CN115036491A - 一种锂离子电池 - Google Patents
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Abstract
本申请涉及一种锂离子电池，其特征在于，负极材料采用如下工艺进行制备：步骤(1)将摩尔比为1:1的硝酸锌和钼酸铵加入到乙二醇中，加入六次甲基四胺和柠檬酸，将混合液转到高压反应釜中，进行溶剂热反应，从而得到片状的ZnMoO4；步骤(2)将纳米片的ZnMoO4分散于乙二醇中，接着继续加入海藻酸钠和硝酸钴、以及尿素，随后将其转移到高压反应釜，溶剂热反应，反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4‑纳米Co3O4；步骤(3)将步骤(2)产物进行两步热处理，第一步为200‑300摄氏度下处理30‑60min；第二步热处理为300‑450摄氏度下处理30‑60min。
Description
技术领域
本发明涉及锂离子电池技术领域，具体涉及一种锂离子电池复合负极材料及其制备方法。
背景技术
锂离子二次电池具有能量密度大、无记忆效应、循环寿命长、工作电压高、自放电小和无环境污染等优点，成为目前发展最快的蓄电池之一。而提高电池性能的关键在于电极材料，因此锂离子二次电池正、负电极材料的研究和开发是目前电池材料的研究重点之一。为了获得更高的能量密度，开发高比容量负极材料是提高锂离子电池比能量的重要途径之一。目前商业化锂离子电池采用廉价且稳定的石墨类碳材料为负极，但是它的理论比容量较低，不能完全满足日益增长的能源存储需求。因此，开发具有高电化学性能的负极材料已迫在眉睫。CN112086629A公开了一种Si@C/ZnNb2O6负极复合材料的制备方法及其应用，包括以下步骤：采用含造孔剂的纺丝液进行静电纺丝，在惰性保护气氛中高温煅烧，清洗，得多孔碳纤维；将软模板、纳米硅、铌源、锌源和多孔碳纤维混合后加入到无水乙醇中，进行溶剂热反应，即得Si@C/ZnNb2O6复合材料。在50mA·g-1电流密度下，首次放电容量为922.8mAh g-1，经过1000次循环后放电比容量为613.2mAh g-1，容量保持率为66.45％，且制备工艺简便。CN113716602A公开了一种ZnSnO3纳米棒/NC纳米膜复合材料的制备方法，包括以下步骤：将锡源、氢氧化钠、锌源溶于去离子水中获得混合溶液，微波水热反应得到浑浊液；浑浊液经离心和洗涤，获得ZnSn(OH)6前驱体；将所述前驱体进行煅烧，获得ZnSnO3纳米棒；将聚丙烯腈与所述ZnSnO3纳米棒按1:(0.5～4)的质量比溶解于氮氮二甲基甲酰胺中，混匀得到预溶液，将预溶液静电纺丝得到预产物；预产物经过固化和煅烧，得到ZnSnO3纳米棒/NC纳米膜复合材料。CN114261991A公开了公开了一种纳米片状的ZnFe2O4锂离子电池负极材料的制备方法，采用溶胶凝胶-燃烧法，将前驱液在水浴环境下制备成凝胶，然后在空气中进行燃烧形成泡沫状固体，最后采用分阶段煅烧的方式制备纳米片状的ZnFe2O4，制备过程简单，过程易于控制，原料价廉易得，纳米片状ZnFe2O4用于锂离子电池负极材料时，在电流密度为500mA·g-1下充放电循环120周之后放电容量为1000mAh·g-1左右，该材料在电流密度为10A·g-1下放电容量仍然可以达到130mAh g-1，表现出优异的倍率性能。但现有技术关于负极材料的制备存在着材料结构不均一稳定，制备工艺繁琐价格高昂等问题。
发明内容
一种锂离子电池，其特征在于，负极材料采用如下工艺进行制备：
(1)将摩尔比为1:1的硝酸锌和钼酸铵加入到乙二醇中，超声10min-20min后，加入六次甲基四胺和柠檬酸，继续超声以混合均匀，将混合液转到高压反应釜中，进行溶剂热反应，反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4；
(2)将纳米片的ZnMoO4分散于乙二醇中，接着继续加入海藻酸钠和硝酸钴、以及尿素，随后将其转移到高压反应釜，溶剂热反应，反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4-纳米Co3O4；
将步骤(3)将步骤(2)产物进行两步热处理，第一步为200-300摄氏度下处理30-60min；第二步热处理为300-450摄氏度下处理30-60min；
优选的，硝酸锌和钼酸铵、六次甲基四胺、柠檬酸摩尔比为1:1:1:1；
