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Article(id=1241416389450330645, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241416382559081210, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2025.03.033, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1734451200000, receivedDateStr=2024-12-18, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773906331645, onlineDateStr=2026-03-19, pubDate=1748707200000, pubDateStr=2025-06-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773906331645, onlineIssueDateStr=2026-03-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773906331645, creator=13701087609, updateTime=1773906331645, updator=13701087609, issue=Issue{id=1241416382559081210, tenantId=1146029695717560320, journalId=1235980550691926019, year='2025', volume='45', issue='3', pageStart='1', pageEnd='223', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773906330003, creator=13701087609, updateTime=1773908015401, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241423451685179940, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241416382559081210, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241423451685179941, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241416382559081210, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=198, endPage=202, ext={EN=ArticleExt(id=1241416393367810901, articleId=1241416389450330645, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Effect of Carbon Coating Structure on Performance of SiO-Based Battery Material, columnId=1236276108207902848, journalTitle=Mining and Metallurgical Engineering, columnName=MATERIALS, runingTitle=null, highlight=null, articleAbstract=

Three types of carbon-coated silicon monoxide (SiO) materials were synthesized with different carbon sources and coating methods, and then their physicochemical properties and electrochemical performance were analyzed. A uniform and dense carbon film on the surface of material can be obtained by using a gaseous carbon source for vapor-phase coating. While a solid carbon source for liquid-phase coating leads to an uneven and loose film on the surface. With a combination of these two coating methods, the obtained carbon film on the surface can exhibit characteristics of two methods, including inner porous layer and outer dense layer. Electrochemical testing shows that with the combined coating method, the synthesized carbon-coated material delivers a specific capacity of 1 688.45 mAh/g, presenting the first charge-discharge efficiency of 76.13% and the capacity retention rate of 79.6% after 100 charge-discharge cycles.

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采用不同碳源和不同包覆方式制备了3种碳包覆氧化亚硅材料，对其进行物化性能和电化学性能结果分析。采用气相碳源进行气相包覆时材料表面的碳层均匀致密，采用固相碳源进行液相包覆时材料表面的碳层疏松且不均匀，采用两种方式组合包覆时材料表面的碳层兼备两种方式的特点，内层疏松、外层致密。电性能测试结果表明组合包覆的材料比容量为1 688.45 mAh/g，首次效率为76.13%，循环100次后容量保持率为79.6%。

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李中良（1988—），男，河南许昌人，硕士，工程师，主要研究方向为新能源材料及器件的研发和检测。E-mail：
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陈功哲（1989—），男，湖南长沙人，硕士，工程师，主要研究方向为新能源材料的研发和工艺设计。E-mail：

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陈功哲（1989—），男，湖南长沙人，硕士，工程师，主要研究方向为新能源材料的研发和工艺设计。E-mail：

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陈功哲（1989—），男，湖南长沙人，硕士，工程师，主要研究方向为新能源材料的研发和工艺设计。E-mail：

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（a）氧化亚硅原料；（b）1#样品；（c）2#样品；（d）3#样品

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（a）1#样品；（b）2#样品；（c）2#样品边缘区域；（d）3#样品

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Particle size parameters of raw materials and samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称d10/μmd50/μmd90/μmdmax/μm
氧化亚硅原料3.756.3010.3515.70
1#样品4.027.0411.8618.25
2#样品4.107.2312.4618.22
3#样品4.047.1212.4018.29
), ArticleFig(id=1241422265422762967, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241416389450330645, language=CN, label=表1, caption=

氧化亚硅原料和3种样品的粒径参数

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称d10/μmd50/μmd90/μmdmax/μm
氧化亚硅原料3.756.3010.3515.70
1#样品4.027.0411.8618.25
2#样品4.107.2312.4618.22
3#样品4.047.1212.4018.29
), ArticleFig(id=1241422265565369312, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241416389450330645, language=EN, label=Table 2, caption=

