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(duì)于不同種類的鋰電池極片需要使用不同的方式進(jìn)行處理。為了檢測(cè)鋰電池正極極片中的多種金屬元素含量，選擇微波消解對(duì)其進(jìn)行前處理，探索最適合的消解參數(shù)，該方法還有回收率高、空白低等特點(diǎn)，有利于后續(xù)對(duì)多種無機(jī)元素的快速準(zhǔn)確測(cè)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(shí)驗(yàn)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(yīng)，組裝消解罐，按照表一設(shè)置參數(shù)進(jìn)行消解實(shí)驗(yàn)：

表一

實(shí)驗(yàn)結(jié)束，待冷卻至60℃以下，消解罐轉(zhuǎn)移至通風(fēng)櫥中緩慢打開，放置在趕酸器上150℃趕酸至近干，將消解液轉(zhuǎn)移至燒杯中加水稀釋，溶液中含有少量白色沉淀。

3.2、調(diào)整實(shí)驗(yàn)參數(shù)

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(yīng)，組裝消解罐，按照表二設(shè)置參數(shù)進(jìn)行消解實(shí)驗(yàn)：

表二

實(shí)驗(yàn)結(jié)束，待冷卻至60℃以下，消解罐轉(zhuǎn)移至通風(fēng)櫥中緩慢打開，放置在趕酸器上150℃趕酸至近干，將消解液轉(zhuǎn)移至燒杯中加水稀釋，溶液中仍含有少量白色沉淀。

四、結(jié)果與討論

實(shí)驗(yàn)選擇的鋰電池正極極片樣品，取樣量為0.1g，選用的兩種實(shí)驗(yàn)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(jìn)行檢測(cè)。

五、注意事項(xiàng)

1、高氯酸與有機(jī)物接觸會(huì)劇烈反應(yīng)，使用時(shí)應(yīng)確保樣品中不含有機(jī)物成分。

2、溶液中高氯酸與氫氟酸的含量較高，實(shí)驗(yàn)人員在處理時(shí)應(yīng)做好防護(hù)，同時(shí)防止溶液接觸玻璃器皿，以免造成腐蝕。

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