CN113178517B - 一种耐高温的声表面波传感器叉指电极及其制备方法 - Google Patents

一种耐高温的声表面波传感器叉指电极及其制备方法 Download PDF

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CN113178517B
CN113178517B CN202110321508.1A CN202110321508A CN113178517B CN 113178517 B CN113178517 B CN 113178517B CN 202110321508 A CN202110321508 A CN 202110321508A CN 113178517 B CN113178517 B CN 113178517B
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轩伟鹏
章弥灵
陈金凯
董树荣
金浩
骆季奎
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Hangzhou Dianzi University
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Abstract

本发明公开了一种耐高温的声表面波传感器叉指电极及其制备方法。现有金属材料叉指电极在高温下容易发生团聚、结块。本发明叉指电极包括衬底、氧化物界面层、复合电极层和氧化物保护层；氧化物界面层置于衬底上，氧化物保护层和多个复合电极层均置于氧化物界面层上，相邻复合电极层之间设有间隙；氧化物保护层包裹各复合电极层；复合电极层的材料为掺杂氧化物的金属。本发明通过在衬底和电极之间加入一层氧化物界面层，有效阻止了高温下衬底中原子扩散至电极中；本发明采用金属和氧化物渐变变化的复合电极，能有效阻碍高温下电极的团聚与凸起，增加了器件的高温耐热性，可用于1200℃以上的高温环境，延长了器件在高温环境下的工作时间。

