CN113122802A - 基于等离激元颗粒的防蓝光保护膜制备方法 - Google Patents
基于等离激元颗粒的防蓝光保护膜制备方法 Download PDFInfo
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- Surface Treatment Of Glass (AREA)
Abstract
基于等离激元颗粒的防蓝光保护膜制备方法,包括以下步骤:在透明基体上镀一层银膜;退火处理,在透明基体表面得到银纳米颗粒;使用原子层沉积方法在银纳米颗粒外部包裹一层氧化铝透明介质层,形成银‑氧化铝核壳结构;在氧化铝透明介质层上方镀一层二氧化硅透明薄膜;在二氧化硅透明薄膜表面镀一层金膜;退火处理,得到金纳米颗粒;使用原子层沉积方法在金纳米颗粒外部包裹一层二氧化钛透明介质层,形成金‑二氧化钛核壳结构;在二氧化钛透明介质层上方镀一层二氧化硅透明薄膜。本发明通过简单的镀膜和退火工艺,能够形成形状规则且大小、共振波段可控的纳米颗粒,从而有效吸收蓝光并减小薄膜发黄,具有重要的应用价值。
Description
技术领域
本发明属于透明显示技术领域,具体涉及一种基于等离激元颗粒的防蓝光保护膜制备方法。
背景技术
电子产品现已成为人们生活和学习不可缺少的重要工具,手机、电脑、电视等电子产品会通过显示屏向人眼辐射蓝光(波长400nm-500nm),其中波长在425-450nm的短波蓝光对人眼有害。在有大量蓝光辐射的环境中工作,经常会感到眼痛、眼胀、近视加重等眼科问题,长时间受到蓝光照射,人眼的视觉细胞会受到损伤,能量较高的蓝光能够使眼睛内的黄斑区毒素量增多,诱发盲眼病,严重影响青少年及老年群体的健康。
随着人们对健康问题越来越重视,蓝光危害问题势必会成为人们健康之路上一道显眼的阻碍。因此减少蓝光辐射量逐渐成为当前研究的热点,并将成为未来电子产品性能优良的一项重要指标,市场前景广阔。
为减少蓝光危害,常用的办法是在电子产品屏幕上方贴一层保护膜,来减少蓝光的辐射量。这种具有减小蓝光辐射量的薄膜制备方式大致有两大类:
其一在于在基体之上涂覆或喷涂具有蓝光吸收功能的吸收剂(如:CN105353436A等)、使用强化液交联吸收剂的方式(如:CN103992672A等)以及使用防蓝光膜成膜液(如:CN109320969A),来实现防蓝光功能。这种薄膜制备工艺存在着流程复杂、使用物品繁多以及制备周期长等诸多不便。
另一类减小蓝光辐射的方法在于使用纳米颗粒吸收层。CN106154384A 、CN108047981A使用镀膜的方法在基体上方镀上具有一定厚度的二氧化钛,或三氧化二铟,或氧化铁或硫化镉,或硒化镉纳米颗粒层来增强对蓝光的吸收,但不足之处在于纳米颗粒形状、大小难以控制、且需要纳米颗粒层厚度较大、成本高; CN111522080A使用由核壳结构微球形成的光子晶体材料制备防蓝光保护膜,但所用的核壳结构制备工艺繁琐,且颗粒分布难以保证均匀。这种薄膜放置一段时间后会出现泛黄的现象,影响其透光效果。
因此,需要发展一种技术简单、能有效吸收有害蓝光且可以减少薄膜泛黄的技术。
金属微纳结构的表面等离激元共振逐渐成为当前物理、化学、材料、信息科学等学科及其交叉领域的研究热点。具有波长选择性的等离激元颗粒能够增强可见光在某一波段的吸收率,将其调控在蓝光波段即可减小蓝光危害。另一方面使用不同种金属纳米颗粒可以吸收蓝光的同时,有效吸收黄光。颗粒材料相比上述材料,更加简单易制,有望解决当前问题。
