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Article(id=1195319924638916796, tenantId=1146029695717560320, journalId=1189873562199433220, issueId=1195319920000012443, articleNumber=null, orderNo=null, doi=10.19710/J.cnki.1003-8817.20240141, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=null, receivedDateStr=null, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1762916078003, onlineDateStr=2025-11-12, pubDate=1739980800000, pubDateStr=2025-02-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1762916078003, onlineIssueDateStr=2025-11-12, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1762916078003, creator=13701087609, updateTime=1762916078003, updator=13701087609, issue=Issue{id=1195319920000012443, tenantId=1146029695717560320, journalId=1189873562199433220, year='2025', volume='', issue='2', pageStart='1', pageEnd='72', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1762916076894, creator=13701087609, updateTime=1762916415896, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1195321341915205752, tenantId=1146029695717560320, journalId=1189873562199433220, issueId=1195319920000012443, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1195321341915205753, tenantId=1146029695717560320, journalId=1189873562199433220, issueId=1195319920000012443, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=6, endPage=10, ext={EN=ArticleExt(id=1195319925729435842, articleId=1195319924638916796, tenantId=1146029695717560320, journalId=1189873562199433220, language=EN, title=Determination of 19 Trace Elements in Ternary Cathode Materials by ICP-OES, columnId=1190284220686766583, journalTitle=Automobile Technology & Material, columnName=Original article, runingTitle=null, highlight=null, articleAbstract=

In the lithium-ion battery ternary anode materials, trace elements affect the battery performance directly, in this study, an analytical method for simultaneous determination of 19 trace elements including Nb, B, Zr, Sr, Ta, Ti, Y, La, Ga, Cu, Fe, K, Mg, P, Na, Al, Cr, Mo and Zn in ternary anode materials of lithium ion batteries is established by inductively coupled plasma emission spectrometry. The influence of different solvents on the determination of trace elements in ternary anode materials is investigated, and the best sample solvent is determined. The results show that the method is simple, rapid, and has good repeatability and reliability. The relative standard deviation of each element is 0.58%~3.56%, and the recovery is 91.81%~104.91%, which can fully meet the needs of trace element content analysis of ternary cathode materials.

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锂离子电池三元正极材料中的微量元素直接影响电池性能，为准确测定其元素含量，利用电感耦合等离子体发射光谱（ICP-OES）法，建立了同时测定锂离子电池三元正极材料中铌、硼、锆、锶、钽、钛、铱、镧、钙、铜、铁、钾、镁、磷、钠、铝、铬、钼、锌共19种微量元素的分析方法。考察了不同溶剂对三元正极材料中微量元素含量测定的影响，最终确定最佳样品溶剂。结果表明：该方法简便、快捷，有良好的分析重复性和可靠性，各元素的相对标准偏差为0.58%~3.56%，回收率为91.81%~104.91%，满足三元正极材料微量元素含量分析的需要。

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李宇升（1994—），男，工程师，硕士学位，研究方向为化学工程。

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李宇升（1994—），男，工程师，硕士学位，研究方向为化学工程。

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李宇升（1994—），男，工程师，硕士学位，研究方向为化学工程。