Description

一种耐高温的声表面波传感器叉指电极及其制备方法
技术领域
本发明属于声表面波器件技术领域，具体涉及一种耐高温的声表面波传感器叉指电极及其制备方法。
背景技术
随着时代的发展与科技的进步，人们对声表面波传感器在各种各样恶劣环境中的使用提出了越来越高的需求。其中，高温这个恶劣条件最常见并且也最需要去克服，比如在航空航天、汽车以及能源化工领域中声表面波传感器往往需要被应用在极端高温条件下，再如涡轮发动机、发电厂燃气燃烧器、市政固体废物发电厂水冷壁以及其他工作环境高于500℃需要传感器稳定运行的工业场所。因此对高温条件下声表面波传感器的制备与研究就显得尤为重要。
声表面波传感器的主要结构由压电材料基片与叉指电极两部分组成。传统的声表面波传感器往往会在高温环境中出现性能衰退乃至完全失效的情况，因此，高温环境下的声表面波传感器性能衰减乃至失效也需要从压电材料与叉指电极这两个方面来讨论。对压电材料而言，最核心的性质就是它的压电性能。一般的压电材料都存在一个特有的相转变温度，当环境温度高于这个相转变温度时，其压电性能被破坏，导致所制备的声表面波器件失效。常见的石英、钽酸锂等压电材料在超过600℃时，将失去压电性能。四硼酸锂压电材料所制备的声表面波传感器在917℃以下都不会因衬底压电性能而失效，但其熔点限制了它在高于1000℃环境中的应用。在对可耐高温的压电材料的需求下，硅酸镓镧(La3Ga5SiO14，LGS)新型压电材料自从被第一次报道后，就一直受到人们的广泛关注。现如今，硅酸镓镧压电材料已经发展成了声表面波高温应用领域的主导材料。LGS的熔点为1470℃，在室温至熔点温度区间内都不会发生相变，表明LGS压电单晶材料能够在极高的温度下保持稳定的压电性能。因此，可耐高温的叉指电极成为了制备高温声表波传感器主要攻克的难题。
通过前人的研究发现，较高的叉指电极电阻会对声表面波器件的性能有一定的影响，比如引起热能损耗、非均匀电压以及产生激励信号的不均匀分布等现象。所以研究者们都选用金属材料来制备叉指电极。但金属材料长时间工作在高温环境下，容易发生团聚、结块等现象，从而导致金属电极断裂，导电性丧失，器件失效。为了使金属电极在高温下能稳定工作，必须探索出有效的方法使得金属在高温下的团聚、结块现象得到抑制。
发明内容
本发明的目的是提供一种耐高温的声表面波传感器叉指电极及其制备方法，解决目前技术存在的难题，使叉指电极在较高的温度下依旧保持导电稳定性。
本发明的技术方案为：
本发明一种耐高温的声表面波传感器叉指电极，包括衬底、氧化物界面层、复合电极层和氧化物保护层；所述的氧化物界面层置于衬底上，氧化物保护层和多个复合电极层均置于氧化物界面层上，相邻复合电极层之间设有间隙；所述的氧化物保护层包裹各复合电极层；所述复合电极层的材料为掺杂氧化物的金属。
优选地，所述衬底的材料为硅酸镓镧、钇铁氧体、LiNbO3或AlN。
优选地，所述衬底的厚度为50μm～1000μm，表面粗糙度RMS在1nm以下。
优选地，所述氧化物界面层的材料为Al2O3、ZrO2、SiO2、Y2O3或HfO2。
优选地，所述复合电极层中的金属材料为Pt、Rh、Ir或其任意配比的合金。
优选地，所述复合电极层中的氧化物材料为Al2O3、ZrO2、SiO2、Y2O3或HfO2，所述氧化物保护层的材料为Al2O3、ZrO2、SiO2、Y2O3或HfO2。
优选地，所述复合电极层中的氧化物掺杂浓度为非线性渐变，最低为0.01％，最高为10％。
更优选地，所述复合电极层中的氧化物掺杂浓度由下至上呈正弦曲线变化，形成高氧化物浓度层和低氧化物浓度层依次交替的排布规律，且高氧化物浓度层的氧化物浓度最大位置出现在高氧化物浓度层的中间位置；其中，正弦曲线取0.5N个周期，N取值为1～20。
该耐高温的声表面波传感器叉指电极的制备方法，包括如下步骤：
步骤一、衬底的清洗与烘干处理。
步骤二、采用原子层沉积技术在经步骤一处理后的衬底上沉积一层厚度为5～100nm的氧化物界面层。
步骤三、将步骤二处理得到的沉积氧化物界面层后的衬底通过光刻工艺处理，在氧化物界面层上得到复合电极层图案。
步骤四、将经步骤三光刻处理后的样片采用磁控溅射技术进行金属靶材与氧化物靶材的共溅射，在氧化物界面层上得到复合电极全覆盖层；其中，金属靶材的功率固定不变，氧化物靶材的功率随时间周期变化。
步骤五、将经步骤四处理后的样片泡在丙酮溶液中，超声清洗，使得复合电极全覆盖层上除复合电极层图案以外的多余电极脱离。
步骤六、采用射频磁控溅射技术在经步骤五处理后的样片上制备一层厚度为50～150nm的氧化物保护层。
优选地，步骤四中，金属靶材为Pt靶材，氧化物靶材为Al2O3靶材。Pt靶材的直径为75mm，纯度为99.999％；Al203靶材的直径为75mm，纯度为99.999％。Pt靶材的功率为300W；AL203靶材的功率变化规律为从500W逐渐下降至300W，再逐渐上升至500W，经过三个周期。
