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Layer stacked SiO_(x) microparticle with disconnected interstices enables stable interphase and particle integrity for lithium-ion batteries

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Journal of Energy Chemistry 2023年第11期86卷 300-307,I0007页

作者： Yang Ren Xucai Yin Lizhi Xiang Rang Xiao hua huo Geping Yin Chunyu Du MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage and Institute of Advanced Chemical Power Sources School of Chemistry and Chemical EngineeringHarbin Institute of TechnologyHarbin 150001HeilongjiangChina Guangxi Key Laboratory of Petrochemical Resource Processing and Process Intensification Technology School of Chemistry and Chemical EngineeringGuangxi UniversityNanning 530004GuangxiChina

Severe mechanical fractu re and unstable interphase,associated with the large volumetric expansion/contraction,significantly hinder the application of high-capacity SiO_(x)materials in lithium-ion batteries.Herein,we report the design and facile synthesis of a layer stacked SiO_(x)microparticle(LS-SiO_(x))material,which presents a stacking structure of SiO_(x)layers with abundant disconnected interstices.This LS-SiO_(x)microparticle can effectively accommodate the volume expansion,while ensuring negligible particle expansion.More importantly,the interstices within SiO_(x)microparticle are disconnected from each other,which efficiently prevent the electrolyte from infiltration into the interior,achieving stable electrode/-electrolyte interface.Accordingly,the LS-SiO_(x)material without any coating delivers ultrahigh average Coulombic efficiency,outstanding cycling stability,and full-cell applicability.Only 6 cycles can attain>99.92%Coulombic efficiency and the capacity retention at 0.05 A g^(-1)for 100 cycles exceeds99%.After 800 cycles at 1 A g^(-1),the thickness swelling of LS-SiO_(x)electrode is as low as 0.87%.Moreover,the full cell with pure LS-SiO_(x)anode exhibits capacity retention of 91.2%after 300 cycles at 0.2 C.This work provides a novel concept and effective approach to rationally design silicon-based and other electrode materials with huge volume variation for electrochemical energy storage applications.

关键词： Lithium-ion batteries Silicon oxide Layer stacked structure Disconnected interstices Coulombic efficiency

Insight into the Electrochemical Behaviors of NCM811|SiO-Gr Pouch Battery through Thickness Variation

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Energy & Environmental Materials 2023年第5期6卷 211-218页

作者： Xingqin Wang Youzhi Song Hao Cui Jianhong Liu hua huo Li Wang Yunzhi Gao Xiangming He Key Laboratory of Materials for New Energy Conversion and Storage(Ministry of Industry and Information Technology) School of Chemistry and Chemical EngineeringHarbin Institute of TechnologyHarbin 150001China Risesun Mengguli new energy Science and Technology Co.LTD Beijing 102200China Institute of Nuclear and New Energy Technology Tsinghua UniversityBeijing 100084China

LiNi0.8Co0.1Mn0.1O2(NCM811)|SiOx-graphite(SiO-Gr.)battery chemistry is of intensive attention because its achievable practical energy density is approaching impressively 300 Wh Kg^(-1).However,it still suffers rapid capacity fades during repeated cycles,both chemical,electrochemical and mechanical irreversibility contribute.A comprehensive understanding behind the fading behavior of the cell chemistry is required before fully realize the benefits of this chemistry.Herein,the in-situ thickness variation is introduced as a diagnostic technique and is performed on 5-55 Ah NCM811|SiO-Gr cells.With the help of Li reference electrode and in-situ X-ray diffraction device,the correspondence between thickness variation and the electrode potential is carefully investigated.Firstly,the NCM811|SiO-Gr cell is characterized with the maximum cell thickness at around 80%state-of-charge(SOC)in the discharge process,rather than at 100%SOC.Secondly,the electrochemical behaviors during rate charge/discharge are diagnosed,and a Li platting signal is resolved from thickness variation profile at 2C.This work confirms that the thickness monitoring is a nondestructive and informative complement to conventional diagnostic techniques for failure analysis of pouch cells.

