concentrations.Meanwhile,the doping also causes the increasing concentrations of the defects and oxygen vacancies which are supported by the XPS,Raman,UV and PL characterizations.The samples exhibit better catalytic activities for improving the hydrogen storage properties and the electrochemical kinetics of the ball milled Mg2Ni based composites.Further,the catalysis effects are improved by increasing the doped contents,which can be ascribed to the increasing contents of the oxygen vacancies,defects,the special electron transition states and the nature of the doped ions in CeO2-based solid solutions.

关键词： Ce1-x(Fe0.5Zn0.5)xO2 solid solutions Hydrothermal method Hydrogen storage Catalysis Rare earths

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Single phase A2B7-type La-Mg-Ni alloy with improved electrochemical properties prepared by melt-spinning and annealing

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Journal of Rare Earths 2019年第12期37卷 1305-1311页

作者： Yiming Li Zhuocheng Liu Guofang zhang Yanghuan Zhang Huiping Ren Key Laboratory of Integrated Exploitation of Bayan Obo Multi-Metal Resources Inner Mongolia University of Science and Technology

La-Mg-Ni alloys were prepared by melt-spinning with different cooling rates and followed by annealing.Elevation of the cooling rate leads to refinement of the grains size and increasing of the abundance of LaNis.Annealing is favorable to formation of the A2 B7-type phase and promotes the discharge capacity,cycling stability and high rate discharge ability of the as-spun alloys.Phase constitution of the annealed alloys is found to be closely related to the microstructure of the as-spun alloys.A single phase A2 B7-type microstructure is obtained in the annealed alloy which is attributed to the lower abundance of the LaNis of the original alloy spun with lower cooling rate.Formation of the single phase A2 B7-type microstructure is also ascribed to the isolated and homogeneous distribution of the morphology of the as-spun alloy.The single phase alloy presents higher discharge capacity and better cycling stability compared with other annealed alloys.

关键词： La-Mg-Ni electrode alloys Melt-spinning Annealing Single phase microstructure Electrochemical properties Rare earths

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Structure and electrochemical hydrogen storage behaviors of Mg-Ce-Ni-Al-based alloys prepared by mechanical milling

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Journal of Rare Earths 2020年第10期38卷 1093-1102,I0003页

作者： Yanghuan Zhang Pengpeng Wang Wei zhang Wengang Bu Yan Qi Shihai Guo Key Laboratory of Integrated Exploitation of Baiyun Obo Multi-Metal Resources Inner Mongolia University of Science and TechnologyBaotou 014010China Department of Functional Material Research Central Iron and Steel Research InstituteBeijing 100081China

The influences of milling time and Ce content on the electrochemical property and micro structure of asmilled Mg1-xCexNi0.9Al0.1(x=0,0.02,0.04,0.06,0.08)+50 wt%Ni alloys were investigated systematically.The as-milled alloys have an outstanding activation property.The cycle stability conspicuously grows up with milling time and Ce proportion increasing.The capacity retention rate at 100 th cycle of x=0.02 alloy augments from 47% to 63% when prolonging milling time from 5 to 30 h and it grows from55% to 82% for the 30 h milled alloy with Ce content growing from 0 to 0.08.The discharge capacity of x=0.02 alloy grows up invariably with milling time prolonging,while that of the 30 h milled alloys has the maximal value of 578.4 mAh/g with Ce content increasing.Moreover,the electrochemical kinetic properties of alloys significantly improve with milling duration extending,while they have the maximal values with Ce proportion varying.

