CN111254414B - 柔性石墨烯基硅纳米线异质结的制备与转移方法 - Google Patents
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Abstract
本发明公开了一种柔性石墨烯基硅纳米线异质结的制备与转移方法，将石墨烯湿法转移至SiO2/Si上，采用金属催化VLS机制的CVD法(化学气相沉积法)，利用2nm厚Au作为催化剂，在石墨烯上直接生长Si纳米线。生长温度为500℃，源气体SiH4流量为10sccm，生长压力1.33×104Pa，生长时间10分钟。生长结束后，关闭SiH4气体阀门，在氩气保护下，CVD炉自然冷却后得到石墨烯基硅纳米线异质结。然后，将制备好的石墨烯基硅纳米线异质结，旋涂PMMA/PDMS双支撑膜，利用NaOH溶液刻蚀掉SiO2，实现石墨烯基硅纳米线异质结的整体转移，得到柔性、可移植的石墨烯基硅纳米线异质结。
Description
技术领域
本发明属于硅纳米线制备及转移技术领域，涉及一种柔性石墨烯基硅纳米线异质结的制备方法，还涉及纳米线异质结的转移方法。
背景技术
硅作为二十世纪最重要的半导体材料之一，由于其适宜的带隙结构，成熟的制造技术，高可靠性，可控性良好的表面状态和低成本的可扩展生产以及高速光电探测能力，成为了用于光电探测器的理想半导体材料。然而体硅的刚度限制了其在柔性光电探测器领域的应用。硅纳米线由于具有独特的机械柔性、优异的陷光能力，为新一代高性能柔性光电探测器的开发提供了可能。研究发现，硅纳米线的独特电子限域作用有利于电子和空穴能态保持分离，能有效延长载流子寿命，展现出了优秀的光电特性；同时，线性的几何结构，使得其对外力具有很好的弹性，在发生形变后，材料表面不会产生裂纹。这些特点都使得Si纳米线在柔性、可移植、高性能光电探测器领域具有巨大应用前景。
石墨烯在光电器件领域主要应用在两方面，一方面，石墨烯良好的电导性能和透光性能，使它在透明电极方面有非常好的应用前景。传统的太阳能电池所用的透明电极一般为氧化铟锡(ITO)或者为掺氟氧化锡(FTO)。但这些材料本身都具有很高的脆性以及对酸碱的敏感性，成本也越來越高。石墨烯在柔韧性、成本和力学强度方面的显著优势，使其作为新的透明导电材料受到了广泛关注。另一方面，石墨烯具有从紫外至远红外的宽光谱吸收特性、室温下超高的载流子迁移率，将石墨烯与半导体材料结合形成异质结光电器件，可应用于超宽谱和超快光电探测器等领域。但是，石墨烯用于光探测也存在着明显的劣势。本征石墨烯由于光吸收率低(单层石墨烯对可见光的吸收率仅为2.3％)，石墨烯探测器的光响应率较低；石墨烯自身的光生载流子寿命短，仅皮秒左右，难以有效收集，也影响了探测器的光电响应度，导致石墨烯探测器无法满足实际应用的需要。
发明内容
本发明的目的是提供一种柔性石墨烯基硅纳米线异质结的制备与转移方法，采用金属催化VLS机制的CVD法(化学气相沉积法)，以石墨烯(Gr)作为基材直接制备硅纳米线并整体转移，具有柔性、可移植的特点。
本发明所采用的技术方案是，柔性石墨烯基硅纳米线异质结的制备方法，采用湿法将石墨烯转移至SiO2/Si上，并利用CVD法制备石墨烯基硅纳米线异质结，具体包括以下步骤：
步骤1.将表面覆盖有约2nm厚Au的石墨烯基材放入CVD炉中，开启机械泵抽真空；
步骤2.待机械泵将CVD炉内气压抽真空至l0-1 Pa，打开分子泵，并将炉腔气压抽真空至l×10-4Pa；
步骤3.关闭分子泵，并打开氩气路阀门，调整气体流量约为0.1slm，调节机械泵旋钮，使CVD炉腔体压力为1.33×104Pa，打开加热系统，并以35℃/min的速率加热到500℃；
步骤4.保持500℃的时间为10min，并通入10sccm的SiH4；
步骤5.待10分钟生长结束后，关闭SiH4气体阀门；在氩气保护下，CVD炉自然冷却到室温，得到石墨烯基硅纳米线异质结。