发明内容
为了解决现有技术中的不足之处,提供一种工艺简单、造价低、金属颗粒分布均匀、防蓝光效果好的基于等离激元颗粒的防蓝光保护膜制备方法。
为解决上述技术问题,本发明采用如下技术方案:基于等离激元颗粒的防蓝光保护膜制备方法,包括以下步骤:
(1)使用溅射镀膜或蒸发镀膜在透明基体上镀一层银膜,透明基体的材料采用玻璃、塑料、树脂或聚合物;
(2)对所镀银膜的透明基体放入退火装置内进行退火处理;
(3)退火处理后在透明基体表面得到银纳米颗粒,银纳米颗粒尺寸与膜厚度有关;根据Mie散射理论计算得出颗粒尺寸;
(4)使用原子层沉积方法在银纳米颗粒外部包裹一层氧化铝透明介质层,形成银-氧化铝核壳结构;
(5)采用溅射或蒸发镀膜法在氧化铝透明介质层上方镀一层二氧化硅透明薄膜;
(6)采用如步骤(1)的方式在二氧化硅透明薄膜表面镀一层金膜;
(7)采用如步骤(2)的方式对所镀金膜的透明基体放入退火装置内进行退火处理;
(8)退火处理后得到金纳米颗粒,金纳米颗粒尺寸与膜厚度有关;根据Mie散射理论计算得出颗粒尺寸;
(9)采用如步骤(4)的方式使用原子层沉积方法在金纳米颗粒外部包裹一层二氧化钛透明介质层,形成金-二氧化钛核壳结构;
(10)采用如步骤(5)的方式在二氧化钛透明介质层上方镀一层二氧化硅透明薄膜。
步骤(1)使用电子束热蒸发镀膜仪在玻璃表面镀银膜,具体步骤如下:将清洗洁净的8cm×8cm的光学玻璃放入电子束热蒸发镀膜仪的基片架上,将纯度99.99%的银颗粒放入蒸发用的钨坩埚内,真空度抽到5×10-4Pa以下,开始镀膜;在镀膜过程中可通过控制电子束电流大小控制镀膜速率,通过调节镀膜速率和时间控制膜厚。
步骤(1)使用氩离子溅射镀膜仪在玻璃表面镀银,具体步骤如下:把清洗洁净的8cm×8cm的光学玻璃放入氩离子溅射镀膜仪的样品杆载物台内,将样品杆载物台推入氩离子溅射镀膜仪中,抽真空,待真空度抽到5×10-4Pa以下,开始溅射镀膜;调节电子枪工作电压和电流,推荐参数7kv/300uA,银的镀膜速率为8nm/min;最终得到的银颗粒尺寸与镀膜时间有关,时间分别控制为15S、30S、45S、60S、75S得到膜状结构,其中30S-75S的银颗粒为岛状。
步骤(2)中的退火装置包括底座,底座上设有圆筒箱,圆筒箱的中心线沿左右方向水平设置,圆筒箱的内圆沿圆周方向均匀设有若干根加热管,圆筒箱的左侧面板中心和右侧面板中心之间转动设有一根空心轴,空心轴外部相对两侧分别固定设有一个空心吸盘,空心轴左端穿出圆筒箱的左侧面板并通过一个旋转接头连接有抽真空管,抽真空管连接有真空泵,圆筒箱的右侧面板右侧设有电机,电机的主轴与空心轴的右端同轴线传动连接,圆筒箱的左侧面板上设有箱门,圆筒箱的右侧面板上部设有进气管。
每根加热管均平行于圆筒箱的中心线,每根加热管右端均伸出圆筒箱的右侧面板并固定连接有一个接线柱,所有的接线柱通过导线串联,导线连接有电源线;圆筒箱内设有温度传感器;圆筒箱内在所有加热管的内侧固定设有圆筒状的隔离网;圆筒箱的外部和箱门的外部均设有隔热材料层;空心吸盘为矩形板体结构,空心吸盘的中心具有矩形空腔,空心吸盘与空心轴固定连接的一侧面沿空心轴长度方向间隔设有若干个第一抽吸口,空心吸盘的另一侧面均匀设有若干个第二抽吸口;箱门在圆筒箱的左侧面板处设有两个,两个箱门关于圆筒箱的中心线左右对称。
