CN114855122A - 一种超薄金属膜及其制备方法和应用 - Google Patents

一种超薄金属膜及其制备方法和应用 Download PDF

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CN114855122A
CN114855122A CN202210356275.3A CN202210356275A CN114855122A CN 114855122 A CN114855122 A CN 114855122A CN 202210356275 A CN202210356275 A CN 202210356275A CN 114855122 A CN114855122 A CN 114855122A
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metal film
substrate
film
ion beam
thickness
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马东旭
陈艺勤
段辉高
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Hunan University
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Abstract

本发明公开一种超薄金属膜的制备方法，包括如下步骤：提供靶金属及衬底，在所述衬底的表面沉积对所述靶金属具有浸润性的缓冲层，其中所述靶金属为以三维岛状模式生长的金属；获取所述靶金属在所述衬底上刚好形成完整连续薄膜的厚度阈值，使用薄膜沉积方法在所述衬底表面沉积一层厚度大于或等于厚度阈值的靶金属膜；在高真空状态下，采用离子束斜角刻蚀方法将惰性气体离子束以一定角度刻蚀所述靶金属膜表面，使所述靶金属膜表面的金属原子逸出，反向减薄至厚度小于厚度阈值，完成超薄金属膜的制备。本发明的超薄金属膜的制备方法可以制备厚度小于成膜厚度阈值的超薄金属膜。本发明还提供一种超薄金属膜及其应用。

Description

一种超薄金属膜及其制备方法和应用
【技术领域】
本发明涉及超薄金属膜技术领域，具体涉及一种超薄金属膜及其制备方法和应用。
【背景技术】
在光电产业中，氧化铟锡(ITO)一直作为透明电极材料被广泛应用于显示屏、光伏电池等光电器件中，然而，氧化铟锡(ITO)本质上是脆性的，不耐弯折，不适用于柔性显示屏等柔性器件中，而超薄金属膜因其有着高的透明度、高的导电性、高的柔性成为了传统氧化铟锡(ITO)透明电极的有希望的替代者。
相关技术中，超薄金属膜通常采用薄膜沉积技术直接沉积在衬底表面，金属在衬底上通常以三维岛状模式(Vomler-Weber模式)生长，在沉积的厚度未达到厚度阈值之前，沉积的金属粒子呈颗粒状分散在衬底上，形成多个不连续的岛状结构，无法形成完整连续的金属薄膜，即通过薄膜沉积技术无法得到厚度小于厚度阈值的连续完整金属薄膜。因此，实有必要提供一种超薄金属膜及其制备方法和应用以解决上述问题。
【发明内容】
本发明要解决的技术问题是在于提供一种超薄金属膜及其制备方法和应用，通过预先沉积厚度大于或等于厚度阈值的靶金属膜，然后再通过刻蚀的方式对靶金属膜进行反向削减，可以得到厚度小于厚度阈值的靶金属膜。
为实现上述目的，本发明的技术方案为：
一种超薄金属膜的制备方法，包括如下步骤：
S1：提供靶金属及衬底，在所述衬底的表面沉积对所述靶金属具有浸润性的缓冲层，其中所述靶金属为以三维岛状模式生长的金属；
