CN107098702B - 一种近净成型反应烧结碳化硅材料的制备方法 - Google Patents
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Abstract
本发明是一种近净成型反应烧结碳化硅材料的制备方法,包括以下步骤:(1)料浆配置:将碳化硅粉体、高残炭率树脂、造孔剂、碳粉、溶剂、表面活性剂等进行球磨,得到均匀混合的料浆;(2)干燥成膜:采用刮刀将步骤(1)得到的料浆均匀涂覆在离型纸上,并充分干燥成膜;(3)固化定型:将干燥后的膜铺叠,并采用热压机或热压罐进行固化定型成素坯;(4)炭化:将步骤(3)所得的定型后的素坯按一定升温程序进行炭化;(5)熔融渗硅:将步骤(4)得到的炭化后的多孔体与硅粉放入石墨坩埚并加热至硅熔点以上实现渗硅。本发明素坯成型压力小,可采用热压机或热压罐进行成型,并且定型后的素坯在炭化及熔渗过程中尺寸稳定性好,得到的反应烧结碳化硅力学性能优良。
Description
技术领域
本发明是一种近净成型反应烧结碳化硅材料的制备方法,属于无机非金属材料技术领域。
背景技术
碳化硅是一种重要的结构陶瓷材料,其具备耐高温、耐腐蚀、密度低、强度高及摩擦性能好等特点,在冶金、化工、航空、能源、运输、机械等领域应用广泛。由于碳化硅烧结温度高,因此其成型特别困难,常用的碳化硅的制备方法有添加助剂烧结法与反应烧结制备法。添加烧结助剂法需要高温、高压的成型条件,因此成本高、能耗大。反应烧结法由于成型温度较低,且易成型复杂构件,因此应用较为广泛,在许多对残余硅要求不严格的场合,此种方法具有很大的优势。
专利CN104030688 A介绍了一种低温反应烧结碳化硅的制备方法,该专利报道了将碳粉、碳化硅粉及酚醛溶液混合,经过球磨、喷雾干燥制粒后,再在模具中压制成形。该专利制备过程中涉及到制粒过程,需专门设备进行造粒,投资成本较高。专利CN102295458 A公开了一种反应烧结碳化硅陶瓷的制备方法,将废弃碳化硅粉末、碳化硅粉料、粘结剂和溶剂按比例加入球磨机,经烘干、成坯、捣碎、过筛、再成坯、排胶及熔渗后制成反应烧结碳化硅陶瓷材料。该专利制备的生坯由粉料热压而成,不利于复杂构件的成型。专利CN101747044A公开了一种碳化硅材料的制备工艺。首先,将碳化硅粉末、中间相炭微球经过无水乙醇湿混、干燥后模压成型,再进行焙烧、渗硅得到反应烧结碳化硅陶瓷。采用该专利制备的反应烧结碳化硅密度相对较低,且制备的碳化硅含有少量未完全反应的碳。
发明内容
本发明的目的是提供一种近净成型反应烧结碳化硅材料的方法,其目的是使素坯成型压力小,可采用热压机或热压罐进行成型,并且定型后的素坯在炭化及熔渗过程中尺寸稳定性好,得到的反应烧结碳化硅力学性能优良。
本发明的目的是通过以下技术方案来实现的:
该种近净成型反应烧结碳化硅材料的制备方法,其特征在于:该方法的步骤如下:
(1)料浆配置:将碳化硅粉体、高残炭率树脂、造孔剂、碳粉、溶剂、表面活性剂混合后进行球磨,球磨时间为5-20小时,得到均匀的料浆;
碳化硅粉体、高残炭率树脂、造孔剂、碳粉、溶剂、表面活性剂的质量份数比为:
所述碳化硅粉体的粒径为0.05-5μm;
所述高残炭率树脂是酚醛树脂、呋喃树脂或沥青中的一种或几种的混合物;
所述碳粉是石墨粉、中间相炭微球、焦炭粉或炭黑中的一种或几种的混合物;
所述溶剂为丙酮、甲醇、乙醇、甲基乙基酮、苯、甲苯、二甲苯、乙二醇单甲醚、乙二醇单丁醚、甲基丁酮中的一种或几种的混合物;
所述表面活性剂是碳粉分散剂;
(2)干燥成膜:采用刮刀将步骤(1)得到的料浆均匀涂覆在离型纸上,并充分干燥成膜;
(3)固化定型:将干燥后的膜层叠在一起,并采用热压机或热压罐进行固化定型成素坯,固化温度100-300℃之间,固化压力0.2-20MPa 之间;
(4)炭化:将步骤(3)所得的定型后的素坯进行炭化,得到多孔体,炭化温度为500-1200℃之间,保温时间0.5-2h;
(5)熔融渗硅:将步骤(4)得到的炭化后的多孔体与硅粉共同放入石墨坩埚中,并加热至1300-1700℃之间实现熔渗,得到近净成型反应烧结碳化硅材料;
硅粉用量为多孔体重量的0.5-5倍。
本发明的优点和特点:
本发明制备的料浆干燥后能够成膜,便于铺贴,尤其对于复杂形状特别有利。
本发明的素坯成型压力低,可采用热压机或热压罐进行成型,便于复杂形状的制备。
本发明素坯炭化及熔渗过程中尺寸变化小,可实现近净尺寸成型。
本发明具有生产工艺简单、投资规模小,毛坯加工量小、适合制备复杂形状制品的特点,适于批量生产。
具体实施方式
以下结合具体实例说明近净成型反应烧结碳化硅的制备方法。
实施例1
本发明所述的近净成型反应烧结碳化硅的制备方法的步骤如下:
(1)将1000g碳化硅粉体、206g酚醛树脂、100g造孔剂、200g石墨粉、3000g乙醇、50g表面活性剂加入到球磨罐进行球磨,球磨时间 12小时,得到均匀混合的料浆;
