一、前言

锂电池可以分为多类，带铜铝极片的、带干性隔膜黑粉铝极片的、黑粉和铝极片的等等。对于不同种类的锂电池极片需要使用不同的方式进行处理。为了检测锂电池正极极片中的多种金属元素含量，选择微波消解对其进行前处理，探索最适合的消解参数，该方法还有回收率高、空白低等特点，有利于后续对多种无机元素的快速准确测定。

二、仪器与试剂

2.1、仪器

NAI-WB24 微波消解仪，赶酸器，分析天平(十万分之一)等。

2.2、试剂

硝酸(68%)，盐酸（37%），氢氟酸（40%），高氯酸（72%），

三、实验方法

3.1、消解

精确称取锂电池正极极片样品约0.1g（精确至0.1mg）置于消解罐底部，加入6mL硝酸、2mL氢氟酸和1mL高氯酸，静置15min左右，待无明显反应，组装消解罐，按照表一设置参数进行消解实验：

表一

实验结束，待冷却至60℃以下，消解罐转移至通风橱中缓慢打开，放置在赶酸器上150℃赶酸至近干，将消解液转移至烧杯中加水稀释，溶液中含有少量白色沉淀。

3.2、调整实验参数

重新称取正极极片样品约0.1g（精确至0.1mg）置于消解罐底部，加入3mL硝酸、3mL盐酸和4mL高氯酸，静置15min左右，待无明显反应，组装消解罐，按照表二设置参数进行消解实验：

