CN113845099B - 一种弧光放电技术用于制备CoSP钠电负极材料的方法 - Google Patents
一种弧光放电技术用于制备CoSP钠电负极材料的方法 Download PDFInfo
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- 238000000151 deposition Methods 0.000 claims abstract description 17
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims abstract description 9
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims abstract description 9
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
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Abstract
一种弧光放电技术用于制备CoSP钠电负极材料的方法,制备出CoSP的方法是先通过水热法制备出氢氧化钴前驱体,然后分别先后对硫单质和磷单质进行弧光放电处理,处理后的正离子通过磁过滤进行筛选,最后结合化学气相沉积将其沉积到靶材上便可以得到硫、磷双掺杂的CoSP空心球材料,将其应用到钠离子电池中可以实现较为优异的电化学性能。在0.1 A g‑1电流密度下,在循环100圈后,其比容量仍可高达633 mAh g‑1,2 A g‑1的电流密度下,经过400圈循环后,其比容量高达456 mAh g‑1,体现其较好的循环稳定性。
Description
技术领域
本发明属于钠离子电池负极材料制备技术领域,具体涉及一种弧光放电技术用于制备CoSP钠电负极材料的方法。
背景技术
目前锂离子电池发展迅速,商用的锂离子电池应用非常广泛,但随着人们需求的不断增长,锂离子电池成本高、资源少,这也成为阻碍锂离子电池实现大规模应用的短板。钠离子电池具有和锂离子电池相似的电池结构,但正负极采用不同的材料,同时电解液也不同。锂离子和钠离子的差异也造成某些方面的不同。对于钠离子电池负极材料,主要分为碳基材料、纳米合金材料、金属化合物、等。碳基材料中硬碳材料在宏观上是无序结构,微观上是不同取向的石墨微晶,钠离子可以嵌入到不同取向的石墨微晶中。对于纳米合金材料来讲由于钠离子的尺寸较大,在循环过程中电极材料的体积变化较大,容易发生材料的塌陷,因此对于合金材料而言其循环稳定性的提高是非常关键性的。金属化合物的研究包括金属氧化物、金属硫化物、金属磷化物、金属硒化物等。和氧化物相比,杂元素的引入可以增加钠离子的存储活性位点,进而提高材料的储钠性能。传统的元素掺杂主要是通过水热、高温裂解、熔融法等方式进行掺杂,这些掺杂方式得到的材料往往是不均匀的,同时反应条件往往涉及到高温反应,不仅会造成资源的浪费,同时排放出的污染物会对环境造成一定的污染。
发明内容
本发明所要解决的技术问题是克服现有技术的不足,提供一种制备双掺杂金属化合物的方法,通过弧光放电技术对原料进行轰击得到等离子体态,然后用磁过滤装置进行过滤从而得到质量均匀且纯度较高的正离子。最后通过化学气相沉积将已过滤的等离子体态沉积到基底上,从而实现均匀的元素掺杂。
本发明提供一种弧光放电技术用于制备CoSP钠电负极材料的方法,包括如下步骤,
步骤S1、通过水热方法制备氢氧化钴的前驱体,然后放在60℃真空干燥箱中干燥12 h;
步骤S2、将氢氧化物前驱体和导电炭黑、PVDF粘结剂按照8:1:1的比例称取适量,以NMP做为溶剂,搅拌24 h后进行涂布,将膏体涂敷在铜箔上,然后在60℃下干燥12 h;
步骤S3、剪裁尺寸为3×4 cm的涂敷后的铜箔作为靶材,先对弧光放电以及此磁过滤装备进行抽真空处理,使其真空度得到1×10-5Pa;