步骤(2)中退火处理的具体过程为:打开两个箱门,先将两个空心吸盘转动到竖向状态,然后将两块镀银膜后的玻璃放入到圆筒箱内,玻璃未镀膜的一侧面与空心吸盘表面接触,开启真空泵,真空泵通过抽真空管、空心轴、第一抽吸口和第二抽吸口将两块玻璃牢牢地吸附在空心吸盘上,然后关闭两个箱门,启动电机和加热管的电源,加热管对封闭的圆筒箱内部空间进行加热,电机驱动空心轴转动,空心轴带动两个空心吸盘转动,吸附在空心吸盘上的两块镀膜玻璃也随着转动,同时通过进气管向圆筒箱内充入0.01MPa的保护性氮气并混合还原性氢气,由于玻璃与空心吸盘之间会存在透气间隙,在吸附空心吸盘的同时,将圆筒箱内部的空气置换为保护性氮气和还原性氢气,然后加热管的加热速度以5℃/min升温至300℃,温度监控通过温度传感器传输到PLC控制器,PLC控制器调控电源为加热管的供电电流,在300℃保温30min后,先关闭电机和加热管的电源,然后打开箱门,关闭真空泵,取出两块玻璃,完成退火工序。
步骤(3)中在透明基体表面得到银纳米颗粒在玻璃上均匀排列,退火后的银纳米颗粒的半径尺寸为10nm;步骤(4)中氧化铝透明介质层的厚度为10 nm,氧化铝透明介质层的折射率为1.59。
步骤(4)的具体过程为:以三甲基铝和高纯水作为反应源,高纯N2作为吹洗气体,在金属纳米颗粒外部生长出氧化铝透明介质,沉积温度: 120℃,三甲基铝脉冲时间:0.2-0.6S; 高纯水脉冲时间: 0.3S; 吹扫时间: 10S; 循环周期: 25 次。
步骤(5)和(10)中的二氧化硅透明薄膜厚度为120-200nm,二氧化硅透明薄膜折射率为1.45。
步骤(8)中得到金纳米颗粒在玻璃上均匀排列,退火后的金纳米颗粒的半径尺寸为15nm;步骤(9)中二氧化钛透明介质层的厚度为5 nm,二氧化钛透明介质层的折射率为2.45。
采用上述技术方案,金属膜的厚度取决于镀膜生长速率和时间,金属可以是银,金或者铝等。如果需要金属颗粒的结构是核壳结构,则在金属颗粒形成后,使用原子层沉积(ALD)方法在金属颗粒外部生长透明介质层。最后在金属颗粒上方镀一层透明薄膜,该过程可以防止金属颗粒在空气中氧化,也可以调节共振位置,薄膜材料是透明的,且不唯一。金属颗粒的均匀分布是靠镀膜方式实现的,本发明中的金属不限制为银也可以是金或者铝等其它金属,例如是金,在一定折射率介质环境下,可以有效吸收黄光。
退火装置采用真空泵对空心吸盘抽气吸附镀膜玻璃的方式,并通过电机带动空心吸盘和两块镀膜玻璃缓慢旋转,这样不仅提高受热面的温度保持一致,同时使镀膜与保护性氮气及还原性氢气动态接触,从而提高退火工序的处理质量。
加热管沿圆筒箱的圆周方向均匀布置若干根,这样也可提高对镀膜加热的均匀度。
隔离网不仅具有良好的透热性,而且具有在取放玻璃时,防止玻璃触碰到加热管。
隔热材料层(可采用聚氨酯保温材料)可避免热量散失,提高加热效率。
退火装置采用圆筒箱具有体积小、结构紧凑的特点,整个退火处理工序也操作方便,采用真空吸附的方式不仅固定牢靠,而且在处理过程中可以旋转,提高镀膜表面温度的一致性,大大提高了产品质量。
综上所述,本发明整体具有以下有益效果:
(1)本发明提供了一种新的基于等离激元颗粒的防蓝光保护膜的制备方法。采用氩离子溅射镀膜仪与电子束热蒸发镀膜仪,在透明基体上镀上一层银膜,然后经退火处理后得到具有强波长选择性光学天线功能的银纳米颗粒,采用ALD法在银纳米颗粒包裹一层氧化铝透明介质,调节不同的共振波长,从而实现对蓝光有效吸收。在上方镀一层二氧化硅环境介质,不仅能对银纳米颗粒的共振位置进行调节,而且可以有效防止银纳米颗粒氧化。本发明制备过程简单,金属颗粒分布均匀,且可以通过控制镀膜时间来控制金属颗粒的尺寸。
(2)镀膜所使用的金属靶材的价格远低于其他方法获得的金属颗粒,造价低廉,市场前景广阔。
(3)本发明制备防蓝光保护膜实验周期短,节省时间成本,更有效率。
(4)与蓝光吸收颗粒层(镀银膜)制备方式一样,使用溅射或蒸发的方式在基板上方镀一层金膜,在保护气体中进行退火得到具有所需尺寸的金纳米颗粒。使用ALD等物理气相沉积的方法在所制备颗粒上方生长二氧化钛介质,通过控制仪器参数控制二氧化钛介质层厚度,最后在上方镀上一层二氧化硅环境介质。从而最终实现对黄光的吸收。
(5)本发明通过简单的镀膜和退火工艺,能够形成形状规则且大小、共振波段可控的纳米颗粒,从而有效吸收蓝光并减小薄膜发黄,具有重要的应用价值。
附图说明
图1是本发明中退火装置的结构示意图;
图2是图1的右视图。
图3是图1的左视图;
图4是石英环境下实现蓝光吸收(420-450nm)的等离激元颗粒的消光、散射和吸收谱;
图5是石英环境下实现黄光吸收(570-600nm)的等离激元颗粒的消光、散射和吸收谱;
图6是电子束热蒸发镀膜仪在光学玻璃基体上镀的银膜退火前后的SEM形貌;
图7是使用电子束热蒸发镀膜仪所得透明显示屏的反射、透射与吸收光谱;
图8是本发明的防蓝光保护膜的层状结构。
具体实施方式
如图8所示,本发明的基于等离激元颗粒的防蓝光保护膜制备方法,包括以下步骤:
(1)使用溅射镀膜或蒸发镀膜在透明基体上镀一层银膜,透明基体23的材料采用玻璃、塑料、树脂或聚合物;
(2)对所镀银膜的透明基体23放入退火装置内进行退火处理;
(3)退火处理后在透明基体23表面得到银纳米颗粒,银纳米颗粒尺寸与膜厚度有关;根据Mie散射理论计算得出颗粒尺寸;
(4)使用原子层沉积方法在银纳米颗粒外部包裹一层氧化铝透明介质层,形成银-氧化铝核壳结构;
(5)采用溅射或蒸发镀膜法在氧化铝透明介质层上方镀一层二氧化硅透明薄膜;形成防蓝光等离激元结构层24;
(6)采用如步骤(1)的方式在二氧化硅透明薄膜表面镀一层金膜;
(7)采用如步骤(2)的方式对所镀金膜的透明基体23放入退火装置内进行退火处理;
(8)退火处理后得到金纳米颗粒,金纳米颗粒尺寸与膜厚度有关;根据Mie散射理论计算得出颗粒尺寸;
(9)采用如步骤(4)的方式使用原子层沉积方法在金纳米颗粒外部包裹一层二氧化钛透明介质层,形成金-二氧化钛核壳结构;
(10)采用如步骤(5)的方式在二氧化钛透明介质层上方镀一层二氧化硅透明薄膜;形成黄光吸附等离激元结构层25。
步骤(1)使用电子束热蒸发镀膜仪在玻璃表面镀银膜,具体步骤如下:将清洗洁净的8cm×8cm的光学玻璃放入电子束热蒸发镀膜仪的基片架上,将纯度99.99%的银颗粒放入蒸发用的钨坩埚内,真空度抽到5×10-4Pa以下,开始镀膜;在镀膜过程中可通过控制电子束电流大小控制镀膜速率,通过调节镀膜速率和时间控制膜厚。
