CN106868458A - 一种宽带热调控红外吸波结构材料及其制备方法 - Google Patents
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Abstract
发明属于红外人工电磁超材料领域,更具体的,涉及一种宽带热调控红外吸波结构材料及其制备方法。本发明是利用相变材料氧化钒的可逆金属‑半导体相变特性和高介电常数特性,合理地设计结构参数,使得“三明治”结构的磁谐振吸收峰和介质层的驻波吸收峰交叠耦合在一起,从而在中远红外波段实现宽带可调吸收。
Description
技术领域
本发明属于红外人工电磁超材料领域,更具体的,涉及一种宽带热调控红外吸波结构材料及其制备方法。
背景技术
随着人工电磁超材料的迅速发展,相比传统电磁材料,红外人工电磁超材料因其具有负折射率、完美吸收和选择吸收等特性而受到越来越多的关注。宽带吸收一直以来都是红外人工电磁超材料的研究重点,传统的电磁材料实现宽带吸收主要通过多层结构、几何渐变结构以及特殊的色散媒质等方式。然而,由于红外波段的电磁波波长处于微米级别,多层结构和几何渐变结构都对工艺有极高的要求,尤其是在薄膜的厚度控制和每层结构的图形制作方面,要求精度更高、工艺兼容性好,然而能够实现的带宽却往往有限。对于特殊色散媒质的宽带红外吸收的研究,由于对媒质色散特性要求较高,人为控制难度较大,因此大多数还停留在理论阶段。传统宽带红外人工电磁超材料的另外一个局限是,一旦结构确定后,其吸波性能也就确定了,这样的性能已经难以满足现在对新型人工电磁超材料的要求了,而且在其实际的应用价值也会因此降低。
因此,现有技术的红外人工电磁材料存在工艺复杂,吸波带宽不可调等缺陷。
发明内容
本发明的目的在于提供一种制备工艺简单,吸波带宽可调的一种宽带热调控红外吸波结构材料及其制备方法。
为解决上述技术问题,本发明提供的技术方案是,一种宽带热调控红外吸波结构材料,由下至上包括TiN薄膜、VO2薄膜、Al2O3薄膜和Al2O3薄膜上的图形层;所述TiN薄膜的厚度大于红外波段电磁波在TiN中的趋肤深度,VO2薄膜的厚度为500nm~700nm,Al2O3薄膜的厚度为100nm~200nm,所述超材料由超材料单元结构周期性排列而成,图形层的单元结构为金属圆柱,金属圆柱直径为2μm~2.4μm,高为50nm~100nm,每个单元结构与相邻最近的单元结构的几何中心距为5μm。
所述图形层的材料为铝、铜、金或银。
上述宽带热调控红外吸波结构材料的制备方法,包括如下步骤:
1)通过薄膜沉积技术在衬底上沉积一层TiN薄膜,TiN薄膜厚度大于红外波段电磁波在TiN中的趋肤深度;再在TiN薄膜上沉积一层厚度为500nm~700nm的VO2薄膜;
2)将沉积好TiN薄膜和VO2薄膜的衬底置于热处理设备中在480℃~500℃下热处理50~100分钟,热处理氧气压为150Pa~200Pa;热处理完成后自然冷却至室温;
3)将热处理后的衬底置于薄膜沉积设备中,在VO2薄膜再沉积一层厚度为100nm~200nm的Al2O3薄膜;
4)通过光刻技术,在Al2O3薄膜上制得一层厚度为0.5μm~1μm的光刻胶膜,光刻胶膜上具有周期排列的圆孔,圆孔直径为2μm~2.4μm,每个圆孔与相邻最近的圆孔的圆心距为5μm;
5)通过薄膜沉积技术,在胶膜上沉积一层厚度为50nm~100nm的金属薄膜,沉积完毕后将样品置于丙酮溶液中进行超声清洗将光刻胶剥离,得到目标宽带热调控红外吸波结构材料。
本发明的有益效果是:
本发明是利用相变材料氧化钒(VO2)的可逆金属-半导体相变特性(MIT)和高介电常数特性,合理地设计结构参数,使得“三明治”结构的磁谐振吸收峰和介质层的驻波吸收峰交叠耦合在一起,从而在中远红外波段实现宽带可调吸收。
附图说明
图1为宽带热调控红外吸波结构材料中一个周期单元的结构模型;
图2为宽带热调控红外吸波结构材料的俯视图;
图3为室温下通过FTIR测得的实施例1的反射率曲线;
图4为在温度从30℃升至85℃的过程中,样品在对应温度下的反射率曲线;
图5为变温测试结果,其中5(a)为升温和降温过程中磁谐振峰位置随温度的变化,图5(b)为升温和降温过程中,在驻波位置(λ=7.8μm)反射率随温度的变化。
具体实施方式
实施例1:
本发明提供的一种宽带热调控红外吸波结构材料,由下至上包括TiN薄膜、VO2薄膜、Al2O3薄膜和Al2O3薄膜上的图形层;所述TiN薄膜的厚度为500nm,VO2薄膜的厚度为550nm,Al2O3薄膜的厚度为200nm,所述超材料为超材料单元结构周期性排列而成,图形层的单元结构为铝圆柱,铝圆柱直径为2μm,高为50nm,每个单元结构与相邻最近单元结构的几何中心距为5μm。
宽带热调控红外吸波结构材料的制备