Tap density and specific surface area of samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称振实密度/（g·cm-3）比表面积/（m2·g-1）
1#样品0.991.220
2#样品0.973.155
3#样品0.991.318
), ArticleFig(id=1241422265926079471, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241416389450330645, language=CN, label=表2, caption=

3种样品的振实密度和比表面积

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称振实密度/（g·cm-3）比表面积/（m2·g-1）
1#样品0.991.220
2#样品0.973.155
3#样品0.991.318
), ArticleFig(id=1241422266081268732, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241416389450330645, language=EN, label=Table 3, caption=

Carbon content of samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称碳含量/%
1#样品3.98
2#样品4.01
3#样品4.09
), ArticleFig(id=1241422266207096837, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241416389450330645, language=CN, label=表3, caption=

3种样品的实际碳含量测试结果

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样品名称碳含量/%
1#样品3.98
2#样品4.01
3#样品4.09
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表面包覆碳层结构对硅氧电池材料性能的影响
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陈功哲 1, 2 , 李中良 3
矿冶工程杂志 | 材料 2025,45(3): 198-202
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矿冶工程杂志 | 材料 2025, 45(3): 198-202
表面包覆碳层结构对硅氧电池材料性能的影响
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陈功哲1, 2 , 李中良3
作者信息
  • 1.中机国际工程设计研究院有限责任公司，湖南　长沙　410021
  • 2.锂离子电池及材料智能制造先进技术湖南省工程研究中心，湖南　长沙　410021
  • 3.长沙矿冶院检测技术有限责任公司，湖南　长沙　410012

    • 陈功哲（1989—），男，湖南长沙人，硕士，工程师，主要研究方向为新能源材料的研发和工艺设计。E-mail：

通讯作者:

李中良（1988—），男，河南许昌人，硕士，工程师，主要研究方向为新能源材料及器件的研发和检测。E-mail：
Effect of Carbon Coating Structure on Performance of SiO-Based Battery Material
Gongzhe CHEN1, 2 , Zhongliang LI3
Affiliations
  • 1.China Machinery International Engineering Design & Research Institute Co., Ltd., Changsha 410021, Hunan, China
  • 2.Advanced Technology of Intelligent Manufacturing of Lithium-Ion Batteries and Materials Hunan Engineering Research Center, Changsha 410021, Hunan, China
  • 3.Testing Technology of Changsha Research Institute of Mining and Metallurgy Co., Ltd., Changsha 410012, Hunan, China
出版时间: 2025-06-01 doi: 10.3969/j.issn.0253-6099.2025.03.033
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摘要
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采用不同碳源和不同包覆方式制备了3种碳包覆氧化亚硅材料，对其进行物化性能和电化学性能结果分析。采用气相碳源进行气相包覆时材料表面的碳层均匀致密，采用固相碳源进行液相包覆时材料表面的碳层疏松且不均匀，采用两种方式组合包覆时材料表面的碳层兼备两种方式的特点，内层疏松、外层致密。电性能测试结果表明组合包覆的材料比容量为1 688.45 mAh/g，首次效率为76.13%，循环100次后容量保持率为79.6%。

硅氧电池  /  负极材料  /  氧化亚硅  /  碳包覆  /  气相包覆  /  液相包覆  /  碳层结构  /  表面包覆

Three types of carbon-coated silicon monoxide (SiO) materials were synthesized with different carbon sources and coating methods, and then their physicochemical properties and electrochemical performance were analyzed. A uniform and dense carbon film on the surface of material can be obtained by using a gaseous carbon source for vapor-phase coating. While a solid carbon source for liquid-phase coating leads to an uneven and loose film on the surface. With a combination of these two coating methods, the obtained carbon film on the surface can exhibit characteristics of two methods, including inner porous layer and outer dense layer. Electrochemical testing shows that with the combined coating method, the synthesized carbon-coated material delivers a specific capacity of 1 688.45 mAh/g, presenting the first charge-discharge efficiency of 76.13% and the capacity retention rate of 79.6% after 100 charge-discharge cycles.

