CN108439985A - 一种耐烧蚀材料的制备方法 - Google Patents
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Abstract
本发明涉及一种耐烧蚀材料的制备方法。本发明包括以下步骤:1)由三维针刺编织法制备炭纤维预制体,其中在炭纤维预制体的炭纤维表面上另外沉积有碳界面层;所述碳界面层为通过化学气相沉积工艺在炭纤维表面上形成的热解炭;炭纤维表面沉积碳界面层后形成炭炭坯体;2)陶瓷相引入到炭炭坯体内,陶瓷相填充于炭炭坯体的内部空隙;陶瓷相为HfC陶瓷;所述陶瓷相是将炭炭坯体浸渍在HfC陶瓷先驱体溶液中并通过交联、固化、裂解后高温热处理而成。本发明中的制备工艺简单,过程可控,成本相对较低。制备的耐烧蚀材料在2500℃条件下烧蚀120s后,样品的质量和线烧蚀率分别为1.64mg/s和2.77μm/s。
Description
技术领域
本发明属于工程材料技术领域,涉及到一种耐烧蚀材料的制备方法。
背景技术
炭炭复合材料具有较低的密度,较高的热导率,以及优异的抗热震性能和良好的抗烧蚀性能,是一种理想的制备高温热端结构部件材料,近年来大量应用于航空、航天领域。但是在高温和高压气流环境下,炭炭复合材料会快速发生氧化和烧蚀,进而限制了其应用。为了提高炭炭复合材料在高温环境下的应用效能,近年来提出的提高抗烧蚀性能一个重要途径是引入难熔金属碳化物(ZrC、HfC)来提高炭炭复合材料的抗氧化能力、降低烧蚀率以及承受更高的燃气温度或更长的工作时间。
HfC具有优异的物理和化学性能,如高硬度、高熔点(3890℃)、固相稳定性、热力学稳定性和好的热震性,在一定温度下还具有高强度、耐磨性,热导率和导电能力,因此它是目前人们感兴趣的超高温材料之一。
目前主要是采用化学气相沉积(CVD)工艺将HfC陶瓷相引入到炭炭复合材料的体系内。CVD工艺制备的碳化铪改性C/C复合材料,虽然HfC涂层均匀性较好,结构易于控制,但是由于基体和涂层之间的结合属于物理吸附,两者之间的结合强度较低。先驱体浸渍裂解(PIP)工艺是一种制备炭炭复合材料极为有效的手段,便于制备形状复杂的大型件和异型件,引入到基体内的陶瓷颗粒能均匀的分散在炭炭复合材料的内部。
发明内容
本发明的目的是:提供一种耐烧蚀材料的制备方法。
本发明的技术方案是:一种耐烧蚀材料的制备方法,包括:
1)由三维针刺编织法制备炭纤维预制体,其中在炭纤维预制体的炭纤维表面上另外沉积有碳界面层;所述碳界面层为通过化学气相沉积工艺在炭纤维表面上形成的热解炭;炭纤维表面沉积碳界面层后形成炭炭坯体。
2)陶瓷相引入到炭炭坯体内,陶瓷相填充于炭炭坯体的内部空隙;陶瓷相为HfC陶瓷,优选陶瓷相是将炭炭坯体浸渍在HfC陶瓷先驱体溶液中并通过交联、固化、裂解后高温热处理而成。
进一步的,炭纤维表面沉积碳界面层后的炭炭坯体密度优选在0.8~1.6g/cm3之间。
进一步的,所述化学气相沉积工艺的过程为:以丙烯为碳源气体,采用等温化学气相沉积工艺在炭纤维预制体表面沉积热解炭界面层,沉积温度为1020~1030℃,总压为3~5KPa,丙烯气体流量为4~6L/min,沉积时间为40~320h。
进一步的,所述炭炭坯体浸渍在HfC陶瓷先驱体溶液中,其步骤为:将沉积有碳界面层的炭炭坯体置入真空浸渍装置内,缓慢加入HfC陶瓷相先驱体浸渍液,装置真空度控制在0.5KPa以下,浸渍时间为60~90min。
进一步的,所述交联固化,其过程为:将浸渍后的样品转移至烘箱中,烘箱温度调节为180~200℃,干燥8~10小时,气氛为大气环境下。
进一步的,所述裂解处理,其过程为:将交联、固化后的样品置入热处理炉中,调节升温速率为5~8℃/min,氩气氛围保护下升温至1700~1800℃,保温时间为3~4h,随炉冷却至室温。
本发明的有益效果是:本发明耐烧蚀材料的制备方法,利用化学气相沉积法对碳纤维预制体进行增密,采用先驱体浸渍裂解法(PIP)对C/C复合材料进行基体改性,将具有优异耐烧蚀组元的HfC陶瓷相引入到C/C复合材料体系内,通过PIP工艺将HfC陶瓷相均匀的引入到炭炭复合材料基体内部,有效解决了炭炭复合材料在高温下应用的难题。本发明中的制备工艺简单,过程可控,成本相对较低。制备的耐烧蚀材料在2500℃条件下烧蚀120s后,样品的质量和线烧蚀率分别为1.64mg/s和2.77μm/s。
