CN111960863A - 一种超高温耐腐蚀复合材料及其制备方法 - Google Patents
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Abstract
本发明涉及复合材料技术领域,具体公开了一种超高温耐腐蚀复合材料及其制备方法,包括复合材料基体,所述复合材料基体上依次沉积有粘接层和陶瓷层,所述陶瓷层为稀土钽酸盐(RETaO4)或稀土铌酸盐(RENbO4)的一种或两种按比例混合。本发明制备的复合材料可适应多种恶劣腐蚀环境,能够有效延长C/C、SiC/SiC、C/C‑SiC等复合材料的服役时间,这大大减少了因腐蚀造成的材料与能源的浪费,开源节流。
Description
技术领域
本发明涉及复合材料技术领域,特别涉及一种超高温耐腐蚀复合材料及其制备方法。
背景技术
C/C、SiC/SiC、C/C-SiC等复合材料由于具有密度低、比强度高、耐磨性好、抗腐蚀性优良,并兼有优异的力学性能和热物理性能等特点,被广泛应用航空航天、汽车工业、医学等领域。其中,C/C复合材料是目前极少数可在2000℃以上保持较高力学性能的材料之一,它具有热膨胀系数较低、耐热冲击、耐烧蚀、耐含固体微粒燃气的冲刷等优异性能,尤其是这种材料的强度随温度的升高不降反升的独特性能,因此被认为是最有前途的高温材料之一,其作为航空航天等高技术领域热结构件使用具有其它材料难以比拟的优势,被广泛应用于高性能固体火箭发动机(SRM)喷管及其喉衬、航天飞机的端头帽和机翼前缘的热防护系统、飞机刹车盘等。
但C/C复合材料在高温环境下有个极大的弱点,即在温度超过400℃的有氧环境下容易发生氧化反应,这一劣势极大的限制了其发展,若无抗氧化措施,在高温氧化环境中长时间使用C/C复合材料必将引起灾难性后果;另外SiC/SiC复合材料、C/C-SiC复合材料也都存在这因热导率较高且在有氧高温气氛中易被氧化,限制了它的后续发展应用,因此要如何解决C/C、SiC/SiC、C/C-SiC等复合材料在高温有氧环境下的耐腐蚀和低热导率的问题是目前该复合材料领域研究的重点方向。
发明内容
本发明提供了一种超高温耐腐蚀复合材料及其制备方法,以解决现有技术中C/C、SiC/SiC、C/C-SiC等复合材料在高温有氧环境下的容易氧化腐蚀和热导率高的问题。
为了达到上述目的,本发明的技术方案为:
一种超高温耐腐蚀复合材料及,包括复合材料基体,所述复合材料基体上依次沉积有粘接层和陶瓷层,所述陶瓷层为稀土钽酸盐(RETaO4)或稀土铌酸盐(RENbO4)的一种或两种按比例混合。
本技术方案的技术原理和效果在于:
1、本方案中的技术方案通过在复合材料基体表面沉积陶瓷层,大幅度降低了其热导率,使其基体能够在长时间保持在低温状态下,同时由于陶瓷涂层的致密性高,高温环境中的氧气难以穿透,从而使其高温耐腐蚀性能得到提升。
2、本方案中陶瓷层采用稀土钽酸盐或稀土铌酸盐,其具有热导低、热膨胀系数高、耐腐蚀、抗氧化等特点,低热导能够降低热量的传输,使复合材料基底表面温度显著降低,高热膨胀系数的陶瓷层能够与粘结层热膨胀系数相匹配,避免因热应力失配而使涂层产生裂纹甚至脱落,陶瓷层耐腐蚀的特性能够有效解决因高温环境产生的熔融盐、CMAS等腐蚀基体导致基体失效的问题,延长复合材料基体使用寿命,陶瓷层能够隔绝环境中水蒸气、氧气等氧化介质与复合材料基体接触,增强复合材料基体的抗氧化能力。
3、本发明制备的复合材料可适应多种恶劣腐蚀环境,能够有效延长C/C、SiC/SiC、C/C-SiC等复合材料的服役时间,这大大减少了因腐蚀造成的材料与能源的浪费,开源节流。
进一步,所述复合材料基体为C/C、SiC/SiC或C/SiC。
