CN106365654A - 一种添加ZrN‑SiAlON的抗锂电材料侵蚀耐火坩埚 - Google Patents

一种添加ZrN‑SiAlON的抗锂电材料侵蚀耐火坩埚 Download PDF

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CN106365654A
CN106365654A CN201610764933.7A CN201610764933A CN106365654A CN 106365654 A CN106365654 A CN 106365654A CN 201610764933 A CN201610764933 A CN 201610764933A CN 106365654 A CN106365654 A CN 106365654A
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sialon
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佘培华
佘文浩
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CHANGXING SHENGHUA REFRACTORY MATERIALS CO LTD
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Abstract

本发明公开了一种添加ZrN‑SiAlON的抗锂电材料侵蚀耐火坩埚，按重量份计由以下原料组分混合制成：六铝酸钙40～80份，板状刚玉细粉10～30份，ZrN‑SiAlON粉10～15份，氧化铝微粉3～10份，硅微粉2～10份，高岭土5～10份，水玻璃2～3份，甲基纤维素1～3份，水5～8份。本发明采用科学的配方和工艺制造出抗锂电材料侵蚀耐火坩埚，导热系数低，抗锂电材料侵蚀性能好，热震稳定性适中，使用寿命长。与同类坩埚相比，本发明可以保护正极材料粉体在烧结过程中不受坩埚材质污染，在使用期限内不出现表面剥落、掉渣等现象。

