CN108411286A - 任意构型三维导电金属微纳结构的制造方法 - Google Patents
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Abstract
本发明公开了一种任意构型三维导电金属微纳结构的制造方法,先利用飞秒激光微加工技术在透明材料内部制作出三维微通道,然后通过蠕动泵将化学镀溶液连续传输通过微通道进行通道内部的表面改性及后续金属层沉积,最后通过化学蚀刻将透明材料基体去除获得三维构型导电金属立体微结构。本发明制造的三维金属微纳结构具有空间构型可任意设计,尺寸可调,高电导率,高熔点的特点,在微电子学,光子学,微纳电机系统,微纳传感,催化等领域具有很大应用前景。
Description
技术领域
本发明涉及三维金属微纳结构制造和飞秒激光微加工,特别是一种利用飞秒激光微加工与流动化学镀以及化学腐蚀结合制造三维导电金属微纳结构的方法。本方法适用于制造金,银,铂,镍等金属结构。
背景技术
三维金属微纳结构兼具金属和三维立体微纳结构的双重特性,目前已在微电子学,光子学,化学传感,生物医学等领域展示很大的应用潜力。与二维金属微纳结构相比,三维金属微纳结构在维度上的拓展可提供更强,更均匀的空间局域性电磁场控制和散热能力,进而实现更高灵敏度的探测,更优异的可调谐能力和器件稳定性。因此,设计和制造各种复杂构型的三维金属微纳结构及阵列,对于开发新型的微电子和光子学以及微纳传感器件及系统具有重要意义和实用价值。但是任意构型三维金属微纳结构的高效快速制造对于当前二维平面光刻工艺为基础的微纳制造技术是个很大的挑战。譬如多层光刻技术与电镀技术结合虽可制造出三维金属微纳结构,但其制作步骤繁杂,空间几何构型设计灵活度不高。三维增材打印技术的出现和兴起为三维金属结构制造提供新的思路。在宏观尺度上,基于激光束和电子束熔覆金属粉末制造三维金属结构已取得商业化成功。但由于熔覆用金属粉末颗粒尺寸的限制以及金属本征的高热耗散特性,上述技术在微纳尺度的三维金属结构制造适用性并不理想(参见文献:D. Herzog, et al., Acta Mater., 2016, 117, 371;M. Vaezi, et al., Int. J. Adv. Manuf. Technol. 2013, 67, 1721; L. Hirt, etal., Adv. Mater. 2017, 29, 1604211)。
飞秒激光由于其超高的峰值功率和超短的脉冲宽度,对透明材料如玻璃和聚合物等具有独特的三维内部加工能力。利用飞秒激光可在透明材料内部实现三维任意形状的微结构制造 (参见文献:K. Sugioka, Y. Cheng. Light: Sci. & Appl. 2014, 3, e149)。对于玻璃材料而言,利用飞秒激光辐照以及后续湿化学腐蚀可实现三维空心微通道结构的灵活制造。对于聚合物材料,通过双光子聚合反应的材料设计,可实现高精度三维聚合物微纳结构的增材制造(参见文献: M. Malinauskas, et al., Phy. Rep. 2013, 533, 1)。而在微米尺度上,利用飞秒激光双光子还原技术在金属盐溶液中,可直接实现高导电率三维金属微结构的直写制造(参见文献:T. Tanaka, et al., Appl. Phys. Lett. 2006, 88,081107)。但是利用这个方法目前报道的结构多是由纳米颗粒间堆积实现的结构互联,结构的表面质量和机械性能很难实现器件的实用化。因此,研究任意空间构型三维导电金属微纳结构的新型制造技术具有重要的实用价值。
发明内容
本发明要解决的技术问题在于克服当前三维导电金属微纳结构制造所存在的挑战和瓶颈,提供一种高效、快速、任意构型设计,可稳定牢固工作等三维金属微纳结构制造方法。
本发明的具体技术方案如下:
一种任意构型三维导电金属微纳结构的制造方法,特征点是该方法包括下列步骤:
(1)飞秒激光辐照:将透明材料样品固定在一台三维可计算机编程位移平台上,通过显微物镜将飞秒激光聚焦在所述的透明材料样品上,按计算机编程驱动位移平台运动同时启动飞秒激光辐照过程,在所述的透明材料样品中直写出所需要的三维微通道图案;
(2)三维微通道加工:将飞秒激光辐照后的透明材料样品放入化学腐蚀溶液中,对所述的三维微通道图案进行化学腐蚀,以在透明材料内部获得具有三维几何构型的微通道结构;
(3)连续流动化学镀:采用蠕动泵先将化学镀敏化活化液以一定流速连续输送通过上述微通道结构对通道内表面进行敏化活化,然后再将化学镀液以一定流速连续输送通过已敏化活化的微通道内部以实现金属微纳薄膜的快速沉积;
(4)透明材料去除:将沉积金属微纳结构的透明材料样品放入HF溶液或有机溶剂进行腐蚀,直至透明材料完全被溶解去除,从而获得真三维的导电金属立体微结构。
所述的透明材料为各种玻璃材料,聚合物。
所述的化学腐蚀溶液为HF水溶液(2%-20%)或KOH水溶液(5-20 mol/L,80-90℃) 。
所述的蠕动泵的流速为1 ml/min-100 ml/min。
所述的化学镀敏化活化液为SnCl2-HCl混合溶液(0.05-30 g/L SnCl2溶液和0.5-300 ml/L HCl溶液混合比为1:1)或SnCl2-PdCl2-HCl混合溶液(0.05-30 g/L SnCl2溶液,0.05-3 g/L PdCl2溶液和0.5-300 ml/L HCl溶液的混合比为1:1:1)。
