CN112552062A - 一种复合材料的制造方法 - Google Patents
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Abstract
本发明公开了一种复合材料的制造方法,其方法包括如下步骤:称取以下质量百分比的原料:30%~40%的碳化硅,20~30%的氮化硅,20~30%的氧化铝,1~5%的粘结剂,1~2%的分散剂,1~2%的固化剂,1~2%的催化剂,1~2%的引发剂;本发明通过改进陶瓷复合材料的制造方法,具有可以有效增加陶瓷复合材料的结构强度,防止陶瓷复合材料内部存在缺陷,进而能够提升陶瓷复合材料生产制造质量的优点,解决了目前陶瓷复合材料中的陶瓷含量比较低,使得陶瓷复合材料的结构强度较差,同时陶瓷复合材料的内部存在气孔和杂质等缺陷,无法满足实际使用需求,且陶瓷复合材料的成型比较困难的问题,从而达到简化工艺和降低成本的目的。
Description
技术领域
本发明涉及复合材料技术领域,具体为一种复合材料的制造方法。
背景技术
航空航天领域中,许多零件需要在高温下工作,而高温合金的使用温度制约了其发展。陶瓷较强的耐高温能力使之成为最有前途的航空航天材料,但是陶瓷的韧性较低容易脆断,因此提高陶瓷的韧性很关键,需要探索一种具有定向组织在零件内部增强的成型方法。
陶瓷材料正是由于它的耐高温、抗氧化、高耐磨、硬度大、耐腐蚀、抗压强度高等众多优异性能,使得陶瓷在当今世界里可谓是无处不在,其在航空航天、机械、电子、能源等军事、民用行业都有它不可替代的贡献和作用,然而陶瓷的致命弱点就是脆性很大,抗拉强度非常低,其对裂纹、气孔、杂质等缺陷特别敏感,大大限制了它在众多领域的应用。
目前陶瓷复合材料中的陶瓷含量比较低,使得陶瓷复合材料的结构强度较差,同时陶瓷复合材料的内部存在气孔和杂质等缺陷,无法满足实际使用需求,且陶瓷复合材料的成型比较困难,导致陶瓷复合材料的生产制造效率以及生产成本较高。
发明内容
本发明的目的在于提供一种复合材料的制造方法,具备可以有效增加陶瓷复合材料的结构强度,防止陶瓷复合材料内部存在缺陷,进而能够提升陶瓷复合材料生产制造质量的优点,解决了目前陶瓷复合材料中的陶瓷含量比较低,使得陶瓷复合材料的结构强度较差,同时陶瓷复合材料的内部存在气孔和杂质等缺陷,无法满足实际使用需求,且陶瓷复合材料的成型比较困难的问题。
为实现上述目的,本发明提供如下技术方案:一种复合材料的制造方法,其方法包括如下步骤:
(1)原料准备:称取以下质量百分比的原料:30%~40%的碳化硅,20~30%的氮化硅,20~30%的氧化铝,1~5%的粘结剂,1~2%的分散剂,1~2%的固化剂,1~2%的催化剂,1~2%的引发剂;
(2)原料预处理:将碳化硅、氮化硅和氧化铝颗粒分别置于反应容器中,进行真空烘干处理,处理完成后将碳化硅、氮化硅和氧化铝原料混合均匀,获得混合料;
(3)制备水基预混液:将有机单体丙烯酰胺和交联剂N,N-亚甲基双丙烯酰胺混合,并配制成质量分数为15%~25%的水基预混液;
(4)制备材料胚:将混合料加入混合容器中,随后向加入水基预混液中,得到陶瓷浆料,并加入分散剂和粘结剂得到预混浆料,接着将预混浆料搅拌均匀,得到固相颗粒分散均匀的悬浮浆料,向悬浮浆料中加入催化剂和引发剂,并使悬浮浆料完全凝固得到材料坯;
(5)高温热处理:将材料坯置于真空脱脂炉中进行保温处理,去除材料坯内部具有定向孔隙的有机物,得到基体材料,然后进行化学气相沉积处理,使碳化硅的表面形成硅薄膜;
(6)浇注成型:将经过熔化处理的基体材料中浇入模具型腔中,并加入固化剂,加压并保压,保压结束后打开模具,即可制得陶瓷基复合材料。
优选的,所述步骤(1)中,原料中碳化硅、氮化硅和氧化铝为陶瓷颗粒和陶瓷纤维,其中陶瓷颗粒的粒径为0.1~1mm,陶瓷纤维的长度为0.1~2mm。
