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CN107098340A - 一种石墨烯量子点分散液的制备方法 - Google Patents

一种石墨烯量子点分散液的制备方法 Download PDF

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CN107098340A
CN107098340A CN201710458545.0A CN201710458545A CN107098340A CN 107098340 A CN107098340 A CN 107098340A CN 201710458545 A CN201710458545 A CN 201710458545A CN 107098340 A CN107098340 A CN 107098340A
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CN107098340B (zh
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于希萌
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    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract

本发明属于材料科学技术领域，涉及一种环保、高效、便捷的石墨烯量子点分散液的制备方法，以化学气相沉积法制备的石墨烯为原料，将生长有石墨烯薄膜的金属箔放入10倍体积的腐蚀液中腐蚀2‑10h以去除金属箔，得到含石墨烯薄膜的腐蚀液，然后将腐蚀液在功率50‑200W下超声处理10‑150min，再用有机溶剂进行萃取以得到石墨烯量子点分散液，较好的利用了化学气相沉积法制备石墨烯时在石墨烯的生长、转移过程中引入的缺陷，无需添加强氧化剂或有毒试剂，也无需繁琐的氧化还原等处理，仅通过超声处理将大片石墨烯粉碎成石墨烯量子点，不会对石墨烯造成氧化破坏，最大程度上保护了石墨烯量子点的晶体结构；该方法操作简便，制备高效，环境友好，适于推广。

