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Article(id=1241081027150533111, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.04.014, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1712419200000, receivedDateStr=2024-04-07, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773826375043, onlineDateStr=2026-03-18, pubDate=1722441600000, pubDateStr=2024-08-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773826375043, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773826375043, creator=13701087609, updateTime=1773826375043, 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='1722441600000', pubDateStr='2024-08-01', 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, articleTotal=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, downloadFileDto=null}, startPage=75, endPage=80, ext={EN=ArticleExt(id=1241081027519631869, articleId=1241081027150533111, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Solid-Phase Synthesis and Properties of Sulfide Solid Electrolyte Li6PS5Cl, columnId=1241081026567533498, journalTitle=Mining and Metallurgical Engineering, columnName=SPECIAL ISSUE: BATTERY MATERIALS, runingTitle=null, highlight=null, articleAbstract=

An argyrodite-type sulfide solid electrolyte Li6PS5Cl (LPSC) was solid-phase synthesized by adopting high energy ball milling in combination with heat treatment. It is found that prolonging ball milling time is conducive to crushing, mixing, grain refinement and amorphization reaction process of raw material powder; increasing sintering temperature is beneficial to the formation of a single pure phase, but too high temperature for sintering can make electrolyte melted and decomposed, leading to destroyed crystal structure. It is found that after 10 hours of ball milling and 8 hours of sintering at 550 ℃, the synthesized sulfide solid electrolyte exhibits higher ionic conductivity, reaching 3.57×10-3S/cm.

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通过高能球磨结合热处理的方法固相合成了硫银锗矿型硫化物固态电解质Li6PS5Cl（LPSC）。研究发现，延长球磨时间有利于原料粉末颗粒的破碎、混合、晶粒细化以及非晶化反应的进行；升高烧结温度有利于生成单一纯相，但烧结温度过高会使电解质熔化分解，破坏晶体结构。球磨时间10 h、550 ℃下烧结8 h所制备的硫化物固态电解质材料具有较高的离子电导率，可达3.57×10-3S/cm。

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陶博文（1999—），男，安徽铜陵人，硕士，主要研究方向为硫化物固态电解质的合成与改性。E-mail：

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涂飞跃（1983—），男，湖南邵阳人，博士，高级工程师，硕士研究生导师，主要研究方向为新能源材料与器件。E-mail：
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陶博文（1999—），男，安徽铜陵人，硕士，主要研究方向为硫化物固态电解质的合成与改性。E-mail：

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陶博文（1999—），男，安徽铜陵人，硕士，主要研究方向为硫化物固态电解质的合成与改性。E-mail：

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（a）350 ℃；（b）450 ℃；（c）550 ℃；（d）650 ℃

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（a）350 ℃；（b）450 ℃；（c）550 ℃；（d）650 ℃

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球磨时间/hLi2S晶粒尺寸/nmLiCl晶粒尺寸/nm
426.0135.66
625.1334.21
822.2421.87
1022.1313.34
1222.0212.41
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不同球磨时间下LPSC-Pre样品晶粒尺寸

, figureFileSmall=null, figureFileBig=null, tableContent=
球磨时间/hLi2S晶粒尺寸/nmLiCl晶粒尺寸/nm
426.0135.66
625.1334.21
822.2421.87
1022.1313.34
1222.0212.41
), ArticleFig(id=1241081041113371619, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081027150533111, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
烧结温度/℃Rb/ΩRgb/Ω
35056.9458.88
45061.6125.06
55064.539.42
65057.2768.88
), ArticleFig(id=1241081041226617839, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081027150533111, language=CN, label=表2, caption=

