CN109534805B - 锂电池粉烧结用镁橄榄石-刚玉匣钵及其制备方法 - Google Patents
锂电池粉烧结用镁橄榄石-刚玉匣钵及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种锂电池粉烧结用镁橄榄石‑刚玉匣钵及其制备方法,匣钵包括如下重量份的组分:预烧镁橄榄石50‑60份、烧结板状氧化铝16‑20份、高岭土4‑8份以及活性氧化铝14‑18份。本发明的匣钵在保障产品抗热震稳定性的情况下,降低匣钵材质中的SiO2含量,增加MgO含量,使匣钵材质偏碱性,不与锂电池粉发生反应,提高新产品的荷重软化温度,使匣钵在使用过程中不发生变形现象;与现用的堇青石匣钵相比,生产成本减少了1500元/吨,在批量试用时,使用寿命平均45次,大于目前使用40次的标准,匣钵表面不起皮,对锂电池粉没有任何污染;同时,本发明的制备方法简单可行,容易实现。
Description
技术领域
本发明涉及一种匣钵及其制备方法,尤其涉及一种锂电池粉烧结用镁橄榄石-刚玉匣钵及其制备方法。
背景技术
近几年锂电池行业蓬勃发展,烧结锂电池粉大多使用推板窑,烧结温度在850-1200℃之间,由于锂电池粉生产循环速度快,岀窑后,内外温差大,装载锂电池粉的匣钵容易断裂。目前烧结生产锂电池粉使用堇青石匣钵,使用寿命25-40次,这与该匣钵本身具有非常好的抗热震稳定性是不相符的。研究发现,该匣钵损坏的主要原因是以下两点:(1)堇青石质含有60-70%的SiO2,在高温时和锂电池粉中的碱性金属氧化物起反应,生成低融点的物质,造成匣钵出现裂纹和起皮脱落,裂纹逐步扩展,最终使匣钵开裂。(2)堇青石的荷重软化温度低,长时间使用后,匣钵底部容易发生下垂变形。
堇青石匣钵的变形开裂并不是匣钵的主要缺点,匣钵内的SiO2和锂电池粉中碱性金属氧化物反应,造成匣钵起皮,这些反应物进入锂电池粉,直接影响了锂电池粉的质量,使锂电池粉的性能大幅降低。因此,锂电池粉生产厂家除了要求匣钵具有一定的使用寿命外,匣钵在使用过程中不能和锂电池粉发生反应起皮,污染锂电池粉,使锂电池粉的性能降低。
发明内容
发明目的:本发明旨在提供一种使匣钵材质偏碱性、不与锂电池粉发生反应且满足钵体抗热震稳定性的镁橄榄石-刚玉匣钵。
技术方案:本发明的镁橄榄石-刚玉匣钵,匣钵包括如下重量份的组分:预烧镁橄榄石50-60份、高岭土4-8份、烧结板状氧化铝16-20份以及活性氧化铝14-18份。
发明人研究发现烧结锂电池粉用匣钵中MgO含量越高,匣钵抵抗锂电池粉的侵蚀性能越好,生产的锂电池粉性能更稳定。镁橄榄石中的氧化镁含量高,能提高匣钵抗碱性锂电池粉的侵蚀能力,但是不烧的镁橄榄石有一些无机杂质,含铁杂质容易造成黑红斑和小融洞,还有少量的低熔点物质经烧结后,渗出匣钵表面,和匣钵基材反应生成鱼鳞状灰色薄皮物,这些鱼鳞状的薄皮物容易进入锂电池粉,污染锂电池粉,使锂电池粉的性能降低,所以本发明先将镁橄榄石预烧,然后作为原料使用。
除了镁橄榄石,还可以通过添加镁砂或镁铝尖晶石增加氧化镁的含量,但是镁砂或镁铝尖晶石容易水化,成型之前的混合料容易因氧化镁水化变干,不好成型;同时,匣钵生产因MgO水化原因,只能添加少量的镁砂或铝镁尖晶石,抗锂电池粉侵蚀不好,一般25次使用就因反应起皮,污染锂电池粉。
为保证产品内部成分的均匀性和强度,使产品密度达到最大紧密堆积,镁橄榄石包括粒径2-1mm 30-35份、1-0mm 5-10份以及160-180目12-15份。
本发明预烧镁橄榄石的制法是将镁橄榄石在1300-1400℃温度下预烧2-4h得到的,优选的烧结温度为1370-1400℃,优选的烧结时间为3-4h。
本发明使用的刚玉为烧结板状刚玉,又叫烧结板状氧化铝,它和普通的氧化铝区别在于晶体结构呈板状,比粒状晶体具有更好的抗热震稳定性且具有较高的荷重软化温度;优选的,烧结板状氧化铝的粒径为1-0mm。