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year=2022, volume=39, issue=9, pageStart=7, pageEnd=10, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=李玉婷, journalName=化学与生物工程, refType=null, unstructuredReference=李玉婷. 碳中和背景下锂离子电池正极材料的发展趋势及应对措施[J]. 化学与生物工程, 2022, 39(9): 7-10., articleTitle=碳中和背景下锂离子电池正极材料的发展趋势及应对措施, refAbstract=null), Reference(id=1195335604562084210, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, doi=null, pmid=null, pmcid=null, year=2021, volume=null, issue=17, pageStart=17, pageEnd=18, url=null, language=null, rfNumber=[2], rfOrder=1, authorNames=涂康安, journalName=当代化工研究, refType=null, unstructuredReference=涂康安. 锂离子电池三元正极材料现状及发展趋势[J]. 当代化工研究, 2021(17): 17-18., articleTitle=锂离子电池三元正极材料现状及发展趋势, refAbstract=null), Reference(id=1195335604633387379, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, doi=null, pmid=null, pmcid=null, year=2020, volume=39, issue=5, pageStart=1044, pageEnd=1049, url=null, language=null, rfNumber=[3], rfOrder=2, authorNames=黄艳, 胡静, 周波, journalName=矿物岩石地球化学通报, refType=null, unstructuredReference=黄艳, 胡静, 周波. 电感耦合等离子体质谱法测定三元正极材料的组成[J]. 矿物岩石地球化学通报, 2020, 39(5): 1044-1049., articleTitle=电感耦合等离子体质谱法测定三元正极材料的组成, refAbstract=null), Reference(id=1195335604692107636, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, doi=null, pmid=null, pmcid=null, year=2023, volume=null, issue=null, pageStart=60, pageEnd=null, url=null, language=null, rfNumber=[4], rfOrder=3, authorNames=GYEONGBIN K, SEONGDEOCK J, SANGHYUK P, journalName=Energy Storage Materials, refType=null, unstructuredReference=GYEONGBIN K, SEONGDEOCK J, SANGHYUK P, et al. Doping Strategies for Enhancing the Performance of Lithium Nickel Manganese Cobalt Oxide Cathode Materials in Lithium-Ion Batteries[J]. Energy Storage Materials, 2023, 60., articleTitle=Doping Strategies for Enhancing the Performance of Lithium Nickel Manganese Cobalt Oxide Cathode Materials in Lithium-Ion Batteries, refAbstract=null), Reference(id=1195335604822131061, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, doi=null, pmid=null, pmcid=null, year=2019, volume=25, issue=4, pageStart=267, pageEnd=272, url=null, language=null, rfNumber=[5], rfOrder=4, authorNames=白晓艳, 谢艳艳, 高燕, journalName=分析测试技术与仪器, refType=null, unstructuredReference=白晓艳, 谢艳艳, 高燕. 采用电感耦合等离子体发射光谱法测定富锂锰基正极材料中9种杂质元素[J]. 分析测试技术与仪器, 2019, 25(4): 267-272., articleTitle=采用电感耦合等离子体发射光谱法测定富锂锰基正极材料中9种杂质元素, refAbstract=null), Reference(id=1195335604914405750, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, doi=null, pmid=null, pmcid=null, year=2022, volume=12, issue=18, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[6], rfOrder=5, authorNames=KIM D H, SONG J H, JUNG C H, journalName=Advanced Energy Materials, refType=null, unstructuredReference=KIM D H, SONG J H, JUNG C H, et al. Stepwise Dopant Selection Process for High-Nickel Layered Oxide Cathodes[J]. Advanced Energy Materials, 2022, 12(18)., articleTitle=Stepwise Dopant Selection Process for High-Nickel Layered Oxide Cathodes, refAbstract=null), Reference(id=1195335604994097527, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, doi=null, pmid=null, pmcid=null, year=2016, volume=6, issue=1, pageStart=45, pageEnd=47, url=null, language=null, rfNumber=[7], rfOrder=6, authorNames=王静, journalName=中国无机分析化学, refType=null, unstructuredReference=王静. 电感耦合等离子体发射光谱(ICP-OES)法测定镍钴锰酸锂中主元素含量[J]. 中国无机分析化学, 2016, 6(1): 45-47., articleTitle=电感耦合等离子体发射光谱(ICP-OES)法测定镍钴锰酸锂中主元素含量, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1195335600468443440, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, xref=null, ext=[AuthorCompanyExt(id=1195335600481026353, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, companyId=1195335600468443440, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Global R&D Center, China FAW Corporation Limited, Changchun 130013), AuthorCompanyExt(id=1195335600493609266, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, companyId=1195335600468443440, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中国第一汽车股份有限公司研发总院， 长春 130013)])], figs=[ArticleFig(id=1195335602989220195, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=EN, label=null, caption=null, figureFileSmall=1UrxNdDnYvnf0Rb/1Idyqg==, figureFileBig=u0v2pWFbSLVLNbBhQPnBiQ==, tableContent=null), ArticleFig(id=1195335603043746148, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=CN, label=图1, caption=不同溶剂对各微量元素溶解效果的影响, figureFileSmall=1UrxNdDnYvnf0Rb/1Idyqg==, figureFileBig=u0v2pWFbSLVLNbBhQPnBiQ==, tableContent=null), ArticleFig(id=1195335603131826533, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
元素 谱线的波长/nm 射频功率/kW 雾化气
流量
/L·min-1		 观测高度/mm 等离子气流量
/L·min-1		 元素 谱线的波长/nm 射频功率/kW 雾化气
流量
/L·min-1		 观测高度/mm 等离子气流量
/L·min-1
Nb 309.418 1.3 0.55 8 12 Fe 259.939 1.3 0.55 8 12
B 249.677 K 766.490
Zr 339.195 Mg 280.271
Sr 407.771 P 178.284
Ta 240.063 Na 589.592
Ti 336.116 Al 396.153
Y 371.029 Cr 267.716
La 398.852 Mo 202.031
Ca 396.843 Zn 206.200
Cu 327.393
), ArticleFig(id=1195335603232489830, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=CN, label=表1, caption=

