CN107177823A - 一种具有激光防护性能的Ag/VO2复合薄膜的制备方法 - Google Patents
一种具有激光防护性能的Ag/VO2复合薄膜的制备方法 Download PDFInfo
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Abstract
本发明属于功能薄膜技术领域,具体涉及一种具有激光防护性能的Ag/VO2复合薄膜的制备方法。本发明在VO2多晶薄膜表面涂覆具有表面等离激元共振特性的银纳米线或银纳米颗粒结构层。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
技术领域
本发明属于功能薄膜技术领域,具体涉及一种具有激光防护性能的Ag/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系统不受打击,已成为亟需解决的重要问题。作为一种热致相变材料,VO2可以在不同温度下实现在金属-绝缘体之间的可逆转变。伴随相变的发生,材料的光电特性发生突变,从而实现强光照射时具有低透过率,保护探测器不受损伤,弱光照射时具有高透过率,不影响探测器接收信号。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。
目前,研究者已经采用了多种途径合成了VO2薄膜材料,然而,由于纯净化学计量比的VO2薄膜较难制备并且其相变温度较高,严重阻碍了VO2薄膜的实际应用。目前虽然可以通过优化制备工艺及元素掺杂对其进行调控,但却存在制备周期长,成本高、薄膜的开关特性减弱等很多不利影响。因此,如何制备具有良好激光防护性能的VO2薄膜成为了一个亟需解决的技术难题。
作为一种贵金属纳米材料,银纳米材料由于具有独特的光学、电学和催化特性,在诸多领域有着广泛的应用价值。尤其银纳米材料具有表面等离子体共振效应,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。目前,银纳米材料已被广泛应用于光伏器件、发光器件、探测器件等光电材料中,可以大幅提高器件的工作效率(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 ofSilverNanostructures for Plasmonic Applications",Chem.Rev.,2011,111:3669-3712)。但是,利用表面等离子体共振效应增强激光防护用Ag/VO2复合薄膜却一直未有报道,其相关技术瓶颈主要在于银纳米结构层的厚度及形貌选择存在困难。具体为一方面,银纳米结构层过厚虽然可以大幅降低VO2薄膜的激光可透过率并提升薄膜的耐激光损伤阈值,但是却会严重削弱银纳米结构的表面等离子体共振效应,并且降低VO2薄膜的实际可接收光信号强度。另一方面,银纳米结构层过薄,虽然可以提高银纳米结构自身的表面等离子体共振效应,提升VO2薄膜可接收的光信号强度,但是却无法降低VO2薄膜的激光可透过率,同时很难提高薄膜的耐激光损伤阈值。同理,在银纳米结构层的形貌选择上也存在上述技术困难。因此,恰当选择银纳米结构层的厚度及形貌是激光防护用Ag/VO2复合薄膜的技术难点。
发明内容
为了解决已有的激光防护用VO2薄膜在制备过程中存在的问题,本发明提供了一种具有激光防护性能的Ag/VO2复合薄膜的制备工艺。
一种具有激光防护性能的Ag/VO2复合薄膜的制备工艺,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100nm厚的金属钒膜,衬底温度保持在200℃;
2)将一端敞口的管式退火炉进行升温,到500℃时进行保温,从炉管的非敞口端通入氮气,氮气流量保持在2L/min;
3)将制备的金属钒膜放入石英坩埚中,之后将坩埚推入上述管式退火炉中进行退火,退火时间为10min,到时后拉出坩埚进行快速空气下冷却。得到所需的VO2薄膜。
4)以AgNO3为银源,乙二醇为还原剂,聚乙烯吡咯烷酮为稳定剂和分散剂,利用化学还原反应得到银纳米线或银纳米颗粒产物,随后将产物离心分离并分散到乙醇中,得到浓度为0.5%的银纳米线或银纳米颗粒分散液。
5)利用旋涂仪将上述银纳米线或银纳米颗粒分散液均匀涂覆于VO2薄膜表面,具体参数为先进行低速旋涂,速度为400转/分钟,旋涂时间5s,再进行高速旋涂,速度为2000转/分钟,旋涂时间30s。
6)将涂覆有湿银胶膜的VO2薄膜进行烘干,随后在空气下进行250℃热处理1h定型成膜,即得到所需的Ag/VO2复合薄膜。
利用本发明方法制备的Ag/VO2复合薄膜具有如下优点:
本发明开发了一种具有激光防护性能的Ag/VO2复合薄膜的制备方法。基于表面等离激元共振技术在VO2薄膜表面制备一层银纳米线(AgNW)或银纳米颗粒(AgNP)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。
1.在激光辐射下,银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。
2.在银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。
