磷酸鐵鋰具有熱穩(wěn)定性好、充放電效率高、環(huán)境友好、價格便宜的特點，被認為是極有潛力的鋰離子電池，特別是動力鋰離子電池正極材料。目前，研究者們廣泛采用高溫固相法、液相法、共沉淀法、微波加熱等方法來合成磷酸鐵鋰，并通過碳包覆或摻雜等方式來提高材料的電導(dǎo)率以發(fā)問其電化學(xué)性能。噴霧干燥法是從料液中獲得超微干粉的一種較好的方法這種由液態(tài)經(jīng)過霧化和干燥在瞬間直接變成粉體的過程，已經(jīng)廣泛應(yīng)用于食品、醫(yī)藥、電子和材料等一些與原材料顆粒大小密切相關(guān)的領(lǐng)域。與其他一些粉末生產(chǎn)相比較，噴霧干燥法具有如下一些優(yōu)點︰

1.可以保證組分分布均勻，精確控制化學(xué)計量比，適合制備多組分的復(fù)合粉末;

2．保證粉末具有較高的純度和活性;

3．噴霧赤豆工序簡單，生產(chǎn)過程連續(xù)，產(chǎn)能大，生產(chǎn)效率高，有利于工業(yè)化生產(chǎn);

4．噴霧干燥的顆粒大都呈規(guī)則的球形，有利于提高粉末的振實密度。

二、實驗用品

(一）器材

(1)噴霧干燥機。

(2)球磨機。

(二）試劑

葡萄糖

(三)材料

磷酸鐵碳酸鋰。

三、LiFePO4/C材料合成。

具體工藝流程如下:

1．按化學(xué)計量比稱取正磷酸鐵和碳酸鋰，以葡萄糖為還原劑和碳添加劑，添加適量葡萄糖;

2.以去離子水為介質(zhì)球磨1h,球磨轉(zhuǎn)速為120r/min;將球磨后的物料進行噴霧干燥﹔

3.將噴霧干燥后所得的粉末裝入瓷舟，置于高純氮氣保護的管式電爐中，于600~800度下

熱處理數(shù)小時;

4.冷卻至室溫，所得灰黑色粉末即為LiFePO4/C材料。

四、料液濃度的影響。

顆粒粒徑隨著料液固含量的降低而減小，當(dāng)固含量降低到20%以下時，顆粒粒徑隨固含量的變化比較緩慢。固含量越低，越有利于合成顆粒細小的磷酸鐵鋰材料，這是因為料液濃度越高，其粘度也越高，在噴霧干燥過程中形成的霧滴也變大。這使得霧化后的液滴與氣體接觸的面積減小，干燥后形成的顆粒粒徑就變大。同時，高濃度的料液還容易導(dǎo)致顆粒團聚結(jié)塊現(xiàn)象的發(fā)生，其原因在于霧滴過大，尚末干燥就被高速離心霧化器甩到干燥塔內(nèi)壁，導(dǎo)致顆粒結(jié)塊和沾壁，在固含量30%時這種現(xiàn)象比較明顯。

五、進料速度對粒度的影響

隨著進料速度的增大，顆粒粒徑逐漸變大。進料速度的增大引起霧滴的變大和霧滴數(shù)量的增加，霧滴在干燥前相互碰撞發(fā)生聚合，導(dǎo)致成核數(shù)量的減少，產(chǎn)品粒徑變大。

五、結(jié)果與分析

1.采用噴霧干燥-熱還原法合成了磷酸鐵鋰材料，噴霧干燥能有效抑制組分的偏析和顆粒的長大，保證物料實現(xiàn)很好的混合均勻度，有利于合成更純更細的磷酸鐵鋰正極材料;

⒉噴霧干燥過程對材料顆粒有較大的影響，低固含量，低進料速率有利小粒徑材料的合成;

3噴霧干燥所得到的材料形狀規(guī)則，顆粒細小且成球狀，對改善材料的電化學(xué)性能有很大意義。

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