S2：获取所述靶金属在所述衬底上刚好形成完整连续薄膜的厚度阈值，使用薄膜沉积方法在所述衬底表面沉积一层厚度大于或等于厚度阈值的靶金属膜；
S3：在高真空状态下，采用离子束斜角刻蚀方法将惰性气体离子束以一定角度刻蚀所述靶金属膜表面，使所述靶金属膜表面的金属原子逸出，反向减薄至厚度小于厚度阈值，完成超薄金属膜的制备。
优选的，所述靶金属为金、银、铜、铝或是各自的合金；所述衬底采用硅、氧化硅、石英、玻璃、聚对苯二甲酸乙二酯、聚萘二甲酸乙二醇酯或聚酰亚胺材料制成；所述缓冲层的材料为二氧化钛、氧化锌或硫化锌。
优选的，所述步骤S2中靶金属的沉积厚度D1与厚度阈值D0的关系为：0纳米≤D1－D0≤20纳米。
优选的，所述惰性气体离子束的中轴线与所述衬底表面的夹角小于或等于45°，所述惰性气体离子束的轰击面积大于所述衬底表面的面积，
优选的，所述惰性气体离子束中的惰性气体选择为氩气、氦气、氖气、氪气或氙气。
优选的，在所述惰性气体离子束刻蚀过程中，所述衬底沿其中轴线均匀旋转，驱动所述靶金属膜均匀旋转。
优选的，所述步骤S2中“薄膜沉积方法”选自离子束溅射沉积、热蒸发沉积、电子束蒸发沉积或磁控溅射沉积中的一种。
优选的，所述步骤S2中“薄膜沉积方法”为离子束溅射沉积，其与步骤S3中的“离子束斜角刻蚀方法”共用一台离子束溅射设备。
本发明还提供一种超薄金属膜，采用上述的制备方法制备而成，所述超薄金属膜的厚度小于等于15纳米，表面均方根粗糙度为0.2-0.5纳米，所述超薄金属膜对550纳米光的透光率不低于30％。
本发明还提供一种超薄金属膜的应用，所述超薄金属膜采用上述的制备方法制备而成，所述超薄金属膜应用于光电器件中的透明电极。
与相关技术相比，本发明提供的一种超薄金属膜的制备方法，通过先沉积后刻蚀的方式，可以制备厚度低于厚度阈值的超薄金属膜，将其应用于光电器件中的透明电极，可以在保证导电性的同时，获得良好的透光性及柔性。
【附图说明】
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其它的附图，其中：
图1为本发明提供的一种超薄金属膜的制备方法的流程图。
【具体实施方式】
为了使本技术领域的人员更好地理解本发明实施例中的技术方案，并使本发明的上述目的、特征和优点能够更加明显易懂，下面结合本申请的附图对本发明的具体实施方式作进一步的说明。
请结合参阅图1，本发明提供一种超薄金属膜的制备方法，包括如下步骤：
S1：提供靶金属及衬底，在所述衬底的表面沉积对所述靶金属具有浸润性的缓冲层，其中所述靶金属为以三维岛状模式生长的金属。
所述靶金属在衬底表面沉积成膜过程中，主要存在两个阶段：
第一阶段：岛状生长模式阶段，由于所述靶金属与所述衬底之间的浸润性较弱，到达所述衬底表面的靶金属原子就会更倾向于自己相互键合起来，而不容易与衬底原子相键合，于是所述靶金属原子首先在衬底表面上凝聚成无数个孤立的小核，进而形成三维的岛；
第二阶段：成膜阶段，随着靶金属的继续沉积，三维岛状结构持续扩大，相邻两个岛之间的间隙减小，并逐渐被靶金属原子填积，形成连续完整的金属膜。
优选的，所述靶金属为金、银、铜、铝或是各自的合金；所述衬底采用硅、氧化硅、石英、玻璃、聚对苯二甲酸乙二酯、聚萘二甲酸乙二醇酯或聚酰亚胺材料制成；所述缓冲层的材料为二氧化钛、氧化锌或硫化锌。
S2：获取所述靶金属在所述衬底上刚好形成完整连续薄膜的厚度阈值，使用薄膜沉积方法在所述衬底表面沉积一层厚度大于或等于厚度阈值的靶金属膜。
