CN116722098A - 一种全生命周期持续补锂的复合负极 - Google Patents
一种全生命周期持续补锂的复合负极 Download PDFInfo
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- CN116722098A CN116722098A CN202310618317.0A CN202310618317A CN116722098A CN 116722098 A CN116722098 A CN 116722098A CN 202310618317 A CN202310618317 A CN 202310618317A CN 116722098 A CN116722098 A CN 116722098A
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- lithium
- negative electrode
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 178
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 177
- 239000002131 composite material Substances 0.000 title claims abstract description 79
- 230000001502 supplementing effect Effects 0.000 title claims abstract description 45
- 238000003860 storage Methods 0.000 claims abstract description 44
- 239000007773 negative electrode material Substances 0.000 claims abstract description 24
- 230000000694 effects Effects 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- 239000011888 foil Substances 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 229910002804 graphite Inorganic materials 0.000 claims description 19
- 239000010439 graphite Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 16
- 239000010405 anode material Substances 0.000 claims description 13
- 239000002482 conductive additive Substances 0.000 claims description 12
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- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 4
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- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
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- GBVSONMCEKNESD-UHFFFAOYSA-N 1,1'-biphenyl;lithium Chemical group [Li].C1=CC=CC=C1C1=CC=CC=C1 GBVSONMCEKNESD-UHFFFAOYSA-N 0.000 claims description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
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- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical group [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 3
