CN1220547C - 氢焰炬 - Google Patents

氢焰炬 Download PDF

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CN1220547C
CN1220547C CNB951940201A CN95194020A CN1220547C CN 1220547 C CN1220547 C CN 1220547C CN B951940201 A CNB951940201 A CN B951940201A CN 95194020 A CN95194020 A CN 95194020A CN 1220547 C CN1220547 C CN 1220547C
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millimeters
carborundum
millimeter
mould
wall thickness
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CN1152262A (zh
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B·D·福斯特
W·J·埃里奥特
J·T·斐达
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Saint Gobain Ceramics and Plastics Inc
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Abstract

一种将两种反应流体混合起来的流体输送系统，它包括内部流体输送管和外部流体输送管，其中：a)外管由第一种材料构成，以及b)内管由第二种材料构成。

Description

氢焰炬
发明领域
本发明涉及一种半导体器件制造业中使用的氢焰炬，具体而言，涉及一种用来在硅基片表面形成二氧化硅层的氢焰炬。
背景技术
在半导体器件制造工业中，经常必须使硅基片的表面氧化从而在表面形成二氧化硅层。通常的一种处理方法是将基片放置于加热的无沾污容器(称为工艺管)内并将高纯度的水蒸气注入工艺管。纯净的水蒸气与基片表面接触和反应从而形成所需的二氧化硅层。
纯净的水蒸气一般由安装在工艺管内部或者外部的氢焰炬系统产生。图1和2表示带有氢气入口A和出口B以及氧气入口C和出口D的已有技术整体式焰炬。该系统沿不同的气路将氢气和氧气充入工艺管(或者外部燃烧室)，管内气体在600℃以上的高温下混合。高温混合气体产生了可燃烧，燃烧温度最高可达1200℃从而形成水蒸气。
有些普通的氢焰炬是复杂的整体式石英管。但是，氢气输送管出口处的温度常常达到1200℃以上。这样高的温度再加上燃烧室内的蒸气气氛会引起一般石英输送管的解体，一开始是释放二氧化硅微粒(这会造成半导体制造工艺中的沾污)而最终会使管体的尺寸发生变化、结构遭到破坏(从而影响了氢气的正常输送)。
已经研制出另外一类氢焰炬，它们能在以上极端环境下使用。特别是已经出现的商用碳化硅焰炬，它可以经受水蒸气腐蚀性环境和高温。但是与石英相比，碳化硅要加工成复杂的形状更加困难，从而使造价更为昂贵。
因此，需要一种价格合理并且加工简便而又能在极端环境下使用的氢焰炬。
发明内容
按照本发明，提供了一种将两种反应流体混合起来的流体输送系统，它包括内部流体输送管和外部流体输送管，其中；
a)外管由第一种材料构成，以及
b)内管由第二种材料构成。
在较佳实施例中，第一种和第二种材料分别用熔融石英和碳化硅，并且两者通过逆向球形接头连接起来。
附图的简要说明
图1为一般用于整体式石英管的已有技术氢焰炬的样式；
图2为另一种一般用于整体式石英管的已有技术氢焰炬的样式；
