CN113480300A - 一种莫来石质复合匣钵及其制备方法 - Google Patents

一种莫来石质复合匣钵及其制备方法 Download PDF

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CN113480300A
CN113480300A CN202110790474.0A CN202110790474A CN113480300A CN 113480300 A CN113480300 A CN 113480300A CN 202110790474 A CN202110790474 A CN 202110790474A CN 113480300 A CN113480300 A CN 113480300A
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fine powder
sagger
mullite composite
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CN113480300B (zh
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李淑静
向坤
李远兵
王海路
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Wuhan University of Science and Engineering WUSE
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Abstract

本发明涉及一种莫来石质复合匣钵及其制备方法。其技术方案是：以44～53wt％的粘土细粉、47～56wt％的α‑Al2O3微粉为原料，外加原料3～5wt％的聚乙烯醇，混匀，困料，机压成型，制得匣钵坯体；再以40～45wt％的轻烧镁橄榄石细粉、30～35wt％的煅烧镁铝尖晶石细粉、10～15wt％的锆英石细粉和15～20wt％的板状刚玉细粉为混合料，外加混合料3～5wt％的聚乙烯醇，混匀，制得工作层混合料；然后在匣钵坯体底部工作面均匀分布一层工作层混合料，料层厚度为3～6mm，将料层机压成型，干燥，于1350～1450℃条件下保温3～5h，制得莫来石质复合匣钵。本发明工艺简单、生产成本低和节能环保，所制制品力学性能好、抗侵蚀性能优良、热震稳定性优异和使用寿命长。

Description

一种莫来石质复合匣钵及其制备方法
技术领域
本发明属于复合匣钵技术领域。特别涉及一种莫来石质复合匣钵及其制备方法。
背景技术
锂离子电池是20世纪70年代以后发展起来的一种新型储能电池。由于其具有高能量、寿命长、低能耗、无公害、无记忆效应以及自放电小、内阻小、性价比高和污染少等优点，在应用中逐步显示出巨大的优势，已广泛应用于移动电话、笔记本电脑、摄像机、数码相机、电动汽车、储能和航天等技术领域，特别是应用于新能源汽车。锂离子电池正极材料是构成锂离子电池的关键部分，在生产中常用高温固相法合成。匣钵作为锂离子电池正极材料高温焙烧过程中盛装原料的窑具，对锂离子电池正极材料的生产起着至关重要的作用。然而，在锂离子电池正极材料的高温煅烧过程中，其前驱体会产生碱性气氛，对匣钵造成侵蚀，使匣钵的寿命受到影响。侵蚀层的剥落会导致剥落物混入锂离子电池正极材料中，对锂电池正极材料造成污染，一方面会降低产品的质量和性能，另一方面增加了生产成本。所以对匣钵的性能提出了更加苛刻的要求，特别是热震稳定性和抗侵蚀性。
“锆莫来石匣钵”(ZL201410189300.9)专利技术，公开了一种以莫来石、板状刚玉和锆英砂等为原料制备匣钵的方法，所制备的匣钵虽热震稳定性好，但是使用的原料比较昂贵，且烧成温度太高，不利于大规模的工业生产。
“一种抗锂电池高温腐蚀层状匣钵及其制备方法”(CN201610159994.0)专利技术，公开了一种具有三层结构匣钵的制备方法，该方法采用的原料不一致，种类较多，所制备的匣钵生产工艺复杂，不仅增加了劳动强度，且结合层之间的结合强度有限，使用过程中易出现开裂。
“一种生产锂离子电池正极材料用耐高温匣钵的制备方法”(CN201010269844.8)专利技术，公开了以纯氧化铝、氧化镁和氧化钇粉体为原料制得耐高温匣钵，该技术采用的原料较为昂贵，增加了生产成本；匣钵烧后体积收缩大,不易成型，增加了劳动强度,且经过高达2000℃的温度条件下反应烧结，处理温度较高，增加了生产成本。
