CN109020592A - 一种锂离子电池正极材料合成用的复合纤维匣钵及其制备方法 - Google Patents
一种锂离子电池正极材料合成用的复合纤维匣钵及其制备方法 Download PDFInfo
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Abstract
一种锂离子电池正极材料合成用的复合纤维匣钵及其制备方法,本发明基体增强复合纤维匣钵材料包括莫来石、纤维莫来石、堇青石、镁铝尖晶石、纤维氧化铝、纤维氧化镁、锆英石、二氧化铈、氧化锆‑氧化钇纤维。本发明合成工艺简单,烧结工艺易控,制成的材料均匀性好,耐高温抗腐蚀相较比传统匣钵明显提升,其重复次数和产品质量明显提高,延长了匣钵的使用寿命;并且抗热震性能优异,可有效地防止匣钵表层脱落。本发明有利于降低合成锂离子电池正极材料的生产成本,提高经济效益。
Description
技术领域
本发明特别涉及一种锂离子电池正极材料合成用的复合纤维匣钵及其制备方法。
背景技术
目前合成锂离子电池正极材料的实际生产中一般都采用高温固相合成法,而合成过程中所用到的耐高温匣钵一般为堇青石、莫来石、石英质和刚玉质等耐高温匣钵,其中堇青石和刚玉质用得最多。然而,由于合成锂离子正极材料所用原料在合成过程中会分解产生渗透能力和反应活性强的氧化锂(Li2O),在高温下碱性物质Li2O与匣钵中的酸性物质和两性氧化物发生化学反应,因此会对耐高温匣钵产生侵蚀,使得耐高温匣钵的使用寿命大大降低。
现有的匣钵按照不同的结构一般分为两种:一种是将多种原料混合均匀后,压制成型后烧结得到的复合材料,此种匣钵在被侵蚀之后,表面有少量难以剥离的正极材料,报废后成为工业垃圾,很容易造成重金属污染。另一种是双层结构,即在基体层匣钵表面喷涂或者涂覆另外一种材料。但是这种双层结构匣钵由于表面会首先受到碱性氧化物的侵蚀,所以当表面的涂覆层发生化学变化后导致成份偏析,造成热膨胀系数和晶格常数不匹配从而致使表面与基体层脱落的现象。脱落的表层物质会对正极材料造成污染,从而影响正极材料的电化学性能,最终降低正极材料产品的合格率。
目前在锂离子电池正极材料合成用的匣钵中,对于高碱性原料,国内匣钵的使用次数普遍不超出五次,因此如何提高匣钵的使用寿命,降低重金属污染,提高企业生产效益,是目前亟待解决的问题。而这一问题的提出就对于所属领域技术人员开发性能优越、成本低廉的耐高温匣钵提出了更加紧迫的要求。
发明内容
鉴于上文所述,本发明针对现有锂离子电池正极材料合成用匣钵对碱性原料具有反应侵蚀现象及其导致的脱落现象,提供一种抗侵蚀、防表面脱落、耐高温且抗热震性良好的表面复合纤维增强型复合匣钵,进而提高匣钵的使用寿命,降低合成锂离子电池正极材料的生产成本以及提高产品质量。本发明的技术方案如下:
一种锂离子电池正极材料合成用的复合纤维匣钵,其特征在于:其由以下重量份的原料和结合剂与水混合后制备而成:莫来石5~25份,纤维莫来石5~10份,堇青石20~60份、镁铝尖晶石5~20份、纤维氧化铝5~10份、纤维氧化镁1~5份、锆英石5~10份、二氧化铈1~5份、氧化锆-氧化钇纤维5~10份,其中结合剂为表面层原料总质量的3~6份,水为表面层原料总质量的3~8份。
进一步地,本发明中结合剂为黄糊精或PVA。
一种锂离子电池正极材料合成用的复合纤维匣钵的制备方法,其特征在于,包括如下步骤:
(1)准备匣钵的原料:莫来石5~25份,纤维莫来石5~10份,堇青石20~60份、镁铝尖晶石5~20份、纤维氧化铝5~10份、纤维氧化镁1~5份、锆英石5~10份、二氧化铈1~5份、氧化锆-氧化钇纤维5~10份;
(2)将原料进行混合制浆,经陈腐处理后将所得浆料通过成型设备压制成产品生坯;
(3)将制得的产品生坯经干燥处理,然后对产品生坯进行烧结,最终制得复合纤维匣钵。
进一步地,本发明步骤(2)中将原料进行混合制浆时采用去离子水作为介质,其中水为原料总质量的3~8份。
进一步地,本发明步骤(2)中将原料进行混合制浆时加入结合剂,所述结合剂为黄糊精或PVA,其中结合剂为原料总质量的3~6份。
进一步地,所述步骤(2)中陈腐处理的时间为8~24小时。
进一步地,所述步骤(3)中干燥处理具体是将产品生坯在常温下阴干24小时,而后进行烘干使得产品生坯的含水量维持在0.8~1.5%。
