CN111331871A - 模具表面处理方法及微针制作方法 - Google Patents

模具表面处理方法及微针制作方法 Download PDF

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CN111331871A
CN111331871A CN202010133816.7A CN202010133816A CN111331871A CN 111331871 A CN111331871 A CN 111331871A CN 202010133816 A CN202010133816 A CN 202010133816A CN 111331871 A CN111331871 A CN 111331871A
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mold
master mold
thin film
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温晓镭
孙剑
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University of Science and Technology of China USTC
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Abstract

一种模具表面处理方法，用于改善微针的脱模效果，包括：对带有微孔结构的母版模具进行清洗；采用氧等离子体对清洗后的母版模具进行活化处理；在活化处理后的母版模具表面依次沉积种子层及薄膜层，其中，薄膜层用于降低母版模具表面的自由能。该方法可促进聚合物材料渗入和填充微孔结构，模具表面沉积Au薄膜层可大幅降低模具表面自由能，有效解决脱模过程中聚合物与模具的粘连问题，提高聚合物微针的加工效率和成功率、延长模具使用寿命。由于Au的生物相容性好，加工过程中不产生有毒有害或危险化学成分，适用于生命科学相关研究，可满足大批量生产需要。并且全过程中采用低温工艺，不会对母版模具造成热损害。

