CN107299345A - 一种SiCf/SiC复合材料导向器叶片的环境防护涂层及其制备方法 - Google Patents
一种SiCf/SiC复合材料导向器叶片的环境防护涂层及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,包括:SiCf/SiC复合材料导向器叶片基体预热,等离子喷涂—物理气相沉积(PS‑PVD)依次制备Si粘结层、莫来石过渡层、Yb2SiO5环境障层、La2Zr2O7热障层,环境防护涂层可用于1400~1700℃的燃气环境。本发明中的Si粘结层、莫来石过渡层、Yb2SiO5环境障层和La2Zr2O7热障层在同一个设备上完成;通过PS‑PVD喷枪加热有效控制基体温度,防止莫来石过渡层沉积过程中发生非晶反应;新增热障层使得环境防护涂层可适应1400~1700℃燃气环境,适用于高性能导向器叶片环境防护涂层的制备。本发明具有如下优点:制备过程简单,易操作,稳定性好,温度适用范围广以及应用范围广。
Description
技术领域
本发明涉及表面工程领域,具体主要涉及一种SiCf/SiC复合材料导向器叶片的环境防护涂层及其制备方法。
背景技术
未来四代航空发动机的导向器叶片将广泛采用SiCf/SiC复合材料。但是,在航空发动机热端部件服役环境中,SiCf/SiC必须面临苛刻的使用环境,包括高温、高压、高应力、氧化气氛与腐蚀气氛等,其中SiC氧化生成的SiO2与水蒸气反应产生挥发性的Si(OH)X,加速了基体材料的氧化,导致复合材料的性能急剧下降,过早失效,因此,必须在复合材料表面制备环境防护涂层来改善其环境使用性能,提高零件的服役寿命。
传统的环境防护涂层主要由硅/莫来石/稀土硅酸镱(Si/莫来石/Yb2SiO5)三层组成,该涂层体系已基本满足1400℃燃气环境中的长期使用。但是,不能满足1400℃以上的长期使用要求,进一步限制了传统环境防护涂层在航空发动机复合材料导向器叶片上的应用。
环境防护涂层主要制备方法有等离子喷涂法、浆料浸渍法。等离子喷涂法可以获得致密、结合强度高的涂层,并在多领域获得实际应用。随着等离子喷涂技术的快速发展,一种新型的涂层制备技术在热障涂层领域出现,该涂层制备技术称为等离子喷涂~物理气相沉积(PS-PVD)。PS-PVD是在物理气相沉积与等离子喷涂方法的基础上发展起来的新型涂层制备方法,可通过气相、液相与固相共沉积,可实现不同组织结构的复合设计。用PS-PVD制备环境防护涂层可以实现粘结层、过渡层、环境障层和热障层的一次制备,涂层组织结构设计性强等独特的优点。目前,并未有公开报道采用PS-PVD制备Si/莫来石/Yb2SiO5/La2Zr2O7环境防护涂层的相关文献及专利。
发明内容
本发明的目的在于克服现有技术的不足,提供一种SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,解决了传统环境保护涂层不能在1400℃以上的燃气环境中长期使用的问题。
本发明一种SiCf/SiC复合材料导向器叶片的环境防护涂层,以确保航空发动机的SiCf/SiC复合材料导向器叶片在1400℃以上燃气环境中长期使用,由里向外依次包括Si粘结层、莫来石过渡层、Yb2SiO5环境障层和La2Zr2O7热障层。
进一步的,上述一种SiCf/SiC复合材料导向器叶片的环境防护涂层,所述Si粘结层的制备原料为硅粉,其纯度≥99.99%,粉末粒度为5~38μm;所述莫来石过渡层由22.0~28.0wt%的SiO2粉末与 72.0~78.0wt%的Al2O3粉末混合制备而成,混合粉末粒度为5~38μm;所述Yb2SiO5环境障层的制备原料为Yb2SiO5粉,其纯度≥99.99%,粉末粒度为5~38μm;所述La2Zr2O7热障层的制备原料为La2Zr2O7粉末,其纯度≥99.99%,粉末粒度为5~38μm。
