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CN101278078B - 用于硅结晶的坩埚及其制造方法 - Google Patents

用于硅结晶的坩埚及其制造方法 Download PDF

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CN101278078B
CN101278078B CN2006800369429A CN200680036942A CN101278078B CN 101278078 B CN101278078 B CN 101278078B CN 2006800369429 A CN2006800369429 A CN 2006800369429A CN 200680036942 A CN200680036942 A CN 200680036942A CN 101278078 B CN101278078 B CN 101278078B
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crucible
silicon
silicon nitride
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G·兰库勒
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Vesuvius Crucible Co
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Abstract

本发明涉及用于硅结晶的坩埚，并涉及熔融材料处理中使用的坩埚的脱离涂层的制备和应用，所述熔融材料在坩埚中凝固并且然后以晶锭形式被移出，且更尤其涉及多晶硅凝固中使用的坩埚的脱离涂层。本发明人的目的是提供包含氮化硅涂层的坩埚，所述涂层可较快且较廉价地制备，并且较牢固，对壁具有改善的附着力。发现使用这样的用于硅结晶的坩埚可解决这些问题，所述坩埚包含：a)包含限定出内部容积的底表面和侧壁的基本体；b)保护涂层，该保护涂层包含80-95重量％氮化硅和5-20重量％低温无机粘结剂，总氧含量为5-15重量％。

