CN106946553B - 一种低成本长寿命的陶瓷匣钵及其制备方法 - Google Patents

一种低成本长寿命的陶瓷匣钵及其制备方法 Download PDF

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CN106946553B
CN106946553B CN201710211686.2A CN201710211686A CN106946553B CN 106946553 B CN106946553 B CN 106946553B CN 201710211686 A CN201710211686 A CN 201710211686A CN 106946553 B CN106946553 B CN 106946553B
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徐晓虹
张亚祥
吴建锋
刘鑫坤
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Wuhan University of Technology WUT
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Abstract

本发明涉及一种低成本长寿命的陶瓷匣钵及其制备方法，其用于烧结锂化合物的粉体，陶瓷匣钵基材由以下重量百分含量的原料组成：滑石20～25％，铝矾土15～20％，60～65目镁铝尖晶石5～35％，100～120目镁铝尖晶石15～45％，堇青石5～15％。本发明以部分天然矿物滑石和铝矾土为原料制备陶瓷匣钵，成本节约1/3以上，采用本发明方法制备得到的陶瓷匣钵能够经受50次热震循环而不开裂，抗热震性能良好，而且陶瓷匣钵在1000℃条件下不与锂离子电池正极材料的合成原料发生反应，耐腐蚀性能好，本发明的陶瓷匣钵的使用寿命可达50次以上。