优选的,所述步骤(2)中,真空烘干时的烘干温度设置为160~200℃,且真空烘干时间为3~5h。
优选的,所述步骤(4)中,分散剂采用25%的四甲基氢氧化铵水溶液,粘结剂为酚醛树脂热固性粘结剂或环氧树脂热固性粘结剂中的一种。
优选的,所述步骤(4)中,催化剂采用质量分数为35%的四甲基乙二胺水溶液,引发剂采用质量分数为45%的硫酸铵水溶液。
优选的,所述步骤(5)中,真空脱脂炉中升温过程:以升温速率为5℃/min从室温升至200℃,然后以升温速率为1℃/min从200℃升至700℃,再以升温速率为2℃/min从700℃升至900~1200℃,并在900~1200℃保温0.5~1h。
优选的,所述步骤(5)中,化学气相沉积处理时通入氮气保护,加热到100~130℃,1~2h后通入硅烷气体升温至380~410℃,保温6~8h。
优选的,所述步骤(6)中,固化剂采用脂肪族胺类固化剂,加压压力为50MPa~200MPa,且保压时间为2~5min。
与现有技术相比,本发明的有益效果如下:
本发明通过改进陶瓷复合材料的制造方法,具有可以有效增加陶瓷复合材料的结构强度,防止陶瓷复合材料内部存在缺陷,进而能够提升陶瓷复合材料生产制造质量的优点,解决了目前陶瓷复合材料中的陶瓷含量比较低,使得陶瓷复合材料的结构强度较差,同时陶瓷复合材料的内部存在气孔和杂质等缺陷,无法满足实际使用需求,且陶瓷复合材料的成型比较困难的问题,从而达到简化工艺和降低成本的目的。
具体实施方式
下面将结合本发明中的实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例一:
一种复合材料的制造方法,其方法包括如下步骤:
(1)原料准备:称取以下质量百分比的原料:30%的碳化硅,30%的氮化硅,30%的氧化铝,5%的粘结剂,1%的分散剂,1%的固化剂,1%的催化剂,2%的引发剂,原料中碳化硅、氮化硅和氧化铝为陶瓷颗粒和陶瓷纤维,其中陶瓷颗粒的粒径为0.1~1mm,陶瓷纤维的长度为0.1~2mm,便于制造陶瓷复合材料,为加工处理步骤带来了便利;
(2)原料预处理:将碳化硅、氮化硅和氧化铝颗粒分别置于反应容器中,进行真空烘干处理,处理完成后将碳化硅、氮化硅和氧化铝原料混合均匀,获得混合料,真空烘干时的烘干温度设置为160℃,且真空烘干时间为3h,可以除去碳化硅、氮化硅和氧化铝原料表面附着的水分,且能够防止杂质进入影响复合材料的制造加工;
(3)制备水基预混液:将有机单体丙烯酰胺和交联剂N,N-亚甲基双丙烯酰胺混合,并配制成质量分数为15%的水基预混液;
(4)制备材料胚:将混合料加入混合容器中,随后向加入水基预混液中,得到陶瓷浆料,并加入分散剂和粘结剂得到预混浆料,接着将预混浆料搅拌均匀,得到固相颗粒分散均匀的悬浮浆料,向悬浮浆料中加入催化剂和引发剂,并使悬浮浆料完全凝固得到材料坯;
(5)高温热处理:将材料坯置于真空脱脂炉中进行保温处理,去除材料坯内部具有定向孔隙的有机物,得到基体材料,然后进行化学气相沉积处理,使碳化硅的表面形成硅薄膜;
(6)浇注成型:将经过熔化处理的基体材料中浇入模具型腔中,并加入固化剂,加压并保压,保压结束后打开模具,即可制得陶瓷基复合材料。
实施例二:
一种复合材料的制造方法,其方法包括如下步骤:
(1)原料准备:称取以下质量百分比的原料:35%的碳化硅,30%的氮化硅,25%的氧化铝,3%的粘结剂,1.5%的分散剂,1.5%的固化剂,2%的催化剂,2%的引发剂,原料中碳化硅、氮化硅和氧化铝为陶瓷颗粒和陶瓷纤维,其中陶瓷颗粒的粒径为0.1~1mm,陶瓷纤维的长度为0.1~2mm,便于制造陶瓷复合材料,为加工处理步骤带来了便利;
