CN106435723A - 外延生长碳化硅‑石墨烯薄膜的制备方法 - Google Patents
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Abstract
本发明涉及功能材料技术领域,具体涉及一种外延生长碳化硅‑石墨烯薄膜的制备方法。外延生长碳化硅‑石墨烯薄膜的制备方法,包括如下步骤:(1)碳化硅‑石墨烯制备;(2)碳化硅‑石墨烯薄膜外延生长。本发明实现碳化硅‑石墨烯的连续生长,从而省去了目前常用在碳化硅上生长石墨烯所需的氢气刻蚀及重新制造富硅集的步骤,减少氢气刻蚀带来的晶格缺陷和表面硅富集严重削减现象。并且石墨烯具有较少的缺陷,层数在4层左右且均匀分布,具有较好的晶体质量。
Description
技术领域
本发明涉及功能材料技术领域,具体涉及一种外延生长碳化硅-石墨烯薄膜的制备方法。
背景技术
石墨烯是一种由单层碳原子紧密堆积成二维蜂窝状结构的碳材料,因具有独特的晶体和电子能带结构而拥有非常优异的力学、热学、光学、电学及化学性能,
如超高的载流子迁移率、超大的比表面积、完美的量子隧道效应、半整数量子霍尔效应等。2004年英国曼切斯特大学A.K.Geim 和K.S.Novoselov 首次发现石墨烯后,石墨烯迅速成为当前材料、物理、化学、半导体、微电子、生物、新能源等研究领域的国际前沿与热点。碳化硅具有层状结构,其基本构成单元为硅原子和碳原子组成的硅碳双原子层。在制作碳化硅晶圆过程中,由于切刀不能做到完全的精细,导致不能完全沿层与层之间Si—C 结合键较弱的方向解理,而是与解理面有个夹角,以致于进行解理操作后,碳化硅沿某一方向上呈台阶状。也正因为如此,在其台阶上生长高品质的石墨烯才成为可能。
制备石墨烯有很多种方法,如机械剥离法、液相或气相解离法、氧化还原法、裁剪纳米管法、化学气相沉积法、单晶金属外延法和SiC 外延生长法等。SiC外延生长法是在一定的真空下,将SiC 加热到一定温度,致使硅原子蒸发,剩下的碳原子进行重构形成石墨烯。由于这样生长石墨烯的衬底SiC 是半绝缘的,生长后的样品无需进行衬底腐蚀、样品迁移等繁琐的工作,直接可以进行电学测试。这样就降低了在转移过程中引入的缺陷、掺杂等因素的影响。这也使得SiC衬底上外延生长石墨烯成为实现石墨烯在微电子领域应用的最有效途径之一。
目前SiC 外延生长石墨烯都是采用单晶SiC 衬底,而传统的单晶制备法得到的SiC 材料缺陷较多,难以控制厚度和掺杂,往往达不到制造器件的要求。并且在外延生长石墨烯之前需要对衬底进行氢气刻蚀的步骤,因为碳化硅经过化学机械抛光(CMP)工艺处理之后表面会存留很多划痕,直接用其来生长制备的石墨形貌品质都较差,而在均匀的台阶上生长得到的样品形貌及品质会好很多,氢气刻蚀就是一种公认的可以除去样品表面的划痕等缺陷的可行的方案。但是不当的氢气刻蚀反而会使SiC 衬底表面形成晶格缺陷,并且会产生硅的化合物沉积现象,过度削减SiC 表面硅富集。通常要用SiO、SiH4等气体来恢复SiC 表面平衡。而CVD 法得到的外延SiC 薄膜质量往往较高,并且能够保证较快的生长速率,非常适合于高质量SiC 薄膜的生长。
发明内容
本发明旨在提出一种外延生长碳化硅-石墨烯薄膜的制备方法。
本发明的技术方案在于:
外延生长碳化硅-石墨烯薄膜的制备方法,包括如下步骤:
(1)碳化硅-石墨烯制备
对碳化硅衬底进行清洗预处理,清洗完成后直接把SiC衬底硅面朝上,放入设备中准备外延生长,
(2)碳化硅-石墨烯薄膜外延生长
第一步,首先进行4H-SiC的同质外延生长:将腔室真空度降至8×10-4Pa 以下,持续通入7L/min 的H2,将腔室温度从室温逐步升至1600℃;在1600℃下保持10min 作为预生长阶段,然后通入9~15mL/min 的SiH4和2~6mL/min 的C3H8生长60min,此时衬底表面的划痕、缺陷被填平覆盖,形成性能优异的新SiC表面;最后将设备温度降至1000℃同时继续通Ar保护,使SiC 形成3×3SiC的稳定结构,并且朝上的面仍然为Si面;
第二步,进行在4H-SiC上的石墨烯外延生长:腔体持续通入1L/min的Ar,压力保持在133Pa,这样可以抑制SiC中Si 原子的过快升华,提过石墨烯的生成质量;先将腔体温度从1000℃上升到1100℃,稳定10min,随着温度的上升,SiC由3×3SiC 结构逐渐转变为1×1SiC结构,最终在1100℃稳定为3×3SiC 结构;随后将温度升至1200℃形成63×63R30°的过渡缓冲层结构;再将温度升至1300~1600℃并保持30~50min,表面结构逐渐从63×63R30°转变为1×1grphene 结构,最后降温至室温得到稳定的石墨烯。
