CN111020515A - 非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置及方法 - Google Patents
非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置及方法 Download PDFInfo
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Abstract
本发明涉及一种镀膜装置及方法,具体涉及一种非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置及方法。本发明的技术方案如下:非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,在离子镀膜的镀膜腔室中,镀膜靶源对向基片台,镀膜腔室中设有辅助靶源和遮挡板,所述遮挡板设置在镀膜靶源与辅助靶源之间,所述遮挡板将辅助靶源的工作区域与镀膜靶源及基片台的工作区域予以隔离。本发明能够实现在非超高真空环境条件下低氧含量易氧化薄膜的制备,一方面镀膜工艺中的本底真空度条件较为宽松,另一方面制成薄膜含氧量显著降低,特别适合在大型工业化镀膜生产线上应用。
Description
技术领域
本发明涉及一种真空镀膜装置及方法,具体涉及一种非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置及方法。
背景技术
磁控溅射或多弧离子镀等离子镀膜技术在大规模集成电路及电子元器件、磁性材料及磁记录介质、平板显示器、光学及光导通讯、能源科学、机械及塑料等产业领域都有着广泛的使用。但是部分材料如金属Al、单质Si和ZrB2等在镀膜过程由于镀膜环境残余气体中O2-离子和OH-离子的存在,特别容易发生制成薄膜的微量氧化,严重情况下会显著影响制成薄膜的使用性能,为此这类易氧化薄膜需要在超高真空环境下制备。而超高真空条件在大面积、大批量镀膜工程实践中存在成本过高或较难实现的问题,制约了相关工艺技术与产品的工程化应用。
发明内容
本发明提供一种非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置及方法,能够实现在非超高真空环境条件下低氧含量易氧化薄膜的制备,一方面镀膜工艺中的本底真空度条件较为宽松,另一方面制成薄膜含氧量显著降低,特别适合在大型工业化镀膜生产线上应用。
本发明的技术方案如下:
非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,在离子镀膜的镀膜腔室中,镀膜靶源对向基片台,镀膜腔室中设有辅助靶源和遮挡板,所述遮挡板设置在镀膜靶源与辅助靶源之间,所述遮挡板将辅助靶源的工作区域与镀膜靶源及基片台的工作区域予以隔离。
所述的非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,其优选方案为,所述辅助靶源的靶材为钛、铝或锆。
所述的非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,其优选方案为,所述辅助靶源的数量为一个或多个。
所述的非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,其优选方案为,所述镀膜靶源的靶材为金属、非金属或化合物。
非超高真空环境离子镀膜制备低氧含量易氧化薄膜的方法,利用上述装置,包含以下步骤:
(1)样品准备:将待镀样品依次用丙酮、无水乙醇及去离子水超声波清洗10分钟,氮气吹干待用;
(2)开启镀膜腔室舱门,将待镀样品放置于基片台中心,合闭镀膜腔室舱门;
(3)启动抽真空机组,将镀膜腔室抽真空至气压5×10-3Pa;
(4)开启并调节质量流量计,使高纯氩气持续流入镀膜腔室并使镀膜腔室气压维持在0.8Pa;
(5)开启辅助靶源驱动电源,功率为100-500W,使辅助靶源辉光放电,在遮挡板后溅射出原子或粒子;
(6)辅助靶源工作10分钟后,开启镀膜靶源驱动电源,功率为100-500W,开始在待镀样品表面镀制镀膜,镀膜时长依沉积速率和镀膜厚度要求确定;
