CN111370676B - 一种在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法 - Google Patents
一种在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法 Download PDFInfo
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Abstract
一种在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法,属于锂离子电池负极制备领域。包括:1)将钛源和氢氧化锂分散于去离子水中,得到混合液A;2)将高分子碳源分散于无水乙醇中,得到混合液B;3)将混合液B和混合液A混合,得到混合液C;4)将混合液C置于不锈钢槽体中,以铜箔作为阳极、不锈钢槽体作为阴极,采用液相等离子体氧化电源供电,在脉冲电压为700V~900V、频率为60Hz~1000Hz的条件下氧化3~8min,即可在铜箔表面形成三维多孔的碳掺杂钛酸锂复合涂层。本发明得到的碳掺杂钛酸锂涂层具有三维多孔的结构,有利于锂离子电池电解液的浸润,能够减少扩散传质的阻力。
Description
技术领域
本发明属于锂离子电池负极制备领域,具体涉及一种在铜箔表面原位生长三维多孔碳掺杂钛酸锂涂层的方法。
背景技术
钛酸锂材料(Li4Ti5O12,简称LTO)被认为是最有应用前景的负极材料之一。在Li+充放电的循环过程中基本没有体积上的变化,结构十分稳定,被称为“零应变”材料,使LTO表现出优异的循环性能和长寿命储能等优势。同时LTO的锂化电压平台在1.55V(Vs Li+/Li)左右,可以有效地抑制锂枝晶的形成,避免锂枝晶生长和电解液分解带来的安全隐患。但是,钛酸锂作为一种绝缘材料,导电率低,倍率性能差,此特性阻碍了LTO负极材料的广泛应用。目前通常采用碳掺杂来提高钛酸锂材料的导电性能和倍率性能。
同时,现有工业化钛酸锂负极的生产制备方法是将钛酸锂、导电剂、粘结剂和溶剂在高速搅拌下均匀混合,形成浆料;然后通过涂布、真空干燥、对辊等工艺制备得到。其工艺过程复杂,耗时长。
公开号为CN109103447A的中国发明专利公布了一种钛酸锂粉体的制备方法,其将锂源和钛源分别配成溶液,混合后经高温烧结,制备得到钛酸锂粉体。公开号为CN106876675A的中国发明专利公布了一种石墨碳和钛酸锂复合粉体的制备方法,其将石墨和钛酸锂粉体混合后经高速球磨制备得到石墨碳和钛酸锂的复合粉体材料。公开号为CN110459770A的中国发明专利公布了一种钛酸锂和碳复合电极的制备方法,其将锂源、钛源以及碳纳米管通过高速球磨混合,而后通过喷雾干燥和高温烧结制备了钛酸锂负极。公开号为CN106410146A的中国发明专利公布了一种通过碳复合提高钛酸锂电极倍率性能的方法,其将钛源、锂源混合形成钛酸锂前驱体溶液,而后将前驱体溶液和酮类、醇类等有机溶液混合,经过高温退火处理,形成碳掺杂的钛酸锂复合材料,该材料用于锂离子电池负极,能够改善钛酸锂的倍率性能。公开号为CN106450261B的中国发明专利公布了一种钛酸锂负极极片的制备方法,其利用EDOT单体与PSS溶液复合作为钛酸锂粉末材料的导电剂和粘结剂,通过聚合、涂布制备了钛酸锂电极极片。公开号为CN110176586A的中国发明专利公布了一种制备钛酸锂涂层极片的方法,其通过溅射沉积的方法形成钛酸锂涂层。然而,上述钛酸锂涂层的制备方法,存在工艺复杂、制备条件严苛、使用大量有机溶剂、得到的钛酸锂涂层电子导电性差等问题。
发明内容
本发明的目的在于,针对背景技术存在的缺陷,提出一种在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法。
本发明的另一目的在于,提供一种钛酸锂负极电极片,以替代现有钛酸锂负极极片制备过程中的制浆、涂布、真空干燥等过程。
为实现上述目的,本发明采用的技术方案如下:
一种在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法,其特征在于,包括以下步骤:
步骤1、将钛源和氢氧化锂分散于去离子水中,搅拌混合均匀,得到混合液A;
步骤2、将高分子碳源分散于无水乙醇中,搅拌混合均匀,得到混合液B;
步骤3、将混合液B加入混合液A中,搅拌混合均匀,得到混合液C;得到的混合液C中,钛源的浓度为3~20g/L,氢氧化锂的浓度为3~40g/L,高分子碳源的浓度为2~10g/L;
步骤4、将配制好的混合液C置于不锈钢槽体中,以铜箔作为阳极、不锈钢槽体作为阴极,采用液相等离子体氧化电源供电,在脉冲电压为700V~900V、频率为60Hz~1000Hz的条件下氧化3~8min,即可在铜箔表面形成三维多孔的碳掺杂钛酸锂复合涂层。
