CN109546112A - 锡纳米球与碳纳米管复合的电极材料的制备方法及其产品和应用 - Google Patents
锡纳米球与碳纳米管复合的电极材料的制备方法及其产品和应用 Download PDFInfo
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 44
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 44
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 5
- 239000007773 negative electrode material Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 60
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
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- 235000019441 ethanol Nutrition 0.000 claims description 17
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- 239000002131 composite material Substances 0.000 claims description 4
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical class CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- PNOXNTGLSKTMQO-UHFFFAOYSA-L diacetyloxytin Chemical compound CC(=O)O[Sn]OC(C)=O PNOXNTGLSKTMQO-UHFFFAOYSA-L 0.000 claims description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 2
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- 238000003860 storage Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
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- 239000011366 tin-based material Substances 0.000 description 1
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Abstract
本发明公开了一种锡纳米球颗粒与碳纳米管复合的电极材料的制备方法及其产品和应用,借助微孔聚合物纳米空心管,微孔聚合物纳米空心管材料用作负载载体,通过高温碳化处理制备金属锡与碳纳米管复合的电极材料。本方法首次尝试将微孔聚合物纳米空心管材料用作负载载体,通过高温碳化处理制备金属锡与碳纳米管复合的电极材料。由于微孔碳纳米管是由微孔聚合物纳米管高温碳化而成,所以此纳米管的管壁也为微孔结构,此微孔结构可以牢固的将金属锡纳米颗粒稳定在管壁上,因此,此材料作为锂离子电池的负极材料可以有效防止金属锡在充放电过程中的团聚现象,提高充放电的循环稳定性。与此同时,碳材料还可以有利于提高锡基负极材料的导电性。
Description
技术领域
本发明涉及一种锡纳米球颗粒与碳纳米管复合的电极材料的制备方法及其产品和应用。具体涉及一种借助管直径约为50 nm的微孔聚合物纳米管为载体,合成高分散的直径约为10-40 nm的金属锡纳米球与碳纳米管复合的电极材料。
背景技术
由于金属锡等金属材料的储锂机理属于合金化储锂过程,此类金属材料在储锂时与锂离子发生反应生成各种锂基合金,与插入式储锂机理的石墨负极材料相比较,金属锡等金属材料具有更高的储锂容量,锡的理论容量可高达994 mAh/g。因此,锡基负极材料近年来受到广泛的关注。但由于金属锡在脱嵌锂的过程中体积膨胀非常严重,体积膨胀率可高达259%,因此在充放电过程中容易发生活性材料的粉化团聚等问题,造成容量衰减快,导致充放电的循环稳定性差。