Description

用于硅结晶的坩埚及其制造方法
本发明涉及用于硅结晶的坩埚，并涉及熔融材料处理中使用的坩埚的保护涂层的制备和应用，所述熔融材料在坩埚中凝固并然后以晶锭形式被移出，且更尤其涉及多晶硅凝固中使用的坩埚的保护涂层。
坩埚(例如由熔融石英、碳化硅、石英、氮化硅、反应结合氮化硅或石墨制成)典型地用于多晶硅的凝固。选择氧化硅的主要原因是它具有高的纯度和可获得性。然而在通过该方法使用氧化硅作为用于制备硅的坩埚中存在问题。
熔融状态的硅可同与其接触的氧化硅坩埚反应。熔融硅与氧化硅反应形成一氧化硅和氧。氧可污染硅。一氧化硅具有挥发性，并且可与炉内的石墨部件反应。一氧化硅与石墨反应形成碳化硅和一氧化碳。一氧化碳然后可与熔融硅反应形成另外的挥发性一氧化硅、碳化硅、金属痕量物质或添加剂的碳化物及氧化物、和碳。碳可污染硅。硅还可与包含在坩埚内和/或包含在氮化物涂层内的多种杂质(铁、硼、铝等等)反应。
氧化硅与硅之间的反应促进硅对坩埚的附着。这种附着与所述两种材料之间的热膨胀系数的差异相结合在硅锭中产生应力，导致其在冷却时开裂。在本领域中已知的是，施用在坩埚内侧与晶锭接触区域上的保护涂层可防止引起晶锭污染和开裂的硅与氧化硅之间的反应。为有效起见，该涂层必须足够厚以防止硅与氧化硅坩埚反应，并且必须不可通过其自身或其内的污染物有害地污染硅。
文献中描述了多种试图解决坩埚与熔融材料接触的反应和附着问题的材料和技术。
已知氮化硅涂层可防止熔融硅与来自坩埚的氧化硅之间的化学反应。美国专利No.4,741,925描述了一种通过化学气相沉积在1250℃下施涂的坩埚用氮化硅涂层，而WO-A1-2004/053207公开了通过等离子喷涂施涂的氮化硅涂层。美国专利No.4,218,418描述了通过快速加热在氧化硅坩埚内侧形成玻璃层以防止硅在熔化处理期间开裂的技术。
现有技术包括在硅的定向凝固中用于对坩埚进行施涂的粉状脱模剂的具体文献。另外，提及了使用化学气相沉积、溶剂蒸发、高温火焰处理和其它昂贵且复杂的手段来施涂坩埚涂层。提及了具体的粘结剂和溶剂。提及了粉末状涂层浆料的混合、喷涂或刷涂。
已知氮化硅涂层可防止熔融硅与来自坩埚的氧化硅之间的化学反应。
然而，氮化硅涂层自身可导致问题。防止硅与氧化硅坩埚反应所需的氮化硅涂层的厚度相当重要(约300μm)，因此使涂层操作昂贵且耗时。此外，这种氮化硅涂层机械上不牢固，并且可在使用期间或者甚至在使用之前脱落或剥落。因此推荐在使用之前的最后时刻施涂该涂层，即在最终用户设备处，从而将施涂这种厚涂层的负担留给最终用户。
将稳定的氮化物涂层提供到陶瓷坩埚上的已知技术包括(1)氮化物涂层在700℃-1450℃的高温下于受控煅烧周期下氧化和(2)向氮化物组合物中添加烧结/粘结(或粘着)辅助剂。添加剂可为金属或氧化物添加剂例如Al2O3、SiO2、AlN、Al、Si、微硅粉或细硅粉及其它。在共同未决申请EP04447105中描述了包含微硅粉的氮化硅涂层。氮化硅氧化成氧化硅提高了涂层中氧的量并且导致上述问题。另外，氧化程度和产生的氧的量不易于控制。
硅生产商的描述光电和半导体应用时化学和物理相互作用的大部分文献，突出了维持坩埚涂层中低氧含量的需要。对于高质量晶片生产推荐使用低氧的氮化硅涂层。美国专利No.6,165,425中特别描述了具有低氧含量的高纯度氮化硅粉末的应用。该文献描述了具有0.3重量％到至多5重量％的极低氧含量的氮化硅涂层。该涂层可包含增粘剂例如聚乙烯醇，并且在优选500℃-700℃的温度下于空气中干燥。在这些低干燥温度下，氮化硅不发生氧化，未在晶界上形成SiO2，并且保持氮化硅的充分有效性。然而，一些问题仍然存在。因为不存在涂层的氧化，该涂层保持粉状且在将液态硅装入坩埚时易于受损。
因此，希望提供不存在上述问题的坩埚，该坩埚包含较强的涂层(避免脱落和剥落)，该涂层具有改善的抗机械磨损性，可快速且廉价地制备，同时防止熔融硅与坩埚之间的化学反应并维持关于氧含量的附加要求。
现已发现使用这样的用于硅结晶的坩埚可解决这些问题，所述坩埚包含：a)包含限定出内部容积的底表面和侧壁的基体；b)在朝向内部容积的侧壁表面处的氮化硅基保护涂层，所述涂层包含80-95重量％的氮化硅和5-20重量％的低温无机粘结剂，总氧含量为5-15重量％。优选地，低温粘结剂是氧化硅基粘结剂。还可使用氧氮化硅(siliconoxinitride)粉末并优选使用氮化硅和氧氮化硅粉末的组合。氧氮化硅粉末通常占5-20重量％。氧氮化硅粉末可以是回收的氧氮化物或水活化氧氮化物。本发明的一个重要优点是，氮化硅粉末中的氧含量不再是关键，并且可考虑使用包含一定量氧的粉末例如回收粉末。氮化硅粉末的晶相可为α或β。
所谓低温粘结剂，是指该粘结剂在比使氮化硅氧化所需温度低的温度下产生粘合。优选在低于800℃或更优选低于500℃的温度下产生粘合。
所谓无机粘结剂，是指包含无机基体的粘结剂，该粘结剂的残留物通常产生无机形式和碳或者无碳。相反，所述有机粘结剂如CMC(羧甲基纤维素)、胶、表面活性剂产生仅为碳的残留物。粘结剂的高反应性部分地由无机基体产生。
氮化硅或氧氮化硅粉末的粒度测定通常是亚微型，颗粒尺寸≤1μm。然而，还可使用包含不同颗粒尺寸并特别包含2-50μm、优选2-5μm的较粗颗粒或晶粒的氮化物粉末的掺混物。对掺混物进行选择以便改善一种或多种特性。掺混物可改善悬浮体的稳定性和/或进一步提高涂层在坩埚上的附着力。如果在根据本发明的氮化物涂层之下和/或顶部上存在另一涂层，掺混物还可促进不同层之间的附着。其它涂层可例如为专利申请WO2005/106084和共同未决申请PCT/EP2006/006347中所描述的氧化硅基涂层。相对于亚微颗粒，较粗颗粒的量通常占20-50重量％。较粗氮化硅粉末较便宜，引入这种粉末还降低了涂层的成本。
根据应用，保护涂层可具有50μm-500μm、优选200-500μm的厚度。为避免任何污染，保护涂层必须具有非常高的纯度且具有超低的碳含量。