本实施例采用的是表面已制备好一层TiN薄膜的Si基片,TiN厚度为500nm;
1)将清洗过的基片通过脉冲激光沉积技术在TiN薄膜上沉积厚度为550nm的VO2薄膜。沉积工艺参数为:腔体真空度为5×10-5Pa,激光能量为500mJ,激光次数为30000次,靶基距为5cm,沉积氧气压为0.86Pa;
2)VO2薄膜沉积完成后,将样品置于热处理设备中,热处理温度为480℃,氧气压为180Pa,热处理时间为50分钟,热处理完毕后自然冷却至室温;
3)将热处理后的样品置于电子束蒸发镀膜机中,在VO2薄膜上沉积厚度为200nm的Al2O3薄膜;沉积工艺参数为:腔体真空度为6x 10-4Pa,束流70mA;
4)通过光刻技术,在Al2O3薄膜上制得一层光刻胶膜,光刻胶膜上具有周期排列的圆孔,圆孔直径为2μm,圆孔深度为50nm,每个圆孔与相邻最近的圆孔的圆心距为5μm;光刻胶采用AZ5214光刻胶,涂胶转速为3000r/min,甩胶完成后在100℃的温度下前烘60s,装载好掩膜版采用接触式曝光,曝光时间为2.5s,曝光后进行后烘,后烘90s,温度为120℃,后烘后进行120s的泛曝,最后进行显影,显影时间为40s;
5)在步骤5中光刻好图形的胶膜上通过电子束蒸发镀膜的方法沉积厚度为50nm的均匀Al薄膜。工艺参数为:腔体真空度为6×10-4Pa,束流230mA。
6)将经过步骤1)-5)制备的样品置于丙酮溶液中清洗掉光刻胶后用酒精冲洗后吹干,得到最终的宽带热调控红外吸波结构的样品。
测试流程:
将背景样品(Au薄膜)放置在恒温控制台中央,设置傅里叶红外光谱分析仪的测试条件为TEM波垂直入射,测试内容为反射,然后测试背景曲线。
取下背景样品,将上述所制得的样品放置在恒温控制台中央。首先测试样品不同区域的几个点的反射率,检查样品的均匀性是否良好。
然后开始逐渐升温,逐渐加热样品从30℃到85℃度(氧化钒的相变特征温度约为68℃)。待样品温度温度后,测试每一个温度点在2μm~15μm波段的反射率曲线。然后降温,采用同样的方式测试降温过程中的反射率曲线。
如图3所示,在室温下测试得到样品在6.8μm~9.8μm波段范围得吸收率在80%以上,即在中远红外波段存在一个带宽为2.9μm、吸收率80%以上的宽带吸收峰。图4和图5的变温测试结果显示,样品的吸收谱会随着温度的改变而改变,同时当温度降低后,样品的吸收谱又恢复到升温之前的状态,即该发明具还有可逆温度调控的效果。
综上,该发明设计方便、制作工艺简单,能够在中远红外波段实现宽带吸收,并且其吸收性能能够受外界温度的调控,在红外传感、红外成像等相关技术领域具有较大的潜在应用价值。
Claims (3)
1.一种宽带热调控红外吸波结构材料,其特征在于,由下至上包括TiN薄膜、VO2薄膜、Al2O3薄膜和Al2O3薄膜上的图形层;所述TiN薄膜的厚度大于红外波段电磁波在TiN中的趋肤深度,VO2薄膜的厚度为500nm~700nm,Al2O3薄膜的厚度为100nm~200nm,所述超材料由超材料单元结构周期性排列而成,图形层的单元结构为金属圆柱,金属圆柱直径为2μm~2.4μm,高为50nm~100nm,每个单元结构与相邻最近的单元结构的几何中心距为5μm。
2.如权利要求1所述的宽带热调控红外吸波结构材料,其特征在于,所述图形层的材料为铝、铜、金或银。
3.如权利要求1所述宽带热调控红外吸波结构材料的制备方法,其特征在于,包括如下步骤:
1)通过薄膜沉积技术在衬底上沉积一层TiN薄膜,TiN薄膜厚度大于红外波段电磁波在TiN中的趋肤深度;再在TiN薄膜上沉积一层厚度为500nm~700nm的VO2薄膜;
2)将沉积好TiN薄膜和VO2薄膜的衬底置于热处理设备中在480℃~500℃下热处理50~100分钟,热处理氧气压150Pa~200Pa;处理完成后自然冷却至室温;
3)将热处理后的衬底置于薄膜沉积设备中,在VO2薄膜再沉积一层厚度为100nm~200nm的Al2O3薄膜;
4)通过光刻技术,在Al2O3薄膜上制得一层厚度为0.5μm~1μm的光刻胶膜,光刻胶膜上具有周期排列的圆孔,圆孔直径为2μm~2.4μm,每个圆孔与相邻最近的圆孔的圆心距为5μm;
5)通过薄膜沉积技术,在胶膜上沉积一层厚度为50nm~100nm的金属薄膜,沉积完毕后将样品置于丙酮溶液中进行超声清洗将光刻胶剥离,得到目标宽带热调控红外吸波结构材料。
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CN107907237A (zh) * | 2017-11-15 | 2018-04-13 | 江西师范大学 | 一种光学吸收型温度传感器 |
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