CN111485278A - 一种电极活性材料单晶的固相反应合成方法 - Google Patents

一种电极活性材料单晶的固相反应合成方法 Download PDF

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CN111485278A
CN111485278A CN202010233435.6A CN202010233435A CN111485278A CN 111485278 A CN111485278 A CN 111485278A CN 202010233435 A CN202010233435 A CN 202010233435A CN 111485278 A CN111485278 A CN 111485278A
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杨建文
王陆阳
刘鑫鑫
熊伟雄
仝蒙恩
黄斌
肖顺华
陈权启
李延伟
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Guilin University of Technology
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Abstract

本发明提供了一种电极活性材料单晶的固相反应合成方法。将市售过渡金属氧化物或过渡金属盐，与氧化锂或锂盐或氢氧化锂，以及掺杂元素化合物，按化学计量比称取物料并置于球磨机或高速分散机中，按(9.0‑2.0)∶(1.0‑8.0)固液重量比加入高效混合剂，开机混料0.5‑24小时，筛除研磨球，将浆状混合物干燥并回收混合剂液体组分，将干燥后的混合物研磨成粉末并盛装于烧舟中，或将浆料直接盛于烧舟中，置于焙烧炉内，通入反应气氛，采用每分钟1‑20℃的升温速率加热至200‑1200℃，保温0.5‑48小时，自然冷却至50‑100℃，出料，粉碎，过筛，包装，得到单晶形貌电极活性材料。本发明为锂离子电池电极活性材料单晶的低成本制备提供了新途径。

Description

一种电极活性材料单晶的固相反应合成方法
技术领域
本发明涉及锂离子电池材料领域，特别是采用固相法合成单晶形貌电极活性材料。
背景技术
锂离子电池综合性能优异，在日用电子产品中已经得到广泛应用，随着电动汽车、新能源储存及智能电网等市场需求的快速增长，具有高容量、高稳定、低成本、安全、环保等性能的电极活性材料及其相关技术进步成为锂离子电池发展的关键。在锂离子电池充放电过程中，活性材料与电解质溶液之间一般均会生成固体电解质膜(SEI)，SEI膜的组成、结构和稳定性对电极活性材料的利用率、充放电速率、循环寿命、可靠性等均具有至关重要的影响。SEI膜的性能在很大程度上与电极活性材料的表面性质有关，单晶材料具有晶体结构发育良好，表面不饱和键少，SEI膜性能稳定等优点，因此，单晶形貌电极活性材料倍受锂离子电池厂商青睐。
目前，锂离子电池电极活性材料，如：钴酸锂、镍酸锂、锰酸锂、镍锰酸锂、三元正极材料、高镍正极材料、聚阴离子正极材料等，一般均采用共沉淀、溶胶-凝胶或水热法先制得特殊性能前驱体，然后经过高温反应才能制得单晶产物，或者采用熔融盐法制备，这些单晶制备方法均存在较复杂的前、后期处理工序，导致单晶材料的生产成本偏高。本发明通过对传统固相法小幅改进，实现了电极活性材料单晶的固相法制备，有望对锂离子电池高性能电极活性材料的低成本制造产生积极作用。
发明内容
本发明的目的是通过对传统固相法工艺环节的改进，实现锂离子电池电极活性材料单晶的短工序低成本制备。
具体步骤为：
将市售过渡金属氧化物或过渡金属盐，与氧化锂或锂盐或氢氧化锂，以及掺杂元素化合物，按化学计量比称取物料并置于球磨机或高速分散机中，按(9.0-2.0)∶(1.0-8.0)固液重量比加入高效混合剂，开机混料0.5-24小时，筛除研磨球，将浆状混合物干燥并回收混合剂液体组分，将干燥后的混合物研磨成粉末并盛装于烧舟中，或将浆料直接盛于烧舟中，置于焙烧炉内，通入反应气氛，采用每分钟1-20℃的升温速率加热至200-1100℃，保温0.5-48小时，自然冷却至50-100℃，出料，粉碎，过筛，包装，得到单晶形貌电极活性材料。
附图说明
图1本发明实施例1 LiNi0.5Mn1.5O4单晶正极材料的SEM照片。
图2本发明实施例1 LiNi0.5Mn1.5O4单晶正极材料的XRD图谱。
图3本发明实施例2 Li1.2Ni0.13Co0.13Mn0.54O2单晶正极材料的SEM照片。
图4本发明实施例2 Li1.2Ni0.13Co0.13Mn0.54O2单晶正极材料的XRD图谱。
图5本发明实施例3 LiNi0.6Mn0.2Co0.2O2单晶正极材料的SEM照片。
图6本发明实施例3 LiNi0.6Mn0.2Co0.2O2单晶正极材料的XRD图谱。
图7本发明实施例4 Li4Ti5O12单晶负极材料的SEM照片。
图8本发明实施例4 Li4Ti5O12单晶负极材料的XRD图谱。
实施例1：
分别称取分析纯级化学试剂碳酸锂1.9592克、二氧化锰7.6710克、一氧化镍1.9055克置于玛瑙罐中，加入10毫升去离子水，在SFM-3型高速振动球磨机上混料0.5小时，用镊子挑出玛瑙球，将反应物浆料置于80℃干燥箱中烘干，手工研磨10分钟，盛于刚玉方舟中并置于马弗炉内，以10℃/分钟升温速率加热至800℃，保温24小时，自然冷却至50℃，出料，用玛瑙研钵手工研磨10分钟，得到LiNi0.5Mn1.5O4单晶正极材料样品。图1、图2分别为LiNi0.5Mn1.5O4单晶样品的SEM照片和XRD图谱，其八面体单晶特征明显，分散性好，为纯相、尖晶石型晶体结构。
实施例2：分别称取分析纯级化学试剂碳酸锂2.2850克、一氧化镍0.4904克、四氧化三钴0.5321克、二氧化锰2.3953克置于玛瑙罐中，加入5毫升去离子水，在SFM-3型高速振动球磨机上混料1.5小时，用镊子挑出玛瑙球，将反应物浆料置于80℃干燥箱中烘干，手工研磨10分钟，盛于刚玉方舟中并置于马弗炉内，以10℃/分钟升温速率加热至850℃，保温32小时，自然冷却至50℃，出料，用玛瑙研钵手工研磨10分钟，得到Li1.2Ni0.13Co0.13Mn0.54O2单晶正极材料样品。图3、图4分别为Li1.2Ni0.13Co0.13Mn0.54O2单晶样品的SEM照片和XRD图谱，其八面体单晶特征明显，分散性好，为α-NaFeO2型层状晶体结构，在2θ衍射角20°-23°范围存在弱的超晶格特征峰。
实施例3：
分别称取分析纯级化学试剂碳酸锂3.2572克、一氧化镍1.8107克、四氧化三钴1.9458克、四水乙酸锰1.9805克置于玛瑙罐中，加入10毫升(1+1)去离子水-乙醇溶液，在SFM-3型高速振动球磨机上混料1.0小时，用镊子挑出玛瑙球，将反应物浆料置于80℃干燥箱中烘干，手工研磨10分钟，盛于刚玉方舟中并置于马弗炉内，以10℃/分钟升温速率加热至850℃，保温24小时，自然冷却至50℃，出料，用玛瑙研钵手工研磨10分钟，得到LiNi0.6Mn0.2Co0.2O2单晶正极材料样品。图5、图6分别为LiNi0.6Mn0.2Co0.2O2单晶样品的SEM照片和XRD图谱，其八面体单晶特征明显，分散性好，为纯相、六方晶系α-NaFeO2型晶体结构。
实施例4：
分别称取分析级纯化学试剂碳酸锂3.8700克、二氧化钛10.0874克置于玛瑙罐中，加入5毫升去离子水和0.5000克乙炔黑，在SFM-3型高速振动球磨机上混料1.0小时，用镊子挑出玛瑙球，将反应物浆料置于80℃干燥箱中烘干，手工研磨10分钟，盛于刚玉方舟中并管式炉内，通入氩气气氛，以10℃/分钟升温速率加热至850℃，保温16小时，自然冷却至50℃，出料，再用原混料球磨机球磨30分钟，得到Li4Ti5O12单晶负极材料样品。图7、图8分别为Li4Ti5O12单晶样品的SEM照片和XRD图谱，其单晶颗粒分散性好，为纯相、尖晶石结构。