这种新技术是基于在涂层中使用有限量或控制量的氧。氧随低温无机粘结剂(溶胶凝胶、有机金属化合物、纳米颗粒、微絮凝物、非互溶溶液、微乳剂、氧化物)引入。在整个涂层中产生极低温度的粘合相，从而提高防护涂层的抗机械磨损性并同时保持氮化硅的所需性能。涂层的脱落或剥落风险大大降低。
对添加剂及量进行选择，以便获得5-15重量％和最优选8-12重量％的总氧含量。低于5％的总氧含量不提供足够的粘合相导致涂层的低机械抗性。在氧含量过高时，出现上述污染问题。
产生粘合的加热温度低于使氮化硅氧化所需的温度。该加热温度低于800℃且优选低于500℃。这样，通过添加确定量的低温无机粘结剂完全控制氧的量。不存在可改变氧含量的另外氧化反应。
粘合分散体中的氧与氮化硅氧化产生的氧不同。结合体系和氮化物粉末之间的低粘着力允许保持作为非润湿剂的氮化物的充分有效性。在晶粒周围产生化学粘合并且氮化硅晶粒在它们的外缘未被氧化成SiO2。由化学凝结而不是典型的氧化热反应产生的结合所需的低温致密化增强了这种作用。本发明的涂层通过良好控制的粘合体系使能够提高涂层的机械抗性并同时维持氮化硅晶粒的充分有效性。
因为根据本发明的涂层不存在脱落或剥落的问题，所以其可在到达终端用户设备之前制得。
本发明的另一目的是用于涂敷硅结晶用坩埚的组合物，该组合物包含80-95重量％的氮化硅和5-20重量％的低温无机粘结剂，总氧含量高于5重量％。可通过不同方法施涂该组合物。在优选方法中，将该组合物与液相混合形成用于施涂到坩埚上的悬浮体。
本发明的另一目的是用于制造包含根据本发明的保护涂层的坩埚的方法；该方法包括步骤：
a)提供包含限定出内部容积的底表面和侧壁的基本体，和
b)在朝向内部容积的侧壁表面处施涂保护涂层，所述涂层包含80-95重量％的氮化硅和5-20重量％的低温无机粘结剂，总氧含量高于5重量％。
通常，可用水或溶剂通过喷涂或刷涂、优选用水基体系通过喷涂来施涂表面层，所述水基体系包含适量的水以使全部组合物悬浮。
在根据本发明的方法的优选实施方案中，在施涂涂层的步骤之后接着是在适于煅烧掉涂层中存在的基本上所有的有机化合物和适于产生粘合的温度和持续时间下的加热步骤c)。在优选实施方案中，加热温度保持低于氮化硅的氧化温度。这样，保持涂层中的氧含量受到控制。氮化硅的氧化温度可取决于涂层组成而改变，但通常为约800℃。涂敷的坩埚的加热还可在用户现场进行。还有可能在发货至用户之前和在用户现场进行最终或进一步加热之前进行预加热。
现将参照附图对本发明进行说明，所述附图仅用于说明本发明并且不意欲限制其范围。图1显示根据本发明的坩埚的横截面。
在该图中，坩埚用参考数字1表示。其包含基本体2，该基本体2包含限定出用于硅结晶的内部容积的底表面21和侧壁22。该坩埚在朝向内部容积的侧壁22的表面处包含保护层3，该保护层3由80-95重量％的氮化硅、5-20重量％的低温无机粘结剂组成，总氧含量高于5重量％。
现将通过根据本发明的实施例和对比例对本发明进行说明。可以不同方式在基本体上施涂涂层。组成取决于选择的方法。
第一优选方法(活性层)包括步骤：
-将氮化硅粉末和优选自如硅氧烷、原硅酸四乙酯、四乙氧基硅烷、聚二甲基硅烷或其组合(如此的有机金属化合物为已知并且可在市场上获得)的基于硅化学的有机金属化合物混合；
-通过来自氯化铵、氨、硝酸溶液或任何其它适合该方法的活性液体类的活性液体将涂料喷涂到坩埚上；
-在低于500℃的温度下加热涂敷的坩埚，用于涂层的稳定化。
第二优选方法(粘结剂溶液)包括步骤：
-将氮化硅粉末和优选自硅油、硅氧烷、氯硅烷或其组合的氧化硅基粘结剂混合；
-用来自酸类的活性液体(盐酸、硝酸、硅酸、四氯化硅或用于该方法的任何其它合适的酸)喷涂涂层，作为对氨基有机金属化合物有关的碱水解的中和；
-在低于500℃的温度下加热涂敷的坩埚以除去反应液体。
在另一实施方案中，采用基于酸水解体系用的氨蒸气或溶液的反应进行喷涂步骤。
第三优选方法(饱和溶液和沉积)包括步骤：
-将氮化硅与适于形成悬浮体的氧化硅亚微颗粒(＜10-6)和/或纳米颗粒、优选胶体氧化硅混合；
-通过热反应、蒸气反应或者甚至化学直接反应在坩埚表面上沉积制备的混合物，所述化学直接反应使用适当的中和化学品产生酸碱、醇或pH反应；
-优选在使用之前，在低于500℃的温度下加热涂敷的坩埚。
在表1中显示了用于这三种方法的涂层组成的实施例。
                表1-保护涂层的组成
Figure S2006800369429D00061
PVA表示聚乙烯醇和PEG表示聚乙二醇。
TEOS表示原硅酸四乙酯
优选的实施例是胶体氧化硅基组合物，因为它们处理起来容易且安全。取决于使用的方法对组成进行选择，以获得目标氧含量和抗机械磨损性。
在下面的表中，使用POSITEST拉脱法附着力测试仪(PULL-OFFADHESION TESTER)(来自DEFELSKO Corp.公司)依据ASTM D4541测定了坩埚上各涂层的附着力。该测试仪通过测定分离前该涂层所能承受的最大受拉拉脱力来评价涂层的附着力。即，使用液压从基底上拉开规定测试直径的涂层所需的力。该力以压强表示(kPa)。
在表2中显示了坩埚的实施例和相关性能：
                   表2
  实施例   保护涂层   坩埚   表面涂层的附着力
  1   1b   氧化硅   良
  2   1b   石英   优
  3   3a   氧化硅   良
  4   3b   RBSN   优
  6*   C1   石英   差
  7*   C2   石英   差
6和7是对比例
RBSN表示“反应结合氮化硅”且是已知类型的坩埚。
6和7是对比例并且对应于美国专利No.6,165,425的实施例1和2。C1包含具有1.3％氧含量的氮化硅粉末并且无低温无机粘结剂。C2包含具有6％氧含量的氮化硅粉末并且无低温无机粘结剂。
关于实施例6，在将硅金属装入坩埚中时观察到涂层的损伤。关于实施例7，如同美国专利No.6,165,425中所说明的，观察到大量的材料损失。