本发明具有如下有益效果：
本发明通过在衬底和电极之间加入一层氧化物界面层，有效阻止了高温下衬底中Si、Ga、La等原子扩散至电极中。且本发明采用金属和氧化物渐变变化的复合电极，在金属电极中掺杂氧化物有利于阻碍金属电极在高温下的自扩散，能有效阻碍高温下电极的团聚与凸起，有效改善电极在高温下的退化现象，增加了器件的高温耐热性，可用于1200℃以上的高温环境，延长了器件在高温环境下的工作时间，使声表面波器件可以应用在一些军工、航空航天等高温复杂环境中。另外，本发明制备工艺简单、可靠。
附图说明
图1是本发明耐高温的声表面波传感器叉指电极的结构剖面图。
图2是本发明中复合电极层的结构示意图。
图3是本发明制备的叉指电极在1200℃保持1h后的扫描电子显微镜(SEM)照片。
具体实施方式
下面结合附图及实施例对本发明做进一步说明。
如图1所示，一种耐高温的声表面波传感器叉指电极，包括衬底1、氧化物界面层2、复合电极层3和氧化物保护层4；氧化物界面层2置于衬底1上，氧化物保护层4和多个复合电极层3均置于氧化物界面层2上，相邻复合电极层3之间设有间隙；氧化物保护层4包裹各复合电极层3；复合电极层3的材料为掺杂氧化物的金属。
作为一个优选实施例，衬底的材料包括但不限于硅酸镓镧、钇铁氧体、LiNbO3、AlN。
作为一个优选实施例，硅酸镓镧包括但不限于Ca3TaGa3Si2O14(CTGS)、La3Ga5.5Ta0.5O14(LGT)、La3Ga5.5Nb5.5O14(LGN)。
作为一个优选实施例，衬底的厚度为50μm～1000μm，表面粗糙度RMS在1nm以下。
作为一个优选实施例，氧化物界面层的材料包括但不限于Al2O3、ZrO2、SiO2、Y2O3、HfO2。
作为一个优选实施例，氧化物界面层的厚度为5～100nm。
作为一个优选实施例，复合电极层3中的金属材料包括但不限于Pt、Rh、Ir。
作为一个优选实施例，复合电极层3中的氧化物材料包括但不限于Al2O3、ZrO2、SiO2、Y2O3、HfO2。
作为一个优选实施例，复合电极层3的厚度为100～300nm。
作为一个优选实施例，复合电极层3中的氧化物掺杂浓度为非线性渐变，最低为0.01％，最高为10％。
作为一个更优选实施例，复合电极层3中的氧化物掺杂浓度由下至上呈正弦曲线变化，形成高氧化物浓度层5和低氧化物浓度层6依次交替的排布规律，且高氧化物浓度层5的氧化物浓度最大位置出现在高氧化物浓度层5的中间位置，如图2所示；其中，正弦曲线取0.5N个周期，N取值为1～20。
作为一个优选实施例，氧化物保护层4的材料包括但不限于Al2O3、ZrO2、SiO2、Y2O3、HfO2。
作为一个优选实施例，氧化物保护层4的厚度为50～150nm。
该耐高温的声表面波传感器叉指电极的制备方法，包括如下步骤：
步骤一、选取切向为(0，138.5，117)的衬底，依次用丙酮、酒精和去离子水超声清洗5min，再用氮气吹干。
步骤二、将经步骤一处理后的衬底放入原子层沉积系统(型号为美国KurtJ.Lesker公司的ALD150LX)中，抽真空，沉积20nm的氧化物界面层。
步骤三、将步骤二处理得到的沉积氧化物界面层后的衬底依次经过涂胶、烘烤、对准、曝光、显影的光刻工艺处理，在氧化物界面层上得到复合电极层图案。
步骤四、将经步骤三光刻处理后的样片固定在磁控溅射系统(型号为美国DENTON公司的DISCOVERY635)的基片台上，然后将基片台放入真空室中，进行金属靶材与氧化物靶材的共溅射，在氧化物界面层上得到复合电极全覆盖层；其中，金属靶材的功率固定不变，氧化物靶材的功率随时间周期变化。
步骤五、将经步骤四处理后的样片泡在丙酮溶液中，超声10分钟，因为丙酮与光刻胶互溶，复合电极全覆盖层上除复合电极层图案以外的多余电极会脱离，从而得到复合电极层。
步骤六、将经步骤五处理后的样片放入磁控溅射系统的基片台上，然后将基片台放入真空室中，溅射50nm的氧化物保护层。
作为一个优选实施例，步骤四中，金属靶材为Pt靶材，氧化物靶材为Al2O3靶材。Pt靶材的直径为75mm，纯度为99.999％；AL203靶材的直径为75mm，纯度为99.999％。Pt靶材的功率为300W；AL203靶材的功率变化规律为从500W逐渐下降至300W，再逐渐上升至500W，经过三个周期。步骤四得到的复合电极全覆盖层为Pt与Al2O3复合的波浪式渐变电极层。
作为一个更优选实施例，步骤四中，复合电极全覆盖层的厚度为200nm。
如图3所示，本发明制备方法制备的叉指电极在1200℃保持1h后的扫描电子显微镜照片中，灰白色的为复合电极层3，可以看出复合电极层3有轻微的起泡现象，但复合电极层3整体依旧保持连续性。因此，本发明制备方法制备的叉指电极在高温下能有效阻碍电极的团聚与凸起，有效改善电极在高温下的退化现象，增加了器件的高温耐热性，延长了器件在高温环境下的工作时间，使声表面波器件可以应用在一些军工、航空航天等高温复杂环境中。

