一、前言

鋰電池可以分為多類，帶銅鋁極片的、帶干性隔膜黑粉鋁極片的、黑粉和鋁極片的等等。對于不同種類的鋰電池極片需要使用不同的方式進行處理。為了檢測鋰電池正極極片中的多種金屬元素含量，選擇微波消解對其進行前處理，探索最適合的消解參數，該方法還有回收率高、空白低等特點，有利于后續(xù)對多種無機元素的快速準確測定。

二、儀器與試劑

2.1、儀器

NAI-WB24 微波消解儀，趕酸器，分析天平(十萬分之一)等。

2.2、試劑

硝酸(68%)，鹽酸（37%），氫氟酸（40%），高氯酸（72%），

三、實驗方法

3.1、消解

精確稱取鋰電池正極極片樣品約0.1g（精確至0.1mg）置于消解罐底部，加入6mL硝酸、2mL氫氟酸和1mL高氯酸，靜置15min左右，待無明顯反應，組裝消解罐，按照表一設置參數進行消解實驗：

表一

實驗結束，待冷卻至60℃以下，消解罐轉移至通風櫥中緩慢打開，放置在趕酸器上150℃趕酸至近干，將消解液轉移至燒杯中加水稀釋，溶液中含有少量白色沉淀。

3.2、調整實驗參數

重新稱取正極極片樣品約0.1g（精確至0.1mg）置于消解罐底部，加入3mL硝酸、3mL鹽酸和4mL高氯酸，靜置15min左右，待無明顯反應，組裝消解罐，按照表二設置參數進行消解實驗：

表二

實驗結束，待冷卻至60℃以下，消解罐轉移至通風櫥中緩慢打開，放置在趕酸器上150℃趕酸至近干，將消解液轉移至燒杯中加水稀釋，溶液中仍含有少量白色沉淀。

四、結果與討論

實驗選擇的鋰電池正極極片樣品，取樣量為0.1g，選用的兩種實驗方法均無法將其完全溶解，建議過濾后或者取溶液上清液進行檢測。

五、注意事項

1、高氯酸與有機物接觸會劇烈反應，使用時應確保樣品中不含有機物成分。

2、溶液中高氯酸與氫氟酸的含量較高，實驗人員在處理時應做好防護，同時防止溶液接觸玻璃器皿，以免造成腐蝕。

微波消解儀，趕酸器，分析天平(十萬分之一)等。"]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658014668,"updatedBy":"144115226580519712","version":8}}}}},{"blockId":"iRucPzm4PnyBy2bkrRwBNy","blockSubtree":{"block":{"iRucPzm4PnyBy2bkrRwBNy":{"role":"editor","value":{"createdAt":1717658006312,"createdBy":"144115226580519712","enabled":true,"id":"iRucPzm4PnyBy2bkrRwBNy","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["2.2、試劑"]]},"spaceId":"300000000$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%)，鹽酸（37%），氫氟酸（40%），高氯酸（72%），"]]},"spaceId":"300000000$dSaDzNIFZGrk","type":"text","updatedAt":1717658006314,"updatedBy":"144115226580519712","version":1}}}}},{"blockId":"wzGM6a4i8ROoDvR7frc6Bm","blockSubtree":{"block":{"wzGM6a4i8ROoDvR7frc6Bm":{"role":"editor","value":{"createdAt":1717658006315,"createdBy":"144115226580519712","enabled":true,"id":"wzGM6a4i8ROoDvR7frc6Bm","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["三、",[["b"]]],["實驗方法",[["b"]]]]},"spaceId":"300000000$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$dSaDzNIFZGrk","type":"text","updatedAt":1717658006317,"updatedBy":"144115226580519712","version":1}}}}},{"blockId":"Q1pH3Zxdmi6wUeQ18Dv0aJ","blockSubtree":{"block":{"Q1pH3Zxdmi6wUeQ18Dv0aJ":{"role":"editor","value":{"createdAt":1717658006318,"createdBy":"144115226580519712","enabled":true,"id":"Q1pH3Zxdmi6wUeQ18Dv0aJ","parentId":"ZwGStta1zb9vHOu3qpeJjl","parentTable":"block","props":{"title":[["精確稱取鋰電池正極極片樣品約"],["0.1g（精確至0.1mg）置于消解罐底部，"],["加入"],["6mL硝酸、2mL氫氟酸和1mL高氯酸，靜置15min左右，待無明顯反應，組裝消解罐，按照表一設置參數進行消解實驗："]]},"spaceId":"300000000$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":[["階段"]],"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":[["溫度"],["/℃"]],"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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