CN104022281B - 一种制备铅蓄电池负极的材料及其制备方法 - Google Patents
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Abstract
一种制备铅蓄电池负极的材料,所述负极材料是由碳纳米管纸及沉积在所述碳纳米管纸上的氧化铅颗粒组成,按质量百分比计,所述负极材料含所述碳纳米管纸0.05‑20%;该负极材料能有效提高铅蓄电池的功率密度、能量密度和循环使用寿命。
Description
技术领域
本发明涉及一种制备电池负极材料及其制备方法,尤其涉及一种应用于制备铅蓄电池的负极材料及其制备方法。
背景技术
随着诸如纯电动车和混合电动车HEV电动汽车的迅速发展,铅蓄电池因其原料丰富、价格低廉、工艺成熟和安全性好等特点,所以在电动车上有较好的应用前景,但由于铅蓄电池的比功率较低以及大功率放电的使用寿命短等缺点,制约了其发展,而导致上述问题主要原因是受限于负极:在高密度电流放电情况下,负极产生大量铅离子进入电解液,随即发生的情况是电解液中硫酸根离子扩散受限,致使铅离子过饱和,在负极表面形成一层致密的硫酸铅沉淀层,造成负极表面钝化;硫酸铅导电性差,溶解度小,负极内部铅的反应活性会降低,增加反应过电位,严重时充电会析氢,充电效率下降,并形成恶性循环;若继续大功率充放电,以上情况会进一步恶化,硫酸铅沉淀颗粒增大且增大过程不可逆,最终导致负极丧失反应活性,电池失效;若在铅活性物质中加入碳纳米管,则能够有效提高电荷输运能力和电解液离子迁移能力,进而提高化成后极板的功率性能和可逆性。然而,碳纳米管与铅的密度相差十倍以上,二者很难均匀混合,碳纳米管高导电性难以发挥出来。201210046590.2号中国专利公开了一种碳纳米管纸电极材料,但该材料是应用于有机电解液体系的锂离子电池中,与含锂材料复合作为活性物质,含锂材料的储能机制为锂离子的嵌入/脱嵌,与碳纳米管材料性能无关,且有机电解液体系电导率低,碳纳米管材料难以充分发挥作用。
发明内容
本发明的目的是提供一种有效提高铅蓄电池的功率密度、能量密度和循环使用寿命的负极材料及其制备方法。
本发明的具体方案为:一种制备铅蓄电池负极的材料,所述负极材料是由碳纳米管纸及沉积在所述碳纳米管纸上的氧化铅颗粒组成,按质量百分比计,所述负极材料含所述碳纳米管纸0.05-20%。
优选的,所述碳纳米管纸为单壁碳纳米管、双壁碳纳米管或多壁碳纳米管相互交织形成的薄膜。
另一优选的,所述氧化铅通过电沉积或化学沉积的方式附着在碳纳米管纸上。
再一优选的,所述碳纳米管纸中的碳纳米管管径在1-100纳米,碳纳米管长度在0.5-2000微米之间。
再一优选的,所述氧化铅颗粒直径在2-2000纳米之间。
所述的制备铅蓄电池负极的材料的制备方法,包括如下步骤:
1)将碳纳米管与表面活性剂混合后均匀分散在水溶液中,通过抽滤得到碳纳米管纸;
2)将碳纳米管纸基底分别在醋酸铅电解液和1M NaOH溶液中浸润5分钟和浸润1分钟;
3)将浸润后的基底经蒸馏水淋洗后于180℃下烘箱中热处理4小时,得到碳纳米管/氧化铅负极材料。
所述的制备铅蓄电池负极的材料的另一制备方法,包括如下步骤:
1)将碳纳米管与表面活性剂混合后均匀分散在水溶液中,通过抽滤得到碳纳米管纸;
2)将该碳纳米管纸裁成方形基底,向浸渍该基底的0.1M的硝酸铅电解液施加1mA/cm2的沉积电流1小时;
3)用蒸馏水淋洗经步骤2)处理的基底,于180℃烘箱处理4小时,得到碳纳米管/氧化铅负极材料。
优选的,所述的负极材料的制备方法中,所述表面活性剂为十六烷基三甲基溴化铵或十二烷基磺酸钠。
采用上述技术方案,本发明的技术效果有:
将氧化铅通过化学或电化学的方法沉积在碳纳米管纸上,使其形成结构紧密、均匀的碳纳米管纸/氧化铅复合材料,用于硫酸电解液体系的铅酸电池,能有效提高氧化铅活性物质的比能量和比功率,从而全面提高铅蓄电池的充放电能力。该负极材料使得铅蓄电池具有了高功率密度(300W/kg以上)和提高长脉冲循环寿命(5万次以上)的优点。
具体实施方式
下面结合实施例对本发明的具体实施方式作进一步的详细说明。
