CN113897609B - 一种超疏水导热多层膜及其制备方法 - Google Patents
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Abstract
本发明公开了一种超疏水导热多层膜及其制备方法，包括如下步骤：采用等离子体增强化学气相沉积技术以高纯甲烷和四氟化碳为碳源气体在单晶硅基片表面制备碳膜；采用磁控溅射技术以高纯铜为靶材在步骤中所生长的碳膜表面溅射沉积铜纳米膜；采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在所生长的铜纳米膜表面再次沉积碳膜；重复制备碳膜及铜纳米膜表面再次沉积碳膜的步骤2～4次；对所制备的多层膜在氢气氛围保护下高温烧结；采用PECVD技术以高纯四氟化碳为工作气体对所烧结处理后的多层膜实施等离子体处理。通过上述步骤所获得的多层膜具有优异的超疏水和导热功能，在电子元器件散热和防水方面具有很好的应用前景。
Description
技术领域
本发明属于超疏水和导热薄膜材料制备技术领域，具体涉及一种超疏水导热多层膜及其制备方法。
背景技术
随着工业和电子科学技术的不断发展，电子产品不断微型化、集成化和高性能化，由此导致电子系统和芯片在运行过程中将产生大量热量。如果产生的热量不能及时散出,这些累积的热量将引起电子系统和芯片温度过高，特别是电子模块与外界环境之间过大的温差会形成热应力，直接影响电子芯片的电性能、工作频率、机械强度以及可靠性。并且，电子系统和设备中的金属电路在长期使用过程中，内部金属电路及芯片可能会受潮或遇到水，这将导致金属电路及芯片发生腐蚀或短路，导致电子产品性能衰退、失效甚至可能引发重大事故。此外，电子产品能够在严苛的高温高湿甚至腐蚀的环境中持续稳定地工作也成为高性能特种电子产品必须具备的性能。因此，开发一种兼具防水和导热功能的薄膜材料在电子系统和芯片散热和防水方面具有很好的应用价值。
发明内容
本发明旨在为电子系统和芯片在散热和防水材料和技术方面提供一种超疏水导热多层膜及其制备方法。该方法包括下述步骤：
（1）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在单晶硅基片表面制备碳膜；
（2）采用磁控溅射技术以高纯铜为靶材在步骤（1）中所生长的碳膜表面溅射沉积铜纳米膜；
（3）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在步骤（2）中所生长的铜纳米膜表面再次沉积碳膜；
（4）重复步骤（2）、步骤（3）2～4次实现多次表面溅射沉积铜纳米膜及表面制备碳膜；
（5）对步骤（3）或步骤（4）中所制备的多层膜在氢气氛围保护下实施高温烧结处理；
（6）采用PECVD技术以高纯四氟化碳为工作气体对步骤（5）中所烧结处理后的多层膜实施等离子体处理。经过上述步骤变可获得一种超疏水导热多层膜。
所述的步骤（1）中高纯甲烷的纯度为99.999%及以上，高纯四氟化碳的纯度为99.9999%及以上。PECVD沉积参数为：射频功率300～450W，射频频率13.56MHz，基片温度350～400℃，腔体压强50～90Pa，通入高纯甲烷气体流量30～50sccm，通入高纯四氟化碳气体流量10～20sccm，沉积时间30～50分钟。在此步骤中，甲烷和四氟化碳一方面为碳膜生长提供碳源，另一方面二者所形成的等离子体能为碳膜提供大量-CHn和-CFn基团。这些低表面能基团有利于降低薄膜表面能，从而提高薄膜超疏水性能。
所述的步骤（2）中高纯铜靶的纯度为99.9995%及以上，磁控溅射沉积参数为：射频功率180～280W，射频频率13.56MHz，基片温度350～400℃，腔体压强3～10Pa，通入纯度为99.999%的氩气气体流量5～15sccm，沉积时间20～40秒。在此步骤中，碳膜表面生长铜纳米膜不仅可以通过异质多层膜结构构造具有一定粗糙度结构的表面，从而提高薄膜疏水性。它还能通过后续热处理工艺诱导碳膜石墨化，并利用铜纳米膜本身的高热导率特性，提高薄膜热导率。
