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Article(id=1241081040383562649, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.04.003, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1707062400000, receivedDateStr=2024-02-05, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773826378197, onlineDateStr=2026-03-18, pubDate=1722441600000, pubDateStr=2024-08-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773826378197, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773826378197, creator=13701087609, updateTime=1773826378197, updator=13701087609, issue=Issue{id=1241081025531540408, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='4', pageStart='1', pageEnd='258', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773826374657, creator=13701087609, updateTime=1773827517159, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241085817590960730, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241085817590960731, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=13, endPage=17, ext={EN=ArticleExt(id=1241081040865907655, articleId=1241081040383562649, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Electrochemiacal Performance of NaNi0.5Mn0.5O2 Material Synthesized by Different Methods, columnId=1241081026567533498, journalTitle=Mining and Metallurgical Engineering, columnName=SPECIAL ISSUE: BATTERY MATERIALS, runingTitle=null, highlight=null, articleAbstract=

A cathode material (NaNi0.5Mn0.5O2) for sodium-ion batteries was synthesized by adopting solid-state, co-precipitation and sol-gel methods, and the effects of synthesis methods on crystal structure, microscopic morphology and electrochemical performance of the cathode material were also explored. The results show that the materials synthesized respectively by those three methods all have O3-type structure, but exhibit different morphology. The cathode material synthesized by solid-state method has a special layered structure, which is conducive to sodium ion de-intercalation. The cathode materials synthesized by solid-state, co-precipitation and sol-gel methods, respectively, deliver an initial specific discharge capacity of 96.1 mAh/g, 92.8 mAh/g and 92.3 mAh/g at 0.1C, with retention rate of 64.3%, 46.5% and 36.5% respectively after 100 cycles at 0.5C. It is concluded that the solid-state synthesis is an appropriate method.

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分别采用固相法、共沉淀法和溶胶-凝胶法合成了钠离子电池正极材料NaNi0.5Mn0.5O2，探究了合成方法对正极材料晶体结构、微观形貌以及电化学性能的影响。结果表明：3种方法合成的材料均表现为O3型结构；不同方法制备的材料形貌各不相同，其中固相法合成的材料颗粒呈现出特殊的层状结构，有利于钠离子的脱嵌；固相法、共沉淀法和溶胶凝胶法合成的材料在0.1C下的首次放电比容量分别为96.1 mAh/g、92.8 mAh/g和92.3 mAh/g，0.5C下循环100次后的容量保持率分别为64.3%、46.5%和36.5%。固相法是适宜的制备方法。

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陈庆荣（1986—），男，海南万宁人，讲师，主要研究方向海洋船舶动力电池材料、新能源材料电催化等。E-mail：
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史世和（1996—），男，山西临汾人，硕士研究生，主要方向钠离子电池正极材料的研究。E-mail：

, authorsList=史世和, 白世伟, 杨波, 吴千惠, 陈庆荣, 廖芝建, 钟胜奎, 刘洁群)}, authors=[Author(id=1241081045819380080, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081040383562649, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=shihe0903@163.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1241081045987152261, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081040383562649, authorId=1241081045819380080, language=EN, stringName=Shihe SHI, firstName=Shihe, middleName=null, lastName=SHI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, 2, address=1.College of Marine Science and Technology, Hainan Tropical Ocean University, Sanya 572022, Hainan, China
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史世和（1996—），男，山西临汾人，硕士研究生，主要方向钠离子电池正极材料的研究。E-mail：

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史世和（1996—），男，山西临汾人，硕士研究生，主要方向钠离子电池正极材料的研究。E-mail：

