CN110387148A - 一种用于树脂基复合材料的抗烧蚀涂层材料及其制备方法 - Google Patents
一种用于树脂基复合材料的抗烧蚀涂层材料及其制备方法 Download PDFInfo
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- 239000010949 copper Substances 0.000 claims abstract description 28
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Abstract
本发明涉及一种用于树脂基复合材料的抗烧蚀涂层材料及其制备方法,所述的抗烧蚀涂层材料为氧化钇稳定氧化锆、树脂、Cu和SiO2均匀混合物,所述混合物为球状颗粒或球状团粒材料。其制备方法包括混合粉体、球磨以及喷雾造粒。本发明有益之处在于采用添加有放热特定的成分复合YSZ陶瓷面层一方面陶瓷层起到很好的隔热、抗烧蚀作用,另一方面在高温下烧蚀相气化散热起到进一步提高复合材料的抗烧蚀、隔热性能。
Description
技术领域
本发明属于树脂基复合材料热防护涂层材料领域,具体涉及一种用于树脂基复合材料的抗烧蚀涂层材料及其制备方法,特别是用于聚酰亚胺树脂基复合材料的抗烧蚀和热防护。
背景技术
聚酰亚胺树脂基复合材料具有比强度高、可设计性强、抗疲劳断裂性能好等一系列优点,已经在航空发动机外涵机匣、静子叶片、转子叶片、包容机匣以及发动机短舱、反推力装置上得到大量的应用,减重效果明显。
先进航空发动机的服役环境温度更高,对聚酰亚胺树脂基复合材料的发动机部件服役性能提出了更高的热防护要求,例如要求在800~850℃高温条件下高温冲刷后仍具有较好的性能稳定性。而目前耐热性最好的聚酰亚胺树脂基复合材料也只能在300℃左右使用,进一步提高耐热性则需要增大成本,并且具有很大难度,因此,通过采用适当的热防护涂层提高其使用温度比研制新的耐高温树脂基复合材料更切合实际。
国内外树脂基复合材料常用的热防护涂层主要有YSZ(Y2O3稳定ZrO2)热障涂层和其他烧蚀型(热容吸热、烧蚀防热、辐射式散热、发汗防热)功能涂层两大类。但树脂基复合材料表面制备热防护涂层面临着很多技术难题,例如烧蚀型涂层防热机理是借助高温冲蚀后涂层烧蚀气化、碳化烧损而保护基体不损伤,但为了达到较好的防热效果一般制备较厚,会显著降低与复材基体的结合强度,且使用寿命有限。热障涂层具有较低的热导率和合适的膨胀系数,具有较好的隔热性能,在金属基表面热防护应用较为成熟,但与树脂基复合材料的结合强度低,且存在层间应力不匹配的问题,易在使用过程中脱落而失去隔热作用。主要原因是相对于金属基体,树脂基复材与涂层之间不可能发生冶金反应或很好的嵌合作用;另外,复合材料的固化温度低,因此采用热喷涂技术时不但不可以追求高温热源(这大大有利于冶金结合),相反应严格控制复合材料基体的表面温度;再者,由于复合材料与金属或陶瓷涂层的热膨胀系数相差较大,过高的温度梯度变化,将在涂层与基体之间产生过大的内应力,使涂层与基体分离,如何最大限度的消除这些问题就成了复材表面热防护涂层研制的重点。
本发明基于传统YSZ热障陶瓷涂层隔热性能好的优势,同时根据烧蚀型涂层防热的理念,提出发汗冷却防热抗烧蚀机理的构想,将烧蚀相(酚醛树脂、改性有机硅树脂、聚酯、Cu、SiO2)与YSZ陶瓷进行复合,在高温条件下,依靠陶瓷基相(YSZ)良好的隔热性能阻滞热量传递,同时复合在YSZ陶瓷涂层内部低熔点烧蚀型材料高温下发生分解、熔化、气化或挥发等相变带走一部分热量,烧蚀后形成的气体不仅能在涂层表面形成热阻塞效应,而且能够在涂层内部形成大量的孔隙进一步降低涂层的热导率,为了减小某单一烧蚀材料在很窄的温度段内分解或气化后产生的内压对涂层所造成的破坏,以及保持涂层在整个防热过程中都可能进行烧蚀防热。
发明内容
本发明的目的是:在于为树脂基复合材料提供热防护,特别是聚酰亚胺树脂基复合材料,给出在树脂基复合材料表面形成抗烧蚀涂层的方法。
本发明的技术方案是:
提供一种用于树脂基复合材料的抗烧蚀涂层材料,所述的抗烧蚀涂层材料为氧化钇稳定氧化锆、树脂、Cu和SiO2均匀混合物,所述混合物为球状颗粒或球状团粒材料。
进一步的,其中,氧化钇稳定氧化锆、树脂、Cu、SiO2之间的质量比为:(70~75):(3~9):(8~10):(6~17)。
进一步的,其中,树脂包括酚醛树脂、改性有机硅树脂和聚酯;酚醛树脂、改性有机硅树脂和聚酯之间的质量比为:(1~3):(2~3):(0~3)。
