CN103298983B - 坩埚 - Google Patents

坩埚 Download PDF

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CN103298983B
CN103298983B CN201180058403.6A CN201180058403A CN103298983B CN 103298983 B CN103298983 B CN 103298983B CN 201180058403 A CN201180058403 A CN 201180058403A CN 103298983 B CN103298983 B CN 103298983B
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silicon
crucible
weight
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鲁内·罗利格海泰
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STEULER SOLAR GmbH
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Abstract

一种用于制造用于硅结晶化的坩埚的方法，包括以下步骤：制备固体和液体的浆料，所述固体由金属硅粉末、至多25％重量的SiC粉末、至多10％重量的SiN、至多0.5％重量的催化剂、至多1％重量的粘接剂组成；用浆料形成坩埚的生坯；在氮气可选地包括惰性气体的氛围中加热生坯，以使硅至少部分与氮化硅反应。

Description

坩埚
技术领域
本发明涉及一种用于制造用于硅锭生产的坩埚的方法和该坩埚。
背景技术
硅是一种具有各种工业用途的元素。
用途之一是在光伏应用中。对于光伏产业，需要超纯硅。
由于涉及气候变化和能源供应的考虑，光伏太阳能正在经历巨大的工业发展。要对传统能源具有竞争力，降低太阳能成本是至关重要的。
为了生产太阳能电池，使用多晶和单晶硅。硅(silicon)或硅(silicium，silicon的旧称)的结晶化通常通过在坩埚中结晶进行。该方法基于可以从熔化的硅缓慢冷却生产硅锭的效果。它是一种定向固化的方法。它生产硅锭，硅锭切割成较小的块，并进一步形成晶圆。
要保持硅的纯度，坩埚必须是高度惰性的，并允许在固化过程中控制温度梯度。因为坩埚直接接触模塑硅，它可能是一个污染源。坩埚应该是化学惰性的，并承受至多1500℃的高温相对长的时间。
典型的市售材料是由石英(SiO2)制成的坩埚。在冷却时的相变过程中，石英材料通常裂缝。因此，石英坩埚只使用一次。石英材料中的杂质可能扩散到晶圆材料中，从而降低太阳能电池的电性能。
已经尝试引入其它材料，特别是氮化硅(Si3N4)作为用于坩埚的材料。
WO2007/148986描述由所谓的“氮化物粘接的氮化硅”制成的坩埚。根据该文献，从超过60％重量的硅硝酸盐颗粒和小于40％重量的硅颗粒的浆料形成的材料形成坩埚并在氮气的氛围中加热。
WO2004/016835公开了一种用于通过干压硅颗粒以及然后转化成氮化硅生产坩埚的方法。
除了这些尝试，生产氮化硅的坩埚，其可重复使用并允许生产高品质硅锭，尚未取得成功。
发明内容
本发明的目的是提供坩埚，其至少克服现有技术的一些缺点，特别是可重复使用的坩埚和/或允许生产具有改进性能的硅锭的坩埚的生产。
该目的通过本发明的方法解决。本发明的方法是一种用于制造坩埚的方法，包括以下步骤：
制备固体和液体的浆料，所述固体由金属硅粉末、至多25％重量的SiC粉末、至多10％重量的SiN、至多0.5％重量的催化剂、至多1％重量的粘接剂组成；
用浆料形成坩埚的生坯；
在氮气可选地包括惰性气体的氛围中加热生坯，以使硅至少部分与氮化硅反应。
根据本发明，在第一步骤中制备浆料。该浆料包括固体和液体。从该材料中的固体，至少60％重量是金属硅粉末(颗粒)。从固体和液体的混合物，固体可以通过在开放设置中在正常压力下加热至250℃的温度24小时进行回收。从这些这样获得的固体，至少60％重量是金属硅粉末。根据本发明的金属硅粉末是具有金属光泽的银灰色或暗灰色粉末。它可以从许多公司以不同的粒径购买到。根据本发明的粉末是具有至多500微米粒径的材料。
在一些具体实施例中，使用小于100微米或小于45微米的粒径是有用的。另外，也可以一起使用不同粒径的硅粉末或其他成分。
根据本发明，金属硅粉末与液体相结合。一种优选的液体是水，但也可以使用有机溶剂或有机溶剂与水的混合物。
颗粒通常在粒径范围内提供，例如0至100微米，或0至45微米。在这些情况下，颗粒分别具有100微米或更小的粒径，或45微米或更小的粒径。
在一个具体实施例中，粒径基于中值粒径进行确定。在这种情况下，根据ISO9276-5分析粒径分布。
质量中值粒径将颗粒划分为两半：颗粒的质量的50％较大，颗粒的质量的50％较小。这也被命名为d50。
在这种情况下，平均质量粒径直径应该优选在15和75微米之间。
在另一具体实施例中，使用具有最高发生率的粒径范围以描述粒径分布的特征。这也被命名为“峰”。15至75微米的峰粒径是优选的。
通过混合至少两种不同的粒径分布，整体的粒径分布变成至少是双峰的。这是尤其优选的。在一个双峰的混合物中，具有两个粒径，以比邻近的粒径更高的频率出现。
