CN101374784B - 用于制备耐火衬里的模制浆料 - Google Patents

用于制备耐火衬里的模制浆料 Download PDF

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CN101374784B
CN101374784B CN2006800434625A CN200680043462A CN101374784B CN 101374784 B CN101374784 B CN 101374784B CN 2006800434625 A CN2006800434625 A CN 2006800434625A CN 200680043462 A CN200680043462 A CN 200680043462A CN 101374784 B CN101374784 B CN 101374784B
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霍尔格·格罗特
玛格丽特·赫茨
马克·特蒂尔特
沃尔夫冈·科伦博格
克里斯丁·雷希
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Abstract

本发明公开一种用于生产耐火衬里，特别是固定的燃气轮机的燃烧室用的耐火衬里的模制浆料，其特征在于，模制浆料由大于约50％碳化硅重量份(8)和小于约50％重量份的硅酸铝(12)构成。

Description

用于制备耐火衬里的模制浆料
本发明涉及一种用于制备一种耐火衬里，尤其是用于制备一种固定的燃气轮机的衬里的模制浆料。本发明还涉及一种在这种模制浆料的基础上制造的、经煅烧的模制件，以及一种附属的耐火衬里以及最后也涉及一种用于制造耐火衬里的、经煅烧的模制件的方法。 
在燃烧室技术领域，如诸如在燃气轮机-燃烧室中，高温反应器的壁必须用合适的内衬或热屏保护，因此尤其是相对热燃气侵蚀保护位于其背后的支撑的结构。陶瓷材料通常比金属材料更适合作为热屏，因为其耐热并耐腐蚀，并且具有较低的导热能力。 
陶瓷内衬，通常也称为陶瓷隔热板，通常是通过烧结方法制造，这时也确定了陶瓷的保护特性。 
对陶瓷隔热板还提出了关于其机械负载能力更高的要求，并在此试图通过制造复合构件改进加强，例如，基于CMC(陶瓷基体复合物)用纤维增强的构件，或者具有结构陶瓷-构件或加强的(gradierten)构件，以达到特别良好的机械特性。 
从现有技术中，如从DE 4242610A1、WO 94/03410和“Pocket ManualRefractory Materials”(G.Routschka，1997，Vulkan-Verlag Essen)中，已知使用了基于碳化硅和硅酸铝的耐火模制浆料。 
本发明所要解决的技术问题是提供一种模制浆料以及由此煅烧的、用于开头所述类型的耐火衬里的模制件，该模制浆料可在相对低的烧结温度下加工，并因此在耐高温的复合构件的开发中开辟了新的可能性。 
模制浆料必需满足用于固定的燃气轮机的热燃气通道或燃烧室的陶瓷构件的要求。 
按照本发明，该技术问题通过一种用于制造耐火内衬的模制浆料解决，其由大于约50％重量份的碳化硅、小于50％重量份的硅酸铝和小于约10％重量份的胶质硅酸溶液构成。该技术问题进一步通过一种用于耐火内衬的、经煅烧的模制件解决，其具有大于约70％重量份并少于约90％重量份的碳化硅、大于约10％重量份和小于约50％重量份的硅酸铝和小于约10％重量份的胶质硅酸溶液。此外，该技术问题按本发明还通过一种用于制造耐火内衬的经煅烧的模制件的方法解决，该方法包括以下步骤：用至少碳化硅、 微石英、氧化铝和硅酸铝成分加入胶质硅酸溶液制成模制浆料；在振荡的情况下浇注模制浆料，急剧降低模制浆料的温度，以及干燥和煅烧浇注的模制件。 
按照本发明由上述确定的碳化硅和氧化铝或硅酸铝的重量份共同组成的模制浆料形成一种基料，其特别有利地通过在所谓的溶胶-凝胶-步骤中加入胶质硅酸溶液固化，并且可进一步在振荡的情况下借助于浇注进行加工。在此，其首先以溶胶或胶体溶液存在的硅酸通过所述温度的急剧下降转变成凝胶，并因而固化模制浆料，其也可称为浇注料或振动料。如下面更详细的解释，本来的干燥步骤和烧结步骤接着可以在较低的煅烧温度下进行。 
在一个优选的实施方案中，在本发明的模制材料中使用的重量份为约70％至约90％的碳化硅，其化学式为SiC。 
特别有利的是在本发明模制浆料中使用氧化铝刚玉，即呈三角形结构的氧化铝，其化学式为Al2O3，尤其使用的重量份为约5％至约20％。 
使用的硅酸铝的重量份特别有利的在约5％至30％间，最优选少于约25％。在此，这种硅酸铝有利的是化学式为3Al2O3-2SiO2或2Al2O3-1SiO2的莫来石。 