有益效果:本申请中的涂层能够对提高上述三种复合材料的耐高温腐蚀能力。
进一步,所述粘结层的成分为MCrAlY,所述MCrAlY为NiCrAlY、NiCoCrAlY、CoNiCrAlY或CoCrAlY。
有益效果:上述粘接层的成分均为常用的粘接剂。
本申请还公开了一种超高温耐腐蚀复合材料的制备方法,包括以下步骤:
步骤1:采用PS-PVD在复合材料基体上沉积粘结层,厚度为100~150μm;
步骤2:采用APS在粘结层的表面沉积陶瓷层,厚度100~150μm。
有益效果:采用本方法制备得到了耐高温腐蚀的复合材料。
进一步,所述步骤1中,在沉积粘结层之前,去除复合材料基体表面的油污。
有益效果:去除油污能够提高复合材料表面的粘接性能。
进一步,对去除油污的复合材料基体的表面进行喷丸处理,使得复合材料基体的表面粗糙度为60~100μm。
有益效果:喷丸处理能够提高复合材料基体的强度,同时提高其与粘接层之间的连接稳定性。
具体实施方式
下面通过具体实施方式进一步详细说明:
实施例1:
一种超高温耐腐蚀复合材料,包括C/C复合材料基体,在C/C复合材料基体上依次沉积有粘接层和陶瓷层,本实施例1中粘接层的成分为NiCrAlY,陶瓷层的成分为YTaO4。
其中稀土钽酸盐(RETaO4)或铌酸盐(RENbO4)的制备方法,包括以下步骤:
步骤1:将RE2O3、Ta2O5或Nb2O5按照摩尔比为1:1加入到球磨机中进行球磨,球磨机的转速为300r/min,球磨后进行干燥过筛得到粉末A。
步骤2:将步骤1干燥过筛后的粉末A采用高温固相反应法制得成分RETaO4/RENbO4的粉末B,反应温度为1700℃,反应时间为10h;并采用300目的筛子对粉末B进行过筛。
步骤3:将步骤2中过筛后的粉末B与去离子水溶剂、有机粘接剂混合得到浆料C,其中浆料C中粉末B的质量百分比为25%,有机粘接剂的质量百分比为2%,其余为溶剂,有机粘接剂采用聚乙烯醇或者阿拉伯树胶;再利用离心雾化法对浆料C进行干燥,干燥时的温度为600℃,离心速度为8500r/min,得到干燥的料粒D;
步骤4:将步骤3得到的料粒D在1200℃的温度下烧结8h,再采用300目的筛子对烧结后的料粒D过筛,得到粒径为10~70nm并且形貌呈球形的RETaO4/RENbO4陶瓷粉体。
上述超高温耐腐蚀复合材料的制备方法,包括以下步骤:
步骤1:将C-C复合材料基体表面进行除油除污,获得干净的基体表面,随后进行喷砂处理,获得60~100μm的粗糙度,提高基体与涂层的结合强度,喷砂操作时采用粒径0.5mm的铁砂;通过PS-PVD在基体上沉积一层成分为NiCrAlY的粘结层,厚度为100μm。
步骤2:利用APS在粘结层的表面沉积一层稀土钽酸盐YTaO4陶瓷层,增强基底耐高温耐腐蚀抗氧化能力,厚度100μm。
实施例2~17:
与实施例1的区别在于,复合材料基体与各涂层的成分或厚度不同,具体见下表1~2所示。
表1为实施例2~9各涂层的成分与厚度表(表中“--”表示不含有)
表2为实施例10~17各涂层的成分与厚度表(表中“--”表示不含有)
实施例18:
与实施例1的区别在于,陶瓷层成分包括YTaO4和SmTaO4,且两种粉末的配比为各自的体积分数分别为50%。
实施例19:
与实施例1的区别在于,陶瓷层的成分包括YTaO4、SmTaO4、NdNbO4和DyNbO4,且四种粉末的配比为各自的体积分数为25%。
实施例20:
与实施例19的区别在于,4种稀土钽/铌酸盐在粘接层上形成梯度涂层,涂层梯度n=11,第1层指与粘接层直接接触的涂层,每一层按照表3所示进行成分配比,再依次沉积到粘接层上,沉积的总厚度为100μm,配比的要求为:4种稀土钽/铌酸盐中至少有一种以上的体积分数是连续递增或递减变化的。
