CN113707848A - 一种全氟硅烷偶联剂修饰的Li负极制备方法 - Google Patents
一种全氟硅烷偶联剂修饰的Li负极制备方法 Download PDFInfo
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- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000007822 coupling agent Substances 0.000 title description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 19
- MLXDKRSDUJLNAB-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F MLXDKRSDUJLNAB-UHFFFAOYSA-N 0.000 claims abstract description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 7
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- 239000011241 protective layer Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 3
- 229910006709 Li—O—Si Inorganic materials 0.000 abstract description 3
- 229910052731 fluorine Inorganic materials 0.000 abstract description 3
- 239000011737 fluorine Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
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- SMBQBQBNOXIFSF-UHFFFAOYSA-N dilithium Chemical compound [Li][Li] SMBQBQBNOXIFSF-UHFFFAOYSA-N 0.000 description 7
- 238000007599 discharging Methods 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical group FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供的一种全氟硅烷偶联剂修饰的Li负极制备方法，属于锂金属电池负极保护技术领域，先在四氢呋喃中加入1～10wt％的1H,1H,2H,2H‑全氟癸基三乙氧基硅烷，搅拌均匀后获得混合溶液；再将Li片完全浸入混合溶液中静置反应30min；取出反应后的Li片，经烘干得到全氟硅烷偶联剂修饰的Li负极。本发明利用1H,1H,2H,2H‑全氟癸基三乙氧基硅烷的分子自发组装特性，在Li片表面形成Li‑O‑Si共价键连接的致密保护层，并与SEI层通过化学键和物理缠绕效应连接，增强SEI层与Li片的粘附性；保护层中的含氟官能团能分解形成LiF，有助形成致密SEI层，提高SEI层稳定性和电池长循环性能。
Description
技术领域
本发明涉及锂金属电池负极保护技术领域，具体而言，涉及一种全氟硅烷偶联剂修饰的Li负极制备方法。
背景技术
锂金属电池(LMB)因其高比容量(3862mAh g-1)和低还原电位(3.04V vs.SHE(标准氢电极)而受到研究人员广泛关注。然而，锂(Li)金属在非水溶剂中的热力学性能不稳定，会连续与电解质发生反应，直到Li金属表面被固体电解质中间相(SEI)层钝化。在电镀/剥离Li的过程中，SEI层会因界面波动而导致机械性能不稳定，不断开裂和重组，并在SEI层开裂和重组的过程中不断消耗负极的Li和电解质，导致Li的不均匀沉积。更糟糕的是，不均匀的Li沉积造成的裂隙和不规则突起会诱发Li枝晶的生长，造成电池容量的快速衰退，留下安全隐患。
SEI层的失效除了与电极的异质体积收缩产生裂纹后无机层的重新溶解，以及放电过程中用于电解液还原的自由基的缺乏有关，还与SEI层和Li片之间的化学粘附性差有关。因而，构筑稳定且坚固的SEI层是实现安全、无枝晶和长寿命的LMB的关键因素。SEI层的稳定性与SEI的组分密切相关，此前已有现有技术表明FEC(氟代碳酸乙烯酯)在负极表面分解形成LiF有助于提高SEI层稳定性(Understanding the thermal instability offluoroethylene carbonate in LiPF6-based electrolytes for lithium ionbatteries,Electrochimica Acta 225(2017)358–368,KoeunKim,Inbok Park,Se-YoungHa,Yeonkyoung Kim,Myung-Heuio Woo,Myung-Hwan Jeong,Woo Cheol Shin,Makoto Ue,Sung You Hong,Nam-Soon Choi)，因此具有高机械强度、低溶解度、宽带隙和高电压窗口特性的LiF，是构成稳定致密的SEI层的重要无机组分之一。并且富含LiF的SEI层在Li+传输方面也具有优势，可以有效调节Li+通量，促进Li+均匀沉积。因而，一些含氟的物质可以在电池充放电的过程中促进富含LiF的致密SEI层的形成，提高SEI层的稳定性，抑制枝晶的生长，提升电池循环稳定性。