如果所存在的模制浆料中有5％至30％间重量份的微硅粉(SiO2)，可以制造特别有利的模制件。 
此外，按本发明的模制件有利的是没有不结合的氧化硅，SiO2或者这种硅的氧化物重量份至少小于约10％。最后如果在模制件中没有铝酸钙也是有利的。 
按本发明添加的胶质硅酸溶液的重量份有利地小于约10％。另外胶质硅酸溶液的固体含量应具有至少约30％重量份。 
为了达到优良的可加工性，模制浆料优先应加入一种液体，尤其是水，其加入量为大于约1％重量份并小于10％重量份。 
最大的颗粒大小通常为约2mm和5mm之间。这种颗粒份额应小于约25％重量份。此外，在模制浆料中的、其粒度小于0.5mm的碳化硅的含量不大于40％，优选至少15％重量份。 
可替换的或额外地，按本发明的模制浆料应补充少于约20％，特别是小于15％重量份的反应性矾土。 
按本发明的经煅烧的模制件在其组成上应具有基本上相当于上述模制 浆料的重量份的重量份。经煅烧模制件的开口孔隙率应大于约10％，尤其是大于约13％并小于约35％。按本发明有利地力求达到的、经煅烧的模制件的体积密度小于约3.5g/cm3，尤其是小于约3.0g/cm3。 
关于所希望的机械性质，按本发明的经煅烧的模制件在标准条件下平均抗弯强度大于约15.0MPa。在此，所给出的抗弯强度是用一种三-点-弯曲试验测量。 
这种由按本发明的模制浆料制造的模制件可有利地用作固定的燃汽轮机的燃烧室的耐火衬里，特别是在面对热燃气的一面具有一种所谓的EBC(环境障涂层)保护层，其带有与热气体温度相适应的、为5mm数量级或优选至少10mm的层厚度。为制造模制件，如上所述，模制浆料在振荡的情况下基于胶状硅酸溶液的固化而制造。为了达到固化，按本发明优选使模制浆料的环境温度急剧下降到小于约0℃的温度并尤其在大于约15分钟并小于约2.5小时的时间间隔内保持该温度。环境的冷却温度尤其优选约为-20℃至-40℃范围。 
浇注完成的模制浆料按本发明优选是在约1300℃和约1650℃之间煅烧。关于陶瓷的煅烧优选是在约1350℃和约1650℃之间的温度范围内进行。纤维加强的陶瓷优选是在约1300℃和约1400℃之间的温度下煅烧。关于结构陶瓷，按本发明优选是在约1300℃和约1600℃之间的煅烧温度下进行。 
下面根据附图详细说明按本发明的模制材料，一种由其制造的经煅烧的模制件，一种由此形成的耐火衬里以及一种用于制造衬里的所属方法的实施例。 
附图示出了一种包括制备所用的模制浆料的耐火衬里的制备方法的示意性流程图。 
一种设计作为固定的燃气轮机的燃烧室的耐火衬里的模制件按图由模制浆料制成，所述模制浆料在第一个工作步骤中基本上由七种组份共同混合。 
这七种成份在图中是以附图标记6，8，10，12，14，16和18表示并按该顺序依次包含有微硅粉(SiO2)，碳化硅(SiC)、刚玉(Al2O3)、莫来石(2Al2O3-1SiO2或3Al2O3-2SiO2)、硅酸(Si(OH)4)、水(H2O)以及反应性矾土。这些材料的重量份对于碳化硅(SiC)优选在70％和90％之间，对于刚玉以氧化铝计为约5％和20％之间，对于莫来石以硅酸铝计为5％和30％之间，而水约3％和7％之间。硅酸的的重量份为约3％和10％之间，而微硅粉(SiO2)的重量份为5％和30％之间。反应性矾土含量为约5％和20％间。 
所述各成份在图中的以附图标记20标记的混合过程中共同混合为模制浆料，该模制浆料接着在一以附图标记22所标示的浇注过程中，在振动的情况在下浇注进铸模。 
通过将其放置在约-25℃温度的环境下，如此制备的铸模被从室温急剧冷却24。通过其急骤冷却，在铸模中存在的模制浆料将其中以溶胶存在的硅酸固化成一种胶体。在此，模制浆料也全部固化并且以尤其有利的方式为以附图标记26标示的干燥和煅烧的最后加工步骤做准备。 
在该加工步骤26中，模制浆料在约1300℃和1600℃之间的烧结温度下进行煅烧。基于这种较低的煅烧温度，可以在模制浆料中掺入纤维加强，因此，可以总共制造一种纤维加强的陶瓷。 
作为模制件制造的陶瓷，最终产品，具有特别有利的机械特性以及具有特别小的、形成热裂缝的倾向。这点特别是由于在陶瓷中通过所述的溶胶-凝胶-工艺并且也由于高的碳化硅成分，产生一种特别的微小裂缝组织，在另一个实施例中有力地减小了边缘裂缝的裂缝长度。 
以这种方式可以通过按本发明的步骤降低在内衬上的陶瓷热屏的损失危险并减少热屏的维护周期和更换周期的数目。总的来说可以达到更高的寿命。 
除此之外，作为本发明特别的优点还要提到的是，浇注浆料全部没有水泥(也就是基本上没有CaO)，并且由于低的烧结温度也进一步在制造过程中获得了成本优势。 
由于其物理、化学和矿物学的性质，浇注浆料十分适于制造复合材料，以及氧化性质。在此列举复合构件，诸如在CMC-基(陶瓷基体复合物)上的用纤维加强的构件，用结构陶瓷加强的构件或加强的构件。 

