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Article(id=1241081026471055859, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.04.015, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1716480000000, receivedDateStr=2024-05-24, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773826374880, onlineDateStr=2026-03-18, pubDate=1722441600000, pubDateStr=2024-08-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773826374880, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773826374880, creator=13701087609, updateTime=1773826374880, 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=81, endPage=83, ext={EN=ArticleExt(id=1241081026814988789, articleId=1241081026471055859, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Modification of Lithium Sulfide Prepared with Lithium Metal by Lithium Nitride, columnId=1241081026567533498, journalTitle=Mining and Metallurgical Engineering, columnName=SPECIAL ISSUE: BATTERY MATERIALS, runingTitle=null, highlight=null, articleAbstract=

Lithium sulfide was prepared by solid phase syntheses, with lithium metal as the lithium source, sulfur powder as the sulfur source, and lithium nitride as the additive. Thermodynamic analysis results show that lithium nitride can promote the reaction of lithium metal with sulfur powder to synthesize lithium sulfide; Li3N firstly reacts with sulfur powder to release N2, leading to holes formed on the molten lithium metal sheet and the contact area between lithium metal and sulfur powder further expanded. Thus a loose and porous skeleton structure is formed, which is conducive to subsequent crushing and can reduce the risk of secondary reactions in the following ball milling process. With Li∶S∶Li3N=2∶2∶0.4 (molar ratio), crude lithium sulfide can be obtained after 8 hours reaction at 100 ℃. It is then subjected to calcination, impurity removal and ball milling processes, and a kind of lithium sulfide products with purity greater than 99.95% and particle size less than 15 μm can be obtained, which can be used in EV. This method provides a new idea for industrial production of lithium sulfide products.

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以金属锂为锂源、硫粉为硫源、氮化锂为添加剂，采用固相法制备了硫化锂。热力学分析结果表明，氮化锂可促进金属锂与硫粉合成硫化锂的反应；Li3N先与硫粉反应释放N2，在熔融的金属锂片上形成孔洞，进一步扩大金属锂与硫粉接触面积，得到疏松多孔的骨架结构，有利于后续破碎且减少球磨过程中二次反应的风险。当Li∶S∶Li3N=2∶2∶0.4（物质的量比）时，在100 ℃下反应8 h即可得到粗品硫化锂，再经700 ℃煅烧、除杂和球磨后可以得到纯度大于99.95%、粒径小于15 μm的电动汽车用硫化锂产品。该方法为工业化生产硫化锂产品提供了新思路。

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田欢（1994—），男，甘肃陇南人，硕士，中级工程师，主要从事新型锂盐产品开发工作。E-mail：；
刘杨（1980—），男，辽宁营口人，博士，主要从事电池材料开发工作。E-mail：
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雷振（1996—），男，四川成都人，硕士，主要从事新型锂盐产品开发工作。E-mail：

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雷振（1996—），男，四川成都人，硕士，主要从事新型锂盐产品开发工作。E-mail：

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雷振（1996—），男，四川成都人，硕士，主要从事新型锂盐产品开发工作。E-mail：

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（a）无添加剂；（b）Li3N添加量x=0.4

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Li3N添加量x粗品硫化锂粒径D50/μm
0.084.46
0.252.43
0.438.63
0.644.20
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Li3N添加量x粗品硫化锂粒径D50/μm
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钾镁铁硅钛铬铝锌硼
3.34.13.59.36.31.36.63.42.7
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硫化锂产品杂质元素含量分析结果（质量分数）

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钾镁铁硅钛铬铝锌硼
3.34.13.59.36.31.36.63.42.7
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氮化锂对金属锂制备硫化锂改性研究
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雷振 1, 2 , 陈格 1, 2 , 徐川 2, 3 , 孙家乐 1 , 杨柳 1 , 田欢 1, 2 , 刘杨 2, 3
矿冶工程杂志 | 电池材料专题 2024,44(4): 81-83
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矿冶工程杂志 | 电池材料专题 2024, 44(4): 81-83
氮化锂对金属锂制备硫化锂改性研究
全屏
雷振1, 2 , 陈格1, 2, 徐川2, 3, 孙家乐1, 杨柳1, 田欢1, 2 , 刘杨2, 3
作者信息
  • 1.天齐锂业（射洪）有限公司，四川 射洪 629200
  • 2.锂资源与锂材料四川省重点实验室，四川 射洪 629200
  • 3.天齐鑫隆科技（成都）有限公司，四川 成都 610000

    • 雷振（1996—），男，四川成都人，硕士，主要从事新型锂盐产品开发工作。E-mail：

通讯作者:

