CN110527962A - 一种低应力耐湿热复合热控薄膜及其制备方法 - Google Patents
一种低应力耐湿热复合热控薄膜及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种低应力耐湿热复合热控薄膜及其制备方法,属于热控薄膜技术领域。所述薄膜包括依次沉积在基底上的反射率层、过渡层、发射率层和导电层;通过在高反射率层和SiO2发射率层之间增加Al2O3过渡层,既可以提高反射率层和主发射率层之间的附着力,又可以调控薄膜的热控参数。通过控制主发射率层的致密度和微观结构,使SiO2内层处于较为疏松的状态,外层致密度较高,使薄膜应力总体处于较低的状况,而外层的高致密度SiO2实现了水汽的有效阻隔,提高整个膜系的耐湿热能力。所述热控薄膜满足大于4N/cm的膜层附着力要求,同时满足24h时长95%湿度的试验要求。
Description
技术领域
本发明涉及一种低应力耐湿热复合热控薄膜及其制备方法,属于热控薄膜技术领域。
背景技术
随着空间技术的发展,卫星等航天器的结构与功能越来越复杂,对热控性能的需求也越来越趋向于多样化,并且要求直接在工件表面实现热控薄膜的直接沉积以减小重量。常规的热控薄膜结构较为简单,其太阳吸收率主要由表层薄膜的特性决定,而红外发射率则基本由基底材料所决定,热控参数可调节范围窄,应用范围受限,且空间环境稳定性不理想。
复合热控薄膜是一种热控参数可调的直接沉积型热控薄膜,具有优异的空间防护性能。该薄膜包括依次沉积在工件上的反射率层、发射率层和导电层。高发射率是热控薄膜最为普遍的一种应用要求,通常发射率层的设计为16μm以上SiO2来实现。由于膜层层数较多且SiO2发射率层为均一结构,单一结构的SiO2导致整个膜层应力较大,且膜层耐湿热能力较弱,不能满足空间航天器的应用要求。
发明内容
有鉴于此,本发明的目的在于提供一种低应力耐湿热复合热控薄膜及其制备方法,通过在反射率层和SiO2发射率层中见增加Al2O3过渡层,提高了反射率层和SiO2发射率层的结合力,同时通过控制SiO2发射率层的溅射条件使SiO2的微观结构呈现一定的密度梯度,与Al2O3过渡层接触的SiO2内层较为疏松,薄膜应力较小,与导电层接触的SiO2外层薄膜致密度较高,具有较好的抵御湿热环境的能力,制备得到的薄膜同时具备低应力和耐湿热的性能,满足航天器热控薄膜的空间通用要求,并具备良好的空间环境稳定性要求。
为实现上述目的,本发明的技术方案如下。
一种低应力耐湿热复合热控薄膜,所述薄膜包括依次沉积在基底上的反射率层、过渡层、发射率层和导电层;其中,过渡层为Al2O3,厚度150nm~3μm;发射率层由依次沉积在过渡层上的SiO2内层和SiO2外层组成,SiO2外层的致密度高于SiO2内层;所述发射率层的厚度>150nm,当150nm<发射率层厚度<750nm时,SiO2外层的厚度为150nm;当发射率层厚度≥750nm时,SiO2内层为发射率层厚度的80~90%,SiO2外层为发射率层厚度的10~20%。反射率层和导电层的材质和厚度为本领域常规选择。
优选的,所述发射率层的厚度为350nm~20μm。
优选的,所述反射率层为Al。
优选的,所述导电层为ITO。
一种低应力耐湿热复合热控薄膜的制备方法,所述方法步骤如下:
(1)使用离子源对工件表面进行活化处理,然后采用磁控溅射法在工件表面镀制反射率层;
(2)采用孪生靶中频反应磁控溅射镀制Al2O3过渡层;
(3)采用孪生靶中频反应磁控溅射镀制SiO2发射率层,其中在工作气压为0.7~1.0Pa,溅射功率为6000~9000W下制备SiO2内层,在工作气压为0.2~0.7Pa,溅射功率为1000~6000W下制备SiO2外层;
(4)采用直流磁控溅射方法镀制导电层。
所述制备方法中其他条件为本领域常规选择。
有益效果
本发明通过增加过渡层以及控制SiO2发射率层的密度梯度来保证复合热控薄膜的膜层附着力和防湿热环境能力,所述热控薄膜具有通用性,具备良好的空间环境的应用要求。具体的,通过在高反射率层和SiO2发射率层之间增加Al2O3过渡层,既可以提高反射率层和主发射率层之间的附着力,又可以调控薄膜的热控参数。通过控制主发射率层的致密度和微观结构,使SiO2内层处于较为疏松的状态,外层致密度较高,使薄膜应力总体处于较低的状况,而外层的高致密度SiO2实现了水汽的有效阻隔,提高整个膜系的耐湿热能力。所述热控薄膜满足大于4N/cm的膜层附着力要求,同时满足24h时长95%湿度的试验要求。
具体实施方式
下面结合具体实施例对本发明作进一步详细的说明。
实施例1
一种低应力耐湿热复合热控薄膜的制备方法,所述方法步骤如下:
(1)使用离子源对工件表面进行活化处理,离子源活化电源为电流工作模式,控制电流大小为1.70A,功率为850W,处理时间30s。
(2)采用溅射方式镀制Al反射率层:溅射压力为0.35Pa,溅射功率为4000W,沉积时间10s,得到膜厚为150nm的Al反射率层。
