CN109708944B - 一种硅的损伤层透射电镜原位纳米压痕方法 - Google Patents
一种硅的损伤层透射电镜原位纳米压痕方法 Download PDFInfo
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Abstract
本发明公开了一种硅的损伤层透射电镜原位纳米压痕方法，属于透射电镜原位纳米力学测试领域。采用湿法刻蚀与离子束刻蚀方法制备出楔形硅样品；利用聚焦离子束对刻蚀出的楔形硅进行减薄和修整，减薄采用离子束束流为30kV：50‑80nA，修整采用离子束束流为5kV：1‑6pA，使楔形硅顶部宽度为80‑100nm。用导电银胶将样品固定在透射电镜原位纳米力学系统的样品座上，在透射电镜中用压针对样品进行压痕，使样品损伤层厚度为2‑200nm；在透射电镜中对样品的损伤层进行原位纳米压痕实验。本发明实现了硅的损伤层透射电镜原位纳米压痕实验，并且能够进行原子尺度表征。
Description
技术领域
本发明属于透射电镜原位纳米力学测试技术领域，涉及纳米压痕方法，特别涉及一种硅的损伤层透射电镜原位纳米压痕方法以及硅片磨粒加工机理研究方法。
背景技术
硅由于储量丰富、具有优异的光电性能，广泛应用于半导体、微电子和光电子产业。传统的机械加工往往会导致硅片表面产生一层较厚的损伤层，而表面损伤层会严重影响器件的性能。超精密磨削方法具有磨削效率高，面型精度好等综合优点，广泛应用于硅片的超精密加工领域，主要用金刚石砂轮对硅片进行超精密磨削，但磨削后硅片的表面损伤层厚度一般大于160nm。因此，通常需要化学机械抛光去除超精密磨削过程中产生的表面损伤层，但化学机械抛光是超精密加工过程中时间和成本最高的一种方法，超精密磨削过程中产生的表面损伤层越薄，化学机械抛光用时越短，成本越低，因此，减小超精密磨削过程中产生的表面损伤层厚度对半导体、微电子、光电子等领域具有重要的现实意义。
减小超精密磨削过程中产生的表面损伤层厚度，就需要知道超精密磨削加工机理，超精密磨削是利用金刚石磨粒不断去除损伤层的过程，在损伤层被去除的同时又不断产生新的损伤层。但是，由于研究技术条件的限制，超精密磨削过程中损伤层的产生过程并不清楚。近年来随着透射电镜原位纳米力学测试技术的发展，研究人员对纳米尺度的晶体硅进行原位压缩实验，用于探索晶体硅到非晶硅的转变过程，但该实验方法中样品只受到单轴压缩应力，且样品为没有损伤层的晶体硅，实验条件与超精密磨削过程相差较大，因此实验结果与超精密磨削结果不同。压痕实验中，样品受力复杂，除了受到轴向压缩应力，还受到剪切应力，与超精密磨削过程中样品受力类似。因此，开发一种硅的损伤层透射电镜原位纳米压痕实验方法，对研究硅片超精密磨削机理是十分重要的。
发明内容
一种硅的损伤层透射电镜原位纳米压痕方法，采用湿法刻蚀与离子束刻蚀方法制备出楔形硅样品，在透射电镜中用金刚石压针压制出硅的损伤层，损伤层厚度为2-200nm，对硅的损伤层进行原位纳米压痕实验，实现了硅的损伤层透射电镜原位纳米压痕实验，并且能够进行原子尺度表征。
本发明的技术方案：
采用湿法刻蚀与离子束刻蚀方法制备出楔形硅样品，楔形硅顶部宽度为80-100nm，压痕实验的压针为cube-corner金刚石压针，压针曲率半径为50-70nm；利用聚焦离子束对刻蚀出的楔形硅进行减薄和修整，减薄采用离子束束流为30kV：50-80nA，修整采用离子束束流为5kV：1-6pA，使楔形硅顶部宽度为80-100nm。用导电银胶将样品固定在透射电镜原位纳米力学系统的样品座上，在透射电镜中用压针对样品进行压痕，使样品损伤层厚度为2-200nm；在透射电镜中对样品的损伤层进行原位纳米压痕实验。本发明实现了硅的损伤层透射电镜原位纳米压痕实验，并且能够进行原子尺度表征。