在一些具体实施例中，形成生坯的浆料包括另外的SiC粉末。如果SiC粉体存在，它以固体的至少1％，优选至少5％重量的量存在。在一些具体实施例中，SiC粉末的量是至多固体的10％或20％或25％重量。
SiC的存在进一步提高热传导性。
在一些具体实施例中，混合物还包括催化剂。已经发现约至多0.5％重量的固体的量是足够的。优选的催化剂是FeO。
在其它具体实施例中，材料包括粘接剂。粘接剂可以帮助稳定生坯。混合物的1.0％重量的粘接剂的量通常是足够的。合适的粘接剂是例如水性聚合物分散体。
在烧制的早期阶段任何有机材料从材料中燃烧掉，不存在在最终的坩埚中。
用于形成生坯的材料还包括氮化硅是可能的。没有使用氮化硅用于生坯的生产是优选的。氮化硅的量在固体材料中应该不超过固体材料的10％重量，优选不超过5％，甚至更优选不超过1％。
为了混合材料，使用球磨机是可能的。可以使用氮化硅球作为研磨介质。
这种材料使用用于形成用于硅的结晶的坩埚的生坯。坩埚是一个容器，该容器能够承受高温(1000℃以上)。它具有带大开口的杯形。它可以具有许多不同的形状，包括圆形，矩形等。形成生坯的具体实施例是灌浆成型、压铸、冻铸、凝胶注模成型等。
这里所用的“生坯”是从浆料制备的成型物件。它包括固体、液体和可选地有机材料，且是可延展的。
在一个具体实施例中，通过使用模具将浆料形成坩埚。具有坩埚的外部比例的模具用本发明的材料填充，内表面通过将柱塞压入材料中形成。
在其它具体实施例中，通过生产扁平元件形成坩埚的部件是可能的。这些元件可以形成或切成形状。这允许一些元件结合成坩埚的壁和底部。为了保证坩埚的气密性，用来自浆料的其它材料填补这样组装的生坯的边缘是可能的。
在一个优选的具有实施例中，允许成形后在室温下干燥浆料一段短的时间。这稳定了生坯。在接下来的步骤中，将生坯在氮气的氛围中加热。加热可以例如在窑中进行。窑的温度缓慢上升。加热在含有氮可选地与惰性气体一起的氛围中进行。典型的惰性气体是氩气或氦气。当窑的温度达到约1000℃时，开始硅金属转化为氮化硅。根据窑的类型，这可以通过在窑中的压力降而观察到。
在优选的具体实施例中，加热步骤的温度至少提高至约1050℃，优选高于1250℃，更优选高于1400℃。
根据坩埚壁的厚度，金属硅至硅硝酸盐的转化需要足够的时间。通常情况下，转化在数天之内进行。
在优选的具体实施例中，加热在1000℃以上的温度进行至少3天的时间。通常情况下，在1000℃以上的温度至多10天的加热是足够的。因为硅至氮化硅的转化是放热的，控制氮气的温度和压力以避免过度加热产品可能导致硅的熔开是重要的。
为了实现至氮化硅的转化，在加热步骤期间保持氮气氛围是重要的。通常情况下，包括氮和可选地惰性气体的氛围的压力在200和1400毫巴之间。优选地，在加热步骤期间氮分压至少为100毫巴。
令人惊讶的，由本发明的方法得到的坩埚具有优越的性能。与其他坩埚相比，它具有在14至25％的范围内的非常低的孔隙率(根据ASTMC-20测量作为表观孔隙率)。这清楚地区别于WO2004/016835，其公开了40至60％的孔隙率。
它还具有在2.3至2.6公斤/升的范围内的高密度，这是高于现有技术的氮化硅坩埚的。优选地，密度为2.4公斤/升或以上，2.45公斤/升或以上，或2.5公斤/升或以上。
WO2004/016835A1公开了坩埚，其具有只有1.85公斤/升的密度。
已经看到，使用本发明的坩埚，有可能生产优质的锭。材料的抗热震性可以按照下列公式计算估计
Rs＝(λ*σf)/(a*E)
其中
Rs＝抗热震性
λ＝热传导率
σf＝抗弯强度
a＝热膨胀系数
E＝弹性模量
因为坩埚具有较高的抗弯强度和较高的热传导率，本发明的坩埚具有改善的寿命，并且可以重新使用多次。
本发明的另一个具体实施例是一种用于制造坩埚的方法，包括以下步骤：
制备固体和液体的浆料，其中固体的至少60％重量是金属硅粉末；
用浆料形成坩埚的生坯；
在氮气可选地包括惰性气体的氛围中加热生坯，以使硅至少部分与氮化硅反应。
根据本发明，最终产品不包括有机材料，基本上没有无机含氧材料，也就是说，它没有如二氧化硅、氧化铝等成分。氧可能存在于浆料中来自液体或有机材料如粘接剂。在坩埚中，没有或只有极少量(<0.5％重量)的含氧无机化合物存在。
具体实施方式
通过下列非限制性例子更详细地说明本发明。
实例1
混合物由具有小于10微米粒径和小于45微米粒径的硅粉末(重量比1:1)和固体的约25％重量的水一起以及水性聚合物分散体粘接剂制备。
扁平元件从混合物形成，并允许在室温干燥约24小时。必要的尺寸由高压水柱裁剪机切割以形成用于坩埚的侧壁和底部的元件。元件通过使用例子的料浆固定在一起。生坯加热至约600℃进行6小时，然后将温度缓慢升至约1050℃，直至窑内的压力下降。在烧制过程中使用约500毫巴的氮气氛围。在接下来的4天里，在进一步的加热过程中温度缓慢升高至1250℃，最后，至多1400℃。然后将坩埚保持在1400℃的温度共剩下的24小时。在这段时间内，氮分压可以慢慢地增加以达到控制的反应速率。
实例2
小于45微米粒径的金属硅粉末和小于100微米粒径及小于10微米粒径的20％重量的SiC粉末(重量比1:3)混合。加入25％固体重量的水，并将该混合物填充到模具中，模具是坩埚的外表面。内表面通过按压柱塞进入材料形成。在室温下干燥30分钟后，生坯可以从模具和柱塞移走，然后根据实例1的条件烧制。