Description

模具表面处理方法及微针制作方法
技术领域
本公开涉及微纳米加工技术领域，特别是涉及一种模具表面处理方法及微针制作方法。
背景技术
微针是由许多微米级针状突起组成的功能性微纳结构，多用于皮肤补水保湿、经皮给药、无痛免疫疗法等美容医药领域。其中，聚合物材料(如透明质酸HA、聚乙烯醇PVA、聚乳酸PLA等)的微针结构由于良好的生物相容性、柔性、高效的药物负载量等特点受到广泛关注。
聚合物微针结构的制作方法一般首先需要一个母版模具(材料通常为聚二甲基硅氧烷PDMS或有机玻璃PMMA等)作为负模，上面加工出许多微孔，再在其上浇铸聚合物材料，待固化成型后进行脱模分离，即可得到与负模的微孔形状互补的微针凸起结构。
但对于微针排列密度大、尺寸小或整体面积较大的情况，在浇铸过程中聚合物可能很难进入微孔内部，导致无法形成与微孔形状互补的微针凸起结构，或由于聚合物与母版模具接触面积大，脱模时发生粘连现象，导致脱模困难、脱模后微针结构出现破损、变形，而母版模具微孔内残留聚合物等问题。这严重影响了聚合物微针结构的加工效率、成品率和母版模具的使用寿命。
为改善上述问题，目前多采用在浇铸聚合物前在模具表面涂敷或沉积含氟聚合物薄膜或长链硅烷抗粘层的方式。但对于PDMS、PMMA等微针常用母版模具材质，这种抗粘层的沉积效率和抗粘效果有限，仍有可能在脱模时发生粘连、脱模困难等情况。另外，旋涂或浸没涂敷方式存在将细小的微孔填没的风险。而气相沉积方式通常较为繁琐，加工过程存在有毒有害或危险化学品成分、不利于生物相容性，并且需要专门的沉积设备，与常规半导体工艺兼容性差。部分气相沉积方式需要加热条件，对常用的母版模具材料(如PDMS等)有潜在影响，可能会导致微孔结构变形，从而影响后续的浇铸工艺。单纯沉积含氟聚合物薄膜或长链硅烷抗粘层的表面处理方式也不能有效促进聚合物填充模具微孔内部，浇铸出的微针结构常有破损、不完整的问题。
发明内容
(一)要解决的技术问题
针对于上述技术问题，本公开提出一种模具表面处理方法及微针制作方法，用于至少解决上述技术问题。
(二)技术方案
根据本公开实施例的第一方面，提供一种模具表面处理方法，用于改善微针的脱模效果，包括：对带有微孔结构的母版模具进行清洗；采用氧等离子体对清洗后的母版模具进行活化处理；在活化处理后的母版模具表面依次沉积种子层及薄膜层，其中，薄膜层用于降低母版模具表面的自由能。
可选地，进行活化处理的时间范围为1-10分钟。
可选地，在活化处理后的母版模具表面沉积Ti种子层或Cr种子层。
可选地，薄膜层为Au薄膜层，Au薄膜层的厚度范围为5-200纳米。
可选地，种子层的厚度范围为1-20纳米。
可选地，对带有微孔结构的母版模具进行清洗，包括：将带有微孔结构的母版模具依次浸入丙酮、异丙醇溶液中超声清洗；采用氮气对超声清洗后的母版模具进行干燥。
可选地，超声清洗的时间范围为5-10分钟。
可选地，Ti种子层或Cr种子层的厚度为3-5纳米。
可选地，采用磁控溅射镀膜机或电子束蒸发镀膜机或热蒸发镀膜机在活化处理后的母版模具表面依次沉积种子层及薄膜层。
根据本公开实施例的第二方面，提供一种微针制作方法，其特征在于，包括：对带有微孔结构的母版模具进行清洗；采用氧等离子体对清洗后的母版模具进行活化处理；在活化处理后的母版模具表面依次沉积种子层及Au薄膜层；在Au薄膜层上浇铸高分子聚合物材料，待聚合物材料固化成型后进行脱模分离，得到聚合物微针。
(三)有益效果
本公开提一种模具表面处理方法及微针制作方法，有益效果为：
1、该方法对母版模具表面进行氧等离子体活化处理，可促进聚合物材料渗入和填充微孔结构，模具表面沉积Au可大幅降低模具表面自由能，有效解决脱模过程中聚合物与模具的粘连问题，提高聚合物微针的加工效率和成功率、延长模具使用寿命。
2、由于Au的生物相容性好，加工过程中不产生有毒有害或危险化学成分，适用于生命科学相关研究。
3、该方法操作简单，使用常规半导体加工设备即可实现，与半导体加工工艺链兼容性好，可满足大批量生产需要。全过程中采用低温工艺，不会对母版模具造成热损害。
附图说明
为了更完整地理解本公开及其优势，现在将参考结合附图的以下描述，此处的附图被并入说明书中并构成本说明书的一部分，示出了符合本公开的实施例，并与说明书一起用于解释本公开的原理。其中：
图1示意性示出了根据本公开一示例性实施例的模具表面的处理方法的流程图；
图2示意性示出了根据本公开一示例性实施例的聚合物微针的制作方法的流程图；
图3示出了根据本公开一示例性实施例的模具表面处理方法对PDMS母版模具表面进行处理后，浇铸透明质酸，固化成型脱模后得到的透明质酸微针阵列显微结构图；
图4示出了不对母版模具进行表面处理，直接浇铸透明质酸，固化成型脱模后得到的透明质酸结构显微结构图；
图5示出了使用常规方法(气相沉积长链硅烷抗粘层)对PDMS母版模具表面进行处理后，浇铸透明质酸，固化成型脱模后得到的透明质酸微针阵列显微结构图。
具体实施方式
以下，将参照附图来描述本公开的实施例。但是应该理解，这些描述只是示例性的，而并非要限制本公开的范围。在下面的详细描述中，为便于解释，阐述了许多具体的细节以提供对本公开实施例的全面理解。然而，明显地，一个或多个实施例在没有这些具体细节的情况下也可以被实施。此外，在以下说明中，省略了对公知结构和技术的描述，以避免不必要地混淆本公开的概念。
本公开实施例提供一种模具表面的处理方法，该方法包括对带有微孔结构的母版模具进行清洗。采用氧等离子体对清洗后的母版模具进行活化处理。在活化处理后的母版模具表面依次沉积种子层及薄膜。该方法可改善聚合物微针脱模效果。
图1示意性示出了根据本公开一示例性实施例的模具表面的处理方法的流程图。如图1所示，该方法例如可以包括操作S101～S103。
S101，对带有微孔结构的母版模具进行清洗。
在本实施例一可行的方式中，可以将带有微孔结构的母版模具依次浸入丙酮、异丙醇溶液中进行超声清洗，超声清洗的时间范围5-10分钟，例如可以超声清洗5分钟，本公开不做限制。母版模具例如可以为PDMS模板。
超声清洗完成后，取出母版模具，使用氮气将其吹干，并转移至干燥环境中。
S102，采用氧等离子体对清洗后的母版模具进行活化处理。
在本实施例一可行的方式中，可以将清洗后的母版模具放入可产生氧等离子体的设备中，采用氧等离子体进行活化处理，以促进聚合物材料渗入和填充母版模具的微孔结构。活化处理的时间范围为1-10分钟，例如可以活化5分钟，本公开不做限制。
在本实施例一可行的方式中，可产生氧等离子体的设备包括但不限于反应离子刻蚀机RIE、电感耦合等离子体刻蚀机ICP、等离子体去胶机等具有氧等离子体轰击功能的设备。优选的，使用反应离子刻蚀机，活化处理时间为5分钟。
S103，在活化处理后的母版模具表面依次沉积种子层及薄膜层，其中，薄膜层用于降低母版模具表面的自由能。
在本实施例一可行的方式中，将活化处理后的母版模具放入真空镀膜设备中，依次沉积种子层及薄膜层，以降低母版模具表面的自由能。其中，种子层的厚度范围可以为1-20纳米。种子层例如可以为Ti种子层或Cr种子层，厚度优选为3-5纳米，本公开不做限制。薄膜层可以为Au薄膜层，其厚度例如可以为5-200纳米，优选的厚度范围为10-20纳米。
在本实施例一可行的方式中，真空镀膜设备包括但不限于磁控溅射镀膜机、电子束蒸发镀膜机、热蒸发镀膜机等，优选的，使用磁控溅射镀膜机。
基于上述模具表面的处理方法，本公开实施例还提供一种聚合物微针的制作方法。图2示意性示出了根据本公开一示例性实施例的聚合物微针的制作方法的流程图。如图2所示，该方法例如可以包括操作S201～S204。
S201，对带有微孔结构的母版模具进行清洗。
S202，采用氧等离子体对清洗后的母版模具进行活化处理。
S203，在活化处理后的母版模具表面依次沉积种子层及薄膜层。
S204，在Au薄膜层上浇铸高分子聚合物材料，待聚合物材料固化成型后进行脱模分离，得到聚合物微针。
在本实施例一可行的方式中，聚合物材料例如可以采用的是透明质酸，抽真空1小时后转移至通风干燥环境中，待透明质酸固化成型后进行脱模分离，得到透明质酸微针阵列结构。
本实施例未尽细节之处，请参见上述模具表面处理方法的实施例，此处不再赘述。
上述实施的方法，对母版模具表面进行氧等离子体活化处理可促进聚合物材料渗入和填充微孔结构。模具表面沉积Au可大幅降低模具表面自由能，有效解决脱模过程中聚合物与模具的粘连问题。并且由于Au的生物相容性好，加工过程中不产生有毒有害或危险化学成分，适用于生命科学相关研究。该表面处理方式使用常规半导体加工设备，适合大批量生产，且采用低温工艺，不会对母版模具造成热损害。
本公开还对本实施例提供的方法进行了验证，图3-图5为不同方法得到微针的表面形貌。
图3示出了根据本公开一示例性实施例的的模具表面处理方法对PDMS母版模具表面进行处理后，浇铸透明质酸，固化成型脱模后得到的透明质酸微针阵列显微结构图。图3显示微针形貌完好，且阵列完整，说明浇铸过程中透明质酸完全填充了母版模具微孔结构，并且脱模时没有发生粘连问题。
图4示出了不对母版模具进行表面处理，直接浇铸透明质酸，固化成型脱模后得到的透明质酸结构显微结构图。图4显示没有形成所需的微针形状，只有部分微针基部残留，说明浇铸过程中透明质酸没有完全渗入填充到母版模具微孔结构内部。
图5示出了使用常规方法(气相沉积长链硅烷抗粘层)对PDMS母版模具表面进行处理后，浇铸透明质酸，固化成型脱模后得到的透明质酸微针阵列显微结构图。图5显示微针阵列不完整、缺陷较多，说明浇铸过程中透明质酸没有完全填充母版模具的微孔结构，且脱模时由于粘连作用造成了部分微针折断、破损和变形。
以上所述的具体实施例，对本公开的目的、技术方案和有益效果进行了进一步详细说明，所应理解的是，以上所述仅为本公开的具体实施例而已，并不用于限制本公开，凡在本公开的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本公开的保护范围之内。