本发明中,高岭土的粒径为300-350目;活性氧化铝的粒径为1300-1600目。
为提高半成品的强度和产品的中高温强度,匣钵还包括如下重量份的组分:络合铝镁胶结合剂1-2份、糊精0.2-0.6份及木质磺酸钙0.1-0.5份,其中,铝镁结合剂主要是促进高温烧结,提高产品的高温性能;优选的,络合铝镁胶结合剂的粒径为80-120目。
本发明镁橄榄石-刚玉匣钵的制备方法,包括如下步骤:按重量份称取所述组分进行混合碾压、静置困料、液压成型、烘干、烧成即得。
其中,所述烘干的温度为100-120℃,烘干的时间为20-30h;所述烧成的温度为1200-1400℃,烧成的时间为3-5h。
反应机理:锂电池粉为偏碱性的氧化物,在高温时与碱性氧化物不浸润,不发生反应,但主要碱性耐火原料镁砂、铝镁尖晶的抗热震稳定性偏差,而且在生产成型时,MgO容易吸水而水化,生成Mg(OH)2,使混炼好的待成型原料变干,影响成型效果。在烧结过程中,由于Mg(OH)2受热分解,会造成产品内部密实度不够,甚至产生小裂纹。而镁铝尖晶石的抗水化性能虽远优于MgO,但不能多加,当加入量超过总体重量的20%时,原料也会发生大量水化,不能成型,同时它的抗热震稳定性也不能满足使用要求。矿物原料镁橄榄石的耐火度超过1710℃,镁含量在35-55%,没有水化现象,具有较好的抗热震稳定性,不经过烧结,可以直接用来生产耐火材料。所以从这些方面来讲,选择镁橄榄石是生产偏碱性匣钵的理想原料。但由于该原料为生矿,本身含有一些较多的无机杂质和腐烂有机物,用该原料生产的匣钵表面存在较多的“黑红斑”和融洞,影响产品的外观和使用效果,另外,原料中含有一些低熔物,生产出来的匣钵表面因低熔物在烧结过程中渗出和匣钵表面物质反应,造成匣钵表面分布鱼鳞状的薄皮,在使用中容易脱落,混入锂电池粉,厂家不愿使用。因此,本产品在生产前,把镁橄榄石放入高温窑预烧处理,使低熔物和镁橄榄石主要物质进行反应,黑红斑主要是铁元素引起的,原料通过预烧,部分铁也可转化为铁橄榄石,降低黑红斑和融洞现象。生产出来的匣钵产品表面较为光洁,“黑红斑”也大幅减少。此外,由于这几种原料的耐火度很高,在不添加其它低融物材料情况下,为使新产品在相对较低的温度下实现烧结,本试验选取络合铝镁胶做结合剂,在高温下实现烧结。
有益效果:与现有技术相比,本发明的匣钵在保障产品抗热震稳定性的情况下,降低匣钵材质中的SiO2含量,增加MgO含量,使匣钵材质偏碱性,不与锂电池粉发生反应,提高新产品的荷重软化温度,使匣钵在使用过程中不发生变形现象;与现用的堇青石匣钵相比,生产成本减少了1500元/吨,在批量试用时,使用寿命平均45次,匣钵表面不起皮,对锂电池粉没有任何污染;同时,本发明的制备方法简单可行,容易实现。
附图说明
图1为本发明的工艺流程图。
具体实施方式
下面结合附图对本发明的技术方案作进一步说明。
实施例1
称取2-1mm的预烧镁橄榄石35份,1-0mm预烧镁橄榄石10份,180目预烧镁橄榄石15份,325目高岭土6份,1-0mm烧结板状氧化铝18份,1500目活性氧化铝16份,外加100目络合镁铝胶1份,外加0.4份的糊精和0.3份的木质磺酸钙,放入泥料混炼机,以15转/分钟的速率,搅拌25-30分钟,使原料充分混合均匀,外加9份水,搅拌混合20分钟出料,放入原料桶,静置24小时困料。使用液压机在350吨压力下成型;坯体放置24小时,进入烘房进行110℃×24小时烘干;然后把匣钵放入高温窑经1380℃×4小时烧成,整个工艺流程参见图1,其中,镁橄榄石的预烧方法是将其1370℃温度下烧结3h得到的。
其中,镁橄榄石购自陕西汇泉冶金耐火材料有限公司,型号为M55;高岭土购自柳州巨州化工有限公司,型号为A35;烧结板状氧化铝购自江苏省晶辉耐火材料有限公司,型号为JGS-325;活性氧化铝购自山东淄博恒环铝业有限公司,型号为HTA-25;络合镁铝胶购自铁岭市朝辉节能技术开发有限公司,型号为W3297BX;糊精购自宜兴市荣茂化工有限公司;木质磺酸钙购自宜兴市荣茂化工有限公司。