进一步地,所述步骤(3)中烧结工艺的参数为:烧结温度为1320℃~1370℃,烧结时间为2~5小时。
本发明为了解决匣钵易受侵蚀现象、表面易脱落和抗热震的问题,在传统制备匣钵所用复合陶瓷基体中大量使用纤维化(包括长纤维和短纤维)的氧化锆-氧化钇(ZrO2-Y2O3)、氧化铝(Al2O3)、纤维氧化镁(MgO),,经过氧化钇和二氧化铈改性得到的纤维氧化锆具有更加优异的稳定性,因而得到的改性纤维制品的耐腐蚀性能比传统的材料更加优异,并且也正是因为其耐高温抗腐蚀性能的提升可以起到延缓或阻止侵蚀的作用,所以当表面层被腐蚀之后,纤维氧化锆、纤维氧化铝、纤维氧化镁不与碱金属氧化物进行反应,在表面层其他成分受到碱金属化合物的腐蚀之后,引入的纤维状物质根据相变增韧、纤维增韧等机理作用,保证了受到腐蚀后的表面层不会由于晶相和化学成分的改变而轻易产生脱落,即纤维状物质在整个表面层中起到了防止表面脱落、增强抗侵蚀能力的作用,从而大大提高了匣钵的使用寿命。同时,经过改性的纤维制品的耐高温性能也比传统的材料更加优异,纤维氧化锆-氧化钇是唯一能在1600℃以上超高温氧化气氛下长期使用的轻质耐火纤维材料。因而对于在氧化气氛下合成的锂离子电池正极材料具有特别优良的耐高温效果,结合上文可知,由于纤维氧化锆-氧化钇的加入,根据相变增韧原理,本发明引入纤维状物质也提高了匣钵的抗热震能力。
相比现有技术,本发明的有益效果如下:
(1)本发明提出一种纤维复合的基体层匣钵,通过在匣钵的基体层表面增加纤维陶瓷复合层,以此来克服匣钵表面受到腐蚀后易脱落的缺点,尤其适用于烧制锂离子正极材料,用以延长匣钵使用寿命以及提高正极材料成品的合格率。
(2)本发明提出一种纤维复合的基体层匣钵,由于所用纤维材料相比传统材料具有更优良的稳定性、耐腐蚀、耐高温的特性。从而使得复合纤维匣钵相比现有匣钵除了不易脱落外还耐碱腐蚀,不易于锂离子电池材料发生反应,从而有效抑制了重金属污染,具有环保效益。
(3)本发明提出一种纤维复合的基体层匣钵,由于所用纤维材料能够显著提升匣钵的抗热震性能,从而大大提高了匣钵的使用寿命。
(4)本发明提出一种纤维复合的基体层匣钵的制备方法,工艺操作简单、成本低廉且生产效率高,有利于企业生产效益的提高。
附图说明
图1是实施例1制得材料的XRD图。
图2是实施例2制得材料的XRD图。
具体实施方式
下面结合说明书附图和具体实施例对本发明技术方案进行清楚、完整的描述,以期本领域技术人员能够理解本发明的原理及特性。
实施例1:
步骤1:准备莫来石15份、纤维莫来石5份,堇青石40份、镁铝尖晶石15份、锆英石5份、二氧化铈2份、纤维氧化铝10份、纤维氧化镁3份、氧化锆-氧化钇纤维5份作为匣钵原料,然后加入匣钵原料总质量5份的黄糊精作为结合剂;
步骤2:将步骤1所述准备的原料以去离子水作为介质进行混合制浆,所述去离子水的用量为匣钵原料总质量6份,待混合浆料搅拌均匀后,陈腐24小时,然后将浆料通过成型设备压制成匣钵生坯;
步骤3:将匣钵生坯在常温下阴干24小时,然后进行烘干,使其含水量维持在1%左右,继而在1320℃条件下烧结2小时,最终制得匣钵成品。
实施例2:
步骤1:准备莫来石20份、纤维莫来石5份,堇青石30份、镁铝尖晶石20份、锆英石5份、二氧化铈3份、纤维氧化铝7份、纤维氧化镁3份、氧化锆-氧化钇纤维7份作为匣钵原料,然后加入匣钵原料总质量5份的黄糊精作为结合剂;
步骤2:将步骤1所述准备的原料以去离子水作为介质进行混合制浆,所述去离子水的用量为匣钵原料总质量6份,待混合浆料搅拌均匀后,陈腐24小时,然后将浆料通过成型设备压制成匣钵生坯;
步骤3:将匣钵生坯在常温下阴干24小时,然后进行烘干,使其含水量维持在1%左右,继而在1330℃条件下烧结4小时,最终制得匣钵成品。
实施例3:
步骤1:准备莫来石5份、纤维莫来石8份,堇青石50份、镁铝尖晶石10份、锆英石8份、二氧化铈3份、纤维氧化铝5份、纤维氧化镁1份、氧化锆-氧化钇纤维10份作为匣钵原料,然后加入匣钵原料总质量5份的黄糊精作为结合剂;
步骤2:将步骤1所述准备的原料以去离子水作为介质进行混合制浆,所述去离子水的用量为匣钵原料总质量6份,待混合浆料搅拌均匀后,陈腐24小时,然后将浆料通过成型设备压制成匣钵生坯;
步骤3:将匣钵生坯在常温下阴干24小时,然后进行烘干,使其含水量维持在1%左右,继而在1340℃条件下烧结3小时,最终制得匣钵成品。