所述的步骤（3）中PECVD工艺参数与步骤（1）中的工艺参数完全一致。
所述的步骤（4）重复步骤（2）、步骤（3）2～4次。在此步骤中，通过重复步骤（2）、步骤（3）的次数调控薄膜表面粗糙度，并利用碳膜内大量-CHn和-CFn基团，实现薄膜的超疏水性能。
所述的步骤（5）中氢气纯度为99.999%及以上，高温烧结的温度为450～500℃，高温烧结时间为1～2小时。
所述的步骤（6）中高纯四氟化碳的纯度为99.9999%及以上。PECVD等离子体处理的参数为：射频功率300～450W，射频频率13.56MHz，基片温度350～400℃，腔体压强50～90Pa，通入高纯四氟化碳气体流量30～40sccm，等离子体处理时间5～10分钟。在此步骤中，对烧结处理后的多层膜实施四氟化碳等离子体处理的主要功能是一方面钝化多层膜表面，减少缺陷的产生和提高薄膜稳定性，另一方面能在多层膜表面补充因退火处理所减少的低表面能基团，提高薄膜超疏水性能。
通过上述步骤，在单晶硅或玻璃基片表面便可制备出一种具有超疏水导热功能的多层膜。
散热和防水是电子系统和芯片高性能稳定运行的两个重要因素。本发明利用碳膜和铜膜的高热导率特性使所制备的碳铜复合膜具有高导热功能。同时，利用多层膜结构、退火以及等离子处理工艺促使多层复合膜表面具有多级粗糙结构，并结合等离子体产生的-CH n 和-CF n 基团实现多层复合膜的低表面能特性。最终，结合多层复合膜表面的多级粗糙结构和低表面能特性实现其超疏水功能。从而，本发明所制备的多层复合膜不仅具有优良的导热特性还具有超疏水功能。由于本发明所采用的技术方法和工艺同传统半导体工艺相兼容，因此在电子系统和芯片的散热和防水方面具有很好的应用前景。
具体实施方式
为进一步阐述本发明所提供的一种超疏水导热多层膜及其制备方法，以下实施案例用以说明本发明，但不用于限制本发明。
实施例1
一种超疏水导热多层膜及其制备方法，该方法包括以下步骤：
（1）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在表面制备碳膜。高纯甲烷的纯度为99.999%，高纯四氟化碳的纯度为99.9999%。PECVD沉积参数为：射频功率300W，射频频率13.56MHz，基片温度350℃，腔体压强50Pa，通入高纯甲烷气体流量30sccm，通入高纯四氟化碳气体流量10sccm，沉积时间50分钟。
（2）采用磁控溅射技术以高纯铜为靶材在步骤（1）中所生长的碳膜表面溅射沉积铜纳米膜。高纯铜靶的纯度为99.9995%，磁控溅射沉积参数为：射频功率180W，射频频率13.56MHz，基片温度350℃，腔体压强3Pa，通入纯度为99.999%的氩气气体流量5sccm，沉积时间20秒。
（3）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在步骤（2）中所生长的铜纳米膜表面再次沉积碳膜。
（4）依次重复步骤（2）、步骤（3）2次。
（5）对步骤（4）中所制备的多层膜在氢气氛围保护下实施高温烧结处理。氢气纯度为99.999%，高温烧结的温度为450℃，高温烧结时间为2小时。
（6）采用PECVD技术以高纯四氟化碳为工作气体对步骤（5）中所烧结处理后的多层膜实施等离子体处理。高纯四氟化碳的纯度为99.9999%。PECVD等离子体处理的参数为：射频功率300W，射频频率13.56MHz，基片温度350℃，腔体压强50Pa，通入高纯四氟化碳气体流量30sccm，等离子体处理时间10分钟。
经过上述步骤变可获得一种超疏水导热多层膜。多层膜的热导率可达12.5W/mK，水接触角可达153°，滚动角可达5°。
实施例1-1
