CN108358636A - 一种碳基耗散防热复合材料的制备方法 - Google Patents
一种碳基耗散防热复合材料的制备方法 Download PDFInfo
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Abstract
一种碳基耗散防热复合材料的制备方法,它涉及一种耗散防热复合材料的制备方法。本发明是要解决现有的碳/碳及其改性的复合材料制备工艺复杂,制备周期长,成本高的技术问题。本发明:一、将浸渗剂装入石墨坩埚中;二、加工碳基体材料;三、将坩埚放入气压浸渗炉中,将基体材料连接到气压浸渗炉中的提拉杆上;四、加热熔化浸渗剂;五、高压将浸渗剂压入到基体孔隙中。本发明所涉及碳基耐烧蚀耗散防热复合材料制备工艺简单、周期短、复合材料可实现近净成型,也可进行电加工和机械加工,制造成本低、耐烧蚀性能好。本发明应用于轻质耐烧蚀复合材料领域。
Description
技术领域
本发明涉及一种耗散防热复合材料的制备方法。
背景技术
耐烧蚀材料是国防和航天领域重要的工程材料,其作用是受热部件在高温和高速气流冲刷条件下,在工作时间内能够维持气动外形以保证飞行器正常飞行速度和轨迹。随着航天技术的不断发展对轻质耐烧蚀材料的需求越来越迫切。现在常用的轻质耐烧蚀材料主要包括树脂基复合材料和碳/碳复合材料等。树脂基复合材料一般通过热解吸收外界热量,因而烧蚀率大;碳/碳及其改性的复合材料主要是辐射和烧蚀式防热机理,C/SiC等改性的碳/碳复合材料具有优异的耐烧蚀性能,在很多重要的受热部件上获得了应用,但其制备工艺复杂,制备周期长,成本高。
发明内容
本发明是要解决现有的碳/碳及其改性的复合材料制备工艺复杂,制备周期长,成本高的技术问题,而提供一种碳基耗散防热复合材料的制备方法。
本发明的碳基耗散防热复合材料的制备方法是按以下步骤进行的:
一、在石墨坩埚的内壁均匀地涂覆一层氮化硼,将浸渗剂装入石墨坩埚中;所述的浸渗剂由2份~6份的硅和2份~8份的金属材料混合组成;
二、将碳基体材料加工成欲浸渗的试样或产品形状,然后进行超声清洗,烘干;步骤一中所述的金属材料的氧化自由能低于步骤二中所述的碳基体材料的氧化自由能;
三、将装有浸渗剂的石墨坩埚放入气压浸渗炉中,将步骤二处理后的碳基体材料连接到气压浸渗炉中的提拉杆上;
四、关闭炉门,抽真空至1.0×10-3Pa以下,然后在升温速率为20℃/min~30℃/min的条件下加热至步骤一中的浸渗剂的熔点以上100℃~200℃,在升温的同时充入氩气至炉内压力为0.1个标准大气压~0.2个标准大气压;
五、在炉内压力为0.1个标准大气压~0.2个标准大气压和温度为浸渗剂的熔点以上100℃~200℃的条件下保温1h~1.5h,然后下降气压浸渗炉中的提拉杆将碳基体材料浸入融化的浸渗剂中,向炉内充入氩气至炉内压力为3MPa~10MPa,在炉内压力为3MPa~10MPa和温度为浸渗剂的熔点以上100℃~200℃的条件下保持1min~5min,然后升起提拉杆将碳基体材料从浸渗剂中提出,关闭加热电源,随炉自然冷却,即可获得碳基耗散防热复合材料。
本发明的复合材料由碳材料作为基体,在真空密闭的炉体内,通过加热将浸渗剂融化,然后将基体浸入熔融的浸渗剂中,向密闭的炉体内通入高压惰性气体,使浸渗剂浸入到基体中形成复合材料,获得一种近净成型的碳基耗散防热复合材料。本发明制备轻质耐烧蚀的耗散防热复合材料工艺简单、周期短、制造成本低。可用于制造固体火箭发动机喷管的喉衬、燃气舵,也可用于制造高超音速飞行器的端头帽、翼前缘、尾舵和用于制造导弹的转向孔板等构件。
本发明所涉及碳基耐烧蚀耗散防热复合材料制备工艺简单、周期短、复合材料可实现近净成型,也可进行电加工和机械加工,制造成本低、耐烧蚀性能好。