待测元素的谱线选择

, figureFileSmall=null, figureFileBig=null, tableContent=
元素 谱线的波长/nm 射频功率/kW 雾化气
流量
/L·min-1		 观测高度/mm 等离子气流量
/L·min-1		 元素 谱线的波长/nm 射频功率/kW 雾化气
流量
/L·min-1		 观测高度/mm 等离子气流量
/L·min-1
Nb 309.418 1.3 0.55 8 12 Fe 259.939 1.3 0.55 8 12
B 249.677 K 766.490
Zr 339.195 Mg 280.271
Sr 407.771 P 178.284
Ta 240.063 Na 589.592
Ti 336.116 Al 396.153
Y 371.029 Cr 267.716
La 398.852 Mo 202.031
Ca 396.843 Zn 206.200
Cu 327.393
), ArticleFig(id=1195335603307987303, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
元素 标准曲线 相关
系数r		 元素含量测量范围
/μg·mL-1		 元素 标准曲线 相关
系数r		 元素含量测量范围
/μg·mL-1
Nb Y=508 787.2X+4 413.9 0.999 8 0.05~5.00 Fe Y=383 857.1X+7 909.0 0.999 8 0.05~5.00
B Y=904 631.5X+598.3 0.999 9 0.05~5.00 K Y=4 435 495.1X-127 939.2 0.999 6 0.05~5.00
Zr Y=2 472 147.4X-4 501.8 0.999 9 0.05~5.00 Mg Y=2 264 051.7X+42 016.3 0.999 8 0.05~5.00
Sr Y=10 081 754.0X+39 347.6 0.999 9 0.05~5.00 P Y=5 136.0X+52.4 0.999 7 0.05~5.00
Ta Y=16 926.4X+166.4 0.999 9 0.05~5.00 Na Y=13 159 493.4X+287 783.4 0.999 8 0.05~5.00
Ti Y=4 489 594.7X+17 992.9 0.999 9 0.05~5.00 Al Y=1 101 219.0X+3 898.7 0.999 9 0.05~5.00
Y Y=8 377 648.7X+8 383.6 0.999 9 0.05~5.00 Cr Y=788 852.2X+12.5 0.999 9 0.05~5.00
La Y=2 249 836.3X+21 884.8 0.999 8 0.05~5.00 Mo Y=13 003.4X+351.9 0.999 9 0.05~5.00
Ca Y=6 679 328.9X+2 871 952.4 0.999 5 0.05~5.00 Zn Y=67 034.3×104X+660.1 0.999 9 0.05~5.00
Cu Y=444 661.9X 0.999 9 0.05~5.00
), ArticleFig(id=1195335603404456296, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=CN, label=表2, caption=

