CN109551123A - 皮秒激光诱导石英玻璃内部裂纹实现微流控器件制备的方法 - Google Patents

皮秒激光诱导石英玻璃内部裂纹实现微流控器件制备的方法 Download PDF

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CN109551123A
CN109551123A CN201811539810.9A CN201811539810A CN109551123A CN 109551123 A CN109551123 A CN 109551123A CN 201811539810 A CN201811539810 A CN 201811539810A CN 109551123 A CN109551123 A CN 109551123A
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quartz glass
picosecond laser
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程亚
徐剑
李晓龙
林子杰
王振华
柴志方
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East China Normal University
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Abstract

本发明公开了一种皮秒激光诱导石英玻璃内部裂纹实现微流控器件制备的方法，先利用聚焦的时域调控皮秒激光在石英玻璃中辐照产生空间选择性微纳裂纹区域，然后通过化学腐蚀将辐照区域去除得到中空且连通的三维微结构，从而实现石英玻璃内部微通道结构的三维制备。本发明通过调控皮秒激光的脉冲宽度可实现偏振不敏感的三维均一性腐蚀，同时具有高的化学腐蚀速率和选择性，适用于大尺寸三维微流控系统制造和高精度三维打印玻璃结构等领域。

Description

皮秒激光诱导石英玻璃内部裂纹实现微流控器件制备的方法
技术领域
本发明涉及三维微通道和微流控器件的制造方法，特别是一种利用皮秒激光诱导石英玻璃内部裂纹实现微流控器件制备的方法。本发明适用于大尺寸石英玻璃微流控系统制备、高精度三维打印玻璃结构等领域。
背景技术
微流控芯片技术，作为一种革命性的技术，当前已在化学分析、化工合成、生物制药、医疗诊断、光子学等领域展现出重要应用。微通道作为微流控芯片的核心单元，其高性能和多功能制备技术对于提升微流控芯片技术的发展具有重要意义。相对于目前普遍得到应用的二维微通道，三维微通道可为微流控芯片技术的进一步技术革新提供更加灵活、更加高效的微尺度空间流体操控能力。
石英玻璃由于其高的耐热性和化学稳定性，低的热膨胀系数，宽的光谱透射范围和良好的生物相容性，是微流控芯片技术目前广泛采用的基底之一。当前在石英玻璃内部制备三维微通道的最具代表性的技术是飞秒激光三维微加工。通过调控聚焦飞秒激光的脉冲能量可在石英玻璃内部诱导出高度非线性的改性如纳米光栅、微空洞等，进而可通过不同途径制备出三维空间构型灵活可控的微通道结构。其中，利用飞秒激光辐照诱导偏振依赖的化学选择性腐蚀是目前研究最广泛、最具应用前景的技术途径之一。通过调控聚焦线偏振飞秒激光的偏振取向，使得激光偏振方向垂直于激光直写方向时，腐蚀速率可得到大大提升（C. Hnatovsky, et al., Opt. Lett. 2005, 30, 1867–1869; M. Hermans, etal., J. Laser Micro Nanoeng. 2014, 9, 126–131）。但是利用这一技术制备三维微通道时，特征结构空间取向的不同会带来腐蚀速度的很大差异，进而会对影响微通道结构的制备效果，譬如会产生锥状的三维微通道。而利用圆偏振光，虽然可以获得三维的均一性腐蚀效果(X. M. Yu, et al., J. Appl. Phys. 2011, 109, 053114)，但是相对于线偏振光而言，腐蚀速率大大降低，不利于微通道的高性能可控制备。而为了获得更高的腐蚀速率，在辐照过程随着直写方向的改变实时变换激光的偏振方向会增加加工系统和加工过程的复杂度。因此，寻求一种简便、可控、三维均一性好的石英玻璃三维微通道制备技术具有重要意义。
发明内容
本发明的目的在于针对当前飞秒激光制备三维微通道的不足，提供一种简便、可控、三维可控的石英玻璃微通道以及微流控器件制备方法。
实现本发明目的的具体技术方案如下：
一种利用皮秒激光诱导石英玻璃内部裂纹实现微流控器件制备的方法，该方法包括下列步骤：
步骤1：皮秒激光辐照
将石英玻璃样品固定在一台可编程三维位移平台上，通过显微物镜将时域调控的皮秒激光聚焦在石英玻璃样品上，驱动位移平台运动同时启动皮秒激光辐照，在石英玻璃样品内部中直写出所需要的内含微纳裂纹的三维微通道图案；