- PDZGAEAUKGKKDE-UHFFFAOYSA-N lithium;naphthalene Chemical compound [Li].C1=CC=CC2=CC=CC=C21 PDZGAEAUKGKKDE-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- BHZCMUVGYXEBMY-UHFFFAOYSA-N trilithium;azanide Chemical compound [Li+].[Li+].[Li+].[NH2-] BHZCMUVGYXEBMY-UHFFFAOYSA-N 0.000 claims description 3
- 238000009736 wetting Methods 0.000 claims description 3
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 claims description 2
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 2
- 229910000676 Si alloy Inorganic materials 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
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- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 2
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 2
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- 229910003002 lithium salt Inorganic materials 0.000 claims description 2
- 159000000002 lithium salts Chemical class 0.000 claims description 2
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- 229910052711 selenium Inorganic materials 0.000 claims description 2
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- 229910021384 soft carbon Inorganic materials 0.000 claims description 2
- 229910052596 spinel Inorganic materials 0.000 claims description 2
- 239000011029 spinel Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 235000019322 gelatine Nutrition 0.000 description 1
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- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- DEUISMFZZMAAOJ-UHFFFAOYSA-N lithium dihydrogen borate oxalic acid Chemical compound B([O-])(O)O.C(C(=O)O)(=O)O.C(C(=O)O)(=O)O.[Li+] DEUISMFZZMAAOJ-UHFFFAOYSA-N 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- MCVFFRWZNYZUIJ-UHFFFAOYSA-M lithium;trifluoromethanesulfonate Chemical compound [Li+].[O-]S(=O)(=O)C(F)(F)F MCVFFRWZNYZUIJ-UHFFFAOYSA-M 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