样品为单晶硅片，金刚石压针为cube-corner压针，压针曲率半径为50-70nm。单晶硅具有优异的光电性能，广泛应用于半导体、微电子和光电子产业，对单晶硅进行超精密磨削的工具往往是金刚石砂轮，选择曲率半径为50-70nm的cube-corner金刚石压针，在进行压痕实验过程中样品可以受到较大的应力，同时样品受力复杂，更接近实际的超精密磨削过程。
利用金刚石笔将硅片切成长度为3-5mm，宽度为2-3mm的块体。为了能使样品固定在透射电镜原位纳米力学测试样品杆上，利用金刚石笔将硅片切成长度为3-5mm，宽度为2-3mm的块体，样品过大会触碰透射电镜极靴，样品过小会增加样品制备的难度。
将硅片表面甩一层厚度为100-300nm的电子束光刻胶，利用电子束刻蚀出宽度为400-800nm，长度为10-60μm的矩形图案。电子束光刻技术是目前已知分辨率最高的光刻技术，并且电子射线波长小，衍射效应可以忽略，所以选择用电子束刻蚀，由于电子束刻蚀速率较慢，所以电子束光刻胶厚度选择100-300nm。
将样品表面镀一层厚度为1-3μm的SiO2保护层。保护层选用SiO2，是因为SiO2膜对碱液具有良好的抗刻蚀性能，在FH溶液中，SiO2的刻蚀速率比Si的刻蚀速率高，所以SiO2膜最终很容易去掉。
将整个样品浸泡在丙酮中超声清洗10-30分钟。丙酮可以有效溶解光刻胶，将整个样品浸泡在丙酮中超声清洗10-30分钟，用于去除样品表面的光刻胶以及光刻胶上面的SiO2保护层，只留下矩形图案的保护层。
用去离子水对样品进行清洗，并用压缩气体将样品吹干，将整个样品浸泡在NaOH溶液中进行刻蚀，刻蚀时间为15-30分钟。NaOH溶液可以刻蚀Si而保护SiO2膜下面的Si不被刻蚀。
用去离子水对样品进行清洗，并用压缩气体将样品吹干，将整个样品浸泡在HF溶液中进行刻蚀，刻蚀时间5-10分钟。HF溶液对SiO2的刻蚀速率较快，将整个样品浸泡在HF溶液中刻蚀5-10分钟，将SiO2膜除去。
用去离子水对样品进行清洗，并用压缩气体将样品吹干，利用聚焦离子束对刻蚀出的楔形硅进行减薄和修整，减薄采用离子束束流为30kV：50-80nA，修整采用离子束束流为5kV：1-6pA，使楔形硅顶部宽度为80-100nm。要对样品进行原子尺度的观察，样品厚度要小于100nm，所以要对刻蚀之后的楔形硅样品进行减薄，由于压针曲率半径为50-70nm，所以楔形硅顶部宽度最终为80-100nm，由于较大的离子束束流会对样品造成损伤，所以减薄时离子束束流选择30kV：50-120pA，并用5kV：10-30pA束流进行修整，用于去除损伤层。
用导电银胶将样品固定在透射电镜原位纳米力学系统的样品座上。在透射电镜中，导电性越好，成像越清晰，并且越稳定，所以利用导电银胶将样品固定在样品座上。
将样品座利用螺钉固定在样品杆上，用金刚石压针在透射电镜中对样品进行压痕，使样品损伤层厚度为2-200nm。在透射电镜中对样品进行压痕，可以精准控制损伤层厚度，从而可以对不同厚度的损伤层进行原位纳米压痕实验。
在透射电镜中对样品的损伤层进行原位纳米压痕实验，从而实现对损伤层的应力诱导损伤起源和演变的实时观测。透射电镜原位纳米力学测试可以实现原子及纳米尺度的加载变形，是研究磨粒加工导致的损伤层的纳米尺寸材料去除机理和损伤起源及演变的有效方法。
本发明的效果和益处是采用湿法刻蚀与离子束刻蚀方法制备出楔形硅样品，实现了硅的损伤层透射电镜原位纳米压痕实验，并且能够进行原子尺度表征。
附图说明
图1a是无损伤层的楔形硅样品的透射电镜低倍形貌图，图1b为图1a方框部分的透射电镜高分辨图。