Claims (10)

1.一种模具表面处理方法，用于改善微针的脱模效果，其特征在于，包括：
对带有微孔结构的母版模具进行清洗；
采用氧等离子体对清洗后的母版模具进行活化处理；
在活化处理后的母版模具表面依次沉积种子层及薄膜层，其中，所述薄膜层用于降低所述母版模具表面的自由能。
2.根据权利要求1所述的方法，其特征在于，所述进行活化处理的时间范围为1-10分钟。
3.根据权利要求1所述的方法，其特征在于，在活化处理后的母版模具表面沉积Ti种子层或Cr种子层。
4.根据权利要求1所述的方法，其特征在于，所述薄膜层为Au薄膜层，所述Au薄膜层的厚度范围为5-200纳米。
5.根据权利要求1所述的方法，其特征在于，所述种子层的厚度范围为1-20纳米。
6.根据权利要求1所述的方法，其特征在于，所述对带有微孔结构的母版模具进行清洗，包括：
将所述带有微孔结构的母版模具依次浸入丙酮、异丙醇溶液中超声清洗；
采用氮气对超声清洗后的母版模具进行干燥。
7.根据权利要求6所述的方法，其特征在于，所述超声清洗的时间范围为5-10分钟。
8.根据权利要求3所述的方法，其特征在于，所述Ti种子层或Cr种子层的厚度为3-5纳米。
9.根据权利要求1所述的方法，其特征在于，采用磁控溅射镀膜机或电子束蒸发镀膜机或热蒸发镀膜机在活化处理后的母版模具表面依次沉积种子层及薄膜层。
10.一种基于权利要求1-9任一项所述方法的微针制作方法，其特征在于，包括：
对带有微孔结构的母版模具进行清洗；
采用氧等离子体对清洗后的母版模具进行活化处理；
在活化处理后的母版模具表面依次沉积种子层及Au薄膜层；
在所述Au薄膜层上浇铸高分子聚合物材料，待所述聚合物材料固化成型后进行脱模分离，得到聚合物微针。
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