一种基于上述钛酸锂复合涂层制备复合电极片的方法,其特征在于,包括以下步骤:上述方法制备得到的钛酸锂复合涂层,经清洗、干燥,即可得到碳掺杂的钛酸锂复合电极片,其中电极片集流体为铜箔,活性物质为碳掺杂的钛酸锂。
采用四探针法测试该复合电极片的导电性;将该电极片作为负极电极片和金属锂组装成半电池,测试该极片材料的容量、倍率性能和循环稳定性。
进一步地,步骤1所述钛源为硫酸钛酰(TiOSO4)、氟钛酸钠中的一种。
进一步地,步骤2所述高分子碳源为PVP(分子量为5000~20000)、PEG(分子量为3000~20000)中的一种。
其中,随着高分子碳源浓度的增加,涂层中碳元素的含量增加,碳层的导电性增强。随着液相等离子体氧化电压的增大,涂层表面孔洞的孔径增加。随着液相等离子体处理时间的增加,涂层的厚度增加,得到的碳掺杂钛酸锂涂层的厚度为1μm~10μm之间。
与现有技术相比,本发明的有益效果为:
本发明提供了一种在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法,得到的碳掺杂钛酸锂涂层具有三维多孔的结构,有利于锂离子电池电解液的浸润,能够减少扩散传质的阻力。同时,这种自支撑电极,能够避免锂离子电池负极制备过程中混料、制浆、涂覆和干燥过程,简化锂离子电池负极材料的制备工艺,降低锂离子电池的制备成本。
附图说明
图1为实施例12制备得到的涂层的XRD图谱;
图2为实施例12制备得到的涂层表面的SEM图;
图3为实施例12制备得到的涂层截面的SEM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
一种在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法,包括以下步骤:
步骤1、将硫酸钛酰和氢氧化锂分散于去离子水中,搅拌混合均匀,得到混合液A;
步骤2、将PVP(分子量为5000~20000)或PEG(分子量为3000~20000)高分子碳源分散于无水乙醇中,搅拌混合均匀,得到混合液B;
步骤3、将混合液B加入混合液A中,搅拌混合均匀,得到混合液C;得到的混合液C中,钛源的浓度为5g/L,氢氧化锂的浓度为15g/L,高分子碳源的浓度为2~10g/L;
步骤4、将配制好的混合液C置于不锈钢槽体中,以铜箔作为阳极、不锈钢槽体作为阴极,采用液相等离子体氧化电源供电,在脉冲电压为700V~900V、频率为600Hz的条件下氧化3~8min,即可在铜箔表面形成三维多孔的碳掺杂钛酸锂复合涂层。
上述方法制备得到的钛酸锂复合涂层,经清洗、干燥,即可得到碳掺杂的钛酸锂复合电极片,其中电极片集流体为铜箔,活性物质为碳掺杂的钛酸锂。采用四探针法测试该复合电极片的导电性;将该电极片作为负极电极片和金属锂组装成半电池,测试该极片材料的容量、倍率性能和循环稳定性。
实施例选择的高分子碳源及其浓度、液相等离子体脉冲电压、氧化时间等参数条件,以及得到的涂层的性能如下表所示:
图1为实施例12制备得到的涂层的XRD图谱;由图1可知,得到的涂层主要由钛酸锂组成,铜的衍射峰来自基底铜箔;图2为实施例12制备得到的涂层表面的SEM图;由图2可知,得到的涂层为三维多孔结构;图3为实施例12制备得到的涂层截面的SEM图;由图3可知,得到的涂层与基体结合较好,界面清晰,没有明显的脱落和裂纹。
Claims (4)
1.一种在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法,其特征在于,包括以下步骤:
步骤1、将钛源和氢氧化锂分散于去离子水中,搅拌混合均匀,得到混合液A;
步骤2、将高分子碳源分散于无水乙醇中,搅拌混合均匀,得到混合液B;
步骤3、将混合液B加入混合液A中,搅拌混合均匀,得到混合液C;其中,混合液C中,钛源的浓度为3~20g/L,氢氧化锂的浓度为3~40g/L,高分子碳源的浓度为2~10g/L;
步骤4、将配制好的混合液C置于不锈钢槽体中,以铜箔作为阳极、不锈钢槽体作为阴极,采用液相等离子体氧化电源供电,在脉冲电压为700 V~900V、频率为60Hz~1000Hz的条件下氧化3~8 min,即可在铜箔表面形成三维多孔的碳掺杂钛酸锂复合涂层。
2.根据权利要求1所述的在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法,其特征在于,步骤1所述钛源为硫酸钛酰、氟钛酸钠中的一种。
3.根据权利要求1所述的在铜箔表面制备三维多孔碳掺杂钛酸锂涂层的方法,其特征在于,步骤2所述高分子碳源为分子量5000~20000的PVP、分子量3000~20000的PEG中的一种。
4.一种基于权利要求1所述方法得到的钛酸锂复合涂层制备复合电极片的方法,其特征在于,权利要求1所述方法得到的钛酸锂复合涂层,经清洗、干燥,即可得到碳掺杂的钛酸锂复合电极。
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