发明内容
针对现有技术中存在的缺陷和不足，本发明提供一种全氟硅烷偶联剂修饰的Li负极制备方法，利用1H,1H,2H,2H-全氟癸基三乙氧基硅烷在Li负极表面形成保护层，有助于构筑坚固稳定的SEI层，提高库伦效率，提升长循环稳定性。
本发明的技术方案如下：
一种全氟硅烷偶联剂修饰的Li负极制备方法，其特征在于，包括以下步骤：
步骤1：在四氢呋喃(THF)中加入1wt％～10wt％的1H,1H,2H,2H-全氟癸基三乙氧基硅烷，搅拌均匀后获得混合溶液；
步骤2：将Li片完全浸入混合溶液中静置反应30min；
步骤3：取出反应后的Li片，经烘干得到全氟硅烷偶联剂修饰的Li负极。
进一步地，步骤1中搅拌时间为30min。
进一步地，步骤3中烘干的温度不高于60℃。
进一步地，在所述全氟硅烷偶联剂修饰的Li负极中，Li片与1H,1H,2H,2H-全氟癸基三乙氧基硅烷自发形成的保护层之间以Li-O-Si的共价键连接。
本发明还提出了一种上述全氟硅烷偶联剂修饰的Li负极在锂金属电池中的应用。
本发明的有益效果为：
1、本发明提出了一种全氟硅烷偶联剂修饰的Li负极制备方法，通过将Li片浸入含有1H,1H,2H,2H-全氟癸基三乙氧基硅烷的混合溶液中，利用1H,1H,2H,2H-全氟癸基三乙氧基硅烷的分子自发组装特性，在Li片表面形成与其以Li-O-Si的共价键连接的致密的保护层，同时保护层与电池充放电过程中形成的SEI层通过化学键和物理缠绕效应连接，进而有效增强SEI层与Li片之间的化学粘附性，以构筑坚固稳定的SEI层；
2、1H,1H,2H,2H-全氟癸基三乙氧基硅烷自发形成的保护层中具有含氟官能团(-CFx)，在电池充放电过程中分解形成LiF，有助于形成致密的SEI层，在提高SEI层稳定性的同时提高电池长循环性能。
附图说明
图1为本发明实施例2所得全氟硅烷偶联剂修饰的Li负极与未修饰的纯Li负极的SEM对比图；其中，图1(a)和图1(c)分别为本发明实施例2所得全氟硅烷偶联剂修饰的Li负极的平面SEM图和斜面SEM图，图1(b)和图1(d)分别为未修饰的纯Li负极的平面SEM图和斜面SEM图；
图2为本发明实施例2所得全氟硅烷偶联剂修饰的Li负极与未修饰的纯Li负极的XPS对比图；其中，图2(a)为本发明实施例2所得全氟硅烷偶联剂修饰的Li负极的XPS图，图2(b)为未修饰的纯Li负极的XPS图；
图3为分别采用本发明实施例2所得全氟硅烷偶联剂修饰的Li负极和未修饰的纯Li负极组装锂-锂对称电池的长循环性能对比图。
具体实施方式
下面结合附图和实施例，详述本发明的技术方案。
实施例1
本实施例提供一种全氟硅烷偶联剂修饰的Li负极制备方法，其制备过程如下：
步骤1：取5mL四氢呋喃至烧杯中，加入56uL(1wt％)的1H,1H,2H,2H-全氟癸基三乙氧基硅烷，搅拌30min后获得混合溶液；
步骤2：将商用的Li片完全浸入混合溶液中静置反应30min；
步骤3：取出反应后的Li片，放在60℃加热台上烘干6h，得到全氟硅烷偶联剂修饰的Li负极。
实施例2
按照实施例1的步骤制备全氟硅烷偶联剂修饰的Li负极，仅将步骤1中加入的1H,1H,2H,2H-全氟癸基三乙氧基硅烷的量调整为280uL(5wt％)；其他步骤不变。
实施例3
按照实施例1的步骤制备全氟硅烷偶联剂修饰的Li负极，仅将步骤1中加入的1H,1H,2H,2H-全氟癸基三乙氧基硅烷的量调整为556uL(10wt％)；其他步骤不变。
将本发明实施例2所得全氟硅烷偶联剂修饰的Li负极与未修饰的纯Li负极分别组装锂-锂对称电池，进行相关表征和长循环稳定性能测试，具体如下：
两个锂-锂对称电池在以1mA充放电且充电容量为1mAh的情况下进行充放电五次之后，对其中的Li负极进行SEM测试，由图1所示的SEM对比图可知，本发明实施例2所得全氟硅烷偶联剂修饰的Li负极相比于未修饰的纯Li负极，在锂-锂对称电池充放电过程中，沉积的Li更加均匀致密，表明形成的SEI层坚固而稳定，能有效抑制Li枝晶的生长。
两个锂-锂对称电池在以1mA充放电且充电容量为1mAh的情况下进行充放电五次之后，对形成的SEI层进行XPS测试，由图2所示的XPS对比图可知，本发明实施例2所得全氟硅烷偶联剂修饰的Li负极形成的SEI层相比于未修饰的纯Li负极，SEI层中LiF的相对峰强度明显增大，表明1H,1H,2H,2H-全氟癸基三乙氧基硅烷有助于提升SEI层中LiF含量，进而提高SEI层的稳定性。
将本发明实施例2所得全氟硅烷偶联剂修饰的Li负极组装的锂-锂对称电池与未修饰的纯Li负极组装的锂-锂对称电池，在以1mA充放电且充电容量为1mAh的情况下进行长循环稳定性能测试，结果如图3所示，本发明实施例2所得全氟硅烷偶联剂修饰的Li负极组装的锂-锂对称电池相比于未修饰的纯Li负极，可以实现稳定循环1000h以上，具有稳定的Li电镀/剥离性能，表明全氟硅烷偶联剂修饰的Li负极能够更有效地固定SEI层，实现更稳定Li电镀/剥离性能。
Claims (3)
1.一种全氟硅烷偶联剂修饰的Li负极制备方法，其特征在于，包括以下步骤：
步骤1：在四氢呋喃中加入1～10wt％的1H,1H,2H,2H-全氟癸基三乙氧基硅烷，搅拌均匀后获得混合溶液；
步骤2：将Li片完全浸入混合溶液中静置反应30min；
步骤3：取出反应后的Li片，经烘干得到全氟硅烷偶联剂修饰的Li负极。
2.根据权利要求1所述全氟硅烷偶联剂修饰的Li负极制备方法，其特征在于，步骤3中烘干的温度不高于60℃。
3.一种如权利要求1所述制备方法制得的全氟硅烷偶联剂修饰的Li负极在锂金属电池中的应用。
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