CN102438965A - 用于耐火材料和陶瓷的胶和涂料 - Google Patents
用于耐火材料和陶瓷的胶和涂料 Download PDFInfo
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Abstract
本发明涉及用于耐火材料和陶瓷的热固性胶或涂料。所述胶或涂料包含25-50重量%硅粉末,5-20重量%SiC粉末,20-60重量%甲醛树脂或聚糠醇和10-30重量%的有机溶剂。
Description
发明领域
本发明涉及用于耐火材料和陶瓷(例如碳材料、氮化硅、碳化硅和石英)的胶和涂料。
背景技术
已知用于胶合耐火材料和陶瓷(例如碳材料、氮化硅、碳化硅和石英,其在高温下使用)的多种胶。由美国专利No.5,474,849因而已知用于碳组分的胶。所述胶包含热固性polysilagen聚合物,占聚合物重量20-50重量%的陶瓷粉末(其能够是SiC),占聚合物重量10-40重量%的Si-粉末和占聚合物重量5-15重量%的碳粉末。
但是,已经发现该类型的胶不适用于在倾向于与熔融硅接触的炉、模具、坩埚或为此的零件(details for such)中使用的碳材料、氮化硅、碳化硅和石英。重要的是,对于部件使用的胶不污染与所提及的炉、模具、坩埚或为此的零件接触的熔融硅。这对用于制造太阳能电池的高纯度硅的处理是特别重要的。还重要的是胶接合部不可由熔融二氧化硅润湿。
发明描述
本发明提供了容易使用的胶和涂料,其具有良好的高温强度,不可由熔融硅润湿并且能够长时间储存。所述胶和涂料进一步具有令人惊讶的效果,其在从高温冷却并降到低于1000℃期间丧失(loose)其强度。该效果在所述胶用于将由分开的片材(例如氮化硅、石英或石墨的片材,用于熔融硅的取向性凝固(directional solidification))制造的模具胶合在一起时特别有用。在硅冷却期间,发生固体相变,其导致体积增加并可能引起模具故障。通过使用由用本发明所述的胶胶合的分开的片材制造的模具,所述胶在发生相变的温度下将具有低强度,并且所述模具将因此在胶层中开裂而同时单独的片材不会受损。所述片材因此能够再用于制造新模具。
本发明因而涉及用于碳材料、氮化硅、碳化硅和石英的热固性的胶或涂料,所述胶或涂料由25-50重量%硅粉末,5-20重量%碳化硅粉末,20-60重量%酚醛树脂(fenol formaldehyde resin)或聚糠醇(polyfurfuryl alcohol)和10-30重量%有机溶剂组成。
根据一个优选的实施方案,所述有机溶剂选自单乙二醇,二乙二醇和三乙二醇。优选的有机溶剂是单乙二醇。
所述溶剂加入的量足以获得适当粘度的胶或涂料。
根据一个优选的实施方案,所述胶或涂料包含35-45重量%硅粉末,8-18重量%硅粉末,25-35重量%甲醛树脂(formaldehyde resin)或聚糠醇和15-25重量%有机溶剂。
根据另一优选实施方案,所述胶或涂料包含固化剂以便降低所述甲醛树脂或所述聚糠醇的聚合温度。所述固化剂优选是乌洛托品,但也能够使用磷酸铝和酸例如硫酸、对甲苯磺酸(PTS)、用尿素中和的PTS和对甲苯磺酸乙酯(PTSEE)。
本发明的胶或涂料在室温下为液态并且能够长时间储存。
当使用不包含固化剂的胶或涂料时,有机溶剂将在150-290℃挥发且甲醛树脂和聚糠醇的聚合将在250℃-400℃的温度范围内进行,由此形成固体结构。如果加入固化剂,聚合过程将在较低温度开始。
在进一步加热期间,将在大约700℃保留由剩余的甲醛树脂或聚糠醇组成的碳结构。在该温度范围内所述胶的强度将高于20MPa。通过进一步的温度升高,在所述胶中的碳结构和硅粉末之间将发生反应,并且随着继续加热至超过1413℃的温度,Si粉末将熔融并与碳反应成SiC。然而,如果温度升高缓慢,Si粉末和碳之间的反应将在固体状态中进行。