Claims (24)

1.一种用于制备固定的燃气轮机燃烧室的耐火衬里的模制浆料，其中，所述模制浆料包含碳化硅(8)和硅酸铝(12)成份，并且所述模制浆料是由大于50％重量份的碳化硅(8)和少于50％重量份的硅酸铝(12)构成，其特征在于，添加胶质硅酸溶液(14)，其中，所述胶质硅酸溶液(14)的重量份少于10％，所述胶质硅酸溶液(14)含有大于30％重量份的固体。
2.按权利要求1的模制浆料，其中加入一种液体，其加入量大于1％重量份并且少于10％重量份。
3.按权利要求2的模制浆料，其中所述液体为水(16)。
4.按权利要求1的模制浆料，其具有少于20％重量份的的反应性矾土(18)。
5.按权利要求4的模制浆料，其具有少于15％重量份的反应性矾土(18)。
6.按权利要求1的模制浆料，其具有多于5％重量份并且少于20％重量份的氧化铝(10)。
7.按权利要求1的模制浆料，其具有多于5％重量份并且少于30％重量份的微硅粉(6)。
8.按权利要求1的模制浆料，其颗粒大小最大为5mm。
9.按权利要求1的模制浆料，其中，颗粒大小小于0.5mm的碳化硅的重量份小于40％。
10.按权利要求9的模制浆料，其中，颗粒大小小于0.5mm的碳化硅的重量份大于15％。
11.一种用于固定的燃气轮机燃烧室的耐火衬里的经煅烧的模制件，其具有大于70％重量份并小于90％重量份的碳化硅(8)，大于10％重量份并小于50％重量份的硅酸铝(12)以及多于10％并小于35％的开口孔隙率。
12.按权利要求11的经煅烧的模制件，其具有多于13％并小于35％的开口孔隙率。
13.按权利要求11的经煅烧的模制件，其体积密度小于3.5g/cm3。
14.按权利要求12的经煅烧的模制件，其体积密度小于3.5g/cm3。
15.按权利要求13的经煅烧的模制件，其体积密度小于3.0g/cm3。
16.按权利要求14的经煅烧的模制件，其体积密度小于3.0g/cm3。
17.按权利要求11至16中任一项的经煅烧的模制件，在标准条件下其平均抗弯强度调整为大于15.0MPa。
18.按权利要求11至16中任一项的经煅烧的模制件，其面向高温的表面配设有一保护层。
19.按权利要求18的经煅烧的模制件，该保护层设计为环境障涂层。
20.一种燃烧室的耐火衬里，其具有至少一个按权利要求11至19中任一项所述的经煅烧的模制件。
21.按权利要求20所述的耐火衬里，其为固定的燃气轮机的燃烧室的耐火衬里。
22.用于固定的燃气轮机燃烧室的耐火衬里的经煅烧的模制件的制造方法，其有以下步骤：
制备(20)一种具有至少碳化硅(8)，氧化铝(10)和硅酸铝(12)成分并加入胶质硅酸溶液(14)的模制浆料，
在振荡的情况下浇注(22)所述模制浆料，
急剧降低(24)所述模制浆料的温度，
以及干燥和煅烧(26)所述浇注的模制浆料，
所述模制浆料包含大于50％重量份的碳化硅(8)、少于50％重量份的硅酸铝(12)、少于10％重量份的胶质硅酸溶液(14)，其中所述胶质硅酸溶液(14)含有大于30％重量份的固体。
23.按权利要求22的方法，其中，所述温度急剧降低(24)到低于0℃。
24.按权利要求23的方法，其中，在多于15分钟和少于2.5小时的时间段内保持该温度。
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