(2)原料预处理:将碳化硅、氮化硅和氧化铝颗粒分别置于反应容器中,进行真空烘干处理,处理完成后将碳化硅、氮化硅和氧化铝原料混合均匀,获得混合料,真空烘干时的烘干温度设置为180℃,且真空烘干时间为4h,可以除去碳化硅、氮化硅和氧化铝原料表面附着的水分,且能够防止杂质进入影响复合材料的制造加工;
(3)制备水基预混液:将有机单体丙烯酰胺和交联剂N,N-亚甲基双丙烯酰胺混合,并配制成质量分数为20%的水基预混液;
(4)制备材料胚:将混合料加入混合容器中,随后向加入水基预混液中,得到陶瓷浆料,并加入分散剂和粘结剂得到预混浆料,接着将预混浆料搅拌均匀,得到固相颗粒分散均匀的悬浮浆料,向悬浮浆料中加入催化剂和引发剂,并使悬浮浆料完全凝固得到材料坯,分散剂采用25%的四甲基氢氧化铵水溶液,粘结剂为酚醛树脂热固性粘结剂或环氧树脂热固性粘结剂中的一种,催化剂采用质量分数为35%的四甲基乙二胺水溶液,引发剂采用质量分数为45%的硫酸铵水溶液,分散剂可均一分散难溶解于液体的颗粒,同时也能防止颗粒的沉降和凝聚,粘结剂可以有效增加原料之间的粘结强度,催化剂和引发剂可以加快原料之间的混合效果,保证浆料混合均匀;
(5)高温热处理:将材料坯置于真空脱脂炉中进行保温处理,去除材料坯内部具有定向孔隙的有机物,得到基体材料,然后进行化学气相沉积处理,使碳化硅的表面形成硅薄膜;
(6)浇注成型:将经过熔化处理的基体材料中浇入模具型腔中,并加入固化剂,加压并保压,保压结束后打开模具,即可制得陶瓷基复合材料。
实施例三:
一种复合材料的制造方法,其方法包括如下步骤:
(1)原料准备:称取以下质量百分比的原料:40%的碳化硅,20%的氮化硅,30%的氧化铝,2%的粘结剂,2%的分散剂,2%的固化剂,2%的催化剂,2%的引发剂,原料中碳化硅、氮化硅和氧化铝为陶瓷颗粒和陶瓷纤维,其中陶瓷颗粒的粒径为0.1~1mm,陶瓷纤维的长度为0.1~2mm,便于制造陶瓷复合材料,为加工处理步骤带来了便利;
(2)原料预处理:将碳化硅、氮化硅和氧化铝颗粒分别置于反应容器中,进行真空烘干处理,处理完成后将碳化硅、氮化硅和氧化铝原料混合均匀,获得混合料,真空烘干时的烘干温度设置为200℃,且真空烘干时间为5h,可以除去碳化硅、氮化硅和氧化铝原料表面附着的水分,且能够防止杂质进入影响复合材料的制造加工;
(3)制备水基预混液:将有机单体丙烯酰胺和交联剂N,N-亚甲基双丙烯酰胺混合,并配制成质量分数为25%的水基预混液;
(4)制备材料胚:将混合料加入混合容器中,随后向加入水基预混液中,得到陶瓷浆料,并加入分散剂和粘结剂得到预混浆料,接着将预混浆料搅拌均匀,得到固相颗粒分散均匀的悬浮浆料,向悬浮浆料中加入催化剂和引发剂,并使悬浮浆料完全凝固得到材料坯,分散剂采用25%的四甲基氢氧化铵水溶液,粘结剂为酚醛树脂热固性粘结剂或环氧树脂热固性粘结剂中的一种,催化剂采用质量分数为35%的四甲基乙二胺水溶液,引发剂采用质量分数为45%的硫酸铵水溶液,分散剂可均一分散难溶解于液体的颗粒,同时也能防止颗粒的沉降和凝聚,粘结剂可以有效增加原料之间的粘结强度,催化剂和引发剂可以加快原料之间的混合效果,保证浆料混合均匀;
(5)高温热处理:将材料坯置于真空脱脂炉中进行保温处理,去除材料坯内部具有定向孔隙的有机物,得到基体材料,然后进行化学气相沉积处理,使碳化硅的表面形成硅薄膜,真空脱脂炉中升温过程:以升温速率为5℃/min从室温升至200℃,然后以升温速率为1℃/min从200℃升至700℃,再以升温速率为2℃/min从700℃升至1000℃,并在1000℃保温1h,化学气相沉积处理时通入氮气保护,加热到120℃,1h后通入硅烷气体升温至410℃,保温8h,可以有效提升复合材料的高温热处理效果,从而对复合材料内部的短纤维具有一定的保护作用,增加复合材料的结构强度;