靶金属在所述衬底上刚好形成完整连续薄膜的厚度阈值D0可以通过经验值获取，也可以通过多次的试验进行测得。对所述衬底进行降温处理，并且设置与所述靶金属具有更好浸润性的缓冲层来细化金属晶粒，可以减小靶金属原子在所述衬底表面的迁移扩散，降低所述靶金属的厚度阈值D0。
以银为例，使用热蒸发沉积方法在硅衬底上沉积金属银膜时，厚度阈值为15纳米，即厚度生长到15纳米左右时才能形成完整连续的薄膜，低于这个厚度时，薄膜表现为颗粒状或者孔洞。
所述薄膜沉积方法采用离子束溅射沉积方法、热蒸发沉积方法、电子束蒸发沉积方法或磁控溅射沉积方法。优选的，所述薄膜沉积方法选择为离子束溅射沉积方法，离子束溅射沉积方法各向同性更好，在后续的刻蚀工艺中，靶金属膜越是呈现非晶态越有利于刻蚀得到均匀的超薄金属膜，这是因为没有明显晶型和晶向的靶金属膜在刻蚀时可以得到各向同性的刻蚀速率和均匀性，有利于制备更均匀的超薄金属膜。进一步的，所述步骤S2采用的“离子束溅射沉积方法”与步骤S3中的“离子束斜角刻蚀方法”共用一台离子束溅射设备，所述离子束溅射设备包括两个离子源，其中一个离子源用于执行步骤S2中的“离子束溅射沉积方法”，另一个离子源用于执行步骤S3中的“离子束斜角刻蚀方法”，采用共用设备的方法，在步骤S2执行完成后，不需要对样品进行转移，直接调换离子源进行步骤S3即可，操作快捷方便，并且可以避免在转移中对样本造成损伤。
所述靶金属的沉积厚度D1越大，对于该步骤中沉积的精度要求就越低，但是由于后续步骤中，需要对靶金属膜的厚度进行反向削减，因此沉积厚度D1越大，在后续的削减过程中，需要削减的厚度也越大，会造成靶金属的大量浪费，因此沉积厚度D1并非是越大越好，在本发明中，靶金属的沉积厚度D1与所述厚度阈值D0的关系为：0纳米≤D1－D0≤20纳米，既可以降低对沉积精度的要求，又可以兼顾后续削减工艺。
S3：在高真空状态下，采用离子束斜角刻蚀方法将惰性气体离子束以一定角度刻蚀所述靶金属膜表面，使所述靶金属膜表面的金属原子逸出，反向减薄至厚度小于厚度阈值，完成超薄金属膜的制备。
刻蚀的原理为：惰性气体离子不是所述靶金属膜的活性刻蚀剂，通过所述惰性气体离子束的物理轰击，可以使所述靶金属膜表面的原子逸出并脱离膜表面，随着惰性气体离子束轰击时间的增加，所述靶金属膜的厚度逐渐减小，形成反向减薄。
为了保证靶金属原子的顺利逸出，所述惰性气体离子束需要以一定角度进行刻蚀，具体的，所述惰性气体离子束的中轴线与所述衬底表面的夹角小于或等于45°。为了保证刻蚀的均匀性，所述惰性气体离子束的轰击面积大于所述衬底表面的面积。
所述靶金属膜的刻蚀质量随着所述惰性气体离子束的束流大小和能量大小变化，呈高斯分布的特点。如果惰性气体离子束的能量太高，会导致靶金属原子获得额外的能量从而热运动增强，更容易重新发生迁移和聚集，不利于形成完整连续的薄膜；如果惰性气体离子束的能量太低，会导致部分惰性气体离子无法到达靶金属膜表面或者无法将金属原子刻蚀逸出，导致获得的超薄金属膜均匀性变差；如果惰性气体离子束的束流太大，会导致刻蚀速率太快，无法更精确地控制超薄金属膜的厚度；如果惰性气体离子束的束流太小，会导致离子源发射出的惰性气体离子数量少，各个位置刻蚀的不均匀，导致获得的超薄金属膜均匀性变差。以考夫曼离子源制备超薄银薄膜为例，提供的惰性气体离子束的束流为40毫安，能量为200电子伏特。
所述惰性气体离子束中的惰性气体选择为氩气、氦气、氖气、氪气或氙气，优选的为氩气。
进一步的，为了提高刻蚀的均匀性，还可以将所述衬底沿其中轴线均匀旋转，驱动所述靶金属膜均匀旋转，使所述靶金属膜表面的各个方向能够均匀的接受所述惰性气体离子束的冲击。具体的，所述衬底可以平整的放置于某一工作台上，由工作台驱动旋转。