本发明的碳基耗散防热复合材料的密度为2g/cm3~2.5g/cm3;在氧乙炔烧蚀条件下烧蚀100s,线烧蚀率为0.9×10-3mm/s~1.2×10-3mm/s。
附图说明
图1为试验一中的气压浸渗炉的示意图。
具体实施方式
具体实施方式一:本实施方式为一种碳基耗散防热复合材料的制备方法,具体是按以下步骤进行的:
一、在石墨坩埚的内壁均匀地涂覆一层氮化硼,将浸渗剂装入石墨坩埚中;所述的浸渗剂由2份~6份的硅和2份~8份的金属材料混合组成;
二、将碳基体材料加工成欲浸渗的试样或产品形状,然后进行超声清洗,烘干;步骤一中所述的金属材料的氧化自由能低于步骤二中所述的碳基体材料的氧化自由能;
三、将装有浸渗剂的石墨坩埚放入气压浸渗炉中,将步骤二处理后的碳基体材料连接到气压浸渗炉中的提拉杆上;
四、关闭炉门,抽真空至1.0×10-3Pa以下,然后在升温速率为20℃/min~30℃/min的条件下加热至步骤一中的浸渗剂的熔点以上100℃~200℃,在升温的同时充入氩气至炉内压力为0.1个标准大气压~0.2个标准大气压;
五、在炉内压力为0.1个标准大气压~0.2个标准大气压和温度为浸渗剂的熔点以上100℃~200℃的条件下保温1h~1.5h,然后下降气压浸渗炉中的提拉杆将碳基体材料浸入融化的浸渗剂中,向炉内充入氩气至炉内压力为3MPa~10MPa,在炉内压力为3MPa~10MPa和温度为浸渗剂的熔点以上100℃~200℃的条件下保持1min~5min,然后升起提拉杆将碳基体材料从浸渗剂中提出,关闭加热电源,随炉自然冷却,即可获得碳基耗散防热复合材料。
具体实施方式二:本实施方式与具体实施方式一不同的是:步骤一中所述的金属材料为铝、钼、锆、铪、钽中的一种或几种的混合物。其他与具体实施方式一相同。
具体实施方式三:本实施方式与具体实施方式一或二不同的是:步骤二中所述的碳基体材料为石墨或低密度的C/C复合材料。其他与具体实施方式一或二相同。
具体实施方式四:本实施方式与具体实施方式三不同的是:步骤二中所述的低密度的C/C复合材料的密度为1.45/cm3~1.8g/cm3。其他与具体实施方式三相同。
具体实施方式五:本实施方式与具体实施方式一至四之一不同的是:步骤二中所述的碳基体材料的孔隙率为10%~35%。其他与具体实施方式一至四之一相同。
具体实施方式六:本实施方式与具体实施方式一至五之一不同的是:步骤二中所述的烘干的条件下为:烘干温度为80℃~100℃,烘干时间为2h~4h。其他与具体实施方式一至五之一相同。
用以下试验对本发明进行验证:
试验一:本试验为一种碳基耗散防热复合材料的制备方法,具体是按以下步骤进行的:
一、在石墨坩埚的内壁均匀地涂覆一层氮化硼,将浸渗剂装入石墨坩埚中;所述的浸渗剂由6份的硅、2份金属钼和1份金属铪混合组成;
二、将碳基体材料加工成欲浸渗的试样或产品形状,然后进行超声清洗,烘干;步骤一中所述的金属材料的氧化自由能低于步骤二中所述的碳基体材料的氧化自由能;
三、将装有浸渗剂的石墨坩埚放入气压浸渗炉中,将步骤二处理后的碳基体材料连接到气压浸渗炉中的提拉杆上;
四、关闭炉门,抽真空至0.8×10-3Pa,然后在升温速率为30℃/min的条件下加热至1800℃,在升温的同时充入氩气至炉内压力为0.2个标准大气压;
五、在炉内压力为0.2个标准大气压和温度为1800℃的条件下保温1.5h,然后下降气压浸渗炉中的提拉杆将碳基体材料浸入融化的浸渗剂中,向炉内充入氩气至炉内压力为8MPa,在炉内压力为8MPa和温度为1800℃的条件下保持1min,然后升起提拉杆将碳基体材料从浸渗剂中提出,关闭加热电源,随炉自然冷却,即可获得碳基耗散防热复合材料。
步骤二中所述的碳基体材料为石墨。
步骤二中所述的烘干的条件下为:烘干温度为100℃,烘干时间为2h。
本试验制备的耗散防热复合材料在氧乙炔烧蚀条件下烧蚀100s,线烧蚀率达到0.9×10-3mm/s。