所述的外延生长设备为CVD 炉。
本发明的技术效果在于:
本发明利用感应加热的高温CVD 设备,先在4H-SiC 衬底上外延生长一层2~10 μm 厚的碳化硅,然后直接再在碳化硅上原位异质外延生长石墨烯,得到了缺陷较少质量较好的石墨烯薄膜。实现碳化硅-石墨烯的连续生长,从而省去了目前常用在碳化硅上生长石墨烯所需的氢气刻蚀及重新制造富硅集的步骤,减少氢气刻蚀带来的晶格缺陷和表面硅富集严重削减现象。并且石墨烯具有较少的缺陷,层数在4层左右且均匀分布,具有较好的晶体质量。
具体实施方式
外延生长碳化硅-石墨烯薄膜的制备方法,包括如下步骤:
(1)碳化硅-石墨烯制备
对碳化硅衬底进行清洗预处理,清洗完成后直接把SiC衬底硅面朝上,放入设备中准备外延生长,
(2)碳化硅-石墨烯薄膜外延生长
第一步,首先进行4H-SiC的同质外延生长:将腔室真空度降至8×10-4Pa 以下,持续通入7L/min 的H2,将腔室温度从室温逐步升至1600℃;在1600℃下保持10min 作为预生长阶段,然后通入9~15mL/min 的SiH4和2~6mL/min 的C3H8生长60min,此时衬底表面的划痕、缺陷被填平覆盖,形成性能优异的新SiC表面;最后将设备温度降至1000℃同时继续通Ar保护,使SiC 形成3×3SiC的稳定结构,并且朝上的面仍然为Si面;
第二步,进行在4H-SiC上的石墨烯外延生长:腔体持续通入1L/min的Ar,压力保持在133Pa,这样可以抑制SiC中Si 原子的过快升华,提过石墨烯的生成质量;先将腔体温度从1000℃上升到1100℃,稳定10min,随着温度的上升,SiC由3×3SiC 结构逐渐转变为1×1SiC结构,最终在1100℃稳定为3×3SiC 结构;随后将温度升至1200℃形成63×63R30°的过渡缓冲层结构;再将温度升至1300~1600℃并保持30~50min,表面结构逐渐从63×63R30°转变为1×1grphene 结构,最后降温至室温得到稳定的石墨烯。
所述的外延生长设备为CVD 炉。
本发明实现碳化硅-石墨烯的连续生长,从而省去了目前常用在碳化硅上生长石墨烯所需的氢气刻蚀及重新制造富硅集的步骤,减少氢气刻蚀带来的晶格缺陷和表面硅富集严重削减现象。并且石墨烯具有较少的缺陷,层数在4层左右且均匀分布,具有较好的晶体质量。
Claims (2)
1.外延生长碳化硅-石墨烯薄膜的制备方法,其特征在于:包括如下步骤:
(1)碳化硅-石墨烯制备
对碳化硅衬底进行清洗预处理,清洗完成后直接把SiC衬底硅面朝上,放入设备中准备外延生长,
(2)碳化硅-石墨烯薄膜外延生长
第一步,首先进行4H-SiC的同质外延生长:将腔室真空度降至8×10-4Pa 以下,持续通入7L/min 的H2,将腔室温度从室温逐步升至1600℃;在1600℃下保持10min 作为预生长阶段,然后通入9~15mL/min 的SiH4和2~6mL/min 的C3H8生长60min,此时衬底表面的划痕、缺陷被填平覆盖,形成性能优异的新SiC表面;最后将设备温度降至1000℃同时继续通Ar保护,使SiC 形成3×3SiC的稳定结构,并且朝上的面仍然为Si面;
第二步,进行在4H-SiC上的石墨烯外延生长:腔体持续通入1L/min的Ar,压力保持在133Pa,这样可以抑制SiC中Si 原子的过快升华,提过石墨烯的生成质量;先将腔体温度从1000℃上升到1100℃,稳定10min,随着温度的上升,SiC由3×3SiC 结构逐渐转变为1×1SiC结构,最终在1100℃稳定为3×3SiC 结构;随后将温度升至1200℃形成63×63R30°的过渡缓冲层结构;再将温度升至1300~1600℃并保持30~50min,表面结构逐渐从63×63R30°转变为1×1grphene 结构,最后降温至室温得到稳定的石墨烯。
2.根据权利要求1所述的外延生长碳化硅-石墨烯薄膜的制备方法,其特征在于:所述的外延生长设备为CVD 炉。
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CN115159512B (zh) * | 2022-07-11 | 2023-10-13 | 陕西科技大学 | 一种基于碳化硅三维泡沫制备石墨烯阵列的方法及石墨烯阵列 |
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