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实验试剂

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试剂纯度生产厂家
无水碳酸钠分析纯阿拉丁试剂有限公司
二氧化锰分析纯上海麦克林生化科技股份有限公司
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不同合成方法制备NaNi0.5Mn0.5O2及其电化学性能研究
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史世和 1, 2 , 白世伟 1, 2 , 杨波 1, 2 , 吴千惠 1, 2 , 陈庆荣 1, 2 , 廖芝建 1, 2 , 钟胜奎 1, 2 , 刘洁群 1, 2
矿冶工程杂志 | 电池材料专题 2024,44(4): 13-17
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矿冶工程杂志 | 电池材料专题 2024, 44(4): 13-17
不同合成方法制备NaNi0.5Mn0.5O2及其电化学性能研究
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史世和1, 2 , 白世伟1, 2, 杨波1, 2, 吴千惠1, 2, 陈庆荣1, 2 , 廖芝建1, 2, 钟胜奎1, 2, 刘洁群1, 2
作者信息
  • 1.海南热带海洋学院 海洋科学技术学院，海南 三亚 572022
  • 2.崖州湾创新研究院，海南 三亚 572022

    • 史世和（1996—），男，山西临汾人，硕士研究生，主要方向钠离子电池正极材料的研究。E-mail：

通讯作者:

陈庆荣（1986—），男，海南万宁人，讲师，主要研究方向海洋船舶动力电池材料、新能源材料电催化等。E-mail：
Electrochemiacal Performance of NaNi0.5Mn0.5O2 Material Synthesized by Different Methods
Shihe SHI1, 2 , Shiwei BAI1, 2, Bo YANG1, 2, Qianhui WU1, 2, Qingrong CHEN1, 2 , Zhijian LIAO1, 2, Shengkui ZHONG1, 2, Jiequn LIU1, 2
Affiliations
  • 1.College of Marine Science and Technology, Hainan Tropical Ocean University, Sanya 572022, Hainan, China
  • 2.Yazhou Bay Innovation Research Institute, Sanya 572022, Hainan, China
出版时间: 2024-08-01 doi: 10.3969/j.issn.0253-6099.2024.04.003
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摘要
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分别采用固相法、共沉淀法和溶胶-凝胶法合成了钠离子电池正极材料NaNi0.5Mn0.5O2，探究了合成方法对正极材料晶体结构、微观形貌以及电化学性能的影响。结果表明：3种方法合成的材料均表现为O3型结构；不同方法制备的材料形貌各不相同，其中固相法合成的材料颗粒呈现出特殊的层状结构，有利于钠离子的脱嵌；固相法、共沉淀法和溶胶凝胶法合成的材料在0.1C下的首次放电比容量分别为96.1 mAh/g、92.8 mAh/g和92.3 mAh/g，0.5C下循环100次后的容量保持率分别为64.3%、46.5%和36.5%。固相法是适宜的制备方法。

钠离子电池  /  正极材料  /  NaNi0.5Mn0.5O2  /  固相法  /  共沉淀法  /  溶胶-凝胶法

A cathode material (NaNi0.5Mn0.5O2) for sodium-ion batteries was synthesized by adopting solid-state, co-precipitation and sol-gel methods, and the effects of synthesis methods on crystal structure, microscopic morphology and electrochemical performance of the cathode material were also explored. The results show that the materials synthesized respectively by those three methods all have O3-type structure, but exhibit different morphology. The cathode material synthesized by solid-state method has a special layered structure, which is conducive to sodium ion de-intercalation. The cathode materials synthesized by solid-state, co-precipitation and sol-gel methods, respectively, deliver an initial specific discharge capacity of 96.1 mAh/g, 92.8 mAh/g and 92.3 mAh/g at 0.1C, with retention rate of 64.3%, 46.5% and 36.5% respectively after 100 cycles at 0.5C. It is concluded that the solid-state synthesis is an appropriate method.

