CN116949556A - 一种氮氧化硅-石英复合材料坩埚及其制备方法 - Google Patents
一种氮氧化硅-石英复合材料坩埚及其制备方法 Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 53
- 239000010703 silicon Substances 0.000 title claims abstract description 53
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- 239000000203 mixture Substances 0.000 claims abstract description 47
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 38
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 38
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- HMOQPOVBDRFNIU-UHFFFAOYSA-N barium(2+);dioxido(oxo)silane Chemical compound [Ba+2].[O-][Si]([O-])=O HMOQPOVBDRFNIU-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种氮氧化硅‑石英复合材料坩埚及其制备方法，以氮氧化硅与石英的复合材料作为坩埚的埚壁，先由石英砂与高纯氮化硅粉混合形成混合料，以混合料为原料采用旋转模具法‑电弧熔制法制作坩埚，加热保温过程中混合料粉体中的氮化硅与部分石英砂在高温下反应形成氮氧化硅，电弧加热保温时间比同等规格纯石英坩埚延长20～80％，坩埚的埚壁的组成为均匀氮氧化硅与石英的复合材料，或氮氧化硅含量从坩埚壁外向里逐渐增加的梯度复合材料，或者外层石英内层上述复合材料。所得复合材料坩埚强度高、抗硅熔体润湿性好、抗气泡迁移能力强、寿命长，以其生产的直拉单晶硅氧含量低，可替代纯石英坩埚用于规模化直拉单晶硅生产。
Description
技术领域
本发明属于无机非金属材料与器件制备技术领域，具体涉及一种氮氧化硅-石英复合材料坩埚及其制备方法。
背景技术
直拉法简称CZ法，在一个直筒型的热系统中，将装在高纯度石英坩埚中的多晶硅熔化，然后将籽晶插入熔体表面进行熔接，将旋转的籽晶下降与熔体浸润接触，逐步提升，经引颈、缩颈、放肩、等径控制、收尾等步骤。
在直拉单晶硅过程中最重要的设备之一就是坩埚，光伏和半导体微电子器件领域用直拉单晶硅的生产普遍采用石英坩埚。这种坩埚存在内壁石英材料在硅熔体中局部溶蚀造成单晶硅产品中氧含量升高、以及坩埚寿命受限的问题。坩埚寿命受限的主要原因是石英坩埚内壁石英材料长期使用后晶化造成剥落颗粒进入熔体破坏单晶硅生长；而坩埚中由气相包裹体聚集形成并内壁迁移鼓出的气泡往往会促进这种剥落。此外行业中还存在坩埚内层制备所需的高纯石英砂原材料紧缺的现实问题。
现有技术中普遍采用对石英坩埚内壁涂覆氢氧化钡涂层，或直接在拉晶装料时添加碳酸钡粉，使之形成一层硅酸钡盐成分的内壁涂层，但这只能够一定程度缓解上述部分问题。
发明内容
针对现有技术中的不足与难题，本发明旨在提供一种一种氮氧化硅-石英复合材料坩埚及其制备方法。本发明以氮氧化硅与石英的复合材料替代现行纯石英材料制作坩埚，并提出了相应的复合材料坩埚制造方法。由于氮氧化硅良好的高温稳定性、高温强度和与硅熔体之间良好的不润湿性，这种坩埚能够大幅度地降低单晶硅产品中氧含量，使用寿命也显著提高，同时也大幅度减少了内层合格高纯石英砂的需求。
本发明通过以下技术方案予以实现：
本发明第一方面提供氮氧化硅-石英复合材料坩埚，其根据坩埚埚壁的材料成分不同分为4类，具体为：
