CN108950492B - 一种具有光限幅性能的vo2复合薄膜的制备方法 - Google Patents

一种具有光限幅性能的vo2复合薄膜的制备方法 Download PDF

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CN108950492B
CN108950492B CN201810741672.6A CN201810741672A CN108950492B CN 108950492 B CN108950492 B CN 108950492B CN 201810741672 A CN201810741672 A CN 201810741672A CN 108950492 B CN108950492 B CN 108950492B
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田野
曹雪
罗飞
刘大博
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AECC Beijing Institute of Aeronautical Materials
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Abstract

本发明属于功能薄膜技术领域，具体涉及一种应用于激光防护技术的VO2复合薄膜的制备方法。本发明基于表面等离激元共振技术在VO2薄膜表面制备一层粒径均一的、尺寸可调的Au/SiO2或Ag/SiO2纳米结构层，有效地提升了薄膜的激光防护性能。同传统的纯VO2激光防护薄膜相比，这种薄膜具有更低的激光可透过率以及更高的耐激光损伤阈值。该工艺可以有效提高薄膜对激光的响应度以及耐激光辐射能力，其制备过程简单可控，不需要昂贵的设备，同时对VO2薄膜的尺寸、形貌无特殊要求，为VO2基激光防护薄膜提供了一种高效率、短周期、可工业化实施的新技术。