由表1可知,该组试验原料配比适当,成型后的坯体表面被基质覆盖,表面光洁;坯体干燥后强度高,产品烧成后,表面光洁,融洞少。
表1实施例1制得匣钵的理化指标
对比例1
与实施例1相比,主要区别为镁橄榄石未经过预烧。
称取2-1mm的镁橄榄石生矿35份,1-0mm镁橄榄石生矿10份,180目镁橄榄石生矿15份,325目高岭土6份,1-0mm烧结板状氧化铝18份,1500目活性氧化铝16份,外加100目络合镁铝胶1份,外加0.4份的糊精和0.3份的木质磺酸钙,放入泥料混炼机,以15转/分钟的速率,搅拌15-20分钟,使原料充分混合均匀,外加9份水,搅拌混合20分钟出料,放入原料桶,静置24小时困料。使用液压机在350吨压力下成型;坯体放置24小时,进入烘房进行110℃×24小时烘干;然后把匣钵放入高温窑经1380℃×4小时烧成。
由表2可知,该组试验原料配比适当,成型后匣钵坯体表面被基质覆盖,表面光洁;坯体干燥后强度高,产品烧成后表面“黑红斑”、小环形裂纹、小融洞多,表面有鱼鳞状起皮。
表2对比例1制得匣钵的理化指标
对比例2
与实施例1相比,主要区别在于:1-0mm预烧镁橄榄石5份以及1-0mm烧结板状氧化铝23份。
称取2-1mm的预烧镁橄榄石35份,1-0mm预烧镁橄榄石5份,180目预烧镁橄榄石15份,325目高岭土6份,1-0mm烧结板状氧化铝23份,1500目活性氧化铝16份,外加100目络合镁铝胶1份,外加0.4份的糊精和0.3份的木质磺酸钙,放入泥料混炼机,以15转/分钟的速率,搅拌25-30分钟,使原料充分混合均匀,外加9份水,搅拌混合20分钟出料,放入原料桶,静置24小时困料。使用液压机在350吨压力下成型;坯体放置24小时,进入烘房进行110℃×24小时烘干;然后把匣钵放入高温窑经1380℃×4小时烧成。
由表3可知,该组试验原料配比适当,匣钵表面被基质覆盖,表面光洁;坯体干燥后强度高,产品烧成后,表面光洁,融洞少,但抗热震稳定性下降了一些,下降的原因在于镁橄榄石加入的总量下降,但得到的匣钵仍然符合一定的要求。
表3对比例2制得匣钵的理化指标
对比例3
与实施例1相比,主要区别在于:1-0mm预烧镁橄榄石20份以及1-0mm烧结板状氧化铝10份。
称取2-1mm的预烧镁橄榄石35份,1-0mm预烧镁橄榄石20份,180目预烧镁橄榄石15份,325目高岭土6份,1-0mm烧结板状氧化铝10份,1500目活性氧化铝16份,外加100目络合镁铝胶1份,外加0.4份的糊精和0.3份的木质磺酸钙,放入泥料混炼机,以15转/分钟的速率,搅拌25-30分钟,使各种原料充分混合均匀,外加9份水,搅拌混合20分钟出料,放入原料桶,静置24小时困料。使用液压机在350吨压力下成型;坯体放置24小时,进入烘房进行110℃×24小时烘干;然后把匣钵放入高温窑经1380℃×4小时烧成。
由表4可知,该组试验原料配比适当,匣钵表面被基质覆盖,表面光洁;坯体干燥后强度高,产品烧成后,表面“黑红斑”增多,融洞少,红斑主要是镁橄榄石中铁元素造成,随着加入量增多,黑红斑增多,但是抗热震稳定性增强,抗热震稳定性增强原因是镁橄榄石的抗热震稳定性比烧结板状氧化铝好,但为了减少“黑红斑”现象,仍然需要将1-0mm预烧镁橄榄石的重量份数控制在5-10份范围内。
表4对比例3制得匣钵的理化指标
对比例4
与实施例1相比,主要区别在于:络合镁铝胶3份。
称取2-1mm的预烧镁橄榄石35份,1-0mm预烧镁橄榄石10份,180目预烧镁橄榄石15份,325目高岭土6份,1-0mm烧结板状氧化铝18份,1500目活性氧化铝16份,100目络合镁铝胶3份,外加0.4份的糊精和0.3份的木质磺酸钙,放入泥料混炼机,以15转/分钟的速率,搅拌25-30分钟,使各种原材料充分混合均匀,外加9份水,搅拌混合20分钟出料,放入原料桶,静置24小时睏料。使用液压机在350吨压力下成型;坯体放置24小时,进入烘房进行110℃×24小时烘干;然后把匣钵放入高温窑经1380℃×4小时烧成。