步骤(1)使用氩离子溅射镀膜仪在玻璃表面镀银,具体步骤如下:把清洗洁净的8cm×8cm的光学玻璃放入氩离子溅射镀膜仪的样品杆载物台内,将样品杆载物台推入氩离子溅射镀膜仪中,抽真空,待真空度抽到5×10-4Pa以下,开始溅射镀膜;调节电子枪工作电压和电流,推荐参数7kv/300uA,银的镀膜速率为8nm/min;最终得到的银颗粒尺寸与镀膜时间有关,时间分别控制为15S、30S、45S、60S、75S得到膜状结构,其中30S-75S的银颗粒为岛状。
如图1-图3所示,步骤(2)中的退火装置包括底座1,底座1上设有圆筒箱2,圆筒箱2的中心线沿左右方向水平设置,圆筒箱2的内圆沿圆周方向均匀设有若干根加热管3,圆筒箱2的左侧面板中心和右侧面板中心之间转动设有一根空心轴4,空心轴4右端封堵,空心轴4外部相对两侧分别固定设有一个空心吸盘5,空心轴4左端穿出圆筒箱2的左侧面板并通过一个旋转接头6连接有抽真空管7,抽真空管7连接有真空泵8,圆筒箱2的右侧面板右侧设有电机9(通过连接板10和螺栓11连接),电机9的主轴与空心轴4的右端同轴线传动连接,圆筒箱2的左侧面板上设有箱门12,圆筒箱2的右侧面板上部设有进气管13。
每根加热管3均平行于圆筒箱2的中心线,每根加热管3右端均伸出圆筒箱2的右侧面板并固定连接有一个接线柱14,所有的接线柱14通过导线15串联,导线15连接有电源线16。圆筒箱2内设有温度传感器17。圆筒箱2内在所有加热管3的内侧固定设有圆筒状的隔离网18。圆筒箱2的外部和箱门12的外部均设有隔热材料层19。空心吸盘5为矩形板体结构,空心吸盘5的中心具有矩形空腔20,空心吸盘5与空心轴4固定连接的一侧面沿空心轴4长度方向间隔设有若干个第一抽吸口21,空心吸盘5的另一侧面均匀设有若干个第二抽吸口22。箱门12在圆筒箱2的左侧面板处设有两个,两个箱门12关于圆筒箱2的中心线左右对称。
步骤(2)中退火处理的具体过程为: 打开两个箱门12,先将两个空心吸盘5转动到竖向状态,然后将两块镀银膜后的玻璃放入到圆筒箱2内,玻璃未镀银膜的一侧面与空心吸盘5表面接触,开启真空泵8,真空泵8通过抽真空管7、空心轴4、第一抽吸口21和第二抽吸口22将两块玻璃牢牢地吸附在空心吸盘5上,然后关闭两个箱门12,启动电机9和加热管3的电源,加热管3对封闭的圆筒箱2内部空间进行加热,电机9驱动空心轴4转动,空心轴4带动两个空心吸盘5转动(旋转接头6的设置,抽真空管7不动),吸附在空心吸盘5上的两块镀膜玻璃也随着转动,同时通过进气管13向圆筒箱2内充入0.01MPa的保护性氮气并混合还原性氢气,由于玻璃与空心吸盘5之间会存在透气间隙,在吸附空心吸盘5的同时,将圆筒箱2内部的空气置换为保护性氮气和还原性氢气,然后加热管3的加热速度以5℃/min升温至300℃,温度监控通过温度传感器17传输到PLC控制器,PLC控制器调控电源为加热管3的供电电流,在300℃保温30min后,先关闭电机9和加热管3的电源,然后打开箱门12,关闭真空泵8,取出两块玻璃,完成退火工序。
步骤(3)中在透明基体23表面得到银纳米颗粒在玻璃上均匀排列,退火后的银纳米颗粒的半径尺寸为10nm;步骤(4)中氧化铝透明介质层的厚度为10 nm,氧化铝透明介质层的折射率为1.59。
步骤(4)的具体过程为:以三甲基铝和高纯水作为反应源,高纯N2作为吹洗气体,在金属纳米颗粒外部生长出氧化铝透明介质,沉积温度: 120℃,三甲基铝脉冲时间:0.2-0.6S; 高纯水脉冲时间: 0.3S; 吹扫时间: 10S; 循环周期: 25 次。
