CN101327920A - 一种薄片状LiFePO4纳米晶粉体及其制备方法 - Google Patents
一种薄片状LiFePO4纳米晶粉体及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种具有(020)取向的薄片状LiFePO4纳米晶粉体及其制备方法。薄片状晶体尺寸在200纳米-5微米,厚度在50纳米-500纳米之间。具体制备方法是:把廉价的水溶性亚铁盐,氢氧化锂分别在不同容器中用蒸馏水溶解,将浓磷酸用蒸馏水稀释。然后将水溶性亚铁盐溶液和磷酸溶液混合,再在强力搅拌下缓慢倒入氢氧化锂溶液。水溶性亚铁盐、磷酸和氢氧化锂用量控制为摩尔比1∶1∶(2.5-3)。最后将三者混合的产物转移到水热反应釜里在120-220℃保温1-10小时,取出放冷,过滤,干燥得到最终产物。本发明可以在较低温度下合成纯的LiFePO4,并且合成的纳米晶具有明显的(020)取向,具有该取向的薄片状纳米晶含有发达的锂离子抽出/插入通道,本发明可用作锂离子电池正极材料。
Description
技术领域
本发明涉及磷酸盐型锂离子电池正极材料及其制备方法,具体为具有(020)取向的薄片状LiFePO4纳米晶粉体及其水热合成方法。
背景技术
锂离子电池是新一代的绿色高能可充电电池,具有电压高、能量密度大、充电/放电循环性能好、自放电小、无记忆效应、工作温度区间宽等众多优点,目前广泛应用在笔记本电脑、手机、录像机、电子仪表等便携式电子产品领域。锂离子电池由正极、负极、电解液及高分子多孔隔膜等部件构成,决定锂离子电池性能的因素主要包括正极、负极材料的性能,尤其是正极材料的性能。具有正交橄榄石结构的LiFePO4是新型的锂离子电池正极材料。初步的研究结果表明,该新型正极材料集中了LiCoO2、LiNiO2、LiMn2O4及其衍生物正极材料的各自特点:不含贵重元素、原料廉价、资源丰富、工作电压适中(3.4V)、电压平稳(平台特性好)、理论容量大(170mAh/g)、晶体结构稳定、安全性能极佳(磷酸根以强共价键牢固结合,使材料很难析氧分解)、高温热稳定性明显优于已知的其它正极材料、充电/放电循环性能好、充电时体积缩小、和碳负极材料配合时的体积效应好、与大多数电解液系统相容性好、储存性能好、无毒,为真正的绿色材料。与LiCoO2、LiNiO2、LiMn2O4及其衍生物正极材料相比,LiFePO4正极材料在成本、高温性能、安全性方面具有突出的优势,可望成为中大容量、中高功率锂离子电池首选的正极材料。
LiFePO4作为锂离子电池正极材料的研究始于1997年,文献1:J.Electrochem.Soc.,Vol.144,1188-1194(1997)首先报道了具有橄榄石结构的LiFePO4具备作为锂离子电池正极材料的特征。LiFePO4晶体结构具有明显的各向异性,通过对LiFePO4晶体结构分析发现,平行于y轴方向,即沿[010]方向是锂离子抽出/插入的便捷通道(参见图1a-c)。在充电过程中,锂离子沿通道从LiFePO4中抽出,发生从LiFePO4到FePO4的相变;在放电过程中,锂离子沿通道插入FePO4,发生从FePO4到LiFePO4的相变。最近,文献2:Chem.Mater.,Vol.19,2108-2111(2007)报道了放电过程中从FePO4到LiFePO4的相变动力学,发现是一维过程,而不是过去认为的三维过程。这就意味着,锂离子抽出/插入的便捷通道沿着[010]方向。
发明内容