Description

一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚
技术领域
本发明涉及一种钴酸锂、锰酸锂、三元材料粉体烧结用的装载器皿，特别涉及一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚。
背景技术
近十年以来，锂电池行业发展迅速，逐渐大量应用在包括3C电子产品、储能领域、新能源汽车等各个新兴行业。锂电池一般由正极材料、负极材料、隔膜等装置组成。正极材料占整个电池成本的40-50%，其性能的提升，是提高电池能量密度的重要影响因素。
正极材料按照技术路线的分类，主要涵盖了钴酸锂、镍钴锰三元锂、镍钴铝三元锂、锰酸锂、磷酸铁锂等多个方向。但正极材料的工业化生产方式接近，即利用碳酸锂（氢氧化锂）、氧化钴、氧化锰、氢氧化镍等原料，通过固相烧结的方法制备正极材料。
随着对锂电池正极材料品质及杂质含量要求的进一步提高，对正极材料烧结用耐火坩埚也提出了更高的要求。特别是要求不污染正极材料。
发明内容
本发明的目的在于提供一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，能较好地抵抗锂、钴、镍等碱性侵蚀，使用寿命长。
本发明解决其技术问题所采用的技术方案是：
一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，按重量份计由以下原料组分混合制成：六铝酸钙40～80份，板状刚玉细粉10～30份，ZrN-SiAlON粉10～15份，氧化铝微粉3～10份，硅微粉2～10份，高岭土5～10份，水玻璃2～3份，甲基纤维素1～3份，水5～8份。
六铝酸钙是CaO-Al2O3二元系统中氧化铝含量最高的中间化合物。高温分解温度为1875℃。人工合成的六铝酸钙矿物相是一种高耐火度，高熔点的矿物质。其具有良好的抗碱侵蚀性能，较好的热震稳定性能，以及在还原气氛下高度稳定等性能特征。目前，在炼铝工业、建材工业、石化工业等已经有了一定的应用。ZrN-SiAlON粉耐高温性能好，抗碱侵蚀性能好。
板状刚玉是一种纯净的、不添加如MgO、B2O3等任何添加剂而烧成收缩彻底的烧结刚玉，具有结晶粗大、发育良好的α- Al2O3晶体结构，Al2O3的含量在99%以上。板片状晶体结构，气孔小且闭气孔较多而气孔率与电熔刚玉大体相当，纯度高，体积稳定性好，极小的重烧收缩，用以生产的材料高温处理后具有良好的热震稳定性和抗弯强度。
氧化铝微粉，是用高温煅烧氧化铝粉体以工业氢氧化铝或工业氧化铝为原料，在适当的温度下煅烧成晶型稳定的α-型氧化铝产品；再以煅烧α-型氧化铝为原料，经过球磨制成的微粉。具有高的化学纯度，主要以氧化铝成分为主。
硅微粉，是铁合金在冶炼硅铁和工业硅（金属硅）时，矿热电炉内产生出大量挥发性很强的SiO2和Si气体，气体排放后与空气迅速氧化冷凝沉淀而成。优质微硅粉主要被用作高性能耐火浇注料、预制件、钢包料、透气砖、自流型耐火浇注料及干湿法喷射材料。在高温陶瓷领域，如：氧化物结合碳化硅制品，高温型硅酸钙轻质隔热材料，电磁窑用刚玉莫来石推板，高温耐磨材料及制品，刚玉及陶瓷制品等，微硅粉的使用具有高流动性、低蓄水量、高致密度和高强度等特点。
高岭土类矿物是由高岭石、地开石、珍珠石、埃洛石等高岭石簇矿物组成，主要矿物成分是高岭石。高岭石的理论化学组成为46.54%的SiO2，39.5%的Al2O3，13.96%的H2O。高岭土类矿物属于1:1型层状硅酸盐，晶体主要由硅氧四面体和氢氧八面体组成。具有良好的增塑性能。
本发明的配方中的坩埚需要在模具中液压成型，并通过烘烤脱水、高温烧结，最终以坩埚为产品形态。有利于实现提高坩埚侧壁的强度，在使用中保证不破损。
作为优选，按重量份计由以下原料组分混合制成：六铝酸钙65～75份，板状刚玉细粉10～20份，ZrN-SiAlON粉10～15份，氧化铝微粉3～8份，硅微粉3～5份，高岭土6～8份，水玻璃2～3份，甲基纤维素1～3份，水5～8份。
作为优选，所述ZrN-SiAlON粉体通过以下步骤制备而得：
（1）将重量份分别为4~8份氧化铝粉，10~15份锆英石，30~45份炭黑混合均匀得基料，置于球磨罐中，以水为介质球磨3~5h，然后冷冻干燥；
（2）将步骤（1）冷冻干燥后的混合料再干混20~30min；
（3）将干混后的混合料以70~80MPa的压力压制成型，再置于微波高温气氛炉中，于1400~1600℃保温5~8h，保温过程中通入流动的氮气，流量为0.5~2L/min；
（4）将上述加热后的混合料在600~800℃的空气中氧化3~5h，冷却后粉碎即得ZrN-SiAlON粉体。本发明采用微波加热合成、烧结制备ZrN-SiAlON粉体，具有降低烧结温度、缩短烧结保温时间的优点。
作为优选，步骤（1）中基料与水的质量比为1.5~2：1。
作为优选，所述板状刚玉细粉的颗粒大小在500-1000目。
作为优选，所述氧化铝微粉的颗粒大小在300-600目。
作为优选，所述硅微粉的颗粒大小在400-800目。