关键词： diagnostic technique electrochemical behavior NCM811 cathode Si-containing anode thickness variation

Construction of polysulfides defense system for greatly improving the long cycle life of metal sulfide anodes for sodium-ion batteries

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Journal of Energy Chemistry 2022年第8期31卷 210-217,I0007页

作者： Xucai Yin Yang Ren Libin Wu Zhiguo Zhang Chunyu Du Jiajun Wang Gepin Yin hua huo Key Laboratory of Materials for New Energy Conversion and Storage Ministry of Industry and Information TechnologySchool of Chemistry and Chemical EngineeringHarbin Institute of TechnologyHarbin 150001HeilongjiangChina

Metal sulfides are promising anode materials for sodium ion batteries(SIBs)due to their high theoretical specific capacity and abundant source.Nevertheless,significant challenges,including large volume change,sluggish Na^(+)transport kinetics and polysulfides intermediates,have greatly affect their long cycle stability.Unfortunately,the majority of current studies only focus on the first two aspects,but lack of sufficient attention and insights into the effect of polysulfides intermediates.Here,a porous of CoS_(x)(P-CoS_(x))electrode material is fabricated as an example to investigate the influence of polysulfides on its cycling performance.The results show that polysulfides cause a slight loss of reversible capacity during the battery cycling,while the failure of the battery is due to its significant fluctuations in reversible capacity after extensive cycles.Detailed analyses demonstrate that the intense fluctuation in capacity originates from the faster growth of dendrites caused by the reaction of sodium polysulfides with sodium foil and/or the reaction of elemental sulfur with sodium foil to penetrate the separator,resulting in a local short circuit.To suppress these undesirable side reaction,N,S co-doped porous carbon tubes(N,S-PC)rich in C–S and C–N bonds have been added to adsorb polysulfides and alleviate their reaction with sodium foil.As a result,the capacity of the P-CoS_(x) electrode with N,S-PC(P-CoS_(x)/N,S-PC)remains stable without significant fluctuations for 1000 cycles,which is much better than that of the pure P-CoS_(x) electrode(intense fluctuation in capacity after 320 cycles).Our work offers insights into the crucial influence of polysulfides on the cycle performance of the P-CoS_(x) anode and provides a feasible strategy to prolong the cycle life of metal sulfide anode for SIBs.

关键词： Intense fluctuation in capacity Polysulfides N,S-PC tubes Anode Sodium-ion batteries

Tuning the phase evolution pathway of LiNi_(0.5)Mn_(1.5)O_(4) synthesis from binary intermediates to ternary intermediates with thermal regulating agent

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Journal of Energy Chemistry 2022年第2期31卷 62-70页

作者： Libin Wu hua huo Qun Wang Xucai Yin Shu Guo Jiajun Wang Chunyu Du Pengjian Zuo Geping Yin Yunzhi Gao Key Laboratory of Materials for New Energy Conversion and Storage(Ministry of Industry and Information Technology) School of Chemistry and Chemical EngineeringHarbin Institute of TechnologyHarbin 150001HeilongjiangChina Center of Analysis and Measurement Harbin Institute of TechnologyHarbin 150001HeilongjiangChina

Transition metal cation ordering is essential for controlling the electrochemical performance of cubic spinel LiNi_(0.5)Mn_(1.5)O_(4)(LNMO),which is conventionally adjusted by optimizing the high temperature sintering and annealing procedures.In this present work,multiple characterization techniques,including 6,7Li NMR,XRD and HRTEM,have been combined to trace the phase transformation and morphology evolution during synthesis.It has been illustrated that simultaneous formation of LiMn_(2)O_(4)(LMO)and LiNiO_(2)(LNO)binary oxides and their conversion into highly reactive LixNi^(3+)_(y)Mn_(3.5+)_(z)O ternary intermediate is a thermal dynamically difficult but crucial step in the synthesis of LNMO ternary oxide.A new strategy of modifying the intermediates formation pathway from binary mode to ternary mode using thermal regulating agent has been adopted.LNMO synthesized with thermal regulating agent exhibits supreme rate capability,long-cycling performance(even at elevated temperature)and excellent capacity efficiency.At a high rate of 100 C,the assembled battery delivers a discharge capacity of 99 mAh g^(-1).This study provides a way to control the formation pathway of complex oxides using thermal regulating agent.