为了解决锡材料在充放电过程中因体积膨胀导致的粉化团聚现象,人们采取了各种方法来提高锡纳米颗粒的分散性和稳定性,比如用碳材料包覆或者负载锡基纳米材料起到分散和锚定锡基纳米颗粒的作用,从而提高锡基材料在充放电过程中的循环稳定性。
微孔聚合物材料属于多孔有机聚合物材料中的一种,其本身含有孔径约2-3 nm的微孔结构,是一种特殊的多孔材料,将纳米颗粒负载到微孔的孔道中可以起到分散和锚定纳米颗粒的作用。在众多的微孔聚合物纳米材料中,微孔聚合物纳米空心管材料不仅管壁本身含有微孔结构,而且其管径约为50 nm左右,非常有利于溶液的浸润从而提高活性物质的负载率。
发明内容
针对锡基负极材料存在的问题及微孔聚合纳米空心管材料本身的结构特点,本发明目的在于提供一种锡纳米球与碳纳米管复合的电极材料的制备方法。
本发明的再一目的在于:提供一种上述方法制备的锡纳米球与碳纳米管复合的电极材料产品。
本发明的又一目的在于:提供一种上述产品的应用。
本发明目的通过下述方案实现:一种锡纳米球与碳纳米管复合的电极材料的制备方法,其特征在于借助微孔聚合物纳米空心管,微孔聚合物纳米空心管材料用作负载载体,通过高温碳化处理制备金属锡与碳纳米管复合的电极材料,技术方案如下:
a、锡盐的乙醇溶液的配制:配制100 ml浓度为50 mg/ml的锡盐的乙醇溶液加入到250ml的三颈烧瓶中;
b、氮气置换:通过抽真空-充氮气操作将上述溶液中的空气用氮气置换,使三颈烧瓶中保持氮气气氛;
c、微孔聚合物纳米管的加入:称取30 mg微孔聚合物纳米管加入到上述氮气保护的溶液中,氮气保护下室温搅拌6-8 h;
d、抽滤并干燥:将上述混合液抽滤并收集固体粉末,将收集到的固体粉末在60℃下真空干燥3h;
e、高温碳化处理:将上述干燥后的固体粉末在氮气保护下800℃高温碳化处理6h,得到锡纳米球与碳纳米管复合的电极材料。
所述的微孔聚合物纳米管为:聚合物纳米管的管壁为微孔结构,孔径范围2-3 nm,纳米管的管径范围10-50 nm。
所述的锡盐为可溶于乙醇的无机锡盐,或二丁基锡类的可溶于乙醇的有机锡盐。
所述的无机锡盐为SnCl2;所述的二丁基锡类的可溶于乙醇的有机锡盐为乙酸亚锡或二月桂酸二丁基锡。
本发明提供一种锡纳米球与碳纳米管复合的电极材料,根据上述任一所述方法制备得到;微孔碳纳米管负载的粒径为10-40 nm的金属锡纳米球的复合材料。
本发明提供一种锡纳米球与碳纳米管复合的电极材料在锂离子电池中作为负极材料的应用。
本发明提出了一种借助微孔聚合物纳米空心管制备锡纳米球与碳纳米管复合的电极材料的方法。本发明方法首先将微孔聚合物纳米空心管加入到溶解有锡盐离子的乙醇溶液中并搅拌一段时间,然后将吸附有锡盐离子乙醇溶液的微孔聚合物纳米管材料进行高温碳化处理,最终得到微孔碳纳米管负载的粒径约为10-40 nm的金属锡纳米球复合材料。在高温碳化的过程中,微孔聚合物纳米管会转变成微孔碳纳米管,微孔孔道中吸附的锡离子会被还原为金属Sn颗粒,由透射电镜TEM的结果可知,此金属锡纳米颗粒的形状为球形且高度分散在微孔碳纳米管的管壁上,没有发生团聚现象。由于微孔碳纳米管是由微孔聚合物纳米管高温碳化而成,所以此纳米管的管壁也为微孔结构,此微孔结构可以牢固的将金属锡纳米颗粒稳定在管壁上,可以有效防止金属锡在充放电过程的团聚现象,提高充放电的循环稳定性。与此同时,碳材料还可以有利于提高锡基负极材料的导电性。
本发明方法首次尝试将微孔聚合物纳米空心管材料用作负载载体,通过高温碳化处理制备金属锡与碳纳米管复合的电极材料。不仅提出了一种新的负载纳米颗粒的载体材料,还提供了一种新的制备碳纳米管材料的方法。通过本发明方法得到了一种微孔碳纳米管负载的粒径约为10-40 nm的金属锡纳米球的复合材料。由于微孔碳纳米管是由微孔聚合物纳米管高温碳化而成,所以此纳米管的管壁也为微孔结构,此微孔结构可以牢固的将金属锡纳米颗粒稳定在管壁上,因此,此材料作为锂离子电池的负极材料可以有效防止金属锡在充放电过程中的团聚现象,提高充放电的循环稳定性。与此同时,碳材料还可以有利于提高锡基负极材料的导电性。
附图说明
图1为本发明实施例1合成的锡纳米球颗粒与碳纳米管复合的电极材料的TEM图;
图2为本发明实施例2合成的锡纳米球颗粒与碳纳米管复合的电极材料的TEM图。
具体实施方式
本发明通过下面具体实施例进行详细的描述,但是本发明的保护范围不受限于这些实施例:
实施例1:
一种锡纳米球与碳纳米管复合的电极材料的制备方法,将微孔聚合物纳米空心管材料作为负载载体,通过高温碳化处理制备金属锡与碳纳米管复合的电极材料,包括如下步骤:
a、锡盐的乙醇溶液配制:配制100 ml浓度为50 mg/ml的SnCl2的乙醇溶液加入到250ml的三颈烧瓶中;
b、氮气置换:通过抽真空-充氮气操作将上述溶液中的空气用氮气置换,使三颈烧瓶中保持氮气气氛;
c、加入微孔聚合物纳米管:称取30 mg微孔聚合物纳米管加入到上述氮气保护的溶液中,氮气保护下室温搅拌6-8 h;
d、抽滤并干燥:将上述混合液抽滤并收集固体粉末,将收集到的固体粉末在60℃下真空干燥3h;
e、高温碳化处理:将上述干燥后的固体粉末在氮气保护下800℃高温碳化处理6h,得到锡纳米球与碳纳米管复合的电极材料的TEM图如图1所示,微孔碳纳米管负载的管径不足40nm,金属锡纳米颗粒稳定在管壁上。
实施例2
一种锡纳米球与碳纳米管复合的电极材料的制备方法,包括如下步骤:
a、锡盐的乙醇溶液配制:配制100 ml浓度为50 mg/ml的乙酸亚锡的乙醇溶液加入到250 ml的三颈烧瓶中;
b、氮气置换:通过抽真空-充氮气操作将上述溶液中的空气用氮气置换,使三颈烧瓶中保持氮气气氛;
c、加入微孔聚合物纳米管:称取30 mg微孔聚合物纳米管加入到上述氮气保护的溶液中,氮气保护下室温搅拌6-8 h;
d、抽滤并干燥:将上述混合液抽滤并收集固体粉末,将收集到的固体粉末在60℃下真空干燥3h;
e、高温碳化处理:将上述干燥后的固体粉末在氮气保护下800℃高温碳化处理6h,得到锡纳米球与碳纳米管复合的电极材料的TEM图如图2,微孔碳纳米管负载的管径不足50 nm,金属锡纳米颗粒稳定在管壁上。
实施例3
一种锡纳米球与碳纳米管复合的电极材料的制备方法,包括如下步骤:
a、锡盐的乙醇溶液配制:配制100 ml浓度为50 mg/ml的二月桂酸二丁基锡的乙醇溶液加入到250 ml的三颈烧瓶中;
b、氮气置换:通过抽真空-充氮气操作将上述溶液中的空气用氮气置换,使三颈烧瓶中保持氮气气氛;
c、加入微孔聚合物纳米管:称取30 mg微孔聚合物纳米管加入到上述氮气保护的溶液中,氮气保护下室温搅拌6-8 h;
d、抽滤并干燥:将上述混合液抽滤并收集固体粉末,将收集到的固体粉末在60℃下真空干燥3h;
e、高温碳化处理:将上述干燥后的固体粉末在氮气保护下800℃高温碳化处理6h,得到锡纳米球与碳纳米管复合的电极材料。
Claims (6)
1.一种锡纳米球与碳纳米管复合的电极材料的制备方法,其特征在于,将微孔聚合物纳米空心管材料作为负载载体,通过高温碳化处理制备金属锡与碳纳米管复合的电极材料,包括如下步骤:
a、锡盐的乙醇溶液配制:配制100 ml浓度为50 mg/ml的锡盐的乙醇溶液加入到250 ml的三颈烧瓶中;
b、氮气置换:通过抽真空-充氮气操作将上述溶液中的空气用氮气置换,使三颈烧瓶中保持氮气气氛;
c、加入微孔聚合物纳米管:称取30 mg微孔聚合物纳米管加入到上述氮气保护的溶液中,氮气保护下室温搅拌6-8 h;
d、抽滤并干燥:将上述混合液抽滤并收集固体粉末,将收集到的固体粉末在60℃下真空干燥3h;
e、高温碳化处理:将上述真空干燥后的固体粉末在氮气保护下800℃高温碳化处理6h,得到锡纳米球与碳纳米管复合的电极材料。
2.根据权利要求1所述的锡纳米球颗粒与碳纳米管复合的电极材料的制备方法,其特征在于,所述的微孔聚合物纳米管为:管壁为微孔结构的聚合物纳米管,孔径范围2-3 nm,纳米管的管径范围10-50 nm。
3.根据权利要求1所述的锡纳米球颗粒与碳纳米管复合的电极材料的制备方法,其特征在于,所述的锡盐为可溶于乙醇的无机锡盐,或二丁基锡类的可溶于乙醇的有机锡盐。
4.根据权利要求3所述的锡纳米球颗粒与碳纳米管复合的电极材料的制备方法,其特征在于所述的无机锡盐为SnCl2;所述的二丁基锡类的可溶于乙醇的有机锡盐为乙酸亚锡、二月桂酸二丁基锡。
5.一种锡纳米球与碳纳米管复合的电极材料,其特征在于根据权利要求1-4任一所述方法制备得到;微孔碳纳米管负载的粒径为10-40 nm的金属锡纳米球的复合材料。
6.一种根据权利要求5所述锡纳米球与碳纳米管复合的电极材料在锂离子电池中作为负极材料的应用。
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