一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚的制备方法，先在六铝酸钙中加入板状刚玉细粉及ZrN-SiAlON粉，搅拌10～15分钟后，加入氧化铝微粉，搅拌8～10分钟后，加入硅微粉，搅拌8～10分钟后，加入高岭土、水玻璃和甲基纤维素，搅拌16～20分钟后，加入水，搅拌均匀后困料24-36小时，之后利用液压压力机成型得坩埚毛坯，坩埚毛坯经过室温干燥，在隧道窑进行高温烧结，最后采用磨具进行表面打磨。
作为优选，所述高温烧结为：先在9小时内升温到600℃，然后在12小时内升温到1450℃，再在1450℃下保温3小时。温度控制精确，产品品质高。
本发明的有益效果是：
本发明采用科学的配方和工艺制造出抗锂电材料侵蚀耐火坩埚，导热系数低，抗锂电材料侵蚀性能好，热震稳定性适中，使用寿命长。与同类坩埚相比，本发明可以保护正极材料粉体在烧结过程中不受坩埚材质污染，在使用期限内不出现表面剥落、掉渣等现象。使用寿命为25次循环以上。
具体实施方式
下面通过具体实施例，对本发明的技术方案作进一步的具体说明。
本发明中，若非特指，所采用的原料和设备等均可从市场购得或是本领域常用的。下述实施例中的方法，如无特别说明，均为本领域的常规方法。
本发明的板状刚玉细粉的颗粒大小在500-1000目，氧化铝微粉的颗粒大小在300-600目，硅微粉的颗粒大小在400-800目。
实施例1：
一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，按重量份计由以下原料组分混合制成：六铝酸钙40份，板状刚玉细粉10份，ZrN-SiAlON粉15份，氧化铝微粉3份，硅微粉2份，高岭土5份，水玻璃2份，甲基纤维素1份，水5份。
所述ZrN-SiAlON粉体通过以下步骤制得：
（1）将重量份分别为4份氧化铝粉，10份锆英石，30份炭黑混合均匀得基料，置于球磨罐中，以水为介质球磨3h，然后冷冻干燥；基料与水的质量比为1.5：1。
（2）将步骤（1）冷冻干燥后的混合料再干混20min。
（3）将干混后的混合料以70MPa的压力压制成型，再置于微波高温气氛炉中，于1400℃保温8h，保温过程中通入流动的氮气，流量为0.5L/min。
（4）将上述加热后的混合料在600℃的空气中氧化5h，冷却后粉碎即得ZrN-SiAlON粉体。
实施例2：
一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，按重量份计由以下原料组分混合制成：六铝酸钙80份，板状刚玉细粉30份，ZrN-SiAlON粉10份，氧化铝微粉10份，硅微粉10份，高岭土10份，水玻璃3份，甲基纤维素3份，水8份。
所述ZrN-SiAlON粉体通过以下步骤制得：
（1）将重量份分别为8份氧化铝粉， 15份锆英石，45份炭黑混合均匀得基料，置于球磨罐中，以水为介质球磨5h，然后冷冻干燥；基料与水的质量比为2：1。
（2）将步骤（1）冷冻干燥后的混合料再干混30min。
（3）将干混后的混合料以80MPa的压力压制成型，再置于微波高温气氛炉中，于1600℃保温5h，保温过程中通入流动的氮气，流量为2L/min。
（4）将上述加热后的混合料在800℃的空气中氧化3h，冷却后粉碎即得ZrN-SiAlON粉体。
实施例3：
一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，按重量份计由以下原料组分混合制成：六铝酸钙65份，板状刚玉细粉20份，ZrN-SiAlON粉12份，氧化铝微粉8份，硅微粉3份，高岭土6份，水玻璃2份，甲基纤维素3份，水6份。
所述ZrN-SiAlON粉体通过以下步骤制得：
（1）将重量份分别为6份氧化铝粉，12份锆英石，40份炭黑混合均匀得基料，置于球磨罐中，以水为介质球磨4h，然后冷冻干燥；基料与水的质量比为2：1。
（2）将步骤（1）冷冻干燥后的混合料再干混25min。
（3）将干混后的混合料以75MPa的压力压制成型，再置于微波高温气氛炉中，于1500℃保温7h，保温过程中通入流动的氮气，流量为1L/min。
（4）将上述加热后的混合料在700℃的空气中氧化4h，冷却后粉碎即得ZrN-SiAlON粉体。
实施例4：
一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，按重量份计由以下原料组分混合制成：六铝酸钙75份，板状刚玉细粉20份，ZrN-SiAlON粉12份，氧化铝微粉6份，硅微粉5份，高岭土8份，水玻璃3份，甲基纤维素2份，水7份。ZrN-SiAlON粉体制备方法同实施例3。
本发明添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚的制备方法为：先在六铝酸钙中加入板状刚玉细粉及ZrN-SiAlON粉，搅拌10～15分钟后，加入氧化铝微粉，搅拌8～10分钟后，加入硅微粉，搅拌8～10分钟后，加入高岭土、水玻璃和甲基纤维素，搅拌16～20分钟后，加入水，搅拌均匀后困料24-36小时，之后利用液压压力机成型得坩埚毛坯，坩埚毛坯经过室温干燥，在隧道窑进行高温烧结，高温烧结为先在9小时内升温到600℃，然后在12小时内升温到1450℃，再在1450℃下保温3小时，最后采用磨具进行表面打磨。
以上所述的实施例只是本发明的一种较佳的方案，并非对本发明作任何形式上的限制，在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。