各烧结温度下LPSC电解质Rb和Rgb值

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烧结温度/℃Rb/ΩRgb/Ω
35056.9458.88
45061.6125.06
55064.539.42
65057.2768.88
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硫化物固态电解质Li6PS5Cl的固相合成及性能研究
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陶博文 , 鞠博伟 , 涂飞跃
矿冶工程杂志 | 电池材料专题 2024,44(4): 75-80
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矿冶工程杂志 |电池材料专题 2024 , 44 (4) : 75 -80
硫化物固态电解质Li6PS5Cl的固相合成及性能研究
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陶博文 , 鞠博伟, 涂飞跃
作者信息
  • 长沙矿冶研究院有限责任公司，湖南 长沙 410012
通讯作者:
涂飞跃（1983—），男，湖南邵阳人，博士，高级工程师，硕士研究生导师，主要研究方向为新能源材料与器件。E-mail：
Solid-Phase Synthesis and Properties of Sulfide Solid Electrolyte Li6PS5Cl
Bowen TAO , Bowei JU, Feiyue TU
Affiliations
  • Changsha Research Institute of Mining and Metallurgy Co, Ltd, Changsha 410012, Hunan, China
出版时间: 2024-08-01 doi: 10.3969/j.issn.0253-6099.2024.04.014
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摘要
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通过高能球磨结合热处理的方法固相合成了硫银锗矿型硫化物固态电解质Li6PS5Cl（LPSC）。研究发现，延长球磨时间有利于原料粉末颗粒的破碎、混合、晶粒细化以及非晶化反应的进行；升高烧结温度有利于生成单一纯相，但烧结温度过高会使电解质熔化分解，破坏晶体结构。球磨时间10 h、550 ℃下烧结8 h所制备的硫化物固态电解质材料具有较高的离子电导率，可达3.57×10-3S/cm。

全固态电池  /  硫化物固态电解质  /  Li6PS5Cl  /  离子电导率  /  硫银锗矿型  /  高能球磨  /  固相合成

An argyrodite-type sulfide solid electrolyte Li6PS5Cl (LPSC) was solid-phase synthesized by adopting high energy ball milling in combination with heat treatment. It is found that prolonging ball milling time is conducive to crushing, mixing, grain refinement and amorphization reaction process of raw material powder; increasing sintering temperature is beneficial to the formation of a single pure phase, but too high temperature for sintering can make electrolyte melted and decomposed, leading to destroyed crystal structure. It is found that after 10 hours of ball milling and 8 hours of sintering at 550 ℃, the synthesized sulfide solid electrolyte exhibits higher ionic conductivity, reaching 3.57×10-3S/cm.

