CN103476733A - 用于含锂化合物的热处理容器 - Google Patents

用于含锂化合物的热处理容器 Download PDF

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CN103476733A
CN103476733A CN201180069879XA CN201180069879A CN103476733A CN 103476733 A CN103476733 A CN 103476733A CN 201180069879X A CN201180069879X A CN 201180069879XA CN 201180069879 A CN201180069879 A CN 201180069879A CN 103476733 A CN103476733 A CN 103476733A
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lithium
containing compound
heat treatment
treatment container
container
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小池康太
阿知波敬
神谷孝广
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TYK Corp
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TYK Corp
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Abstract

本发明的用于含锂化合物的热处理容器，当热处理含锂化合物时用于盛装含锂化合物，其特征在于，当全部为100质量%时，含有60～95质量%的氧化铝，且空隙率为10～30%。

Description

用于含锂化合物的热处理容器
技术领域
本发明涉及当热处理含锂化合物时使用的用于含锂化合物的热处理容器。
背景技术
各种化合物、特别是无机类化合物是通过热处理工艺制造。通常，热处理是在耐热性的热处理容器中盛装被热处理化合物(无机类化合物或其原料)的状态下通过加热来进行。热处理容器不仅要求耐热性，还要求对于被热处理化合物的稳定性。
通过上述热处理工艺制造的无机类化合物之一，有含锂化合物。含锂化合物是例如用于锂离子电池的正极活性材料。作为含锂化合物，可以例示出LiMnO2类化合物、LiNi1/3Co1/3Mn1/3O2类化合物、LiMn2O4类化合物、LiCoO2类化合物、LiNiO2类化合物。
锂离子电池用正极活性材料(含锂化合物)通过烧成原料粉末而制造。该含锂化合物的热处理(烧成)，一般收纳在以氧化铝、多铝红柱石、堇青石、尖晶石等具备耐热性的材料作为主要构成成分而烧成的容器(匣钵)中进行。匣钵例如记载在特开2009-292704号公报中。
以堇青石为主要成分的匣钵，具有高抗热震性。然而，与含锂化合物反应活性高，所以存在因反应产物的混入而热处理后的含锂化合物纯度下降的问题。特别是，锂离子电池的正极活性材料中，若混入这种杂质，则不仅会导致锂离子电池的电池性能下降，还存在成为发生短路的来源的风险。
此外，以氧化铝或尖晶石为主要成分的匣钵，与含锂化合物反应活性低。然而，热膨胀系数高，且这些成分的含有率越高，存在因热冲击容易开裂的问题。因此，很难使氧化铝或尖晶石的含有率高。
在特开2009-292704号公报中，记载有由尖晶石、堇青石、多铝红柱石形成的匣钵。这些材料，具有上述问题。
在先技术文献
专利文献
专利文献1：特开2009-292704号公报
发明内容
发明所要解决的问题
本发明鉴于上述实际情况而提出，其目的在于提供一种能够抑制含锂化合物被污染且抗热震性优异的用于含锂化合物的热处理容器。
解决问题的方法
为了解决上述问题，本发明人等反复研究用于含锂化合物的热处理容器的结果，完成了本发明。
即，本发明的用于含锂化合物的热处理容器，当热处理含锂化合物时用于盛装含锂化合物，其特征在于，当所述容器的全部质量为100质量%时，含有60～95质量%的氧化铝(Al2O3)，且空隙率为10～30%。