“复合匣钵的制备方法”(CN201610409237.4)专利技术，公开了一种复合匣钵的制备方法，在匣钵坯体预烧后进行水淬，然后油冷，干燥，工艺复杂，不利于大规模的工业生产，且在烧成后还需在匣钵侧面切割若干条膨胀缝，会导致匣钵在反复使用过程中易出现开裂和掉渣的现象。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种生产成本低、节能环保和生产工艺简单的莫来石质复合匣钵的制备方法；用该技术制备的莫来石质复合匣钵力学性能好、热震稳定性优良、抗侵蚀性能优异和使用寿命长。
为实现上述目的，本发明所采用的技术方案的步骤是：
步骤一、以44～53wt％的粘土细粉、47～56wt％的α-Al2O3微粉为原料，外加所述原料3～5wt％的聚乙烯醇，混合均匀，困料20～24h，机压成型，制得匣钵坯体。
步骤二、以40～45wt％的轻烧镁橄榄石细粉、30～35wt％的煅烧镁铝尖晶石细粉、10～15wt％的锆英石细粉和15～20wt％的板状刚玉细粉为混合料，外加所述混合料3～5wt％的聚乙烯醇，混合均匀，制得工作层混合料。
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为3～6mm，然后将所述料层机压成型，于80～110℃的条件下干燥18～24h，再于1350～1450℃条件下保温3～5h，制得莫来石质复合匣钵。
所述粘土细粉：Al2O3含量≥34wt％，SiO2含量≥47wt％；所述粘土细粉的粒径小于10μm。
所述α-Al2O3微粉的Al2O3含量≥98wt％；所述α-Al2O3微粉的粒径小于10μm。
所述轻烧镁橄榄石细粉的MgO含量≥45wt％；所述轻烧镁橄榄石细粉的粒径小于74μm。
所述煅烧镁铝尖晶石细粉的Al2O3含量≥70wt％；所述煅烧镁铝尖晶石细粉的粒径小于74μm。
所述锆英石细粉的ZrO2含量≥60wt％；所述锆英石细粉的粒径小于50μm。
所述板状刚玉细粉的Al2O3含量≥98wt％；所述板状刚玉细粉的粒径小于74μm。
所述机压成型的压强为70～90MPa。
步骤一和步骤二所述聚乙烯醇相同。
由于采用上述技术方案，本发明与现有技术相比具有如下积极效果：
1、本发明采用的原料均为耐火材料中的常用原料，来源丰富且价格低廉，故生产成本低；本发明的制备方法为高温固相法，所涉及的工艺简单，烧成温度低，节能环保。
2、本发明在匣钵表面工作层中引入轻烧镁橄榄石细粉、煅烧镁铝尖晶石细粉和和板状刚玉细粉，均能够与莫来石发生复合效应，形成复合结构，从而提高莫来石质复合匣钵在循环使用过程中的抗侵蚀性能。表面形成了抗侵蚀性能好的工作层，从而延长了莫来石质复合匣钵的使用寿命。
3、本发明在匣钵基体中原位反应生成膨胀系数低的莫来石，莫来石自身具有良好的抗热震性能，且表面工作层中的锆英石中含有氧化锆，利用氧化锆的相变增韧不仅能大幅度提高莫来石质复合匣钵的力学性能，且增强了莫来石质复合匣钵在反复使用过程中的抗热震性能。
4、本发明的匣钵坯体与工作层混合料之间的热膨胀系数相匹配，保证了莫来石质复合匣钵具有小的热膨胀系数，抗热冲击能力强，匣钵基体与表面工作层之间能够较好的结合，不易出现表面开裂掉渣现象。
本发明制备的莫来石质复合匣钵经检测：烧成后的显气孔率为20～30％；体积密度低于2.5g/cm3；耐压强度为100～130MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数超过29次时，工作面出现剥落。
因此，本发明工艺简单、生产成本低和节能环保，所制备的莫来石质复合匣钵力学性能好、抗侵蚀性能优良、热震稳定性优异和使用寿命长。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述，并非对其保护范围的限制：
为避免重复，先将本具体实施方式所涉及的技术参数统一描述如下，实施例中不再赘述：
所述粘土细粉：Al2O3含量≥34wt％，SiO2含量≥47wt％；所述粘土细粉的粒径小于10μm。
所述α-Al2O3微粉的Al2O3含量≥98wt％；所述α-Al2O3微粉的粒径小于10μm。
所述轻烧镁橄榄石细粉的MgO含量≥45wt％；所述轻烧镁橄榄石细粉的粒径小于74μm。
所述煅烧镁铝尖晶石细粉的Al2O3含量≥70wt％；所述煅烧镁铝尖晶石细粉的粒径小于74μm。
所述锆英石细粉的ZrO2含量≥60wt％；所述锆英石细粉的粒径小于50μm。
所述板状刚玉细粉的Al2O3含量≥98wt％；所述板状刚玉细粉的粒径小于74μm。
步骤一和步骤二所述聚乙烯醇相同。
实施例1
一种莫来石质复合匣钵及其制备方法。本实施例所述制备方法的步骤是：
步骤一、以44～47wt％的粘土细粉、53～56wt％的α-Al2O3微粉为原料，外加所述原料3～4wt％的聚乙烯醇，混合均匀，困料22～23h，机压成型，制得匣钵坯体。
步骤二、以42～44wt％的轻烧镁橄榄石细粉、30～32wt％的煅烧镁铝尖晶石细粉、11～13wt％的锆英石细粉和15～17wt％的板状刚玉细粉为混合料，外加所述混合料3～4wt％的聚乙烯醇，混合均匀，制得工作层混合料。