all-solid state battery  /  sulfide solid electrolyte  /  Li6PS5Cl  /  ionic conductivity  /  argyrodite type  /  high energy ball milling  /  solid-phase synthesis
陶博文, 鞠博伟, 涂飞跃. 硫化物固态电解质Li6PS5Cl的固相合成及性能研究. 矿冶工程杂志, 2024 , 44 (4) : 75 -80 . DOI: 10.3969/j.issn.0253-6099.2024.04.014
Bowen TAO, Bowei JU, Feiyue TU. Solid-Phase Synthesis and Properties of Sulfide Solid Electrolyte Li6PS5Cl[J]. Mining and Metallurgical Engineering, 2024 , 44 (4) : 75 -80 . DOI: 10.3969/j.issn.0253-6099.2024.04.014
正文
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随着能源存储需求的增加和对环境友好型能源技术的追求，提高对风能和太阳能等可再生能源的存储与利用已成为人类面临的关键问题。作为高效的电能/化学能转化装置，锂离子电池的普及使用为上述问题提供了有效解决策略[1-3]。然而，液态电解液存在的蒸发、燃烧和化学不稳定性等问题限制了其在安全性和能量密度方面的进一步提升[4]。近年来，固态电解质作为一种潜在的解决方案，受到广泛关注[5-7]。相较于传统的液态电解液，固态电解质具有更高的化学稳定性、较低的燃烧风险、更广泛的操作温度范围等优点。其中硫化物是一种典型的固态电解质材料，由于其良好的离子传输性能、优异的化学稳定性和机械性能，为固态电池的应用提供了广阔空间，硫银锗矿型硫化物固态电解质具有良好的对锂稳定性、高室温离子电导率、合成简单、重复性高等优点，成为当下的研究热点[8]。
本文以Li2S、P2S5、LiCl为原料，通过高能球磨和热处理相结合的方式固相合成硫银锗矿型硫化物固态电解质Li6PS5Cl（LPSC），并结合X射线衍射、扫描电子显微镜、拉曼光谱及相关电化学测试手段探究球磨时间、烧结温度对LPSC电解质材料形貌、结构、电化学性能的影响。
1 实验
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1.1 实验原料及设备
主要原料有：硫化锂（Li2S，99.9%，泰坦科技股份有限公司）；五硫化二磷（P2S5，99%，泰坦科技股份有限公司）；氯化锂（LiCl，99%，泰坦科技股份有限公司）；导电炭黑（SP，电池级，特密高石墨有限公司）；金属锂片（99.9%，天津中能锂业有限公司）；铟片（99.995%，琪睿金属材料有限公司）。
主要设备有：威格手套箱（威格科技股份有限公司）；立式行星球磨机（XQM-0.4，长沙天创粉末技术有限公司）；电子天平（AUW-120D，岛津有限公司）；分体炉（KSL-1200X-J-F，合肥科晶材料技术有限公司）；电化学工作站（Zennium Pro德国札纳电化学公司）；电化学工作站（CHI660E上海辰华仪器有限公司）。
1.2 材料合成
按照LPSC中Li、P、S、Cl元素物质的量比6∶1∶5∶1称取原料，置于球磨罐中进行高能球磨。磨球氧化锆珠与原料质量比为40∶1，锆珠直径8 mm，球磨机转速650 r/min。正转时间29 min，反转时间29 min，间隔休息60 s，球磨总时间设置为4 h、6 h、8 h、10 h、12 h。由于硫化物质地较“软”[9]，期间每隔2 h打开球磨罐进行刮料，防止原料沾壁，影响球磨效果。球磨完成后将其转移到研钵中手动研磨15 min，得到LPSC电解质材料前驱体（LPSC-Pre）。
称取一定量LPSC-Pre于不锈钢模具中，在375 MPa下用粉末压片机压成具有一定厚度的圆形片体，放于石英管中密封好后进行热处理。烧结温度设置为350 ℃、450 ℃、550 ℃、650 ℃，升温速率2 ℃/min，保温时间8 h，烧结片体随炉体自然冷却到室温，而后在研钵中手动研磨15 min，得到LPSC电解质材料粉末。
以上高能球磨、热处理等实验步骤均在氩气气氛保护下的手套箱中进行，水、氧值均小于0.01×10-6。
1.3 物化性能测试
采用日本JSM-7900F型场发射扫描电子显微镜（SEM）和能谱仪（EDS）分析硫化物固态电解质材料的微观形貌和元素分布。制样、测试过程在手套箱中进行，以免样品受空气中水、氧的影响。
采用德国D8 Advance型X射线衍射仪（XRD）表征硫化物固态电解质材料的物相组成及结构。采用聚酰亚胺薄膜覆盖样品，以免在制样、转移测试过程中受空气中水、氧的影响。