Claims (19)

1.一种用于制造用于硅结晶化的坩埚的方法，其特征在于，包括以下步骤：
制备固体和液体的浆料，所述固体由金属硅粉末、至多25％重量的SiC粉末、至多10％重量的Si3N4、至多0.5％重量的催化剂、至多1％重量的粘接剂组成；
用浆料形成坩埚的生坯；
在氮气可选地包括惰性气体的氛围中加热生坯，以使硅至少部分反应生成氮化硅。
2.根据权利要求1所述的方法，其特征在于，金属硅粉末的粒径在0至100微米的范围内。
3.根据权利要求2所述的方法，其特征在于，金属硅粉末的粒径在0至45微米的范围内。
4.根据权利要求1或2所述的方法，其特征在于，至少75％重量的固体是金属硅粉末。
5.根据权利要求1或2所述的方法，其特征在于，固体包括至多15％重量的SiC粉末。
6.根据权利要求1或2所述的方法，其特征在于，催化剂是FeO和/或粘接剂是水性聚合物分散体。
7.根据权利要求1或2所述的方法，其特征在于，惰性气体选自氩气、氦气和它们的混合物。
8.根据权利要求1或2所述的方法，其特征在于，氮气可选地包括惰性气体的氛围的压力在200至1400毫巴之间。
9.根据权利要求1或2所述的方法，其特征在于，加热在1050℃以上。
10.根据权利要求9所述的方法，其特征在于，加热在高于1250℃的温度进行。
11.根据权利要求9所述的方法，其特征在于，加热在高于1400℃的温度进行。
12.根据权利要求1或2所述的方法，其特征在于，加热在高于1000℃的温度进行3至14天。
13.根据权利要求1或2所述的方法，其特征在于，金属硅粉末是在双峰或多峰的粒径分布中。
14.一种根据权利要求1至3任一所述的方法得到的坩埚。
15.根据权利要求14所述的坩埚，其特征在于，所述坩埚具有根据ASTMC-20测得的14至25％的表观孔隙率。
16.根据权利要求14或15所述的坩埚，其特征在于，所述坩埚具有2.3至2.6kg/dm3的密度。
17.根据权利要求14或15所述的坩埚用于硅的结晶化的应用。
18.根据权利要求17所述的应用，其特征在于，所述硅是单晶的。
19.根据权利要求17所述的应用，其特征在于，所述硅是多晶的。
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