关键词： Mg-based alloy Ce substituting Mg Mechanical milling Electrochemical property Rare earths

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Enhanced hydrogen storage performance of Mg-Cu-Ni system catalyzed by CeO2 additive

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Journal of Rare Earths 2020年第9期38卷 983-993,I0003页

作者： Yi Yin Bo Li Zeming Yuan Yan Qi Yanghuan Zhang Department of Functional Material Research Central Iron and Steel Research InstituteBeijing 100081China Key Laboratory of Integrated Exploitation of Baiyun Obo Multi-Metal Resources Inner Mongolia University of Science and TechnologyBaotou 014010China

In this paper,the as-cast Mg85Cu5Ni10 alloy and Mg85Cu5Ni10-x wt%CeO2(x=0,4,8)alloys were prepared successfully by vacuum induction smelting and ball milling.The microstructure,hydrogen absorption/desorption kinetics and thermodynamics performances of the alloys were studied in detail.The results show that the Mg85Cu5Ni10 alloys with CeO2 additive have faster hydrogenation/dehydrogenation kinetics and better thermodynamic properties.The dehydrogenation activation energy is reduced to 81.211 kJ/mol from 119.142 by adding 8 wt%CeO2.CeO2 contributes to producing structural defects,nanocrystallines,grain boundaries,partial amorphous,lattice dislocations and cracks which are favorable to provide more hydrogen diffusion channels during hydriding/dehydriding process.Meanwhile,CeO2 additive weakens the bond energy of Mg-H.These micro structural changes caused by CeO2 additive improve the hydrogen storage performance of Mg85Cu5Ni10 markedly.

关键词： Mg-Cu-Ni alloy CeO2 additive Ball milling Dehydrogenation activation energy Thermodynamic property

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Catalytic effect comparison of TiO_(2) and La_(2)O_(3) on hydrogen storage thermodynamics and kinetics of the as-milled La-Sm-Mg-Ni-based alloy

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Journal of Magnesium and Alloys 2021年第6期9卷 2063-2077页

作者： Yanghuan Zhang Xin Wei Wei zhang Zeming Yuan Jinliang Gao Huiping Ren Key Laboratory of Integrated Exploitation of Baiyun Obo Multi-Metal Resources Inner Mongolia University of Science and TechnologyNo.7 Aerding RoadKun DistrictBaotou 014010China Department of Functional Material Research Central Iron and Steel Research InstituteNo.76 Xueyuannan RoadHaidian DistrictBeijing 100081China Weishan Cisri-Rare Earth Materials Co. Ltd.Jining 277600China

In this investigation,mechanical grinding was applied to fabricating the Mg-based alloys La_(7)Sm_(3)Mg_(80)Ni_(10)+5 wt.%M(M=None,TiO_(2),La_(2)O_(3))(named La_(7)Sm_(3)Mg_(80)Ni_(10)-5 M(M=None,TiO_(2),La_(2)O_(3))).The result reveals that the structures of as-milled alloys consist of amorphous and nanocrystalline.The particle sizes of the added M(M=TiO_(2),La_(2)O_(3))alloys obviously diminish in comparison with the M=None specimen,suggesting that the catalysts TiO_(2)and La_(2)O_(3)can enhance the grinding efficiency.What’s more,the additives TiO_(2)and La_(2)O_(3)observably improve the activation performance and reaction kinetics of the composite.The time required by releasing 3 wt.%hydrogen at553,573 and 593 K is 988,553 and 419 s for the M=None sample,and 578,352 and 286 s for the M=TiO_(2)composite,and 594,366,301 s for the La_(2)O_(3)containing alloy,respectively.The absolute value of hydrogenation enthalpy change|△H|of the M(M=None,TiO_(2),La_(2)O_(3))alloys is 77.13,74.28 and 75.28 kJ/mol.Furthermore,the addition of catalysts reduces the hydrogen desorption activation energy(E_(a)^(de)).

