CN106129171B - 一种大面积非层状结构NiSe纳米薄膜的制备方法 - Google Patents
一种大面积非层状结构NiSe纳米薄膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种大面积非层状结构NiSe纳米薄膜的制备方法，其包括NiSe纳米薄膜的制备、NiSe纳米薄膜的转移、NiSe纳米薄膜光探测器的构筑等步骤。本发明通过固相反应法生长得到的非层状结构的NiSe纳米薄膜质量好，晶粒尺寸大，晶界数量少；基于本发明高质量的NiSe纳米薄膜制备的光电探测器，获得的光电流比NiSe纳米晶薄膜提高了4个数量级；本发明制备工艺简单，成本低廉，具有较好的实用价值，而且这种方法可以被用来制备其他与传统平面工艺兼容的非层状结构材料纳米薄膜。
Description
技术领域
本发明属于半导体薄膜材料领域，涉及一种通过固相反应法制备大面积非层状结构NiSe纳米薄膜的方法。
背景技术
由于具有独特的结构和性能，石墨烯和其他二维材料包括六方相氮化硼和过渡金属硫化物等，引起了广泛的关注。尤其通过化学气相沉积等方法可以在特定基底上制备出高质量、大面积的二维薄膜，这显著加快了二维材料的应用发展。受层状结构二维材料的启发，可以预见非层状结构材料的纳米薄膜与传统平面工艺相兼容，相比于他维度，更有利于其应用。而且，与纳米晶构成的薄膜相比，所制备出的具有大尺寸晶粒的非层状结构纳米薄膜拥有更优越的性能，这是因为晶界会引起电子的散射。层状结构材料在层内有较强的横向化学键，而在层之间有较弱的范德华力，这在形核和生长过程中，使得原子更容易生长成二维薄膜。而非层状结构的材料是在三个方向上都具有很强的原子键，从而使其缺乏内在各向异性生长驱动力，造成非层状结构纳米薄膜的生长很难实现。非层状结构材料的二维超薄纳米片和非层状结构纳米薄膜已经分别通过湿化学模板法和剥离的方法制备出来，但是尺寸分别仅限制在几百纳米和几微米之内。大面积非层状结构材料的纳米薄膜可以通过分子束外延法在单晶基底外延生长得到，但是成本较高。
发明内容
本发明的目的在于提供一种大面积非层状结构NiSe纳米薄膜的制备方法。本发明提供的这种大面积非层状结构NiSe纳米薄膜的生长方法工艺简单，成本低廉，具有较强的实用价值，而且可以被用来制备与传统平面工艺兼容的其他非层状结构材料纳米薄膜。
为实现上述目的，本发明采用如下的技术方案：
一种大面积非层状结构NiSe纳米薄膜的制备方法，包括以下步骤：
(1) NiSe纳米薄膜的制备：选择厚度为50 μm、纯度为99.99%的Ni箔在通有10sccm H2 和20 sccm Ar 的低压气氛中，450-550 ℃退火25-35 min，去除Ni箔表面的氧化物；退火完之后，利用电子束蒸发的方法在Ni箔表面沉积ZnSe薄膜，在整个沉积过程中，真空度保持在1×10-4-3×10-4 Pa；随后将ZnSe/Ni箔在1.5×10-4-2.5×10-4 Pa的真空度下650-750 ℃退火25-35 min，得到NiSe纳米膜；
(2) NiSe纳米薄膜的转移：在50 μm厚的Ni箔表面得到的NiSe纳米薄膜上旋涂浓度为80-120 mg/ml PMMA，旋涂条件为：先在400-600 r/min的转速下匀胶甩胶5-7 s，然后在1500-2500 r/min的转速下匀胶30-50 s；旋涂完之后放置于加热台上70-90 ℃烘烤4-6min；然后将PMMA/NiSe/Ni箔放入2.0 mol/L FeCl3的溶液中刻蚀Ni箔；在Ni箔刻蚀完之后，将PMMA/NiSe膜放置于去离子水中清洗其表面残留的FeCl3刻蚀液；接着，将SiO2/Si基底捞起PMMA支撑的NiSe纳米薄膜；待完全风干后，将PMMA/NiSe/SiO2/Si放置于通有10 sccm H2和20 sccm Ar 的低压气氛中，350-450 ℃退火1-3 h除去PMMA，即得到了转移至SiO2/Si基底上的NiSe纳米薄膜；
(3) NiSe纳米薄膜光探测器的构筑：在NiSe纳米薄膜转移至SiO2/Si基底上后，利用光刻的方法构造出长度为5 μm，宽度为10 μm的沟道；通过高真空热蒸发系统沉积10/35nm Cr/Au来制作电极。
本发明的有益效果：
（1）本发明通过固相反应法生长得到的非层状结构的NiSe纳米薄膜质量好，晶粒尺寸大，晶界数量少。
（2）基于本发明高质量的NiSe纳米薄膜制备的光电探测器，获得的光电流比NiSe纳米晶薄膜提高了4个数量级。
(3) 本发明制备工艺简单，成本低廉，具有较好的实用价值，而且这种方法可以被用来制备其他与传统平面工艺兼容的非层状结构材料纳米薄膜。
具体实施方式
一种大面积非层状结构NiSe纳米薄膜的制备方法，包括以下步骤：
(1) NiSe纳米薄膜的制备：选择厚度为50 μm、纯度为99.99%的Ni箔在通有10sccm H2 和20 sccm Ar 的低压气氛中，500 ℃退火30 min，去除Ni箔表面的氧化物；退火完之后，利用电子束蒸发的方法在Ni箔表面沉积ZnSe薄膜，在整个沉积过程中，真空度保持在2×10-4 Pa；随后将ZnSe/Ni箔在2×10-4 Pa的真空度下700 ℃退火30 min，得到NiSe纳米膜；
