CN110240483A - 一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法 - Google Patents
一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法 Download PDFInfo
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Abstract
本发明属于晶硅废砂浆二次利用技术领域,公开了一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法。本发明利用晶硅废砂浆固体废料为主要原料,通过较低温无压烧结,850℃下即可在碳化硅表面原位生长莫来石棒,进而制备出具有高气孔率和高强度的碳化硅多孔陶瓷,最终实现了晶硅废砂浆固体废料的二次利用和低成本制备碳化硅多孔陶瓷的目标。本发明充分利用资源,变废为宝;在使用传统烧结助剂的同时加入了催化剂,使得烧结温度大幅下降,从而减少了能源消耗和降低了制造成本。
Description
技术领域
本发明属于晶硅废砂浆二次利用技术领域,具体涉及一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法。
背景技术
本世纪以来,由于太阳能具有可再生性和清洁性等特点,人类对太阳能的利用日益增多,在全世界范围内掀起了开发和利用太阳能的热潮,太阳能光伏产业迅猛发展。太阳能电池所使用的多晶硅板是由硅锭经切割后再加工而成。在硅锭切割过程中,会有约一半比例的晶体硅以硅粉形式进入切削液中,并最终与碳化硅磨料、聚乙二醇(PEG)切削液、少量铁屑等一起形成废砂浆。晶硅废砂浆为光伏行业产生的大宗工业固液废弃物,如果不处理将其直接排放,不仅对环境会造成污染,而且也浪费了废砂浆中的硅和碳化硅等不可再生资源。因而,如何将硅锭切割过程中产生的大量废砂浆进行有效回收和利用,一直是光伏晶硅相关行业重点关注的一个课题。
目前,晶硅废砂浆处理领域主要采用双层有机溶剂沉淀法、相转移分离法、水力旋流器工艺、离心分离法等方法将废砂浆中的硅或碳化硅进行初步回收。然而,由于晶硅废砂浆中的硅和碳化硅颗粒粒径小而且粒度范围有重叠,两者理化性质又相近,因此分离硅和碳化硅的难度很高。基于此,通过预处理除去废砂浆中聚乙二醇,再以剩下的硅和碳化硅为主要原料制备碳化硅等先进陶瓷引起了研究者的注意。主要方法包括:一是加入炭黑与废砂浆中的硅反应,制备碳化硅粉体;二是通过反应烧结制备碳化硅致密陶瓷;三是通过炭黑填埋法在空气中1600℃以上高温烧结制备碳化硅多孔陶瓷。
但是,上述关于晶硅废砂浆的回收和利用方法仍存在一些明显不足。光伏企业在对晶硅废砂浆进行在线回收后,仍存在大量以碳化硅磨料为主,硅粉为辅的固体废料作为二次废料未能有效利用。在利用晶硅废砂浆为原料制备碳化硅等先进陶瓷过程中,烧结温度往往在1200℃以上,所以整个过程能源消耗较大。因此,如何将晶硅废砂浆经回收后的二次固体废料完全利用,同时低成本制备出性能较好的碳化硅陶瓷制品具有十分重要的意义。
发明内容
本发明目的在于提供一种通过晶硅废砂浆在较低温制备碳化硅多孔陶瓷的方法。这是一种利用晶硅废砂浆经在线回收后剩余的二次固体废料为主要原料,通过原位催化反应生长大量棒状莫来石晶体,从而在较低温度下制备出拥有高强度和高气孔率碳化硅多孔陶瓷的新技术方案,最终实现晶硅废砂浆固体废料的二次利用。
本发明目的通过以下技术方案实现:
一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,包括如下步骤:
(1)对晶硅废砂浆固体废料进行预处理,得到预处理后的固体废料;
(2)向预处理后的固体废料中加入造孔剂、烧结助剂、催化剂,再经球磨混料、过筛,得到原料粉体;
(3)向原料粉体中加入成型剂,混合均匀后置于模具中加压成型,干燥脱脂后得到多孔陶瓷生坯;
(4)将多孔陶瓷生坯置于烧结炉中,在空气气氛下无压烧结,得到碳化硅多孔陶瓷制品。
步骤(1)中所述预处理方法为:将晶硅废砂浆固体废料依次经盐酸溶液除铁、水洗和干燥。
所述预处理后的固体废料中各组分的质量分数为:碳化硅大于等于90%,硅粉小于等于10%。
优选地,步骤(2)中所述造孔剂为活性炭粉,其加入量占原料粉体质量分数的15%~20%。
优选地,所述烧结助剂为氧化铝粉,其加入量占原料粉体质量分数的20%~35%。
优选地,所述催化剂为三氧化钼粉,其加入量占原料粉体质量分数的0.5%~6%。
优选地,所述球磨混料的条件为:球料比为(8~10):1,球磨混合时间为10~40h。
优选地,步骤(3)中所述成型剂为羧甲基纤维素钠溶液,其加入量为原料粉体质量分数的1%~5%。
优选地,所述干燥脱脂的温度为110~120℃,时间12~24h。