3.银纳米结构层与基层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Ag/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。
4.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AgNW/VO2复合薄膜的SEM图;
图2为不同脉冲激光能量入射下探测到的VO2薄膜及AgNW/VO2复合薄膜的激光可透过率变化曲线;
图3为实施例2中制备的AgNP/VO2复合薄膜的SEM图;
图4为不同脉冲激光能量入射下探测到的VO2薄膜及AgNP/VO2复合薄膜的激光可透过率变化曲线。
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100nm厚的金属钒膜,衬底温度保持在200℃;
2)将一端敞口的管式退火炉进行升温,到500℃时进行保温,从炉管的非敞口端通入氮气,氮气流量保持在2L/min;
3)将制备的金属钒膜放入石英坩埚中,之后将坩埚推入上述管式退火炉中进行退火,退火时间为10min,到时后拉出坩埚进行快速空气下冷却。得到所需的VO2薄膜。
4)以AgNO3为银源,乙二醇为还原剂,聚乙烯吡咯烷酮为稳定剂和分散剂,HCl为成核控制剂,利用化学还原反应得到银纳米线,将产物离心分离并分散到乙醇中,得到浓度为0.5%的银纳米线分散液。
5)利用旋涂仪将上述银纳米线分散液均匀涂覆于VO2薄膜表面,具体参数为先进行低速旋涂,速度为400转/分钟,旋涂时间5s,再经高速旋涂,速度为2000转/分钟,旋涂时间30s。
6)将涂覆有湿银胶膜的VO2薄膜进行烘干,随后在空气下进行250℃热处理1h定型成膜,即得到所需的AgNW/VO2复合薄膜。
图1给出了AgNW/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银纳米线结构层,银纳米线的长度在5μm左右,具有较高的长径比和均匀性。紫外-可见吸收光谱的测试结果表明该银纳米线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,AgNW/VO2复合薄膜在不同脉冲能量下的激光可透过率均低于单一的VO2薄膜,最低可达5%,如图2所示。这说明经过Ag纳米线复合的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100nm厚的金属钒膜,衬底温度保持在200℃;
2)将一端敞口的管式退火炉进行升温,到500℃时进行保温,从炉管的非敞口端通入氮气,氮气流量保持在2L/min;
3)将制备的金属钒膜放入石英坩埚中,之后将坩埚推入上述管式退火炉中进行退火,退火时间为10min,到时后拉出坩埚进行快速空气下冷却。得到所需的VO2薄膜。
4)以AgNO3为银源,乙二醇为还原剂,聚乙烯吡咯烷酮为稳定剂和分散剂,利用化学还原反应得到银纳米颗粒,将产物离心分离并分散到乙醇中,得到浓度为0.5%的银纳米颗粒分散液。
5)利用旋涂仪将上述银纳米颗粒分散液均匀涂覆于VO2薄膜表面,具体参数为先进行低速旋涂,速度为400转/分钟,旋涂时间5s,再经高速旋涂,速度为2000转/分钟,旋涂时间30s。
6)将涂覆有湿银胶膜的VO2薄膜进行烘干,随后在空气下进行250℃热处理1h定型成膜,即得到所需的AgNP/VO2复合薄膜。
图3给出了AgNP/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银纳米颗粒结构层,银纳米颗粒的直径在几十至几百纳米左右,呈岛状随机分布。紫外-可见吸收光谱的测试结果表明该银纳米颗粒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,AgNP/VO2复合薄膜在不同脉冲能量下的激光可透过率均低于单一的VO2薄膜,最低可达5%,如图4所示。这说明经过Ag纳米颗粒复合的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)
1.一种具有激光防护性能的Ag/VO2复合薄膜的制备方法,其特征在于该工艺包括下述步骤:
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100nm厚的金属钒膜,衬底温度保持在200℃;
2)将一端敞口的管式退火炉进行升温,到500℃时进行保温,从炉管的非敞口端通入氮气,氮气流量保持在2L/min;
3)将制备的金属钒膜放入石英坩埚中,之后将坩埚推入上述管式退火炉中进行退火,退火时间为10min,到时后拉出坩埚进行快速空气下冷却。得到所需的VO2薄膜;
4)以AgNO3为银源,乙二醇为还原剂,聚乙烯吡咯烷酮为稳定剂和分散剂,利用化学还原反应得到银纳米线或银纳米颗粒产物,随后将产物离心分离并分散到乙醇中,得到浓度为0.5%的银纳米线或银纳米颗粒分散液;
5)利用旋涂仪将上述银纳米线或银纳米颗粒分散液均匀涂覆于VO2薄膜表面,具体参数为先进行低速旋涂,速度为400转/分钟,旋涂时间5s,再进行高速旋涂,速度为2000转/分钟,旋涂时间30s;
6)将涂覆有湿银胶膜的VO2薄膜进行烘干,随后在空气下进行250℃热处理1h定型成膜,即得到所需的Ag/VO2复合薄膜。
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