步骤S4、将靶材放置于旋转台中央,首先进行等离子体清洗,同时提前将S单质和P单质都提前放在弧光放电舱体中,再设置好弧光放电仪器参数,先进行弧光放电处理,再将弧光放电后的等离子体态物质施加有效磁场进行磁过滤处理;
步骤S5、进行沉积,沉积完成后,关闭弧光放电、磁过滤电源,取出样品。
作为本发明的进一步技术方案,步骤S4中设置好的弧光放电仪器参数为电流1~1.8A、电压150~200 V、磁场50~200 WB。
进一步的,步骤S4中、将射频放电后的等离子态的正离子引入磁过滤管中进行筛选,沉积10min结束,关闭射频放电、磁过滤电源,释放真空度,获取双掺杂的复合材料。
本发明的优点在于,通过水热法制备出氢氧化钴前驱体,然后分别先后对硫单质和磷单质进行弧光放电处理,处理后的正离子体结合磁过滤进行筛选,最后结合化学气相沉积将其沉积到靶材上便可以得到硫、磷双掺杂的CoSP空心球材料,将其应用到钠离子电池中可以实现较为优异的电化学性能。在0.1 A g-1电流密度下,在循环100圈后,其比容量仍可高达633 mAh g-1, 2 A g-1的电流密度下,经过400圈循环后,其比容量高达456 mAh g-1,体现其较好的循环稳定性。
附图说明
图1为本发明的实施例1所制备的CoSP材料的SEM图;
图2为本发明的实施例1所制备的CoSP材料的TEM图;
图3为本发明的实施例1所制备的CoS和CoSP材料在2 Ag-1电流密度下的循环性能图。
具体实施方式
实施例1
一种利用弧光放电技术进行钠离子电池负极材料的制备,它包括以下步骤:首先通过水热方法制备氢氧化钴的前驱体,然后放在60℃真空干燥箱中干燥12 h。接下来将氢氧化物前驱体和导电炭黑、PVDF粘结剂按照8:1:1的比例称取适量,以NMP做为溶剂,搅拌24h后进行涂布,将膏体涂敷在铜箔上,然后在60℃下干燥12 h。然后剪取尺寸大小为3×4 cm的涂敷后的铜箔作为靶材。先对弧光放电以及此磁过滤装备进行抽真空处理,使其真空度得到1×10-5Pa。然后将靶材放置于旋转台中央,首先进行等离子体清洗。同时提前将S单质和P单质都提前放在弧光放电舱体中,再设置好弧光放电仪器参数,电压为180 V,电流为1.5 A,100 WB,先进性弧光放电处理,再将弧光放电后的等离子体态物质施加有效磁场进行磁过滤处理。最后进行沉积,沉积完成后,关闭弧光放电、磁过滤电源,取出样品。请参阅图1-图3,本实施例所制备的CoSP材料的SEM图、TEM图以及制备的CoS和CoSP材料在2 A g-1电流密度下的循环性能图。
实施例2
一种利用弧光放电技术进行钠离子电池负极材料的制备,它包括以下步骤:首先通过水热方法制备氢氧化钴的前驱体,然后放在60℃真空干燥箱中干燥12 h。接下来将氢氧化物前驱体和导电炭黑、PVDF粘结剂按照8:1:1的比例称取适量,以NMP做为溶剂,搅拌24h后进行涂布,将膏体涂敷在铜箔上,然后在60℃下干燥12 h。然后剪取尺寸大小为3×4 cm的涂敷后的铜箔作为靶材。先对弧光放电以及此磁过滤装备进行抽真空处理,使其真空度得到1×10-5Pa。然后将靶材放置于旋转台中央,首先进行等离子体清洗。同时提前将S单质和P单质都提前放在弧光放电舱体中,再设置好弧光放电仪器参数,电压为180 V,电流为1.5 A,120 WB,先进性弧光放电处理,再将弧光放电后的等离子体态物质施加有效磁场进行磁过滤处理。最后进行沉积,沉积完成后,关闭弧光放电、磁过滤电源,取出样品。
实施例3
一种利用弧光放电技术进行钠离子电池负极材料的制备,它包括以下步骤:首先通过水热方法制备氢氧化钴的前驱体,然后放在60℃真空干燥箱中干燥12 h。接下来将氢氧化物前驱体和导电炭黑、PVDF粘结剂按照8:1:1的比例称取适量,以NMP做为溶剂,搅拌24h后进行涂布,将膏体涂敷在铜箔上,然后在60℃下干燥12 h。然后剪取尺寸大小为3×4 cm的涂敷后的铜箔作为靶材。先对弧光放电以及此磁过滤装备进行抽真空处理,使其真空度得到1×10-5Pa。然后将靶材放置于旋转台中央,首先进行等离子体清洗。同时提前将S单质和P单质都提前放在弧光放电舱体中,再设置好弧光放电仪器参数,电压为180 V,电流为1.5 A,140 WB,先进性弧光放电处理,再将弧光放电后的等离子体态物质施加有效磁场进行磁过滤处理。最后进行沉积,沉积完成后,关闭弧光放电、磁过滤电源,取出样品。