关键词： Mg-based alloy Ball milling Catalysts Hydrogen storage kinetics

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Phase transformation,thermodynamics and kinetics property of Mg90Ce5RE5(RE=La,Ce,Nd)hydrogen storage alloys

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Journal of Materials Science & Technology 2020年第16期47卷 84-93页

作者： Hui Yong Shihai Guo Zeming Yuan Yan Qi Dongliang Zhao Yanghuan Zhang Department of Functional Material Research Central Iron and Steel Research InstituteBeijing 100081China Key Laboratory of Integrated Exploitation of Baiyun Obo Multi-Metal Resources Inner Mongolia University of Science and TechnologyBaotou 014010China

The Mg90Ce5 RE5(RE=La,Ce,Nd)alloys were prepared by a vacuum induction furnace and their micro structure,phase transformation,thermodynamics and kinetics property were systematically studied by XRD,SEM,TEM,and PCT characterization methods.The result shows that the activated alloys are composed of Mg/MgH2 and corresponding REH2+x with nanoscale.The REH2+x grain with Ce and La or Nd functional group have lower nucleation potential barriers than CeH2+x grains as the nucleation location,thus improve the hydrogen absorption kinetics of these alloys among which the Mg90Ce5Nd5 alloy can absorb 90%of the hydrogen within 2 min at 320℃.In addition,the Mg90Ce10 alloy has the lowest activation energy with 103.2 kJ mol-1 and the fastest desorption kinetics,which can release 5 wt%of the hydrogen within 20 min at 320℃.This is a correlation with grain size and the in-suit formed CeH2.73/CeO2 interface.Moreover,the co-doping Ce and La or Nd can effectively disorganize the thermodynamic stability of Mg-based hydrogen storage alloys to a certain degree,but the dehydrogenation kinetics of that still is restricted by the recombination energy of hydrogen ions on the surface.

关键词： RE-Mg-based alloy Hydrogen storage Thermodynamics Kinetics Intermetallic

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Phase evolution,hydrogen storage thermodynamics and kinetics of ternary Mg90Ce5Sm5 alloy

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Journal of Rare Earths 2020年第6期38卷 633-641页

作者： Hui Yong Shihai Guo Zeming Yuan Wei zhang Yan Qi Dongliang Zhao Yanghuan Zhang Department of Functional Material Research Central Iron and Steel Research InstituteBeijing 100081China Key Laboratory of Integrated Exploitation of Baiyun Obo Multi-Metal Resources Inner Mongolia University of Science and TechnologyBaotou 014010China

Greatly stable thermodynamics and sluggish kinetics impede the practical application of Mg-based hydrogen storage alloys.The modifications of composition and structure are important strategies in turning these hydrogen storage properties.In this study,Mg-based Mg90Ce5 Sm5 ternary alloy fabricated by vacuum induction melting was investigated to explore the performance and the reaction mechanism as hydrogen storage material by X-ray diffraction(XRD),scanning electron microscope(SEM),transmission electron microscopy(TEM) and pressure-composition isotherms(PCI) measurements.The results indicate that the Mg-based Mg90Ce5 Sm5 ternary alloy consists of two solid solution phases,including the major phases(Ce,Sm)5 Mg41 and the minor phases(Ce,Sm)Mg12.After hydrogen absorption,these phases transform into the MgH2 and(Ce,Sm)H2.73 phase,while after hydrogen desorption,the MgH2 transforms into the Mg phase,but the(Ce,Sm)H2.73 phases are not changed.The alloy has a reversible hydrogen capacity of about 5.5 wt% H2 and exhibits well isothermal hydrogen absorption kinetics.Activation energy of 106 kJ/mol was obtained from the hydrogen desorption data between 573 and 633 K,which also exhibits the enhanced kinetics compared with the pure MgH2 sample,as a result of bimetallic synergy catalysis function of(Ce,Sm)H2.73 phases.The rate of hydrogen desorption is controlled by the release and recombination of H2 from the Mg surface.Furthermore,the changes of enthalpy and entropy of hydrogen absorption/desorption were calculated to be-80.0 kJ/mol H2,-137.5 J/K/mol H2 and 81.2 kJ/mol H2,139.2 J/K/mol H2,respectively.