提供一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,将粒度为10~20nm的氧化钇稳定氧化锆(YSZ)粉末、粒度1~2μm的树脂粉末、粒度3~5μm的Cu粉末和粒度3~5μm的SiO2粉末进行均匀混合形成混合粉末,其中氧化钇稳定氧化锆粉末、树脂粉末、Cu粉末和SiO2粉末之间的质量比为(70~75):(3~9):(8~10):(6~17);其中树脂粉末为酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末;酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为(1~3):(2~3):(0~3);对混合粉末进行喷雾造粒,得到球状团粒或球状颗粒。
进一步的,混合粉末的喷雾造粒的粘结剂为聚乙烯醇,中间层喷雾造粒的工艺参数为:加热温度60~80℃,搅拌时间60~90min,搅拌速率500~700rpm/min;造粒环节在真空条件下进行,获得粒径为30μm~45μm的球状团粒。
进一步的,所述混合粉末在混合时于液态介质(优选为酒精)中球磨混合得到,球磨参数为:转速10~20rpm/s,混合10~20小时;随后在10~20Hz频率下超声处理1~2小时;于60~90℃下烘干处理1~2小时。
进一步的,所述树脂粉末为酚醛树脂粉末和改性有机硅树脂粉末;所述酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为(1~3):(2~3)。
本发明的优点是:1)本发明通过添加金属(Cu)、非金属(SiO2)、有机材料(酚醛树脂、改性有机硅树脂、聚酯粉末)多元材料复合,制备低热导的陶瓷基具有发汗放热特性的热障烧蚀涂层。热障烧蚀复合涂层的特性在于高温环境服役过程中YSZ陶瓷基相通过良好的隔热性能阻滞热量传递,同时还利用相对低熔点的烧蚀型材料(Cu、SiO2、酚醛树脂、改性有机硅树脂、聚酯粉末)在高温下发生分解、熔化、气化或挥发等相变带走一部分热量。烧蚀后形成的气体不仅能在涂层表面形成热阻塞效应,而且还能够在涂层内部形成大量的孔隙进一步降低涂层的热导率。
2)为了减小某单一烧蚀材料在很窄的温度段内分解或气化后产生的内压对涂层所造成的破坏,以及保持涂层在整个防热过程中都可能进行烧蚀防热。本发明设计的发汗放热特性的热障烧蚀涂层是YSZ陶瓷相和有机聚合物、低熔点金属、SiO2的烧蚀相的复合材料,相比添加单一烧蚀相,本发明设计材料在较宽温度范围内均有物质烧蚀卸载部分热量的特性,同时残留的多孔结构则起到进一步提高隔热防热功能,可有效的延长热平衡的时间界限,减少热量在涂层内部的输入率,保证涂层在较长时间不会使热量聚集在复材基体界面,影响复合材料的力学性能。
附图说明
图1为实例1制备的YSZ复合烧蚀相(Cu、SiO2、酚醛树脂、改性有机硅树脂、聚酯)粉末的扫描电镜图。
具体实施方式
下面将结合实施例,对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例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1:
提供一种用于树脂基复合材料的抗烧蚀涂层材料,所述的抗烧蚀涂层材料为氧化钇稳定氧化锆、树脂、Cu和SiO2均匀混合物,所述混合物为球状颗粒或球状团粒材料。
进一步的,其中,氧化钇稳定氧化锆、树脂、Cu、SiO2之间的质量比为:72:3:8:17。
进一步的,其中,树脂包括酚醛树脂、改性有机硅树脂和聚酯;酚醛树脂、改性有机硅树脂和聚酯之间的质量比为:1:2:1。
提供一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,将粒度为10~20nm的氧化钇稳定氧化锆(YSZ)粉末、粒度1~2μm的树脂粉末、粒度3~5μm的Cu粉末和粒度3~5μm的SiO2粉末进行均匀混合形成混合粉末,其中氧化钇稳定氧化锆粉末、树脂粉末、Cu粉末和SiO2粉末之间的质量比为72:3:8:17;其中树脂粉末为酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末;酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为1:2:1;对混合粉末进行喷雾造粒,得到球状团粒或球状颗粒。
进一步的,混合粉末的喷雾造粒的粘结剂为聚乙烯醇,中间层喷雾造粒的工艺参数为:加热温度60℃,搅拌时间60min,搅拌速率500rpm/min;造粒环节在真空条件下进行,获得粒径为30μm的球状团粒。