图2a是损伤层厚度为67nm的楔形硅样品的透射电镜低倍形貌图，图2b为图2a方框部分的透射电镜高分辨图。
图3a是对楔形硅样品损伤层进行透射电镜原位纳米压痕之后的透射电镜低倍形貌图，图3b为图3a方框部分的透射电镜高分辨图。
具体实施方式
以下结合附图和技术方案，进一步说明本发明的具体实施方式。
实施例
利用金刚石笔将硅片切成长度为4mm，宽度为3mm的块体，将硅片表面甩一层厚度为200nm的电子束光刻胶，利用电子束刻蚀出宽度为600nm，长度为30μm的矩形图案；将样品表面镀一层厚度为1.5μm的SiO2保护层，将整个样品浸泡在丙酮中超声清洗20分钟，用于去除电子束光刻胶以及光刻胶上面的SiO2保护层，只留下矩形图案的SiO2保护层；用去离子水对样品进行清洗，并用压缩气体将样品吹干，将整个样品浸泡在NaOH溶液中进行刻蚀，刻蚀时间为25分钟；用去离子水对样品进行清洗，并用压缩气体将样品吹干，将整个样品浸泡在HF溶液中进行刻蚀，刻蚀时间为8分钟，用于去除SiO2保护层；用去离子水对样品进行清洗，并用压缩气体将样品吹干，利用聚焦离子束对刻蚀出的楔形硅进行减薄和修整，减薄采用的离子束束流为30kV：50pA，修整采用的离子束束流为5kV：20pA，使楔形硅顶部宽度为80nm；利用导电银胶将样品固定在透射电镜原位纳米力学系统样品杆的样品座上，将样品座利用螺钉固定在样品杆上，制备好的楔形硅样品的透射电镜图如图1a所示，图1b为图1a方框部分的透射电镜高分辨图，可看出样品为无晶格缺陷的晶体硅；用曲率半径为66nm的cube-corner金刚石压针在透射电镜中对样品进行压痕，使样品损伤层厚度为67nm，如图2a所示，图2b为图2a方框部分的透射电镜高分辨图；在透射电镜中对样品的损伤层进行原位压痕实验，图3a是对楔形硅样品损伤层进行透射电镜原位纳米压痕之后的透射电镜低倍形貌图，图3b为图3a方框部分的透射电镜高分辨图。
Claims (1)
1.一种硅的损伤层透射电镜原位纳米压痕方法，采用湿法刻蚀与离子束刻蚀方法制备出楔形硅样品，在透射电镜中用金刚石压针压制出硅的损伤层，对硅的损伤层进行原位纳米压痕实验，其特征在于：
(1)样品为单晶硅片，金刚石压针为cube-corner压针，压针曲率半径为50-70nm；
(2)利用金刚石笔将单晶硅片切成长度为3-5mm，宽度为2-3mm的块体；
(3)将单晶硅片表面甩一层厚度为100-300nm的电子束光刻胶，利用电子束刻蚀出宽度为400-800nm，长度为10-60μm的矩形图案；
(4)将样品表面镀一层厚度为1-3μm的SiO2保护层；
(5)将整个样品浸泡在丙酮中超声清洗10-30分钟；
(6)用去离子水对样品进行清洗，并用压缩气体将样品吹干，将整个样品浸泡在NaOH溶液中进行刻蚀，刻蚀时间为15-30分钟，形成楔形硅；
(7)用去离子水对楔形硅进行清洗，并用压缩气体将楔形硅吹干，楔形硅浸泡在HF溶液中进行刻蚀，刻蚀时间5-10分钟，以去除SiO2保护层；
(8)用去离子水对样品进行清洗，并用压缩气体将样品吹干，利用聚焦离子束对刻蚀出的楔形硅进行减薄和修整，减薄采用离子束束流为30kV：50-80nA，修整采用离子束束流为5kV：1-6pA，使楔形硅顶部的宽度为80-100nm；
(9)用导电银胶将样品固定在透射电镜原位纳米力学系统的样品座上；
(10)将样品座利用螺钉固定在样品杆上，用金刚石压针在透射电镜中对样品进行压痕，使样品损伤层厚度为2-200nm；
(11)在透射电镜中对样品的损伤层进行原位纳米压痕实验，从而实现对损伤层的应力诱导损伤起源和演变的实时观测。
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