实施例4:
步骤1:准备莫来石25份、纤维莫来石7份,堇青石20份、镁铝尖晶石20份、锆英石10份、二氧化铈3份、纤维氧化铝5份、纤维氧化镁2份、氧化锆-氧化钇纤维8份作为匣钵原料,然后加入匣钵原料总质量5份的黄糊精作为结合剂;
步骤2:将步骤1所述准备的原料以去离子水作为介质进行混合制浆,所述去离子水的用量为匣钵原料总质量6份,待混合浆料搅拌均匀后,陈腐24小时,然后将浆料通过成型设备压制成匣钵生坯;
步骤3:将匣钵生坯在常温下阴干24小时,然后进行烘干,使其含水量维持在1%左右,继而在1350℃条件下烧结5小时,最终制得匣钵成品。
实施例5:
步骤1:准备莫来石10份、纤维莫来石5份,堇青石55份、镁铝尖晶石10份、锆英石5份、二氧化铈2份、纤维氧化铝5份、纤维氧化镁3份、氧化锆-氧化钇纤维5份作为匣钵原料,然后加入匣钵原料总质量5份的黄糊精作为结合剂;
步骤2:将步骤1所述准备的原料以去离子水作为介质进行混合制浆,所述去离子水的用量为匣钵原料总质量6份,待混合浆料搅拌均匀后,陈腐24小时,然后将浆料通过成型设备压制成匣钵生坯;
步骤3:将匣钵生坯在常温下阴干24小时,然后进行烘干,使其含水量维持在1%左右,继而在1370℃条件下烧结3小时,最终制得匣钵成品。
下表是各实施例的抗腐蚀性能测试结果:
从表中数据可看出,采用本发明提供的组合物制备匣钵,制得匣钵的重复使用次数明显高于现在行业内的普遍使用次数。本发明匣钵在使用过程中具有良好的高温抗腐蚀性能,并且多次重复使用不存在表面脱落的现象作用,显著提高了产品的质量,而且生产原料低廉,制备工艺与传统工艺兼容,有利于企业生产效益的提高。
以上结合附图对本发明的实施例进行了详细阐述,但是本发明并不局限于上述的具体实施方式,上述具体实施方式仅仅是示意性的,而不是限制性的,本领域的普通技术人员在本发明的启示下,不脱离本发明宗旨和权利要求所保护范围的情况下还可以做出很多变形,这些均属于本发明的保护。
Claims (8)
1.一种锂离子电池正极材料合成用的复合纤维匣钵,其特征在于:其由以下重量份的原料和结合剂与水混合后制备而成:莫来石5~25份,纤维莫来石5~10份,堇青石20~60份、镁铝尖晶石5~20份、纤维氧化铝5~10份、纤维氧化镁1~5份、锆英石5~10份、二氧化铈1~5份、氧化锆-氧化钇纤维5~10份,其中结合剂为表面层原料总质量的3~6份,水为表面层原料总质量的3~8份。
2.根据权利要求1所述的一种锂离子电池正极材料合成用的复合纤维匣钵,其特征在于,所述结合剂为黄糊精或PVA。
3.一种锂离子电池正极材料合成用的复合纤维匣钵的制备方法,其特征在于,包括如下步骤:
(1)准备匣钵的原料:莫来石5~25份,纤维莫来石5~10份,堇青石20~60份、镁铝尖晶石5~20份、纤维氧化铝5~10份、纤维氧化镁1~5份、锆英石5~10份、二氧化铈1~5份、氧化锆-氧化钇纤维5~10份;
(2)将原料进行混合制浆,经陈腐处理后将所得浆料通过成型设备压制成产品生坯;
(3)将制得的产品生坯经干燥处理,然后对产品生坯进行烧结,最终制得复合纤维匣钵。
4.根据权利要求3所述的一种锂离子电池正极材料合成用的复合纤维匣钵的制备方法,其特征在于,所述步骤(2)中将原料进行混合制浆时采用去离子水作为介质,其中水为原料总质量的3~8份。
5.根据权利要求3所述的一种锂离子电池正极材料合成用的复合纤维匣钵的制备方法,其特征在于,所述结合剂为黄糊精或PVA,其中结合剂为原料总质量的3~6份。
6.根据权利要求3所述的一种锂离子电池正极材料合成用的复合纤维匣钵的制备方法,其特征在于,所述步骤(2)中陈腐处理的时间为8~24小时。
7.根据权利要求3所述的一种锂离子电池正极材料合成用的复合纤维匣钵的制备方法,其特征在于,所述步骤(3)中干燥处理具体是将产品生坯在常温下阴干24小时,而后进行烘干使得产品生坯的含水量维持在0.8~1.5%。
8.根据权利要求3所述的一种锂离子电池正极材料合成用的复合纤维匣钵的制备方法,其特征在于,所述步骤(3)中烧结工艺的参数为:烧结温度为1320℃~1370℃,烧结时间为2~5小时。
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