CN110079765A - 制备多晶陶瓷膜的方法 - Google Patents

制备多晶陶瓷膜的方法 Download PDF

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CN110079765A
CN110079765A CN201910159284.1A CN201910159284A CN110079765A CN 110079765 A CN110079765 A CN 110079765A CN 201910159284 A CN201910159284 A CN 201910159284A CN 110079765 A CN110079765 A CN 110079765A
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M.施雷特
W.维尔兴
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Baioman Western Europe Co.,Ltd.
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Abstract

本发明涉及制备多晶陶瓷膜的方法。具体地，本发明涉及在基材（10）的表面（12）上制备多晶陶瓷膜的方法，其中在表面（12）上导入粒子流并且通过所述粒子在表面（12）上的沉积而形成所述陶瓷膜，其中借助隔板沿着优选方向在表面（12）上导入所述粒子流直到达到第一预定层厚度，该优选方向与表面（12）的平面法线形成了预定的入射角。根据本发明，在达到预定的层厚度之后，将所述隔板从粒子流中移除，并且在表面（12）上导入另外的粒子直到达到第二预定层厚度。

Description

制备多晶陶瓷膜的方法
本专利申请是申请日为2013年6月18日、申请号为201380034791.3、同题的专利申请的分案申请。
技术领域
本发明涉及在基材的表面上制备多晶陶瓷膜的方法。
背景技术
在生物传感器领域，越来越多地使用薄膜体声波谐振器（FBAR）；当特定连接到检测物质时，它能在其表面上获取其共振频率的变化。其中，它是指在相应基材（例如硅晶片）上施加的压电晶体层。
因为生物分子的检测通常在液体中进行，所以需要特别高的共振品质和敏感度。为此必须在声学剪切模式中激发谐振器。
为了实现这样的激发，需要使极性晶轴相对于激发场倾斜（Verkippung）。在经典的谐振器结构（其中压电体包裹在两个电极层之间）的情况下，所述极性轴必须具有电极平面中的组分。
当使用ZnO作为介电体时，在倾斜大约40°和大约90°的情况下激发纯粹的剪切波（N.F. Foster等人, Cadmium Sulfide and Zinc Oxide Thin-Film Transducers, IEEETransactions on sonics and ultrasonics, Vol. SU-15, No.1, 1968年1月）。相对小的倾斜（例如15°）也足够获得起作用的剪切模式谐振器。
为了达到极性轴的这种倾斜，DE 10 2005 014 160 A1描述了一种方法，其中通过反应性溅射沉积压电体。在此借助隔板（Blende）调节粒子的优选入射方向，该入射方向与基材表面的平面法线形成了所需的角度，从而在基材表面上沉积陶瓷。
已知方法的缺点在于，材料流的主要部分沉积在隔板上而不是沉积在基材上。这导致低的沉积速率，并且使得所述装置在不多次的沉积过程之后就需要清洁和重新调整。这样会消耗很多时间和费用。使用隔板系统还会导致低的沉积结果的可重复性，特别是在层均匀性方面。
发明内容
因此，本发明的目的在于提供根据权利要求1的前序部分的方法，该方法可以快速地、低成本地和很好可重复性地制造具有倾斜的极性轴的陶瓷膜。
该目的通过具有权利要求1的特征的方法而实现。
对于在基材的表面上制备多晶陶瓷膜的这种方法，在表面上导入粒子的粒子流并且通过所述粒子在表面上的沉积而形成所述陶瓷膜。在此，借助隔板沿着优选方向在表面上导入所述粒子流直到达到第一预定层厚度，该优选方向与表面的平面法线形成了预定的入射角。
根据本发明，在达到预定的层厚度之后，将所述隔板从粒子流中移除，并且在表面上导入另外的粒子直到达到第二预定层厚度。
换言之，所述隔板只是用于产生陶瓷材料的晶种层，即具有所述第一预定层厚度的层，其具有所需的轴取向。在形成该晶种层之后，可以不用借助隔板继续进行沉积，因为晶种层的晶体在不定向的材料施加时也会沿着已经预定的优选取向继续生长。
这样可以在产生晶种层之后实现明显更高的沉积速率。此外，在产生晶种层之后不使用隔板可以在基材上沉积明显更多的所使用的陶瓷材料，并且通过在隔板上捕获的材料减少了装置的污染。这提高了装置的使用寿命并且降低了维护消耗和费用。
此外已经发现，借助本发明的方法可以更有效地产生明显更均匀的层。特别是改善了层厚度均匀性，从而使制成的谐振器具有明显更好规定的共振频率，并且因此在用作生物传感器时也具有提高的敏感度。
一方面，所述在表面上导入的粒子可以是所需陶瓷本身的粒子；另一方面，可以例如通过反应性溅射沉积金属粒子，该金属粒子在表面上才与反应性气体形成所需的陶瓷。
优选地，所述预定的入射角选自0-90°的范围和特别是选自10-30°的范围。由此确保可以进行充分的剪切激发。
另外有利的是所述第一预定层厚度（即晶种层的厚度）为50-150 nm和优选100nm。由此确保在接下来不定向施加时也可以在通过晶种层预定的优选取向中进行可重复性的层生长。
总的层厚度（即所述第二预定层厚度）优选为450-600 nm和优选540 nm。在这个范围内可以形成具有所需共振频率（100 MHz至10 GHz）的谐振器。
在此优选地使用由ZnO和/或AlN或者相应的金属构成的粒子作为所述粒子。它们是低成本的材料，这些材料具有所需的压电性能并且可以通过常规的施涂方法，例如通过溅射或反应性溅射施加。
附图说明
下面借助附图进一步说明本发明及其具体实施方式。唯一的附图示意了具有多个测量点的基材晶片，这些测量点用于检测借助本发明的方法的具体实施例施加的层的质量。
具体实施方式
为了制造薄膜体声波谐振器（FBAR），在基材（例如硅晶片10）上制备由压电陶瓷（例如ZnO）构成的包裹在两个平面电极之间的层。其中层的施加通过本身已知的沉积方法进行，例如溅射。
为了实现所需的谐振器性能，特别是为了实现剪切模式的激发，必须使压电材料的极性轴与基材的平面法线形成一个角度。为此，首先产生约100 nm厚度的晶种层。在晶种层的沉积过程中，在待沉积的粒子的源和基材表面12之间安装隔板系统，该系统形成一定的入射角，从而使粒子在优选的取向（具有以所需方式倾斜的极性轴）中沉积在基材表面12上。
只要达到所需的晶种层厚度，就可以移除隔板系统并且以不定向的方式继续沉积。基于在晶种层中已经产生的轴取向，层的进一步生长同样定向进行，从而总的来说实现了极性轴所需的倾斜。继续该过程直到达到约540 nm的总层厚度。
在产生晶种层的过程中，可以达到约4 nm/min的沉积速率，在移除隔板系统之后可以将沉积速率提高到最多40 nm/min。相比于现有技术已知的在整个沉积过程中使用隔板系统的方法，由此实现了明显更快的工艺进程。
为了检测所产生的层的质量，在附图所示的6”-晶片的多个测量点14分析所述层的样品，并且与由现有技术已知的方法制造的晶片的样品比较。
如从表中获知的，使用本发明的方法的具体实施例产生明显更均匀的层。层厚度的控制（由层厚度标准化的标准偏差测量）从10.3%提高到3%，同时可以将工艺时间由132分钟缩短为34分钟。剪切耦合系数基本没有受影响。
此外，所述隔板在粒子流中明显更短的停留时间也减少了隔板的污染，并且因此需要更少的清洁和调整消耗。
本发明的具体实施例 现有技术
平均层厚度 [nm] 550 530
σ (层厚度)/层厚度 [%] 3.0 10.3
剪切耦合系数 [%] 11 12
工艺时间 [min] 34 132
隔板的停留时间比例 [%] 17 100
表：比较了根据现有技术和根据本发明的具体实施例而产生的层的基本工艺性能和层性能。
总之，本发明提供了可以快速地、低成本地和更有效地制造具有预定的轴倾斜的压电陶瓷层的方法。