19种微量元素的标准工作曲线

, figureFileSmall=null, figureFileBig=null, tableContent=
元素 标准曲线 相关
系数r		 元素含量测量范围
/μg·mL-1		 元素 标准曲线 相关
系数r		 元素含量测量范围
/μg·mL-1
Nb Y=508 787.2X+4 413.9 0.999 8 0.05~5.00 Fe Y=383 857.1X+7 909.0 0.999 8 0.05~5.00
B Y=904 631.5X+598.3 0.999 9 0.05~5.00 K Y=4 435 495.1X-127 939.2 0.999 6 0.05~5.00
Zr Y=2 472 147.4X-4 501.8 0.999 9 0.05~5.00 Mg Y=2 264 051.7X+42 016.3 0.999 8 0.05~5.00
Sr Y=10 081 754.0X+39 347.6 0.999 9 0.05~5.00 P Y=5 136.0X+52.4 0.999 7 0.05~5.00
Ta Y=16 926.4X+166.4 0.999 9 0.05~5.00 Na Y=13 159 493.4X+287 783.4 0.999 8 0.05~5.00
Ti Y=4 489 594.7X+17 992.9 0.999 9 0.05~5.00 Al Y=1 101 219.0X+3 898.7 0.999 9 0.05~5.00
Y Y=8 377 648.7X+8 383.6 0.999 9 0.05~5.00 Cr Y=788 852.2X+12.5 0.999 9 0.05~5.00
La Y=2 249 836.3X+21 884.8 0.999 8 0.05~5.00 Mo Y=13 003.4X+351.9 0.999 9 0.05~5.00
Ca Y=6 679 328.9X+2 871 952.4 0.999 5 0.05~5.00 Zn Y=67 034.3×104X+660.1 0.999 9 0.05~5.00
Cu Y=444 661.9X 0.999 9 0.05~5.00
), ArticleFig(id=1195335603563839849, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
元素 含量 元素 含量 元素 含量 元素 含量
Nb 0.068 B Zr 0.045 Sr
Ta 0.051 Ti 0.173 Y La
Ca 0.043 Cu Fe 0.028 K 0.017
Mg 0.015 P 0.121 Na 0.023 Al
Cr Mo Zn
), ArticleFig(id=1195335603714834794, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=CN, label=表3, caption=

三元正极材料中各微量元素含量（质量分数） %

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元素 含量 元素 含量 元素 含量 元素 含量
Nb 0.068 B Zr 0.045 Sr
Ta 0.051 Ti 0.173 Y La
Ca 0.043 Cu Fe 0.028 K 0.017
Mg 0.015 P 0.121 Na 0.023 Al
Cr Mo Zn
), ArticleFig(id=1195335603853246827, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
元素 本底值
/μg·mL-1		 加标量
/μg·mL-1		 回收率/% 相对标准偏差（RSD）/% 元素 本底值
/μg·mL-1		 加标量
/μg·mL-1		 回收率/% RSD/%
Nb 0.68 0.08 95.19 1.45 Fe 0.28 0.08 104.91 3.21
1.00 97.37 2.57 1.00 97.94 2.34
5.00 101.36 1.83 5.00 102.46 1.56
B 0.08 96.46 3.05 K 0.17 0.08 103.87 2.48
1.00 97.55 2.48 1.00 102.33 3.48
5.00 98.87 1.12 5.00 98.98 1.86
Zr 0.45 0.08 96.15 1.35 Mg 0.15 0.08 97.94 0.87
1.00 104.13 3.56 1.00 96.69 2.69
5.00 103.55 2.87 5.00 103.84 2.57
Sr 0.08 98.58 1.01 P 1.21 0.08 98.83 3.01
1.00 99.54 0.89 1.00 104.57 2.21
5.00 96.94 1.05 5.00 100.54 1.57
Ta 0.51 0.08 102.98 1.98 Na 0.23 0.08 97.59 1.35
1.00 98.87 2.57 1.00 97.18 1.62
5.00 101.22 3.04 5.00 99.75 1.09
Ti 1.73 0.08 99.74 2.94 Al 0.08 104.35 0.97
1.00 103.88 1.04 1.00 102.17 2.43
5.00 103.92 0.89 5.00 99.38 2.14
Y 0.08 98.96 1.54 Cr 0.08 96.35 1.54
1.00 96.83 1.98 1.00 97.34 1.97
5.00 99.95 0.61 5.00 100.68 0.58
La 0.08 98.76 1.52 Mo 0.08 97.86 2.34
1.00 101.27 1.94 1.00 98.94 1.05
5.00 100.32 2.41 5.00 101.28 1.45
Ca 0.43 0.08 91.81 3.11 Zn 0.08 103.99 1.82
1.00 98.78 1.36 1.00 99.45 0.98
5.00 102.49 1.05 5.00 98.77 1.56
Cu 0.08 99.45 0.87
1.00 98.73 1.46
5.00 97.63 2.04
), ArticleFig(id=1195335603949715820, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=CN, label=表4, caption=

