Fluorination of Li‐Rich Lithium‐Ion‐Battery Cathode Materials by Fluorine Gas: Chemistry, Characterization, and Electrochemical Performance in Half Cells

Breddemann Ulf; Erickson Evan M.; Davis Victoria; Schipper Florian; Ellwanger Mathias; Daub Michael; Hoffmann Anke; Erk Christoph; Markovsky Boris; Aurbach Doron; Krossing Ingo

摘要

Abstract > Mild fluorination of high‐energy nickel‐cobalt‐manganese (HE‐NCM) materials with low pressures of elementary fluorine gas (F <sub>2</sub> ) at room temperature was systematically studied. The fluorinated HE‐NCM samples were analysed by ion chromatography, inductively coupled plasma mass spectrometry, FT‐IR spectroscopy, powder X‐ray diffraction, magic angle spinning NMR spectroscopy, scanning electron microscopy, thermo‐gravimetric analysis, differential thermal analysis, electrochemical testing, and X‐ray photoelectron spectroscopy. The treatment of the cathode materials with low pressures (a few hundred mbar) of elementary fluorine gas at room temperature led to the elimination of the basic surface film (LiOH, Li <sub>2</sub> CO <sub>3</sub> , Li <sub>2</sub> O, etc.), and the resulting thin amorphous LiF film led to increased capacity and long‐term stability of the battery. Impedance built‐up was greatly reduced for these systems throughout cycling. Fluorination with F <sub>2</sub> only causes the formation of O?Me?F bonds (Me=Transition Metal), when treated with F <sub>2</sub> at higher pressures. If O?Me?F bonds are formed, it may be detrimental to the electrode surface film resistance and cycle stability of the electrodes. However, it may be that the LiF surface content, which can expand as long as the LiMeO <sub>2</sub> structure can be oxidized and Li + can be extracted, has become too large and thus detrimental. Considering the evolution of differential capacity plots and taking into account the thermodynamic driving force of the F <sub>2</sub> treatment, it is likely that the same activation processes that occur electrochemically in Li‐rich materials also occur chemically, when the material is exposed to F <sub>2</sub> . Differential capacity plots show enhanced Mn 4+ reduction peaks upon lithiation, when the material was exposed to F <sub>2</sub> , only possible after activation of the Li <sub>2</sub> MnO <sub>3</sub> phase. For this reason, we believe fluorination promotes to some extent an activation of this phase. </abstract> </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> <div class="translation abstracttxt"> <span class="zhankaihshouqi fivelineshidden" id="abstract"> <span>机译：</span><Abstract Type =“Main”XML：Lang =“en”> <标题类型=“main”>抽象</ title> > 高能量镍 - 钴 - 锰（HE-NCM）材料的温和氟化，基本氟气的压力低（F. <sub> 2 </ sub> ）在室温下系统地研究。通过离子色谱法，电感耦合等离子体质谱法，FT-IR光谱，粉末X射线衍射，扫描电子显微镜，热重分析，差动热分析，电化学检测，电化学检测和X射线光电子能谱。在室温下用低压力（几百毫巴）的阴极材料（几百毫巴）的含氟气体导致消除碱性表面膜（LioH，Li <sub> 2 </ sub> CO. <sub> 3 </ sub> ，李 <sub> 2 </ sub> o等），并得到的薄非晶Lif膜导致电池的容量和长期稳定性。在整个骑自行车的这些系统中，阻抗建立了很大减少。用F氟化 <sub> 2 </ sub> 仅导致o？M键（ME =过渡金属）的形成，当用F处理时 <sub> 2 </ sub> 在更高的压力下。如果o？me？f键形成，它可能对电极的电极表面膜电阻和循环稳定性可能是有害的。然而，它可能是LIF表面含量，可以扩展只要泥沼 <sub> 2 </ sub> 结构可以氧化和李 + </ sup> 可以提取，变得太大，因此有害。考虑到差分容量图的演变，考虑到F的热力学驱动力 <sub> 2 </ sub> 治疗，当材料暴露于f时，可能在富含富含量的材料中发生的相同激活过程也很可能会发生化学发生 <sub> 2 </ sub> 。差分容量绘图显示增强型Mn 4 + </ sup> 当材料暴露于F时，锂锂化后的峰值 <sub> 2 </ sub> ，只有在激活李后 <sub> 2 </ sub> mno. <sub> 3 </ sub> 阶段。因此，我们认为氟化在某种程度上促进了这种阶段的激活。 </ p> </摘要> </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> </div> <div class="record"> <h2 class="all_title" id="enpatent33" >著录项</h2> <ul> <li> <span class="lefttit">来源</span> <div style="width: 86%;vertical-align: text-top;display: inline-block;"> <a href='/journal-foreign-16042/'>《ChemElectroChem》</a> <b style="margin: 0 2px;">|</b><span>2019年第13期</span><b style="margin: 0 2px;">|</b><span>共13页</span> </div> </li> <li> <div class="author"> <span class="lefttit">作者</span> <p id="fAuthorthree" class="threelineshidden zhankaihshouqi"> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Breddemann Ulf&option=202" target="_blank" rel="nofollow">Breddemann Ulf;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Erickson Evan M.&option=202" target="_blank" rel="nofollow">Erickson Evan M.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Davis Victoria&option=202" target="_blank" rel="nofollow">Davis Victoria;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Schipper Florian&option=202" target="_blank" rel="nofollow">Schipper Florian;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Ellwanger Mathias&option=202" target="_blank" rel="nofollow">Ellwanger Mathias;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Daub Michael&option=202" target="_blank" rel="nofollow">Daub Michael;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Hoffmann Anke&option=202" target="_blank" rel="nofollow">Hoffmann Anke;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Erk Christoph&option=202" target="_blank" rel="nofollow">Erk Christoph;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Markovsky Boris&option=202" target="_blank" rel="nofollow">Markovsky Boris;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Aurbach Doron&option=202" target="_blank" rel="nofollow">Aurbach Doron;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Krossing Ingo&option=202" target="_blank" rel="nofollow">Krossing Ingo;</a> </p> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zkzz" style="display: none;">展开▼</span> </div> </li> <li> <div style="display: flex;"> <span class="lefttit">作者单位</span> <div style="position: relative;margin-left: 3px;max-width: 639px;"> <div class="threelineshidden zhankaihshouqi" id="fOrgthree"> <p>Institut für Anorganische und Analytische Chemie and Freiburger Materialforschungszentrum (FMF)Universit?t FreiburgAlbertstr. 21 79104 Freiburg Germany;</p> <p>Department of ChemistryBar-llan UniversityRamat-Gan 5290002 Israel;</p> <p>Institut für Anorganische und Analytische Chemie and Freiburger Materialforschungszentrum (FMF)Universit?t FreiburgAlbertstr. 21 79104 Freiburg Germany;</p> <p>Department of ChemistryBar-llan UniversityRamat-Gan 5290002 Israel;</p> <p>Institut für Anorganische und Analytische Chemie and Freiburger Materialforschungszentrum (FMF)Universit?t FreiburgAlbertstr. 21 79104 Freiburg Germany;</p> <p>Institut für Anorganische und Analytische Chemie and Freiburger Materialforschungszentrum (FMF)Universit?t FreiburgAlbertstr. 21 79104 Freiburg Germany;</p> <p>Institut für Anorganische und Analytische Chemie and Freiburger Materialforschungszentrum (FMF)Universit?t FreiburgAlbertstr. 21 79104 Freiburg Germany;</p> <p>BASF SECarl-Bosch-Str. 38 67056 Ludwigshafen Germany;</p> <p>Department of ChemistryBar-llan UniversityRamat-Gan 5290002 Israel;</p> <p>Department of ChemistryBar-llan UniversityRamat-Gan 5290002 Israel;</p> <p>Institut für Anorganische und Analytische Chemie and Freiburger Materialforschungszentrum (FMF)Universit?t FreiburgAlbertstr. 