本发明的用于含锂化合物的热处理容器，当其全部质量为100质量%时，优选含有5～30质量%的二氧化硅(SiO2)。
本发明的用于含锂化合物的热处理容器，优选，由氧化铝和多铝红柱石形成。
发明效果
由于含有60～95质量%的大量的氧化铝，抑制了本发明的用于含锂化合物的热处理容器与含锂化合物的反应。而且，空隙率为10～30%，抑制了所述容器受热冲击时开裂。
即，本发明的用于含锂化合物的热处理容器，由于抑制与含锂化合物反应，从而能够抑制反应产物污染含锂化合物，且抑制因热冲击开裂(损坏)。
具体实施方式
(用于含锂化合物的热处理容器)
本发明的用于含锂化合物的热处理容器(以下称为本发明的热处理容器)是，当热处理含锂化合物时盛装含锂化合物的用于含锂化合物的热处理容器。在本发明的热处理容器中进行热处理的含锂化合物，只要是在其化学式中包含锂(Li)的化合物均可。进一步，也可以是混合有含有锂的化合物的混合物。
而且，本发明的热处理容器，含有大量的对被热处理的含锂化合物(被热处理化合物)反应活性低的材料(氧化铝)(作为主要构成成分)，且空隙率调节为10～30%。
而且，本发明的热处理容器，当所述容器的全部质量为100质量%时，含有60～95质量%的氧化铝(Al2O3)。
本发明的热处理容器的主要构成成分的氧化铝是，对含锂化合物反应活性低的材料。也就是说，本发明的热处理容器，由于含有大量的氧化铝，所以当热处理含锂化合物时，能够抑制含锂化合物与热处理容器反应以及抑制生成反应产物。其结果，能够抑制被热处理的含锂化合物被反应产物污染。
而且，本发明的热处理容器，当所述容器的全部质量为100质量%时，含有60～95质量%的氧化铝。由于含有60～95质量%的氧化铝，从而能够抑制所述容器与含锂化合物反应的同时，提高抗热震性。在此，若氧化铝的含有比例低于60质量%时，所述容器容易与含锂化合物发生反应，而超出95质量%时，热处理容器容易开裂。更优选的含有比例为70～90质量%。
此外，本发明的热处理容器，空隙率为10～30%。由于空隙率在该范围内，所以热处理容器的抗热震性提高。若空隙率小于该范围，则所述容器由于热处理容易开裂，若超出该范围，则由于锂侵蚀造成剥离。优选，空隙率为15～25%。
本发明的热处理容器，当其全部质量为100质量%时，优选含有5～30质量%的二氧化硅(SiO2)。二氧化硅是有效提高热处理容器的抗热震性的化合物。此外，由于二氧化硅具有与被热处理的含锂化合物的反应活性，所以优选其含有量较少。若二氧化硅的含有比例小于该范围时，氧化铝的含有比例相对增加，从而抗热震性下降，热处理容器容易开裂(损伤)。此外，若含有比例超出该范围时，所述容器容易与含锂化合物发生反应，含锂化合物由于反应产物容易受污染。因此，通过使二氧化硅的含有量在该范围内，能够提高热处理容器的抗热震性的同时，抑制含锂化合物被污染。更优选二氧化硅的含有比例为10～20质量%。
本发明的热处理容器，优选由氧化铝和多铝红柱石形成。氧化铝是由化学式Al2O3表示的化合物，多铝红柱石是氧化铝(Al2O3)和二氧化硅(SiO2)的化合物(铝硅酸盐)，具有Al6O13Si2的组成式。也就是说，由于由氧化铝和多铝红柱石形成，所以所述容器不含有容易与含锂化合物发生反应的物质(化合物)，从而本发明的热处理容器能够提高抗热震性的同时，抑制含锂化合物被污染。在本发明中，所述容器优选不含有容易与含锂化合物发生反应的物质(化合物)，作为这种物质，可以例示出氧化镁(MgO)。在此，由氧化铝和多铝红柱石形成是指，不仅仅由氧化铝和多铝红柱石形成，也包括以氧化铝和多铝红柱石为主要成分形成的情况。还有，在本发明中，也可以含有不可避免的杂质。
本发明的热处理容器，优选仅由氧化铝和多铝红柱石形成。由于仅由氧化铝和多铝红柱石形成，所以所述容器不含有与含锂化合物具有反应活性的其它无机元素，从而本发明的热处理容器能够提高抗热震性的同时，抑制含锂化合物被污染。例如，作为现有匣钵的主要构成材料的堇青石中含有氧化镁，该氧化镁与含锂化合物发生反应而生成反应产物。