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为3～4mm；然后对所述料层进行机压成型，置于80～90℃的条件下干燥18～20h，再于1370～1390℃条件下保温3～4h，制得莫来石质复合匣钵。
所述机压成型的压强为70～80MPa。
本实施例1制备的莫来石质复合匣钵经检测：烧成后的显气孔率为26～28％；体积密度低于2.4g/cm3；耐压强度为100～108MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数达到31次时，工作面出现剥落。
实施例2
一种莫来石质复合匣钵及其制备方法。本实施例所述制备方法的步骤是：
步骤一、以47～50wt％的粘土细粉、50～53wt％的α-Al2O3微粉为原料，外加所述原料4～5wt％的聚乙烯醇，混合均匀，困料22～24h，机压成型，制得匣钵坯体。
步骤二、以40～42wt％的轻烧镁橄榄石细粉、31～33wt％的煅烧镁铝尖晶石细粉、11～14wt％的锆英石细粉和15～18wt％的板状刚玉细粉为混合料，外加所述混合料4～5wt％的聚乙烯醇，混合均匀，制得工作层混合料。
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为4～5mm；然后对所述料层进行机压成型，置于90～110℃的条件下干燥20～22h，再于1390～1410℃条件下保温4～5h，制得莫来石质复合匣钵。
所述机压成型的压强为70～80MPa。
本实施例2制备的莫来石质复合匣钵经检测：烧成后的显气孔率为25～28％；体积密度低于2.4g/cm3；耐压强度为111～120MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数达到32次时，工作面出现剥落。
实施例3
一种莫来石质复合匣钵及其制备方法。本实施例所述制备方法的步骤是：
步骤一、以50～53wt％的粘土细粉、47～50wt％的α-Al2O3微粉为原料，外加所述原料3～4wt％的聚乙烯醇，混合均匀，困料21～23h，机压成型，制得匣钵坯体。
步骤二、以40～43wt％的轻烧镁橄榄石细粉、30～32wt％的煅烧镁铝尖晶石细粉、12～15wt％的锆英石细粉和15～17wt％的板状刚玉细粉为混合料，外加所述混合料3～4wt％的聚乙烯醇，混合均匀，制得工作层混合料。
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为5～6mm；然后对所述料层进行机压成型，置于90～110℃的条件下干燥21～23h，再于1410～1430℃条件下保温4～5h，制得莫来石质复合匣钵。
所述机压成型的压强为80～90MPa。
本实施例3制备的莫来石质复合匣钵经检测：烧成后的显气孔率为24～25％；体积密度低于2.5g/cm3；耐压强度为120～133MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数达到34次时，工作面出现剥落。
实施例4
一种莫来石质复合匣钵及其制备方法。本实施例所述制备方法的步骤是：
步骤一、以46～49wt％的粘土细粉、51～54wt％的α-Al2O3微粉为原料，外加所述原料3～4wt％的聚乙烯醇，混合均匀，困料20～22h，机压成型，制得匣钵坯体。
步骤二、以41～43wt％的轻烧镁橄榄石细粉、30～32wt％的煅烧镁铝尖晶石细粉、11～13wt％的锆英石细粉和16～18wt％的板状刚玉细粉为混合料，外加所述混合料3～4wt％的聚乙烯醇，混合均匀，制得工作层混合料。
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为3.5～4.5mm；然后对所述料层进行机压成型，置于80～100℃的条件下干燥22～24h，再于1390～1410℃条件下保温3～4h，制得莫来石质复合匣钵。
所述机压成型的压强为70～80MPa。
本实施例4制备的莫来石质复合匣钵经检测：烧成后的显气孔率为25～26％；体积密度低于2.4g/cm3；耐压强度为100～106MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数达到30次时，工作面出现剥落。
实施例5
一种莫来石质复合匣钵及其制备方法。本实施例所述制备方法的步骤是：
步骤一、以49～52wt％的粘土细粉、48～51wt％的α-Al2O3微粉为原料，外加所述原料4～5wt％的聚乙烯醇，混合均匀，困料21～23h，机压成型，制得匣钵坯体。