sodium-ion battery  /  cathode material  /  NaNi0.5Mn0.5O2  /  solid-state synthesis  /  co-precipitation synthesis  /  sol-gel synthesis
史世和, 白世伟, 杨波, 吴千惠, 陈庆荣, 廖芝建, 钟胜奎, 刘洁群. 不同合成方法制备NaNi0.5Mn0.5O2及其电化学性能研究. 矿冶工程杂志, 2024 , 44 (4) : 13 -17 . DOI: 10.3969/j.issn.0253-6099.2024.04.003
Shihe SHI, Shiwei BAI, Bo YANG, Qianhui WU, Qingrong CHEN, Zhijian LIAO, Shengkui ZHONG, Jiequn LIU. Electrochemiacal Performance of NaNi0.5Mn0.5O2 Material Synthesized by Different Methods[J]. Mining and Metallurgical Engineering, 2024 , 44 (4) : 13 -17 . DOI: 10.3969/j.issn.0253-6099.2024.04.003
正文
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化石燃料的大量开采和使用不仅造成了能源枯竭，而且严重污染环境，因此，绿色、可持续发展的能源得到大力开发[1-3]。为了有效储存和使用这些新能源，必须开发大规模储能系统[4]。在绿色储能方面，锂离子电池得到广泛应用，但锂资源短缺以及成本高，其可持续发展面临考验[5]。因此，开发资源丰富且成本较低的新型二次储能电池已迫在眉睫[6-8]。与锂离子电池相比，钠离子电池具有钠金属资源丰富、能量密度高且钠不与铝反应形成合金[9]、成本低等特点，已成为锂离子电池的有力替代者。
近年来，钠离子电池正极材料已得到广泛研究，如层状氧化物、聚阴离子型化合物和普鲁士蓝及其类似物[10-13]。其中层状氧化物（NaTMO2）因电化学活性高、理论比容量高和易于合成等优点受到广泛关注[14]。在层状氧化物中，NaNi0.5Mn0.5O2材料具有较高的氧化还原电位，且电位受材料嵌钠量影响较小[15]，被认为是具有前景的正极材料候选物。然而NaNi0.5Mn0.5O2材料存在相变及环境敏感性等问题，不利于电池长期稳定循环[16-17]。目前，层状氧化物的合成方法趋于多样化，但多以固相法、共沉淀法和溶胶-凝胶法为主[18-24]，3种合成方法都操作简单、成本低。在合成效果方面，材料形貌呈现多样性，优化形貌可缓和Na+脱嵌过程带来的体积应变，改善材料的循环性能[25]。本文采用固相法、共沉淀法和溶胶-凝胶法制备钠离子电池正极材料NaNi0.5Mn0.5O2，观察不同合成方法制备的材料晶体结构与微观形貌，测试其电化学性能。
1 实验
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1.1 实验试剂
实验所用试剂见表1。
1.2 材料制备
固相法制备NaNi0.5Mn0.5O2：按照n（Na）∶n（Mn）∶n（Ni）=2∶1∶1的计量比称取NaCO3、MnO2、Ni（OH）2，将材料混合研磨直至均匀，将混合均匀的材料放入管式炉中，在空气气氛下以5 ℃/min升温速度升温至850 ℃，保温12 h，随炉冷却后，快速研磨并置于手套箱中保存。样品标记为SS。
共沉淀法制备NaNi0.5Mn0.5O2：分别称取1 mol的硝酸镍、硝酸锰置于烧杯中，加入150 mL去离子水搅拌2 h，制得金属离子溶液；随后将溶解的碳酸钠水溶液（碳酸钠加入量2 mol，同时过量5%，确保锰离子、镍离子完全沉淀）缓慢倒入上述金属离子溶液中，持续搅拌3 h后进行离心、冷冻干燥得到碳酸盐沉淀；最后按照化学计量比将碳酸钠与碳酸盐沉淀充分混合研磨，将混合均匀的材料放入管式炉中，在空气气氛下以5 ℃/min升温速度升温至850 ℃，保温12 h，随炉冷却后，快速研磨并置于手套箱中保存。样品标记为CP。
溶胶-凝胶法制备NaNi0.5Mn0.5O2：按照n（Na）∶n（Mn）∶n（Ni）=2∶1∶1的计量比称取醋酸钠、醋酸镍和醋酸锰置于烧杯中，加入去离子水搅拌溶解，之后滴加一定浓度的柠檬酸水溶液并在水浴中搅拌6 h形成凝胶，干燥后进行研磨并置于管式炉中以5 ℃/min升温速度升温至850 ℃，保温12 h，随炉冷却后，快速研磨并置于手套箱中保存。样品标记为SG。