(2) NiSe纳米薄膜的转移：在50 μm厚的Ni箔表面得到的NiSe纳米薄膜上旋涂浓度为100 mg/ml PMMA，旋涂条件为：先在500 r/min的转速下匀胶甩胶6 s，然后在2000 r/min的转速下匀胶40 s；旋涂完之后放置于加热台上80 ℃烘烤5 min；然后将PMMA/NiSe/Ni箔放入2.0 mol/L FeCl3的溶液中刻蚀Ni箔；在Ni箔刻蚀完之后，将PMMA/NiSe膜放置于去离子水中清洗其表面残留的FeCl3刻蚀液；接着，将SiO2/Si基底捞起PMMA支撑的NiSe纳米薄膜；待完全风干后，将PMMA/NiSe/SiO2/Si放置于通有10 sccm H2 和20 sccm Ar 的低压气氛中，400 ℃退火2 h除去PMMA，即得到了转移至SiO2/Si基底上的NiSe纳米薄膜；
(3) NiSe纳米薄膜光探测器的构筑：在NiSe纳米薄膜转移至SiO2/Si基底上后，利用光刻的方法构造出长度为5 μm，宽度为10 μm的沟道；通过高真空热蒸发系统沉积10/35nm Cr/Au来制作电极。
气相法已经广泛应用于晶体生长中，通过气相法实现晶体的生长需要一定过饱和度。在经历一个气固转变过程之后，原子或者分子开始形核和生长。在这个非平衡动态过程中，在对应于薄膜生长的过饱和度下，气体源的供应速率远远大于晶体生长的速率，因此由动态过程决定的产物形貌一般呈现出孤立岛状结构而不是连续的纳米薄膜，这是由非层状结构产生的三维生长行为所导致的。基于对单晶非层状结构纳米薄膜的分子束外延生长的考虑，对气体源供应与晶体生长二者之间的相对速率的控制是非层状结构纳米薄膜生长的一个关键要素。以Ni箔上的NiSe为例，我们通过固相反应法的引入发明了一种界面限域外延生长非层状结构纳米薄膜的方法。在特定的温度下，通过Zn原子和Ni原子的相互扩散形成NiSe之后，NiSe在ZnSe-Ni界面处成核。在这个没有气固转变的热力学平衡过程中，NiSe生长速率被认为由扩散和反应速率所决定。这使得在弛豫时间内，NiSe与Ni基底形成共格界面((102)NiSe/(111)Ni 和 (110)NiSe/(200)Ni)，即实现了NiSe在Ni箔表面的外延生长，从而产生较低能量的NiSe-Ni界面。与此同时，Zn原子和Ni原子沿ZnSe-NiSe界面扩散，NiSe反应物随后在NiSe-Ni台阶或者在NiSe成核点的上表面外延生长。从而，NiSe晶粒通过ZnSe源的消耗以及NiSe-ZnSe界面在横向和纵向向前推进的方式进一步长大。当位于NiSe成核点上方的ZnSe薄膜先于横向的ZnSe薄膜消耗完之后，NiSe晶粒的生长只能通过NiSe-ZnSe界面的横向推进得到延续，并最终通过晶粒的相互拼接形成连续的NiSe纳米薄膜。
本发明通过固相反应法生长得到的非层状结构的NiSe纳米薄膜质量好，晶粒尺寸大，晶界数量少；基于本发明高质量的NiSe纳米薄膜制备的光电探测器，获得的光电流比NiSe纳米晶薄膜提高了4个数量级；本发明制备工艺简单，成本低廉，具有较好的实用价值，而且这种方法可以被用来制备其他与传统平面工艺兼容的非层状结构材料纳米薄膜。
Claims (1)
1.一种大面积非层状结构NiSe纳米薄膜的制备方法，其特征在于，包括以下步骤：
(1) NiSe纳米薄膜的制备：选择厚度为50 μm、纯度为99.99%的Ni箔在通有10 sccm H2和20 sccm Ar 的低压气氛中，450-550 ℃退火25-35 min，去除Ni箔表面的氧化物；退火完之后，利用电子束蒸发的方法在Ni箔表面沉积ZnSe薄膜，在整个沉积过程中，真空度保持在1×10-4-3×10-4 Pa；随后将ZnSe/Ni箔在1.5×10-4-2.5×10-4 Pa的真空度下650-750 ℃退火25-35 min，得到NiSe纳米薄膜；
(2) NiSe纳米薄膜的转移：在所述的50 μm厚的Ni箔表面上得到的所述的NiSe纳米薄膜上旋涂浓度为80-120 mg/ml PMMA，旋涂条件为：先在400-600 r/min的转速下匀胶甩胶5-7 s，然后在1500-2500 r/min的转速下匀胶30-50 s；旋涂完之后放置于加热台上70-90℃烘烤4-6 min；然后将PMMA/NiSe/Ni箔放入2.0 mol/L FeCl3的溶液中刻蚀Ni箔；在Ni箔刻蚀完之后，将PMMA/NiSe膜放置于去离子水中清洗其表面残留的FeCl3刻蚀液；接着，将SiO2/Si基底捞起PMMA支撑的NiSe纳米薄膜；待完全风干后，将PMMA/NiSe/SiO2/Si放置于通有10 sccm H2 和20 sccm Ar 的低压气氛中，350-450 ℃退火1-3 h除去PMMA，即得到了转移至SiO2/Si基底上的NiSe纳米薄膜；
(3) NiSe纳米薄膜光探测器的构筑：在NiSe纳米薄膜转移至SiO2/Si基底上后，利用光刻的方法构造出长度为5 μm，宽度为10 μm的沟道；通过高真空热蒸发系统沉积10/35 nmCr/Au来制作电极。
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