本发明还提供一种SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法。
本发明SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,依次包括:
Si粘结层制备,采用喷涂设备在叶片表面喷涂制作Si粘结层;
莫来石过渡层制备,采用喷涂设备在Si粘结层外喷涂制作莫来石过渡层;
Yb2SiO5环境障层制备,采用喷涂设备在莫来石过渡层外喷涂制作Yb2SiO5环境障层;
La2Zr2O7热障层制备,采用喷涂设备在Yb2SiO5环境障层外喷涂制作La2Zr2O7热障层。
进一步的,上述SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,所述的喷涂设备为等离子喷涂—物理气相沉积设备,所述的等离子喷涂—物理气相沉积设备通过气相、液相与固相共沉积,实现不同组织结构的复合设计。
进一步的,上述SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,还包括在制备Si粘结层前,对SiCf/SiC复合材料导向器叶片基体进行预热处理,预热温度为1000~1200℃。
进一步的,上述SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,所述Si粘结层的喷涂工艺参数为:真空度为150~200Pa,工作电流为2000~2200A,氩气流量为60~65L/min,氦气流量为50~55L/min,送粉量为5 ~6g/min,喷涂距离为1000~1200mm,喷涂厚度为20~50μm,喷涂5~7次。
进一步的,上述SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,所述莫来石过渡层的喷涂工艺参数为:真空度150~200Pa,工作电流为2500~2700A,氩气流量为60~65L/min,氦气流量为60~65L/min,送粉量为5~6g/min,喷涂距离为400~450mm,喷涂厚度为20~50μm,喷涂7~9次。
进一步的,上述SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,所述Yb2SiO5环境障层的喷涂工艺参数为:真空度150~200Pa,工作电流为2000~2200A,氩气流量为60~65L/min,氦气流量为60~65L/min,送粉量为5~6g/min,喷涂距离为400~450mm,喷涂厚度为50~150μm,喷涂18~22次。
进一步的,上述SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,所述La2Zr2O7热障层的喷涂工艺参数为:真空度为150~200Pa,工作电流为2000~2200A,氩气流量为70~75L/min,氦气流量为70~75L/min,送粉量为10~15g/min,喷涂距离为1000~1100mm,喷涂厚度为50~150μm,喷涂15~17次。
本发明的有益效果是:在传统环境防护涂层中新增La2Zr2O7热障层,使其在1400~1700℃的燃气冲刷试验持续1000h涂层无失效,适用于高性能导向器叶片环境防护涂层的制备;PS-PVD工艺可调范围广,组织结构变化多样,通过工艺参数的调整,可以在同一个设备上完成硅粘结层、莫来石过渡层、环境障层和热障层的制备;PS-PVD通过喷枪加热可以有效控制基体温度,在制备莫来石涂层的沉积过程中可有效防止发生非晶反应,提高涂层的使用寿命;PS-PVD具有非视线工艺性,可以更方便应用于制备航空发动机导向器叶片等复杂零件的喷涂。本发明具有制备过程简单、易操作、稳定性好、温度适用范围广以及应用范围广的优点。
