CN109608176B - 一种烧蚀维形纤维涂层及制备、施工方法 - Google Patents

一种烧蚀维形纤维涂层及制备、施工方法 Download PDF

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CN109608176B
CN109608176B CN201811547572.6A CN201811547572A CN109608176B CN 109608176 B CN109608176 B CN 109608176B CN 201811547572 A CN201811547572 A CN 201811547572A CN 109608176 B CN109608176 B CN 109608176B
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fiber
coating
sol
auxiliary agent
ablation
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CN109608176A (zh
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刘坤
孙连来
王伟远
时卓
刘磊
薛健
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Liaoning Light Industry Science Research Institute Co ltd
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Abstract

本发明所公开的一种新型烧蚀维形纤维涂层的制备方法，属于特种涂料涂层领域，具体涉及一种具有烧蚀维形性能的纤维复合梯度涂层的制备、施工方法。本专利制备的新型烧蚀维形纤维涂层摆脱了树脂基底高温分解的缺点，以复配无机纤维作为涂层的主要组分，具有出色的耐高温、抗气流冲刷性能，同时具有良好的施工效率与较低的物料成本，特别适合具有大面积烧蚀维形防护要求的高速飞行器、再入飞行器、导弹等装备一次性或重复性热防护需求。

Description

一种烧蚀维形纤维涂层及制备、施工方法
技术领域
本发明所公开的一种烧蚀维形纤维涂层的制备方法，属于特种涂料涂层领域，具体涉及一种具有烧蚀维形性能的纤维复合梯度涂层的制备、施工方法。
背景技术
飞行器再入或亚轨道高速飞行过程中，飞行器表面受气动加热，需要良好的防热材料进行保护，为了维持高速飞行器的气动外形，该防热材料还需要具有良好的烧蚀维形性能。防热材料的烧蚀维形性能对于亚轨道可控高速飞行器的发展尤其重要。
我国现有烧蚀材料以树脂基复合材料为主，通过材料自身的隔热性能与树脂高温烧蚀吸热现象共同起到气动热防护的效果。随着飞行器使用工况要求的提高，现有烧蚀材料烧蚀量大、烧蚀面不平整、维持气动外形能力较差等问题逐渐凸显。在飞行器某些部位、某些飞行器型号表面，现有烧蚀材料已经很难满足防护要求。
发明内容
针对上述问题及结合实际，本发明公开一种烧蚀维形纤维涂层的制备及配套施工方法。本发明的技术方案实施如下：
本发明公开一种烧蚀维形纤维涂层的制备及配套施工方法。发明中所公开的配方和制备方法，能够在多种飞行器结构、蒙皮材料表面形成一层微烧蚀或不烧蚀的具有维持气动外形能力的热防护纤维涂层，在某些气动热环境下具有重复使用的能力。蒙皮表面新型烧蚀维形纤维涂层内部梯度示意图如图1所示。
一种新型烧蚀维形纤维涂层的质量份数配方如下：
复配无机纤维 150~300份
纳米无机溶胶 30~50份