表二

实验结束，待冷却至60℃以下，消解罐转移至通风橱中缓慢打开，放置在赶酸器上150℃赶酸至近干，将消解液转移至烧杯中加水稀释，溶液中仍含有少量白色沉淀。

四、结果与讨论

实验选择的锂电池正极极片样品，取样量为0.1g，选用的两种实验方法均无法将其完全溶解，建议过滤后或者取溶液上清液进行检测。

五、注意事项

1、高氯酸与有机物接触会剧烈反应，使用时应确保样品中不含有机物成分。

2、溶液中高氯酸与氢氟酸的含量较高，实验人员在处理时应做好防护，同时防止溶液接触玻璃器皿，以免造成腐蚀。

微波消解仪，赶酸器，分析天平(十万分之一)等。"]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658014668,"updatedBy":"144115226580519712","version":8}}}}},{"blockId":"iRucPzm4PnyBy2bkrRwBNy","blockSubtree":{"block":{"iRucPzm4PnyBy2bkrRwBNy":{"role":"editor","value":{"createdAt":1717658006312,"createdBy":"144115226580519712","enabled":true,"id":"iRucPzm4PnyBy2bkrRwBNy","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["2.2、试剂"]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658006312,"updatedBy":"144115226580519712","version":1}}}}},{"blockId":"ZhWfvZ81RxYk2bvarhuxtk","blockSubtree":{"block":{"ZhWfvZ81RxYk2bvarhuxtk":{"role":"editor","value":{"createdAt":1717658006314,"createdBy":"144115226580519712","enabled":true,"id":"ZhWfvZ81RxYk2bvarhuxtk","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["硝酸"],["(68%)，盐酸（37%），氢氟酸（40%），高氯酸（72%），"]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658006314,"updatedBy":"144115226580519712","version":1}}}}},{"blockId":"wzGM6a4i8ROoDvR7frc6Bm","blockSubtree":{"block":{"wzGM6a4i8ROoDvR7frc6Bm":{"role":"editor","value":{"createdAt":1717658006315,"createdBy":"144115226580519712","enabled":true,"id":"wzGM6a4i8ROoDvR7frc6Bm","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["三、",[["b"]]],["实验方法",[["b"]]]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658006315,"updatedBy":"144115226580519712","version":1}}}}},{"blockId":"bg2JIweub2pjqYbtKlWcBZ","blockSubtree":{"block":{"bg2JIweub2pjqYbtKlWcBZ":{"role":"editor","value":{"createdAt":1717658006317,"createdBy":"144115226580519712","enabled":true,"id":"bg2JIweub2pjqYbtKlWcBZ","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["3.1、消解"]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658006317,"updatedBy":"144115226580519712","version":1}}}}},{"blockId":"Q1pH3Zxdmi6wUeQ18Dv0aJ","blockSubtree":{"block":{"Q1pH3Zxdmi6wUeQ18Dv0aJ":{"role":"editor","value":{"createdAt":1717658006318,"createdBy":"144115226580519712","enabled":true,"id":"Q1pH3Zxdmi6wUeQ18Dv0aJ","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["精确称取锂电池正极极片样品约"],["0.1g（精确至0.1mg）置于消解罐底部，"],["加入"],["6mL硝酸、2mL氢氟酸和1mL高氯酸，静置15min左右，待无明显反应，组装消解罐，按照表一设置参数进行消解实验："]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658006318,"updatedBy":"144115226580519712","version":1}}}}},{"blockId":"0ZKFNe31JIfYHssOV05QNU","blockSubtree":{"block":{"0ZKFNe31JIfYHssOV05QNU":{"role":"editor","value":{"createdAt":1717658006320,"createdBy":"144115226580519712","enabled":true,"id":"0ZKFNe31JIfYHssOV05QNU","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["表一"]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658006320,"updatedBy":"144115226580519712","version":1}}}}},{"blockId":"YWLwpTraSRLhLXNiOutfiO","blockSubtree":{"block":{"YWLwpTraSRLhLXNiOutfiO":{"role":"editor","value":{"children":["ih4n1zUR7cVkEWkkkXXYY2","sgutto3lYAX0cqZW8hJtE1","9azlxaNak6uxFq03eM6Ns1","ac4a6pXzROBHHTkAjvp3Hl"],"createdAt":1717658006328,"createdBy":"144115226580519712","enabled":true,"id":"YWLwpTraSRLhLXNiOutfiO","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"tableColumnOrder":["ZFz8Zi","PI0w-F","lpB8wa","GwqMuc"],"tableColumnWidthMap":{"GwqMuc":120,"PI0w-F":120,"ZFz8Zi":120,"lpB8wa":120}},"spaceId":"300000000$dSaDzNIFZGrk","type":"simple_table","updatedAt":1717658006328,"updatedBy":"144115226580519712","version":1}},"k22wwzf3eZHrvkT7dyvWkY":{"role":"editor","value":{"children":["aDZxYwtlWoGSVPYQTbwK0d"],"type":"simple_table_cell","id":"k22wwzf3eZHrvkT7dyvWkY","version":1,"enabled":true,"parentId":"ih4n1zUR7cVkEWkkkXXYY2","parentTable":"block","props":{"columnKey":"ZFz8Zi"}}},"aDZxYwtlWoGSVPYQTbwK0d":{"role":"editor","value":{"type":"text","id":"aDZxYwtlWoGSVPYQTbwK0d","version":1,"enabled":true,"parentId":"k22wwzf3eZHrvkT7dyvWkY","parentTable":"block","props":{"title":[["阶段"]],"textAlign":"left"}}},"G4M5vfO1HL0q6DiTyi7GLT":{"role":"editor","value":{"children":["qA5e009GbW4dasduvH9b5B"],"type":"simple_table_cell","id":"G4M5vfO1HL0q6DiTyi7GLT","version":1,"enabled":true,"parentId":"ih4n1zUR7cVkEWkkkXXYY2","parentTable":"block","props":{"columnKey":"PI0w-F"}}},"qA5e009GbW4dasduvH9b5B":{"role":"editor","value":{"type":"text","id":"qA5e009GbW4dasduvH9b5B","version":1,"enabled":true,"parentId":"G4M5vfO1HL0q6DiTyi7GLT","parentTable":"block","props":{"title":[["温度"],["/℃"]],"textAlign":"left"}}},"HPywQsOtrmN3KJ6BCSywIC":{"role":"editor","value":{"children":["rnqbkoeNCsFT54BRgffIvq"],"type":"simple_table_cell","id":"HPywQsOtrmN3KJ6BCSywIC","version":1,"enabled":true,"parentId":"ih4n1zUR7cVkEWkkkXXYY2","parentTable":"block","props":{"columnKey":"lpB8wa"}}},"rnqbkoeNCsFT54BRgffIvq":{"role":"editor","value":{"type":"text","id":"rnqbkoeNCsFT54BRgffIvq","version":1,"enabled":true,"parentId":"HPywQsOtrmN3KJ6BCSywIC","parentTable":"block","props":{"title":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