CN108866483B - 一种智能热控器件及其制备方法 - Google Patents

一种智能热控器件及其制备方法 Download PDF

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CN108866483B
CN108866483B CN201810673033.0A CN201810673033A CN108866483B CN 108866483 B CN108866483 B CN 108866483B CN 201810673033 A CN201810673033 A CN 201810673033A CN 108866483 B CN108866483 B CN 108866483B
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刘东青
彭任富
程海峰
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National University of Defense Technology
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Abstract

本发明公开了一种智能热控器件，为多层复合结构，从下至上依次为反射层、介质层、相变层和吸收率调控层，所述多层复合结构位于基底层上。本发明的制备方法为：(1)采用采用物理气相沉积法在基底上制备反射层；(2)在反射层表面，采用物理气相沉积法方法制备介质层；(3)采用磁控溅射方法在介质层表面制备二氧化钒薄膜相变层；(4)在相变层上覆一层吸收率调控层，即得到智能热控器件。本发明制备的智能热控器件发射率变化范围大，对温度的调控效果好，而且高温时对应的高发射率大于0.8，有利于降低热控器件的面积，提高功能密度；同时对太阳光的吸收率小于0.3，可保证器件的智能调节能力，基本满足航天器热控的实际需求。

Description

一种智能热控器件及其制备方法
技术领域
本发明属于航天器热控技术领域，尤其涉及一种智能热控器件及其制备方法。
背景技术
在轨道空间环境中，航天器内部与外空间环境的主要热交换方式为热辐射。由于外部环境温度波动范围大，为使航天器内部的温度处于合适的范围，保证各设备部件的正常工作，必须采用有效的热控技术。目前在航天器上采用的热控手段主要是使用热控涂层、百叶窗、热管等复杂装置，但这些装置存在体积和重量大、能耗多以及机械移动装置复杂等缺点，严重影响了航天器的有限载荷能力。
近年来人们关注的最多的是智能热控器件，该器件进行温度调控的关键是具有热致变发射率特性的薄膜，其发射率可随外部环境温度的变化而变化，从而主动调节航天器部件的温度。低温时，智能热控器件的发射率较低，减少热量辐射损耗；高温时，智能热控器件的发射率较高，通过热辐射的方式把多余的热量辐射出去。而且，智能热控器件主要是基于薄膜技术，其重量较轻，可以方便直接集成到航天器的现有部件上。
发射率变化量和太阳吸收率是衡量智能热控器件能否应用于航天器中的两个重要的性能指标。发射率变化量越大，智能热控器件对温度调控的效果越好。但是当太阳照射时，过高的太阳吸收率会使得器件的温度急剧升高，从而对于航天器部件温度的变化丧失智能调节能力，因此需要在保证发射率变化量大的情况下尽可能的降低太阳吸收率。而现有的智能热控器件发射率变化量仍相对较小、太阳吸收率较高，且复杂的结构使得制备过程较为困难，难以满足航天器热控的实际需求。
发明内容
本发明所要解决的技术问题是，克服以上背景技术中提到的不足和缺陷，提供一种智能热控器件及其制备方法。
为解决上述技术问题，本发明提出的技术方案为：
一种智能热控器件，所述智能热控器件为多层复合结构，从下至上依次为反射层、介质层、相变层和吸收率调控层，所述多层复合结构位于基底层上；其中，所述介质层为硫化锌薄膜、氧化镁薄膜、氧化铝薄膜、氟化钡薄膜、氟化镁薄膜、氟化钙薄膜、氟化锂薄膜或锗薄膜。
上述的智能热控器件，优选的，所述反射层为钨薄膜、金薄膜、银薄膜、铝薄膜、铜薄膜、铂薄膜或氧化铟锡薄膜。
上述的智能热控器件，优选的，所述相变层为二氧化钒薄膜。