SiO-based battery material  /  anode material  /  silicon monoxide  /  carbon coating  /  vapor-phase coating  /  liquid-phase coating  /  carbon coating structure  /  surface coating
陈功哲, 李中良. 表面包覆碳层结构对硅氧电池材料性能的影响. 矿冶工程杂志, 2025 , 45 (3) : 198 -202 . DOI: 10.3969/j.issn.0253-6099.2025.03.033
Gongzhe CHEN, Zhongliang LI. Effect of Carbon Coating Structure on Performance of SiO-Based Battery Material[J]. Mining and Metallurgical Engineering, 2025 , 45 (3) : 198 -202 . DOI: 10.3969/j.issn.0253-6099.2025.03.033
正文
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硅氧电池材料是以氧化亚硅为主的负极材料，氧化亚硅（SiOx，0<x<2）是一种无机化合物，属于Si的不完全氧化物。氧化亚硅负极理论比容量（2 600 mAh/g）远大于石墨负极的理论比容量（372 mAh/g），是极具应用前景的下一代锂离子电池负极材料[1-2]。但氧化亚硅固有的低电导率和较低的首次库仑效率（ICE）导致其倍率性能下降和容量衰减，阻碍了其在锂离子电池中的实际应用[3-4]。对此研究者尝试了很多改性策略[5-7]，其中表面包覆改性是有效手段之一。碳包覆改性的碳层能够缓冲硅材料体积膨胀产生的应力，提高材料稳定性，并且保证表面SEI膜的稳定存在[8-10]。碳材料具备优良的导电性，可以提升材料的导电性，碳层能够为锂离子和电解质提供快速转运通道，并且电化学稳定，可以使氧化亚硅保持相对独立，保护氧化亚硅不受电解液的影响[11]。
在氧化亚硅碳包覆过程中，碳源会影响碳层结构[12-13]，包覆方式会影响碳层分布，碳层结构和分布直接影响硅氧材料的电性能。本文通过研究不同碳源包覆对碳层结构的影响以及不同包覆方式对碳层分布的影响，以期找到一种较佳的方式，制备出电化学性能优异的硅氧负极材料。
1　实验
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1.1　实验方法
将块状氧化亚硅（自制，采用真空沉积法制备，硅含量63.51%）通过气流破碎机进行破碎分级，筛分后得到粒径d50=8 μm的粉体。碳源采用固相有机碳PAM（聚丙烯酰胺，分子量大于50 000，分析纯）和气相碳源乙烯气体（瓶装气体，纯度99.99%），包覆过程中的保护气体采用氮气（瓶装气体，纯度99.99%）。其中固相碳源采用液相包覆方式，气相碳源采用化学气相沉积（CVD）包覆方式。
液相包覆方式：将PAM按照比例加入去离子水中，采用高速分散机（西丽研磨，实验分散机，XL-JSF550）搅拌分散，制备成2%的PAM水溶液；把氧化亚硅按照比例加入PAM水溶液中，利用高速分散机分散均匀后，形成稳定的浆料，此时PAM均匀黏附在氧化亚硅表面；采用喷雾干燥设备进行喷雾干燥造粒，喷雾后的粉体放入气氛炉中进行碳化，PAM在高温下碳化，氢、氧反应生成水被脱去，剩下碳均匀包覆在材料表面，得到液相包覆材料。
CVD包覆方式：将氧化亚硅粉体放入CVD炉（科源窑炉，KY-R-SJQC1）中，在氮气保护下加热到700 ℃后通入乙烯气体，乙烯在高温下裂解，生成碳和氢气，碳均匀沉积在材料表面，形成包覆层，通过控制通入乙烯气体的流量和时间来控制碳包覆量，包覆完成后在保护气氛下冷却，得到气相包覆材料。
1.2　材料制备
