CN109280902B - 一种氮硅双修饰石墨烯量子点固态膜的制备方法 - Google Patents
一种氮硅双修饰石墨烯量子点固态膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种氮硅双修饰石墨烯量子点固态膜的制备方法。该方法以射频等离子体增强化学气相沉积技术作为石墨烯量子点固态膜生长方法，以高纯乙烯作为石墨烯量子点生长的碳源气体，以硅烷混合气和高纯氮气分别为石墨烯量子点的生长提供硅元素修饰和氮元素修饰。相对于目前常用的石墨烯量子点制备方法，如电化学法、水热法、酸氧化法、溶液化学法以及微波超声等方法，该方法的突出优点是石墨烯量子点不是以液态和胶体态的形式存在，而是以固态膜的形式存在且制备工艺同传统半导体工艺相兼容。本发明所提出的这种氮硅双修饰石墨烯量子点固态膜的制备方法能使石墨烯量子点在太阳能电池、光电探测器以及发光二极管等半导体器件中得到很好的应用。
Description
技术领域
本发明涉及纳米薄膜材料制备技术领域，具体涉及一种氮硅双修饰石墨烯量子点固态膜制备方法。
背景技术
研究发现石墨烯量子点具有优良的电学性质、生物相容性、低毒性、耐强酸强碱、结构稳定以及较好的机械强度等特性。此外，它还拥有量子点所具有的一些独特纳米结构效应，如量子限域效应、边缘效应以及优异的宽吸收窄发射特性、光电转换能力和电子迁移率等。以上特性使石墨烯量子点具有很多优异的物理和化学性质，因此它在生物成像、疾病检测、药物运输、电子器件、太阳能光伏电池、拉曼增强、催化剂、传感器等各领域具有重要的应用价值。由此也激起了多种石墨烯量子点制备方法，如强酸氧化法、电化学法、水热法、微波超声法、剥离法、溶剂热法等。以上方法在石墨烯量子点制备过程中存在使用强酸强碱或者石墨烯量子点产量低或者石墨烯量子点结晶度差等缺点。此外，这些方法所制备的石墨烯量子点一般分散在溶液或胶体中，这种液体或胶体状石墨烯量子点在光电器件中应用时将产生封装方面的困难。因此，在不使用强酸强碱的条件下，为减少半导体器件封装技术困难，寻求一种石墨烯量子点固态薄膜制备方法不仅有利于提高石墨烯量子点在光电器件中的应用，而且有利于环保。
发明内容
本发明目的是在纳米材料制备技术领域提供一种氮硅双修饰石墨烯量子点固态膜制备方法。该方法通过控制高纯乙烯、硅烷混合气和高纯氮气的进气流量以及优化石墨烯量子点生长射频功率、温度和气压等工艺参数进行氮硅双修饰石墨烯量子点的制备。
本发明提供的一种氮硅双修饰石墨烯量子点固态膜制备方法，包括以下简单步骤：
（1）采用常规清洗方法清洗单晶硅基片。首先，采用丙酮超声清洗单晶硅片10-15分钟，之后，采用超纯水超声清洗10-15分钟；接着，使用乙醇超声清洗10-15分钟，之后，采用超纯水超声清洗10-15分钟；再次，使用稀释浓度为3%-5%的氢氟酸超声清洗3-5分钟，之后，采用超纯水超声清洗10-15分钟；最后，清洗后的单晶片用氮气吹干并备用。
（2）以高纯乙烯、硅烷混合气和高纯氮气为工作气体，采用等离子体增强化学气相沉积技术在单晶硅基片表面生长氮硅双修饰石墨烯量子点固态膜。
所述的高纯乙烯的纯度大于99.995%；所述的高纯氮气的纯度大于99.999%；所述的硅烷混合气为采用氩气稀释到体积浓度为5-10%的硅烷。
步骤（2）中，采用等离子体增强化学气相沉积技术在步骤（1）中的单晶硅基片表面生长氮硅双修饰石墨烯量子点固态膜，其工艺参数是：射频功率密度为400～750 mW/cm-2，射频频率为13.56MHz，基片温度为200～350℃，腔体压强为60～100Pa，高纯乙烯气体流量为60～100sccm，高纯氮气气体流量为10～15sccm，硅烷混合气气体流量为5～10sccm，镀膜时间为60～100分钟。
本发明的技术方案以射频等离子体增强化学气相沉积技术作为石墨烯量子点固态膜生长方法，以高纯乙烯作为石墨烯量子点生长的碳源气体，以硅烷混合气和高纯氮气分别为石墨烯量子点的生长提供硅元素修饰和氮元素修饰。相对于目前常用的石墨烯量子点制备方法，如电化学法、水热法、酸氧化法、溶液化学法以及微波超声等方法，该方法的突出优点是石墨烯量子点不是以液态和胶体态的形式存在，而是以固态膜的形式存在且制备工艺同传统半导体工艺相兼容。并且，氮硅双元素修饰还可修正石墨烯量子点的电子态密度和调整石墨烯量子点光学带隙。这种石墨烯量子点固态膜制备方法简单、快捷且能有效避免石墨烯量子点液体或胶体的泄露，从而克服液态和胶体状石墨烯量子点密封难的问题。因此，本发明所提出的这种氮硅双修饰石墨烯量子点固态膜的制备方法能使石墨烯量子点在太阳能电池、光电探测器以及发光二极管等半导体器件中得到很好的应用。
附图说明
图1为实施例1样品氮硅双修饰石墨烯量子点固态膜HRTEM图。
具体实施方式
为进一步阐述本发明所提供的一种氮硅双修饰石墨烯量子点固态膜制备方法，以下实施案例用以说明本发明，但不用于限制本发明。
实施例1：
一种氮硅双修饰石墨烯量子点固态膜制备方法，该方法包括以下步骤：
（1）采用常规清洗方法清洗单晶硅基片；