本发明涉及一种全生命周期持续补锂的复合负极,包括以下原料:高电位的负极材料,低电位的负极材料,补锂剂;其中高电位的负极材料,低电位的负极材料,补锂剂的用量通过以下公式计算得到:补锂剂用量=(2‑复合负极首效)*锂存储率*电芯容量+(1‑复合负极首效)*电芯容量*A;其中锂存储率定义为补锂剂补充首圈活性锂损失后剩余锂相对于电芯容量的百分比;0<锂存储率≤60%;A为1‑1.2。本发明提出的全电池在全生命周期循环中均可实现缓释补锂,具有更加优异的循环性能;制备工艺简单,材料易得,适合大规模生产。
Description
技术领域
本发明属于电池领域,具体涉及一种全生命周期持续补锂的复合负极。
背景技术
在新能源电池领域,随着人们对能量密度的需求,电池体系从最早的铅酸电池、镍铬、镍氢电池到目前成熟发展的以石墨为负极的锂离子电池,在能量密度上已经有了巨大的提升,但随着动力汽车的发展,以及市场对于更轻薄的3C产品的需求,以石墨为负极的锂离子电池开始无法满足能量密度的需求。
目前,负极材料经过今年的大力研发,其性能已经取得了长足的进步,目前对于负极材料是包括高能量密度、高功率密度、高循环性能、低成本在内的综合性能的要求。最受关注的是具有更好能量密度的锂金属负极以及硅基负极,其中,硅基负极凭借其高容量,较好的循环稳定性开始走向应用,硅基与石墨的混合体系开始走向大众的视野,然而,针对硅基和石墨复合的复合负极,由于两者之间具有不同的锂化电位以及不尽相同的物理化学性质,在复合后会表现出与单颗粒不同的锂化机理与锂化行为。
由于硅基材料在首圈的库伦效率低,在应用过程中,通常需要对含硅负极进行预锂化处理。针对预锂化的研究已获诸多报道,例如:利用电位较低的化学预锂化试剂例如萘锂、联苯锂等,利用高压分解的方法在正极侧加入氧化锂、氮化锂等,利用电化学预锂的方法等。然而,对于长循环电池体系而言,由于硅的体积膨胀,会使SEI持续形成,以及在电池工作过程中,对电解液也会有持续的分解,因此需要对电池体系提供一个持续补锂的锂源。而硅凭借其高的理论比容量,以及先前我们在锂化机理中探究得到的结论,存储锂主要储存在动力学差的硅之中。
CN115732634A公开了一种负极补锂极片,其实将PTFE微粉喷涂于锂箔,在高温和保护气体条件下发生原位反应,生成复合层,将PTFE微粉和金属锂箔形成的复合层通过辊压和负极片表面复合得到补锂负极。CN113921747A公开了制备补锂负极的方法以及补锂负极,是将未压实的负极和超薄锂箔或锂合金箔辊压得到预成型的补锂负极,其中所述超薄锂箔或锂合金箔与所述未压实的负极活性材料层接触;和2)二次辊压步骤:将所述预成型的补锂负极再一次辊压以将其厚度减小10%至30%,得到补锂负极。CN115642228A公开了一种制备预锂化负极的方法,包括:步骤一:将负极和超薄锂箔或锂合金箔通过压力复合得到补锂负极,所述超薄锂箔或锂合金箔的厚度为1-50μm;步骤二:将补锂负极用电解液浸泡,得到预锂化负极;步骤三:将预锂化负极用溶剂清洗;步骤四:将清洗后的预锂化负极烘干,得到成品预锂化负极。但是上述专利涉及的均是针对于首圈的补锂预锂方式,无法做到全生命周期持续补锂以达到优异的循环稳定性。但是并不是简单过量补锂就可以实现在全生命周期补锂的情况,因为锂过量的情况下会导致析锂等一系列问题,本发明针对全电池循环过程中会有持续性的锂损耗的问题,利用高容量负极活性材料在储锂过程中结构稳定的特性,利用电位差在活化过程将锂存储在高电位区域,在循环过程中持续进行锂补充且弥补负极损失容量,这种复合负极的构筑可以大幅提高高能量密度锂离子电池的循环寿命。
发明内容
本发明提供了一种全生命周期持续补锂的复合负极,所述全电池通过高电位的负极材料和低电位负极材料构成的复合负极,配合补锂活性物质按照一定比例规律构建锂离子电池,负极材料之间存在一定的电位差,高电位的负极材料在循环中既可发挥高的容量,又可满足电池在生命周期内缓释锂,低电位的负极材料具有优异的循环性能;补锂添加剂可通过加入量控制负极的含锂量。本发明提供的全生命周期持续补锂全电池的优点在于制备技术简单,原料易得,兼具高能量密度和长循环优势,有极高的实用化和规模化前景。
本发明通过以下技术方案实现上述目的:
一种全生命周期持续补锂的复合负极,包括以下原料:高电位的负极材料,低电位的负极材料,补锂剂;其中高电位的负极材料,低电位的负极材料,补锂剂的用量通过以下公式计算得到:补锂剂用量=(2-复合负极首效)*锂存储率*电芯容量+(1-复合负极首效)*电芯容量*A;