附图说明
图1为烧蚀前C/C-HfC复合材料截面微观形貌图;
图2为烧蚀后C/C-HfC复合材料无纬布层微观形貌图;
图3为烧蚀后C/C-HfC复合材料网胎层微观形貌图。
具体实施方式
下面结合附图和具体实施例对本发明进一步进行描述。本领域技术人员应当理解,以下举例示出的实施例仅用于解释本发明而非用于对其作出任何限制。比如:下面描述的各步骤的顺序并非唯一和不可改变的,只要其符合正常的逻辑顺序而能够实施本发明即可。
实施例1
采用炭纤维针刺毡预制体。以丙烯为碳源气体,采用化学气相沉积工艺,在预制体的炭纤维表面沉积热解炭层。具体条件如下:沉积温度为1020-1030℃,压力为3-5KPa,丙烯流量为4-6L/min,沉积时间为40-50h,沉积后样品的密度为0.8g/cm3。将沉积有炭界面层的炭纤维预制体置入真空浸渍装置内,缓慢加入HfC陶瓷相先驱体浸渍液,真空度控制在0.5KPa以下,浸渍时间为60-90min之间。将浸渍后的样品转移至烘箱中,烘箱温度调节为180-200℃,干燥8-10小时,气氛为大气环境下,将交联固化后的样品置入热处理炉中,调节升温速率为5-8℃/min,氩气氛围保护下升温至1700-1800℃,保温时间为3-4h,随炉冷却至室温。利用酒精将陶瓷化后的样品进行超声清洗,而后进行烘干。重复上述浸渍、交联固化、裂解处理,样品最终体积密度为2.12g/cm3。
实施例2
采用炭纤维针刺毡预制体。以丙烯为碳源气体,采用化学气相沉积工艺,在预制体的炭纤维表面沉积热解炭层。具体条件如下:沉积温度为1020-1030℃,压力为3-5KPa,丙烯流量为4-6L/min,沉积时间为80-90h,沉积后样品的密度为1.0g/cm3。将沉积有碳界面层的炭纤维预制体置入真空浸渍装置内,缓慢加入HfC陶瓷相先驱体浸渍液,真空度控制在0.5KPa以下,浸渍时间为60-90min之间。将浸渍后的样品转移至烘箱中,烘箱温度调节为180-200℃,干燥8-10小时,气氛为大气环境下,将交联固化后的样品置入热处理炉中,调节升温速率为5-8℃/min,氩气氛围保护下升温至1700-1800℃,保温时间为3-4h,随炉冷却至室温。利用酒精将陶瓷化后的样品进行超声清洗,而后进行烘干。重复上述浸渍、交联固化、裂解处理,样品最终体积密度为2.09g/cm3。
实施例3
采用炭纤维针刺毡预制体。以丙烯为碳源气体,采用化学气相沉积工艺,在预制体的炭纤维表面沉积热解炭层。具体条件如下:沉积温度为1020-1030℃,压力为3-5KPa,丙烯流量为4-6L/min,沉积时间为130-140h,沉积后样品的密度为1.2g/cm3。将沉积有碳界面层的炭纤维预制体置入真空浸渍装置内,缓慢加入HfC陶瓷相先驱体浸渍液,真空度控制在0.5KPa以下,浸渍时间为60-90min之间。将浸渍后的样品转移至烘箱中,烘箱温度调节为180-200℃,干燥8-10小时,气氛为大气环境下,将交联固化后的样品置入热处理炉中,调节升温速率为5-8℃/min,氩气氛围保护下升温至1700-1800℃,保温时间为3-4h,随炉冷却至室温。利用酒精将陶瓷化后的样品进行超声清洗,而后进行烘干。重复上述浸渍、交联固化、裂解处理,样品最终体积密度为2.07g/cm3。
实施例4
采用炭纤维针刺毡预制体。以丙烯为碳源气体,采用化学气相沉积工艺,在预制体的炭纤维表面沉积热解炭层。具体条件如下:沉积温度为1020-1030℃,压力为3-5KPa,丙烯流量为4-6L/min,沉积时间为210-220h,沉积后样品的密度为1.4g/cm3。将沉积有碳界面层的炭纤维预制体置入真空浸渍装置内,缓慢加入HfC陶瓷相先驱体浸渍液,真空度控制在0.5KPa以下,浸渍时间为60-90min之间。将浸渍后的样品转移至烘箱中,烘箱温度调节为180-200℃,干燥8-10小时,气氛为大气环境下,将交联固化后的样品置入热处理炉中,调节升温速率为5-8℃/min,氩气氛围保护下升温至1700-1800℃,保温时间为3-4h,随炉冷却至室温。利用酒精将陶瓷化后的样品进行超声清洗,而后进行烘干。重复上述浸渍、交联固化、陶瓷化处理,样品最终体积密度为2.03g/cm3。