上述的智能热控器件，优选的，所述吸收率调控层为掺杂纳米介质的三元乙丙薄膜、聚乙烯薄膜、氟碳树脂薄膜或聚丙烯薄膜；所述纳米介质为硫化锌、硒化锌、氧化锌、氧化钛、氧化锰、氧化镁和氧化锆中的一种或几种。进一步优选的，所述吸收率调控层为掺杂氧化镁颗粒的纳米聚乙烯膜。掺杂纳米介质可以调节可见近红外光的吸收率，适当的纳米介质的掺杂有利于增强吸收率调控层的反射，降低太阳光吸收。
上述的智能热控器件，优选的，所述反射层的厚度为50nm～500nm；所述介质层的厚度为300nm～1500nm；所述相变层的厚度为10nm～80nm；所述吸收率调控层的厚度为1μm～20μm。进一步优选的，所述反射层的厚度为300nm～500nm；所述介质层的厚度为1000nm～1300nm；所述相变层的厚度为20nm～40nm；所述吸收率调控层的厚度为1μm～5μm。
上述的智能热控器件，优选的，所述基底为玻璃片、硅片或金属片。
本发明的智能热控器件，在最下层设置一层反射层，可保证相变层二氧化钒发射率变化趋势符合热控的需求，即低温时低发射，减少目标自身热量损失；高温时高发射，目标向外辐射出多余的热量，降低自身的热量，此种结构虽然发射率变化趋势符合热控需求，但发射率变化量太小，而且二氧化钒本身的颜色较深，容易吸收太阳光，不利于温度的调控，因此需要调节发射率变化量(尽可能大)和太阳吸收率(尽可能小)。基于此，本发明在反射层和相变层之间加一层介质层，通过介质层可调节发射率变化量，低温时，介质层/相变层是红外透明的，而底下的反射层是红外高反射的，因此低温时整个结构处于高反射的状态，此时发射率较低；高温时，相变层发生相变，介质层/相变层是红外半透明的，此时介质层/相变层的吸收和表面反射都增加，同时通过合理设计两个膜层的厚度，经过多次反射和吸收，在某些波长处由于干涉相消现象将出现反射率大幅降低，从而使结构处于高发射率的状态，从而实现对发射率变化量的调节。由于此时最表面的膜层还是二氧化钒层，二氧化钒薄膜为蓝黑色，颜色较深导致太阳吸收很强，有可能使整个器件结构一直吸收热量从而始终处于相变后的状态，从而丧失了温度调节能力，因此本发明在尽可能不影响发射率变化量的基础上降低太阳吸收率，在相变层上设计了一层吸收率调节层。
作为一个总的发明构思，本发明还提供一种智能热控器件的制备方法，包括以下步骤：
(1)采用采用物理气相沉积法(电子束蒸发、磁控溅射)在基底上制备反射层；
(2)在步骤(1)制备的反射层表面，采用物理气相沉积法(电子束蒸发、磁控溅射)方法制备一层介质层；
(3)采用磁控溅射方法在介质层表面制备一层二氧化钒薄膜相变层；
(4)在所述相变层上覆一层吸收率调控层，即得到所述智能热控器件。
上述的制备方法，优选的，步骤(3)中，磁控溅射的工艺条件为：以金属钒靶为溅射靶材，反应气体为氧气，溅射气体为氩气，本底真空小于1×10为2％～3％。由于钒的氧化态多达二十多种，要准备出纯的二氧化钒的很难，申请人发现，只有在同时满足这些条件时，才可制备出纯的二氧化钒薄膜，才具有相变性质。
上述的制备方法，优选的，步骤(4)中，吸收率调控层的制备方式是先将纳米介质与三元乙丙、聚乙烯、氟碳树脂或聚丙烯混合，然后以喷涂、刮涂或旋涂覆在相变层上；或者将纳米介质与三元乙丙、聚乙烯、氟碳树脂或聚丙烯混合，先以喷涂、刮涂或者旋涂的方式覆在其他基底(如硅片、玻璃片)上，然后将得到的薄膜贴附在相变层上；其中，吸收率调控层中纳米介质的掺杂量(质量比)为1％～5％。
上述的制备方法，优选的，步骤(2)中，所述物理气相沉积法为电子束蒸发时，电子束蒸发的工艺条件为：腔室压力小于1×10-5Torr，样品台温度为250℃～350℃，蒸发速率为
Figure BDA0001709028550000031
温度低于250℃，由于应力存在薄膜容易脱落、质量不好，高于350℃时，浪费能量，温度在250℃～350℃，即可保证制备出的薄膜质量好，又不会浪费能量；同时蒸发速率太小，会导致制备时间长，浪费时间，但是蒸发速率过大，又会造成薄膜均匀性变差、质量不好，选择
Figure BDA0001709028550000032
的速率制备薄膜最合适。
与现有技术相比，本发明的优点在于：