第一类，坩埚埚壁为氮氧化硅-石英均匀复合材料，该复合材料为整体均匀的材料；
第二类，坩埚埚壁为氮氧化硅-石英的梯度复合材料，该梯度复合材料的氮氧化硅含量从坩埚外壁向内壁梯度增加；
第三类，坩埚埚壁分为两层，外层为纯石英、里层为氮氧化硅-石英均匀复合材料该复合材料为整体均匀的材料；
第四类，坩埚埚壁分为两层，外层为纯石英、里层为氮氧化硅-石英的梯度复合材料，该梯度复合材料的氮氧化硅含量从坩埚外壁向内壁梯度增加。
本发明另一方面提供了上述氮氧化硅-石英复合材料坩埚的制备方法，以氮氧化硅与石英的复合材料作为坩埚的埚壁，先由石英砂与高纯氮化硅粉混合形成混合料，以混合料为原料采用旋转模具法-电弧熔制法制作坩埚，加热保温过程中混合料粉体中的氮化硅与部分石英砂在高温下反应形成氮氧化硅，坩埚的埚壁的组成为氮氧化硅与石英的复合材料。
当旋转布料时，设计混合料为石英砂与高纯氮化硅粉均匀混合的混合料，氮化硅粉重量百分比范围为3～60％，制得以氮氧化硅-石英均匀复合材料为埚壁的坩埚；
当旋转布料时，按梯度变化设计混合料成份，即沿坩埚壁厚度方向从外向内，从0到x逐渐增加氮化硅含量，X的范围为30～80％，制得以氮氧化硅-石英的梯度复合材料为埚壁的坩埚；
当旋转布料时，初始布以纯石英砂作为外层材料，继而布以石英砂与高纯氮化硅粉均匀混合料作为里层材料，所述混合料氮化硅含量范围为10～80％，制得埚壁外层为纯石英、里层为氮氧化硅-石英均匀复合材料的坩埚；
当旋转布料时，初始布以纯石英砂作为外层材料，继而布以梯度混合料作为里层材料，梯度混合料的成份按照沿坩埚壁厚度方向从外向内，从0到Y逐渐增加氮化硅含量，Y的范围为30～80％；形成埚壁外层为纯石英、里层为氮氧化硅-石英的梯度复合材料的坩埚；
旋转模具法-电弧熔制法是石英坩埚的常规制备工艺，该方法是利用离心力使原料堆积于旋转着的具有坩埚形状的模具的内表面，通过电弧放电热使堆积于旋转着的模具中的石英粉熔融、玻璃化，成形为坩埚形状。
优选地，常规的纯石英砂制备坩埚时熔制阶段(即加热保温)时间一般为15～30min，本发明电弧加热保温时间比采用纯石英砂的时间延长20～80％。
与现有技术相比，本发明具有以下有益效果：
1、本发明所制造的坩埚可广泛应用于光伏和半导体微电子领域用直拉单晶硅的生产，本发明制得的坩埚具有使用强度高、寿命长、抗硅熔体润湿性好、抗气泡迁移能力强等优点。
2、采用本发明坩埚直拉法制备单晶硅产品时，能够明显降低单晶硅产品中氧含量，制得的单晶硅品质高；
3、本发明可大幅度减少了高纯石英砂的需求。
具体实施方式
下面结合实施例，对本发明作进一步地说明。
实施例1
将符合单晶硅坩埚标准的石英砂与高纯氮化硅粉均匀混合，以该混合料代替石英砂以常规采用旋转模具法-电弧熔制法制作坩埚，加热保温过程中混合料粉体中的氮化硅与部分石英砂在高温下反应约30min形成氮氧化硅，最终所制得坩埚即为氮氧化硅与石英的均匀复合材料制成。
混合料中设置高纯氮化硅粉重量百分比范围为3～60％，本实施例中分别选取3％、10％、20％、30％、40％、50％、60％重量百分比的氮化硅粉。
实施例2
将石英砂与高纯氮化硅粉混合形成混合料，以混合料为原料采用旋转模具法-电弧熔制法制作坩埚，当旋转布料时，按梯度变化设计混合料成份，即沿坩埚壁厚度方向从外向内，从0到X逐渐增加氮化硅含量，加热保温过程中混合料粉体中的氮化硅与部分石英砂在高温下反应约40min形成氮氧化硅，最终所制得坩埚即为氮氧化硅与石英的梯度复合材料制成。
梯度混合料中设置X的范围为30～80％，本实施例中分别选取30％、40％、50％、60％、70％、80％重量百分比的氮化硅粉。
实施例3
石英砂与高纯氮化硅粉混合形成混合料，以混合料为原料采用旋转模具法-电弧熔制法制作坩埚，当旋转布料时，初始布以纯石英砂作为外层材料，继而布以均匀混合料作为里层材料；加热保温过程中混合料粉体中的氮化硅与部分石英砂在高温下反应约40min形成氮氧化硅，制得埚壁外层为纯石英、里层为氮氧化硅-石英均匀复合材料的坩埚。