Claims (9)

1.一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，其特征在于，按重量份计由以下原料组分混合制成：六铝酸钙40～80份，板状刚玉细粉10～30份，ZrN-SiAlON粉10～15份，氧化铝微粉3～10份，硅微粉2～10份，高岭土5～10份，水玻璃2～3份，甲基纤维素1～3份，水5～8份。
2.根据权利要求1所述的一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，其特征在于，按重量份计由以下原料组分混合制成：六铝酸钙65～75份，板状刚玉细粉10～20份，ZrN-SiAlON粉10～15份，氧化铝微粉3～8份，硅微粉3～5份，高岭土6～8份，水玻璃2～3份，甲基纤维素1～3份，水5～8份。
3.根据权利要求1或2所述的一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，其特征在于，所述ZrN-SiAlON粉体通过以下步骤制备而得：
（1）将重量份分别为4~8份氧化铝粉，10~15份锆英石，30~45份炭黑混合均匀得基料，置于球磨罐中，以水为介质球磨3~5h，然后冷冻干燥；
（2）将步骤（1）冷冻干燥后的混合料再干混20~30min；
（3）将干混后的混合料以70~80MPa的压力压制成型，再置于微波高温气氛炉中，于1400~1600℃保温5~8h，保温过程中通入流动的氮气，流量为0.5~2L/min；
（4）将上述加热后的混合料在600~800℃的空气中氧化3~5h，冷却后粉碎即得ZrN-SiAlON粉体。
4.根据权利要求3所述的一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，其特征在于，步骤（1）中基料与水的质量比为1.5~2：1。
5.根据权利要求1或2所述的一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，其特征在于，所述板状刚玉细粉的颗粒大小在500-1000目。
6.根据权利要求1或2所述的一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，其特征在于，所述氧化铝微粉的颗粒大小在300-600目。
7.根据权利要求1或2所述的一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚，其特征在于，所述硅微粉的颗粒大小在400-800目。
8.如权利要求1所述的一种添加ZrN-SiAlON的抗锂电材料侵蚀耐火坩埚的制备方法，其特征在于，先在六铝酸钙中加入板状刚玉细粉及ZrN-SiAlON粉，搅拌10～15分钟后，加入氧化铝微粉，搅拌8～10分钟后，加入硅微粉，搅拌8～10分钟后，加入高岭土、水玻璃和甲基纤维素，搅拌16～20分钟后，加入水，搅拌均匀后困料24-36小时，之后利用液压压力机成型得坩埚毛坯，坩埚毛坯经过室温干燥，在隧道窑进行高温烧结，最后采用磨具进行表面打磨。
9.根据权利要求8所述的制备方法，其特征在于，所述高温烧结为：先在9小时内升温到600℃，然后在12小时内升温到1450℃，再在1450℃下保温3小时。
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108610024A (zh) * 2018-05-07 2018-10-02 武汉科技大学 一种用于锂离子电池正极材料焙烧的匣钵及其制备方法
CN108658611A (zh) * 2018-05-07 2018-10-16 武汉科技大学 一种堇青石结合六铝酸钙匣钵及其制备方法
CN109320216A (zh) * 2018-11-06 2019-02-12 江苏中正陶瓷科技有限公司 一种基于片层状结构的稀土氧化物修饰的六铝酸钙坩埚制造方法
CN115849952A (zh) * 2022-12-26 2023-03-28 宜兴瑞泰耐火材料工程有限公司 一种六铝酸钙-赛隆轻质砖及其制备工艺

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101921130A (zh) * 2010-09-04 2010-12-22 潘起雄 刚玉莫来石坩埚

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101921130A (zh) * 2010-09-04 2010-12-22 潘起雄 刚玉莫来石坩埚

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
尹洪基: "六铝酸钙在侵蚀环境下的优点", 《耐火与石灰》 *
李悦彤 等: "配碳量对锆英石和氧化铝碳热还原氮化合成ZrN－SiAlON 的影响", 《耐火材料》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108610024A (zh) * 2018-05-07 2018-10-02 武汉科技大学 一种用于锂离子电池正极材料焙烧的匣钵及其制备方法
CN108658611A (zh) * 2018-05-07 2018-10-16 武汉科技大学 一种堇青石结合六铝酸钙匣钵及其制备方法
CN108610024B (zh) * 2018-05-07 2020-11-03 武汉科技大学 一种用于锂离子电池正极材料焙烧的匣钵及其制备方法
CN109320216A (zh) * 2018-11-06 2019-02-12 江苏中正陶瓷科技有限公司 一种基于片层状结构的稀土氧化物修饰的六铝酸钙坩埚制造方法
CN115849952A (zh) * 2022-12-26 2023-03-28 宜兴瑞泰耐火材料工程有限公司 一种六铝酸钙-赛隆轻质砖及其制备工艺
CN115849952B (zh) * 2022-12-26 2023-11-21 宜兴瑞泰耐火材料工程有限公司 一种六铝酸钙-赛隆轻质砖及其制备工艺

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