加标回收率结果

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元素 本底值
/μg·mL-1		 加标量
/μg·mL-1		 回收率/% 相对标准偏差（RSD）/% 元素 本底值
/μg·mL-1		 加标量
/μg·mL-1		 回收率/% RSD/%
Nb 0.68 0.08 95.19 1.45 Fe 0.28 0.08 104.91 3.21
1.00 97.37 2.57 1.00 97.94 2.34
5.00 101.36 1.83 5.00 102.46 1.56
B 0.08 96.46 3.05 K 0.17 0.08 103.87 2.48
1.00 97.55 2.48 1.00 102.33 3.48
5.00 98.87 1.12 5.00 98.98 1.86
Zr 0.45 0.08 96.15 1.35 Mg 0.15 0.08 97.94 0.87
1.00 104.13 3.56 1.00 96.69 2.69
5.00 103.55 2.87 5.00 103.84 2.57
Sr 0.08 98.58 1.01 P 1.21 0.08 98.83 3.01
1.00 99.54 0.89 1.00 104.57 2.21
5.00 96.94 1.05 5.00 100.54 1.57
Ta 0.51 0.08 102.98 1.98 Na 0.23 0.08 97.59 1.35
1.00 98.87 2.57 1.00 97.18 1.62
5.00 101.22 3.04 5.00 99.75 1.09
Ti 1.73 0.08 99.74 2.94 Al 0.08 104.35 0.97
1.00 103.88 1.04 1.00 102.17 2.43
5.00 103.92 0.89 5.00 99.38 2.14
Y 0.08 98.96 1.54 Cr 0.08 96.35 1.54
1.00 96.83 1.98 1.00 97.34 1.97
5.00 99.95 0.61 5.00 100.68 0.58
La 0.08 98.76 1.52 Mo 0.08 97.86 2.34
1.00 101.27 1.94 1.00 98.94 1.05
5.00 100.32 2.41 5.00 101.28 1.45
Ca 0.43 0.08 91.81 3.11 Zn 0.08 103.99 1.82
1.00 98.78 1.36 1.00 99.45 0.98
5.00 102.49 1.05 5.00 98.77 1.56
Cu 0.08 99.45 0.87
1.00 98.73 1.46
5.00 97.63 2.04
), ArticleFig(id=1195335604058767725, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
元素 加标量
/μg·mL-1		 RSD/% 元素 加标量
/μg·mL-1		 RSD/% 元素 加标量
/μg·mL-1		 RSD/% 元素 加标量
/μg·mL-1		 RSD/%
Nb 0.10 2.53 Ti 0.10 2.52 Fe 0.10 2.68 Al 0.10 2.64
2.00 1.57 2.00 1.98 2.00 1.74 2.00 2.36
B 0.10 2.78 Y 0.10 2.98 K 0.10 3.98 Cr 0.10 0.76
2.00 1.83 2.00 3.27 2.00 4.28 2.00 1.48
Zr 0.10 1.96 La 0.10 2.58 Mg 0.10 1.56 Mo 0.10 2.05
2.00 2.68 2.00 2.86 2.00 2.51 2.00 1.38
Sr 0.10 3.56 Ca 0.10 1.38 P 0.10 4.21 Zn 0.10 3.03
2.00 2.63 2.00 1.05 2.00 3.27 2.00 2.19
Ta 0.10 1.75 Cu 0.10 3.75 Na 0.10 1.49 Al 0.10 2.64
2.00 2.59 2.00 2.56 2.00 1.38 2.00 2.36
), ArticleFig(id=1195335604138459502, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=CN, label=表5, caption=