(1)本发明制备的智能热控器件发射率变化范围大，对温度的调控效果好，而且高温时对应的高发射率大于0.8，有利于降低热控器件的面积，提高功能密度；同时对太阳光的吸收率小于0.3，可保证器件的智能调节能力，基本满足航天器热控的实际需求。
(2)本发明通过精确控制各个膜层的厚度，有效降低了器件的重量，有利于减少对航天器载荷能力的干扰。
(3)本发明提供的智能热控器件结构简单，容易实现大规模制备。
附图说明
图1为本发明智能热控器件的结构示意图。
图2为本发明实施例1智能热控器件在不同温度下的发射率变化曲线。
图3为本发明实施例1智能热控器件的反射光谱曲线。
图例说明：1、反射层；2、介质层；3、相变层；4、吸收率调控层。
具体实施方式
为了便于理解本发明，下文将结合说明书附图和较佳的实施例对本文发明做更全面、细致地描述，但本发明的保护范围并不限于以下具体实施例。
除非另有定义，下文中所使用的所有专业术语与本领域技术人员通常理解含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的，并不是旨在限制本发明的保护范围。
除非另有特别说明，本发明中用到的各种原材料、试剂、仪器和设备等均可通过市场购买得到或者可通过现有方法制备得到。
实施例1：
一种本发明的智能热控器件，其结构图如图1所示，为四层复合结构，所述复合结构覆在硅基底上，复合结构从下至上依次为反射层1(厚度为300nm的金薄膜)、介质层2(厚度为1000nm的氟化镁薄膜)、相变层3(厚度为30nm的二氧化钒薄膜)和吸收率调控层4(厚度为5μm的掺杂氧化镁颗粒的纳米聚乙烯膜)。
本实施例的智能热控器件的制备方法，包括以下步骤：
(1)采用电子束蒸发方法在硅基底上制备厚度为300nm的金薄膜；
(2)采用电子束蒸发方法在步骤(1)制备的金薄膜上制备厚度为1000nm的氟化镁薄膜，电子束蒸发的工艺条件为腔室压力小于1×10-5Torr，样品台温度为250℃，蒸发速率为
Figure BDA0001709028550000041
(3)采用磁控溅射方法在步骤(2)制备的氟化镁薄膜上制备厚度为30nm的二氧化钒薄膜，磁控溅射的工艺条件为以金属钒靶为溅射靶材，反应气体为氧气，溅射气体为氩气，本底真空小于1×10-6Torr，溅射温度为500℃，溅射压力为8mTorr，溅射功率为100W，反应气体比例为2％；
(4)将纳米氧化镁颗粒合聚乙烯树脂混合(氧化镁掺杂量为1％)，然后以旋涂的方式将其覆在二氧化钒薄膜上，控制掺杂氧化镁颗粒的纳米聚乙烯膜厚度为5μm，完成智能热控器件的制备。
图2为本实施例1中智能热控器件在不同温度下的发射率变化曲线，由图2可知，当温度从30℃变到100℃时，该器件在3μm～14μm波段发射率变化量约为0.33。图3为本实施例中智能热控器件的吸收光谱曲线，由图3可知，该器件的平均太阳吸收率小于0.28。
实施例2：
一种本发明的智能热控器件，如图1所示，为四层复合结构，复合结构覆在硅基底上，复合结构从下至上依次为反射层1(厚度为100nm的铝薄膜)，介质层2(厚度为680nm的硫化锌薄膜)，相变层3(厚度为60nm的二氧化钒薄膜)和吸收率调控层4(厚度为1μm的掺杂氧化钛颗粒的氟碳树脂薄膜)。
本实施例的智能热控器件的制备方法，包括以下步骤：
(1)采用磁控溅射方法在硅基底上制备厚度为100nm铝薄膜；
(2)采用电子束蒸发方法在步骤(1)制备的铝薄膜上制备厚度为680nm的硫化锌介质层，电子束蒸发的工艺条件为腔室压力小于1×10-5Torr，样品台温度为350℃，蒸发速率为
Figure BDA0001709028550000042
(3)采用磁控溅射方法在步骤(2)制备的氟化镁薄膜制备厚度为60nm的二氧化钒薄膜，磁控溅射的工艺条件为以金属钒靶为溅射靶材，反应气体为氧气，溅射气体为氩气，本底真空小于1×10-6Torr，溅射温度为650℃，溅射压力为10mTorr，溅射功率为200W，反应气体比例为3％；
(4)将纳米氧化钛颗粒和氟碳树脂树脂混合(氧化钛掺杂量为5％)，然后以刮涂的方式将其刮涂在二氧化钒薄膜上，控制掺杂氧化钛颗粒的氟碳树脂膜厚度为1μm，完成智能热控器件的制备。
当温度从30℃变到100℃时，本实施例制备得到的热控器件在3μm～14μm波段发射率变化量约为0.31，平均太阳吸收率小于0.27。