(2)采用刮刀将步骤(1)得到的料浆均匀涂覆在离型纸上,并充分干燥成膜;
(3)固化定型:将干燥后的膜裁剪成100x100mm大小,并进行铺贴于模具,采用热压机进行固化定型成素坯,固化温度为180℃,固化时间为2h,固化压力为20MPa;
(4)炭化:将步骤(3)所得的定型后的素坯加热至1000℃进行炭化,保温时间1h,升温速率为5℃/min;
(5)熔融渗硅:将步骤(4)得到的炭化后的多孔体与3.5倍的硅粉结合并加热至1500℃实现熔渗。得到近净成型的反应烧结碳化硅平板件。
实施例2
本发明所述的近净成型反应烧结碳化硅的制备方法的步骤如下:
(1)将1000g碳化硅粉体、356g酚醛树脂、130g造孔剂、105g 焦炭粉、3000g丙酮、50g表面活性剂加入到球磨罐进行球磨,球磨时间 12小时,得到均匀混合的料浆;
(2)采用刮刀将步骤(1)得到的料浆均匀涂覆在离型纸上,并充分干燥成膜;
(3)固化定型:将干燥后的膜裁剪成100x100mm大小,并叠层铺贴于模具,采用热压机进行固化定型成素坯,固化温度为180℃,固化时间为2h,固化压力为15MPa;
(4)炭化:将步骤(3)所得的定型后的素坯加热至1000℃进行炭化,保温时间1h,升温速率为10℃/min;
(5)熔融渗硅:将步骤(4)得到的炭化后的多孔体与3.5倍的硅粉结合并加热至1500℃实现熔渗。得到近净成型的反应烧结碳化硅平板件。
实施例3
本发明所述的近净成型反应烧结碳化硅的制备方法的步骤如下:
(1)将1100g碳化硅粉体、206g酚醛树脂、120g造孔剂、120g石墨粉、4000g乙醇、60g表面活性剂加入到球磨罐进行球磨,球磨时间 12小时,得到均匀混合的料浆;
(2)采用刮刀将步骤(1)得到的料浆均匀涂覆在离型纸上,并充分干燥成膜;
(3)固化定型:将干燥后的膜裁剪成80x80mm大小,并进行铺贴于模具,采用热压机进行固化定型成素坯,固化温度为180℃,固化时间为2h,固化压力为15MPa;
(4)炭化:将步骤(3)所得的定型后的素坯加热至1000℃进行炭化,保温时间1h,升温速率为5℃/min;
(5)熔融渗硅:将步骤(4)得到的炭化后的多孔体与3倍的硅粉结合并加热至1500℃实现熔渗。得到近净成型的反应烧结碳化硅平板件。
Claims (2)
1.一种近净成型反应烧结碳化硅材料的制备方法,其特征在于:该方法的步骤如下:
(1)料浆配置:将碳化硅粉体、高残炭率树脂、造孔剂、碳粉、溶剂、表面活性剂混合后进行球磨,球磨时间为5-20小时,得到均匀的料浆;
碳化硅粉体、高残炭率树脂、造孔剂、碳粉、溶剂、表面活性剂的质量份数比为:
所述高残炭率树脂是酚醛树脂或呋喃树脂中的一种或两种的混合物;
所述碳粉是石墨粉、中间相炭微球、焦炭粉或炭黑中的一种或几种的混合物;
所述溶剂为丙酮、甲醇、乙醇、甲基乙基酮、苯、甲苯、二甲苯、乙二醇单甲醚、乙二醇单丁醚、甲基丁酮中的一种或几种的混合物;
所述表面活性剂是碳粉分散剂;
(2)干燥成膜:采用刮刀将步骤(1)得到的料浆均匀涂覆在离型纸上,并充分干燥成膜;
(3)固化定型:将干燥后的膜层叠在一起,并采用热压机或热压罐进行固化定型成素坯,固化温度100-300℃之间,固化压力0.2-20MPa之间;
(4)炭化:将步骤(3)所得的定型后的素坯进行炭化,得到多孔体,炭化温度为500-1200℃之间,保温时间0.5-2h;
(5)熔融渗硅:将步骤(4)得到的炭化后的多孔体与硅粉共同放入石墨坩埚中,并加热至1300-1700℃之间实现熔渗,得到近净成型反应烧结碳化硅材料;
硅粉用量为多孔体重量的0.5-5倍。
2.根据权利要求1所述近净成型反应烧结碳化硅材料的制备方法,其特征在于:所述碳化硅粉体的粒径为0.05-5μm。
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CN102180674A (zh) * | 2011-01-31 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | 一种反应烧结SiC陶瓷的制备方法 |
CN102557722A (zh) * | 2011-12-27 | 2012-07-11 | 中原工学院 | 一种使用造孔剂制备多孔碳化硅陶瓷的方法 |
CN103342570A (zh) * | 2013-07-11 | 2013-10-09 | 山东宝纳新材料有限公司 | 一种低成本熔硅浸渗法制备 C/SiC 复合材料的方法 |
CN103721577A (zh) * | 2013-12-17 | 2014-04-16 | 杭州创享环境技术有限公司 | 一种多通道对称结构纯质碳化硅膜及其制备的方法 |
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