其中锂存储率定义为补锂剂补充首圈活性锂损失后剩余锂相对于电芯容量的百分比(锂存储率=补锂剂存储锂容量/电芯容量);即补锂剂容量=(2-复合负极首效)*锂存储率*电芯容量+(1-复合负极首效)*电芯容量*A;0<锂存储率≤60%;A为1-1.2。
优选地,5%<锂存储率≤40%;A为1.05-1.1。
所述高电位的负极材料特性在于平均锂化电压高,容量高,选自氧化亚硅,纳米硅、硅碳复合材料、硅合金中的至少一种;所述低电位的负极材料特性在于锂化平均电压低,循环稳定性好,选自石墨,硬碳,软碳中的至少一种;所述补锂剂选自锂单质、无机锂、有机锂中的至少一种;进一步地,所述锂单质选自锂箔、锂粉;所述无机锂盐选自氧化锂,过氧化锂,草酸锂,氮化锂等;所述有机锂选自联苯锂,萘锂等。
本发明进行精确补锂的策略如下
一、首先根据所需设计的电芯能量密度,得到复合负极的质量,根据公式:电芯能量密度=平均电压*容量/(正极质量+负极质量+其余各组分总质量)。对于某一能量密度的电芯进行调控时:通过设计的电芯能量密度,可以得到负极的质量。
二、根据不同能量密度下所需的存储锂容量,得到复合负极的容量:复合负极容量=电芯容量*A+存储锂容量;一般在电池设计时,为了防止析锂,负极容量会比正极稍微过量,即A>1。按照公式,复合负极的容量只与存储锂容量有关,变化存储锂的容量主要改变的是复合负极的容量。
三、利用复合负极容量得到高电位的负极材料和低电位的负极材料之间的比例,比如对于复合负极材料为石墨和硅基材料(氧化亚硅)而言,复合负极容量/负极质量=石墨比容量*石墨质量占比+硅基材料比容量*硅基材料质量占比。因此根据复合负极的容量,可以计算出石墨和硅的质量占比。
四、最后根据公式得到补锂剂容量:
补锂剂的容量=存储锂容量+负极首圈不可逆的锂损耗;
负极首圈不可逆的锂损耗=(1-复合负极首效)*复合负极容量;
补锂剂的容量为设计存储锂容量以及不同比例下复合负极的首效相关根据上述策略,复合负极可针对不同能量密度需求,通过存储锂容量的设计,并基于此改变复合负极的质量占比及补锂剂容量来得到一款可在全电池循环过程中持续锂补充的复合负极。通过精准控制补锂剂用量,和复合负极中高电位负极材料与低电位负极材料的配比相配合,达到了在锂离子电池全生命周期中持续补锂,显著提高了复合负极电化学性能,特别是循环稳定性。本发明提供的全生命周期持续补锂的复合负极可以防止正极发生过充:主要原因是在全电池后续循环中,活性锂损耗会导致负极低电压区在锂化过程没有足够的锂进行锂化,会导致负极电压上升,从而出现正极过充的现象。
本发明所述全生命周期持续补锂的复合负极还包括以下原料:导电添加剂,粘结剂,溶剂,集流体。
其中导电添加剂,粘接剂,溶剂,集流体的种类和用量为本领域所熟知。在本发明具体实施方式中,导电添加剂为Super P、科琴黑、石墨烯、导电碳纳米管中的一种或几种;所述粘结剂为聚偏二氟乙烯(PVDF),羧甲基纤维素钠(CMC),丁苯橡胶/羧甲基纤维素钠(CMC/SBR)、海藻酸钠(SA)、明胶中的一种或几种;所述溶剂为N-甲基吡咯烷酮、水、乙醇中的一种或几种;所述集流体选自平板铜箔、涂炭铜箔、三维铜箔集流体的一种或几种。
在复合负极中,高电位的负极材料和低电位的负极材料的总和占负极材料质量的70-99%,优选90-95%。
本发明第二个目的是提供上述全生命周期持续补锂的复合负极的制备方法,包括以下步骤:将高电位的负极材料,低电位的负极材料与导电添加剂,粘结剂和溶剂研磨混合,制成浆料,浆料涂覆在集流体表面,用电解液润湿,加入补锂剂。优选地,补锂剂为锂箔时,通过机械辊压机、热平压机或冷平压机将锂箔负载于集流体表面。具体是将超薄金属锂箔整体覆盖于用电解液润湿的负极表面,使用液压平衡电动对辊及将金属锂滚压至与基底材料紧密贴合,保持含锂复合负极表面平整且金属锂不脱落。
本发明第三个目的是提供一种全生命周期持续补锂的全电池,包括正极,负极,电解液,隔膜;所述负极为上述复合负极。
所述电解液溶剂选自碳酸二甲酯、碳酸二乙酯、碳酸乙烯酯、碳酸丙烯酯、1,3二氧戊环、四氢呋喃、二甲基四氢呋喃、乙二醇二甲醚、二乙二醇二甲醚等中的一种或几种;优选地,所述电解液溶质为三氟甲基磺酸锂、双(三氟甲基磺酸)亚胺锂、六氟磷酸锂、四氟硼酸锂、二草酸硼酸锂中的一种或几种。所述隔膜材料选自聚乙烯、聚丙烯、羟甲基纤维素、醋酸纤维素中的一种或几种。所述正极选自层状氧化物正极、尖晶石正极、聚阴离子型正极、有机正极、硫正极、硒正极、氟化物正极、无锂金属氧化物正极、无锂金属硫化物等中的一种或几种。