由表5可知,该组试验原料配比适当,匣钵表面被基质覆盖,表面光洁;坯体干燥后强度高,产品烧成后,表面光洁,融洞少,表面有瓷化的现象,常温抗折强度升高,显气孔率下降,抗热震稳定性下降,这说明络合铝镁胶加入过量。
表5对比例4制得匣钵的理化指标
实施例2
称取2-1mm的预烧镁橄榄石30份,1-0mm预烧镁橄榄石8份,160目预烧镁橄榄石12份,300目高岭土8份,1-0mm烧结板状刚玉10份,1600目活性氧化铝14份,外加80目络合镁铝胶2份,外加0.2份的糊精和0.1份的木质磺酸钙,放入泥料混炼机,以15转/分钟的速率,搅拌25-30分钟,使原料充分分散,外加9份水,搅拌混合20分钟出料,放入原料桶,静置24小时困料。使用液压机在350吨压力下成型;坯体放置24小时,进入烘房进行100℃×30小时烘干;然后把匣钵放入高温窑经1200℃×5小时烧成,其中,镁橄榄石的预烧方法是将其1300℃温度下烧结4h得到的。
由表6可知,由于络合铝镁胶结合剂存在,其强度大于7.0Mpa,完全满足用户使用对强度的要求。
表6实施例2制得匣钵的理化指标
实施例3
称取2-1mm的预烧镁橄榄石33份,1-0mm预烧镁橄榄石9份,160目预烧镁橄榄石13份,350目高岭土4份,1-0mm烧结板状刚玉25份,1500目活性氧化铝18份,外加120目络合镁铝胶2份,外加0.6份的糊精和0.5份的木质磺酸钙,放入泥料混炼机,以15转/分钟的速率,搅拌25-30分钟,使原料充分分散,外加9份水,搅拌混合20分钟出料,放入原料桶,静置24小时困料。使用液压机在350吨压力下成型;坯体放置24小时,进入烘房进行120℃×20小时烘干;然后把匣钵放入高温窑经1400℃×3小时烧成,其中,镁橄榄石的预烧方法是将其1400℃温度下烧结2h得到的。
由表7可知,产品的烧结温度从1380℃提高至1400℃对产品的物理性能影响不是很大,产品的显气孔率减少,使产品的抗热震稳定性降低,这是因为产品受热后产生的体积膨胀,一定量显气孔的存在能够抵消其受热产生的体积效应。
表7实施例3制得匣钵的理化指标
Claims (8)
1.一种锂电池粉烧结用镁橄榄石-刚玉匣钵,其特征在于所述匣钵由如下重量份的原料制成:预烧镁橄榄石50-60份、烧结板状氧化铝10-25份、高岭土4-8份、活性氧化铝14-18份、络合铝镁胶结合剂1-2份、糊精0.2-0.6份及木质磺酸钙0.1-0.5份,所述预烧镁橄榄石包括粒径2mm 30-35份、1mm 5-10份以及160-180目12-15份。
2.根据权利要求1所述匣钵,其特征在于:所述预烧镁橄榄石的制法是将镁橄榄石在1300-1400℃温度下烧结2-4h。
3.根据权利要求1所述匣钵,其特征在于:所述烧结板状氧化铝的粒径为1mm。
4.根据权利要求1所述匣钵,其特征在于:所述高岭土的粒径为300-350目。
5.根据权利要求1所述匣钵,其特征在于:所述活性氧化铝的粒径为1300-1600目。
6.根据权利要求1所述匣钵,其特征在于:所述络合铝镁胶结合剂的粒径为80-120目。
7.权利要求1所述镁橄榄石-刚玉匣钵的制备方法,其特征在于包括如下步骤:按重量份称取各组分进行混合碾压、静置困料、液压成型、烘干、烧成即得。
8.根据权利要求7所述镁橄榄石-刚玉匣钵的制备方法,其特征在于:所述烘干的温度为100-120℃,烘干的时间为20-30h;所述烧成的温度为1200-1400℃,烧成的时间为3-5h。
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