实施例5
采用炭纤维针刺毡预制体。以丙烯为碳源气体,采用化学气相沉积工艺,在预制体的炭纤维表面沉积热解炭层。具体条件如下:沉积温度为1020-1030℃,压力为3-5KPa,丙烯流量为4-6L/min,沉积时间为310-320h,沉积后样品的密度为1.6g/cm3。将沉积有碳界面层的炭纤维预制体置入真空浸渍装置内,缓慢加入HfC陶瓷相先驱体浸渍液,真空度控制在0.5KPa以下,浸渍时间为60-90min之间。将浸渍后的样品转移至烘箱中,烘箱温度调节为180-200℃,干燥8-10小时,气氛为大气环境下,将交联固化后的样品置入热处理炉中,调节升温速率为5-8℃/min,氩气氛围保护下升温至1700-1800℃,保温时间为3-4h,随炉冷却至室温。利用酒精将陶瓷化后的样品进行超声清洗,而后进行烘干。重复上述浸渍、交联固化、陶瓷化处理,样品最终体积密度为1.95g/cm3。
图1为通过先驱体浸渍裂解工艺制备的耐烧蚀复合材料截面的微观形貌图。从图中可知,HfC陶瓷相填充于纤维之间的孔隙内,且HfC陶瓷颗粒均匀的分散于材料内部,其中黑色相为炭纤维和热解碳,白色相为HfC陶瓷相。在本发明中的改性C/C复合材料中,炭纤维起到增强增韧的作用,碳化铪陶瓷相均匀地分布于材料的内部。
图2为烧蚀后C/C-HfC复合材料无纬布层微观形貌图。从图中可见试样经等离子体火焰的烧蚀与冲刷后,原先包裹在纤维周围的基体炭和陶瓷相都已脱落,纤维呈“楔形”状。该区域内纤维上的陶瓷含量相对较少,因此该区域的烧蚀相对较为严重。引入的HfC发生氧化反应生成二氧化铪颗粒物,等离子体火焰强大的冲刷能力,将这些颗粒不断地吹向中心区的两侧,该烧蚀区域内只能观察到少量的白色固体颗粒物。
图3为烧蚀后C/C-HfC复合材料网胎层微观形貌图。该层由大量的短炭纤维组成,陶瓷含量较高。烧蚀后纤维之间生产大量的颗粒物质,其由两部分组成,一方面,该区域内碳化铪含量较高发生氧化后生成的二氧化铪颗粒比较多,大多都填充于纤维之间;另一方面,无纬布层中生成的二氧化铪颗粒物受到等离子体火焰强大的冲刷能力,这些颗粒物质不断地流动和堆积到该区域。因此,我们可以从图中观察到该区域内存在大量的白色颗粒物质。
Claims (6)
1.一种耐烧蚀材料的制备方法,其特征为所述制备方法包括以下步骤:
1)由三维针刺编织法制备炭纤维预制体,其中在炭纤维预制体的炭纤维表面上另外沉积有碳界面层;所述碳界面层为通过化学气相沉积工艺在炭纤维表面上形成的热解炭;炭纤维表面沉积碳界面层后形成炭炭坯体;
2)陶瓷相引入到炭炭坯体内,陶瓷相填充于炭炭坯体的内部空隙;陶瓷相为HfC陶瓷;所述陶瓷相是将炭炭坯体浸渍在HfC陶瓷先驱体溶液中并通过交联、固化、裂解后高温热处理而成。
2.根据权利要求1所述的制备方法,其特征为:所述炭纤维表面沉积碳界面层后的炭炭坯体密度在0.8~1.6g/cm3之间。
3.根据权利要求1所述的制备方法,其特征为:所述化学气相沉积工艺的过程为:以丙烯为碳源气体,采用等温化学气相沉积工艺在炭纤维预制体表面沉积热解炭界面层,沉积温度为1020~1030℃,总压为3~5KPa,丙烯气体流量为4~6L/min,沉积时间为40~320h。
4.根据权利要求1所述的制备方法,其特征为:所述炭炭坯体浸渍在HfC陶瓷先驱体溶液中,其步骤为:将沉积有碳界面层的炭炭坯体置入真空浸渍装置内,缓慢加入HfC陶瓷相先驱体浸渍液,装置真空度控制在0.5KPa以下,浸渍时间为60~90min。
5.根据权利要求1所述的制备方法,其特征为:所述交联固化,其过程为:将浸渍后的样品转移至烘箱中,烘箱温度调节为180~200℃,干燥8~10小时,气氛为大气环境下。
6.根据权利要求1所述的制备方法,其特征为:所述裂解处理,其过程为:将交联、固化后的样品置入热处理炉中,调节升温速率为5~8℃/min,氩气氛围保护下升温至1700~1800℃,保温时间为3~4h,随炉冷却至室温。
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