Description

一种具有光限幅性能的VO2复合薄膜的制备方法
技术领域
本发明属于功能薄膜技术领域，具体涉及一种应用于激光防护技术的VO2复合薄膜的制备方法。
背景技术
随着激光干扰与致盲武器的迅速发展，寻找一种适用于激光防护的新型材料，保护军事人员和各种光电探测***不受打击，已成为亟需解决的重要问题。1959年，Morin首次发现钒和钛的氧化物具有半导体-金属相变特性，即在半导体态时，材料具有高透射特性；在金属态时，材料则具有高反射特性。这种特性使其具有智能光限幅开关的潜力。同其它激光防护材料相比，VO2具有防护波段宽，制备成本低，性能稳定等优点，是智能激光防护材料的研究热点，在航空航天领域有着广泛的应用潜力。
在材料制备方面，研究者通过各种方法如：溶胶-凝胶，磁控溅射，脉冲激光沉积，化学气相沉积，反应蒸镀等制备了VO2薄膜，并对薄膜的组分、形貌、相变温度、电学及光学性能进行了研究。虽然相关科研单位已经开展了大量研究工作，但由于钒氧体系的复杂性和纯VO2薄膜相变温度较高等关键问题尚没有完全解决，严重阻碍了VO2薄膜的实际应用。
表面等离子体共振(SPR)是一种新型的光波操控手段，目前已经在化工、医疗、材料、食品、环境等诸多领域有着广泛的应用。通过在传统薄膜表面复合Au、Ag等有序纳米结构，会使其表现出许多奇异的光学性质，比如局域电场增强效应、纳米天线效应、强烈的光散射、光吸收以及光热特性等(M.Rycenga,C.M.Cobley,J.Zeng,W.Y.Li,C.H.Moran,Q.Zhang,D. Qin,and Y.N.Xia,"Controlling the Synthesis and Assembly of SilverNanostructures for Plasmonic Applications",Chem.Rev.,2011,111:3669-3712)。但是，关于复合有贵金属纳米颗粒的VO2光限幅薄膜却一直未见报道。其主要技术瓶颈在于一方面表面等离子体共振技术的有效实施需要Au和Ag等纳米材料的粒径具有良好的均一性；另一方面，表面等离子体共振技术的有效实施需要对Au或Ag等贵金属纳米结构实现尺寸可调控，这进一步增加了材料的复合难度。因此，如果能在VO2薄膜表面制备粒径均一的，尺寸可调的Au、Ag纳米结构，利用材料的表面等离子体共振特性提升VO2薄膜的激光防护能力，无疑是一条制备VO2基光限幅薄膜的有效途径。
发明内容
为了解决已有的光限幅VO2薄膜在制备过程中存在的问题，本发明提供了一种具有光限幅性能的VO2复合薄膜的制备方法。
其工艺过程为：
1)以金属钒靶作为溅射源，在氩气条件下在洁净石英衬底上溅射200nm厚的金属V膜，衬底温度保持在200℃，溅射时间为60min，溅射功率为150W；
2)将溅射有V膜的基片放置在管式炉中，通入氮氧混合气进行退火，其中氮气与氧气的比例是10：1，退火温度为480℃，退火时间60min，冷却至室温后取出；
3)将50ml无水乙醇，7ml去离子水，7ml浓氨水混合，搅拌均匀得到反应溶液；在40℃恒温水浴中，将5～20ml正硅酸乙酯缓慢滴加至上述溶液中，搅拌反应30min，反应24h。反应完毕后用无水乙醇反复离心，洗涤，再经超声分散即得到SiO2微球溶液。
4)利用旋涂仪将上述SiO2微球溶液均匀涂覆于VO2薄膜表面，具体参数为先进行低速旋涂，速度为300转/分钟，旋涂时间10s，再进行高速旋涂，速度为1000转/分钟，旋涂时间30s。随后在空气下进行150℃热处理1h定型成膜。
5)以Au靶或Ag靶作为溅射源，在氩气条件下在上述薄膜上溅射Au膜或Ag膜，衬底温度保持在150℃，溅射时间为2min，溅射功率为50W。即得到所需的VO2复合薄膜。
本发明具有的优点和有益效果
本发明开发了一种具有光限幅性能的VO2复合薄膜的制备方法。基于表面等离激元共振技术在VO2薄膜表面制备一层粒径均一的，尺寸可调的Au/SiO2或Ag/SiO2纳米结构层，有效地提升了薄膜的激光防护性能。同传统的纯VO2激光防护薄膜相比，这种薄膜具有更低的激光可透过率以及更高的耐激光损伤阈值。该工艺可以有效提高薄膜对激光的响应度以及耐激光辐射能力，其制备过程简单可控，不需要昂贵的设备，同时对VO2薄膜的尺寸、形貌无特殊要求，为VO2基激光防护薄膜提供了一种高效率、短周期、可工业化实施的新技术。利用本发明方法制备的VO2复合薄膜具有如下优点：
1.Au/SiO2或Ag/SiO2纳米结构层的粒径均一性高，且颗粒尺寸可实现连续调节。
2.Au/SiO2或Ag/SiO2纳米结构层具有表面等离子体共振特性，在激光辐射下，Au或Ag纳米结构层的光热效应会产生大量热能，从而使VO2薄膜的表面温度更快升至相变温度，缩短薄膜的相变响应时间，弥补薄膜自身的热滞效应缺陷。
3.在Au/SiO2或Ag/SiO2纳米结构层的强散射作用下，激光束在VO2薄膜内的传播长度被大大增加，使激光辐照下的薄膜表面温度场更加均匀，利于VO2薄膜快速向金属态转变。
4.Au/SiO2或Ag/SiO2纳米结构层与基层VO2薄膜具有良好的结合性和兼容性，在不影响VO2薄膜固有性能的前提下，可以大幅降低该VO2复合薄膜的激光可透过率，同时大幅提升薄膜的耐激光损伤阈值。
5.制备工艺简单，无需昂贵的设备，可方便实现大面积制备及批量化生产。
附图说明
图1为实施例1中制备的Au/SiO2/VO2复合薄膜的SEM图；
图2为实施例1中制备的Ag/SiO2/VO2复合薄膜的SEM图；
图3为实施例2中制备的Au/SiO2/VO2复合薄膜的SEM图；
图4为实施例2中制备的Ag/SiO2/VO2复合薄膜的SEM图。