Claims (9)

1.在基材（10）的表面（12）上制备多晶陶瓷膜的方法，其中在表面（12）上导入粒子流并且通过所述粒子在表面（12）上的沉积而形成所述陶瓷膜，其中借助隔板沿着优选方向在表面（12）上导入所述粒子流直到达到第一预定层厚度，该优选方向与表面（12）的平面法线形成了预定的入射角，
其特征在于，
在达到预定的层厚度之后，将所述隔板从粒子流中移除，并且在表面（12）上不定向地导入另外的粒子直到达到第二预定层厚度。
2.权利要求1的方法，其特征在于，所述预定入射角选自0-90°的范围。
3.权利要求1的方法，其特征在于，所述预定入射角选自10-30°的范围。
4.权利要求1或2的方法，其特征在于，所述第一预定层厚度为50至150 nm。
5.权利要求1或2的方法，其特征在于，所述第一预定层厚度为100 nm。
6.权利要求1或2的方法，其特征在于，所述第二预定层厚度为450至600 nm。
7.权利要求1或2的方法，其特征在于，所述第二预定层厚度为540 nm。
8.权利要求1或2的方法，其特征在于，使用由ZnO和/或AlN构成的粒子作为所述粒子。
9.权利要求1或2的方法，其特征在于，所述粒子流通过溅射提供。
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