CN105541311B - 多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法 - Google Patents
多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法 Download PDFInfo
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Abstract
本发明涉及无机非金属材料领域,是一种多晶硅铸锭应氮化硅结合熔融石英坩埚的制备方法,采用原位固化成型工艺、氮化烧成制备氮化硅结合熔融石英坩埚,该方案选用一定粒度和纯度的粉料做原料,配制含有有机单体、交联剂、水和粉体的悬浮浆料,加入适量引发剂,搅拌均匀,对料浆除气处理,倒入石膏模具中,静置固化,坯体干燥养护,在氮气气氛下烧成得到制品。该方法制得的坩埚,具有材料内部结构均一,抗热震稳定性好、高温强度优异,使用稳定性好,使用寿命长等优点。
Description
技术领域
本发明涉及无机非金属材料技术领域,具体涉及一种多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法。
背景技术
太阳能电池是将光能直接转换为电能的一种装置,太阳能电池的开发是人类科学利用太阳能的突破进展,是解决传统燃料能源日益枯竭及环境污染的新途径。一般可做太阳能电池材料的有单晶硅、多晶硅、GaAs、CdTe、InP等,但在现有技术推广使用的多为多晶硅材料。
太阳能级多晶硅多采用冶金法制备,使用坩埚承装多晶硅原料,在高温下多晶硅原料熔化结晶,冷却,产出多晶硅铸锭。坩埚是多晶硅生产不可替代的关键部件,目前采用熔融石英坩埚坩埚作为多晶硅铸锭的容器,熔融石英坩埚多采用传统的注浆浇注成型工艺,因体积较大而造成生产技术难度大、产品成品率低等问题。
在制备多晶硅铸锭时,在原料高温熔化、晶体生长过程中,熔融硅与熔融石英坩埚长时间接触后产生渗透侵蚀,同时坩埚中的杂质渗透到硅熔体中,在晶体冷却过程中,很容易因两者结合紧密而造成晶体硅和坩埚破裂,影响多晶硅铸锭的性能,现有技术采用在坩埚内壁涂敷氮化硅涂层,阻止坩埚中的杂质在铸造过程中进入硅熔体中,但因氮化硅涂层基本没有自烧结,在高温冶炼过程中,因氮化硅涂层与熔融石英坩埚结合强度差导致涂层开裂、脱落,二次污染铸锭,造成多晶硅铸锭生产效率低下,产品合格率不高的问题。
氮化硅结合熔融石英坩埚采用浇注成型、氮化烧成制备,制备的制品结合熔融石英和氮化硅两者的优点,具有良好的热震稳定性、优异的高温性能、成品率高和可重复使用等优点,坩埚制品表面因氮化烧成形成氮化硅表层。在使用过程中,表层不会因与本体热膨胀系数不同而产生高温开裂、脱落等问题。与传统方法相比较,缩短了坩埚生产周期,降低了生产成本,坩埚可重复使用,降低了多晶硅杂质含量,提高了多晶硅成品率。
通过大量文献查阅,多晶硅生产基本使用复合氮化硅涂层的高纯融融熔融石英坩埚,仅有少量反应烧结氮化硅陶瓷坩埚的研究,但使用性能和经济效益并不能满足多晶硅厂家的要求。对于氮化硅结合熔融石英坩埚的技术和使用未见专利和文献报道。
发明内容
为解决上述技术问题,本发明的目的是提出一种多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法。
本发明为完成上述目的采用如下技术方案:
一种多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法,所述的制备方法选用一定粒度和纯度的粉体做原料采用原位固化成型工艺、氮化烧成工艺制备氮化硅结合熔融石英坩埚,其具体工艺步骤为:
1)原料的选取:
选取平均粒径为20um,SiO2≥99.99wt%的熔融石英微粉、平均粒径为2.5 um,Si≥99 wt%的金属硅粉和平均粒径3.5 um,Si3N4≥95 wt%的氮化硅粉体为原料,其中,金属硅粉的加入量为熔融石英质量的20%~50%;氮化硅粉体的加入量为熔融石英质量的30%~100%;
2)预混液的制备:
采用水为分散介质,将水、有机单体、交联剂配置成预混液;预混中水与步骤1)与原料的质量比为3:7~1:1;预混液中有机单体、交联剂的加入量分别为水质量的10%~40%、10%~1%;
3)悬浮浆料的制备:
将步骤1)中的原料、步骤2)中所制备的预混液与分散剂一同放入球磨罐中,球磨混合制得分散均匀、流动性好的悬浮浆料;其中分散剂的加入量为原料质量的1%~10%;
4)悬浮浆料的原位固化成型:
在步骤3)所制备的悬浮浆料中加入引发剂,搅拌均匀后对悬浮浆料进行真空除气处理,导入石膏模具中,在一定的温度和湿度下浆料原位固化成型后脱模;引发剂的加入量为有机单体质量的5%~10%;
5)坯体的干燥和氮化烧成:
将脱模后的坯体干燥后在氮气气氛炉中以1~3℃/min的升温速率升温至1000~1200℃,并保温2~4小时烧成,制得氮化硅结合熔融石英坩埚。
所述的有机单体为丙烯酸胺、羟甲基丙烯酸胺、甲基丙烯酸胺中的一种。
所述的交联剂为亚甲基双丙烯酸胺、多已二甲二醇二甲基丙烯酸胺、聚乙二醇二甲基丙烯酸脂中的一种。
所述的分散剂为十二烷基硫酸钠、磷酸三乙酯和聚丙烯酸中的一种。
所述的引发剂为过硫酸铵或过硫酸钾。
浆料原位固化成型的温度为30~60℃、湿度为75%~95%。
本发明提出的一种多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法,通过原位固化成型、氮化烧成制备氮化硅结合石英坩埚,材料组织结构均一,具备良好的热震稳定性、优异的高温强度等性能,满足多晶硅铸锭冶金的要求,解决了坩埚涂层开裂、脱落的问题,提高了多晶硅铸锭的成品率和性能,此方法制备的坩埚成品率高,可重复使用,具备良好的使用性能。
具体实施方式
实施例1:
1.1、配制浆料:以丙烯酰胺为单体,亚甲基双丙烯酰胺为交联剂,十二烷基硫酸钠为分散剂,以水为分散介质,其中水、丙烯酰胺和亚甲基双丙烯酰胺按质量比100:10:10的比例制备预混液;SiO2:Si:Si3N4按质量比为100:20:30的比例配置原料;然后按照原料与水的质量比为3:7的比例加入到球磨机中进行球磨;以氧化锆球为球磨介质,球磨混合50min,制备分散均匀、稳定、流动性好的浆料,分散剂为粉料质量的10%;
1.2、成型和干燥:将料浆倒入搅拌罐中,引发剂过硫酸铵加入量为有机单体质量的5%;搅拌均匀,对浆料进行除气抽真空处理,然后注入到石膏模具内,在30℃、90%RH湿度下原位固化成型。脱模得到坯体,养护干燥,干燥温度和湿度分别控制在50℃和95%RH;
1.3、烧成:将干燥好的坯体放入到电炉中,在氮气气氛下以1℃/min升温至1000℃保温4h,制得氮化硅结合石英坩埚。
实施例2:
2.1、配制浆料:以羟甲基丙烯酸胺为单体,聚乙二醇二甲基丙烯酸脂为交联剂,磷酸三乙酯为分散剂,以水为分散介质,其中水、丙烯酰胺和亚甲基双丙烯酰胺按质量比为100:40:1的比例制备预混液;SiO2:Si:Si3N4按质量比为100:50:30的比例配置原料;然后按照原料与水的质量比为1:1的比例加入到球磨机中进行球磨;以氧化锆球为球磨介质,球磨混合50min,制备分散均匀、稳定、流动性好的浆料,分散剂为原料质量的1%;
2.2、成型和干燥:将料浆倒入搅拌罐中,引发剂过硫酸钾加入量为有机单体质量的10%。搅拌均匀,对浆料进行除气抽真空处理,然后注入到石膏模具内,在60℃、75%RH湿度下原位固化成型。脱模得到坯体,养护干燥,干燥温度和湿度分别控制在60℃和90%RH;
2.3、烧成:将干燥好的坯体放入到电炉中,在氮气气氛下以1℃/min升温至1200℃保温2h,制得氮化硅结合石英坩埚。
实施例3:
3.1、配制浆料:以羟甲基丙烯酸胺为单体,多已二甲二醇二甲基丙烯酸胺为交联剂,聚丙烯酸为分散剂,以水为分散介质,其中水、丙烯酰胺和亚甲基双丙烯酰胺按质量比为100:40:5的比例制备预混液;SiO2:Si:Si3N4按质量比为100:20:100的比例配置原料;然后按照原料与水的质量比为1:1的比例加入到球磨机中进行球磨;以氧化锆球为球磨介质,球磨混合50min,制备分散均匀、稳定、流动性好的二氧化锆浆料,分散剂为粉料质量的5%;