(6)浇注成型:将经过熔化处理的基体材料中浇入模具型腔中,并加入固化剂,加压并保压,保压结束后打开模具,即可制得陶瓷基复合材料,固化剂采用脂肪族胺类固化剂,加压压力为100MPa,且保压时间为5min,脂肪族胺类固化剂具有良好的高温表现,很好的耐化学腐蚀性并具有良好的电性能和机械性能,进而能够提升复合材料的制造质量。
本发明通过改进陶瓷复合材料的制造方法,具有可以有效增加陶瓷复合材料的结构强度,防止陶瓷复合材料内部存在缺陷,进而能够提升陶瓷复合材料生产制造质量的优点,解决了目前陶瓷复合材料中的陶瓷含量比较低,使得陶瓷复合材料的结构强度较差,同时陶瓷复合材料的内部存在气孔和杂质等缺陷,无法满足实际使用需求,且陶瓷复合材料的成型比较困难的问题,从而达到简化工艺和降低成本的目的。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (8)
1.一种复合材料的制造方法,其特征在于:其方法包括如下步骤:
(1)原料准备:称取以下质量百分比的原料:30%~40%的碳化硅,20~30%的氮化硅,20~30%的氧化铝,1~5%的粘结剂,1~2%的分散剂,1~2%的固化剂,1~2%的催化剂,1~2%的引发剂;
(2)原料预处理:将碳化硅、氮化硅和氧化铝颗粒分别置于反应容器中,进行真空烘干处理,处理完成后将碳化硅、氮化硅和氧化铝原料混合均匀,获得混合料;
(3)制备水基预混液:将有机单体丙烯酰胺和交联剂N,N-亚甲基双丙烯酰胺混合,并配制成质量分数为15%~25%的水基预混液;
(4)制备材料胚:将混合料加入混合容器中,随后向加入水基预混液中,得到陶瓷浆料,并加入分散剂和粘结剂得到预混浆料,接着将预混浆料搅拌均匀,得到固相颗粒分散均匀的悬浮浆料,向悬浮浆料中加入催化剂和引发剂,并使悬浮浆料完全凝固得到材料坯;
(5)高温热处理:将材料坯置于真空脱脂炉中进行保温处理,去除材料坯内部具有定向孔隙的有机物,得到基体材料,然后进行化学气相沉积处理,使碳化硅的表面形成硅薄膜;
(6)浇注成型:将经过熔化处理的基体材料中浇入模具型腔中,并加入固化剂,加压并保压,保压结束后打开模具,即可制得陶瓷基复合材料。
2.根据权利要求1所述的一种复合材料的制造方法,其特征在于:所述步骤(1)中,原料中碳化硅、氮化硅和氧化铝为陶瓷颗粒和陶瓷纤维,其中陶瓷颗粒的粒径为0.1~1mm,陶瓷纤维的长度为0.1~2mm。
3.根据权利要求1所述的一种复合材料的制造方法,其特征在于:所述步骤(2)中,真空烘干时的烘干温度设置为160~200℃,且真空烘干时间为3~5h。
4.根据权利要求1所述的一种复合材料的制造方法,其特征在于:所述步骤(4)中,分散剂采用25%的四甲基氢氧化铵水溶液,粘结剂为酚醛树脂热固性粘结剂或环氧树脂热固性粘结剂中的一种。
5.根据权利要求1所述的一种复合材料的制造方法,其特征在于:所述步骤(4)中,催化剂采用质量分数为35%的四甲基乙二胺水溶液,引发剂采用质量分数为45%的硫酸铵水溶液。
6.根据权利要求1所述的一种复合材料的制造方法,其特征在于:所述步骤(5)中,真空脱脂炉中升温过程:以升温速率为5℃/min从室温升至200℃,然后以升温速率为1℃/min从200℃升至700℃,再以升温速率为2℃/min从700℃升至900~1200℃,并在900~1200℃保温0.5~1h。
7.根据权利要求1所述的一种复合材料的制造方法,其特征在于:所述步骤(5)中,化学气相沉积处理时通入氮气保护,加热到100~130℃,1~2h后通入硅烷气体升温至380~410℃,保温6~8h。
8.根据权利要求1所述的一种复合材料的制造方法,其特征在于:所述步骤(6)中,固化剂采用脂肪族胺类固化剂,加压压力为50MPa~200MPa,且保压时间为2~5min。
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