进一步的,所述混合粉末在混合时于液态介质(优选为酒精)中球磨混合得到,球磨参数为:转速10rpm/s,混合10小时;随后在10Hz频率下超声处理1小时;于60℃下烘干处理1小时。
进一步的,所述树脂粉末为酚醛树脂粉末和改性有机硅树脂粉末;所述酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为1:2。
实施例2:
在上述实施例的基础上,本实施例步骤为:
提供一种用于树脂基复合材料的抗烧蚀涂层材料,所述的抗烧蚀涂层材料为氧化钇稳定氧化锆、树脂、Cu和SiO2均匀混合物,所述混合物为球状颗粒或球状团粒材料。
进一步的,其中,氧化钇稳定氧化锆、树脂、Cu、SiO2之间的质量比为:72:4:8:16。
进一步的,其中,树脂包括酚醛树脂、改性有机硅树脂和聚酯;酚醛树脂、改性有机硅树脂和聚酯之间的质量比为:2:2:1。
提供一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,将粒度为15nm的氧化钇稳定氧化锆(YSZ)粉末、粒度1μm的树脂粉末、粒度3μm的Cu粉末和粒度3μm的SiO2粉末进行均匀混合形成混合粉末,其中氧化钇稳定氧化锆粉末、树脂粉末、Cu粉末和SiO2粉末之间的质量比为72:4:8:16;其中树脂粉末为酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末;酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为2:2:1;对混合粉末进行喷雾造粒,得到球状团粒或球状颗粒。
混合粉末的喷雾造粒的粘结剂为聚乙烯醇,中间层喷雾造粒的工艺参数为:加热温度70℃,搅拌时间60min,搅拌速率500rpm/min;造粒环节在真空条件下进行,获得粒径为30μm的球状团粒。
所述混合粉末在混合时于液态介质(优选为酒精)中球磨混合得到,球磨参数为:转速15rpm/s,混合15小时;随后在15Hz频率下超声处理1小时;于70℃下烘干处理1小时。
所述树脂粉末为酚醛树脂粉末和改性有机硅树脂粉末;所述酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为2:2。
实施例3:
在上述实施例的基础上,本实施例步骤为:
提供一种用于树脂基复合材料的抗烧蚀涂层材料,所述的抗烧蚀涂层材料为氧化钇稳定氧化锆、树脂、Cu和SiO2均匀混合物,所述混合物为球状颗粒或球状团粒材料。
进一步的,其中,氧化钇稳定氧化锆、树脂、Cu、SiO2之间的质量比为:74:8:8:10。
进一步的,其中,树脂包括酚醛树脂、改性有机硅树脂和聚酯;酚醛树脂、改性有机硅树脂和聚酯之间的质量比为:2:2:2。
提供一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,将粒度为15nm的氧化钇稳定氧化锆(YSZ)粉末、粒度2μm的树脂粉末、粒度2μm的Cu粉末和粒度4μm的SiO2粉末进行均匀混合形成混合粉末,其中氧化钇稳定氧化锆粉末、树脂粉末、Cu粉末和SiO2粉末之间的质量比为74:8:8:10;其中树脂粉末为酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末;酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为2:2:2;对混合粉末进行喷雾造粒,得到球状团粒或球状颗粒。
混合粉末的喷雾造粒的粘结剂为聚乙烯醇,中间层喷雾造粒的工艺参数为:加热温70℃,搅拌时间80min,搅拌速率600rpm/min;造粒环节在真空条件下进行,获得粒径为45μm的球状团粒。
所述混合粉末在混合时于液态介质(优选为酒精)中球磨混合得到,球磨参数为:转速15rpm/s,混合15小时;随后在20Hz频率下超声处理2小时;于90℃下烘干处理2小时。
所述树脂粉末为酚醛树脂粉末和改性有机硅树脂粉末;所述酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为2:2。
实例4:
在上述实施例的基础上,本实施例步骤为:
提供一种用于树脂基复合材料的抗烧蚀涂层材料,所述的抗烧蚀涂层材料为氧化钇稳定氧化锆、树脂、Cu和SiO2均匀混合物,所述混合物为球状颗粒或球状团粒材料。
其中,氧化钇稳定氧化锆、树脂、Cu、SiO2之间的质量比为:75:9:10:6。
其中,树脂包括酚醛树脂、改性有机硅树脂和聚酯;酚醛树脂、改性有机硅树脂和聚酯之间的质量比为:3:3:3。