步骤(5)和(10)中的二氧化硅透明薄膜厚度为120-200nm,二氧化硅透明薄膜折射率为1.45。
步骤(8)中得到金纳米颗粒在玻璃上均匀排列,退火后的金纳米颗粒的半径尺寸为15nm;步骤(9)中二氧化钛透明介质层的厚度为5 nm,二氧化钛透明介质层的折射率为2.45。
金属膜的厚度取决于镀膜生长速率和时间,金属可以是银,金或者铝等。如果需要金属颗粒的结构是核壳结构,则在金属颗粒形成后,使用原子层沉积(ALD)方法在金属颗粒外部生长透明介质层。最后在金属颗粒上方镀一层透明薄膜,该过程可以防止金属颗粒在空气中氧化,也可以调节共振位置,薄膜材料是透明的,且不唯一。金属颗粒的均匀分布是靠镀膜方式实现的,本发明中的金属不限制为银也可以是金或者铝等其它金属,例如是金,在一定折射率介质环境下,可以有效吸收黄光。
采用真空泵8对空心吸盘5抽气吸附镀膜玻璃的方式,并通过电机9带动空心吸盘5和两块镀膜玻璃缓慢旋转,这样不仅提高受热面的温度保持一致,同时使镀膜与保护性氮气及还原性氢气动态接触,从而提高退火工序的处理质量。
加热管3沿圆筒箱2的圆周方向均匀布置若干根,这样也可提高对镀膜加热的均匀度。
隔离网18不仅具有良好的透热性,而且具有在取放玻璃时,防止玻璃触碰到加热管3。
隔热材料层19(可采用聚氨酯保温材料)可避免热量散失,提高加热效率。
退火装置采用圆筒箱2具有体积小、结构紧凑的特点,整个退火处理工序也操作方便,采用真空吸附的方式不仅固定牢靠,而且在处理过程中可以旋转,提高镀膜表面温度的一致性,大大提高了产品质量。
图4是石英(透明基体23)环境下防蓝光等离激元结构层24实现蓝光吸收(420-450nm)的等离激元颗粒的消光、散射和吸收谱,所用颗粒为银-氧化铝核壳结构,其中内层银颗粒半径可以是10-15nm中的任意尺寸,壳层介质氧化铝厚度可以是10-15nm中的任意尺寸。另外颗粒还可以是纯银颗粒,半径在10-20nm之间,环境介质折射率n b =1.7;纯铝颗粒,半径为10-15nm之间,环境介质折射率n b =2.45。
图5是石英环境下黄光吸附等离激元结构层25实现黄光吸收(570-600nm)的等离激元颗粒的消光、散射和吸收谱,所用颗粒为金-二氧化钛核壳结构,其中内层银颗粒半径可以是15-20nm中的任意尺寸,壳层介质二氧化钛厚度可以是5-10nm中的任意尺寸。另外颗粒还可以是纯金颗粒,半径在15-20nm之间,环境介质折射率n b =1.7。
图6为电子束热蒸发镀膜仪在光学玻璃基体上镀的银膜退火前后的SEM形貌。左侧为镀膜后的SEM形貌,膜厚为5nm,右侧为相应的退火后的SEM形貌,所得银颗粒尺寸大部分在20nm以下。
图7为使用电子束热蒸发镀膜仪所得透明显示屏的反射、透射与吸收光谱,A=1-R-T。Reflection指反射率,所得防蓝光保护膜在420nm-470nm左右的蓝光波段反射率最强,在0.18-0.24之间,在其他大部分可见光波段都降到0.12以下。Transmittance指透射率,在420nm-470nm左右的蓝光波段透射率最弱,在0.5-0.7之间,而其他大部分波段都在0.8以上。Absorption指吸收率在420nm-470nm左右的蓝光吸收最强,在0.15-0.28之间,而其他大部分波段都在0.05以下。