21 79104 Freiburg Germany;</p> </div> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zhdw" style="display: none;">展开▼</span> </div> </div> </li> <li > <span class="lefttit">收录信息</span> <span style="width: 86%;vertical-align: text-top;display: inline-block;"></span> </li> <li> <span class="lefttit">原文格式</span> <span>PDF</span> </li> <li> <span class="lefttit">正文语种</span> <span>eng</span> </li> <li> <span class="lefttit">中图分类</span> <span><a href="https://www.zhangqiaokeyan.com/clc/1186.html" title="物理化学（理论化学）、化学物理学">物理化学（理论化学）、化学物理学;</a></span> </li> <li class="antistop"> <span class="lefttit">关键词</span> <p style="width: 86%;vertical-align: text-top;"> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=lithium-ion batteries&option=203" rel="nofollow">lithium-ion batteries;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Li-rich cathode materials&option=203" rel="nofollow">Li-rich cathode materials;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=surface fluorination&option=203" rel="nofollow">surface fluorination;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=fluorine gas&option=203" rel="nofollow">fluorine gas;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=electrochemical testing&option=203" rel="nofollow">electrochemical testing;</a> </p> <div class="translation"> 机译：锂离子电池;富含量的阴极材料;表面氟化;氟气;电化学测试; </div> </li> </ul> </div> </div> <div class="literature cardcommon" id="literaturereference" style="display:none"> <div class="similarity "> <h3 class="all_title" id="enpatent111">引文网络</h3> <div class="referencetab clearfix"> <ul id="referencedaohang"> <li dataid="referenceul">参考文献</li> <li dataid="citationul">引证文献</li> <li dataid="commonreferenceul">共引文献</li> <li dataid="commoncitationul">同被引文献</li> <li dataid="tworeferenceul">二级参考文献</li> <li dataid="twocitationul">二级引证文献</li> </ul> </div> <div class="reference_details" id="referenceList"> <ul 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href="/patent-detail/06120109911293.html">一种改善富锂材料电化学性能的表面修饰方法、所得富锂材料及应用</a> <b>[P]</b> . <span> 中国专利： CN107437617A </span> <span> . 2017-12-05</span> </div> </li> <li> <div> <b>3. </b><a class="enjiyixqcontent" href="/patent-detail/06130414135731.html">METHOD OF MANUFACTURING FLUORINE COMPOUNDS AS A CATHODE MATERIAL FOR LITHIUM SECONDARY BATTERIES USING SOLID STATE REACTION AND A CATHODE AND A LITHIUM SECONDARY BATTERY COMPRISING THE CATHODE</a> <b>[P]</b> . <span> 外国专利：  KR101489779B1 </span> <span> . 2015-02-04</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：使用固态反应制造氟化合物作为锂二次电池的阴极材料的方法以及包括该阴极的阴极和锂二次电池 </span> </p> </li> <li> <div> <b>4. </b><a class="enjiyixqcontent" href="/patent-detail/06130416780453.html">METHOD OF MANUFACTURING FLUORINE COMPOUNDS AS A CATHODE MATERIAL FOR LITHIUM SECONDARY BATTERIES USING SOLID STATE REACTION AND A CATHODE AND A LITHIUM SECONDARY BATTERY COMPRISING THE CATHODE</a> <b>[P]</b> . <span> 外国专利：  KR20140094172A </span> <span> . 2014-07-30</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：使用固态反应制造氟化合物作为锂二次电池的阴极材料的方法以及包括该阴极的阴极和锂二次电池 </span> </p> </li> <li> <div> <b>5. </b><a class="enjiyixqcontent" href="/patent-detail/06130409701969.html">Cathode active material coated with fluorine-doped lithium metal manganese oxide and lithium-ion secondary battery comprising the same</a> <b>[P]</b> . <span> 外国专利：  US9660260B2 </span> <span> . 2017-05-23</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：涂有氟掺杂的锂金属锰氧化物的阴极活性材料和包括该阴极活性材料的锂离子二次电池 </span> </p> </li> </ul> </div> </div> </div> <div class="theme cardcommon" style="overflow: auto;display:none"> <h3 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