本试验中的气压浸渗炉的示意图如图1所示,1为提拉杆,2为抽气阀门,3为炉体,4为浸渗剂,5为碳基体材料,6为石墨坩埚,7为充气阀门,8为熔炼炉。
试验二:本试验为一种碳基耗散防热复合材料的制备方法,具体是按以下步骤进行的:
一、在石墨坩埚的内壁均匀地涂覆一层氮化硼,将浸渗剂装入石墨坩埚中;所述的浸渗剂由4份的硅和6份的铝混合组成;
二、将碳基体材料加工成欲浸渗的试样或产品形状,然后进行超声清洗,烘干;步骤一中所述的金属材料的氧化自由能低于步骤二中所述的碳基体材料的氧化自由能;
三、将装有浸渗剂的石墨坩埚放入气压浸渗炉中,将步骤二处理后的碳基体材料连接到气压浸渗炉中的提拉杆上;
四、关闭炉门,抽真空至1.0×10-3Pa,然后在升温速率为30℃/min的条件下加热至1200℃,在升温的同时充入氩气至炉内压力为0.1个标准大气压;
五、在炉内压力为0.1个标准大气压和温度为1200℃的条件下保温1h,然后下降气压浸渗炉中的提拉杆将碳基体材料浸入融化的浸渗剂中,向炉内充入氩气至炉内压力为3MPa,在炉内压力为3MPa和温度为1200℃的条件下保持1min,然后升起提拉杆将碳基体材料从浸渗剂中提出,关闭加热电源,随炉自然冷却,即可获得碳基耗散防热复合材料。
步骤二中所述的碳基体材料为C/C复合材料,密度为1.73g/cm3,孔隙率为22%。
步骤二中所述的烘干的条件下为:烘干温度为80℃,烘干时间为2h。
本试验制备的耗散防热复合材料在氧乙炔烧蚀条件下烧蚀100s,线烧蚀率达到1.2×10-3mm/s。
Claims (6)
1.一种碳基耗散防热复合材料的制备方法,其特征在于碳基耗散防热复合材料的制备方法是按以下步骤进行的:
一、在石墨坩埚的内壁均匀地涂覆一层氮化硼,将浸渗剂装入石墨坩埚中;所述的浸渗剂由2份~6份的硅和2份~8份的金属材料混合组成;
二、将碳基体材料加工成欲浸渗的试样或产品形状,然后进行超声清洗,烘干;步骤一中所述的金属材料的氧化自由能低于步骤二中所述的碳基体材料的氧化自由能;
三、将装有浸渗剂的石墨坩埚放入气压浸渗炉中,将步骤二处理后的碳基体材料连接到气压浸渗炉中的提拉杆上;
四、关闭炉门,抽真空至1.0×10-3Pa以下,然后在升温速率为20℃/min~30℃/min的条件下加热至步骤一中的浸渗剂的熔点以上100℃~200℃,在升温的同时充入氩气至炉内压力为0.1个标准大气压~0.2个标准大气压;
五、在炉内压力为0.1个标准大气压~0.2个标准大气压和温度为浸渗剂的熔点以上100℃~200℃的条件下保温1h~1.5h,然后下降气压浸渗炉中的提拉杆将碳基体材料浸入融化的浸渗剂中,向炉内充入氩气至炉内压力为3MPa~10MPa,在炉内压力为3MPa~10MPa和温度为浸渗剂的熔点以上100℃~200℃的条件下保持1min~5min,然后升起提拉杆将碳基体材料从浸渗剂中提出,关闭加热电源,随炉自然冷却,即可获得碳基耗散防热复合材料。
2.根据权利要求1所述的一种碳基耗散防热复合材料的制备方法,其特征在于步骤一中所述的金属材料为铝、钼、锆、铪、钽中的一种或几种的混合物。
3.根据权利要求1所述的一种碳基耗散防热复合材料的制备方法,其特征在于步骤二中所述的碳基体材料为石墨或低密度的C/C复合材料。
4.根据权利要求1所述的一种碳基耗散防热复合材料的制备方法,其特征在于步骤二中所述的低密度的C/C复合材料的密度为1.45/cm3~1.8g/cm3。
5.根据权利要求1所述的一种碳基耗散防热复合材料的制备方法,其特征在于步骤二中所述的碳基体材料的孔隙率为10%~35%。
6.根据权利要求1所述的一种碳基耗散防热复合材料的制备方法,其特征在于步骤二中所述的烘干的条件下为:烘干温度为80℃~100℃,烘干时间为2h~4h。
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