本发明的目的在于提供一种具有(020)取向薄片状LiFePO4纳米晶的制备方法。通常晶体在生长过程中,不同的晶面生长需要不同的能量,需要能量较低的晶面生长较快,结果生成的晶体具有取向。所谓(020)取向是指晶体在生长过程中(020)晶面生长快,生成的晶体呈薄片状,薄片平行于(020)晶面。(020)取向薄片状LiFePO4纳米晶具有发达的锂离子抽出/插入的便捷通道。
本发明的技术方案:
水热合成具有发达的锂离子抽出/插入便捷通道的薄片状LiFePO4纳米晶,薄片状晶体尺寸在200纳米-5微米,厚度在50纳米-500纳米之间。
所述具有发达的锂离子抽出/插入便捷通道的薄片状LiFePO4纳米晶的水热合成方法,以廉价的水溶性亚铁盐(硫酸亚铁,氯化亚铁),磷酸,氢氧化锂为原料。水溶性亚铁盐、磷酸用量和氢氧化锂控制为摩尔比1∶1∶(2.5-3)。原料溶于水后再混合,混合后的产物在水热反应釜里处理。处理温度120-220℃,处理时间1-10小时。
本发明的优点是:
1、本发明方法可制备片状晶;
2、本发明可控制片状晶沿(020)取向,具有该取向的薄片状LiFePO4纳米晶具有发达的锂离子抽出/插入便捷通道;
3、本发明与高温固态反应法(文献1)比较,本发明在低温通过水热反应合成目标产物,水热反应温度在120-220℃之间,可大幅度节约能源;
4、本发明水热反应时间在1-10小时之间;
5、本发明可通过优化处理温度和时间来精确控制LiFePO4片状纳米晶的大小和厚度。
本发明提供了一种制备具有(020)取向的薄片状LiFePO4纳米晶的水热合成方法。具有该取向的薄片状LiFePO4纳米晶具有发达的锂离子抽出/插入的便捷通道。采用具有(020)取向薄片状LiFePO4纳米晶作为锂离子电池正极材料有利于提高电池的容量和充电/放电循环性能。
附图说明
图1a为LiFePO4沿y轴方向投影图。锂离子沿y轴方向,即[010]方向,具有最便捷的抽出/插入通道;图1b为LiFePO4沿z轴方向投影图;图1c为LiFePO4沿x轴方向投影图。
图2a为制备样品的X-射线衍射分析结果;图2b为计算模拟的X-射线衍射结果。
图3为扫描电镜照片,显示片状形貌。
图4a为透射电镜照片,显示结晶体有规则的结晶形貌;图4b为高分辨照片及其傅立叶变换图,清晰地揭示了片状晶是(020)取向,即片状晶的[010]方向垂直纸面。
图5a-图5d为计算模拟的具有不同取向的LiFePO4晶形貌。模拟的具有(020)取向的结晶体形貌与透射电镜观察的结果吻合。
具体实施方式
本发明具有(020)取向的薄片状LiFePO4纳米晶粉体具体制备方法是:把廉价的水溶性亚铁盐、氢氧化锂分别在不同容器中用蒸馏水溶解,将浓磷酸(市售磷酸,重量浓度85%)用蒸馏水稀释,浓磷酸很粘稠不容易从容器里倒出来,所以要用水稀释来降低黏度以便从容器里倒出来,具体是加约3倍浓磷酸体积的水。然后将水溶性亚铁盐溶液和磷酸溶液混合,再在强力搅拌下缓慢倒入氢氧化锂溶液。水溶性亚铁盐、磷酸和氢氧化锂用量控制为摩尔比1∶1∶(2.5-3)。最后将三者混合的产物转移到水热反应釜里在120-220℃保温1-10小时,取出放冷,过滤,干燥得到最终产物。本发明可以在较低温度下合成纯的LiFePO4,并且合成的纳米晶具有明显的(020)取向,具有该取向的薄片状纳米晶含有发达的锂离子抽出/插入通道。
下面通过实施例详述本发明。
实施例1