附图说明
图1为环境防护涂层示意图;
图2为环境防护涂层燃气冲刷前的扫描电镜微观组织形貌图;
图3为环境防护涂层燃气冲刷后的扫描电镜微观组织形貌图;
图中,1-La2Zr2O7热障层,2-Yb2SiO5环境障层,3-莫来石过渡层,4-Si粘结层,5-SiCf/SiC复合材料导向器叶片基体。
具体实施方式
下面结合具体实施例进一步详细描述本发明的技术方案,但本发明的保护范围不局限于以下所述。
实施例1
某型航空发动机SiCf/SiC复合材料导向器叶片5,长度为600 mm,宽度为200 mm,厚度为10 mm。采用本发明提供的方法制备Si粘结层4/莫来石过渡层3/Yb2SiO5环境障层2/La2Zr2O7热障层1,该涂层由粘结层、过渡层、环境障层和热障层组成,均采用PS-PVD设备。首先采用喷枪对基体进行预热,预热温度为1000℃,然后按照以下四步进行涂层的制备。
步骤1:制备Si粘结层4
粉末原料为高纯度硅粉,纯度为99.99%,粉末粒度为5~38μm;喷涂速度1000 mm/s,喷涂5次,涂层厚度达到20μm;Si粘结层的喷涂工艺参数为:真空度为150Pa,工作电流为2000A,氩气流量为60 L/min,氦气流量为50L/min,送粉量为5g/min,喷涂距离为1000mm。
步骤2:制备莫来石过渡层3
在步骤1制备完Si粘结层后,在Si粘结层上随即制备莫来石过渡层,莫来石化学成分:SiO2重量百分比为25.0 %、Al2O3为余量,粉末粒度为5~38μm,喷涂速度1000 mm/s, 喷涂8次,喷涂厚度为35μm;莫来石过渡层喷涂工艺参数为:真空度为170 Pa,工作电流为2600 A,氩气流量为63 L/min,氦气流量为63 L/min,送粉量为5.5g/min,喷涂距离为420 mm。
步骤3:制备Yb2SiO5环境障层2
在步骤2喷涂完莫来石过渡层后,在莫来石过渡层上随即喷涂Yb2SiO5环境障层,纯度≥99.99%,粉末粒度为5~38μm,喷涂速度1000 mm/s,喷涂22次,喷涂厚度为150μm;Yb2SiO5环境障层喷涂工艺参数为:真空度为200Pa,工作电流为2200A,氩气流量为65 L/min,氦气流量为65L/min,送粉量为6g/min,喷涂距离为450mm。
步骤4:制备La2Zr2O7热障层1
在步骤3喷涂完Yb2SiO5环境障层后,随即喷涂La2Zr2O7热障层,粉末纯度≥99.99%,粒度为5~38μm,喷涂速度1000 mm/s,喷涂17次,喷涂厚度为150μm;La2Zr2O7热障层喷涂工艺参数为:真空度为200Pa,工作电流为2200 A,氩气流量为75L/min,氦气流量为75L/min,送粉量为15g/min,喷涂距离为1100mm,零件旋转速度为15r/min。
实施例2
某型航空发动机SiCf/SiC复合材料导向器叶片5,长度为600 mm,宽度为200 mm,厚度为10 mm。采用本发明提供的方法制备Si粘结层4/莫来石过渡层3/Yb2SiO5环境障层2/La2Zr2O7热障层1,该涂层由粘结层、过渡层、环境障层和热障层组成,均采用PS-PVD设备。首先采用喷枪对基体进行预热,预热温度为1090℃,然后按照以下四步进行涂层的制备。
步骤1:制备Si粘结层4
粉末原料为高纯度硅粉,纯度为99.99%,粉末粒度为5~38μm;喷涂速度1000 mm/s,喷涂7次,涂层厚度达到50μm;Si粘结层的喷涂工艺参数为:真空度为200Pa,工作电流为2200A,氩气流量为65L/min,氦气流量为55L/min,送粉量为6g/min,喷涂距离1000mm。
步骤2:制备莫来石过渡层3