采用拉曼光谱（Raman spectra）分析硫化物固态电解质材料的特征基团。将电解质粉末压入毛细管中，而后用真空脂对毛细管两端进行密封处理，防止测试过程中样品受空气中水、氧的影响。
1.4 电化学性能测试
称取100～300 mg LPSC固态电解质粉末置于内衬为聚醚醚酮（PEEK）的专用固态锂离子电池测试模具中，两边采用不锈钢片作为阻塞电极，外加不锈钢夹具，在375 MPa下压制，保压3 min。采用Zennium Pro德国札纳电化学工作站测试离子电导率，测试频率范围0.1 mHz～8 MHz，电压偏扰5 mV；采用电化学工作站测试电子电导率，所加直流电压为1 V，测试时间30 min。通过CHI660E电化学工作站对电解质样品进行室温下的循环伏安（CV）测试。
2 结果与讨论
收起
2.1 球磨时间对LPSC-Pre物相和微观形貌的影响
图1为不同球磨时间下LPSC-Pre样品XRD图谱。由图1可知，不同球磨时间下样品衍射图谱中均能观察到Li2S、LiCl和聚酰亚胺薄膜（PI）所对应的衍射峰，在2θ=18°附近出现的非晶峰来自于覆盖样品的聚酰亚胺薄膜。球磨时间4～12 h条件下，Li2S和LiCl衍射峰强度逐渐降低，说明在此过程中原料晶粒尺寸逐渐减小，逐渐发生非晶化反应。
对XRD图谱拟合计算获得了不同球磨时间下所得LPSC-Pre样品的晶粒尺寸，如表1所示。Li2S较“软”的性能[9]使其具有较低的硬度和较高的柔韧性，即材料抵抗表面穿透或断裂变形的能力更强，在球磨过程中更易发生塑性变形，其晶粒尺寸变化没有LiCl晶粒尺寸变化那么明显。球磨时间达到10 h后，再延长球磨时间，Li2S、LiCl晶粒尺寸变化不明显，说明此时原料中各粉末的破碎、细化、混合反应过程已经较为充分。
球磨时间10 h所得LPSC-Pre样品SEM微观形貌如图2所示。经过高能球磨后，前驱体粉末颗粒尺寸为10～20 μm。
图3为球磨时间10 h所得LPSC-Pre样品的EDS元素分布图。从P、S、Cl元素的分布可以看出，原料中各组分均匀分布，可满足后续烧结实验要求。
2.2 烧结温度对LPSC形貌的影响
不同烧结温度下所得LPSC电解质粉末微观形貌如图4所示。随着烧结温度升高，小颗粒发生聚集并通过固相反应熔化形成尺寸较大的颗粒；温度达到650 ℃时，由于烧结温度高于原料主要组分熔点，电解质材料发生熔化，冷却过程中应力的释放导致粉末颗粒表面产生裂痕，同时高温下电解质材料发生分解，原有结构被破坏，电化学性能下降[10]。
不同烧结温度下所得LPSC电解质粉末EDS面扫结果如图5所示。P、S、Cl等元素在所有样品中的分布都较为均匀，说明所得LPSC电解质成分均匀性较好，能满足实验要求。
2.3 烧结温度对LPSC物相的影响
不同烧结温度下所得LPSC电解质粉末XRD图谱如图6所示。350 ℃下烧结所得样品中除了LPSC衍射峰外仍可观察到Li2S、LiCl的衍射峰；烧结温度提高到450 ℃时，Li2S和LiCl的衍射峰强度明显降低，LPSC衍射峰的半高宽随着温度升高逐渐减小；烧结温度550 ℃时，样品为较纯的单一相LPSC。说明烧结过程中原料发生固相反应生成了LPSC，且提高烧结温度，固相反应更充分，LPSC结晶性更好。但温度继续升高到650 ℃时，LPSC衍射峰强度急剧减弱，推测是LPSC熔化分解、结构被破坏所致。
2.4 烧结温度对LPSC拉曼基团的影响
图7为不同烧结温度下所得LPSC电解质粉末拉曼光谱。所有烧结样品均能在425 cm-1处观察到最强的散射峰，且在200 cm-1和580 cm-1有两处弱峰，这些峰都来自LPSC电解质的PS43-基团。结合XRD表征结果，进一步表明各反应物之间已充分反应，生成了LPSC单一相，同时，550 ℃下烧结所得LPSC样品PS43-基团对应的峰强度最高。此外，现有实验结果表明，与其他P—S基团相比，PS43-基团在空气中更不易水解，电解质中PS43-质量浓度越高，电解质材料稳定性越好[11]。
2.5 烧结温度对LPSC离子电导率和电子电导率的影响
图8为不同烧结温度下所得LPSC电解质粉末电化学阻抗（EIS）曲线。由图8可知，LPSC的EIS曲线由一条长尾直线和高频区域的两个半圆构成，两个半圆分别代表材料本体阻抗和晶界阻抗[12]。实际测试过程中受限于设备最高测试频率，或因电解质样品离子电导率较高、晶界阻抗值较小，其中一个半圆消失，通常只能观察到一个半圆或仅仅只有一条直线。此时，半圆与直线的交点或直线与X轴的交点横坐标即为电解质材料的阻抗值。
LPSC阻抗拟合电路图见图9。通过电路拟合可计算得到LPSC电解质的本体电阻Rb和晶界电阻Rgb，结果如表2所示。随着烧结温度升高，电解质本体电阻Rb变化不大；晶界电阻Rgb逐渐减小，但在650 ℃时又突然增大，说明适宜的烧结温度可以减小材料的整体电阻。