以上实施例说明了本发明的基本原理和特点,但上述仅仅说明了本发明的较优实施例,并不受所述实施例的限制。本领域的普通技术人员在本专利的启发下,在不脱离本发明宗旨和权利要求所保护的范围情况下,还可以做出很多形式变形和改进,这些均属于本发明的保护范围之内。因此,本发明专利和保护范围应以所附权利要求书为准。
Claims (10)
1.基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:包括以下步骤:
(1)使用溅射镀膜或蒸发镀膜在透明基体上镀一层银膜,透明基体的材料采用玻璃、塑料、树脂或聚合物;
(2)对所镀银膜的透明基体放入退火装置内进行退火处理;
(3)退火处理后在透明基体表面得到银纳米颗粒,银纳米颗粒尺寸与膜厚度有关;根据Mie散射理论计算得出颗粒尺寸;
(4)使用原子层沉积方法在银纳米颗粒外部包裹一层氧化铝透明介质层,形成银-氧化铝核壳结构;
(5)采用溅射或蒸发镀膜法在氧化铝透明介质层上方镀一层二氧化硅透明薄膜;
(6)采用如步骤(1)的方式在二氧化硅透明薄膜表面镀一层金膜;
(7)采用如步骤(2)的方式对所镀金膜的透明基体放入退火装置内进行退火处理;
(8)退火处理后得到金纳米颗粒,金纳米颗粒尺寸与膜厚度有关;根据Mie散射理论计算得出颗粒尺寸;
(9)采用如步骤(4)的方式使用原子层沉积方法在金纳米颗粒外部包裹一层二氧化钛透明介质层,形成金-二氧化钛核壳结构;
(10)采用如步骤(5)的方式在二氧化钛透明介质层上方镀一层二氧化硅透明薄膜。
2.根据权利要求1所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:步骤(1)使用电子束热蒸发镀膜仪在玻璃表面镀银膜,具体步骤如下:将清洗洁净的8cm×8cm的光学玻璃放入电子束热蒸发镀膜仪的基片架上,将纯度99.99%的银颗粒放入蒸发用的钨坩埚内,真空度抽到5×10-4Pa以下,开始镀膜;在镀膜过程中可通过控制电子束电流大小控制镀膜速率,通过调节镀膜速率和时间控制膜厚。
3.根据权利要求1所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:步骤(1)使用氩离子溅射镀膜仪在玻璃表面镀银,具体步骤如下:把清洗洁净的8cm×8cm的光学玻璃放入氩离子溅射镀膜仪的样品杆载物台内,将样品杆载物台推入氩离子溅射镀膜仪中,抽真空,待真空度抽到5×10-4Pa以下,开始溅射镀膜;调节电子枪工作电压和电流,推荐参数7kv/300uA,银的镀膜速率为8nm/min;最终得到的银颗粒尺寸与镀膜时间有关,时间分别控制为15S、30S、45S、60S、75S得到膜状结构,其中30S-75S的银颗粒为岛状。
4.根据权利要求2或3所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:步骤(2)中的退火装置包括底座,底座上设有圆筒箱,圆筒箱的中心线沿左右方向水平设置,圆筒箱的内圆沿圆周方向均匀设有若干根加热管,圆筒箱的左侧面板中心和右侧面板中心之间转动设有一根空心轴,空心轴外部相对两侧分别固定设有一个空心吸盘,空心轴左端穿出圆筒箱的左侧面板并通过一个旋转接头连接有抽真空管,抽真空管连接有真空泵,圆筒箱的右侧面板右侧设有电机,电机的主轴与空心轴的右端同轴线传动连接,圆筒箱的左侧面板上设有箱门,圆筒箱的右侧面板上部设有进气管。