去离子水 5~15份
熔融助剂 5~30份
高发射率助剂 5~30份
表面封闭助剂 5~30份
其中，所述复配无机纤维为多包括玻璃纤维、高硅氧纤维、莫来石纤维、玄武岩纤维、氧化铝纤维、石棉纤维、氧化锆纤维、碳纤维、硼纤维、碳化硅纤维等在内的一种或多种纤维的混合物。
其中，所述复配无机纤维直径为1~20微米，纤维长度0.1~5毫米，纤维长径比1：50~300。
其中，所述复配无机纤维直径优选为5~10微米，纤维长度优选为0.5~2毫米，纤维长径比优选:1：100~200。
其中，所述纳米无机溶胶为包括锆溶胶、铝溶胶、硅溶胶以及锆溶胶、铝溶胶、硅溶胶中的两种或以上形成的复合溶胶在内的一种或多种纳米无机溶胶的混合物。
其中，所述的纳米无机溶胶的溶胶颗粒粒径为10～50纳米。
其中，所述的纳米无机溶胶的溶胶颗粒粒径优选为30～40纳米。
其中，所述的熔融助剂为锂、钠、钾、镁、钙、锌、铅、铝等的氯化物、氧化物、碳酸盐、碳酸氢盐、硅酸盐等中的一种或几种的混合物。
其中，所述的熔融助剂还可以是D245、D250等低熔点玻璃粉中的一种或几种的混合物。
其中，所述的熔融助剂还可以是硼的碳化物、氮化物、氧化物中的一种或几种的混合物。
其中，所述的高发射率助剂为碳化硅、氮化硅、尖晶石型铁氧体、堇青石、二氧化钛、二氧化锆中的一种或几种的混合物。
其中，所述的表面封闭助剂为钠、铝、镁的硅酸盐中的一种或几种的混合物。
其中，所述的熔融助剂、高发射率助剂、表面封闭助剂颗粒度为150～1000目。
其中，所述的熔融助剂、高发射率助剂、表面封闭助剂颗粒度优选为500～800目。
本发明公开了一种新型烧蚀维形纤维涂层的制造方法，它按照下述步骤进行：
（1）将无机纤维按照配比将不同种类纤维进行复配、短切、球磨达到预期纤维长度后，进行300～500℃热处理1小时冷却待用。
（2）将纳米无机溶胶、熔融助剂、高发射率助剂、表面封闭助剂进行充分润湿、混合待用。
（3）将（1）中的复配无机纤维、（2）中的混合浆料进行混合，用去离子水调节混合后涂料流动性，得到烧蚀维形纤维涂料。
本发明公开了一种新型烧蚀维形纤维涂层的施工方法，它按照下述步骤进行：
（1）将飞行器蒙皮、结构件等基底表面进行喷砂打毛处理。
（2）基底表面进行NiCoCrAlY、NiCrAlY、ZrO2等过渡层热喷涂，喷涂涂层厚度为0.1～0.3mm。
（3）使用如图2所示的，由流量控制系统、压盘上料辅助系统、调压式隔膜泵、单管喷涂装置组成的三维纤维涂料喷涂机，进行纤维涂层的喷涂作业。纤维喷涂机喷口直径5～10mm，出口流量0.5～2L/min。按照设计要求厚度一次喷涂成型。
（4）根据设计要求，可进行纤维涂层表面封闭处理。本发明使用红外辐照表面封闭机，由电源、控制器、短波红外辐照模组、热电偶装置与水冷系统组成，结构示意图如图3所示。采用脉冲式功率控制模式，在一定表面温度下对涂层样品表面进行辐照，处理温度为300～500℃，表面封闭处理时间为3～10min。
（5）表面修整打磨后，完成工件表面新型烧蚀维形纤维涂层的施工工作。
本发明的有益效果：
本发明制备的新型烧蚀维形纤维涂层摆脱了树脂基底高温分解的缺点，以复配无机纤维作为涂层的主要组分，具有出色的耐高温、抗气流冲刷性能，同时具有良好的施工效率与较低的物料成本，特别适合具有大面积烧蚀维形防护要求的高速飞行器、再入飞行器、导弹等装备一次性或重复性热防护需求。
附图说明
为了便于本领域技术人员理解，下面结合附图对本发明作进一步的说明。
图1为蒙皮表面新型烧蚀维形纤维涂层构件示意图；
图2 三维纤维涂料喷涂机结构示意图；
图3 红外辐照表面封闭机结构示意图。
具体实施方式
实施例1