3.2、成型和干燥:将料浆倒入搅拌罐中,引发剂过硫酸钾加入量为有机单体质量的5%。搅拌均匀,对浆料进行除气抽真空处理,然后注入到石膏模具内,在60℃、90%RH湿度下原位固化成型。脱模得到坯体,养护干燥,干燥温度和湿度分别控制在70℃和95%RH;
3.3、烧成:将干燥好的坯体放入到电炉中,在氮气气氛下以2℃/min升温至1000℃保温4h,制得氮化硅结合石英坩埚;
实施例4:
4.1、配制浆料:以甲基丙烯酸胺为单体,亚甲基双丙烯酰胺为交联剂,十二烷基硫酸钠为分散剂,以水为分散介质,其中水、丙烯酰胺和亚甲基双丙烯酰胺按质量比为100:10:10的比例制备预混液,SiO2:Si:Si3N4按质量比为100:50:100的比例配置原料;然后按照原料与水的质量比为3:7的比例加入到球磨机中进行球磨;以氧化锆球为球磨介质,球磨混合50min,制备分散均匀、稳定、流动性好的二氧化锆浆料,分散剂为粉料质量的1%;
4.2、成型和干燥:将料浆倒入搅拌罐中,引发剂过硫酸铵加入量为有机单体质量的7%。搅拌均匀,对浆料进行除气抽真空处理,然后注入到石膏模具内,在40℃、80%RH湿度下原位固化成型。脱模得到坯体,养护干燥,干燥温度和湿度分别控制在60℃和75%RH。
4.3、烧成:将干燥好的坯体放入到电炉中,在氮气气氛下以3℃/min升温至1200℃保温2h,制得氮化硅结合石英坩埚。
实施例5:
5.1、配制浆料:以丙烯酰胺为单体,多已二甲二醇二甲基丙烯酸胺为交联剂,十二烷基硫酸钠为分散剂,以水为分散介质,其中水、丙烯酰胺和亚甲基双丙烯酰胺按质量比为100:20:1的比例制备预混液,SiO2:Si:Si3N4按质量比为100:20:50的比例配置原料,然后按照原料与水的质量比为5:7的比例加入到球磨机中进行球磨;以氧化锆球为球磨介质,球磨混合50min,制备分散均匀、稳定、流动性好的二氧化锆浆料,分散剂为粉料质量的6%。
5.2、成型和干燥:将料浆倒入搅拌罐中,引发剂过硫酸铵加入量为有机单体质量的10%。搅拌均匀,对浆料进行除气抽真空处理,然后注入到石膏模具内,在30℃、90%RH湿度下原位固化成型。脱模得到坯体,养护干燥,干燥温度和湿度分别控制在50℃和75%RH。
5.3、烧成:将干燥好的坯体放入到电炉中,在氮气气氛下以1℃/min升温至1100℃保温4h,制得氮化硅结合石英坩埚。
实施例6:
6.1、配制浆料:以甲基丙烯酸胺为单体,聚乙二醇二甲基丙烯酸脂为交联剂,磷酸三乙酯为分散剂,以水为分散介质,其中水、丙烯酰胺和亚甲基双丙烯酰胺按质量比100:20:5的比例制备预混液,SiO2:Si:Si3N4按质量比为100:30:70的比例配置原料,然后按照原料与水的质量比为6:7的比例加入到球磨机中进行球磨;以氧化锆球为球磨介质,球磨混合50min,制备分散均匀、稳定、流动性好的二氧化锆浆料,分散剂为粉料质量的8%;
6.2、成型和干燥:将料浆倒入搅拌罐中,引发剂过硫酸加入量为有机单体质量的5%。搅拌均匀,对浆料进行除气抽真空处理,然后注入到石膏模具内,在40℃、85%RH湿度下原位固化成型。脱模得到坯体,养护干燥,干燥温度和湿度分别控制在100℃和95%RH;
6.3、烧成:将干燥好的坯体放入到电炉中,在氮气气氛下以2℃/min升温至1200℃保温3h,制得氮化硅结合石英坩埚。
实施例7:
7.1、配制浆料:以丙烯酰胺为单体,聚乙二醇二甲基丙烯酸脂为交联剂,聚丙烯酸为分散剂,以水为分散介质,其中水、丙烯酰胺和亚甲基双丙烯酰胺按质量比100:30:8的比例制备预混液,SiO2:Si:Si3N4按质量比为100:50:50的比例配置原料,然后按照原料与水的质量比为4:7的比例加入到球磨机中进行球磨;以氧化锆球为球磨介质,球磨混合50min,制备分散均匀、稳定、流动性好的二氧化锆浆料,分散剂为粉料质量的10%;
7.2、成型和干燥:将料浆倒入搅拌罐中,引发剂过硫酸钾加入量为有机单体质量的6%。搅拌均匀,对浆料进行除气抽真空处理,然后注入到石膏模具内,在50℃、75%RH湿度下原位固化成型。脱模得到坯体,养护干燥,干燥温度和湿度分别控制在90℃和95%RH;