关键词： Cation ordering LiNi_(0.5)Mn_(1.5)O_(4) Lithium ion batteries Synthesis of ternary oxide Thermal regulation

The origins of kinetics hysteresis and irreversibility of monoclinic Li_(3)V_(2)(PO_(4))_(3)

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Journal of Energy Chemistry 2022年第4期31卷 593-603页

作者： hua huo Zeyu Lin Guiming Zhong Shuaifeng Lou Jiajun Wang Yulin Ma Changsong Dai Yueping Xiong Geping Yin Yong Yang Key Laboratory of Materials for New Energy Conversion and Storage(Ministry of Industry and Information Technology) School of Chemistry and Chemical EngineeringHarbin Institute of TechnologyHarbin 150001HeilongjiangChina State Key Laboratory for Physical Chemistry of Solid Surface and Department of Chemistry College of Chemistry and Chemical EngineeringXiamen UniversityXiamen 361005FujianChina Xiamen Institute of Rare Earth Materials Haixi InstitutesChinese Academy of SciencesXiamen 361021FujianChina

Monoclinic Li_(2)V_(2)(PO_(4))_(3);is a promising cathode material with complex charge–discharge behavior.Previous structural investigation of this compound mainly focuses on local environments;while the reaction kinetics and the driving force of irreversibility of this material remain unclear.To fully understand the above issues,both the equilibrium and the non-equilibrium reaction routes have been systematically investigated in this study.Multiple characterization techniques including X-ray diffraction,variable temperature(spinning rate)and ex/in situ ^(7)Li,^(31)P solid state NMR have been employed to provide comprehensive insights into kinetics,dynamics,framework structure evolution and charge ordering,which is essential to better design and application of lithium transition metal phosphate cathodes.Our results suggest that the kinetics process between the non-equilibrium and the quasi-equilibrium delithiation pathways from Li_(2)V_(2)(PO_(4))_(3);to V_(2)(PO_(4))_(3);is related with a slow relaxation from two-site to one-site delithiation.More importantly,it has been demonstrated that the irreversibility in this system is not solely affected by cation and/or charge ordering/disordering,but mainly driven by framework structure distortion.

关键词： NMR spectroscopy Electrochemistry Solid-state structures Kinetics

Nuclear magnetic resonance studies of organic-inorganic composite solid electrolytes

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Magnetic Resonance Letters 2021年第2期1卷 142-152页

作者： Xueyan Zhang hua huo MIIT Key Laboratory of Cnitical Materials Technology for New Energy Conversion and Storage School of Chemistry and Chermical EngineeringHarbin Institute of TechnologyNo.92 West Da Zhi StreetHarbin150001China

Solid electrolytes have received widespread attention due to their higher safety than liquid electrolytes in the past decades.In particular,organic-inorganic composite solid electro-lytes(CSEs)in which inorganic fllers dispersed in polymer solid electrolytes are consid-ered to be one of the most promising candidate electrolytes for high-performance solid-state lithium batteries.Understanding the local environments and the conduction pathway/dynamics of Lit is essential for the design of high-performance CSEs.Nuclear magnetic resonance(NMR)is a non-invasive quantitative technique that has unique ca-pabilities in providing molecular structure information,morphological evolution,and measuring the movement of ions at different time scales.Therefore,for battery re-searchers,an accurate and comprehensive under standing of the basic principles and experimental design of solid-state NMR(SSNMR)is of great significance for investigating the abundant molecular structure and dynamics information in CSEs.The specific appli-cations of the SSNMR technique in CSEs are briefly introduced in this present review.

关键词： Composite solid electrolytes(CSEs) Conduction pathway Solid-state NMR(SSNMR) Solid-state lithium batteries

Effect of La0.8Sr0.2Co0.2Fe0.8O3-δ morphology on the performance of composite cathodes

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Progress in Natural Science:Materials International 2014年第1期24卷 24-30页

作者： Erqing Zhao Xiaotian Liu Lianbao Liu hua huo Yueping Xiongn School of Chemical Engineering and Technology Harbin Institute of Technology