日内重复性结果

, figureFileSmall=null, figureFileBig=null, tableContent=
元素 加标量
/μg·mL-1		 RSD/% 元素 加标量
/μg·mL-1		 RSD/% 元素 加标量
/μg·mL-1		 RSD/% 元素 加标量
/μg·mL-1		 RSD/%
Nb 0.10 2.53 Ti 0.10 2.52 Fe 0.10 2.68 Al 0.10 2.64
2.00 1.57 2.00 1.98 2.00 1.74 2.00 2.36
B 0.10 2.78 Y 0.10 2.98 K 0.10 3.98 Cr 0.10 0.76
2.00 1.83 2.00 3.27 2.00 4.28 2.00 1.48
Zr 0.10 1.96 La 0.10 2.58 Mg 0.10 1.56 Mo 0.10 2.05
2.00 2.68 2.00 2.86 2.00 2.51 2.00 1.38
Sr 0.10 3.56 Ca 0.10 1.38 P 0.10 4.21 Zn 0.10 3.03
2.00 2.63 2.00 1.05 2.00 3.27 2.00 2.19
Ta 0.10 1.75 Cu 0.10 3.75 Na 0.10 1.49 Al 0.10 2.64
2.00 2.59 2.00 2.56 2.00 1.38 2.00 2.36
), ArticleFig(id=1195335604213956975, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
元素 测试值 元素 测试值
1# 2# 3# 1# 2# 3#
Nb <0.05 <0.05 0.28 Fe <0.05 4.89 2.45
B 0.21 0.17 0.71 K 0.32 0.32 0.35
Zr 2.21 1.44 1.99 Mg 0.28 0.31 0.25
Sr 0.36 0.25 0.28 P 0.61 3.87 0.85
Ta 0.28 <0.05 <0.05 Na 0.38 0.37 0.31
Ti <0.05 1.32 0.52 Al 1.43 1.52 1.15
Y <0.05 <0.05 1.31 Cr 0.27 <0.05 <0.05
La 0.36 <0.05 <0.05 Mo <0.05 0.36 <0.05
Ca 0.28 0.35 0.23 Zn <0.05 0.21 0.16
Cu <0.05 0.87 <0.05
), ArticleFig(id=1195335604306231664, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1195319924638916796, language=CN, label=表6, caption=

样品分析结果 μg/mL

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元素 测试值 元素 测试值
1# 2# 3# 1# 2# 3#
Nb <0.05 <0.05 0.28 Fe <0.05 4.89 2.45
B 0.21 0.17 0.71 K 0.32 0.32 0.35
Zr 2.21 1.44 1.99 Mg 0.28 0.31 0.25
Sr 0.36 0.25 0.28 P 0.61 3.87 0.85
Ta 0.28 <0.05 <0.05 Na 0.38 0.37 0.31
Ti <0.05 1.32 0.52 Al 1.43 1.52 1.15
Y <0.05 <0.05 1.31 Cr 0.27 <0.05 <0.05
La 0.36 <0.05 <0.05 Mo <0.05 0.36 <0.05
Ca 0.28 0.35 0.23 Zn <0.05 0.21 0.16
Cu <0.05 0.87 <0.05
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ICP-OES法测定三元正极材料中19种微量元素含量
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李宇升 , 韩小龙 , 李军 , 孙硕 , 姜晓娜 , 孙凯
汽车工艺与材料 | 视界 2025,(2): 6-10
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汽车工艺与材料 | 视界 2025, (2): 6-10
ICP-OES法测定三元正极材料中19种微量元素含量
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李宇升, 韩小龙, 李军, 孙硕, 姜晓娜, 孙凯
作者信息
  • 中国第一汽车股份有限公司研发总院， 长春 130013

    • 李宇升（1994—），男，工程师，硕士学位，研究方向为化学工程。

Determination of 19 Trace Elements in Ternary Cathode Materials by ICP-OES
Yusheng Li, Xiaolong Han, Jun Li, Shuo Sun, Xiaona Jiang, Kai Sun
Affiliations
  • Global R&D Center, China FAW Corporation Limited, Changchun 130013
出版时间: 2025-02-20 doi: 10.19710/J.cnki.1003-8817.20240141
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摘要
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锂离子电池三元正极材料中的微量元素直接影响电池性能，为准确测定其元素含量，利用电感耦合等离子体发射光谱（ICP-OES）法，建立了同时测定锂离子电池三元正极材料中铌、硼、锆、锶、钽、钛、铱、镧、钙、铜、铁、钾、镁、磷、钠、铝、铬、钼、锌共19种微量元素的分析方法。考察了不同溶剂对三元正极材料中微量元素含量测定的影响，最终确定最佳样品溶剂。结果表明：该方法简便、快捷，有良好的分析重复性和可靠性，各元素的相对标准偏差为0.58%~3.56%，回收率为91.81%~104.91%，满足三元正极材料微量元素含量分析的需要。

电感耦合等离子体原子发射光谱法  /  锂电池  /  三元正极  /  微量元素

In the lithium-ion battery ternary anode materials, trace elements affect the battery performance directly, in this study, an analytical method for simultaneous determination of 19 trace elements including Nb, B, Zr, Sr, Ta, Ti, Y, La, Ga, Cu, Fe, K, Mg, P, Na, Al, Cr, Mo and Zn in ternary anode materials of lithium ion batteries is established by inductively coupled plasma emission spectrometry. The influence of different solvents on the determination of trace elements in ternary anode materials is investigated, and the best sample solvent is determined. The results show that the method is simple, rapid, and has good repeatability and reliability. The relative standard deviation of each element is 0.58%~3.56%, and the recovery is 91.81%~104.91%, which can fully meet the needs of trace element content analysis of ternary cathode materials.