把原料硫酸亚铁、氢氧化锂分别在不同容器中用蒸馏水溶解,将浓磷酸用蒸馏水稀释。然后将硫酸亚铁溶液和磷酸溶液混合,再在强力搅拌下缓慢倒入氢氧化锂溶液。硫酸亚铁、磷酸和氢氧化锂用量控制为摩尔比1∶1∶3。最后将三者混合的产物转移到水热反应釜里在150℃保温5小时,取出放冷,过滤,真空干燥得到最终产物,获得具有(020)取向的薄片状LiFePO4纳米晶。本实施例中,薄片状晶体尺寸为1-4微米,厚度为150-250纳米。对制备的样品进行了X-射线衍射分析,结果表明是单一相LiFePO4(图2a)。与计算模拟的结果(图2b)比较,由本发明提出的方法制备的样品的(020)峰的强度明显高很多,表明有取向。扫描电镜观察,晶粒成片状(图3)。透射电镜的观察结果表明晶体结晶完整(图4a),高分辨照片及其傅立叶变换图清晰地揭示了晶是(020)取向(图4b)。与计算模拟的晶体形貌(图5a-d)比较,图5a为(200)和(210)晶面生长比较快的时候生成晶体的形貌,图5b为(020)晶面生长比较快的时候生成晶体的形貌,图5c为(200)比(101)晶面生长快的时候生成晶体的形貌,图5d为(200)和(101)晶面生长速度都比较快的时候生成晶体的形貌,充分证实片状晶是(020)取向。
实施例2
把原料氯化亚铁、氢氧化锂分别在不同容器中用蒸馏水溶解,将浓磷酸用蒸馏水稀释。然后将氯化亚铁溶液和磷酸溶液混合,再在强力机械搅拌下缓慢倒入氢氧化锂溶液。氯化亚铁、磷酸和氢氧化锂用量控制为摩尔比1∶1∶2.5。最后将三者混合的产物转移到水热反应釜里在120℃保温10小时,取出放冷,过滤,真空干燥得到最终产物,获得具有(020)取向的薄片状LiFePO4纳米晶。本实施例中,薄片状晶体尺寸为200纳米-1微米,厚度为50-200纳米。
实施例3
把原料硫酸亚铁、氢氧化锂分别在不同容器中用蒸馏水溶解,将浓磷酸用蒸馏水稀释。然后将硫酸亚铁溶液和磷酸溶液混合,再在强力搅拌下缓慢倒入氢氧化锂溶液。硫酸亚铁、磷酸和氢氧化锂用量控制为摩尔比1∶1∶3。最后将三者混合的产物转移到水热反应釜里在220℃保温1小时,取出放冷,过滤,充氮气干燥得到最终产物,获得具有(020)取向的薄片状LiFePO4纳米晶。本实施例中,薄片状晶体尺寸为2-5微米,厚度为200-500纳米。
Claims (5)
1、一种薄片状LiFePO4纳米晶粉体,其特征在于:通过水热合成制备出具有(020)取向的薄片状LiFePO4纳米晶,薄片状晶体尺寸在200纳米-5微米,厚度在50纳米-500纳米之间。
2、按照权利要求1所述的薄片状LiFePO4纳米晶粉体的制备方法,其特征在于:首先,把水溶性亚铁盐、氢氧化锂分别在不同容器中用蒸馏水溶解,将浓磷酸用蒸馏水稀释;然后,将水溶性亚铁盐溶液和磷酸溶液混合,再在强力搅拌下倒入氢氧化锂溶液,水溶性亚铁盐、磷酸和氢氧化锂用量控制为摩尔比1∶1∶(2.5-3);最后,将三者混合的产物转移到水热反应釜里在120-220℃保温1-10小时,取出放冷,过滤,干燥得到最终产物。
3、按照权利要求书2所述的薄片状LiFePO4纳米晶粉体的制备方法,其特征在于:所述水溶性亚铁盐为硫酸亚铁或氯化亚铁。
4、按照权利要求书2所述的薄片状LiFePO4纳米晶粉体的制备方法,其特征在于:所述强力搅拌为磁力搅拌或机械搅拌。
5、按照权利要求书2所述的薄片状LiFePO4纳米晶粉体的制备方法,其特征在于:所述干燥为真空干燥或充氮气保护干燥。
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