均匀混合料中设置高纯氮化硅粉氮化硅含量范围为10～80％，本实施例中分别选取10％、20％、30％、40％、50％、60％、70％、80％重量百分比的氮化硅粉。
实施例4
以石英砂与高纯氮化硅粉混合形成混合料，以混合料为原料采用旋转模具法-电弧熔制法制作坩埚，当旋转布料时，初始布以纯石英砂作为外层材料，继而布以梯度混合料作为里层材料，梯度混合料的成份按照沿坩埚壁厚度方向从外向内，从0到Y逐渐增加氮化硅含量；加热保温过程中混合料粉体中的氮化硅与部分石英砂在高温下反应约45min形成氮氧化硅，坩埚的埚壁的组成为氮氧化硅与石英的复合材料。
梯度混合料中设置Y的范围为30～80％，本实施例中分别选取30％、40％、50％、60％、70％、80％重量百分比的氮化硅粉。
对比例1
与实施例1相同，区别在于，原料为纯石英砂，高温保温时间为20min。
应用实施例
以实施例1至4、对比例1分别制得的坩埚作为反应容器，在相同的工艺条件下采用常规的直拉法制备单晶硅，其中实施例1中混合料选择30％氮化硅粉，实施例2中X的范围选择50％，实施例3中混合料选择40％氮化硅粉，实施例4中Y的范围选择60％。各个实施例和对比例的坩埚制得的单晶硅性能分析见下表1。
表1
由表1可以看出，相比较纯石英制得的坩埚，采用本发明坩埚直拉法制备单晶硅产品时，能够大幅度地降低单晶硅产品中氧含量且增加使用寿命，其中以实施例4的效果最优。
以上所述仅表达了本发明的优选实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形、改进及替代，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (7)
1.一种氮氧化硅-石英复合材料坩埚的制备方法，其特征在于：所述制备方法以氮氧化硅与石英的复合材料作为坩埚的埚壁，先由石英砂与高纯氮化硅粉混合形成混合料，以混合料为原料采用旋转模具法-电弧熔制法制作坩埚，加热保温过程中混合料粉体中的氮化硅与部分石英砂在高温下反应形成氮氧化硅，坩埚的埚壁的组成为氮氧化硅与石英的复合材料。
2.根据权利要求1所述的一种氮氧化硅-石英复合材料坩埚的制备方法，其特征在于：所述混合料为石英砂与高纯氮化硅粉均匀混合的混合料，氮化硅粉重量百分比范围为3～60％，制得以氮氧化硅-石英均匀复合材料为埚壁的坩埚。
3.根据权利要求1所述的一种氮氧化硅-石英复合材料坩埚的制备方法，其特征在于：所述复合材料旋转布料时按梯度变化设计混合料成份，即沿坩埚壁厚度方向从外向内，从0到X逐渐增加氮化硅含量，X的范围为30～80％，制得以氮氧化硅-石英的梯度复合材料为埚壁的坩埚。
4.根据权利要求1所述的一种氮氧化硅-石英复合材料坩埚的制备方法，其特征在于：所述复合材料旋转布料时初始布以纯石英砂作为外层材料，继而布以均匀混合料作为里层材料，所述混合料氮化硅含量范围为10～80％，制得埚壁外层为纯石英、里层为氮氧化硅-石英均匀复合材料的坩埚。
5.根据权利要求1所述的一种氮氧化硅-石英复合材料坩埚的制备方法，其特征在于：所述复合材料旋转布料时初始布以纯石英砂作为外层材料，继而布以梯度混合料作为里层材料，梯度混合料的成份按照沿坩埚壁厚度方向从外向内，从0到Y逐渐增加氮化硅含量，X的范围为30～80％；形成埚壁外层为纯石英、里层为氮氧化硅-石英的梯度复合材料的坩埚。
6.权利要求1至5任意一项的一种氮氧化硅-石英复合材料坩埚的制备方法，其特征在于：所述旋转模具法-电弧熔制法中电弧加热保温时间比采用纯石英砂的时间延长20～80％。
7.权利要求1至6任意一项所述方法制备得到的一种氮氧化硅-石英复合材料坩埚。
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