Claims (16)

1.用于硅结晶的坩埚(1)，其包括
a)包含限定出内部容积的底表面(21)和侧壁(22)的基本体(2)；
b)朝向内部容积的氮化硅基保护涂层(3)；
其特征在于，所述保护涂层(3)包含80-95重量％氮化硅、5-20重量％低温无机粘结剂，总氧含量为5-15重量％，所述低温无机粘结剂是在比氮化硅氧化所需温度低的温度下产生粘合的无机粘结剂，所述无机粘结剂是指包含无机基体的粘结剂，该粘结剂的残留物产生无机形式，含碳或者无碳。
2.根据权利要求1的坩埚，其特征在于，总氧含量为8-12重量％。
3.根据权利要求1或2的坩埚，其特征在于，氮化硅保护涂层(3)具有50μm-500μm的厚度。
4.根据权利要求1或2的坩埚，其特征在于，氮化硅保护涂层(3)具有200-500μm的厚度。
5.根据权利要求1或2的坩埚，其特征在于，氮化硅保护涂层包含颗粒尺寸≤1μm的颗粒。
6.根据权利要求5的坩埚，其特征在于，氮化硅保护涂层还包含颗粒尺寸为2-50μm的较粗颗粒。
7.根据权利要求5的坩埚，其特征在于，氮化硅保护涂层还包含颗粒尺寸为2-5μm的较粗颗粒。
8.根据权利要求6的坩埚，其特征在于，所述较粗颗粒的量为20-50重量％。
9.根据权利要求7的坩埚，其特征在于，所述较粗颗粒的量为20-50重量％。
10.根据权利要求1或2的坩埚，其特征在于，所述低温无机粘结剂包含选自硅氧烷、原硅酸四乙酯、四乙氧基硅烷、聚二甲基硅烷或其组合的化合物。
11.根据权利要求1或2的坩埚，其特征在于，所述低温无机粘结剂包含选自硅油、硅氧烷、氯硅烷或其组合的化合物。
12.根据权利要求1或2的坩埚，其特征在于，所述低温无机粘结剂包含适于形成悬浮体的氧化硅亚微颗粒和/或纳米颗粒。
13.根据权利要求12的坩埚，其特征在于，所述低温无机粘结剂包含氧化硅胶体。
14.制备用于硅结晶的坩埚(1)的方法，该方法包括步骤：
a)提供包含限定出内部容积的底表面(21)和侧壁(22)的基本体(2)；和
b)在朝向内部容积的侧壁(22)的表面处，施涂包含80-95重量％的氮化硅和5-20重量％的低温无机粘结剂的保护涂层(3)，该保护涂层的总氧含量高于5重量％，所述低温无机粘结剂是在比氮化硅氧化所需温度低的温度下产生粘合的无机粘结剂，所述无机粘结剂是指包含无机基体的粘结剂，该粘结剂的残留物产生无机形式，含碳或者无碳。
15.根据权利要求14的方法，其特征在于，包括另外的步骤c)，步骤c)为在低于氮化硅的氧化温度的温度下加热涂敷的坩埚。
16.根据权利要求14或15的方法，其特征在于，步骤b)通过喷涂进行。
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