本发明的特点还在于：
柔性石墨烯基硅纳米线异质结的转移方法，将制备好的石墨烯基硅纳米线异质结，旋涂PMMA/PDMS双支撑膜，利用NaOH溶液刻蚀掉SiO2，实现石墨烯基硅纳米线异质结的整体转移，具体方法如下：
步骤1.将石墨烯基硅纳米线异质结放入匀胶机中，滴上PMMA溶液进行旋涂，使PMMA溶液均匀覆盖硅纳米线；
步骤2.将步骤1旋涂好的样品放在120℃的电热板上20min，进行固化PMMA；
步骤3.配置PDMS溶液，并将PDMS溶液均匀滴涂在样品表面，然后将样品放入95℃的烘箱中40min，进行固化PDMS；
步骤4.切除多余的PDMS，然后放入1mol/L的NaOH溶液中，以刻蚀衬底中的SiO2。
步骤5.采用去离子水将刻蚀后的样品清洗干净，并将覆盖有PDMS/PMMA的石墨烯基硅纳米线异质结从SiO2/Si衬底上剥离。
步骤6.石墨烯基硅纳米线异质结转移到柔性衬底上，完成转移过程。
步骤1中匀胶机的转速为800r/min，保持6s，并以2000r/min旋涂30s，重复一次匀胶旋涂过程。
步骤3中，PDMS溶液采用聚二甲基硅氧烷(PDMS)和固化剂(Sylgard184，DowCorning)按10：1的比例混合制得。
步骤5中，刻蚀的NaOH溶液为90℃，水浴加热下反应40min。
本发明的有益效果是：
本发明采用金属催化VLS机制的CVD法，以石墨烯作为基材直接制备硅纳米线，辅以转移方法，在柔性石墨烯衬底上制备可移植的石墨烯基异质结三维结构，结合硅纳米线对可见-近红外光的高敏感度和石墨烯高柔韧性、高载流子迁移率、高热导率等优良材料性能，得到可见-近红外高响应度的柔性石墨烯基硅纳米线异质结。石墨烯一方面作为三维结构移植至其他柔性塑料衬底前的柔性基材，与硅纳米线形成异质结；另一方面，石墨烯也是器件电极的优选材料，可以提高器件的光响应度和响应速度；另外，鉴于其超高热导率，石墨烯甚至可以作为散热窗口使用。硅纳米线则作为可见-近红外光的主要吸收材料，弥补石墨烯材料光吸收率低的缺憾，提高器件的性能。
附图说明
图1是本发明石墨烯/硅纳米线异质结转移过程意图；
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明柔性石墨烯基硅纳米线异质结的制备方法，采用湿法将石墨烯转移至SiO2/Si上，并利用CVD法制备石墨烯基硅纳米线异质结，具体包括以下步骤：
步骤1.将表面覆盖有约2nm厚Au的石墨烯基材放入CVD炉中，开启机械泵，将管式炉内抽真空；
步骤2.待机械泵将CVD管式炉内气压抽真空至l0-1 Pa，打开分子泵，并将炉腔气压抽真空至l×10-4Pa；
步骤3.关闭分子泵，并打开氩气路阀门，调整气体流量约为0.1slm，调节机械泵旋钮，使CVD炉腔体压力为1.33×104Pa；打开加热系统，并以35℃/min的速率加热到500℃；
步骤4.保持500℃的时间为10min，并通入10sccm的SiH4；
步骤5.待10分钟生长结束后，关闭SiH4气体阀门，在氩气保护下，CVD炉自然冷却后得到石墨烯基硅纳米线异质结。
如图1所示，柔性石墨烯基硅纳米线异质结的转移方法，将制备好的石墨烯基硅纳米线异质结，旋涂PMMA/PDMS双支撑膜，利用NaOH溶液刻蚀掉SiO2，实现石墨烯基硅纳米线异质结的整体转移，具体方法如下：
步骤1.将石墨烯基硅纳米线异质结放入匀胶机中，滴上PMMA溶液进行旋涂，使PMMA溶液均匀覆盖硅纳米线；
步骤2.将步骤1旋涂好的样品放在120℃的电热板上20min，进行固化PMMA；
步骤3.配置PDMS溶液，并将PDMS溶液均匀滴涂在样品表面，然后将样品放入95℃的烘箱中40min，进行固化PDMS；
步骤4.切除多余的PDMS，然后放入1mol/L的NaOH溶液中，以刻蚀衬底中的SiO2。