(7)镀膜时间达到确定值后,依次关闭镀膜靶源驱动电源和辅助靶源驱动电源,然后再关闭质量流量计;
(8)待待镀样品和其上沉积的镀膜温度降至室温后,关闭抽真空机组,镀膜腔室放气,开启镀膜腔室舱门,将带镀膜的待镀样品取出,镀膜过程完成。
本发明的有益效果为:
1、在启动镀膜靶源沉积镀膜前和沉积镀膜过程中,启动辅助靶源并使其连续工作,利用辅助靶源溅射出的原子或粒子的亲氧活性吸收镀膜腔室内部的残余气体如氧、碳、和水蒸气等,能够达到降低沉积镀膜中的杂质含量特别是氧含量的目的。
2、用遮挡板将辅助靶源的溅射区域与镀膜靶源的工作区域隔开,能够使辅助靶源上溅射出的原子或粒子不能混入镀膜靶源的薄膜中影响其成份及性能。
3、本发明提供的非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,能够实现在非超高真空环境条件下低氧含量易氧化薄膜的制备,一方面镀膜工艺中的本底真空度条件较为宽松,另一方面制成薄膜含氧量显著降低,特别适合在大型工业化镀膜生产线上应用。
附图说明
图1为实施例1中非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置(一套辅助靶源)结构示意图;
图2为实施例2中非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置(两套辅助靶源)结构示意图;
图3为实施例1中磁控溅射镀ZrB2膜过程辅助钛靶开启与否对制成ZrB2薄膜成份的X射线光电子能谱对比图。
具体实施方式
实施例1
在单晶Si基片上采用磁控溅射镀膜技术沉积低氧含量ZrB2薄膜
如图1所示,非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,在离子镀膜的镀膜腔室1中,镀膜靶源2对向基片台3,镀膜腔室1中设有辅助靶源4和遮挡板5,所述遮挡板5设置在镀膜靶源2与辅助靶源4之间,所述遮挡板5将辅助靶源4的工作区域与镀膜靶源2及基片台3的工作区域予以隔离。
镀膜靶源2上安装直径76毫米厚度6毫米ZrB2化合物靶材,镀膜靶源驱动电源7为1000W直流溅射电源,辅助靶源4上安装直径76毫米厚度6毫米Ti靶材,辅助靶源驱动电源8为1000W直流溅射电源,待镀样品6选用单晶Si基片。
在单晶Si基片上采用磁控溅射镀膜技术沉积200nm厚低氧含量ZrB2薄膜,具体步骤如下:
(1)样品准备:将待镀单晶Si基片依次用丙酮、无水乙醇及去离子水超声波清洗10分钟,氮气吹干待用;
(2)开启镀膜腔室1舱门,将单晶Si基片放置于基片台3中心,合闭镀膜腔室1舱门;
(3)启动抽真空机组9,通过压力检测仪11进行检测,将镀膜腔室1抽真空至气压5×10-3Pa;
(4)开启并调节质量流量计10,使高纯氩气持续流入镀膜腔室1并使镀膜腔室1气压维持在0.8Pa;
(5)开启辅助靶源驱动电源8,功率为100W,使Ti靶辉光放电,在遮挡板5后溅射出Ti原子或粒子;
(6)Ti靶工作10分钟后,开启镀膜靶源驱动电源7,功率为200W,开始在单晶Si基片表面镀制ZrB2膜,镀膜时长为15分钟;
(7)镀膜时间达到15分钟时,依次关闭镀膜靶源驱动电源7和镀膜靶源驱动电源8,然后再关闭质量流量计10;
(8)待单晶Si基片和其上沉积的ZrB2薄膜温度降至室温后,关闭抽真空机组9,镀膜腔室1放气,开启镀膜腔室1舱门,将镀膜后的单晶Si基片取出,镀膜过程完成。
将制成的ZrB2薄膜样品采用X射线光电子能谱仪进行薄膜化学成份测试,测试结果如图3所示,开启辅助Ti靶制成的ZrB2薄膜样品中O的含量仅为2.93at.%,制成的ZrB2薄膜样品XPS能谱图上几乎看不见O峰的存在;而与之对比的是,不开启辅助Ti靶,制成的ZrB2薄膜样品XPS能谱图上检测出很强的O峰,经计算薄膜中O的含量高达26.4at.%。
实施例2
在无氧铜基片上采用多弧离子镀技术沉积低氧含量Ti膜
如图2所示,本实施例中辅助靶源4为两套。镀膜靶源2上安装直径80毫米厚度30毫米纯度99.99%Ti靶材,镀膜靶源驱动电源7为200A直流弧源;两个辅助靶源4上安装直径76毫米厚度6毫米Al靶材,辅助靶源驱动电源8均为1000W直流溅射电源,待镀样品6选用3mm厚无氧铜基片。