在本发明的热处理容器中，对含锂化合物实施的热处理，不仅包括含锂化合物由本发明的热处理容器盛装的状态下对其进行加热的处理，还包括为了生成含锂化合物而进行加热(烧成)的处理。即，并不限制热处理温度。此外，关于热处理时的气氛，除了优选不与热处理容器发生反应之外，并不特别限定。
本发明的热处理容器，只要是能够放置(盛装)含锂化合物的形状，对其形状并不特别限定。例如，可以举出将含锂化合物放置(盛装、固定)在其上表面的大致板状形状、上方或侧方开口的槽状(筒状)形状、用盖部件覆盖槽状(筒状)开口的封闭形状(所谓匣钵)等形状。还有，在本发明的热处理容器中，不与含锂化合物接触的部分，也可以由不同材料形成。
此时，在本发明的热处理容器中被热处理的含锂化合物，也可以以粉末状、被成形的成形体等任一形态由热处理容器盛装。
(用于含锂化合物的热处理容器的制造方法)
本发明的用于含锂化合物的热处理容器，其制造方法并不特别限定，只要是由规定材料制造成具有规定范围的空隙率的制造方法均可。
例如，热处理容器能够通过混合粒度(粒径)不同的粉末而成形、烧成规定形状来制得。此时，使得热处理容器的空隙率在规定范围(10～30%)内的进行成形、烧成。此外，也可以适当实施干燥工艺等工艺。
实施例
下面，用实施例详细说明本发明。
作为本发明的实施例，制造出板状的用于含锂化合物的热处理容器。
(实施例)
将氧化铝粉末、多铝红柱石粉末及其它添加剂，按表1所示的质量份称重，并充分混合。
将充分混合的混合粉末压成正方形的板状。该成形通过加压6kN/㎝2的压力进行。
接着，自然干燥成形体之后，保持在1350℃的大气气氛下烧结5个小时(烧成)。
烧成后，放置冷却，制造出板状的用于含锂化合物的热处理容器(试样1～2)。
表1
Figure BDA0000391719170000051
分别测量了制造的试样1～2的用于含锂化合物的热处理容器的空隙率、堆积比重、抗弯强度，将测量结果表示于表2。
空隙率及堆积比重的测量，根据日本工业标准(JIS R1614(真空法))规定的方法进行。
抗弯强度的测量，使用电子万能试验机(株式会社米仓制作所制造，CATY)，设定支点之间距离为6cm，通过3点弯曲试验来进行。
表2
Figure BDA0000391719170000061
如表2所示，试样1的用于含锂化合物的热处理容器，已证实含有77.9质量%的氧化铝、19.0质量%的二氧化硅，且空隙率为19.2%。此外，试样2的用于含锂化合物的热处理容器，已证实含有87.2质量%的氧化铝、10.9质量%的二氧化硅，且空隙率为20.0%。
评价
作为实施例的用于含锂化合物的热处理容器的评价，反复进行含锂化合物(LiNi1/3Co1/3Mn1/3O2类化合物)的烧成之后，观察了烧成后的热处理容器的状态。
具体而言，按下列方式进行。
首先，称重碳酸锂粉末(Li2CO3)3/2摩尔%、氧化钴粉末(Co3O4)1/3摩尔%、二氧化锰粉末(MnO2)1摩尔%、氢氧化镍粉末(Ni(OH)2)1摩尔%，充分混合之后成形为圆盘形颗粒状。该颗粒成形为直径φ18mm、厚度5mm、一颗4g。
将制造的颗粒载置在各试样的用于含锂化合物的热处理容器的表面上，并配置在烧成炉内之后进行加热烧成。
颗粒的烧成，在大气气氛中，用4小时升温至1100℃，升温后在1100℃保持4小时之后，在空气中放置冷却。
放置冷却后，去除各试样的用于含锂化合物的热处理容器表面上的颗粒，而载置另一批新的颗粒(未烧成)，进行烧成。加热是在同样的处理条件下进行的。
该颗粒的烧成反复进行20次。
对市售的用于含锂化合物的热处理容器(试样3～6)也进行了同样的评价试验。再有，试样3～6具有表2所示的组成及特性。
烧成20次之后观察了各试样的横截面。
在此，试样3是由多铝红柱石形成的热处理容器，含有75.9质量%的氧化铝、21.8质量%的二氧化硅，且空隙率为34.1%。即，与试样1～2相比，具有较大的空隙率。
试样4是由多铝红柱石和堇青石形成的热处理容器，含有64.0质量%的氧化铝、30.6质量%的二氧化硅、3.3质量%的氧化镁，且空隙率为30.2%。即，与试样1～2相比，不仅含有氧化镁，还具有较大的空隙率。
试样5是由氧化锆(ZrO2)和堇青石形成的热处理容器，含有34.7质量%的氧化铝、41.8质量%的二氧化硅、4.7质量%的氧化镁、15.7质量%的氧化锆，且空隙率为33.9%。即，与试样1～2相比，不仅含有氧化镁、氧化锆，还具有较大的空隙率。