实施例1:
将多壁碳纳米管与十六烷基三甲基溴化铵混合后均匀分散在水溶液中,通过抽滤得到0.1mm厚的多壁碳纳米管纸;将该碳纳米管纸裁成1cm见方的基底,将该基底在0.1M醋酸铅电解液中浸润5分钟后提出,立刻再浸润到1M NaOH溶液中1分钟,将浸润后的产物用蒸馏水淋洗后,放在温度控制在180度的烘箱中热处理4小时,得到碳纳米管/氧化铅负极材料,其中碳纳米管纸占负极材料质量的1.2%,氧化铅占复合材料质量的98.8%,其中氧化铅质量中的65%为α晶形氧化铅。
性能测试:
对使用该负极材料制备出的铅蓄电池进行测试,测得该铅蓄电池的比功率达到280W/kg,脉冲循环寿命达48000次。
将日本产的电容用活性炭材料与氧化铅混合形成负极材料,使用该负极材料制备铅酸电池并对其进行测试,其中活性炭占负极材料质量的2%,测得该铅蓄电池的比功率为150W/kg,脉冲循环寿命为8000次,远低于碳纳米管纸/氧化铅复合材料制备的样品。
实施例2:
将单壁碳纳米管与十二烷基磺酸钠混合后均匀分散在水溶液中,通过抽滤得到0.05mm厚的单壁碳纳米管纸;将该碳纳米管纸裁成2cm见方的基底,将该基底浸渍在0.1M的硝酸铅电解液中,向该电解液施加1mA/cm2的沉积电流1小时;将电沉积后的产物用蒸馏水淋洗后,放在温度控制在180度的烘箱中热处理4小时,得到碳纳米管/氧化铅负极材料;其中碳纳米管纸占负极材料质量的0.4%,氧化铅占负极材料质量的99.6%,其中负极材料质量的50%为α晶形氧化铅。
性能测试:
对使用该负极材料制备出的铅蓄电池进行测试,测得该铅蓄电池的比功率达到220W/kg,脉冲循环寿命达44500次。
将湖南产的电池用石墨材料与氧化铅混合形成负极材料,使用该负极材料制备铅酸电池并对其进行测试,其中,石墨材料占负极材料质量的1%,测得该铅蓄电池的比功率为180W/kg,脉冲循环寿命为12000次,远低于碳纳米管纸/氧化铅复合材料制备的样品。
最后应当说明的是:以上实施例仅用以说明本发明的技术方案而非对其限制,尽管参照上述实施例对本发明进行了详细的说明,所属领域的普通技术人员应当理解:依然可以对本发明的具体实施方式进行修改或者等同替换,而未脱离本发明精神和范围的任何修改或者等同替换,其均应涵盖在本发明的权利要求范围当中。
Claims (6)
1.一种制备铅蓄电池负极的材料,其特征在于,所述负极材料是由碳纳米管纸及沉积在所述碳纳米管纸上的氧化铅颗粒组成,按质量百分比计,所述负极材料含所述碳纳米管纸0.05-20%;所述氧化铅通过电沉积或化学沉积的方式附着在碳纳米管纸上;所述氧化铅颗粒直径在2-2000纳米之间。
2.如权利要求1所述的负极材料,其特征在于,所述碳纳米管纸为单壁碳纳米管、双壁碳纳米管或多壁碳纳米管相互交织形成的薄膜。
3.如权利要求1所述的负极材料,其特征在于,所述碳纳米管纸中的碳纳米管管径在1-100纳米,碳纳米管长度在0.5-2000微米之间。
4.如权利要求1-3任一项权利要求所述的负极材料的制备方法,其特征在于,所述制备方法包括如下步骤:
1)将碳纳米管与表面活性剂混合后均匀分散在水溶液中,通过抽滤得到碳纳米管纸;
2)将碳纳米管纸基底分别在醋酸铅电解液和1M NaOH溶液中浸润5分钟和浸润1分钟;
3)将浸润后的基底经蒸馏水淋洗后于180℃下烘箱中热处理4小时,得到碳纳米管/氧化铅负极材料。
5.如权利要求1-3任一项权利要求所述的负极材料的制备方法,其特征在于,所述制备方法包括如下步骤:
1)将碳纳米管与表面活性剂混合后均匀分散在水溶液中,通过抽滤得到碳纳米管纸;
2)将该碳纳米管纸裁成方形基底,向浸渍该基底的0.1M的硝酸铅电解液施加1mA/cm2的沉积电流1小时;
3)用蒸馏水淋洗经步骤2)处理的基底,于180℃烘箱处理4小时,得到碳纳米管/氧化铅负极材料。
6.如权利要求4或5所述的负极材料的制备方法,其特征在于,所述表面活性剂为十六烷基三甲基溴化铵或十二烷基磺酸钠。
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