图3表示本发明氢焰炬的一个实施例；
图4表示与工艺管相连的本发明的氢焰炬；
图5表示逆向球形接头的一个实施例。
实施发明的较佳方式
本发明的焰炬对系统中耐高温性能要求较高的区域用耐热材料(例如碳化硅)，而对加工要求较高的区域石英。因此，与整体式碳化硅焰炬相比，加工比较容易(因而也比较便宜)而与石英整体式焰炬相比更为耐用，从而克服两者的缺点。
组成内管的第二种材料至少应能经受1200℃下含水蒸气的环境而在性能上无明显的退化。该材料应是气密性的并且主要由浸渍硅的高纯碳化硅、涂覆有CVD碳化硅的高纯碳化硅或者整体式CVD碳化硅组成。比较好的碳化硅是CRYSTAR(TM)牌碳化硅，这可以从位于Worcester，MA的Norton公司购得。
也可以考虑用其它的耐热陶瓷材料(例如氮化硅和氮氧化硅)做成整个内管或者作为内管涂层。在有些实施例中，内管由陶瓷基体材料和基体材料上的涂层组成，其中涂层与陶瓷基体材料相比，纯度更高或者耐高温性能更佳。
构成外管的第一种材料可以是任何易于成形的高纯度石英，并且能够经受至少600℃下含水蒸气的环境而在性能上无明显的下降。比较好的第一材料是玻璃。更好的是熔融石英。
在由图3表示的一个较佳实施例中，焰炬包括一根碳化硅管1和两根石英管2和3。利用双面球形接头4将这些管道连接在一起，该接头将碳化硅管1固定在相对于石英管2和3的合适位置上并将流过系统的不同气体隔绝开来。球形接头4包括固定在两个相对的内石英插座6和7(它们与碳化硅管2和3连为一体)之间的碳化硅球形部分5(与碳化硅管1连为一体)。第一石英管2带有一个容纳氧气气流经过的入口14，该石英管留出了足够的空隙使碳化硅管1通过，而氧气可以流过由第一石英管2的内径和碳化硅管2的外径限定的环形空间。在第一石英管2的相对一端是另一个可以与将要进行所需燃烧的工艺管(未画出)连接起来的内插座。第二石英管3带有一个容纳氢气气流通过的入口12。在有些实施例中，还在焰炬内部安装了热电偶13。
现在参见图4，碳化硅管1的长度能使其穿过第一石英管2并进入工艺管11，从而使得从碳化硅管1尖端9出来的氢气位于工艺管11内合适的位置上。为了方便安装，碳化硅管1的外径和尖端9应能穿过第一石英管2。尖端9可以采用各种通用的结构来控制和引导出来的氢气气流。
由于引向球形接头的石英管尺寸较小且气体是在室温下流经球形接头4的两侧，所以球形接头4上碳化硅球的温度一般低于300℃。
在有些实施例中，碳化硅管1的外径为13毫米，内径为8毫米而长度为300毫米；石英管2和3的外径为20毫米，内径为15毫米而长度为50毫米；并且球形接头4为28/15，即内径公隙为15毫米而直径为28毫米的球形。
本发明中的连接端(例如图3中的部件5、6、7、8、12和14)可以设计成在半导体制造工业中普遍使用的连接样式。例如接头可以是球形的、插座型的、圆锥形或者法兰型的，并且可以采用通常的方法制造。比较好的是球形接头与标准的金属夹固定在一起。虽然图3和4中的SiC球和石英插座之间看上去有空隙，但应理解为，这些接头是精确配合的，因而不会有流体流出接头。如果需要，可以采用O形圈来加强球形接头的密封。
图3和4揭示了一种将不同材料的SiC管1和石英管2连接起来的新型装置(称为“逆向球形接头”)。因此，按照本发明，还提供了一种用于多种流体输送系统的逆向球形接头。现在参见图5，该逆向球形接头包括：
a)第一部件50，它包括：
i)带有第一端口53的第一管51，和
ii)由第一端口53朝外开口的第一空心半球凸起52，以及
b)第二部件54，它包括：
i)具有第一端口56的第二管55，
ii)由第二管55的第一端口56向外开口的第二空心半球凸起58，以及
iii)与第二管55流通的第三管57，
所述第二管55的直径大于第一管52并基本上与其同心，第一管52装配在第二管55内从而使第一凸起55的凸面与第二凸起58的凹面形成合适的密封配合。