一种烧蚀维形纤维涂层的制备与施工方法。将无机纤维（高硅氧纤维：玄武岩纤维：碳纤维＝5：1：1，纤维直径15～20um）进行混合、短切（纤维长度3～4mm）、300℃高温处理后，制备为250份复配无机纤维待用。向分散机内加入35份纳米无机溶胶（锆/硅复合溶胶，溶胶颗粒D90为45nm），15份熔融助剂（氯化钾：碳酸钠：氧化铅＝2：2：1，颗粒度为500目）、10份高发射率助剂（尖晶石型铁氧体：堇青石＝1：1，颗粒度为800目）、5份表面封闭助剂（硅酸镁，颗粒度800目），在200转/分下搅拌分散2分钟。将分散好的混合物，复配无机纤维、10份去离子水放入砂浆混合搅拌器中，以400转/分速度混合搅拌18分钟，制得烧蚀维形纤维涂料。高温合金基底表面喷砂处理后，等离子喷涂0.2～0.3mm厚的NiCoCrAlY过渡涂层。使用三维纤维涂料喷涂机（5mm喷口、出口流量0.8～1L/min）喷涂纤维涂层5～6mm。使用红外辐照表面封闭机（450℃，表面处理10min）进行表面封闭处理。经打磨处理后，得到新型烧蚀维形纤维涂层。
实施例2.
将无机纤维（玻璃纤维：莫来石纤维：氧化铝纤维：石棉纤维＝3：5：1：1，纤维直径10～12um）进行混合、短切（纤维长度2～3mm）、500℃高温处理后，制备为300份复配无机纤维待用。向分散机内加入50份纳米无机溶胶（锆/铝复合溶胶，溶胶颗粒D90为30nm），20份熔融助剂（氧化铅：氧化镁：氧化铝＝2：1：1，颗粒度为625目）、15份高发射率助剂（氮化硅：氧化锆＝2：1，颗粒度为625目）、5份表面封闭助剂（硅酸钠，颗粒度500目），搅拌分散后待用。将分散好的混合物，复配无机纤维、5份去离子水放入砂浆混合搅拌器中，以200转/分速度混合搅拌15分钟，制得烧蚀维形纤维涂料。钛合金基底表面喷砂处理后，等离子喷涂0.1厚的NiCrAlY过渡涂层。使用三维纤维涂料喷涂机（10mm喷口、出口流量1L/min）喷涂纤维涂层8mm。使用红外辐照表面封闭机（500℃，表面处理10min）进行表面封闭处理。经打磨处理后，得到新型烧蚀维形纤维涂层。
实施例3.
将无机纤维（玄武岩纤维：碳化硅纤维＝5：3，纤维直径10～15um）进行混合、短切（纤维长度1～2mm）、300℃高温处理后，制备为250份复配无机纤维待用。向分散机内加入25份纳米无机溶胶（锆溶胶：铝溶胶=1：1，溶胶颗粒D90为50nm），5份熔融助剂（硅酸钠：碳酸钠＝2：1，颗粒度为800目）、5份高发射率助剂（氮化硅：二氧化钛＝1：1，颗粒度为800目）、5份表面封闭助剂（硅酸钠：硅酸铝＝1：1，颗粒度800目），搅拌分散后待用。将分散好的混合物，复配无机纤维、15份去离子水放入砂浆混合搅拌器中，以400转/分速度混合搅拌10分钟，制得烧蚀维形纤维涂料。6061铝合金基底表面喷砂处理后，等离子喷涂0.1mm厚的NiCoCrAlY过渡涂层。使用三维纤维涂料喷涂机（10mm喷口、出口流量1.5L/min）喷涂纤维涂层3～4mm。使用红外辐照表面封闭机（500℃，表面处理3min）进行表面封闭处理。经打磨处理后，得到新型烧蚀维形纤维涂层。
在本发明所公开的制备方法中，根据所公开的配方而相应设定的各个材料的性能指标及制备、施工参数等，均为得到性能更为优异和稳定的新型烧蚀维形纤维涂层发挥了各自的作用，将各个参数设置等加和形成一个完整的制备体系，并配合本发明所公开的配方时，则可以得到性能最为优异和稳定的新型烧蚀维形纤维涂层产品。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该发明仅为所述的具体实施方式。显然，根据本说明书的内容，可做很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。