步骤2：选择性化学腐蚀
将皮秒激光辐照后的石英玻璃样品放入化学腐蚀溶液中，对所述的三维微通道图案进行空间选择性腐蚀去除，进而在石英玻璃样品内部获得具有三维几何构型的微通道结构。
所述的时域调控的皮秒激光的脉冲宽度为1-20 ps，重复频率为1-1000 kHz，聚焦物镜的数值孔径为0.1-1.4。
所述的化学腐蚀溶液为5-20 mol/L 氢氧化钾溶液（80-95℃）或1-20% 氢氟酸溶液。
与现有的技术相比较，本发明的优点在于：
1）、对加工用光的偏振不敏感性：采用时域调控的皮秒激光加工产生不同于通常纳米光栅的微纳裂纹区域，不同取向的线偏振光和圆偏振光带来的化学腐蚀速率差异，相对于飞秒激光辅助化学蚀刻微通道的偏振依赖程度大大降低。这种偏振不敏感性将有助于改善化学腐蚀过程控制，用于制备高保真度的三维微通道以及复杂曲面的三维空腔结构。
2）、高的腐蚀速率：由于时域调控的皮秒激光与石英玻璃的非线性作用过程中产生的随机纳米裂纹，在实际腐蚀过程中腐蚀液更容易进入这些裂纹并通过上述裂纹的快速连通从而加快整个腐蚀过程，可获得与飞秒激光微加工方法最快腐蚀速率相当的效果。
3）、三维可控制备：尽管皮秒激光相比飞秒激光与石英玻璃作用过程会具有更多的能量沉积产生较大的热应力，从而影响微通道的制备效果，但是通过调控皮秒激光的辐照参数如脉冲宽度、辐照能量以及辐照时间，在石英玻璃内部可以通过对产生随机纳米裂纹的有效控制稳定实现三维微通道的可控制备。
附图说明
图1是利用皮秒激光诱导石英玻璃内部裂纹实现微流控器件制备的流程示意图；
图2是不同偏振状态的6 ps激光制备微通道的腐蚀对比图；
图3是8 ps激光辐照制备三维微通道网络结构光学显微图（正视图）；
图4是8 ps激光辐照制备三维微通道网络结构光学显微图（侧视图）。
具体实施方式
下面结合实施例和附图对本发明作进一步说明，但不应以此限制本发明的保护范围。
实施例1
本实施例包括如下步骤：
步骤1：皮秒激光辐照
如图1所示，取尺寸为20 mm× 10 mm× 2 mm且六面抛光的洁净石英玻璃样品，固定在三维位移台上；激光的中心波长为1026 nm，重复频率为 50 kHz，脉冲宽度为6 ps；采用数值孔径为0.45的显微物镜聚焦激光，聚焦深度为在石英玻璃表面以下300 μm。为评估偏振对腐蚀速率的影响，利用出射激光的本征偏振方向与直写方向平行（图2a）和垂直（图2b）以及在聚焦之前放置四分之一波片调整产生圆偏振光（图2c）三种情况分别来直写图案，平均功率为400 mW，扫描速度为0.5 mm/s。
步骤2：选择性化学腐蚀
将皮秒激光辐照后的石英玻璃样品放入在10 mol/L 氢氧化钾溶液（85℃）中进行超声波辅助腐蚀1 h后取出观察拍照。从图2腐蚀（虚线为腐蚀痕迹）的对比可看出，同等条件下，不同的偏振情况，6 ps的腐蚀速率差异性不大（即偏振不敏感），同时具有较高的腐蚀速率。
实施例2
本实施例包括如下步骤：
步骤1：皮秒激光辐照
如图1所示，取尺寸为5 mm× 5 mm× 5 mm且六面抛光的洁净石英玻璃样品，固定在三维位移台上；激光的中心波长为1026 nm，重复频率为 50 kHz，脉冲宽度为8 ps；采用数值孔径为0.30的显微物镜聚焦，在聚焦之前放置四分之一波片调整产生圆偏振光，在石英玻璃样品内部直写六面贯通的微通道多层网格图案，平均功率为450 mW，扫描速度为0.5 mm/s。
步骤2：选择性化学腐蚀
将皮秒激光辐照后的石英玻璃样品放入在10 mol/L 氢氧化钾溶液（85℃）中进行超声波辅助腐蚀，直至激光辐照的区域完全被去除而在玻璃样品内部形成三维连贯的空心多层微通道网络结构（图3为正视图，图4为侧视图），通道腐蚀的均一性较好，没有明显的锥状结构。

Claims (3)

1.一种皮秒激光诱导石英玻璃内部裂纹实现微流控器件制备的方法，其特征在于，该方法包括下列步骤：
步骤1：皮秒激光辐照
将石英玻璃样品固定在一台可编程三维位移平台上，通过显微物镜将时域调控的皮秒激光聚焦在石英玻璃样品上，驱动位移平台运动同时启动皮秒激光辐照，在石英玻璃样品内部中直写出所需要的内含微纳裂纹的三维微通道图案；
步骤2：选择性化学腐蚀
将皮秒激光辐照后的石英玻璃样品放入化学腐蚀溶液中，对直写的三维微通道图案进行空间选择性腐蚀去除，进而在石英玻璃样品内部获得具有三维几何构型的微通道结构。
2.根据权利要求1所述的方法，其特征在于，所述的时域调控的皮秒激光的脉冲宽度为1-20 ps，重复频率为1-1000 kHz，聚焦物镜的数值孔径为0.1-1.4。
3.根据权利要求1所述的方法，其特征在于，所述的化学腐蚀溶液为80-95℃的5-20mol/L 氢氧化钾溶液或1-20% 氢氟酸溶液。
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