试样6是由尖晶石和堇青石形成的热处理容器，含有56.8质量%的氧化铝、25.9质量%的二氧化硅、13.4质量%的氧化镁，且空隙率为31.6%。即，与试样1～2相比，不仅含有氧化镁，还具有较大的空隙率。进一步，氧化铝的含有量也相当低。
在试样1～2中，在与颗粒接触的部分附近，观察到含锂化合物的侵蚀(渗透、扩散)。此外，已证实轻微膨胀(体积变化)。还有，已证实在与颗粒接触的部分附近，试样1～2的表面，大致保持平滑状态。即，在试样1～2中，虽然已证实含锂化合物的侵蚀(及侵蚀引起的轻微体积变化)，但没有证实到与含锂化合物的反应产物。也就是说，不具有与含锂化合物的反应活性(几乎没有)。
在试样3中，在与颗粒接触的部分附近，观察到含锂化合物的侵蚀(渗透、扩散)。此外，在与颗粒接触的部分，已证实表面变粗糙及膨胀(体积变化)。这种表面粗糙，与容器及含锂化合物侵蚀的部分相比具有不同的颜色，可知是与含锂化合物的反应产物。进一步，这种表面粗糙，脆弱、容易剥离。这种表面变粗糙(及体积变化)是，由于与颗粒接触的部分与颗粒的含锂化合物发生反应而发生。即，试样3已证实，与含锂化合物发生反应，而在其表面形成了容易剥离的反应产物。
试样4～6已证实，与颗粒接触的部分附近变成海绵状的泡沫体而大大膨胀。该泡沫体部分，与试样3的情况相同，可知是与含锂化合物的反应产物。通过与试样1～3比较，认为与含锂化合物的反应产物是与氧化镁、氧化锆的反应产物。该海绵状泡沫体部分，其体积的大部分为气孔，所以特别脆弱、容易损坏而粉末剥离。即，试样4～6已证实，与含锂化合物发生反应而在其表面形成大量的容易剥离的反应产物。
其次，测量试样1、2、4容器在1000℃时的热膨胀系数，并表示在表2中。
如表2所示，已证实氧化铝的含有比例越高热膨胀系数越大。进一步，如表2所示，可以证实试样1～2，与试样3～6相比，具有相当高的抗弯强度。
即，试样1～2的容器，不仅热膨胀系数大，同时强度也高，从而提高抗热震性。除此之外，如上所述的抑制与含锂化合物反应，从而也抑制含锂化合物被污染。
如上所述，作为本发明的用于含锂化合物的热处理容器的试样1～2的容器，由于不含有氧化镁等，所以抑制了上述容器与含锂化合物的反应活性，从而能够抑制含锂化合物被污染，且能够抑制因热冲击开裂(损坏)。
(实施例的变形形态)
在上述实施例中，采用板状热处理容器进行了颗粒状含锂化合物的烧成，但热处理容器的形状及含锂化合物的配置形态，并不限定于此。
热处理容器也可以采用上方或侧方开口的槽状(筒状)形状、用盖部件覆盖槽状(筒状)开口的封闭形状(所谓匣钵)等形状。此外，含锂化合物也可以为粉末状。
特别是，当热处理容器为槽状的形状、含锂化合物为粉末状时，能够更好地发挥上述实施例的热处理容器的效果。
具体地说，在槽状容器内部放入粉末状含锂化合物进行烧成(热处理)时，烧成后，使槽状容器的开口朝下而取出烧成后的含锂化合物。此时，在热处理容器的内表面(与含锂化合物接触的表面)未发生反应产物引起的剥离，所以烧成后的含锂化合物不会发生污染。
与此相反，例如，作为本发明的比较例的试样3～6同样形状的容器而言，在与含锂化合物接触的表面发生了反应产物引起的剥离。而且，取出含锂化合物时，反应产物与含锂化合物一同从热处理容器取出。也就是说，反应产物污染含锂化合物。

Claims (3)

1.一种用于含锂化合物的热处理容器，当热处理含锂化合物时用于盛装该含锂化合物，其特征在于，
当所述容器的全部质量为100质量%时，含有60～95质量%的氧化铝，且空隙率为10～30%。
2.根据权利要求1所述的用于含锂化合物的热处理容器，
当所述容器的全部质量为100质量%时，含有5～30质量%的二氧化硅。
3.根据权利要求1所述的用于含锂化合物的热处理容器，
由氧化铝和多铝红柱石形成。
CN201180069879XA 2011-03-30 2011-06-28 用于含锂化合物的热处理容器 Pending CN103476733A (zh)

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