1#样品采用CVD包覆方式，碳含量4%；2#样品采用液相包覆方式，碳含量4%；3#样品先采用液相包覆方式再采用CVD包覆方式，液相包覆碳含量2%，气相包覆碳含量2%，总碳含量4%。
1.3　材料表征
采用X-射线衍射仪（XRD，D8 ADVANCE型）分析晶体结构；采用场发射扫描电子显微镜（SEM，JSM-7900F型）分析材料表面形貌；采用场发射透射电子显微镜（TEM，FEI Talos F200i型）分析包覆层厚度；采用红外碳硫仪（力可CS844型）测试材料碳含量；采用比表面积与孔径分析仪（理化联科iPro 400型）分析材料比表面积；采用激光粒度仪（MASTERSIZER-3000型）分析材料粒径分布。
1.4　电化学性能测试
按照样品∶导电剂∶黏结剂=85∶10∶5（质量比）分别称取1#、2#、3#样品，加入适量去离子水调成均匀浆料，然后涂覆至铜箔上。干燥后冲切成Φ16 mm的圆片，在氩气环境手套箱内，以金属锂片为对电极，采用20 μm厚的PE隔膜，电解液为1 mol/L LiPF6溶于EC∶DEC∶EMC体积比1∶1∶1的溶剂中，组装成CR2430型号扣式电池，用LAND测试系统测试其充放电性能和首次充放电效率，充放电制度为0.1C放电至0.01 V，然后依次使用0.09C、0.08C、0.07C、0.06C、0.05C、0.04C、0.03C、0.02C、0.01C的电流放电至0.005 V，静置20 min后0.1C恒流充电至1.5 V，其中充电容量为材料的容量，充电容量与放电容量的比值为材料的首次效率。
电池的循环性能测试方法为：电池首次充放电后，再以测试充放电性能和首次效率的工步循环2圈后，以0.1C恒流充放制度进行充放电循环，电压区间为0.005～1.5 V。
2　结果与讨论
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2.1　材料物理性能表征
图1为3种样品的XRD图谱。从图1可见，3种样品的XRD图谱基本相同，在28.3°（111）、47.2°（220）、58.9°（311）3个位置均没有硅特征峰出现[10]，表明材料未发生歧化。氧化亚硅发生歧化需要在800 ℃以上[14]，同时包覆过程中，碳材料的裂解均是吸热反应，会降低硅氧材料的温度，从而减少歧化反应发生的可能。
表1是氧化亚硅原料和3种样品的粒径参数。从表1可见，包覆材料和原材料的粒径区别很小，整体粒径依然是正态分布，说明生成的游离碳球量很少，碳包覆层均匀分布在材料表面，并且厚度有限，不影响材料粒径。
表2为3种样品的振实密度和比表面积。从表2可见，3种样品振实密度差异不大，但比表面积有明显区别，1#样品比表面积最低，说明气相沉积的碳在硅氧表面形成了致密均匀的包覆层。2#样品比表面积高，因为PAM属于高分子链状，在碳化过程中形成链状碳，相对而言较为疏松[15]。3#样品包覆了两层碳，内部为链状碳，表面为致密的气相碳，所以比表面积接近1#样品的比表面积，而内部有疏松的链状碳，使得3#样品比表面积比1#样品的比表面积高一点。
2.2　材料碳层分析
图2为氧化亚硅原料和3种样品的SEM图。从图2可以看出，材料的粒径均匀，包覆前后的材料粒径基本相同，未见到明显的球状游离碳。
图3为3种样品的TEM图。从图3可知，1#样品表面包覆一层5～15 nm的碳层，该碳层均匀分布在颗粒表面。将氧化亚硅原料视为标准球形，假设表面碳层为致密碳层，经理论计算，碳层厚度约为12.6 nm[16]。理论计算结果表明，1#样品表面分布的是致密碳层。内部晶格位置经过计算为氧化亚硅相关物相的晶格。2#样品碳包覆层不均匀，既存在图3（b）中包覆碳层厚度均匀的情况，也存在图3（c）中边缘基本上不含碳层的情况，根据晶格尺寸计算，该处的物质为氧化亚硅，外侧无碳层，说明材料表面没有形成均匀的包覆层。3#样品表面包覆一层15～30 nm的碳层，该碳层均匀分布在材料表面。
3种样品在制备过程中碳含量设置为4%，实际碳含量测试结果如表3所示。3种样品的碳含量均在设定值的误差范围内，可以认为3种样品的碳含量是一致的，而3#样品碳层更厚，根据上述分析，1#样品表面为致密碳层，2#样品表面碳层分布不匀、厚度不一，3#样品碳层具备1#样品和2#样品的特点，其内部包覆了一层疏松碳层，外部为一层均匀的致密碳层。