优选地,步骤(4)中所述烧结的工艺条件为:先升温至500~800℃保温1~2h去除造孔剂,然后升温至850~1000℃进行多孔陶瓷烧结,保温时间为2~5h。所述升温速率优选为2~10℃/min。
相比现有技术,本发明具有如下突出优点及有益效果:
(1)本发明制备碳化硅多孔陶瓷的主要原料来自光伏行业晶硅废砂浆在线回收后剩余工艺废弃物,解决了晶硅废砂浆回收中资源化利用过低的问题,同时降低了碳化硅多孔陶瓷的原料成本。
(2)本发明通过添加氧化铝作烧结助剂,使得碳化硅表面原位生长出大量棒状莫来石晶体,最终可以制备出既具有较高孔隙率也具有较高抗弯强度的碳化硅多孔陶瓷。
(3)本发明通过添加三氧化钼作为棒状莫来石晶体生长的催化剂,可显著降低碳化硅多孔陶瓷的烧结温度,减少了能源消耗,因而降低了碳化硅多孔陶瓷的生产成本。
附图说明
图1为本发明实施例1所得碳化硅多孔陶瓷的XRD衍射图。
图2和图3为本发明实施例1所得碳化硅多孔陶瓷的断口扫描电镜图。
具体实施方式
下面结合实施例及附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例1
(1)取1kg废砂浆粉,加入浓度为2mol/L的盐酸溶液1.5L,机械搅拌升温至85℃,直到不再有气泡冒出时停止搅拌。放入漏斗中过滤,将得到的滤饼用蒸馏水多次冲洗至滤液pH=7。取出滤饼置于烘箱干燥,过250目筛后得主原料粉体待用。
(2)取61.5g步骤(1)预处理后的废砂浆粉和9g MoO3、30g活性炭粉、52.5g纳米氧化铝,将各原料加入球磨罐中,按球料比10:1加入磨球后封罐,于球磨机上混料40h,过筛得到混合原料。
(3)步骤(2)的混合原料加入5wt.%的羧甲基纤维素钠溶液,混合均匀后用不锈钢模具压制成长40mm、宽3mm、厚3mm的长方体生坯。将压制好的生坯置于烘箱中于120℃下脱脂24h。
(4)将脱脂后的生坯放入烧结炉中,开始以2℃/min升温至800℃保温1h,进行除炭,然后以2℃/min升温至850℃,保温3h,之后随炉冷却至室温得到碳化硅多孔陶瓷。经测试,碳化硅多孔陶瓷的气孔率为42.12%,抗弯强度44.66MPa。
本实施例所得碳化硅多孔陶瓷的XRD衍射图谱如图1所示。图1在本专利所述的温度范围内,将于一定温度烧结的碳化硅多孔陶瓷的XRD衍射图展示。从图中可以看出在850℃所得的多孔陶瓷的主要物相为碳化硅和莫来石。
本实施例所得碳化硅多孔陶瓷的断口扫描电镜图片如图2和图3所示。(图2是在850℃的多孔陶瓷的断口的形貌全图,可以看出有明显的孔隙存在,具有多孔陶瓷的结构特征。图3是断口的微观形貌图,可以看出在碳化硅颗粒和在颗粒周围原位生长出大量棒状莫来石。)
实施例2
(1)取1kg废砂浆粉,加入浓度为2mol/L的盐酸溶液1.5L,机械搅拌升温至85℃,直到不再有气泡冒出时停止搅拌。放入漏斗中过滤,将得到的滤饼用蒸馏水多次冲洗至滤液pH=7。取出滤饼置于烘箱干燥,过250目筛后待用。
(2)取96.75g步骤(1)预处理后的废砂浆粉和0.75g MoO3、22.5g活性炭粉、30g氧化铝,将各原料加入球磨罐中,按球料比8:1加入磨球后封罐,于球磨机上混料10h,过筛得到混合原料。
(3)往步骤(2)的混合原料加入1wt.%的羧甲基纤维素钠溶液,混合均匀后用不锈钢模具压制成长40mm、宽3mm、厚3mm的长方体生坯。将压制好的生坯置于烘箱中于110℃下脱脂12h。
(4)将脱脂后的生坯放入烧结炉中,开始以10℃/min升温至800℃保温1h,进行除碳,然后以10℃/min升温至1000℃,保温3h,之后随炉冷却至室温得到碳化硅多孔陶瓷。经测试,所得碳化硅多孔陶瓷的气孔率为44.96%,抗弯强度为50.17MPa。
实施例3
(1)取1kg废砂浆粉,加入浓度为2mol/L的盐酸溶液1.5L,机械搅拌升温至85℃,直到不再有气泡冒出时停止搅拌。放入漏斗中过滤,将得到的滤饼用蒸馏水多次冲洗至滤液pH=7。取出滤饼置于烘箱干燥,过250目筛后待用。
(2)取81.5g步骤(1)预处理后的废砂浆粉和4g MoO3、27g活性炭粉、37.5g氧化铝,将各原料加入球磨罐中,按球料比10:1加入磨球后封罐,于球磨机上混料20h,过筛得到混合原料。
(3)往步骤(2)的混合原料加入2wt.%的羧甲基纤维素钠溶液,混合均匀后用不锈钢模具压制成长40mm、宽3mm、厚3mm的长方体生坯。将压制好的生坯置于烘箱中于120℃下脱脂15h。
(4)将脱脂后的生坯放入烧结炉中,开始以2.5℃/min升温至800℃保温1h,进行除碳,然后以2.5℃/min升温至950℃,保温3h,之后随炉冷却至室温得到碳化硅多孔陶瓷。经测试,所得碳化硅多孔陶瓷的气孔率为45.60%,抗弯强度为41.12MPa。
实施例4