本发明还提出全电池的设计策略:
(1)正极为有锂正极时:复合负极容量大于正极循环容量加存储锂容量;金属锂容量等于存储锂容量加首圈不可逆的锂损耗。优选地,复合负极容量=正极循环容量*1.05+存储锂的容量。优选地,存储锂容量为正极容量的5%-40%。
(2)正极为无锂正极时:复合负极容量大于正极循环容量加存储锂容量;金属锂容量等于存储锂容量加首圈不可逆的锂损耗加正极容量。优选地,复合负极容量=正极循环容量*1.05+存储锂的容量。优选地,存储锂容量为正极容量的5%-40%。
本发明提出的全电池设计策略,与现有技术相比具有如下优势:(1)相比于传统的全电池体系,本发明提出的全电池在全生命周期循环中均可实现缓释补锂,具有更加优异的循环性能;(2)相比于目前市面上的电池,由于更高比能的硅基活性物质的参与,其能量密度也具有显著的提升;(3)在全电池设计策略中,未牺牲能量密度换取循环性能;(4)兼容目前锂二次电池的工艺;(5)制备工艺简单,材料易得,适合大规模生产。
附图说明
图1是全周期补锂全电池中复合负极的设计;
图2是实施例1所得全周期补锂全电池的电化学性能循环图;
图3是对比例1电池循环1000圈后复合负极中氧化亚硅的SEM图;
图4是实验例1电池循环1000圈后复合负极中氧化亚硅的SEM图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
下述实施例中所述实验方法,如无特殊说明,均为常规方法;所述试剂和材料均可从商业途径获得。
图1是本发明全周期补锂全电池中复合负极的设计。
实施例1
(一)40%储锂复合负极的制备
步骤1)根据含锂复合负极的制备策略对石墨、氧化亚硅的质量占比及补锂剂的量进行计算,根据电芯能量密度设计:电芯面容量为4mAh/cm2,电芯容量/负极质量=500mAh/g。因此根据公式:石墨比容量*石墨质量占比+氧化亚硅比容量*氧化亚硅质量占比=(电芯容量+存储锂容量)/负极质量=700mAh/g,得到石墨质量占比为67%,氧化亚硅质量占比为33%,首先对复合负极涂布,将石墨、氧化亚硅、导电添加剂Super P、聚丙烯酸(PAA)按质量比6.4:3.1:0.25:0.25,面载为5.6mAh/cm2,60℃真空干燥24小时。
步骤2)对负极进行一次辊压,并用电解液润湿。
步骤3)计算补锂剂用量,根据公式:补锂剂容量=(2-复合负极首效)*存储率*电芯容量+(1-复合负极首效)*电芯容量,得到所需补锂剂的面容量为2.7mAh/cm2,对应锂箔为14μm,将14μm金属锂箔覆盖在步骤2)得到的负极片表面,然后用对辊装置进行二次辊压,得到含锂复合负极。
步骤4)将NCM811、导电添加剂Super P、聚偏二氟乙烯(PVDF)按质量比为9.5:0.25:0.25混合,加入N-甲基吡咯烷酮(NMP)打浆涂布到铝集流体上,正极面载为4mAh/cm2,60℃真空干燥24小时。
步骤5)高纯氩气下,在正极侧滴加溶剂为碳酸乙烯酯,碳酸二甲酯,碳酸二乙酯(v/v/v=1:1:1),溶质为六氟磷酸锂(摩尔浓度为1M)的电解液,随后按顺序加入Celgard隔膜,步骤3)得到的复合负极,在电池壳中依次按顺序叠放。将上述电池壳完全密封,进行电池性能测试。
(二)金属锂电池性能测试
在电池测试系统中测试电池的电化学性能。测试温度为25℃,电池容量和充放电电流均以NCM811的质量计算。记录其首圈库伦效率,500圈后的容量保持率以及库伦效率(图1),测试结果列于表1。
实施例2
5%储锂复合负极的制备及在锂离子电池中的应用
其他条件与实施例1相同,不同之处为步骤1)中石墨、氧化亚硅、导电添加剂SuperP、聚丙烯酸(PAA)按质量比8:1.5:0.25:0.25,面载为4.2mAh/cm2,步骤3)中金属锂箔为5μm(1.0mAh/cm2)。
实施例3
20%储锂复合负极的制备及在锂离子电池中的应用
其他条件与实施例1相同,不同之处为步骤1)中石墨、氧化亚硅、导电添加剂SuperP、聚丙烯酸(PAA)按质量比7.3:2.2:0.25:0.25,面载为4.8mAh/cm2,步骤3)中金属锂箔为8.5μm(1.7mAh/cm2)。
实施例4
60%储锂复合负极的制备及在锂离子电池中的应用
其他条件与实施例1相同,不同之处为步骤1)中石墨、氧化亚硅、导电添加剂SuperP、聚丙烯酸(PAA)按质量比5.5:4:0.25:0.25,面载为6.4mAh/cm2,步骤3)中金属锂箔为19μm(3.8mAh/cm2)。