采用本发明的制备方法各步骤得到的产物如图1所示，通过薄膜沉积技术在所述衬底1表面沉积缓冲层2，然后继续沉积靶金属，在沉积的初始阶段，靶金属在所述衬底1上形成不连续的岛状结构3，随着沉积的继续，离散的靶金属团簇越来越密集，进一步连接、合并，最后形成覆盖整个衬底1表面的连续完整靶金属膜4；刻蚀阶段，在高真空状态下使用惰性气体Ar+离子以一定角度轰击靶金属膜4表面，在离子束的轰击下，靶金属膜4表面的金属原子发生逸出脱离薄膜表面，随着离子束轰击时间的增加，靶金属膜4的厚度逐渐减小，最后得到厚度小于厚度阈值的纳米级超薄金属膜5。
本发明还提供一种超薄金属膜，采用上述超薄金属膜的制备方法制备而成。所述超薄金属膜的靶金属为以三维岛状模式生长的金属，例如金、银、铜、铝或是各自的合金，优选的为金、银，由于金、银在常见衬底上有着较差的浸润性，因此形成完整连续薄膜的厚度阈值更高，采用本发明提供的超薄金属膜的制备方法进行制备更具有优势。
所述超薄金属膜的厚度小于等于15纳米，表面均方根粗糙度为0.2-0.5纳米，所述超薄金属膜对550纳米光的透光率不低于30％。
本发明还提供一种超薄金属膜的应用，所述超薄金属膜采用上述超薄金属膜的制备方法制备而成，由于所述超薄金属膜的制备方法采用物理减薄的方式制得，并未改变金属的性质，因此所述超薄金属膜仍然具有导电性，同时超薄的厚度带来了较好的透光性及柔性，可以应用于光电器件中的透明电极，例如有机发光二极管、有机太阳能电池、交流电电致发光器件及透明显示器件等。
实施例1
本实施例提供一种超薄银膜的制备方法，包括如下步骤：
准备好表面清洁的硅衬底，使用原子层沉积设备在硅衬底表面沉积2纳米厚的二氧化钛作为缓冲层；
然后使用聚酰亚胺胶带将表面已沉积2纳米二氧化钛的硅衬底固定于离子束溅射沉积设备腔体中的工作台表面；
对离子束溅射沉积设备腔体抽真空，真空度抽至5×10-4Pa；
通过与离子源相连的进气管路向离子束溅射沉积设备腔体中通入高纯氩气(纯度为99.99％)，控制进气的压力和流量，使腔体真空度稳定在2.6×10-2Pa；
开启离子源，离子源能量500eV、束流50mA、中和63mA，氩离子束以45°夹角轰击银靶材表面，靶材银原子逸出靶材表面扩散到腔体真空中，部分银原子到达并吸附于硅衬底表面，成核，生长，逐渐成膜；控制离子源开启工作的时间，直至银薄膜的厚度为20纳米；
然后将上一步制得的银薄膜样品转移至离子束斜角刻蚀设备中，使用聚酰亚胺胶带将样品固定于离子束斜角刻蚀设备的工作台表面；
对离子束斜角刻蚀设备腔体抽真空，真空度抽至5×10-4Pa；
通过离子源进气管路向设备腔体中通入高纯氩气(纯度为99.99％)，控制进气的压力和流量，使设备腔体真空度稳定在2.6×10-2Pa；
开启离子源，离子源能量200eV、束流40mA、中和48mA，氩离子束以45°夹角轰击银薄膜表面，随着离子束的轰击，银薄膜的厚度逐渐减薄；控制离子源的工作时间，最后得到4纳米厚度的超薄银薄膜。
实施例2
本实施例提供一种超薄金膜的制备方法，包括如下步骤：
准备好表面清洁的氧化硅衬底，使用原子层沉积设备在氧化硅衬底表面沉积3纳米厚的氧化锌作为缓冲层；
然后使用聚酰亚胺胶带将表面已沉积3纳米氧化锌的氧化硅衬底固定于双离子束溅射沉积设备腔体中的工作台表面；
对双离子束溅射沉积设备腔体抽真空，真空度抽至5×10-4Pa；
通过离子源相连的进气管路向设备腔体中通入高纯氩气(纯度为99.99％)，控制进气的压力和流量，使设备腔体真空度稳定在2.6×10-2Pa。