5.根据权利要求4所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:每根加热管均平行于圆筒箱的中心线,每根加热管右端均伸出圆筒箱的右侧面板并固定连接有一个接线柱,所有的接线柱通过导线串联,导线连接有电源线;圆筒箱内设有温度传感器;圆筒箱内在所有加热管的内侧固定设有圆筒状的隔离网;圆筒箱的外部和箱门的外部均设有隔热材料层;空心吸盘为矩形板体结构,空心吸盘的中心具有矩形空腔,空心吸盘与空心轴固定连接的一侧面沿空心轴长度方向间隔设有若干个第一抽吸口,空心吸盘的另一侧面均匀设有若干个第二抽吸口;箱门在圆筒箱的左侧面板处设有两个,两个箱门关于圆筒箱的中心线左右对称。
6.根据权利要求5所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:步骤(2)中退火处理的具体过程为:打开两个箱门,先将两个空心吸盘转动到竖向状态,然后将两块镀银膜后的玻璃放入到圆筒箱内,玻璃未镀膜的一侧面与空心吸盘表面接触,开启真空泵,真空泵通过抽真空管、空心轴、第一抽吸口和第二抽吸口将两块玻璃牢牢地吸附在空心吸盘上,然后关闭两个箱门,启动电机和加热管的电源,加热管对封闭的圆筒箱内部空间进行加热,电机驱动空心轴转动,空心轴带动两个空心吸盘转动,吸附在空心吸盘上的两块镀膜玻璃也随着转动,同时通过进气管向圆筒箱内充入0.01MPa的保护性氮气并混合还原性氢气,由于玻璃与空心吸盘之间会存在透气间隙,在吸附空心吸盘的同时,将圆筒箱内部的空气置换为保护性氮气和还原性氢气,然后加热管的加热速度以5℃/min升温至300℃,温度监控通过温度传感器传输到PLC控制器,PLC控制器调控电源为加热管的供电电流,在300℃保温30min后,先关闭电机和加热管的电源,然后打开箱门,关闭真空泵,取出两块玻璃,完成退火工序。
7.根据权利要求6所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:步骤(3)中在透明基体表面得到银纳米颗粒在玻璃上均匀排列,退火后的银纳米颗粒的半径尺寸为10nm;步骤(4)中氧化铝透明介质层的厚度为10 nm,氧化铝透明介质层的折射率为1.59。
8.根据权利要求7所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:步骤(4)的具体过程为:以三甲基铝和高纯水作为反应源,高纯N2作为吹洗气体,在金属纳米颗粒外部生长出氧化铝透明介质,沉积温度: 120℃,三甲基铝脉冲时间:0.2-0.6S; 高纯水脉冲时间: 0.3S; 吹扫时间: 10S; 循环周期: 25 次。
9.根据权利要求8所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:步骤(5)和(10)中的二氧化硅透明薄膜厚度为120-200nm,二氧化硅透明薄膜折射率为1.45。
10.根据权利要求8所述的基于等离激元颗粒的防蓝光保护膜制备方法,其特征在于:步骤(8)中得到金纳米颗粒在玻璃上均匀排列,退火后的金纳米颗粒的半径尺寸为15nm;步骤(9)中二氧化钛透明介质层的厚度为5 nm,二氧化钛透明介质层的折射率为2.45。
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