实施例4
一种利用弧光放电技术进行钠离子电池负极材料的制备,它包括以下步骤:首先通过水热方法制备氢氧化钴的前驱体,然后放在60℃真空干燥箱中干燥12 h。接下来将氢氧化物前驱体和导电炭黑、PVDF粘结剂按照8:1:1的比例称取适量,以NMP做为溶剂,搅拌24h后进行涂布,将膏体涂敷在铜箔上,然后在60℃下干燥12 h。然后剪取尺寸大小为3×4 cm的涂敷后的铜箔作为靶材。先对弧光放电以及此磁过滤装备进行抽真空处理,使其真空度得到1×10-5Pa。然后将靶材放置于旋转台中央,首先进行等离子体清洗。同时提前将S单质和P单质都提前放在弧光放电舱体中,再设置好弧光放电仪器参数,电压为180 V,电流为1.5 A,160 WB,先进性弧光放电处理,再将弧光放电后的等离子体态物质施加有效磁场进行磁过滤处理。最后进行沉积,沉积完成后,关闭弧光放电、磁过滤电源,取出样品。
实施例5
一种利用弧光放电技术进行钠离子电池负极材料的制备,它包括以下步骤:首先通过水热方法制备氢氧化钴的前驱体,然后放在60℃真空干燥箱中干燥12 h。接下来将氢氧化物前驱体和导电炭黑、PVDF粘结剂按照8:1:1的比例称取适量,以NMP做为溶剂,搅拌24h后进行涂布,将膏体涂敷在铜箔上,然后在60℃下干燥12 h。然后剪取尺寸大小为3×4 cm的涂敷后的铜箔作为靶材。先对弧光放电以及此磁过滤装备进行抽真空处理,使其真空度得到1×10-5Pa。然后将靶材放置于旋转台中央,首先进行等离子体清洗。同时提前将S单质和P单质都提前放在弧光放电舱体中,再设置好弧光放电仪器参数,电压为180 V,电流为1.5 A,180 WB,先进性弧光放电处理,再将弧光放电后的等离子体态物质施加有效磁场进行磁过滤处理。最后进行沉积,沉积完成后,关闭弧光放电、磁过滤电源,取出样品。
以上显示和描述了本发明的基本原理、主要特征和优点。本领域的技术人员应该了解,本发明不受上述具体实施例的限制,上述具体实施例和说明书中的描述只是为了进一步说明本发明的原理,在不脱离本发明精神范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护的范围由权利要求书及其等效物界定。
Claims (3)
1.一种弧光放电技术用于制备CoSP钠电负极材料的方法,其特征在于,包括如下步骤,
步骤S1、通过水热方法制备氢氧化钴的前驱体,然后放在60℃真空干燥箱中干燥12h;
步骤S2、将氢氧化物前驱体和导电炭黑、PVDF粘结剂按照8:1:1的比例称取适量,以NMP做为溶剂,搅拌24h后进行涂布,将均匀的膏体涂敷在铜箔上,然后在60℃下干燥12h;
步骤S3、剪裁尺寸为3×4cm的涂敷后的铜箔作为靶材,先对弧光放电以及磁过滤装备进行抽真空处理,使其真空度得到1×10-5Pa;
步骤S4、将靶材放置于旋转台中央,首先进行等离子体清洗,同时提前将S单质和P单质放在弧光放电舱体中,再设置好弧光放电仪器参数,先进行弧光放电处理,再将弧光放电后的等离子体态物质施加有效磁场之后对其进行磁过滤处理;
步骤S5、进行沉积,沉积完成后,关闭弧光放电、磁过滤电源,取出样品。
2.根据权利要求1所述的一种弧光放电技术用于制备CoSP钠电负极材料的方法,其特征在于,所述步骤S4中设置好的弧光放电仪器参数为电流1~1.8A、电压150~200V、磁场50~200WB。
3.根据权利要求1所述的一种弧光放电技术用于制备CoSP钠电负极材料的方法,其特征在于,所述步骤S5中、将射频放电后的正离子引入磁过滤管中进行筛选,沉积10min后,关闭射频放电、磁过滤电源,释放真空度,获取双掺杂的复合材料。
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