与普通的球形接头相反，本发明的逆向球形接头在两根管道之间限定出一适合于第二流体在其中流动而与内管中流体隔绝开来的环形空间。
任何普通的方法都适合于本发明的石英和碳化硅部件的加工。例如，美国专利No.3,951,587中揭示的石膏模型内双峰碳化硅注浆法(“Alliegro工艺”)可以用来制造硅化碳化硅管。但是当所需的SiC管较小时(即直径小于20毫米和/或壁厚小于3毫米)，实践证明应采用新技术以确保加工质量。
特别的是，现在有一种适合于本发明的脱水浇注重结晶碳化硅陶瓷的方法，其壁厚在0.75-3毫米之间，在室温下4点挠曲强度至少为250MPa，比较好的至少为290MPa。更好的是该陶瓷在1200℃下的4点挠曲强度至少为290MPa，而最好的情况是至少为375MPa。在一些较佳实施例中，这种新型陶瓷的制造工艺包括以下的步骤：
a)制作石膏模具
b)在模具上涂覆浇注阻滞剂，
c)在涂覆过的模具内填充呈双峰粒度分布的碳化硅注浆，
d)使模具内的注浆脱水以形成厚度在0.75-3毫米左右的浇注件。
就本发明的用途而言，“脱水浇注”SiC陶瓷包括通过脱水浇注、注浆成型或者压力浇注方法制造的产品，这些产品的表面较为光滑并且具有各向同性的颗粒取向。因此，“脱水浇注”产品不包括沿挤压表面带有条纹并且颗粒具有选择性取向的注模SiC陶瓷。同样，“重结晶”SiC陶瓷基本上都为非游离碳并且不含碳质生坯与硅反应烧结后的SiC陶瓷，所以也就不含未反应的游离碳或硅。
当在注浆引入之前于石膏模具上涂覆一层藻酸铵涂层时，意外发现获得了强度合适的薄壁注件。在本领域内，对于浇注所关心的主要问题是如何实现高密度浇注。典型的是采用双峰注浆来实现高密度浇注(即理论密度为85％左右)，其中精细颗粒(典型的粒径为2-3微米)填充在由粗糙颗粒(典型的粒径为50微米左右)堆积形成的空隙内。但是，熟石膏模经常会呈现多孔状(即含有直径为2-3微米的孔隙)。因此，如果不拘泥于理论上的限制，据信多孔石膏的高密度将通过下列两种方式对这种双峰注浆产生不利的影响。首先，因注浆与多孔石膏之间的作用产生的毛细管张力将诱发过快的浇注速率(即在0.5分钟内完成壁厚1毫米注件的浇注)。过快的浇注速率影响了双模态注浆在浇注前锋处的正确排列，因而在注件厚度方向上产生不均匀的微结构。其次，由于一开始较快的浇注速率，SiC精细颗粒被抽吸至注浆-石膏界面处，从而形成以精细粒度级为主的浇注表面。第二种现象据信是在现有注件技术中出现橘皮剥离的原因。
如果不拘泥于理论上的限制，据信当浇注阻滞剂涂覆在多孔密度较高的石膏模具表面时，可以降低有效孔隙率和渗透率，从而减慢了浇注速率，有利于产生排序度高的注件并提高了注件密度。它还阻滞了精细颗粒渗入模具，使其滞留在注件内，从而获得光滑的成品，并且很容易与模具脱离。
浇注阻滞剂可以任何一种降低多孔石膏孔隙率的涂层。比较好的是氨水或藻酸钠以及聚丙烯酸。更好的是藻酸铵。典型的是涂覆一层浓度在0.01与1.0w/o之间的水溶液，比较好的是在0.03w/o左右。
本发明的石膏模具可以是任何在浇注技术中使用的模具。比较好的是熟石膏并且通道(孔隙)的大小为2微米左右。比较好的是它具有60％的稠度。
本发明中涉及的注浆一般为双峰分布，其中包含浓度介于45-55w/o之间而粒径范围为10-100微米的粗糙SiC颗粒(“粗糙粒度级”)和浓度介于45-55w/o之间而粒径范围为1-4微米的精细SiC颗粒(“精细粒度级”)。比较好的是精细粒度级的平均粒径为2-3微米左右而粗糙粒度级的平均粒径为60微米左右。
注浆的其它成份包括诸如散凝剂之类的普通添加剂(例如NaOH、NH3OH和Na2SiO3)；12-16w/o左右的水；以及0.25-1.0w/o左右的丙烯酸胶乳粘结剂固态物。