（2）以高纯乙烯（纯度大于99.995%）、高纯氮气（纯度大于99.999%）和被氩气稀释浓度为5%的硅烷混合气为工作气体，采用等离子体增强化学气相沉积技术在步骤（1）中的单晶硅基片表面沉积一层氮硅双修饰石墨烯量子点固态膜，其工艺参数是：射频功率密度为400W/cm2，基片温度为200℃，射频频率为13.56MHz，腔体压强为60Pa，高纯乙烯气体流量为60sccm，高纯氮气气体流量为10sccm，硅烷混合气体流量为5sccm，镀膜时间为60分钟。
通过以上步骤一种氮硅双修饰石墨烯量子点固态膜便制备完成。图1为实施例1样品氮硅双修饰石墨烯量子点HRTEM图，其中图中的圈代表固态膜中所形成的石墨烯量子点。
实施例2：
一种氮硅双修饰石墨烯量子点固态膜制备方法，该方法包括以下步骤：
（1）采用常规清洗方法清洗单晶硅基片；
（2）以高纯乙烯（纯度大于99.995%）、高纯氮气（纯度大于99.999%）和被氩气稀释浓度为5%的硅烷混合气为工作气体，采用等离子体增强化学气相沉积技术在步骤（1）中的单晶硅基片表面沉积一层氮硅双修饰石墨烯量子点固态膜，其工艺参数是：射频功率密度为500W/cm2，基片温度为250℃，射频频率为13.56MHz，腔体压强为80Pa，高纯乙烯气体流量为80sccm，高纯氮气气体流量为12sccm，硅烷混合气体流量为7sccm，镀膜时间为80分钟。
通过以上步骤一种氮硅双修饰石墨烯量子点固态膜便制备完成。
实施例3：
一种氮硅双修饰石墨烯量子点固态膜制备方法，该方法包括以下步骤：
（1）采用常规清洗方法清洗单晶硅基片；
（2）以高纯乙烯（纯度大于99.995%）、高纯氮气（纯度大于99.999%）和被氩气稀释浓度为10%的硅烷混合气为工作气体，采用等离子体增强化学气相沉积技术在步骤（1）中的单晶硅基片表面沉积一层氮硅双修饰石墨烯量子点固态膜，其工艺参数是：射频功率密度为600W/cm2，基片温度为300℃，射频频率为13.56MHz，腔体压强为90Pa，高纯乙烯气体流量为90sccm，高纯氮气气体流量为15sccm，硅烷混合气体流量为10sccm，镀膜时间为90分钟。
通过以上步骤一种氮硅双修饰石墨烯量子点固态膜便制备完成。
实施例4：
一种氮硅双修饰石墨烯量子点固态膜制备方法，该方法包括以下步骤：
（1）采用常规清洗方法清洗单晶硅基片；
（2）以高纯乙烯（纯度大于99.995%）、高纯氮气（纯度大于99.999%）和被氩气稀释浓度为10%的硅烷混合气为工作气体，采用等离子体增强化学气相沉积技术在步骤（1）中的单晶硅基片表面沉积一层氮硅双修饰石墨烯量子点固态膜，其工艺参数是：射频功率密度为750W/cm2，基片温度为350℃，射频频率为13.56MHz，腔体压强为100Pa，高纯乙烯气体流量为100sccm，高纯氮气气体流量为15sccm，硅烷混合气体流量为10sccm，镀膜时间为100分钟。
通过以上步骤一种氮硅双修饰石墨烯量子点固态膜便制备完成。
以上所述为本发明较佳实施例而已，但本发明不应该局限于该实施例所公开的内容。所以凡是不脱离本发明所公开的精神下完成的等效或修改，都落入本发明保护的范围。
Claims (2)
1.一种氮硅双修饰石墨烯量子点固态膜制备方法，其特征在于，该方法包括下述步骤：
（1）清洗单晶硅基片；
（2）以高纯乙烯、硅烷混合气和高纯氮气为工作气体，高纯乙烯气体流量为60～100sccm，高纯氮气气体流量为10～15sccm，硅烷混合气气体流量为5～10sccm，采用等离子体增强化学气相沉积方法在步骤（1）中的单晶硅基片表面生长氮硅双修饰石墨烯量子点固态膜，其工艺参数是：射频功率密度为400～750 mW/cm-2，射频频率为13.56MHz，基片温度为200～350℃，腔体压强为60～100Pa，镀膜时间为60～100分钟，即可得到氮硅双修饰石墨烯量子点。
2.权利要求1所述的氮硅双修饰石墨烯量子点固态膜制备方法，其特征在于，所述的高纯乙烯的纯度大于99.995%；所述的高纯氮气的纯度大于99.999%；所述的硅烷混合气为采用氩气稀释到体积浓度为5-10%的硅烷。
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Application publication date: 20190129 Assignee: Henan Chaomei Building Materials Co.,Ltd. Assignor: CHINA THREE GORGES University Contract record no.: X2024980000728 Denomination of invention: Preparation method of nitrogen silicon double modified graphene quantum dot solid-state film Granted publication date: 20201009 License type: Common License Record date: 20240116 |