CN111233471A - 一种四方钨青铜结构Mo3Nb2O14材料的制备方法及其应用 - Google Patents

一种四方钨青铜结构Mo3Nb2O14材料的制备方法及其应用 Download PDF

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CN111233471A
CN111233471A CN202010077441.7A CN202010077441A CN111233471A CN 111233471 A CN111233471 A CN 111233471A CN 202010077441 A CN202010077441 A CN 202010077441A CN 111233471 A CN111233471 A CN 111233471A
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tungsten bronze
bronze structure
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方雪
卢锋奇
匡小军
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Guilin University of Technology
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Abstract

本发明公开了一种四方钨青铜结构Mo3Nb2O14材料的制备方法及其应用。按照MoO3与Nb2O5的摩尔比为3:2称取原料；将称取的原料放于玛瑙研钵中进行研磨混合，然后用红外灯加热干燥，重复研磨干燥步骤3~5次，将获得的粉末用4 MPa的压力压制成直径为10 mm的片，将片放入玻璃管中，采用真空封管的技术进行密封，然后置于马弗炉中以5℃/min的升温速率升温至700℃保温12 h进行烧结，即制得四方钨青铜结构Mo3Nb2O14材料。该材料应用于锂离子电池负极材料。本发明具有制备方法简单，原料丰富，无污染等优点，且首次提出利用真空合成技术制造氧空位的合成方法，所得到的Mo3Nb2O14富含氧空位，当作为锂离子负极材料时，该氧空位能显著提高材料的电化学性能。