图10为不同烧结温度下所得LPSC电解质室温下的直流极化曲线。LPSC的极化电流开始时为离子和电子电流混合的高瞬态电流；离子电流很快下降，经过长时间达到稳态后，得到基本不变的电子电流[12]。值得注意的是，达到稳态所需时间一般超过60 min，而测试时间为30 min，尚未达到稳态。此外，稳态电流仅1×10-9A甚至更低，超过电化学工作站的检测极限。考虑以上两点因素，实际测量得到的稳态电流应大于电解质本身电子贡献的电流，即实际测量的电子电导率一般高于电解质实际的电子电导率。
不同烧结温度下所得LPSC电解质离子电导率和电子电导率如图11所示。由图11可知，LPSC室温离子电导率随着烧结温度升高而上升，在烧结温度550 ℃时最大，为3.57×10-3S/cm；温度继续升高导致电解质材料分解破坏，离子电导率下降。LPSC室温电子电导率均小于2×10-8S/cm，能满足硫化物固态电解质的理想电子绝缘条件[13]。结合材料XRD和拉曼光谱分析结果，适宜的烧结温度为550 ℃。
2.6 LPSC固态电解质的循环伏安测试
固态电解质与不锈钢金属阻塞电极接触面积有限，导致分解反应动力学缓慢。采用锂/电解质/不锈钢阻塞电极的传统实验方法可能高估了固态电解质的电化学稳定窗口。因此，有研究[14]建立了一类利用锂/电解质/电解质-碳导电剂体系测量固态电解质电化学稳定窗口的实验方法。将碳导电剂和固体电解质混合在一起，形成复合电极。由于固态电解质与电子导电添加剂之间的接触面积显著增加，复合电极中固体电解质的还原或氧化动力学显著加快，更能准确评估固态电解质的电化学稳定窗口[15]。
为了进一步探究LPSC电解质的电化学性能，选用550 ℃下烧结8 h所得LPSC电解质组装成LPSC-C/LPSC/Li-In夹层电池，对LPSC固态电解质电化学稳定性进行表征。负极采用锂铟合金是由于循环过程中锂铟合金与硫化物固态电解质的副反应较少，且能保持一个稳定的对电位（对锂电位+0.6 V）。LPSC固态电解质CV曲线如图12所示。
首圈从开路电压扫描至-1 V，该过程中锂负极中的锂溶出（即），锂离子经过固态电解质穿梭到阻塞电极侧，获得电子（即），生成金属锂，沉积到阻塞电极与电解质的界面处。锂溶出-沉积电流的大小与施加的电压成正比，在电压-1 V时达到最大。LPSC氧化、还原时的分解电流远低于锂的溶出-沉积电流，故在-1～5 V范围内观察不到明显的电解质氧化、还原峰，但放大循环伏安曲线可以发现，在2.2 V左右出现一个氧化峰，对应电解质的氧化分解[12]，且没有对应的还原峰，说明电解质材料分解是不可逆的。
上述结果表明，LPSC固态电解质的电化学稳定窗口约0～2.2 V（vs Li-In），但过程中发生的不可逆分解所产生的副反应产物会存留在电解质与正负极的界面处并逐渐累积，使电池阻抗增大，因此LPSC固态电解质电化学稳定性仍有一定提升空间。
3 结论
收起
1）延长高能球磨时间，有利于LPSC固态电解质原料粉末细化、混合以及非晶化反应的进行。球磨机转速650 r/min，球磨时间10 h时，所得LPSC-Pre能满足后续烧结实验要求。
2）升高烧结温度，LPSC电解质结晶度变好、杂相减少、物相变纯。但烧结温度过高会导致电解质分解，破坏原有结构。550 ℃下烧结制备的LPSC电解质室温离子电导率为3.57×10-3S/cm，满足电子绝缘条件。适宜的烧结参数为：烧结温度550 ℃，升温速率2 ℃/min，烧结时间8 h。
3）550 ℃下烧结所得LPSC电解质离子电导率性能优异，但循环伏安测试结果表明LPSC电解质的电化学稳定窗口为0～2.2 V（vs Li-In），电化学稳定性仍有提升空间。该实验结果为LPSC固态电解质的改性奠定了基础，具有一定参考意义。

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doi: 10.3969/j.issn.0253-6099.2024.04.014
  • 接收时间：2024-04-07
  • 首发时间：2026-03-18
  • 出版时间：2024-08-01
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    长沙矿冶研究院有限责任公司，湖南 长沙 410012

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涂飞跃（1983—），男，湖南邵阳人，博士，高级工程师，硕士研究生导师，主要研究方向为新能源材料与器件。E-mail：
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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
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光柄菇属 Pluteus 5 2.39
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