Description

一种低成本长寿命的陶瓷匣钵及其制备方法
技术领域
本发明属于耐火窑具制备领域，涉及一种用于烧制锂离子电池正极材料的陶瓷匣钵及其制备方法。
背景技术
锂离子电池正极材料一般以陶瓷匣钵为载体经高温固相合成法(950～1000℃)制得。由于合成正极材料所用原料在高温条件下会分解，产生渗透能力强、反应活性高的氧化锂，对匣钵造成侵蚀，造成匣钵内壁剥落和粉化，导致匣钵使用寿命往往不超过20次。因此，研发抗腐蚀性能好、长寿命的匣钵对于锂离子电池正极材料的生产及技术进步具有重要意义。
目前，陶瓷匣钵主要以氧化铝、氧化锆、莫来石和堇青石等为原料。比如，中国发明专利《循环式锂电池正极材料用焙烧匣钵及其制备方法》(CN 103311498 B)公布了一种双层匣钵的制备方法，其基体层配方组成为堇青石10～90％、莫来石5～20％、刚玉5～25％、氧化铝5～25％、高岭土5～10％、氧化镁5～10％和锂辉石2～10％；表层配方组成为氧化锆60～90％、氧化铈1～5％、锂辉石5～10％和刚玉5～40％，烧成温度为1300±50℃。中国发明专利《一种用于锂电池正极材料焙烧的高安定长寿命匣钵及制造方法》(CN 102914165B)公布了以配方组成：氧化铝55％、二氧化硅13％、氧化镁为4％、钛酸铝15％、氧化钙10％和氧化锆3％，经1300～1550℃烧成制备的成品匣钵，经锂电池正极材料试验26～40次后开裂。中国发明专利《锂电池材料焙烧匣钵的制作配方》(CN101486586A)公布了一种锂电池焙烧匣钵的配方组成为：氧化铝45～70％、二氧化硅15～35％、氧化镁10～20％、氧化锆3～5％和金属铝粉2～5％。中国发明专利《用于制造锂离子电池的正极活性物质的匣钵及其制造方法》(CN101604751A)公布了一种制造锂离子电池的匣钵，其配方组成为：尖晶石30～70％、堇青石15～70％和莫来石0～35％。以上提及的陶瓷匣钵采用较大比例的合成原料，成本较高，使用寿命也较短，比如《一种用于锂电池正极材料焙烧的高安定长寿命匣钵及制造方法》(CN 102914165B)提供的匣钵的寿命比现有技术略有延长，但由于抗热震性能的限制，其使用次数仍不能超过40次。
发明内容
本发明所要解决的技术问题是针对现有技术中存在的上述不足，提供一种陶瓷匣钵及其制备方法，主要以天然矿物为原料，成本低，而且制备的陶瓷匣钵具有良好的耐腐蚀性能和抗热震性能，使用寿命长。
为解决上述技术问题，本发明提供的技术方案是：
提供一种低成本长寿命的陶瓷匣钵，其用于烧结锂化合物的粉体，陶瓷匣钵基材由以下重量百分含量的原料组成：滑石20～25％，铝矾土15～20％，60～65目镁铝尖晶石5～35％，100～120目镁铝尖晶石15～45％，堇青石5～15％。
按上述方案，所述陶瓷匣钵基材表面还含有一层涂料，所述涂料由以下重量百分含量的原料组成：氧化镁50～80％，熔块20～50％，添加剂0.5～1％，其中所述添加剂为羧甲基纤维素、聚乙烯醇、三聚磷酸铵中的一种或多种按任意比例的混合物。
本发明还提供上述陶瓷匣钵的制备方法，其步骤如下：
1)原料配比：将滑石、铝矾土、镁铝尖晶石和堇青石分别用球磨机球磨，其中镁铝尖晶石分成两份分别球磨，其中一份球磨0.5～1h后过60～65目筛，另一份球磨1.5～2h后过100～120目筛，其它原料球磨5～10h后过200～350目筛，随后按以下质量百分含量配料：滑石20～25％，铝矾土15～20％，60～65目镁铝尖晶石5～35％，100～120目镁铝尖晶石15～45％，堇青石5～15％；
2)制备陶瓷匣钵坯体：将步骤1)配好的原料置于捏合机中混合，得到混合粉料，然后向混合粉料中再加入水溶性粘结剂和水，继续混合30～50min得到混合料，陈腐24～48h，然后将陈腐好的混合料通过压机压制成型得到陶瓷匣钵坯体；
3)制备陶瓷匣钵支撑体：将步骤2)压制成型的陶瓷匣钵坯体放入100～120℃的烘箱中干燥5～10h，然后将干燥好的陶瓷匣钵坯体放入电窑或梭式窑中烧制得到陶瓷匣钵支撑体；
4)制备陶瓷匣钵：通过浸渍提拉法在步骤3)所得陶瓷匣钵支撑体表面施一层料浆，形成表面涂层，涂层干燥后放入电窑或梭式窑中烧成制得陶瓷匣钵。
按上述方案，步骤2)所述水溶性粘结剂为羧甲基纤维素、聚乙烯醇、水玻璃中的一种或多种按任意比例的混合物；所述水溶性粘结剂的加入量为混合粉料质量的3～8％，水的加入量为混合粉料质量的5～10％。
按上述方案，步骤2)所述压制成型的压力为100～150kN。
按上述方案，步骤3)所述烧制工艺条件为：室温下以3～5℃/min的速率升温至1300～1400℃烧制20～30h。
按上述方案，步骤4)所述料浆制备方法为：按质量配比称取原料，然后加水搅拌均匀制得，料浆含水量为总质量的40％，制备料浆的原料及质量比例为：氧化镁50～80％，熔块20～50％，添加剂0.5～1％。
按上述方案，步骤4)所述烧成工艺条件为：室温下以3～5℃/min的速率升温至1100～1200℃烧成10～15h。
本发明的有益效果在于：本发明以部分天然矿物滑石和铝矾土为原料制备陶瓷匣钵，与常见的锆莫来石、莫来石-堇青石质陶瓷匣钵相比原材料成本节约1/3以上，采用本发明方法制备得到的陶瓷匣钵能够经受超过50次热震循环而不开裂(1100℃～室温)，抗热震性能良好。而且，陶瓷匣钵在1000℃条件下不与锂离子电池正极材料的合成原料发生反应，耐腐蚀性能好。因此，本发明的陶瓷匣钵的使用寿命可达50次以上。
附图说明
图1为本发明实施例1所制备的陶瓷匣钵的示意图。