Claims (8)

1.一种耐高温的声表面波传感器叉指电极，包括衬底和氧化物保护层，其特征在于：还包括氧化物界面层和复合电极层；所述的氧化物界面层置于衬底上，氧化物保护层和多个复合电极层均置于氧化物界面层上，相邻复合电极层之间设有间隙；所述的氧化物保护层包裹各复合电极层；所述复合电极层的材料为掺杂氧化物的金属；
所述复合电极层中的氧化物掺杂浓度为非线性渐变，最低为0.01%，最高为10%；
所述复合电极层中的氧化物掺杂浓度由下至上呈正弦曲线变化，形成高氧化物浓度层和低氧化物浓度层依次交替的排布规律，且高氧化物浓度层的氧化物浓度最大位置出现在高氧化物浓度层的中间位置；其中，正弦曲线取0.5N个周期，N取值为1～20。
2.根据权利要求1所述一种耐高温的声表面波传感器叉指电极，其特征在于：所述衬底的材料为硅酸镓镧、钇铁氧体、LiNbO3或AlN。
3.根据权利要求1所述一种耐高温的声表面波传感器叉指电极，其特征在于：所述衬底的厚度为50μm～1000μm，表面粗糙度RMS在1nm以下。
4.根据权利要求1所述一种耐高温的声表面波传感器叉指电极，其特征在于：所述氧化物界面层的材料为Al2O3、ZrO2、SiO2、Y2O3或HfO2。
5.根据权利要求1所述一种耐高温的声表面波传感器叉指电极，其特征在于：所述复合电极层中的金属材料为Pt、Rh、Ir或其任意配比的合金。
6.根据权利要求1所述一种耐高温的声表面波传感器叉指电极，其特征在于：所述复合电极层中的氧化物材料为Al2O3、ZrO2、SiO2、Y2O3或HfO2，所述氧化物保护层的材料为Al2O3、ZrO2、SiO2、Y2O3或HfO2。
7.根据权利要求1至6中任一项所述一种耐高温的声表面波传感器叉指电极的制备方法，其特征在于：该方法包括如下步骤：
步骤一、衬底的清洗与烘干处理；
步骤二、采用原子层沉积技术在经步骤一处理后的衬底上沉积一层厚度为5～100nm的氧化物界面层；
步骤三、将步骤二处理得到的沉积氧化物界面层后的衬底通过光刻工艺处理，在氧化物界面层上得到复合电极层图案；
步骤四、将经步骤三光刻处理后的样片采用磁控溅射技术进行金属靶材与氧化物靶材的共溅射，在氧化物界面层上得到复合电极全覆盖层；其中，金属靶材的功率固定不变，氧化物靶材的功率随时间周期变化；
步骤五、将经步骤四处理后的样片泡在丙酮溶液中，超声清洗，使得复合电极全覆盖层上除复合电极层图案以外的多余电极脱离；
步骤六、采用射频磁控溅射技术在经步骤五处理后的样片上制备一层厚度为50～150nm的氧化物保护层。
8.根据权利要求7所述一种耐高温的声表面波传感器叉指电极的制备方法，其特征在于：步骤四中，金属靶材为Pt靶材，氧化物靶材为Al2O3靶材；Pt靶材的直径为75mm，纯度为99.999％；AL203靶材的直径为75mm，纯度为99.999％；Pt靶材的功率为300W；AL203靶材的功率变化规律为从500W逐渐下降至300W，再逐渐上升至500W，经过三个周期。
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