Claims (7)

1.一种烧蚀维形纤维涂层的制备方法，其特征在于，所述烧蚀维形纤维涂层包括如下质量份数的组分：
复配无机纤维 150~300份
纳米无机溶胶 30~50份
去离子水 5~15份
熔融助剂 5~30份
高发射率助剂 5~30份
表面封闭助剂 5~30份
所述复配无机纤维包括玻璃纤维、高硅氧纤维、莫来石纤维、玄武岩纤维、氧化铝纤维、石棉纤维、氧化锆纤维、碳纤维、硼纤维、碳化硅纤维在内的多种纤维的混合物；
其中，所述复配无机纤维直径为1~20微米，纤维长度0.1~5毫米，纤维长径比1：50~300；
所述纳米无机溶胶包括锆溶胶、铝溶胶、硅溶胶以及锆溶胶、铝溶胶、硅溶胶中的两种或以上形成的复合溶胶在内的一种或多种纳米无机溶胶的混合物；所述的纳米无机溶胶的溶胶颗粒粒径为10～50纳米；
所述熔融助剂为锂、钠、钾、镁、钙、锌、铅、铝的氯化物、氧化物、碳酸盐、碳酸氢盐、硅酸盐等中的一种或几种的混合物；或为D245、D250低熔点玻璃粉中的一种或几种的混合物；或为硼的碳化物、氮化物、氧化物中的一种或几种的混合物；
所述高发射率助剂为碳化硅、氮化硅、尖晶石型铁氧体、堇青石、二氧化钛、二氧化锆中的一种或几种的混合物；
所述的表面封闭助剂为钠、铝、镁的硅酸盐中的一种或几种的混合物；
所述制备方法依次包括如下步骤：
（1）将无机纤维按照配比按不同种类纤维进行复配、短切、球磨达到预期纤维长度后，进行300～500℃热处理1小时冷却待用；
（2）将纳米无机溶胶、熔融助剂、高发射率助剂、表面封闭助剂进行充分润湿、混合待用；
（3）将（1）中的复配无机纤维、（2）中的混合浆料进行混合，用去离子水调节混合后涂料流动性，得到烧蚀维形纤维涂料。
2.如权利要求1所述的一种烧蚀维形纤维涂层的制备方法，其特征在于，所述复配无机纤维直径为5~10微米，长度为0.5~2毫米，长径比:1：100~200；
所述纳米无机溶胶的溶胶颗粒粒径为30～40纳米；
所述熔融助剂、高发射率助剂、表面封闭助剂颗粒度为150～1000目。
3.根据权利要求2所述的一种烧蚀维形纤维涂层的制备方法，其特征在于，所述熔融助剂、高发射率助剂、表面封闭助剂颗粒度为500～800目。
4.如权利要求1所述的一种烧蚀维形纤维涂层的施工方法，其特征在于，依次包括如下步骤进行：
（1）将飞行器蒙皮、结构件基底表面进行喷砂打毛处理；
（2）基底表面进行NiCoCrAlY、NiCrAlY、ZrO2过渡层热喷涂，喷涂涂层厚度为0.1～0.3mm；
（3）使用三维纤维涂料喷涂机进行纤维涂层的喷涂作业，纤维喷涂机喷口直径5～10mm，出口流量0.5～2L/min，按照设计要求厚度一次喷涂成型；
（4）根据设计要求，使用红外辐照表面封闭机对纤维涂层表面进行封闭处理，采用脉冲式功率控制模式，在一定表面温度下对涂层样品表面进行辐照，处理温度为300～500℃，表面封闭处理时间为3～10min；
（5）表面修整打磨后，完成工件表面新型烧蚀维形纤维涂层的施工工作。
5.如权利要求4所述的一种烧蚀维形纤维涂层的施工方法，其特征在于，所述三维纤维涂料喷涂机由流量控制系统、压盘上料辅助系统、调压式隔膜泵、单管喷涂装置组成。
6.根据权利要求4所述的一种烧蚀维形纤维涂层的施工方法，其特征在于，所述红外辐照表面封闭机由电源、控制器、短波红外辐照模组、热电偶装置与水冷系统组成。
7.如权利要求1所述的一种烧蚀维形纤维涂层的应用，其特征在于，所述烧蚀维形纤维涂层能够在多种飞行器结构、蒙皮材料表面形成一层微烧蚀或不烧蚀的具有维持气动外形能力的热防护纤维涂层，在某些气动热环境下具有重复使用的能力，其中蒙皮表面烧蚀维形纤维涂层内部梯度结构依次为：飞行器蒙皮、过渡涂层、轻质抗烧蚀纤维涂层、表面封闭高热发射率涂层。
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