方法及步骤同实施例1，仅不进行步骤（2）在步骤（1）中所生长的碳膜表面溅射沉积铜纳米膜工艺。则步骤（3）为：采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在步骤（1）中所生长的碳膜表面再次沉积碳膜。步骤（4）为：重复步骤（3）2次。得到的多层膜的热导率为4.5W/mK，水接触角可达150°，滚动角可达6°。
实施例1-2
方法及步骤同实施例1，仅不进行步骤（3）的铜纳米膜表面再次沉积碳膜的步骤，则步骤（4）为：重复步骤（2）2次。得到的多层膜的热导率为5.6W/mK，水接触角低于130°，滚动角高达30°。
实施例1-3
方法及步骤同实施例1，仅步骤（4）中仅重复步骤（2）2次。得到的多层膜的热导率为5.3W/mK，水接触角低于120°，滚动角高于35°。
实施例1-4
方法及步骤同实施例1，仅步骤（4）中仅重复步骤（3）2次。得到的多层膜的热导率为4.5W/mK，水接触角可达151°，滚动角可达8°。
实施例1-5
方法及步骤同实施例1，不进行步骤（4）的重复性步骤。得到的多层膜的热导率为5.6W/mK，水接触角小于140°，滚动角高于60°。
实施例1-6
方法及步骤同实施例1，不进行步骤（6）的步骤。得到的多层膜的热导率为12.5W/mK，水接触角可达150°，滚动角可达8°。
实施例2
一种超疏水导热多层膜及其制备方法，该方法包括以下步骤：
（1）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在单晶硅基片表面制备碳膜。高纯甲烷的纯度为99.999%，高纯四氟化碳的纯度为99.9999%。PECVD沉积参数为：射频功率450W，射频频率13.56MHz，基片温度400℃，腔体压强90Pa，通入高纯甲烷气体流量50sccm，通入高纯四氟化碳气体流量20sccm，沉积时间30分钟。
（2）采用磁控溅射技术以高纯铜为靶材在步骤（1）中所生长的碳膜表面溅射沉积铜纳米膜。高纯铜靶的纯度为99.9995%，磁控溅射沉积参数为：射频功率280W，射频频率13.56MHz，基片温度400℃，腔体压强10Pa，通入纯度为99.999%的氩气气体流量15sccm，沉积时间40秒。
（3）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在步骤（2）中所生长的铜纳米膜表面再次沉积碳膜。
（4）依次重复步骤（2）、步骤（3）4次。
（5）对步骤（4）中所制备的多层膜在氢气氛围保护下实施高温烧结处理。氢气纯度为99.999%，高温烧结的温度为500℃，高温烧结时间为1小时。
（6）采用PECVD技术以高纯四氟化碳为工作气体对步骤（5）中所烧结处理后的多层膜实施等离子体处理。高纯四氟化碳的纯度为99.9999%。PECVD等离子体处理的参数为：射频功率450W，射频频率13.56MHz，基片温度400℃，腔体压强90Pa，通入高纯四氟化碳气体流量40sccm，等离子体处理时间5分钟。
经过上述步骤变可获得一种超疏水导热多层膜。多层膜的热导率可达13.7W/mK，水接触角可达158°，滚动角可达4°。
实施例3
一种超疏水导热多层膜及其制备方法，该方法包括以下步骤：
（1）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在单晶硅基片表面制备碳膜。高纯甲烷的纯度为99.999%，高纯四氟化碳的纯度为99.9999%。PECVD沉积参数为：射频功率400W，射频频率13.56MHz，基片温度380℃，腔体压强70Pa，通入高纯甲烷气体流量40sccm，通入高纯四氟化碳气体流量15sccm，沉积时间40分钟。
（2）采用磁控溅射技术以高纯铜为靶材在步骤（1）中所生长的碳膜表面溅射沉积铜纳米膜。高纯铜靶的纯度为99.9995%，磁控溅射沉积参数为：射频功率230W，射频频率13.56MHz，基片温度380℃，腔体压强7Pa，通入纯度为99.999%的氩气气体流量10sccm，沉积时间30秒。