在一个特别好的实施例中，制备了由48w/o左右平均粒径为60微米的F240尺度未烧结碳化硅和52w/o左右平均粒径为2-3微米的未烧结碳化硅组成的碳化硅混合物。向该混合物加入足够数量的散凝剂(NaOH)以达到优化的散凝作用。随后加水以获得500-750左右的粘滞度。还加入了约为0.25w/o的丙烯酸胶乳粘结剂固态物。这些成份在真空度为27-30英寸汞柱的球形研磨机中混合并辊压至少17个小时。
与此同时，在稠度为70％的石膏模具上涂覆一层0.03％的藻铵酸溶液。模具被揭去底盖并将海藻酸溶液灌入腔体。溶液随着模具的吸收而不断加入。当海藻酸溶液充满模具3分钟后，其盖子被揭去并抽干溶液。
被抽干的模具在引入注浆之前可以在空气中干燥10分钟。模具随后再次被揭去底盖并将注浆灌入腔体。浇注时间取决于所需的壁厚和注浆的粘度。如果所需的粘度为750cps而标称壁厚为1.5毫米，则在去掉底盖之前注浆可以在模具内保存4-6分钟。
当注浆被从模具内抽干之后，将少量去离子水注入腔体以确保抽干的表面没有疙瘩。浇注部分可以在模具内干燥20-30分钟。随后拆开模具并利用脱模夹具移走焰炬。该夹具的形状与浇注部件的外形相仿，从而可以使其在干燥时形状大小保持不变。
在制成生坯之前浇注部件可以在空气中干燥一个晚上或者在炉子内54℃下至少干燥2小时。随后从浇注部件上去除干化的海藻酸表层并将浇注部件切割成一定的长度，这样就完成了最终的成品。
现在将浇注部件进行烧结。开始步骤是在真空度为0.5torr的Ar气氛下将加热炉加热至1950℃。初烧完毕根据部件的大小和用途可采取两种不同的最终烧结步骤。第二次烧结步骤分别为将浇注部件浸入硅中以消除孔隙或采用CVD方法涂覆碳化硅。第二次烧结完毕部件被加工成最终的形状。
按照本发明，可以获得外径在4-20毫米之间(比较好的是6毫米)而壁厚在0.75-3.0毫米之间(比较好的是1毫米)的碳化硅陶瓷。由于浇注的速度足够得慢，所以有利于有序化浇注，从而避免出现粗糙的“橘皮剥离”型抽干浇注表面并获得了表面光滑的注件。
按照上述较佳实施例制造的未烧结注件的体密度至少为2.75g/cc左右而四点弯曲强度至少为7MPa左右。其孔隙大小介于0.1-4.0微米。其平均尺寸为0.4微米。与此相反，普通的未烧结浇注SiC体的平均孔隙大小为1.8微米。
对于按照本发明较佳实施例制造的硅化碳化硅产品的物理和机械特性进行了分析。在4点四分点卡具上进行了挠曲强度测试，其中上跨度为20毫米而下跨度为40毫米。尺寸为3毫米×4毫米×50毫米的挠曲试验条在0.02英寸/分钟的加载速率下弯曲。测得的室温下挠曲强度为296MPa左右。与普通硅化碳化硅产品相比，其强度提高了38％。测得的1200℃下挠曲强度为375MPa，与普通硅化碳化硅产品相比，其强度提高了60％。此外还测量了壁厚的变化。测得的本发明壁厚为1毫米时的壁厚变化为0.2毫米/米，即在1米长度范围内厚度从0.9毫米变化至1.1毫米(从顶端至底部)。与此相反，普通硅化碳化硅陶瓷的壁厚变化约为0.6毫米/米。
本发明的新型重结晶碳化硅陶瓷可以用于普通硅化碳化硅或者CVD涂层碳化硅的应用场合，包括美国专利No.3,951,587中所揭示的那些应用。

Claims (3)

1.一种脱水浇注碳化硅陶瓷管，其特征在于，所述陶瓷管的外径在4毫米-20毫米之间，所述陶瓷管的壁厚在0.75毫米-3毫米之间，壁厚为1毫米时的壁厚变化为0.2毫米/米，并且所述陶瓷的室温下挠曲强度至少为250MPa。
2.如权利要求1所述的陶瓷管，其特征在于，所述陶瓷呈双峰SiC颗粒分布，所述分布包括平均粒径为2微米到3微米之间的精细粒度级和平均粒径在60微米左右的粗糙粒度级。
3.如权利要求1所述的陶瓷管，其特征在于，碳化硅基本上由重结晶碳化硅组成。
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