Claims (7)

1.一种智能热控器件，其特征在于，所述智能热控器件为多层复合结构，从下至上依次为反射层、介质层、相变层和吸收率调控层，所述多层复合结构位于基底层上；其中，所述介质层为硫化锌薄膜、氧化镁薄膜、氧化铝薄膜、氟化钡薄膜、氟化镁薄膜、氟化钙薄膜、氟化锂薄膜或锗薄膜；
所述吸收率调控层为掺杂纳米介质的三元乙丙薄膜、聚乙烯薄膜、氟碳树脂薄膜或聚丙烯薄膜；所述纳米介质为硫化锌、硒化锌、氧化锌、氧化钛、氧化锰、氧化镁和氧化锆中的一种或几种；
所述反射层的厚度为50nm～500nm；所述介质层的厚度为300nm～1500nm；所述相变层的厚度为10nm～80nm；所述吸收率调控层的厚度为1μm～20μm。
2.如权利要求1所述的智能热控器件，其特征在于，所述基底为玻璃片、硅片或金属片。
3.如权利要求1所述的智能热控器件，其特征在于，所述反射层为钨薄膜、金薄膜、银薄膜、铝薄膜、铜薄膜、铂薄膜或氧化铟锡薄膜。
4.如权利要求1所述的智能热控器件，其特征在于，所述相变层为二氧化钒薄膜。
5.一种如权利要求1～4任一项所述的智能热控器件的制备方法，其特征在于，包括以下步骤：
(1)采用物理气相沉积法在基底上制备反射层；
(2)在步骤(1)制备的反射层表面，采用物理气相沉积法制备一层介质层；
(3)采用磁控溅射方法在介质层表面制备一层二氧化钒薄膜相变层；
(4)在所述相变层上覆一层吸收率调控层，即得到所述智能热控器件。
6.如权利要求5所述的制备方法，其特征在于，步骤(3)中，磁控溅射的工艺条件为：以金属钒靶为溅射靶材，反应气体为氧气，溅射气体为氩气，本底真空小于1×10-6Torr，溅射温度为500℃～650℃，溅射压力为8mTorr～10mTorr，溅射功率为100W～200W，反应气体体积比例为2％～3％。
7.如权利要求5所述的制备方法，其特征在于，所述物理气相沉积法为电子束蒸发法或磁控溅射法。
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