步骤5.采用去离子水将刻蚀后的样品清洗干净，并将覆盖有PDMS/PMMA的石墨烯基硅纳米线异质结从SiO2/Si衬底上剥离。
步骤6.石墨烯基硅纳米线异质结转移到柔性衬底上，完成转移过程。
步骤1中匀胶机的转速为800r/min，保持6s，并以2000r/min旋涂30s，重复一次匀胶旋涂过程。
步骤3中，PDMS溶液采用聚二甲基硅氧烷(PDMS)和固化剂(Sylgard184，DowCorning)按10：1的比例混合制得。
步骤5中，刻蚀的NaOH溶液为90℃，水浴加热下反应40min。
本发明的有益效果是：
本发明采用金属催化VLS机制的CVD法，以石墨烯作为基材直接制备硅纳米线，辅以转移方法，在柔性石墨烯衬底上制备可移植的石墨烯基异质结三维结构，结合硅纳米线对可见-近红外光的高敏感度和石墨烯高柔韧性、高载流子迁移率、高热导率等优良材料性能，得到可见-近红外高响应度的柔性石墨烯基硅纳米线异质结。石墨烯一方面作为三维结构移植至其他柔性塑料衬底前的柔性基材，与硅纳米线形成异质结；另一方面，石墨烯也是器件电极的优选材料，可以提高器件的光响应度和响应速度；另外，鉴于其超高热导率，石墨烯甚至可以作为散热窗口使用。硅纳米线则作为可见-近红外光的主要吸收材料，弥补石墨烯材料光吸收率低的缺憾，提高器件的性能。
Claims (4)
1.柔性石墨烯基硅纳米线异质结的制备与转移方法，其特征在于，采用湿法将石墨烯转移至SiO2/Si上，并利用CVD法制备石墨烯基硅纳米线异质结，将制备好的石墨烯基硅纳米线异质结，旋涂PMMA/PDMS双支撑膜，利用NaOH溶液刻蚀掉SiO2，实现石墨烯基硅纳米线异质结的整体转移，具体包括以下步骤：
步骤1.将表面覆盖有2nm厚Au的石墨烯基材放入CVD炉中，开启机械泵抽真空；
步骤2.待机械泵将CVD炉内气压抽真空至l0-1Pa，打开分子泵，并将炉腔气压抽真空至l×10-4Pa；
步骤3.关闭分子泵，并打开氩气路阀门，调整气体流量为0.1slm，调节机械泵旋钮，使CVD炉腔体压力为1.33×104Pa，打开加热系统，并以35℃/min的速率加热到500℃；
步骤4.保持500℃的时间为10 min，并通入10 sccm的SiH4；
步骤5.待10分钟生长结束后，关闭SiH4气体阀门；在氩气保护下，CVD炉自然冷却到室温，得到石墨烯基硅纳米线异质结；
步骤6.将石墨烯基硅纳米线异质结放入匀胶机中，滴上PMMA溶液进行旋涂，使PMMA溶液均匀覆盖硅纳米线；
步骤7.将旋涂好的样品放在120℃的电热板上20min，进行固化PMMA；
步骤8.配置PDMS溶液，并将PDMS溶液均匀滴涂在样品表面，然后将样品放入95℃的烘箱中40min，进行固化PDMS；
步骤9.切除多余的PDMS，然后放入1mol/L的NaOH溶液中，以刻蚀衬底中的SiO2；
步骤10.采用去离子水将刻蚀后的样品清洗干净，并将覆盖有PDMS/PMMA的石墨烯基硅纳米线异质结从SiO2/Si衬底上剥离；
步骤11.石墨烯基硅纳米线异质结转移到柔性衬底上，完成转移过程。
2.根据权利要求1所述的柔性石墨烯基硅纳米线异质结的制备与转移方法，其特征在于，步骤6中，匀胶机的转速为800r/min，保持6s，并以2000r/min旋涂30s，重复一次匀胶旋涂过程。
3.根据权利要求1所述的柔性石墨烯基硅纳米线异质结的制备与转移方法，其特征在于，步骤8中，PDMS溶液采用聚二甲基硅氧烷（PDMS）和固化剂按10：1的比例混合制得。
4.根据权利要求1所述的柔性石墨烯基硅纳米线异质结的制备与转移方法，其特征在于，步骤9中，刻蚀的NaOH溶液为90℃，水浴加热下反应40min。
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