田欢（1994—），男，甘肃陇南人，硕士，中级工程师，主要从事新型锂盐产品开发工作。E-mail：；
刘杨（1980—），男，辽宁营口人，博士，主要从事电池材料开发工作。E-mail：
Modification of Lithium Sulfide Prepared with Lithium Metal by Lithium Nitride
Zhen LEI1, 2 , Ge CHEN1, 2, Chuan XU2, 3, Jiale SUN1, Liu YANG1, Huan TIAN1, 2 , Yang LIU2, 3
Affiliations
  • 1.Tianqi Lithium (Shehong) Co., Ltd., Shehong 629200, Sichuan, China
  • 2.Sichuan Key Laboratory of Lithium Resources and Materials, Shehong 629200, Sichuan, China
  • 3.Tianqi Xinlong Technology (Chengdu) Co., Ltd., Chengdu 610000, Sichuan, China
出版时间: 2024-08-01 doi: 10.3969/j.issn.0253-6099.2024.04.015
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摘要
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以金属锂为锂源、硫粉为硫源、氮化锂为添加剂，采用固相法制备了硫化锂。热力学分析结果表明，氮化锂可促进金属锂与硫粉合成硫化锂的反应；Li3N先与硫粉反应释放N2，在熔融的金属锂片上形成孔洞，进一步扩大金属锂与硫粉接触面积，得到疏松多孔的骨架结构，有利于后续破碎且减少球磨过程中二次反应的风险。当Li∶S∶Li3N=2∶2∶0.4（物质的量比）时，在100 ℃下反应8 h即可得到粗品硫化锂，再经700 ℃煅烧、除杂和球磨后可以得到纯度大于99.95%、粒径小于15 μm的电动汽车用硫化锂产品。该方法为工业化生产硫化锂产品提供了新思路。

固态电池  /  固态电解质  /  氮化锂  /  锂  /  硫  /  EV级

Lithium sulfide was prepared by solid phase syntheses, with lithium metal as the lithium source, sulfur powder as the sulfur source, and lithium nitride as the additive. Thermodynamic analysis results show that lithium nitride can promote the reaction of lithium metal with sulfur powder to synthesize lithium sulfide; Li3N firstly reacts with sulfur powder to release N2, leading to holes formed on the molten lithium metal sheet and the contact area between lithium metal and sulfur powder further expanded. Thus a loose and porous skeleton structure is formed, which is conducive to subsequent crushing and can reduce the risk of secondary reactions in the following ball milling process. With Li∶S∶Li3N=2∶2∶0.4 (molar ratio), crude lithium sulfide can be obtained after 8 hours reaction at 100 ℃. It is then subjected to calcination, impurity removal and ball milling processes, and a kind of lithium sulfide products with purity greater than 99.95% and particle size less than 15 μm can be obtained, which can be used in EV. This method provides a new idea for industrial production of lithium sulfide products.