Description

一种四方钨青铜结构Mo3Nb2O14材料的制备方法及其应用
技术领域
本发明属于锂离子电池负极材料技术领域，具体涉及一种四方钨青铜结构Mo3Nb2O14材料的制备方法及其应用。
背景技术
目前，商业化较多的锂离子电池的负极材料依旧是碳基材料，而这类材料所面临的易产生枝晶存在安全隐患的问题依旧没有得到解决。开发新型适用于锂离子电池的负极材料迫在眉睫。
钨青铜及类钨青铜结构中存在大量的通道，为锂离子的储存提供了足够的空间，有望成为下一代负极材料的重点研究备选对象。而Mo5O14型四方钨青铜结构的氧化物Mo3Nb2O14氧化物虽可作为锂离子电池负极材料，但由于其自身导电率差的特点，影响了其具有优异的电化学性能，因此便提出通过制备含有氧缺陷的Mo3Nb2O14在很大程度上提高材料导电率从而提高了电化学性能。此结构氧化物是首次提出的采用真空合成技术制造氧空位提高电化学性能的方法简单并且十分新颖。
发明内容
针对目前就氧化物材料作为锂离子电池负极材料的研究，本发明的目的在于提供一种四方钨青铜结构Mo3Nb2O14材料的制备方法及其应用。
本发明的材料具有大量通道可以提供足够的锂离子储存空间实现锂离子的快速传输。同时本材料中的Mo和Nb两种元素具有多电子对的转移，使得本材料具有较高的理论容量。
本发明为了提高材料本身的导电率提供了一种在真空条件下制备含有氧空位的氧化物从而提高此材料作为锂离子电池负极材料的电化学性能的技术方案。
制备四方钨青铜结构Mo3Nb2O14材料的具体步骤为：
（1）按照MoO3与Nb2O5的摩尔比为3:2称取原料；将称取的原料放于玛瑙研钵中进行混合，加入无水乙醇进行研磨，然后用红外灯加热干燥，重复上述研磨干燥步骤3~5次，获得粉末。
（2）将步骤（1）获得的粉末用4 MPa的压力压制成直径为10 mm的片，将压制好的片放入玻璃管中，采用真空封管的技术进行密封，然后置于马弗炉中以5 ℃/min的升温速率升温至700 ℃保温12 h进行烧结，即制得四方钨青铜结构Mo3Nb2O14材料。
本发明的四方钨青铜结构Mo3Nb2O14材料应用于锂离子电池负极材料。
本发明所采用的利用真空合成技术制备含有氧空位的Mo3Nb2O14材料，氧空位可作为潜在浅层供氧体，从而增加载流子浓度从而提高材料本身的导电率，继而提高了材料作为锂离子电池负极材料的电化学性能。由于具有大量的通道，可以提供大量储存锂离子的空间已经便于锂离子的传输，此类材料适用于锂离子电池的负极材料，再解决材料本身电导率差的问题后，此类材料展现出较好的倍率性能及循环性能。
本发明与现有技术相比，本发明的技术方案带来的有益技术效果：本发明所提供的传统固相法合成技术是一种简单易操作，节约资源的制备方法，并且在真空中直接制备含有氧空位的技术工艺简易且十分新颖。制得的材料是具有多通道的 Mo5O14 型四方钨青铜结构材料。本发明提出的此制造氧空位提高材料性能提供了新思路，具有普遍适用性，在能源储存的发展上就有较大的意义。解决了大部分氧化物由于自身导电率差限制作为锂离子电池负极材料性能的问题，此方法可推广应用于其他氧化物中，具有普适性。
附图说明
图1是本发明实施例制得的四方钨青铜结构Mo3Nb2O14材料的XRD图。
图2是本发明实施例制得的四方钨青铜结构Mo3Nb2O14材料的扫描电镜图。
图3是不含氧空位的Mo3Nb2O14材料和本发明实施例制得的四方钨青铜结构Mo3Nb2O14材料的Mo元素的XPS图。
图4是不含氧空位的Mo3Nb2O14材料和本发明实施例制得的四方钨青铜结构Mo3Nb2O14材料的O 元素的XPS图。
图5是本发明实施例制得的四方钨青铜结构Mo3Nb2O14材料在氧气气氛下升温的热重图。
图6是不含氧空位的Mo3Nb2O14材料和本发明实施例制得的四方钨青铜结构Mo3Nb2O14材料在不同电流密度下的倍率循环图。
图7是不含氧空位的Mo3Nb2O14材料和本发明实施例制得的四方钨青铜结构Mo3Nb2O14材料在100 mA g-1电流密度下循环性能对比图。
具体实施方式
下面将结合实例对本发明做进一步的详细说明，但本发明内容不仅仅只局限于以下的实例。
实施例：
1) 称取0.619 g MoO3与0.3810 g Nb2O5，将称取的原料粉末放于玛瑙研钵中进行混合，加入适量无水乙醇进行研磨，然后用红外灯加热干燥，重复上述研磨干燥步骤3~5次，获得粉末。
2) 将研磨好的粉末用4 Mpa的压力压制成直径为10 mm的片。
3) 将压制好的片放入干净的玻璃管中；将玻璃管采用真空封管的技术进行密封，然后置于马弗炉中以5 ℃/min的升温速率升温至700 ℃保温12 h进行烧结，即制得四方钨青铜结构Mo3Nb2O14材料。
本实施例制得的四方钨青铜结构Mo3Nb2O14材料含有氧空位，对其表征如下：
图1是该材料的XRD图。表明此材料属于四方钨青铜TTB相，空间群为Pbam，也表明该物质为纯相，不存在其他杂质相。
图2是该材料的SEM图。可以看出此材料的形貌为长为1 μm左右的短棒。
图3和图4是该材料与不含氧空位的Mo3Nb2O14材料的XPS图，通过各个元素价态分布的对比可以得知该材料确实存在氧空位。
图5为该材料在氧气气氛下升温到800 ℃的质量变化图，说明此材料中确实存在氧空位，并且含量为2.05 %。
本实施例制得的四方钨青铜结构Mo3Nb2O14材料应用于作为锂离子电池负极材料，组装成纽扣式半电池，并对其性能进行测试：称取上述材料80 wt %，10 wt % 粘结剂PVDF，导电剂碳黑10 wt％混合经研磨充分。将研磨好的上述粉末加入NMP溶液中搅拌均匀成黑色糊状浆料，然后将搅拌好的电极浆料在自动涂布机上均匀的涂在铜箔上。之后放置在真空干燥箱中100 ℃干燥12 h。将烘干的电极片用切片机切成直径为12 mm的圆形电极片，再将其在压片机上4 MPa的压力下压制10 s制成电极片。选取锂片作为半电池的对电极和参比电极极，隔膜为Celgard 2400，使用的电解液是电解液为浓度1 mol/L的LiPF6溶于碳酸乙烯酯（EC）和碳酸二甲酯（DMC）1:1体积混合的有机溶液。电池的组装在手套箱中进行，水氧含量均小于1 ppm。组装CR2030型号的的扣式电池最后将组装好的电池静置2小时左右便可进行电化学测试。其电化学性能如图6和图7所示，可以看出本实施例制备的四方钨青铜结构Mo3Nb2O14材料相比不含有氧空位的材料在任何电流密度下比容量明显要高出很多，并且本实施例制备的四方钨青铜结构Mo3Nb2O14材料的容量在经过200次循环以后还能保持在150 mAh g-1，相比较没有氧空位的材料容量得到了很大的提高。

Claims (2)

1.一种四方钨青铜结构Mo3Nb2O14材料的制备方法，其特征在于具体步骤为：
（1）按照MoO3与Nb2O5的摩尔比为3:2称取原料；将称取的原料放于玛瑙研钵中进行混合，加入无水乙醇进行研磨，然后用红外灯加热干燥，重复上述研磨干燥步骤3~5次，获得粉末；
（2）将步骤（1）获得的粉末用4 MPa的压力压制成直径为10 mm的片，将压制好的片放入玻璃管中，采用真空封管的技术进行密封，然后置于马弗炉中以5 ℃/min的升温速率升温至700 ℃保温12 h进行烧结，即制得四方钨青铜结构Mo3Nb2O14材料。
2.一种如权利要求1所述的制备方法制备的四方钨青铜结构Mo3Nb2O14材料的应用，其特征在于：该四方钨青铜结构Mo3Nb2O14材料应用于锂离子电池负极材料。
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