2.3　材料电化学性能
3种样品首次充放电性能如图4所示。由图4可知，1#样品比容量为1 707.39 mAh/g，首次效率为75.82%；2#样品比容量为1 654.20 mAh/g，首次效率为75.89%；3#样品比容量为1 688.45 mAh/g，首次效率为76.13%。2#、3#样品的放电电压平台比1#样品的放电电压平台更低，说明2#、3#样品的极化更小，反应过程阻力更小。分析原因，放电过程为材料嵌入锂离子的过程，1#样品的碳层为均匀致密的层状炭，致密结构会阻碍锂离子的快速嵌入，2#、3#样品的碳层具有疏松链状碳，可以提供更多的锂离子嵌入通道，有利于锂离子的快速嵌入。
图5为3种样品的循环放电曲线。3#样品的循环性能更优，循环100次后，容量保持率为79.6%；1#和2#样品循环容量衰减较快，循环100次后容量保持率分别为72.6%和69.8%。3种样品在循环100次后，循环性能相差很大，性能较好的为3#样品，结合碳层包覆情况来看，3#样品碳层内部疏松、外部致密。疏松碳层可有效缓冲硅的膨胀，同时又可以提供锂离子快速嵌入的通道。致密碳层具备良好的刚性，可以保证材料在充放电过程中的结构稳定性，因此循环效果更好。
3　结论
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1）以气相碳源气相包覆的碳层均匀分布且致密，以固相碳源PAM液相包覆的碳层疏松且不均匀，组合两种碳源、两种包覆方式的碳层，具有内层疏松、外层致密的特点，且均匀分布在材料表面。
2）固相碳源包覆形成的疏松包覆结构有利于锂离子的快速嵌入，降低了材料在放电过程中的极化，放电电压平台较低。
3）3种不同包覆方式制备的氧化亚硅材料的首次容量和首次效率相当，但循环性能有明显差异。气相碳源和固相碳源组合包覆方式，既有疏松的碳层缓冲材料充放电过程中的膨胀，又有致密的碳层提升材料结构稳定性，具有较优的循环性能，循环放电100次后，容量保持率为79.6%。
基金
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  • 湖南省重点研发计划(2023SK2072)
  • 长沙市科技重大专项(kh2301023)
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2025年第45卷第3期
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doi: 10.3969/j.issn.0253-6099.2025.03.033
  • 接收时间：2024-12-18
  • 首发时间：2026-03-19
  • 出版时间：2025-06-01
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  • 收稿日期：2024-12-18
基金
湖南省重点研发计划(2023SK2072)
长沙市科技重大专项(kh2301023)
作者信息
    1.中机国际工程设计研究院有限责任公司，湖南　长沙　410021
    2.锂离子电池及材料智能制造先进技术湖南省工程研究中心，湖南　长沙　410021
    3.长沙矿冶院检测技术有限责任公司，湖南　长沙　410012

通讯作者:

李中良（1988—），男，河南许昌人，硕士，工程师，主要研究方向为新能源材料及器件的研发和检测。E-mail：
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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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