对比例1
未储锂复合负极的制备及在锂离子电池中的应用
其他条件与实施例1相同,不同之处为步骤1)中石墨、氧化亚硅、导电添加剂SuperP、聚丙烯酸(PAA)按质量比8.3:1.2:0.25:0.25,负极面载为4.1mAh/cm2;步骤3)金属锂箔为3.5μm。
对比例2
其他条件与实施例1相同,不同之处为步骤3)中无金属锂箔辊压。
表1:实施例与对比例电化学性能
实施例1-4说明电池设计存在最佳比例,在锂存储为40%时循环最好,这表现在电池在500圈后的容量保持率最高。当补锂剂用量过多,会导致复合负极相对应的硅含量过高,极片体积膨胀过大,也不利于复合负极电化学性能的发挥。
实施例1和对比例1比较,说明补锂剂用量只用于补充首圈不可逆的活性锂损失,虽然提高了首效,但是对于锂离子电池在全生命周期运行中,容量保持率并不高。实施例1与对比例2对比,说明如果不进行补锂,由于硅基的存在,首圈库伦效率低,而且容量保持率也显著降低。合适的锂补充可用来前期氧化亚硅不可逆的锂损耗和固态电解质的形成,提高全电池首圈库伦效率和容量保持率。
图3和图4分别是对比例1和实验例1电池循环1000圈后复合负极中氧化亚硅的SEM图。可以看出,对比例1由于仅补充了首圈循环中不可逆损失的活性锂,在后续的锂离子电池全生命周期中,锂化过程没有足够的锂进行锂化,导致负极在完全放电状态下受到更大的应力,导致负极颗粒开裂严重。
综上所述,活性材料在循环中既可发挥高的容量,又可起到“锂储存室”的作用,防止金属锂的析出及在电池循环过程中缓释释锂;金属锂箔可通过厚度的调节控制负极的含锂量;通过全电池的设计策略,调控含锂复合负极中活性物质和锂的容量,可组装出长循环的高比能锂二次电池。用含锂复合负极组装的二次电池可以表现出优异的循环稳定性,能够满足高能量密度、长寿命、安全稳定等条件。
Claims (10)
1.一种全生命周期持续补锂的复合负极,其特征在于,包括以下原料:高电位的负极材料,低电位的负极材料,补锂剂;其中高电位的负极材料,低电位的负极材料,补锂剂的用量通过以下公式计算得到:补锂剂用量=(2-复合负极首效)*锂存储率*电芯容量+(1-复合负极首效)*电芯容量*A;
其中锂存储率定义为补锂剂补充首圈活性锂损失后剩余锂相对于电芯容量的百分比;0<锂存储率≤60%;A为1-1.2。
2.根据权利要求1所述的全生命周期持续补锂的复合负极,其特征在于,5%<锂存储率≤40%;A为1.05-1.1。
3.根据权利要求1所述的全生命周期持续补锂的复合负极,其特征在于,所述高电位的负极材料选自氧化亚硅,纳米硅、硅碳复合材料、硅合金中的至少一种;所述低电位的负极材料选自石墨,硬碳,软碳中的至少一种;所述补锂剂选自锂单质、无机锂、有机锂中的至少一种。
4.根据权利要求3所述的全生命周期持续补锂的复合负极,其特征在于,所述锂单质选自锂箔、锂粉;所述无机锂盐选自氧化锂,过氧化锂,草酸锂,氮化锂;所述有机锂选自联苯锂,萘锂。
5.根据权利要求1所述的全生命周期持续补锂的复合负极,其特征在于,复合负极还包括以下原料:导电添加剂,粘结剂,溶剂,集流体。
6.根据权利要求1所述的全生命周期持续补锂的复合负极,其特征在于,高电位的负极材料和低电位的负极材料的总和占负极材料质量的70-99%。
7.根据权利要求6所述的全生命周期持续补锂的复合负极,其特征在于,高电位的负极材料和低电位的负极材料的总和占负极材料质量的优选90-95%。
8.权利要求1-7任一项所述全生命周期持续补锂的复合负极的制备方法,其特征在于,包括以下步骤:将高电位的负极材料,低电位的负极材料与导电添加剂,粘结剂和溶剂研磨混合,制成浆料,浆料涂覆在集流体表面,用电解液润湿,加入补锂剂。
9.一种全生命周期持续补锂的全电池,包括正极,负极,电解液,隔膜;其特征在于,所述负极为全路要求1-7任一项所述复合负极。
10.根据权利要求9所述的全生命周期持续补锂的全电池,其特征在于,所述电解液溶剂选自碳酸二甲酯、碳酸二乙酯、碳酸乙烯酯、碳酸丙烯酯、1,3二氧戊环、四氢呋喃、二甲基四氢呋喃、乙二醇二甲醚、二乙二醇二甲醚等中的一种或几种;所述隔膜材料选自聚乙烯、聚丙烯、羟甲基纤维素、醋酸纤维素中的一种或几种;所述正极选自层状氧化物正极、尖晶石正极、聚阴离子型正极、有机正极、硫正极、硒正极、氟化物正极、无锂金属氧化物正极、无锂金属硫化物等中的一种或几种。
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