具体实施方式
下面结合具体实施例进一步阐述本发明，应理解，这些实施例仅用于说明本发明而不用于限制本发明的保护范围。
实施例1
1)以金属钒靶作为溅射源，在氩气条件下在洁净石英衬底上溅射200nm厚的金属V膜，衬底温度保持在200℃，溅射时间为60min，溅射功率为150W；
2)将溅射有V膜的基片放置在管式炉中，通入氮氧混合气进行退火，其中氮气与氧气的比例是10：1，退火温度为480℃，退火时间60min，冷却至室温后取出；
3)将50ml无水乙醇，7ml去离子水，7ml浓氨水混合，搅拌均匀得到反应溶液；在40℃恒温水浴中，将5ml正硅酸乙酯缓慢滴加至上述溶液中，搅拌反应30min，反应24h。反应完毕后用无水乙醇反复离心，洗涤，再经超声分散即得到SiO2微球溶液。
4)利用旋涂仪将上述SiO2微球溶液均匀涂覆于VO2薄膜表面，具体参数为先进行低速旋涂，速度为300转/分钟，旋涂时间10s，再进行高速旋涂，速度为1000转/分钟，旋涂时间30s。随后在空气下进行150℃热处理1h定型成膜。
5)以Au靶或Ag靶作为溅射源，在氩气条件下在上述薄膜上溅射Au膜或Ag膜，衬底温度保持在150℃，溅射时间为2min，溅射功率为50W。即得到所需的VO2复合薄膜。
图1给出了实施例1制备的Au/SiO2/VO2复合薄膜的SEM照片，可以看到在VO2多晶薄膜表面覆盖着一层较薄的Au/SiO2纳米结构层，Au/SiO2纳米颗粒的粒径在300nm左右，具有较高的球形度和均匀性。紫外-可见吸收光谱的测试结果表明该Au/SiO2纳米结构层具有良好的表面等离激元共振吸收特性。在脉冲激光辐射下，进一步对薄膜的透过率进行比较可以发现，Au/SiO2/VO2复合薄膜在不同脉冲能量下的透过率均低于单一的VO2薄膜。这说明经过Au/SiO2纳米结构层复合的VO2薄膜可以有效降低VO2薄膜的激光可透过率。进一步的相关测试还发现薄膜的耐激光损伤阈值也有了明显的提升，这种激光限幅性能的增强可能是由于Au的表面等离激元共振效应导致的。
图2给出了实施例1制备的Ag/SiO2/VO2复合薄膜的SEM照片，可以看到在VO2多晶薄膜表面覆盖着一层较薄的Ag/SiO2纳米结构层，Ag/SiO2纳米颗粒的粒径在300nm左右，具有较高的球形度和均匀性。紫外-可见吸收光谱的测试结果表明该Ag/SiO2纳米结构层具有良好的表面等离激元共振吸收特性。在脉冲激光辐射下，进一步对薄膜的透过率进行比较可以发现，Ag/SiO2/VO2复合薄膜在不同脉冲能量下的透过率均低于单一的VO2薄膜。这说明经过Ag/SiO2纳米结构层复合的VO2薄膜可以有效降低VO2薄膜的激光可透过率。进一步的相关测试还发现薄膜的耐激光损伤阈值也有了明显的提升，这种激光限幅性能的增强可能是由于Ag的表面等离激元共振效应导致的。
实施例2
1)以金属钒靶作为溅射源，在氩气条件下在洁净石英衬底上溅射200nm厚的金属V膜，衬底温度保持在200℃，溅射时间为60min，溅射功率为150W；
2)将溅射有V膜的基片放置在管式炉中，通入氮氧混合气进行退火，其中氮气与氧气的比例是10：1，退火温度为480℃，退火时间60min，冷却至室温后取出；
3)将50ml无水乙醇，7ml去离子水，7ml浓氨水混合，搅拌均匀得到反应溶液；在40℃恒温水浴中，将20ml正硅酸乙酯缓慢滴加至上述溶液中，搅拌反应30min，反应24h。反应完毕后用无水乙醇反复离心，洗涤，再经超声分散即得到SiO2微球溶液。
4)利用旋涂仪将上述SiO2微球溶液均匀涂覆于VO2薄膜表面，具体参数为先进行低速旋涂，速度为300转/分钟，旋涂时间10s，再进行高速旋涂，速度为1000转/分钟，旋涂时间30s。随后在空气下进行150℃热处理1h定型成膜。
5)以Au靶或Ag靶作为溅射源，在氩气条件下在上述薄膜上溅射Au膜或Ag膜，衬底温度保持在150℃，溅射时间为2min，溅射功率为50W。即得到所需的VO2复合薄膜。
图3给出了实施例2制备的Au/SiO2/VO2复合薄膜的SEM照片，可以看到在VO2多晶薄膜表面覆盖着一层较薄的Au/SiO2纳米结构层，Au/SiO2纳米颗粒的粒径在1μm左右，具有较高的球形度和均匀性。紫外-可见吸收光谱的测试结果表明该Au/SiO2纳米结构层具有良好的表面等离激元共振吸收特性。同图1的结果进行对比可以看到，Au/SiO2的粒径有了明显增大。在脉冲激光辐射下，进一步对薄膜的透过率进行比较可以发现，Au/SiO2/VO2复合薄膜在不同脉冲能量下的透过率均低于单一的VO2薄膜。这说明经过Au/SiO2纳米结构层复合的VO2薄膜可以有效降低VO2薄膜的激光可透过率。进一步的相关测试还发现薄膜的耐激光损伤阈值也有了明显的提升，这种激光限幅性能的增强可能是由于Au的表面等离激元共振效应导致的。
图4给出了实施例2制备的Ag/SiO2/VO2复合薄膜的SEM照片，可以看到在VO2多晶薄膜表面覆盖着一层较薄的Ag/SiO2纳米结构层，Ag/SiO2纳米颗粒的粒径在1μm左右，具有较高的球形度和均匀性。紫外-可见吸收光谱的测试结果表明该Ag/SiO2纳米结构层具有良好的表面等离激元共振吸收特性。同图2的结果进行对比可以看到，Ag/SiO2的粒径有了明显增大。在脉冲激光辐射下，进一步对薄膜的透过率进行比较可以发现，Ag/SiO2/VO2复合薄膜在不同脉冲能量下的透过率均低于单一的VO2薄膜。这说明经过Ag/SiO2纳米结构层复合的VO2薄膜可以有效降低VO2薄膜的激光可透过率。进一步的相关测试还发现薄膜的耐激光损伤阈值也有了明显的提升，这种激光限幅性能的增强可能是由于Ag的表面等离激元共振效应导致的。