表3为实施例19中各梯度层稀土钽/铌酸盐的体积分数表(体积分数%)
对比例1:
与实施例17的区别在于,本对比例中在粘接层的外部沉积了两层稀土钽酸盐,依次为YTaO4和SmTaO4,两层稀土钽酸盐的总厚度为100μm。
选取实施例1~19、对比例1得到的合金材料试样进行热导率实验检测:
采用激光热导仪进行测试,在700K温度时,以实施例1~3、实施例10~12、实施例18~20与对比例1的测试结果为例,如下表4所示。
表4为实施例1~3、10~12、18~20与对比例1的热导率
从上表4可以得出:
1、采用本申请中的技术方案通过在复合材料基体表面沉积陶瓷涂层,大幅度降低了其热导率,使其基体能够在长时间保持在低温状态下,同时由于陶瓷涂层的致密性高,高温环境中的氧气难以穿透,从而使其高温耐腐蚀性能得到提升。
2、实施例18和19通过将陶瓷涂层设计为多种稀土钽或铌酸盐的物理混合,再进行沉积,以这样的方式得到的复合陶瓷涂层发现其热导率出现大幅度的下降,原因在于,物理混合的多种陶瓷粉体在形成涂层时,不同成分之间不会存在明显的界面,使得涂层中界面效应消失,而相比于传统(对比例1)的方式,不同稀土钽或铌酸盐成分之间是存在明显的界面的,因此对比例1的热导率虽然要略低于实施例1,但依旧要远高于实施例17。
3、实施例20通过对多种稀土钽/铌酸盐陶瓷粉体进行设计,得到多元梯度涂层,即涂层中至少一种粉体的体积分数是在连续变化,这样的方式能够使其热导率进一步下降,原因在于采用这样的方式进行沉积得到的陶瓷涂层,各梯度涂层之间成分呈渐变的形式,各梯度涂层之间形成的界面少,使得界面效应弱,同时最重要的一点在于,在各梯度涂层沉积过程中,每一层的成分还会不断的扩散,使得界面效应继续减弱,从而使得热导率下降,因此实施例20相比与实施例19而言,其热导率要低一些,但是实施例20这样沉积的方式在操作上比实施例19难一些,因此需要结合生产实际选择最佳的制备方法。
以上所述的仅是本发明的实施例,方案中公知的具体材料及特性等常识在此未作过多描述。应当指出,对于本领域的技术人员来说,在不脱离本发明的前提下,还可以作出若干变形和改进,这些也应该视为本发明的保护范围,这些都不会影响本发明实施的效果和专利的实用性。本申请要求的保护范围应当以其权利要求的内容为准,说明书中的具体实施方式等记载可以用于解释权利要求的内容。
Claims (6)
1.一种超高温耐腐蚀复合材料,其特征在于:包括复合材料基体,所述复合材料基体上依次沉积有粘接层和陶瓷层,所述陶瓷层为稀土钽酸盐(RETaO4)或稀土铌酸盐(RENbO4)的一种或两种按比例混合。
2.根据权利要求1所述的一种超高温耐腐蚀复合材料,其特征在于:所述复合材料基体为C/C、SiC/SiC或C/SiC。
3.根据权利要求1所述的一种超高温耐腐蚀复合材料,其特征在于:所述粘结层的成分为MCrAlY,所述MCrAlY为NiCrAlY、NiCoCrAlY、CoNiCrAlY或CoCrAlY。
4.一种制备如权利要求1所述的超高温耐腐蚀复合材料的方法,其特征在于:包括以下步骤:
步骤1:采用PS-PVD在复合材料基体上沉积粘结层,厚度为100~150μm;
步骤2:采用APS在粘结层的表面沉积陶瓷层,厚度100~150μm。
5.根据权利要求4所述的一种超高温耐腐蚀复合材料的制备方法,其特征在于:所述步骤1中,在沉积粘结层之前,去除复合材料基体表面的油污。
6.根据权利要求5所述的一种超高温耐腐蚀复合材料的制备方法,其特征在于:对去除油污的复合材料基体的表面进行喷丸处理,使得复合材料基体的表面粗糙度为60~100μm。
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