当使用所述胶来胶合用于熔炼坩埚的碳盖时,本发明所述的胶显示出针对与熔融硅的接触产生密封。在所述熔炼坩埚已经用于熔炼硅之后的冷却期间,所述胶的强度消失且胶合在一起的部件能够从彼此脱开而没有阻力。因而只要胶合的部件保持在高温,根据本发明所述的胶就保持其强度。
通过在用于熔融硅的凝固的石墨模具中使用涂料进行的测试显示,所述涂料提供了填充孔和腔隙的层并针对硅透入所述石墨模具壁中完全密封。
在冷却硅并除去硅坯料之后,剩余的涂料能够以粉尘样粉末的形式刷掉并且所述模具能够用本发明所述的涂料再次涂覆。
本发明所述的胶还能够用于胶合在硅的取向性凝固中使用的模具,其中所述模具由胶合在一起的底部片材和侧片材组成。所述胶密封腔隙,所述片材中的表面粗糙度和对片材表面抛光的要求因此能够降低。在凝固和冷却之后,所述胶将如上所述丧失其强度且所述片材因此能够用于制造新模具。胶合的片材能够由碳材料制造,例如预烘干的碳片材或石墨片材、氮化硅片材或石英片材。
附图说明
图1显示了用于测试用本发明所述的胶胶合的石墨部件强度的装备。
发明详述。
实施例
图1显示了用于测试胶强度的装备,所述胶用于用本发明所述的胶胶合的石墨部件。所述胶具有以下组成:
38重量%硅粉末,12重量%碳化硅粉末,28重量%甲醛树脂,18%单乙二醇和4重量%乌洛托品。
在图1上,示意性地显示了放置在感应炉(未显示)中的石墨坩埚1。制备了由直径为24毫米且借助于本发明所述胶胶合至下部石墨柱体3的上部石墨柱体2组成的三个样品。所述柱体3与所述石墨柱体2相比较具有更大的直径。将所述三个胶合的样品拧至坩埚1的盖子4的下侧。借助于热电偶测量坩埚中的温度并通过经管道6添加氩气而使所述坩埚中的气氛保持惰性。穿过所述盖子4插入陶瓷杆7以便将力施加至样品的部件3。陶瓷杆7连接至20千克的轻磅(feather-weight)。
根据以下程序加热坩埚:
20-1000℃:20分钟
1000-1600℃:60分钟
在1600℃的保留时间:60分钟
从1600℃冷却至1000℃:60分钟
此后关闭所述炉并将样品缓慢地冷却至室温。
在不同温度和不同时间对样品1-3加载20千克的力。结果显示在表I中。
表1
表1中显示的结果表明,在加热阶段期间加载有20千克重量的样品1在直至1600℃具有良好强度。
样品2在1600℃保持60分钟之后加载20千克的重量并在该温度具有良好的强度。样品2还在冷却至1350℃之后显示出良好的强度。
样品3在1600℃保持60分钟之后并在冷却至1350℃期间和在进一步冷却至1000℃期间加载20千克的重量。结果显示,所述胶的强度在这些温度非常好。通过进一步冷却至室温,样品3的部件3从样品的上部部件2落下。
来自这些实施例的结果表明,本发明所述胶在加热至1600℃期间具有很好的强度并在冷却至低于1000℃的温度期间保持其强度,而所述强度在此后降低。
Claims (6)
1.用于耐火材料和陶瓷的可热固化的胶或涂料,特征在于所述胶或涂料包含25-50重量%硅粉末,5-20重量%碳化硅粉末,20-60重量%酚醛树脂或聚糠醇和10-30重量%有机溶剂。
2.根据权利要求1所述的胶或涂料,特征在于所述有机溶剂选自单乙二醇、二乙二醇和三乙二醇。
3.根据权利要求1所述的胶或涂料,特征在于胶或涂料包含35-45重量%硅粉末,8-18重量%硅粉末,25-35重量%甲醛树脂或聚糠醇和15-25重量%有机溶剂。
4.根据权利要求1-3所述的胶或涂料,特征在于所述胶或涂料包含固化剂以便降低所述甲醛树脂或所述聚糠醇的聚合温度。
5.根据权利要求4所述的胶或涂料,特征在于所述固化剂选自乌洛托品、磷酸铝或酸。
6.根据权利要求5所述的胶或涂料,特征在于所述酸选自硫酸、用尿素中和的对甲苯磺酸和对甲苯磺酸乙酯。
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US20120088876A1 (en) | 2012-04-12 |
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