优选的，溶剂热的反应温度为180-230摄氏度；反应时间为12-18h；
优选的，海藻酸钠和硝酸钴、尿素的加入量为(10-20)mg：(5-20)mmol：(5-20)mmol；
有益效果：本发明采用溶剂热工艺制备得到片状的ZnMoO4-纳米Co3O4颗粒的电池负极材料，其具有较高的比表面积，有利于增大负极材料与电解液的接触面积，提高锂离子的传输速率，ZnMoO4-纳米Co3O4之间通过热处理形成异质结，有利于提升电子传递速率，提高电池循环和倍率性能。
附图说明
图1为实施例1的产物的的SEM图。
具体实施方式
实施例1
(1)将20mmol硝酸锌和20mmol钼酸铵加入到100ml乙二醇中，超声10min后，加入20mmol六次甲基四胺和20mmol柠檬酸，继续超声以混合均匀，将混合液转到高压反应釜中，进行溶剂热反应，反应温度为180℃，反应时间为15h；反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4；
(2)将片状的ZnMoO4分散于100ml乙二醇中，接着继续加入15mg海藻酸钠和5mmol硝酸钴、以及5mmol尿素，随后将其转移到高压反应釜，溶剂热反应，反应温度为180℃，反应时间为15h，反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4-纳米Co3O4；
(3)将步骤(3)将步骤(2)产物进行两步热处理，第一步为200摄氏度下处理60min；第二步热处理为450摄氏度下处理60min。
实施例2
(1)将18mmol硝酸锌和18mmol钼酸铵加入到100ml乙二醇中，超声10min后，加入18mmol六次甲基四胺和18mmol柠檬酸，继续超声以混合均匀，将混合液转到高压反应釜中，进行溶剂热反应，反应温度为200℃，反应时间为18h；反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4；
(2)将片状的ZnMoO4分散于100ml乙二醇中，接着继续加入15mg海藻酸钠和5mmol硝酸钴、以及5mmol尿素，随后将其转移到高压反应釜，溶剂热反应，反应温度为180℃，反应时间为15h，反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4-纳米Co3O4；
(3)将步骤(3)将步骤(2)产物进行两步热处理，第一步为200摄氏度下处理30min；第二步热处理为450摄氏度下处理60min。
将实施例1的产物用作锂离子电池负极材料并进行电化学性能测试，结果如下表。
| 电流密度(A·g<sup>-1</sup>) | 放电容量(mAh·g<sup>-1</sup>) |
| 0.1 | 749 |
| 0.2 | 684 |
| 0.5 | 563 |
| 1 | 483 |
| 2 | 437 |
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。
Claims (4)
1.一种锂离子电池，其特征在于，负极材料采用如下工艺进行制备：
(1)将摩尔比为1:1的硝酸锌和钼酸铵加入到乙二醇中，超声10min-20min后，加入六次甲基四胺和柠檬酸，继续超声以混合均匀，将混合液转到高压反应釜中，进行溶剂热反应，反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4；
(2)将纳米片的ZnMoO4分散于乙二醇中，接着继续加入海藻酸钠和硝酸钴、以及尿素，随后将其转移到高压反应釜，溶剂热反应，反应结束后，对产物进行过滤，洗涤，从而得到片状的ZnMoO4-纳米Co3O4；
(3)将步骤(2)产物进行两步热处理，第一步为200-300摄氏度下处理30-60min；第二步热处理为300-450摄氏度下处理30-60min。
2.根据权利要求1所述的一种锂离子电池，硝酸锌和钼酸铵、六次甲基四胺、柠檬酸摩尔比为1:1:1:1。
3.根据权利要求1-2所述的一种锂离子电池，溶剂热的反应温度为120-230摄氏度；反应时间为12-18h。
4.根据权利要求1所述的一种锂离子电池，海藻酸钠和硝酸钴、尿素的加入量为(10-20)mg：(5-20)mmol：(5-20)mmol。
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