(1)取1kg废砂浆粉,加入浓度为2mol/L的盐酸溶液1.5L,机械搅拌升温至85℃,直到不再有气泡冒出时停止搅拌。放入漏斗中过滤,将得到的滤饼用蒸馏水多次冲洗至滤液pH=7。取出滤饼置于烘箱干燥,过250目筛后待用。
(2)取80g步骤(1)预处理后的废砂浆粉和4g MoO3、27g活性炭粉、35g氧化铝,将各原料加入球磨罐中,按球料比10:1加入磨球后封罐,于球磨机上混料40h,过筛得到混合原料。
(3)往步骤(2)的混合原料加入3wt.%的羧甲基纤维素钠溶液,混合均匀后用不锈钢模具压制成长40mm、宽3mm、厚3mm的长方体生坯。将压制好的生坯置于烘箱中于110℃下脱脂20h。
(4)将脱脂后的生坯放入烧结炉中,开始以2℃/min升温至800℃保温1h,进行除碳,然后以5℃/min升温至900℃,保温3h,之后随炉冷却至室温得到碳化硅多孔陶瓷。经测试,所得碳化硅多孔陶瓷的气孔率为45.44%,抗弯强度为42.96MPa。
实施例5
(1)取1kg废砂浆粉,加入浓度为2mol/L的盐酸溶液1.5L,机械搅拌升温至85℃,直到不再有气泡冒出时停止搅拌。放入漏斗中过滤,将得到的滤饼用蒸馏水多次冲洗至滤液pH=7。取出滤饼置于烘箱干燥,过250目筛后待用。
(2)取76g步骤(1)预处理后的废砂浆粉和4g MoO3、27g活性炭粉、45g氧化铝,将各原料加入球磨罐中,按球料比10:1加入磨球后封罐,于球磨机上混料35h,过筛得到混合原料。
(3)往步骤(2)的混合原料加入1.5wt.%的羧甲基纤维素钠溶液,混合均匀后用不锈钢模具压制成长40mm、宽3mm、厚3mm的长方体生坯。将压制好的生坯置于烘箱中于115℃下脱脂20h。
(4)将脱脂后的生坯放入烧结炉中,开始以2℃/min升温至800℃保温1h,进行除碳,然后以5℃/min升温至875℃,保温3h,之后随炉冷却至室温得到碳化硅多孔陶瓷。经测试,所得碳化硅多孔陶瓷的气孔率为44.78%,抗弯强度为42.78MPa。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (10)
1.一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于包括如下步骤:
(1)对晶硅废砂浆固体废料进行预处理,得到预处理后的固体废料;
(2)向预处理后的固体废料中加入造孔剂、烧结助剂、催化剂,再经球磨混料、过筛,得到原料粉体;
(3)向原料粉体中加入成型剂,混合均匀后置于模具中加压成型,干燥脱脂后得到多孔陶瓷生坯;
(4)将多孔陶瓷生坯置于烧结炉中,在空气气氛下无压烧结,得到碳化硅多孔陶瓷制品。
2.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于步骤(1)中所述预处理方法为:将晶硅废砂浆固体废料依次经盐酸溶液除铁、水洗和干燥。
3.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于:所述预处理后的固体废料中所含成分的质量分数为:碳化硅大于等于90%,硅小于等于10%。
4.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于:步骤(2)中所述造孔剂为活性炭粉,其加入量占原料粉体质量分数的15%~20%。
5.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于:所述烧结助剂为氧化铝粉,其加入量占原料粉体质量分数的20%~35%。
6.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于:所述催化剂为三氧化钼粉,其加入量占混合粉体质量分数的0.5%~6%。
7.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于所述球磨混料的条件为:球料比为(8~10):1,球磨混合时间为10~40h。
8.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于:步骤(3)中所述成型剂为羧甲基纤维素钠溶液,其加入量为原料粉体质量分数的1%~5%。
9.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于:步骤(3)中所述干燥脱脂的温度为110~120℃,时间12~24h。
10.根据权利要求1所述的一种利用晶硅废砂浆制备碳化硅多孔陶瓷的方法,其特征在于步骤(4)中所述烧结的工艺条件为:先升温至500~800℃保温1~2h去除造孔剂,然后升温至850~1000℃进行多孔陶瓷烧结,保温时间为2~5h,所述升温速率为2~10℃/min。
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