图中：1-陶瓷匣钵支撑体；2-陶瓷匣钵涂层；3-正极材料合成原料。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合附图对本发明作进一步详细描述。
实施例1
一种低成本长寿命的陶瓷匣钵及其制备方法，它包括如下步骤：
1)原料配比：将滑石、铝矾土、镁铝尖晶石和堇青石分别用球磨机球磨，其中镁铝尖晶石分成两份分别球磨，其中一份球磨0.5h后过60目筛，另一份球磨1.5h后过100目筛，其它原料球磨5h后过200目筛，随后按以下质量百分含量配料：滑石20％，铝矾土15％，60目镁铝尖晶石35％，100目镁铝尖晶石15％，堇青石15％；
2)制备陶瓷匣钵坯体：将步骤1)配好的原料置于捏合机中混合，得到混合粉料，然后向混合粉料中再加入水溶性粘结剂和水，继续混合30min得到混合料，陈腐24h，然后将陈腐好的混合料通过压机压制成型得到陶瓷匣钵坯体，成型压力为100kN；
所述水溶性粘结剂为羧甲基纤维素，加入量为混合粉料质量的4％、水的加入量为混合粉料质量的6％。
3)制备陶瓷匣钵支撑体：将步骤2)压制成型的陶瓷匣钵坯体放入100℃的烘箱中干燥6h，然后将干燥好的陶瓷匣钵坯体放入电窑或梭式窑中经1300℃烧制20h得到陶瓷匣钵支撑体，升温速率为3℃/min；
4)制备陶瓷匣钵：通过浸渍提拉法在步骤3)所得陶瓷匣钵支撑体表面施一层料浆，形成表面涂层，涂层干燥后放入电窑或梭式窑中经1100℃烧制10h得到陶瓷匣钵，升温速率为3℃/min。
所述料浆制备方法为：按质量配比称取原料，然后加水搅拌均匀制得，料浆含水量为总质量的40％，制备料浆的原料及质量比例为：氧化镁50％，熔块49.5％，羧甲基纤维素0.5％。所述熔块为锆白熔块，其化学组成及质量百分含量如下表1所示。
表1
Figure BDA0001261051160000041
所制得的陶瓷匣钵如图1所示。其中1为陶瓷匣钵支撑体，2为陶瓷匣钵涂层，3为正极材料合成原料。
经测试，本发明的陶瓷匣钵经50次热震循环后不开裂(1100℃～室温)。而且，陶瓷匣钵在1000℃条件下不与锂离子电池正极材料的合成原料发生反应，即不被腐蚀。因此，本发明的陶瓷匣钵的使用寿命可达50次以上。
实施例2
一种低成本长寿命的陶瓷匣钵及其制备方法，它包括如下步骤：
1)原料配比：将滑石、铝矾土、镁铝尖晶石和堇青石分别用球磨机球磨，其中镁铝尖晶石分成两份分别球磨，其中一份球磨1h后过65目筛，另一份球磨2h后过120目筛，其它原料球磨10h后过350目筛，随后按以下质量百分含量配料：滑石25％，铝矾土20％，65目镁铝尖晶石35％，120目镁铝尖晶石15％，堇青石5％；
2)制备陶瓷匣钵坯体：将步骤1)配好的原料置于捏合机中混合，得到混合粉料，然后向混合粉料中再加入水溶性粘结剂和水，继续混合50min得到混合料，陈腐48h，然后将陈腐好的混合料通过压机压制成型得到陶瓷匣钵坯体，成型压力为150kN；
所述水溶性粘结剂为羧甲基纤维素和聚乙烯醇1:1的混合物，加入量为混合粉料质量的8％、水的加入量为混合粉料质量的5％。
3)制备陶瓷匣钵支撑体：将步骤2)压制成型的陶瓷匣钵坯体放入120℃的烘箱中干燥8h，然后将干燥好的陶瓷匣钵坯体放入电窑或梭式窑中经1400℃烧制30h得到陶瓷匣钵支撑体，升温速率为5℃/min；
4)制备陶瓷匣钵：通过浸渍提拉法在步骤3)所得陶瓷匣钵支撑体表面施一层料浆，形成表面涂层，涂层干燥后放入电窑或梭式窑中经1200℃烧制15h得到陶瓷匣钵，升温速率为5℃/min。
所述料浆制备方法为：按质量配比称取原料，然后加水搅拌均匀制得，料浆含水量为总质量的40％，制备料浆的原料及质量比例为：氧化镁70％，熔块29％，聚乙烯醇1％。
经测试，本发明的陶瓷匣钵经55次热震循环后不开裂(1100℃～室温)。而且，陶瓷匣钵在1000℃条件下不与锂离子电池正极材料的合成原料发生反应，即不被腐蚀。因此，本发明的陶瓷匣钵的使用寿命可达50次以上。
实施例3
一种低成本长寿命的陶瓷匣钵及其制备方法，它包括如下步骤：
1)原料配比：将滑石、铝矾土、镁铝尖晶石和堇青石分别用球磨机球磨，其中镁铝尖晶石分成两份分别球磨，其中一份球磨0.6h后过60目筛，另一份球磨1.6h后过100目筛，其它原料球磨8h后过350目筛，随后按以下质量百分含量配料：滑石25％，铝矾土15％，60目镁铝尖晶石25％，100目镁铝尖晶石30％，堇青石5％。
2)制备陶瓷匣钵坯体：将步骤1)配好的原料置于捏合机中混合，得到混合粉料，然后向混合粉料中再加入水溶性粘结剂和水，继续混合40min得到混合料，陈腐36h，然后将陈腐好的混合料通过压机压制成型得到陶瓷匣钵坯体，成型压力为120kN；
所述水溶性粘结剂为聚乙烯醇和水玻璃1:1的混合物，加入量为混合粉料质量的6％、水的加入量为混合粉料质量的8％。
3)制备陶瓷匣钵支撑体：将步骤2)压制成型的陶瓷匣钵坯体放入110℃的烘箱中干燥8h，然后将干燥好的陶瓷匣钵坯体放入电窑或梭式窑中经1350℃烧制25h得到陶瓷匣钵支撑体，升温速率为4℃/min；
4)制备陶瓷匣钵：通过浸渍提拉法在步骤3)所得陶瓷匣钵支撑体表面施一层料浆，形成表面涂层，涂层干燥后放入电窑或梭式窑中经1150℃烧制12h得到陶瓷匣钵，升温速率为3℃/min。
所述料浆制备方法为：按质量配比称取原料，然后加水搅拌均匀制得，料浆含水量为总质量的40％，制备料浆的原料及质量比例为：氧化镁60％，熔块39％，三聚磷酸铵1％。
经测试，本发明的陶瓷匣钵经50次热震循环后不开裂(1100℃～室温)。而且，陶瓷匣钵在1000℃条件下不与锂离子电池正极材料的合成原料发生反应，即不被腐蚀。因此，本发明的陶瓷匣钵的使用寿命可达50次以上。