步骤二、以40～42wt％的轻烧镁橄榄石细粉、30～32wt％的煅烧镁铝尖晶石细粉、10～12wt％的锆英石细粉和18～20wt％的板状刚玉细粉为混合料，外加所述混合料4～5wt％的聚乙烯醇，混合均匀，制得工作层混合料。
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为4.5～5.5mm；然后对所述料层进行机压成型，置于80～100℃的条件下干燥19～21h，再于1350～1370℃条件下保温3～5h，制得莫来石质复合匣钵。
所述机压成型的压强为80～90MPa。
本实施例5制备的莫来石质复合匣钵经检测：烧成后的显气孔率为24～26％；体积密度低于2.4g/cm3；耐压强度为113～125MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数达到32次时，工作面出现剥落。
实施例6
一种莫来石质复合匣钵及其制备方法。本实施例所述制备方法的步骤是：
步骤一、以45～48wt％的粘土细粉、52～55wt％的α-Al2O3微粉为原料，外加所述原料3～4wt％的聚乙烯醇，混合均匀，困料23～24h，机压成型，制得匣钵坯体。
步骤二、以40～43wt％的轻烧镁橄榄石细粉、32～35wt％的煅烧镁铝尖晶石细粉、10～12wt％的锆英石细粉和15～18wt％的板状刚玉细粉为混合料，外加所述混合料3～4wt％的聚乙烯醇，混合均匀，制得工作层混合料。
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为5～6mm；然后对所述料层进行机压成型，置于90～110℃的条件下干燥18～20h，再于1430～1450℃条件下保温3～4h，制得莫来石质复合匣钵。
所述机压成型的压强为80～90MPa。
本实施例6制备的莫来石质复合匣钵经检测：烧成后的显气孔率为25～26％；体积密度低于2.4g/cm3；耐压强度为110～120MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数达到32次时，工作面出现剥落。
实施例7
一种莫来石质复合匣钵及其制备方法。本实施例所述制备方法的步骤是：
步骤一、以48～51wt％的粘土细粉、49～52wt％的α-Al2O3微粉为原料，外加所述原料3～4wt％的聚乙烯醇，混合均匀，困料21～22h，机压成型，制得匣钵坯体。
步骤二、以43～45wt％的轻烧镁橄榄石细粉、30～32wt％的煅烧镁铝尖晶石细粉、10～12wt％的锆英石细粉和15～17wt％的板状刚玉细粉为混合料，外加所述混合料3～4wt％的聚乙烯醇，混合均匀，制得工作层混合料。
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为4～5mm；然后对所述料层进行机压成型，置于80～100℃的条件下干燥21～23h，再于1400～1410℃条件下保温3～4h，制得莫来石质复合匣钵。
所述机压成型的压强为75～85MPa。
本实施例7制备的莫来石质复合匣钵经检测：烧成后的显气孔率为23～26％；体积密度低于2.5g/cm3；耐压强度为115～122MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数达到33次时，工作面出现剥落。
本具体实施方式与现有技术相比具有如下积极效果：
1、本具体实施方式采用的原料均为耐火材料中的常用原料，来源丰富且价格低廉，故生产成本低；且本具体实施方式的制备方法为高温固相法，所涉及的工艺简单，烧成温度低，节能环保。
2、本具体实施方式在匣钵表面工作层中引入轻烧镁橄榄石细粉、煅烧镁铝尖晶石细粉和和板状刚玉细粉，均能够与莫来石发生复合效应，形成复合结构，从而提高莫来石质复合匣钵在循环使用过程中的抗侵蚀性能。表面形成了抗侵蚀性能好的工作层，从而延长了莫来石质复合匣钵的使用寿命。
3、本具体实施方式在匣钵基体中原位反应生成膨胀系数低的莫来石，莫来石自身具有良好的抗热震性能，且表面工作层中的锆英石中含有氧化锆，利用氧化锆的相变增韧不仅能大幅度的提高莫来石质复合匣钵的力学性能，且增强了莫来石质复合匣钵在反复使用过程中的抗热震性能。
4、本具体实施方式的匣钵坯体与工作层混合料之间的热膨胀系数相匹配，保证了莫来石质复合匣钵具有小的热膨胀系数，抗热冲击能力强，匣钵基体与表面工作层之间能够较好的结合，不易出现表面开裂掉渣现象。
本具体实施方式制备的莫来石质复合匣钵经检测：烧成后的显气孔率为20～30％；体积密度低于2.5g/cm3；耐压强度为100～130MPa；1100℃下合成锂离子电池正极材料镍钴锰酸锂，所制备的莫来石质复合匣钵循环使用次数超过29次时，工作面出现剥落。
因此，本具体实施方式工艺简单、生产成本低和节能环保，所制备的莫来石质复合匣钵力学性能好、抗侵蚀性能优良、热震稳定性优异和使用寿命长。