提供一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,将粒度为20nm的氧化钇稳定氧化锆(YSZ)粉末、粒度2μm的树脂粉末、粒度5μm的Cu粉末和粒度5μm的SiO2粉末进行均匀混合形成混合粉末,其中氧化钇稳定氧化锆粉末、树脂粉末、Cu粉末和SiO2粉末之间的质量比为75:9:10:6;其中树脂粉末为酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末;酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为3:3:3;对混合粉末进行喷雾造粒,得到球状团粒或球状颗粒。
混合粉末的喷雾造粒的粘结剂为聚乙烯醇,中间层喷雾造粒的工艺参数为:加热温度80℃,搅拌时间90min,搅拌速率700rpm/min;造粒环节在真空条件下进行,获得粒径为45μm的球状团粒。
所述混合粉末在混合时于液态介质(优选为酒精)中球磨混合得到,球磨参数为:转速20rpm/s,混合20小时;随后在20Hz频率下超声处理2小时;于90℃下烘干处理2小时。
所述树脂粉末为酚醛树脂粉末和改性有机硅树脂粉末;所述酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为3:3。
应当理解的是,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,而所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (8)
1.一种用于树脂基复合材料的抗烧蚀涂层材料,所述的抗烧蚀涂层材料为氧化钇稳定氧化锆、树脂、Cu和SiO2均匀混合物,所述混合物为球状颗粒或球状团粒材料。
2.如权利要求1所述的一种用于树脂基复合材料的抗烧蚀涂层材料,其特征在于:其中,氧化钇稳定氧化锆、树脂、Cu、SiO2之间的质量比为:(70~75):(3~9):(8~10):(6~17)。
3.如权利要求1所述的一种用于树脂基复合材料的抗烧蚀涂层材料,其特征在于:其中,树脂包括酚醛树脂、改性有机硅树脂和聚酯;酚醛树脂、改性有机硅树脂和聚酯之间的质量比为:(1~3):(2~3):(0~3)。
4.一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,将粒度为10~20nm的氧化钇稳定氧化锆(YSZ)粉末、粒度1~2μm的树脂粉末、粒度3~5μm的Cu粉末和粒度3~5μm的SiO2粉末进行均匀混合形成混合粉末,其中氧化钇稳定氧化锆粉末、树脂粉末、Cu粉末和SiO2粉末之间的质量比为(70~75):(3~9):(8~10):(6~17);其中树脂粉末为酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末;酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为(1~3):(2~3):(0~3);对混合粉末进行喷雾造粒,得到球状团粒或球状颗粒。
5.如权利要求4所述的一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,其特征在于:混合粉末的喷雾造粒的粘结剂为聚乙烯醇,中间层喷雾造粒的工艺参数为:加热温度60~80℃,搅拌时间60~90min,搅拌速率500~700rpm/min;造粒环节在真空条件下进行,获得粒径为30μm~45μm的球状团粒。
6.如权利要求4所述的一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,其特征在于:所述混合粉末在混合时于液态介质(优选为酒精)中球磨混合得到,球磨参数为:转速10~20rpm/s,混合10~20小时;随后在10~20Hz频率下超声处理1~2小时;于60~90℃下烘干处理1~2小时。
7.如权利要求6所述的一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,其特征在于:所述液态介质为酒精。
8.如权利要求4所述的一种用于树脂基复合材料的抗烧蚀涂层材料的制备方法,其特征在于:所述树脂粉末为酚醛树脂粉末和改性有机硅树脂粉末;所述酚醛树脂粉末、改性有机硅树脂粉末和聚酯粉末之间的质量比为(1~3):(2~3)。
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