1.3 分析与表征
采用XRD-600型X射线衍射仪（XRD，日本Rigaku公司，Cu-Kα射线，λ=0.154 06 nm）表征材料的物相；采用JSM-7610F PULS型扫描电子显微镜（SEM）观察材料的微观形貌；采用ESCALAB250Xi型X射线光电子能谱仪测定过渡金属元素价态；采用新威CT-ZWJ-4S-T-1U型测试系统在恒温25 ℃下测试电化学性能；采用上海辰华CHI660C电化学工作站测试循环伏安曲线和交流阻抗。
1.4 电池组装与测试
按质量比8∶1∶1称取活性物质、科琴黑、聚偏二氟乙烯（PVDF）黏合剂，混合均匀，加入适量N-甲基-2-吡咯烷酮溶剂形成浆液，使用刮刀均匀涂覆到铝箔，在真空干燥箱中干燥12 h，并制成正极片（直径12 mm的圆片）。在充满氩气的手套箱中将正极片、金属钠片、玻璃纤维隔膜、电解液（NaClO4/PC）、泡沫镍按顺序组装扣式电池，将组装好的扣式电池静置12 h后进行测试。
2 实验结果与讨论
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2.1 结构与形貌分析
图1为不同合成方法制备的NaNi0.5Mn0.5O2样品XRD图谱。所有合成样品都表现出相似的衍射峰，衍射峰都与标准卡片（PDF#54-0887）一致，位于16.53°、33.43°、36.58°、37.05°和41.94°的衍射峰分别对应（003）、（006）、（101）、（012）和（101）晶面，表明所有合成样品均表现为O3型结构，空间群为R3m[26]。固相法合成的样品衍射峰锐利且强度较高，说明样品的结晶性良好。溶胶-凝胶法合成的样品在43°左右存在NiO杂质，原因是Ni在O3相中的溶解度有限，存在少量NiO[27]。
图2为不同方法合成的NaNi0.5Mn0.5O2样品SEM图。从图2可见，样品SS由不规则片状颗粒组成，表面光滑且呈特殊的层状结构，有利于提高充放电过程中钠离子的脱嵌速率，从而提高材料的电化学性能。样品CP呈球状，球体结构可增大材料表面与电解液的接触面积，但材料容易被电解液侵蚀，导致材料表面结构发生变化。样品SG有明显的部分团聚现象，这会导致充放电过程中离子传输阻力增大，从而恶化材料的电化学性能。
利用XPS测试了固相法合成的NaNi0.5Mn0.5O2样品中锰和镍元素的价态，结果如图3所示。位于642.2 eV和653.7 eV处的结合能峰分别对应于Mn2p3/2和Mn2p1/2，表明锰以+4价形式存在[28]。Ni2p的结合能位于854.3 eV和872.3 eV，对应于Ni2p3/2和Ni2p1/2，证明Ni2+的存在[29]，而在860.3 eV、864.9 eV和879.3 eV处的结合能峰属于卫星峰。
2.2 电化学性能分析
图4为不同合成方法制备的NaNi0.5Mn0.5O2样品在不同倍率下的首次充放电曲线图。固相法、共沉淀法和溶胶-凝胶法合成的材料在0.1C倍率下的首次充放电比容量分别为96.1 mAh/g、92.8 mAh/g和92.3 mAh/g，且固相法合成的材料在其他倍率下的首次放电比容量都优于其他2种方法。另外，3种方法合成的样品充放电曲线包含多个充放电平台和斜坡，反映了Na+/空位有序以及由过渡金属层滑动引起的多重相变[30]。
不同方法合成的NaNi0.5Mn0.5O2样品倍率性能和循环性能见图5。由图5（a）可见，固相法合成的材料表现出较优异的倍率性能，材料在0.2C、0.5C、1C、2C和5C倍率下的放电比容量分别为86.7 mAh/g、75.2 mAh/g、63.4 mAh/g、51.1 mAh/g和35.1 mAh/g，当电流密度回到0.1C时，放电比容量仍能达到88.5 mAh/g，表明材料具有良好的电化学可逆性和结构稳定性。由图5（b）可见，经过100次循环周期后，固相法、共沉淀法、溶胶-凝胶法制备的材料放电比容量分别为48.2 mAh/g、32.9 mAh/g、17.7 mAh/g，对应的容量保持率分别为64.3%、46.5%、35.5%。固相法合成的材料拥有更高的比容量和更好的循环性能，其原因在于材料表面光滑且呈特殊的层状结构，有利于加快充放电过程中钠离子的迁移速率，从而提高材料的电化学性能。