solid-state battery  /  solid electrolyte  /  lithium nitride  /  lithium  /  sulphur  /  material for EV
雷振, 陈格, 徐川, 孙家乐, 杨柳, 田欢, 刘杨. 氮化锂对金属锂制备硫化锂改性研究. 矿冶工程杂志, 2024 , 44 (4) : 81 -83 . DOI: 10.3969/j.issn.0253-6099.2024.04.015
Zhen LEI, Ge CHEN, Chuan XU, Jiale SUN, Liu YANG, Huan TIAN, Yang LIU. Modification of Lithium Sulfide Prepared with Lithium Metal by Lithium Nitride[J]. Mining and Metallurgical Engineering, 2024 , 44 (4) : 81 -83 . DOI: 10.3969/j.issn.0253-6099.2024.04.015
正文
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近年来，具有高能量密度及安全性的全固态电池受到广泛关注，有望成为下一代电化学储能电池的候选者[1-2]。固态电解质是全固态电池的关键组成部分，其中硫化物电解质具有极高的离子电导率，其离子电导率与商业有机液体电解质相当，甚至高于商业有机液体电解质[1,3]。
硫化锂（Li2S）作为硫化物固态电解质的重要原材料，其纯度决定了电解质性能以及固态电池性能[4-6]。目前合成硫化锂的方法主要有固相法[7]、液相法[8-9]、高温碳热还原法[10-12]以及气固法[13-14]。其中，固相法因其操作简单、无有毒有害气体产生等优势在众多制备方法中广受关注，但该方法依然存在反应不充分、产品纯度低的问题。
基于此，本文从反应热力学过程分析着手，通过添加氮化锂（Li3N）解决合成反应中反应不充分、易二次反应的问题，提高产品纯度。同时，通过球磨的方式将所得产品的粒径控制在20 μm以内。该研究有望提供一种可产业化的硫化锂生产方案。
1 实验部分
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按Li、S、Li3N物质的量比2∶2∶x（x=0，0.2，0.4，0.6）称取反应物料，分别放入金属锆材反应釜中，釜内通氩气，维持微正压。反应温度100 ℃、搅拌转速20 r/min、反应时间8 h；待反应结束后取出物料，然后进行高温煅烧，除去未反应完全的硫粉，煅烧温度为700 ℃，煅烧过程通氩气保护；对煅烧后的粗品物料进行干法球磨，球磨参数为：球磨转速400 r/min、球磨时间4 h；球磨后得到硫化锂产品。
采用马尔文激光粒度仪测试样品粒径，溶剂为异丙醇；通过电感耦合等离子谱仪（ICP）测试杂质元素含量。
2 结果与讨论
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2.1 热力学分析
固相法制备硫化锂过程中发生的化学反应有：
2个反应的吉布斯自由能变化ΔG与温度T的关系如图1所示。由图1可知，2个反应均为自发反应（ΔG<0），其中反应（2）的ΔG较反应（1）更负，表明反应（2）进行的趋势更大。由于反应（2）产生的气体可在熔融的金属锂块中形成孔洞，从而形成疏松多孔的骨架结构，有利于后期球磨。
2.2 添加剂Li3N的作用分析
由热力学分析结果可见，氮化锂与金属锂均可与硫粉进行自发反应。氮化锂添加量对中间产品（粗品硫化锂）形貌及粒径的影响分别见图2及表1。从图2可见，添加氮化锂使粗品硫化锂中存在较多孔隙结构（图2（b）），而在空白对照组的粗品硫化锂表面平整无孔隙（图2（a））；从表1可知，氮化锂的添加可充分促进硫化锂的生成，得到较小粒径的疏松多孔硫化锂。未反应完全的金属锂和硫粉在球磨过程中由于金属锂摩擦生热，极易产生二次反应，造成球磨罐开裂；添加Li3N后与硫粉反应生成硫化锂和惰性气体N2，氮气释放后在产品表面形成带有孔洞的骨架结构，产品在球磨过程中可轻易磨细。
2.3 硫化锂产品纯度分析
对Li3N添加量x=0.4制备的硫化锂产品进行了X射线衍射分析，结果如图3所示。由图3可见，制备的硫化锂产品峰型与标准卡片PDF#89-1730的峰型一一对应，无明显杂质峰。
采用ICP对硫化锂产品杂质成分进行了分析，结果见表2。结果显示，其主要金属杂质质量分数均低于1 000×10-6，硫化锂样品纯度大于99.95%。
2.4 硫化锂产品形貌及粒径分析
图4为硫化锂产品SEM形貌。硫化锂呈不规则颗粒，部分硫化锂内部存在孔洞（3～5 μm），这是因为反应（2）生成的N2从内部逸出形成的孔穴，该带孔结构具有提升反应效率及易于球磨的优点。通过激光粒度仪对球磨后硫化锂产品进行了粒度测试，结果见图5。硫化锂D50粒度约12 μm，与SEM观察结果基本符合。
3 结论
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1）热力学分析结果证明Li3N可作为添加剂促进金属锂与硫粉合成硫化锂的反应，在100 ℃下反应8 h即可得到粗品硫化锂，经煅烧除杂和球磨后可得到高品质小粒径硫化锂产品。
2）Li3N作为添加剂，可先与硫粉反应释放N2，在熔融的金属锂片上形成孔洞，从而进一步扩大金属锂与硫粉接触面积，得到疏松多孔的骨架结构，有利于后续破碎且减少球磨过程中二次反应的风险。
3）Li3N添加量x=0.4时可以得到纯度大于99.95%、粒径小于15 μm的电动汽车用硫化锂产品。
基金
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  • 四川省科技计划重点研发项目(2022YFG0124)
  • 四川省科技计划苗子工程项目(2023JDRC0071)
  • 遂宁市校企合作“揭榜挂帅”项目(2022CDSN-02)
文献
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2024年第44卷第4期
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doi: 10.3969/j.issn.0253-6099.2024.04.015
  • 接收时间：2024-05-24
  • 首发时间：2026-03-18
  • 出版时间：2024-08-01
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  • 收稿日期：2024-05-24
基金
四川省科技计划重点研发项目(2022YFG0124)
四川省科技计划苗子工程项目(2023JDRC0071)
遂宁市校企合作“揭榜挂帅”项目(2022CDSN-02)
作者信息
    1.天齐锂业（射洪）有限公司，四川 射洪 629200
    2.锂资源与锂材料四川省重点实验室，四川 射洪 629200
    3.天齐鑫隆科技（成都）有限公司，四川 成都 610000

通讯作者:

田欢（1994—），男，甘肃陇南人，硕士，中级工程师，主要从事新型锂盐产品开发工作。E-mail：；
刘杨（1980—），男，辽宁营口人，博士，主要从事电池材料开发工作。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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