Claims (7)

1.一种电极活性材料单晶的固相反应合成方法，其特征在于具体步骤为：将市售过渡金属氧化物或过渡金属盐，与氧化锂或锂盐或氢氧化锂，以及掺杂元素化合物，按化学计量比称取物料并置于球磨或高速分散机中，按(9.0-2.0)∶(1.0-8.0)固液重量比加入高效混合剂，开机混料0.5-24小时，筛除研磨球，将浆状混合物干燥并回收混合剂液体组分，将干燥后的混合物研磨成粉末并盛装于烧舟中，或将浆料直接盛于烧舟中，置于焙烧炉内，通入反应气氛，采用每分钟1-20℃的升温速率加热至200-1100℃，保温0.5-48小时，自然冷却至50-100℃，出料，粉碎，过筛，包装，得到单晶形貌电极活性材料。
2.根据权利要求1所述过渡金属氧化物或过渡金属盐，包括锰、铁、钴、镍、铜、锌、钛、钒、铌、钨、钼、铬的氧化物或盐的一种或几种。
3.根据权利要求1所述锂盐，包括碳酸锂、乙酸锂、硝酸锂、硫酸锂、氯化锂、氟化锂、硼酸锂、磷酸锂中一种或几种。
4.根据权利要求1所述掺杂元素化合物包括钙、镁、铝、钾、钠、稀土元素等的氢氧化物、氧化物、有机酸盐、碳酸盐、氟化物，或权力2中的过渡金属化合物。
5.根据权利要求1所述反应气氛主要包括空气、氧气、氩气、氮气、二氧化碳等加热炉反应气氛。
6.根据权利要求1所述电极活性材料主要是指锂离子电池正、负极活性材料、也适用于这些材料用作钠离子电池、钾离子电池、镁离子电池或锌离子电池等的电极活性材料。
7.根据权利要求1所述高效混合剂主要包括水，或各种碳材料、淀粉、葡萄糖、蔗糖、纤维素、乙醇、乙二醇、丙三醇、表面活性剂等的水分散液。
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CN113307311A (zh) * 2021-04-08 2021-08-27 桂林理工大学 一种Mg2+双重掺杂提高镍酸锂正极材料电化学性能的制备方法

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