Claims (1)

1.一种具有光限幅性能的VO2复合薄膜的制备方法，其特征在于该方法包括下述步骤：
1)以金属钒靶作为溅射源，在氩气条件下在洁净石英衬底上溅射200nm厚的金属V膜，衬底温度保持在200℃，溅射时间为60min，溅射功率为150W；
2)将溅射有V膜的基片放置在管式炉中，通入氮氧混合气进行退火，其中氮气与氧气的比例是10：1，退火温度为480℃，退火时间60min，冷却至室温后取出；
3)将50ml无水乙醇，7ml去离子水，7ml浓氨水混合，搅拌均匀得到反应溶液；在40℃恒温水浴中，将5～20ml正硅酸乙酯缓慢滴加至上述溶液中，搅拌反应30min，反应24h；反应完毕后用无水乙醇反复离心，洗涤，再经超声分散即得到SiO2微球溶液；
4)利用旋涂仪将上述SiO2微球溶液均匀涂覆于步骤2)制得的薄膜表面，具体参数为先进行低速旋涂，速度为300转/分钟，旋涂时间10s，再进行高速旋涂，速度为1000转/分钟，旋涂时间30s，随后在空气下进行150℃热处理1h定型成膜；
5)以Au靶或Ag靶作为溅射源，在氩气条件下在步骤4)制得的薄膜上溅射Au膜或Ag膜，衬底温度保持在150℃，溅射时间为2min，溅射功率为50W，即得到所需的VO2复合薄膜。
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