7.3、烧成:将干燥好的坯体放入到电炉中,在氮气气氛下以3℃/min升温至1000℃保温3h,制得氮化硅结合石英坩埚。
实施例8:
8.1、配制浆料:以羟甲基丙烯酸胺为单体,亚甲基双丙烯酰胺为交联剂,磷酸三乙酯为分散剂,以水为分散介质,其中水、丙烯酰胺和亚甲基双丙烯酰胺按质量比100:20:7的比例制备预混液,SiO2:Si:Si3N4按质量比为100:50:60的比例配置原料,然后按照原料与水的质量比为1:1的比例加入到球磨机中进行球磨;以氧化锆球为球磨介质,球磨混合50min,制备分散均匀、稳定、流动性好的二氧化锆浆料,分散剂为粉料质量的10%;
8.2、成型和干燥:将料浆倒入搅拌罐中,引发剂过硫酸铵加入量为有机单体质量的8%。搅拌均匀,对浆料进行除气抽真空处理,然后注入到石膏模具内,在60℃、75%RH湿度下原位固化成型。脱模得到坯体,养护干燥,干燥温度和湿度分别控制在10℃和75%RH;
8.3、烧成:将干燥好的坯体放入到电炉中,在氮气气氛下以1℃/min升温至1050℃保温4h,制得氮化硅结合石英坩埚。
Claims (6)
1.一种多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法,其特征在于:所述的制备方法选用一定粒度和纯度的粉体做原料采用原位固化成型工艺、氮化烧成工艺制备氮化硅结合熔融石英坩埚,其具体工艺步骤为:
1)原料的选取:
选取平均粒径为20um,SiO2≥99.99wt%的熔融石英微粉、平均粒径为2.5 um,Si≥99wt%的金属硅粉和平均粒径3.5 um,Si3N4≥95 wt%的氮化硅粉体为原料;其中,金属硅粉的加入量为熔融石英质量的20%~50%;氮化硅粉体的加入量为熔融石英质量的30%~100%;
2)预混液的制备:
采用水为分散介质,将水、有机单体、交联剂配置成预混液;预混中水与步骤1)与原料的质量比为3:7~1:1;预混液中有机单体、交联剂的加入量分别为水质量的10%~40%、10%~1%;
3)悬浮浆料的制备:
将步骤1)中的原料、步骤2)中所制备的预混液与分散剂一同放入球磨罐中,球磨混合制得分散均匀、流动性好的悬浮浆料;其中分散剂的加入量为原料质量的1%~10%;
4)悬浮浆料的原位固化成型:
在步骤3)所制备的悬浮浆料中加入引发剂,搅拌均匀后对悬浮浆料进行真空除气处理,导入石膏模具中,在一定的温度和湿度下浆料原位固化成型后脱模;引发剂的加入量为有机单体质量的5%~10%;
5)坯体的干燥和氮化烧成:
将脱模后的坯体干燥后在氮气气氛炉中以1~3℃/min的升温速率升温至1000~1200℃,并保温2~4小时烧成,制得氮化硅结合熔融石英坩埚。
2.如权利要求1所述的多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法,其特征在于:所述的有机单体为丙烯酸胺、羟甲基丙烯酸胺、甲基丙烯酸胺中的一种。
3.如权利要求1所述的多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法,其特征在于:所述的交联剂为亚甲基双丙烯酸胺、聚乙二醇二甲基丙烯酸脂中的一种。
4.如权利要求1所述的多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法,其特征在于:所述的分散剂为十二烷基硫酸钠、磷酸三乙酯和聚丙烯酸中的一种。
5.如权利要求1所述的多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法,其特征在于:所述的引发剂为过硫酸铵或过硫酸钾。
6.如权利要求1所述的多晶硅铸锭用氮化硅结合熔融石英坩埚的制备方法,其特征在于:浆料原位固化成型的温度为30~60℃、湿度为75%~95%。
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