在步骤1制备完Si粘结层后,在Si粘结层上随即制备莫来石过渡层,莫来石化学成分:SiO2重量百分比为22.0 %、Al2O3为余量,粉末粒度为5~38μm,喷涂速度1000mm/s, 喷涂5次,喷涂厚度为20μm;莫来石过渡层喷涂工艺参数为:真空度为150Pa,工作电流为2500A,氩气流量为60L/min,氦气流量为60L/min,送粉量为5g/min,喷涂距离为400mm。
步骤3:制备Yb2SiO5环境障层2
在步骤2喷涂完莫来石过渡层后,在莫来石过渡层上随即喷涂Yb2SiO5环境障层,纯度≥99.99%,粉末粒度为5~38μm,喷涂速度1000mm/s,喷涂18次,喷涂厚度为50μm;Yb2SiO5环境障层喷涂工艺参数为:真空度为150Pa,工作电流为2000A,氩气流量为60L/min,氦气流量为60L/min,送粉量为5g/min,喷涂距离为400mm。
步骤4:制备La2Zr2O7热障层1
在步骤3喷涂完Yb2SiO5环境障层后,随即喷涂La2Zr2O7热障层,粉末纯度≥99.99%,粒度为5~38μm,喷涂速度1000 mm/s,喷涂16次,喷涂厚度为107μm;La2Zr2O7热障层喷涂工艺参数为:真空度为176Pa,工作电流为2100 A,氩气流量为72L/min,氦气流量为73L/min,送粉量为13g/min,喷涂距离为1060mm,零件旋转速度为15r/min。
实施例3
某型航空发动机SiCf/SiC复合材料导向器叶片5,长度为600 mm,宽度为200 mm,厚度为10 mm。采用本发明提供的方法制备Si粘结层4/莫来石过渡层3/Yb2SiO5环境障层2/La2Zr2O7热障层1,该涂层由粘结层、过渡层、环境障层和热障层组成,均采用PS-PVD设备。首先采用喷枪对基体进行预热,预热温度为1200℃,然后按照以下四步进行涂层的制备。
步骤1:制备Si粘结层4
粉末原料为高纯度硅粉,纯度为99.99%,粉末粒度为5~38μm;喷涂速度1000 mm/s,喷涂6次,涂层厚度达到35μm;Si粘结层的喷涂工艺参数为:真空度为182Pa,工作电流为2100A,氩气流量为62L/min,氦气流量为52L/min,送粉量为5.5g/min,喷涂距离为1100mm。
步骤2:制备莫来石过渡层
在步骤1制备完Si粘结层后,在Si粘结层上随即制备莫来石过渡层,莫来石化学成分:SiO2重量百分比为28%、Al2O3为余量,粉末粒度为5~38μm,喷涂速度1000mm/s, 喷涂9次,喷涂厚度为50μm;莫来石过渡层喷涂工艺参数为:真空度为200Pa,工作电流为2700A,氩气流量为65L/min,氦气流量为65L/min,送粉量为6g/min,喷涂距离为450mm。
步骤3:制备Yb2SiO5环境障层
在步骤2喷涂完莫来石过渡层后,在莫来石过渡层上随即喷涂Yb2SiO5环境障层,纯度≥99.99%,粉末粒度为5~38μm,喷涂速度1000 mm/s,喷涂20次,喷涂厚度为108μm;Yb2SiO5环境障层喷涂工艺参数为:真空度为174Pa,工作电流为2100A,氩气流量为63 L/min,氦气流量为61L/min,送粉量为5.5g/min,喷涂距离为420mm。
步骤4:制备La2Zr2O7热障层
在步骤3喷涂完Yb2SiO5环境障层后,随即喷涂La2Zr2O7热障层,粉末纯度≥99.99%,粒度为5~38μm,喷涂速度1000mm/s,喷涂15次,喷涂厚度为50μm;La2Zr2O7热障层喷涂工艺参数为:真空度为150Pa,工作电流为2000A,氩气流量为70L/min,氦气流量为70L/min,送粉量为10g/min,喷涂距离为1000mm,零件旋转速度为15r/min。
用上述方法制备的环境防护涂层的结构如图1所示,环境防护涂层燃气冲刷前的扫描电镜微观组织形貌图如图2所示,在1700℃的燃气冲刷试验持续1000 h涂层未失效。1000h测试后涂层形貌如图3所示,可以看出微结构有少量变化,表层的La2Zr2O7热障层有部分烧结现象,而Yb2SiO5环境障层没有明显变化,整个测试过程中涂层体系结构保持完整,这种四层体系的环境防护涂层可用于1400~1700℃的发动机环境。