Claims (7)

1.一种低成本长寿命的陶瓷匣钵，其用于烧结锂化合物的粉体，其特征在于：陶瓷匣钵基材由以下重量百分含量的原料组成：滑石20~25%，铝矾土15~20%，60~65目镁铝尖晶石5~35%，100~120目镁铝尖晶石15~45%，堇青石5~15%；
所述陶瓷匣钵基材表面还含有一层涂料，所述涂料由以下重量百分含量的原料组成：氧化镁50~80%，熔块20~50%，添加剂0.5~1%，上述原料之和为100%，其中所述添加剂为羧甲基纤维素、聚乙烯醇、三聚磷酸铵中的一种或多种按任意比例的混合物。
2.一种权利要求1所述的陶瓷匣钵的制备方法，其特征在于步骤如下：
1）原料配比：将滑石、铝矾土、镁铝尖晶石和堇青石分别用球磨机球磨，其中镁铝尖晶石分成两份分别球磨，其中一份球磨0.5~1h后过60~65目筛，另一份球磨1.5~2h后过100~120目筛，其它原料球磨5~10h后过200~350目筛，随后按以下质量百分含量配料：滑石20~25%，铝矾土15~20%，60~65目镁铝尖晶石5~35%，100~120目镁铝尖晶石15~45%，堇青石5~15%；
2）制备陶瓷匣钵坯体：将步骤1）配好的原料置于捏合机中混合，得到混合粉料，然后向混合粉料中再加入水溶性粘结剂和水，继续混合30~50min得到混合料，陈腐24~48h，然后将陈腐好的混合料通过压机压制成型得到陶瓷匣钵坯体；
3）制备陶瓷匣钵支撑体：将步骤2）压制成型的陶瓷匣钵坯体放入100~120℃的烘箱中干燥5~10h，然后将干燥好的陶瓷匣钵坯体放入电窑或梭式窑中烧制得到陶瓷匣钵支撑体；
4）制备陶瓷匣钵：通过浸渍提拉法在步骤3）所得陶瓷匣钵支撑体表面施一层料浆，形成表面涂层，涂层干燥后放入电窑或梭式窑中烧成制得陶瓷匣钵。
3.根据权利要求2所述的制备方法，其特征在于步骤2）所述水溶性粘结剂为羧甲基纤维素、聚乙烯醇、水玻璃中的一种或多种按任意比例的混合物；所述水溶性粘结剂的加入量为混合粉料质量的3~8%，水的加入量为混合粉料质量的5~10%。
4.根据权利要求2所述的制备方法，其特征在于步骤2）所述压制成型的压力为100~150kN。
5.根据权利要求2所述的制备方法，其特征在于步骤3）所述烧制工艺条件为：室温下以3~5℃/min的速率升温至1300~1400℃烧制20~30h。
6.根据权利要求2所述的制备方法，其特征在于步骤4）所述料浆制备方法为：按质量配比称取原料，然后加水搅拌均匀制得，料浆含水量为总质量的40%，制备料浆的原料及质量比例为：氧化镁50~80%，熔块20~50%，添加剂0.5~1%。
7.根据权利要求2所述的制备方法，其特征在于步骤4）所述烧成工艺条件为：室温下以3~5℃/min的速率升温至1100~1200℃烧成10~15h。
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