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近球形MoS2負極材料的強化水熱合成與電化學性能
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1.河南科技大學 材料科學與工程學院;2.珠海冠宇電池股份有限公司

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國家自然科學基金資助(項目號U1704152);河南省高等學校重點科研項目(20A430011);河南省高等學校青年骨干教師培養(yǎng)計劃(2019GGJS073);河南科技大學大學生研究訓練計劃(2022033)


Enhanced Hydrothermal Synthesis and Eletrochemical performance of Subsphaeroidal MoS2 used as Anode material for Lithium-ion BatteriesSS
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1.School of Material Science and Engineerign,Henan University of Science and Technology;2.Zhuhai CosMX Battery Co.

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    摘要:

    分別以鉬酸銨和硫脲為鉬源和硫源,在聚乙烯吡咯烷酮(PVP)軟模板作用下,采用強化水熱法在較短時間內制備出了近球形純MoS2粉體材料。通過X射線衍射(XRD)、鎢燈絲掃描電鏡(SEM)、場發(fā)射掃描電鏡(FESEM)、高分辨透射電鏡(HRTEM),X射線光電子能譜(XPS)等表征方法,研究了近球形純MoS2材料的微觀形貌、晶體結構、元素組成及表面價態(tài)。結果表明:所制備得到的MoS2材料為由片狀二硫化鉬所構成的球體,尺寸為150nm左右,經過500℃加熱處理2h后,微觀形貌不變。經過恒流充放電測試,其在500mA/g的電流密度下,加熱處理前的MoS2材料首次放電比容量高達874.7mAh/g,但存在較大的容量衰減,其循環(huán)充放電100次后容量保持率僅為53.3%,并且其首次充放電庫倫效率僅為68.88%,直到第47次充放電時才穩(wěn)定在100%;而經過500℃加熱處理2h后的MoS2材料充放電的容量損失較小,循環(huán)穩(wěn)定性增強,經過100次充放電后容量達571.3 mAh/g,容量保持率為83.2%,且?guī)靷愋室恢睘?00%穩(wěn)定不衰減。加熱處理后性能提升的原因一方面在于材料中殘留氧化鉬揮發(fā),材料內部出現(xiàn)部分空隙,從而增大了活性物質與電解液的接觸面積。另一方面加熱處理提高了材料的結晶性,可以穩(wěn)定MoS2的晶體結構,抑制嵌鋰-脫嵌過程中的體積膨脹問題。

    Abstract:

    Subsphaeroidal MoS2 anode powder material with good electrochemical performance for lithium-ion batteries (LIBs) were synthesized by enhanced hydro-thermal process (EHP) in relatively short reaction time. The ammonium molybdate, thiourea and polyvinyl pyrrolidone (PVP) were used as molybdenum source, sulfur source and soft mold surfactant, respectively. The crystal structure, morphology, element component and valencies of the as-prepared samples were characterized by XRD, SEM, FESEM, TEM, HRTEM and XPS. Galvanostatic charge-discharge, cyclic voltammetry and electrochemical impedance spectroscopy test was utilized to evaluate the electrochemical performance of the batteries assembled by the as prepared powder. The experimental results showed that the as-prepared powder was subsphaeroidal MoS2 particles with an average grain size of about 150nm. After annealing at 500℃ for 2h, there is no significant change in morphology. As anodes for LIBs, subsphaeroidal MoS2 without annealing delivered an relatively high initial discharge capacity of 874.7 mAh/g at a current density of 500 mA/g, which decays in the following cycles. The capacity retention rate after 100 cycles was only 53.3%. As a contrast, electrochemical properties were enhanced for the counterparts after annealing, which exhibited an ultimate (100 cycles) discharge capacity of 571.3 mAh/g and a capacity retention rate of 83.2%. The coulomb efficiency of samples without annealing for the first cycle was only 68.88% and elevated afterwards to reach 100% at the 47th cycle while it is 100% for the annealed specimens in the initial stage and without decay in the following cycles, which indicating an improvement of charge-discharge efficiency. The performance of the annealed specimens enhanced due to the following reasons. The residual molybdenum oxide in the material sublimates during annealing, and lead to some voids appear inside the material, which increase the contact area between the active substance and the electrolyte. Furthmore, the heating treatment improves the crystallinity of the specimens, which can stabilize the crystal structure of MoS2, and inhibit the volume expansion in the discharge/charge process.

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吳楊,張亮亮,王偉,范東昇,楊慎慎,白云豪,李繼文,劉偉.近球形MoS2負極材料的強化水熱合成與電化學性能[J].稀有金屬材料與工程,2023,52(8):2893~2900.[Wu Yang, Zhang Liangliang, Wang Wei, Fan Donghseng, Yang Shenshen, Bai Yunhao, Li Jiwen, Liu Wei. Enhanced Hydrothermal Synthesis and Eletrochemical performance of Subsphaeroidal MoS2 used as Anode material for Lithium-ion BatteriesSS[J]. Rare Metal Materials and Engineering,2023,52(8):2893~2900.]
DOI:10.12442/j. issn.1002-185X.20220662

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  • 收稿日期:2022-08-22
  • 最后修改日期:2022-10-13
  • 錄用日期:2022-10-21
  • 在線發(fā)布日期: 2023-08-28
  • 出版日期: 2023-08-24