（3）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在步骤（2）中所生长的铜纳米膜表面再次沉积碳膜。
（4）依次重复步骤（2）、步骤（3）3次。
（5）对步骤（4）中所制备的多层膜在氢气氛围保护下实施高温
烧结处理。氢气纯度为99.999%，高温烧结的温度为480℃，高温烧结时间为1.5小时。
（6）采用PECVD技术以高纯四氟化碳为工作气体对步骤（5）中所烧结处理后的多层膜实施等离子体处理。高纯四氟化碳的纯度为99.9999%。PECVD等离子体处理的参数为：射频功率380W，射频频率13.56MHz，基片温度380℃，腔体压强70Pa，通入高纯四氟化碳气体流量35sccm，等离子体处理时间8分钟。
经过上述步骤变可获得一种超疏水导热多层膜。多层膜的热导率可达11.6W/mK，水接触角可达152°，滚动角可达6°。
以上所述为本发明较佳实施例而已，但本发明不应该局限于该实施实例所公开的内容。所以凡是不脱离本发明所公开的精神下完成的等效或修改，都落入本发明保护的范围。
Claims (6)
1.一种超疏水导热多层膜的制备方法，其特征在于，该方法包括下述步骤：
（1）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在单晶硅基片表面制备碳膜，PECVD沉积参数为：射频功率300～450W，射频频率13.56MHz，基片温度350～400℃，腔体压强50～90Pa，通入高纯甲烷气体流量30～50sccm，通入高纯四氟化碳气体流量10～20sccm，沉积时间30～50分钟；
（2）采用磁控溅射技术以高纯铜为靶材在步骤（1）中所生长的碳膜表面溅射沉积铜纳米膜；
（3）采用PECVD技术以高纯甲烷和四氟化碳为碳源气体在步骤（2）中所生长的铜纳米膜表面再次沉积碳膜，PECVD沉积参数为：射频功率300～450W，射频频率13.56MHz，基片温度350～400℃，腔体压强50～90Pa，通入高纯甲烷气体流量30～50sccm，通入高纯四氟化碳气体流量10～20sccm，沉积时间30～50分钟；
（4）依次重复步骤（2）、步骤（3）2～4次；
（5）对步骤（4）中所制备的多层膜在氢气氛围保护下实施高温烧结处理；
（6）采用PECVD技术以高纯四氟化碳为工作气体对步骤（5）中所烧结处理后的多层膜实施等离子体处理，获得超疏水导热多层膜。
2.根据权利要求1所述的一种超疏水导热多层膜的制备方法，其特征在于，步骤（1）中高纯甲烷的纯度为99.999%及以上，高纯四氟化碳的纯度为99.9999%。
3.根据权利要求1所述的一种超疏水导热多层膜的制备方法，其特征在于，步骤（2）中高纯铜靶的纯度为99.9995%及以上，磁控溅射沉积参数为：射频功率180～280W，射频频率13.56MHz，基片温度350～400℃，腔体压强3～10Pa，通入纯度为99.999%及以上的氩气气体流量5～15sccm，沉积时间20～40秒。
4.根据权利要求1所述的一种超疏水导热多层膜的制备方法，其特征在于，步骤（3）中高纯甲烷的纯度为99.999%及以上，高纯四氟化碳的纯度为99.9999%。
5.根据权利要求1所述的一种超疏水导热多层膜的制备方法，其特征在于，步骤（5）中氢气纯度为99.999%及以上，高温烧结的温度为450～500℃，高温烧结时间为1～2小时。
6.根据权利要求1所述的一种超疏水导热多层膜的制备方法，其特征在于，步骤（6）中高纯四氟化碳的纯度为99.9999%及以上，PECVD等离子体处理的参数为：射频功率300～450W，射频频率13.56MHz，基片温度350～400℃，腔体压强50～90Pa，通入高纯四氟化碳气体流量30～40sccm，等离子体处理时间5～10分钟。
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