以上所述仅是本发明的优选实施方式,应当理解本发明并非局限于本文所披露的形式,不应看作是对其他实施例的排除,而可用于各种其他组合、修改和环境,并能够在本文所述构想范围内,通过上述教导或相关领域的技术或知识进行改动。而本领域人员所进行的改动和变化不脱离本发明的精神和范围,则都应在本发明所附权利要求的保护范围内。
Claims (9)
1.一种SiCf/SiC复合材料导向器叶片的环境防护涂层,其特征在于,由里向外依次包括Si粘结层、莫来石过渡层、Yb2SiO5环境障层和La2Zr2O7热障层。
2.根据权利要求1所述一种SiCf/SiC复合材料导向器叶片的环境防护涂层,其特征在于,所述Si粘结层的制备原料为硅粉,其纯度≥99.99%,粉末粒度为5~38μm;所述莫来石过渡层由22.0~28.0wt%的SiO2粉末与 72.0~78.0wt%的Al2O3粉末混合制备而成,混合粉末粒度为5~38μm;所述Yb2SiO5环境障层的制备原料为Yb2SiO5粉,其纯度≥99.99%,粉末粒度为5~38μm;所述La2Zr2O7热障层的制备原料为La2Zr2O7粉末,其纯度≥99.99%,粉末粒度为5~38μm。
3.权利要求1或2所述的一种SiCf/SiC复合材料导向器叶片的环境防护涂层的制备方法,其特征在于,包括:
Si粘结层制备,采用喷涂设备在叶片表面喷涂制作Si粘结层;
莫来石过渡层制备,采用喷涂设备在Si粘结层外喷涂制作莫来石过渡层;
Yb2SiO5环境障层制备,采用喷涂设备在莫来石过渡层外喷涂制作Yb2SiO5环境障层;
La2Zr2O7热障层制备,采用喷涂设备在Yb2SiO5环境障层外喷涂制作La2Zr2O7热障层。
4.根据权利要求3所述的制备方法,其特征在于,所述的喷涂设备为等离子喷涂—物理气相沉积设备,所述的等离子喷涂—物理气相沉积设备通过气相、液相与固相共沉积,实现不同组织结构的复合设计。
5.根据权利要求3所述的制备方法,其特征在于,还包括在制备Si粘结层前,对SiCf/SiC复合材料导向器叶片基体进行预热处理,预热温度为1000~1200℃。
6.根据权利要求3~5任一项所述的制备方法,其特征在于,所述Si粘结层喷涂工艺参数:真空度为150~200Pa,工作电流为2000~2200A,氩气流量为60~65L/min,氦气流量为50~55L/min,送粉量为5 ~6g/min,喷涂距离为1000~1200mm,喷涂厚度为20~50μm,喷涂5~7次。
7.根据权利要求3~5任一项所述的制备方法,其特征在于,所述莫来石过渡层喷涂工艺参数为:真空度150~200Pa,工作电流为2500~2700A,氩气流量为60~65L/min,氦气流量为60~65L/min,送粉量为5~6g/min,喷涂距离为400~450mm,喷涂厚度为20~50μm,喷涂7~9次。
8.根据权利要求3~5任一项所述的制备方法,其特征在于,所述Yb2SiO5环境障层喷涂工艺参数为:真空度150~200Pa,工作电流为2000~2200A,氩气流量为60~65L/min,氦气流量为60~65L/min,送粉量为5~6g/min,喷涂距离为400~450mm,喷涂厚度为50~150μm,喷涂18~22次。
9.根据权利要求3~5任一项所述的制备方法,其特征在于,所述La2Zr2O7热障层喷涂工艺参数为:真空度为150~200Pa,工作电流为2000~2200A,氩气流量为70~75L/min,氦气流量为70~75L/min,送粉量为10~15g/min,喷涂距离为1000~1100mm,喷涂厚度为50~150μm,喷涂15~17次。
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