开启溅射离子源(主源)，离子源能量500eV、束流50mA、中和63mA，氩离子束以45°夹角轰击金靶材表面，靶材金原子逸出靶材表面扩散到腔体真空中，部分金原子到达并吸附于硅衬底表面，成核，生长，逐渐成膜；控制溅射离子源开启工作的时间，直至沉积金薄膜的厚度为20纳米；
关闭溅射离子源(主源)，开启刻蚀离子源(辅源)，离子源能量200eV、束流40mA、中和48mA，氩离子束以45°夹角轰击金薄膜表面，随着离子束的轰击，金薄膜的厚度逐渐减薄；控制离子源的工作时间，从而控制减薄的厚度，减薄16纳米最后得到4纳米厚度的超薄金薄膜。
与相关技术相比，本发明提供的一种超薄金属膜的制备方法，通过先沉积后刻蚀的方式，可以制备厚度低于厚度阈值的超薄金属膜，将其应用于光电器件中的透明电极，可以在保证导电性的同时，获得良好的透光性及柔性。
以上对本发明的实施方式作出详细说明，但本发明不局限于所描述的实施方式。对本领域的技术人员而言，在不脱离本发明的原理和精神的情况下对这些实施例进行的多种变化、修改、替换和变型均仍落入在本发明的保护范围之内。

Claims (10)

1.一种超薄金属膜的制备方法，其特征在于，包括如下步骤：
S1：提供靶金属及衬底，在所述衬底的表面沉积对所述靶金属具有浸润性的缓冲层，其中所述靶金属为以三维岛状模式生长的金属；
S2：获取所述靶金属在所述衬底上刚好形成完整连续薄膜的厚度阈值，使用薄膜沉积方法在所述衬底表面沉积一层厚度大于或等于厚度阈值的靶金属膜；
S3：在高真空状态下，采用离子束斜角刻蚀方法将惰性气体离子束以一定角度刻蚀所述靶金属膜表面，使所述靶金属膜表面的金属原子逸出，反向减薄至厚度小于厚度阈值，完成超薄金属膜的制备。
2.根据权利要求1所述的超薄金属膜的制备方法，其特征在于，所述靶金属为金、银、铜、铝或是各自的合金；所述衬底采用硅、氧化硅、石英、玻璃、聚对苯二甲酸乙二酯、聚萘二甲酸乙二醇酯或聚酰亚胺材料制成；所述缓冲层的材料为二氧化钛、氧化锌或硫化锌。
3.根据权利要求1所述的超薄金属膜的制备方法，其特征在于，所述步骤S2中靶金属的沉积厚度D1与厚度阈值D0的关系为：0纳米≤D1－D0≤20纳米。
4.根据权利要求1所述的超薄金属膜的制备方法，其特征在于，所述惰性气体离子束的中轴线与所述衬底表面的夹角小于或等于45°，所述惰性气体离子束的轰击面积大于所述衬底表面的面积。
5.根据权利要求1所述的超薄金属膜的制备方法，其特征在于，所述惰性气体离子束中的惰性气体选择为氩气、氦气、氖气、氪气或氙气。
6.根据权利要求1所述的超薄金属膜的制备方法，其特征在于，在所述惰性气体离子束刻蚀过程中，所述衬底沿其中轴线均匀旋转，驱动所述靶金属膜均匀旋转。
7.根据权利要求1所述的超薄金属膜的制备方法，其特征在于，所述步骤S2中“薄膜沉积方法”选自离子束溅射沉积、热蒸发沉积、电子束蒸发沉积或磁控溅射沉积中的一种。
8.根据权利要求7所述的超薄金属膜的制备方法，其特征在于，所述步骤S2中“薄膜沉积方法”为离子束溅射沉积，其与步骤S3中的“离子束斜角刻蚀方法”共用一台离子束溅射设备。
9.一种超薄金属膜，其特征在于，采用权利要求1-8任一项所述的制备方法制备而成，所述超薄金属膜的厚度小于等于15纳米，表面均方根粗糙度为0.2-0.5纳米，所述超薄金属膜对550纳米光的透光率不低于30％。
10.一种超薄金属膜的应用，其特征在于，所述超薄金属膜采用权利要求1-8任一项所述的制备方法制备而成，所述超薄金属膜应用于光电器件中的透明电极。
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