不同方法合成的NaNi0.5Mn0.5O2样品的循环伏安（CV）曲线和交流阻抗图见图6。其中图6（a）～（c）的操作条件为：扫速0.1 mV/s、扫描圈数3圈。3种方法合成的材料表现出相似的氧化还原峰，在2.49 V/2.85 V、3.20 V/3.26 V、3.45 V/3.51 V、3.58 V/3.69 V左右分别出现了成对的氧化还原峰，曲线中3.0 V电压以上出现的氧化还原峰对由Ni2+/Ni3+和Ni3+/Ni4+以及钠层Na+/空位有序形成；低于3.0 V电压所表现出来的氧化还原峰对归于Mn3+/Mn4+可逆的氧化还原反应[31]。对比3种方法合成材料的CV曲线，固相法合成的材料CV曲线重叠性优于其他2种方法，说明其具有更好的电化学可逆性且电极结构较稳定。
由图6（d）可见，交流阻抗图谱由高频区的半圆（对应于电荷转移电阻Rct）及低频区倾斜直线（Zw，与Na+扩散有关）组成[32]，固相法制备的材料Rct较小，共沉淀法与溶胶-凝胶法的Rct较大，表明固相法合成的材料钠离子嵌入/嵌出动力学明显优于其他2种方法。
3 结论
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1）通过固相法、共沉淀法和溶胶-凝胶法制备了NaNi0.5Mn0.5O2正极材料，3种合成方法制备的材料均表现为O3型结构。固相法合成的材料呈层状结构，有利于钠离子的脱嵌；共沉淀法合成的材料呈球状，但材料容易被电解液侵蚀，导致材料表面结构发生变化；溶胶-凝胶法合成的材料有明显的部分团聚现象，这会导致充放电过程中离子传输阻力增大。
2）固相法、共沉淀法和溶胶-凝胶法合成的材料在0.1C下的首次放电比容量分别为96.1 mAh/g、92.8 mAh/g和92.3 mAh/g，0.5C下循环100次后的容量保持率分别为64.3%、46.5%和36.5%。
3）固相法合成的材料拥有较高的循环可逆性和较低的电荷转移电阻，展现出良好的电化学性能，因此，固相法是适宜的合成方法。
基金
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  • 国家自然科学基金(52164029)
  • 国家自然科学基金(52074099)
  • 海南省自然科学基金(821MS0782)
  • 海南省自然科学基金(221MS048)
  • 海南省自然科学基金(221RC585)
  • 海南省自然科学基金(SQ2022GXJS0018)
  • 海南省自然科学基金(221RC1072)
  • 海南热带海洋学院引进人才科研启动资助项目(RHDRC202002)
文献
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2024年第44卷第4期
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doi: 10.3969/j.issn.0253-6099.2024.04.003
  • 接收时间：2024-02-05
  • 首发时间：2026-03-18
  • 出版时间：2024-08-01
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  • 收稿日期：2024-02-05
基金
国家自然科学基金(52164029)
国家自然科学基金(52074099)
海南省自然科学基金(821MS0782)
海南省自然科学基金(221MS048)
海南省自然科学基金(221RC585)
海南省自然科学基金(SQ2022GXJS0018)
海南省自然科学基金(221RC1072)
海南热带海洋学院引进人才科研启动资助项目(RHDRC202002)
作者信息
    1.海南热带海洋学院 海洋科学技术学院，海南 三亚 572022
    2.崖州湾创新研究院，海南 三亚 572022

通讯作者:

陈庆荣（1986—），男，海南万宁人，讲师，主要研究方向海洋船舶动力电池材料、新能源材料电催化等。E-mail：
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https://castjournals.cast.org.cn/joweb/kygczz/CN/10.3969/j.issn.0253-6099.2024.04.003
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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