在无氧铜基片上采用多弧离子镀膜技术沉积10μm厚低氧含量Ti薄膜,具体步骤如下:
(1)样品准备:将待镀无氧铜基片依次用丙酮、无水乙醇及去离子水超声波清洗10分钟,氮气吹干待用;
(2)开启镀膜腔室1舱门,将无氧铜基片放置于基片台3中心,合闭镀膜腔室1舱门;
(3)启动抽真空机组9,将镀膜腔室1抽真空至气压5×10-3Pa;
(4)开启并调节质量流量计10,使高纯氩气持续流入镀膜腔室1并使镀膜腔室1气压维持在0.8Pa;
(5)开启辅助靶源驱动电源8,功率均为200W,使两个Al靶均辉光放电,在遮挡板5后溅射出Al原子或粒子;
(6)Al靶工作10分钟后,开启镀膜靶源驱动电源7,电流为60A,开始在无氧铜基片表面镀制Ti膜,镀膜时长为12分钟;
(7)镀膜时间达到12分钟时,依次关闭镀膜靶源驱动电源7和辅助靶源驱动电源8,然后再关闭质量流量计10;
(8)待无氧铜基片和其上沉积的Ti薄膜温度降至室温后,关闭抽真空机组9,镀膜腔室1放气,开启镀膜腔室1舱门,将镀膜后的无氧铜基片取出,镀膜过程完成。
将制成的Ti薄膜样品采用俄歇电子能谱仪进行薄膜表层与深层化学成份测试,测试结果表明Ti膜中的含氧量低于1at.%,远低于无辅助Al靶时制成Ti膜中的含氧量5-8at.%。
Claims (5)
1.非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,在离子镀膜的镀膜腔室中,镀膜靶源对向基片台,其特征在于,镀膜腔室中设有辅助靶源和遮挡板,所述遮挡板设置在镀膜靶源与辅助靶源之间,所述遮挡板将辅助靶源的工作区域与镀膜靶源及基片台的工作区域予以隔离。
2.根据权利要求1所述的非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,其特征在于,所述辅助靶源的靶材为钛、铝或锆。
3.根据权利要求1所述的非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,其特征在于,所述辅助靶源的数量为一个或多个。
4.根据权利要求1所述的非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,其特征在于,所述镀膜靶源的靶材为金属、非金属或化合物。
5.非超高真空环境离子镀膜制备低氧含量易氧化薄膜的方法,其特征在于,利用如权利要求1-4之一所述的非超高真空环境离子镀膜制备低氧含量易氧化薄膜的装置,具体包括如下步骤:
(1)样品准备:将待镀样品依次用丙酮、无水乙醇及去离子水超声波清洗10分钟,氮气吹干待用;
(2)开启镀膜腔室舱门,将待镀样品放置于基片台中心,合闭镀膜腔室舱门;
(3)启动抽真空机组,将镀膜腔室抽真空至气压5×10-3Pa;
(4)开启并调节质量流量计,使高纯氩气持续流入镀膜腔室并使镀膜腔室气压维持在0.8Pa;
(5)开启辅助靶源驱动电源,功率为100-500W,使辅助靶源辉光放电,在遮挡板后溅射出原子或粒子;
(6)辅助靶源工作10分钟后,开启镀膜靶源驱动电源,功率为100-500W,开始在待镀样品表面镀制镀膜,镀膜时长依沉积速率和镀膜厚度要求确定;
(7)镀膜时间达到确定值后,依次关闭镀膜靶源驱动电源和辅助靶源驱动电源,然后再关闭质量流量计;
(8)待待镀样品和其上沉积的镀膜温度降至室温后,关闭抽真空机组,镀膜腔室放气,开启镀膜腔室舱门,将带镀膜的待镀样品取出,镀膜过程完成。
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JP2003313662A (ja) * | 2002-04-25 | 2003-11-06 | Mutsuo Yamashita | スパッタリング装置 |
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JP2012238637A (ja) * | 2011-05-10 | 2012-12-06 | Panasonic Corp | スパッタリング方法およびスパッタリング装置 |
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