ICP-OES  /  Lithium-ion battery  /  Ternary cathode  /  Trace element
李宇升, 韩小龙, 李军, 孙硕, 姜晓娜, 孙凯. ICP-OES法测定三元正极材料中19种微量元素含量. 汽车工艺与材料, 2025 , (2) : 6 -10 . DOI: 10.19710/J.cnki.1003-8817.20240141
Yusheng Li, Xiaolong Han, Jun Li, Shuo Sun, Xiaona Jiang, Kai Sun. Determination of 19 Trace Elements in Ternary Cathode Materials by ICP-OES[J]. Automobile Technology & Material, 2025 , (2) : 6 -10 . DOI: 10.19710/J.cnki.1003-8817.20240141
正文
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1 前言
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近年来，新能源汽车凭借其环保、节能、智能等诸多优势，越来越受到消费者的青睐。得益于新能源汽车的旺盛需求，特别是新能源汽车对更高续航里程的需求，三元锂电池成为当下应用最广泛的新能源汽车动力电池之一[1]。作为三元锂电池关键材料的锂层状氧化物（LiNi1-x-yCoxMnyO2）正极材料，其优劣直接影响电池的各项性能指标[2]，其中，微量元素的影响不可忽略。
三元正极材料中的微量元素主要由异质掺杂元素和有害杂质元素组成[3]，这些元素的存在对正极材料的晶格结构、电化学性能和电池安全性影响很大[4-5]。一方面，为提升电池性能、降低成本，常掺杂异质元素，目前，研究人员已经使用不少于46种元素对正极材料进行改性，可使正极材料获得更高的能量密度[4]，但掺杂元素的含量需要严格控制；另一方面，有研究表明，部分杂质元素（铁、锌、铬等元素）的引入会导致电池隔膜刺穿，加快自放电速度[6]，该类杂质元素的含量越低越好。因此，精准高效测定三元正极材料中的微量元素含量对三元锂电池的生产研发与质量控制具有重要意义。近年来，已有关于三元正极材料中微量元素含量测定的报道，但随着技术的不断发展，电池材料涉及的元素也越来越多，如Zr、V、Nb、La等逐渐受到关注[5]，这些元素的测试方法有待进一步探究。
传统的元素测定方法有重量法、滴定法等，其分析时间长、工作量大，测定结果可靠性易受操作误差影响[7]。电感耦合等离子体发射光谱（Inductively Coupled Plasma Atomic Emission Spectrometry，ICP-AES）法能够同时测定多元素和多谱线，过程简单，测试周期大幅缩短，同时消除了样品前处理差异对测定结果的影响，提高了测定可靠性，非常适合锂电池材料的多元素含量测定。因此，本文利用电感耦合等离子体发射光谱法同时测定三元正极材料中19种微量元素。
2 试验部分
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2.1 仪器与试剂
2.1.1 仪器设备
试验仪器包括：控温电热板；ME235S型分析天平（德国Sartorius公司）；Avio200型电感耦合等离子体发射光谱仪（Inductively Coupled Plasma Optical Emission Spectrometer，ICP-OES）（美国Perkin Elmer）。
2.1.2 试剂
试验试剂包括：浓度为1 000 μg/mL的铌、硼、锆、锶、钽、钛、铱、镧、钙、铜、铁、钾、镁、磷、钠、铝、铬、钼、锌标准储备溶液（国家钢铁材料测试中心）；浓盐酸、浓硝酸均为分析纯；试验用水为去离子水；浓盐酸与浓硝酸按体积比3∶1混合均匀所得的王水；浓盐酸与浓硝酸按体积比1∶3混合均匀所得的逆王水；盐酸（体积分数2%）。
2.2 标准溶液配制
2.2.1 混合标准溶液配制
分别取5.00 mL铌、硼、锆、锶、钽、钛、铱、镧、钙、铜、铁、钾、镁、磷、钠、铝、铬、钼、锌的标准储备溶液，置于100 mL容量瓶中，用盐酸（2+98）稀释至刻度，充分混匀，所得的溶液中铌、硼、锆、锶、钽、钛、铱、镧、钙、铜、铁、钾、镁、磷、钠、铝、铬、钼、锌元素浓度均为50 μg/mL。