Claims (9)

1.一种莫来石质复合匣钵的制备方法，其特征在于所述制备方法的步骤是：
步骤一、以44～53wt％的粘土细粉、47～56wt％的α-Al2O3微粉为原料，外加所述原料3～5wt％的聚乙烯醇，混合均匀，困料20～24h，机压成型，制得匣钵坯体；
步骤二、以40～45wt％的轻烧镁橄榄石细粉、30～35wt％的煅烧镁铝尖晶石细粉、10～15wt％的锆英石细粉和15～20wt％的板状刚玉细粉为混合料，外加所述混合料3～5wt％的聚乙烯醇，混合均匀，制得工作层混合料；
步骤三、在所述匣钵坯体底部工作面均匀分布一层所述工作层混合料，工作层混合料的料层厚度为3～6mm，然后将所述料层机压成型，于80～110℃的条件下干燥18～24h，再于1350～1450℃条件下保温3～5h，制得莫来石质复合匣钵。
2.根据权利要求1所述的莫来石质复合匣钵的制备方法，其特征在于所述粘土细粉：Al2O3含量≥34wt％，SiO2含量≥47wt％；所述粘土细粉的粒径小于10μm。
3.根据权利要求1所述的莫来石质复合匣钵的制备方法，其特征在于所述α-Al2O3微粉的Al2O3含量≥98wt％；所述α-Al2O3微粉的粒径小于10μm。
4.根据权利要求1所述的莫来石质复合匣钵的制备方法，其特征在于所述轻烧镁橄榄石细粉的MgO含量≥45wt％；所述轻烧镁橄榄石细粉的粒径小于74μm。
5.根据权利要求1所述的莫来石质复合匣钵的制备方法，其特征在于所述煅烧镁铝尖晶石细粉的Al2O3含量≥70wt％；所述煅烧镁铝尖晶石细粉的粒径小于74μm。
6.根据权利要求1所述的莫来石质复合匣钵的制备方法，其特征在于所述锆英石细粉的ZrO2含量≥60wt％；所述锆英石细粉的粒径小于50μm。
7.根据权利要求1所述的莫来石质复合匣钵的制备方法，其特征在于所述板状刚玉细粉的Al2O3含量≥98wt％；所述板状刚玉细粉的粒径小于74μm。
8.根据权利要求1所述的莫来石质复合匣钵的制备方法，其特征在于所述机压成型的压强为70～90MPa。
9.一种莫来石质复合匣钵，其特征在于所述莫来石质复合匣钵是根据权利1～8项中任一项所述莫来石质复合匣钵的制备方法所制备的莫来石质复合匣钵。
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009292704A (ja) * 2008-06-09 2009-12-17 Noritake Co Ltd リチウムイオン電池の正極活物質製造用匣鉢及びその製造方法
CN105698542A (zh) * 2016-03-21 2016-06-22 武汉理工大学 一种抗锂电池高温腐蚀层状匣钵及其制备方法
CN108373324A (zh) * 2018-03-28 2018-08-07 广东山摩新材料科技有限公司 一种用于锂电池正极材料焙烧的轻质匣钵及其制备方法
CN110194673A (zh) * 2019-05-31 2019-09-03 武汉科技大学 一种节能型莫来石氧化锆复相耐火材料及其制备方法
CN110282964A (zh) * 2019-06-20 2019-09-27 武汉科技大学 莫来石-堇青石质锂电池正极材料烧结用匣钵及其制备方法
CN110590341A (zh) * 2019-09-29 2019-12-20 武汉科技大学 溶胶结合的锂电池正极材料烧结用匣钵及其制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009292704A (ja) * 2008-06-09 2009-12-17 Noritake Co Ltd リチウムイオン電池の正極活物質製造用匣鉢及びその製造方法
CN105698542A (zh) * 2016-03-21 2016-06-22 武汉理工大学 一种抗锂电池高温腐蚀层状匣钵及其制备方法
CN108373324A (zh) * 2018-03-28 2018-08-07 广东山摩新材料科技有限公司 一种用于锂电池正极材料焙烧的轻质匣钵及其制备方法
CN110194673A (zh) * 2019-05-31 2019-09-03 武汉科技大学 一种节能型莫来石氧化锆复相耐火材料及其制备方法
CN110282964A (zh) * 2019-06-20 2019-09-27 武汉科技大学 莫来石-堇青石质锂电池正极材料烧结用匣钵及其制备方法
CN110590341A (zh) * 2019-09-29 2019-12-20 武汉科技大学 溶胶结合的锂电池正极材料烧结用匣钵及其制备方法

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