(3)采用孪生靶中频反应磁控溅射镀制Al2O3过渡层:溅射压力0.35Pa,溅射功率5000W,沉积时间1.5h,得到膜厚为3μm的Al2O3过渡层。
(4)采用孪生靶中频反应磁控溅射镀制SiO2发射率层:其中溅射压力为1.0Pa,溅射功率为9000W下,沉积时间6h,得到膜厚为13μm的疏松SiO2内层,在溅射压力为0.6Pa,溅射功率为6000W下,沉积时间1h,得到膜厚为2μm的致密SiO2外层;
(5)采用直流磁控溅射方法镀制ITO导电层:溅射压力为0.35Pa,溅射功率为2000W,沉积时间10s,得到膜厚为40nm为ITO导电层。
按照GJB2502《航天器热控涂层试验方法》进行测试:所述低应力耐湿热复合热控薄膜的太阳吸收率为0.14,红外发射率为0.7,膜层附着力大于4N/cm,50℃湿热试验24h满足不脱落。
实施例2
一种低应力耐湿热复合热控薄膜的制备方法,所述方法步骤如下:
(1)使用离子源对工件表面进行活化处理,离子源活化电源为电流工作模式,控制电流大小为1.70A,功率为850W,处理时间30s。
(2)采用溅射方式镀制Al反射率层:溅射压力为0.35Pa,溅射功率为4000W,沉积时间10s,得到膜厚为150nm的Al反射率层。
(3)采用孪生靶中频反应磁控溅射镀制Al2O3过渡层:溅射压力0.35Pa,溅射功率5000W,沉积时间45min,得到膜厚为750nm的Al2O3过渡层。
(4)采用孪生靶中频反应磁控溅射镀制SiO2发射率层:其中溅射压力为0.7Pa,溅射功率为6000W下,沉积时间8min,得到膜厚为200nm的疏松SiO2内层,在溅射压力为0.2Pa,溅射功率为1000W下,沉积时间18min,制备得到膜厚为150nm的致密SiO2外层;
(5)采用直流磁控溅射方法镀制ITO导电层:溅射压力为0.35Pa,溅射功率为2000W,沉积时间10s,得到膜厚为40nm的ITO导电层。
按照GJB2502《航天器热控涂层试验方法》进行测试:所述低应力耐湿热复合热控薄膜的太阳吸收率为0.29,红外发射率为0.30,膜层附着力大于4N/cm,50℃湿热试验24h满足不脱落。
实施例3
一种低应力耐湿热复合热控薄膜的制备方法,所述方法步骤如下:
(1)使用离子源对工件表面进行活化处理,离子源活化电源为电流工作模式,控制电流大小为1.70A,功率为850W,处理时间30s。
(2)采用溅射方式镀制Al反射率层:溅射压力为0.35Pa,溅射功率为4000W,得到膜厚为150nm的Al反射率层。
(3)采用孪生靶中频反应磁控溅射镀制Al2O3过渡层:溅射压力0.35Pa,溅射功率5000W,得到膜厚为膜厚150nm的Al2O3过渡层。
(4)采用孪生靶中频反应磁控溅射镀制SiO2发射率层:其中溅射压力为0.8Pa,溅射功率为8000W下,得到膜厚为16μm的疏松SiO2内层,在溅射压力为0.4Pa,溅射功率为5000W下,得到膜厚为3μm的致密SiO2外层;
(5)采用直流磁控溅射方法镀制ITO导电层:溅射压力为0.35Pa,溅射功率为2000W,沉积时间10s,得到膜厚为40nm的ITO导电层。
按照GJB2502《航天器热控涂层试验方法》进行测试:所述低应力耐湿热复合热控薄膜的太阳吸收率为0.14,半球发射率为0.75,膜层附着力大于4N/cm,50℃湿热试验24h满足不脱落。
综上所述,发明包括但不限于以上实施例,凡是在本发明的精神和原则之下进行的任何等同替换或局部改进,都将视为在本发明的保护范围之内。
Claims (5)
1.一种低应力耐湿热复合热控薄膜,其特征在于:所述薄膜包括依次沉积在基底上的反射率层、过渡层、发射率层和导电层;其中,过渡层为Al2O3,厚度150nm~3μm;发射率层由依次沉积在过渡层上的SiO2内层和SiO2外层组成,SiO2外层的致密度高于SiO2内层;当150nm<发射率层厚度<750nm时,SiO2外层的厚度为150nm;当发射率层厚度≥750nm时,SiO2内层为发射率层厚度的80~90%,SiO2外层为发射率层厚度的10~20%。
2.如权利要求1所述的一种低应力耐湿热复合热控薄膜,其特征在于:所述发射率层的厚度为350nm~20μm。
3.如权利要求1所述的一种低应力耐湿热复合热控薄膜,其特征在于:所述反射率层为Al。
4.如权利要求1所述的一种低应力耐湿热复合热控薄膜,其特征在于:所述导电层为ITO。
5.一种如权利要求1~4任意一项所述的低应力耐湿热复合热控薄膜的制备方法,其特征在于:所述方法步骤如下:
(1)使用离子源对工件表面进行活化处理,然后采用磁控溅射法在工件表面镀制反射率层;
(2)采用孪生靶中频反应磁控溅射镀制Al2O3过渡层;
(3)采用孪生靶中频反应磁控溅射镀制SiO2发射率层,其中在工作气压为0.7~1.0Pa,溅射功率为6000~9000W下制备SiO2内层,在工作气压为0.2~0.7Pa,溅射功率为1000~6000W下制备SiO2外层;
(4)采用直流磁控溅射方法镀制导电层。
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