2.2.2 标准溶液配制
分别取0.1 mL、0.4 mL、1.0 mL、4.0 mL、10.0 mL混合标准溶液，置于100 mL容量瓶中，用盐酸（2+98）稀释至刻度，充分混匀，得到0.05 μg/mL、0.2 μg/mL、0.5 μg/mL、2 μg/mL、5 μg/mL系列标准溶液。
2.3 样品前处理
称取0.2 g（精度为0.000 1 g）三元正极材料样品放入50 mL聚四氟乙烯烧杯中，加入20 mL逆王水，置于控温电热板上150 ℃低温加热溶解，加热30 min后黄烟冒尽，取下烧杯冷却至室温，过滤后转移至100 mL容量瓶中，用盐酸（体积分数2%）稀释至刻度，混匀待测。
2.4 谱线选择和仪器工作条件
综合考虑待测元素谱线的强度、信噪比及谱线干扰等因素，ICP-OES的工作条件和各元素分析谱线选择如表1所示，每条分析谱线测量3次。
3 结果与讨论
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3.1 样品溶剂选择
三元正极材料中微量元素的种类较多，其中Nb、Ta等元素较难溶解。为达到最佳溶解效果，称取0.2 g三元正极材料若干份，在其他条件相同的情况下，分别使用浓盐酸、浓硝酸、王水和逆王水进行溶解，试验结果如图1所示。由图1可知，单独使用浓盐酸或浓硝酸溶解样品时，溶液中留有黑色残余，王水和逆王水溶解样品均可得到澄清溶液，逆王水作为溶剂测得的元素回收率优于王水，在4种溶剂中溶解效果最好。
3.2 标准工作曲线
采用外标法，按照2.4节中选择的谱线和仪器工作条件分别测定2.2节中的系列标准溶液，以测得的目标元素的光谱强度为纵坐标，目标元素的浓度为横坐标，绘制标准工作曲线，如表2所示，工作曲线的相关系数r的范围为0.999 5~0.999 9，表明19种微量元素含量在0.05~5.00 μg/mL范围内呈现良好的线性关系。
3.3 加标回收率
按照2.3节试验方法处理某三元正极材料，三元正极材料中各微量元素含量如表3所示。在0.08 μg/mL、1 μg/mL和5 μg/mL的加标浓度下，对所得溶液的19种元素进行加标回收率测定，结果如表4所示。由表4可知，根据测试结果计算得到的加标回收率范围为91.81%~104.91%，相对标准偏差为0.58%~3.56%。试验结果表明，用本研究方法处理样品测定三元材料中的19种微量元素能获得理想的准确度和良好的精密度。
3.4 重复性
为评价该方法的可靠性，分别在0.1 μg/mL、2.0 μg/mL的加标浓度下检测日内（一天内，每个浓度的试验重复3次）重现性，试验结果如表5所示。由表5可知，日内测定的相对标准偏差（Relative Standard Deviation，RSD）为0.76%~3.98%，表明该方法具有良好的重现性。由于三元正极材料微量元素的含量较低，样品需要当日处理当日检测，避免前处理过程带来误差，因此，本文未探究日间重复性。
3.5 样品分析
为验证该方法的通用性，选择3种不同三元正极材料测定各样品的微量元素含量，结果如表6所示，结果表明，该方法能够满足三元正极材料微量元素的测定要求。
4 结束语
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本研究通过考察合理的溶样方式，选择恰当的分析谱线，建立了电感耦合等离子体发射光谱法同时测定锂离子电池三元正极材料中19种微量元素的分析方法。该方法具有良好的精密度、重现性及令人满意的回收率，证明该方法可行、有效，能够满足三元正极材料微量元素分析的需要。
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doi: 10.19710/J.cnki.1003-8817.20240141
  • 首发时间：2025-11-12
  • 出版时间：2025-02-20
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    中国第一汽车股份有限公司研发总院， 长春 130013
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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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