In the present work,one dimensional La0.8Sr0.2Co0.2Fe0.8O3 δ(LSCF) nanofibers with the mean diameter of about 100 nm prepared by electrospinning were deposited on Gd0.2Ce0.8O1.9(GDC) electrolyte followed by sintering to form one dimensional LSCF nanofiber cathode. And LSCF/GDC composite cathodes were formed by introducing GDC phases into LSCF nanofiber scaffold using infiltration method. The polarization resistances for the composite cathode with an optimal LSCF/GDC mass ratio of 1/0.56 are 0.27,0.14 and 0.07 Ω cm2at 650,700 and750 1C,respectively,which are obviously smaller than 2.26,0.78 and 0.29 Ω cm2of pure LSCF nanofiber cathode. And the activation energy is1.194 eV,which is much lower than that of pure LSCF nanofiber cathode(1.684 eV). These results demonstrate that the infiltration of GDC into LSCF nanofiber scaffold is an effective approach to achieve high performance cathode for solid oxide fuel cells(SOFCs). In addition,the performance of composite cathode in this work was also compared with that of our previous nanorod structured LSCF/GDC composite cathode.

关键词： La0.8Sr0.2Co0.2Fe0.8O3-δ Composite cathode Electrospinning Infiltration

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钾霞石制备体系碱性滤液的利用技术

岩石矿物学杂志 2024年第1期43卷 125-130页

作者：路华龙霍光祥段永华勾明雷刘军娜刘晨河南科技大学化学化工学院河南洛阳471000

为处理钾长石水热制备钾霞石所产生的碱性滤液,本文采用水热法,考察了氢氧化铝溶解时间、晶化时间、晶化温度、水碱比对钾霞石产率和白度的影响,并对合成钾霞石物相进行了表征。结果表明,合成钾霞石的最佳条件为,氢氧化铝溶解时间为1.5... 详细信息

为处理钾长石水热制备钾霞石所产生的碱性滤液,本文采用水热法,考察了氢氧化铝溶解时间、晶化时间、晶化温度、水碱比对钾霞石产率和白度的影响,并对合成钾霞石物相进行了表征。结果表明,合成钾霞石的最佳条件为,氢氧化铝溶解时间为1.5 h,晶化时间为4 h,晶化温度280℃,水碱比为1.8。XRD结果表明,产物为钾霞石粉体。傅里叶变换红外光谱表明,Al(OH)_(3)中的Al在水热条件下进入到Si—O骨架中形成了Si—O—Al官能团,从而印证了钾霞石的合成。差热分析结果表明,合成钾霞石具有良好的热稳定性。氮气吸附结果表明,合成钾霞石比表面积为5.18 m^(2)/g,平均孔径为32.98 nm。实现了钾长石水热制备钾霞石所剩碱性滤液的资源化利用,并为钾长石水热制备钾霞石提供了一种母液循环的思路,使水热制备钾霞石工业化成为一种可能。

关键词：钾霞石水热法氢氧化铝

Unraveling the reaction mechanism of low dose Mn dopant in Ni(OH)_(2) supercapacitor electrode

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Journal of Energy Chemistry 2021年第10期30卷 497-506,I0013页

作者： Zhiguo Zhang hua huo Zhenjiang Yu Lizhi Xiang Bingxing Xie Chunyu Du Jiajun Wang Geping Yin Key Laboratory of Materials for New Energy Conversion and Storage(Ministry of Industry and Information Technology) School of Chemistry and Chemical EngineeringHarbin Institute of TechnologyHarbin 150001HeilongjiangChina

Mn doping is deemed as a promising strategy to improve the electrochemical performance of the a-Ni(OH)_(2)battery-type supercapacitor electrode.However,the internal structure evolution,the pathways and the dynamics of the proton/intercalated anion migration,as well as the functioning mechanism of Mn dopant to stabilize the layered structure during cycles remain unclear.Here,we unveil that irreversible oxidization of Mn^(3+)at the initial CV cycles,which will remain as Mn^(4+)in the NiO_(2)slabs after the first oxidization to effectively suppress the phase transformation fromα-Ni(OH)_(2)/γ-NiOOH toβ-Ni(OH)_(2)/β-NiOOH and further maintain the structural integrity of electrode.With a synergistic combination of theoretical calculations and various structural probes including XRD and^(2)H MAS solid state NMR,we decode the structure evolution and dynamics in the initial CV(cyclic voltammetry)cycles,including the absorption/desorption of hydrogen containing species,migration of intercalated anions/water molecules and the change of interlayer space.This present work elucidates a close relationship between doping chemistry and structural reliability,paving a novel way of reengineering supercapacitor electrode materials.

关键词： Reaction mechanism Structure evolution ^(2)H MAS NMR Layered double hydroxides Local environments