所述任意构型三维导电金属微纳结构为三维银、金、铂或镍微纳结构。
与现有技术相比较,本发明的优点在于:
1)、空间构型的可任意设计性:利用飞秒激光三维直写特性,可在透明材料内部设计出任意空间构型的微通道结构,进而通过流动化学镀在通道内实现金属微纳结构连续沉积,最后实现任意构型的三维金属微结构制造。在整个制造过程由于每个步骤均具有很好的选择性和可控性,金属微纳结构可以有很高的保真度。
2)、高的电导率和高的机械强度:利用连续流动化学镀可在微通道内连续沉积出多种高电导率,厚度可控的金属如银,金,铂,镍等。与飞秒激光直接光还原得到的三维金属微结构相比,通过控制连续流动化学镀,金属微纳薄膜的表面质量和机械强度有很大改善。
3)、可控的金属结构尺寸:通过飞秒激光微加工调控微通道设计尺寸和流动化学镀的时间和镀液成分设计可实现三维金属微纳结构尺寸的灵活控制。
附图说明
图1是本发明用于任意三维构型导电金属微结构制造的流程示意图;
图2是连续流动化学镀三维微通道的装置示意图。
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。请参阅图1,图1是任意构型三维导电金属微纳结构制造的流程示意图。
现以石英玻璃为例来说明本发明,由图1可见本发明利用飞秒激光在玻璃内集成三维导电金属微纳结构的方法包括如下四步骤:
(1)飞秒激光辐照:取尺寸为10 mm×10 mm×2 mm且六面抛光的洁净石英玻璃样品6,固定在三维位移台上;飞秒激光在石英玻璃样品内部直写微通道图案时的中心波长为515nm,重复频率为 400 kHz,脉冲宽度为290 fs;直写微通道图案时采用的数值孔径为0.45的显微物镜聚焦,平均功率为600 mW,扫描速度为0.5 mm/s。
(2)化学腐蚀:将飞秒激光辐照后的石英玻璃样品放入在80℃的10 mol/L KOH溶液中进行超声波辅助刻蚀,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微通道结构。
(3)连续流动化学镀:如图2所示,用蠕动泵7先将化学镀敏化活化液(0.3 g/LSnCl2溶液和10 ml/L HCl溶液等体积混合)从容器8中经橡胶管9及连接器10输送到上述三维微通道内进行通道内表面敏化活化5 min;然后再将化学镀银液(温度为35℃的0.05mol/L的硝酸银溶液和0.025 g/L的葡萄糖溶液混合,混合比为50:1)用类似方法连续输送至上述通道内进行施镀20 min(所有废液经另一个连接器10收集在容器11中),样品清洗干燥后可在玻璃内部获得三维金属银微结构。整个过程蠕动泵的流速为20 ml/min。
(4)玻璃基底去除:将玻璃内部沉积金属微结构的样品放入HF溶液进行腐蚀,直至玻璃基底完全被溶解去除,从而获得真三维的导电金属银立体微结构5(电导率接近体积银电导率)。
本发明方法适用于制造在微米尺度上任意构型三维导电金属微纳结构,只要对飞秒激光加工微通道的方式,连续流动化学镀的参数进行适当的选取即可。
Claims (5)
1.一种任意构型三维导电金属微纳结构的制造方法,其特征在于,该方法包括下列步骤:
步骤1:飞秒激光辐照
将透明材料样品固定在一台三维可计算机编程位移平台上,通过显微物镜将飞秒激光聚焦在所述的透明材料样品上,按计算机编程驱动位移平台运动同时启动飞秒激光辐照过程,在所述的透明材料样品中直写出所需要的三维微通道图案;
步骤2:三维微通道加工
将飞秒激光辐照后的透明材料样品放入化学腐蚀溶液中,对所述的三维微通道图案进行化学腐蚀,以在透明材料内部获得具有三维几何构型的微通道结构;
步骤3:连续流动化学镀
采用蠕动泵先将化学镀敏化活化液以1-100 ml/min的流速连续输送通过上述微通道结构对通道内表面进行敏化活化,然后再将化学镀液以1-100 ml/min的流速连续输送通过已敏化活化的微通道内部以实现金属微纳薄膜的快速沉积;
步骤4:透明材料去除
将沉积金属微纳结构的透明材料样品放入HF溶液或有机溶剂进行腐蚀,直至透明材料完全被溶解去除,从而获得所述任意构型三维导电金属微纳结构。
2.根据权利要求1所述的制造方法,其特征在于,所述的透明材料为玻璃或聚合物。
3.根据权利要求1所述的制造方法,其特征在于,所述化学腐蚀溶液为2%-20%的HF水溶液或5-20 mol/L、温度为80-90℃的KOH水溶液。
4.根据权利要求1所述的制造方法,其特征在于,所述的化学镀敏化活化液为SnCl2-HCl混合溶液或SnCl2-PdCl2-HCl混合溶液;其中,所述SnCl2-HCl混合溶液为0.05-30 g/L的SnCl2溶液和0.5-300 ml/L的 HCl溶液混合,体积比为1∶1;所述SnCl2-PdCl2-HCl混合溶液为0.05-30 g/L 的SnCl2溶液、0.05-3 g/L 的PdCl2溶液和0.5-300 ml/L 的HCl溶液混合,体积比为1∶1∶1。
5.根据权利要求1所述的制造方法,其特征在于,所述任意构型三维导电金属微纳结构为三维银、金、铂或镍微纳结构。
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