关键词： Hydrogen storage Reaction mechanism Kinetics Thermodynamics Activation energy Rare earths

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通信标准必要专利跨领域许可FRAND义务研究

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交大法学 2024年第1期 126-147页

作者：张扬欢汕头大学马克思主义学院

在通信标准必要专利跨领域许可的进程中,通信产业与标准产品产业就供应链上的许可模式存在分歧。回溯分歧的发生背景和诉讼呈现可知,该分歧的实质为FRAND义务分歧,且应被锚定为终端级自由许可和组件级优先许可两种模式的争议。经总体检... 详细信息

在通信标准必要专利跨领域许可的进程中,通信产业与标准产品产业就供应链上的许可模式存在分歧。回溯分歧的发生背景和诉讼呈现可知,该分歧的实质为FRAND义务分歧,且应被锚定为终端级自由许可和组件级优先许可两种模式的争议。经总体检视,终端级许可将引致上游供应商实施行为法律确定性缺失、高交易成本困境与专利劫持的潜在风险,组件级许可则具有提升许可效率和抑制专利劫持的合理性,然而组件级优先许可义务的设定不符合比例原则。SEP持有人在有权自由选择许可层级的基础上,应充分履行包含FRAND谈判义务与SEP开放义务的FRAND义务,以消除前述风险。SEP持有人违反FRAND谈判义务的,将受SEP侵权不停止规则的规制,SEP开放义务则依托利益第三人条款的明确约定或合同解释得到履行。

关键词：标准必要专利 FRAND义务专利劫持侵权不停止利益第三人合同

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A comparison study of hydrogen storage properties of as-milled Sm_5Mg_(41) alloy catalyzed by CoS_2 and MoS_2 nano-particles

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Journal of Materials Science & Technology 2018年第10期34卷 1851-1858页

作者： Zeming Yuan Bangwen zhang Yanghuan Zhang Shihai Guo Xiaoping Dong Dongliang Zhao InstrumentalAnalysis Center Inner Mongolia University of Science and Technology Baotou 014010 China Department of Functional Material Research Central Iron and Steel Research Institute Beijing 100081 China Key Laboratory of Integrated Exploitation of Baiyun Obo Multi-Metal Resources Inner Mongolia University of Science and Technology Baotou 014010China Department of Mechanical Engineering Hebei University Baoding 071002 China

The influences of the catalysts of CoS2 and MoB2 nano-particles on microstructure and hydrogen stor-age behaviors of as-milled SmsMg41 alloy have been compared in this work. The SmsMg41 ＋ 5 wt.% M （M = COS2, MoS2） alloys were prepared by milling the mechanical ground as-cast SmsMg41 alloy powders （particle size ≤75 μm） with 5 wt.% CoS2 or MoS2 nano-particles （particle size ≤ 30 nm）, respectively. The results demonstrate that the CoS2 and MoS2 nanoparticles are embedded into the alloy surface, which is nanostructure containing some crystal defects, such as dislocation, grain boundary and twin etc. Those microstructures play a beneficial role in reducing the total potential barrier that the hydrogen absorption or desorption reactions must overcome, hence improving the hydrogen storage kinetics of the alloys. The as-milled alloys are composed of SmsMg41 and SmMg3 phases, and ball milling refines their crys-tal grains. The MgH2 and Sm3H7 phases appear after hydrogenation, while Mg and Sm3H7 phases exist after dehydrogenation. The dehydriding activation energy of M = CoS2 and MoS2 alloys are 101.67 and 68.25 kJ/mol H2 respectively. The initial hydrogen desorption of M = CoS2 and MoS2 alloys are 252.9 ℃ and 247.8 ℃.The hydrogenation and dehydrogenation enthalpy changes of M = MoS2 alloy are a little smaller than that of MzCoS2 alloy. Therefore, the catalyst MoS2 can improve the as-milled SmsMg41 alloy in hydrogen storage property more effectively than C0S2.

关键词： SmsMg41 alloy CoS2 and MoS2 catalyst Milling Activation energy Hydrogen storage kinetics

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