Description

一种石墨烯量子点分散液的制备方法
技术领域：
本发明属于材料科学技术领域，涉及一种环保、高效、便捷的石墨烯量子点分散液的制备方法，能够将利用化学气相沉积法制备的有缺陷的石墨烯经超声粉碎后制备出高质量的石墨烯量子点分散液。
背景技术：
石墨烯量子点(GQDs)是一种准零维碳材料，其作为石墨烯家族的最新一员，除了具有石墨烯的优异性能外，还因量子限制效应和边界效应而展现出一系列新的特性，其在生物、医学、材料、新型半导体器件等领域具有重要潜在应用，在太阳能电池、电子设备、光学染料、生物标记和复合微粒系统等方面也具有广泛应用；因此吸引了化学、物理、材料和生物等各领域科学家的广泛关注。仅近两三年内，关于这种新型零维材料的研究，在实验和理论方面均取了极大进展。实践中，制备石墨烯量子点的方法有多种，大体分为自上而下和自下而上两大类，自上而下的方法主要包括水热法、电化学方法和化学剥离碳纤维法；自下而上的方法主要包括溶液化学法、超声波法和微波法、可控热解多环芳烃法；但是上述方法均无法避免使用强氧化剂或有毒试剂，而且涉及的步骤繁琐复杂、工艺不稳定。例如中国专利201410591905.0公开的一种石墨烯量子点及其制备方法、中国专利201410362988.6公开的一种石墨烯量子点薄膜的制备方法、中国专利201410658230.7公开的一种多孔石墨烯和石墨烯量子点及其制备方法、中国专利201410778272.4公开的一种微波法制备多色荧光石墨烯量子点的方法等等。
另外，化学气相沉积法虽然是目前最佳的制备大片高质量石墨烯的方法，但是该方法制备的石墨烯在生长、转移等过程中无可避免的会引入褶皱、孔洞等缺陷，这些缺陷对石墨烯的机械性能、电学性能都将带来严重影响；因此，本发明结合化学气相沉积法和超声波法，研究出一种简单易行、环保高效的石墨烯量子点分散液的制备方法，能够轻松、简便、大量地制备出高质量石墨烯量子点，具有良好的应用价值和市场前景。
发明内容：
本发明的发明目的在于克服现有技术存在的缺点，寻求设计一种新型的、环保简易的石墨烯量子点分散液的制备方法，以化学气相沉积法制备的石墨烯为原料，经腐蚀去基底后通过超声处理，一步法制得石墨烯量子点的分散液。
为了实现上述目的，本发明涉及的石墨烯量子点分散液的制备方法具体包括以下工艺步骤：
(1)以化学气相沉积法制备的石墨烯为原料，将生长有石墨烯薄膜的金属箔放入10倍体积的腐蚀液中腐蚀2-10h以去除金属箔，得到含石墨烯薄膜的腐蚀液；
(2)将步骤(1)中得到的含石墨烯薄膜的腐蚀液在功率50-200W下超声处理10-150min，再用有机溶剂进行萃取以得到石墨烯量子点分散液。
进一步的，所述腐蚀液为硝酸铁溶液、硝酸溶液或过硫酸铵溶液；所述金属箔为铜箔或镍箔；所述有机溶剂为极性2-5的有机溶剂，包括环己烷(极性0.1)、二氯甲烷(极性3.5)、氯仿(极性4.4)和三氯甲烷。
本发明与现有技术相比，用化学气相沉积法制备的石墨烯膜为原料，经腐蚀液腐蚀去除金属箔后再超声处理使得石墨烯片粉碎成石墨烯量子点，从而制备出石墨烯量子点分散液；本发明涉及的方法较好的利用了化学气相沉积法制备石墨烯时在石墨烯的生长、转移过程中引入的缺陷，无需添加强氧化剂或有毒试剂，也无需繁琐的氧化还原等处理，仅通过超声处理将大片石墨烯粉碎成石墨烯量子点，不会对石墨烯造成氧化破坏，最大程度上保护了石墨烯量子点的晶体结构；该方法操作简便，制备高效，环境友好，适于推广。
附图说明：
图1为本发明涉及的石墨烯量子点制备方法的工艺流程示意框图。
图2为本发明的实施例1中制备的石墨烯量子点分散液在自然光下的图片。
图3为本发明的实施例1中石墨烯量子点的原子力显微镜扫描图。
图4为本发明的实施例1中石墨烯量子点的高度分布图。
图5为本发明的实施例2中制备的石墨烯量子点分散液在紫外光下的图片。
图6为本发明的实施例2中石墨烯量子点的透射电子显微镜图。
图7为本发明的实施例2中石墨烯量子点的高分辨透射电子显微镜图。
图8为本发明的实施例2中石墨烯量子点的尺寸分布图。
具体实施方式：
下面结合附图并通过实施例对本发明作进一步详细说明，但本发明并不局限于以下实施方式。
实施例1：
本实施例中涉及的石墨烯量子点的制备方法具体步骤为：
(1)将1cm×1cm或2cm×2cm的生长有石墨烯薄膜的铜箔放入20-80mL过硫酸铵(0.05-0.5M)腐蚀液中腐蚀3-8h以去除铜箔，得到含石墨烯薄膜的腐蚀液；
(2)将步骤(1)中得到的含石墨烯薄膜的腐蚀液超声(功率50-200W)处理10-150min，再用二氯甲烷萃取以得到石墨烯量子点分散液。
本实施例中制备的石墨烯量子点分散液在自然光下照片(如图2所示)荧光好；其中石墨烯量子点的原子力显微镜扫描图(如图3所示)和高度分布图(如图4所示)。
实施例2：
本实施例中涉及的石墨烯量子点的制备方法具体步骤为：
(1)以化学气相沉积法制备的石墨烯为原料，将2-20cm2生长有石墨烯薄膜的金属箔放入20-200mL硝酸铁(0.1-0.5g/ml)溶液中腐蚀2-10h以去除金属箔，得到含石墨烯薄膜的腐蚀液；
(2)将步骤(1)中得到的含石墨烯薄膜的腐蚀液超声(功率50-200W)处理10-150min，再用三氯甲烷萃取以得到石墨烯量子点分散液。
本实施例中制备的石墨烯量子点分散液在365nm紫外光下照片(如图5所示)；其中石墨烯量子点的透射电子显微镜图(如图6所示)、高分辨透射电子显微镜图(如图7所示)和尺寸分布图(如图8所示)。
以上所述仅为本发明的较佳实施方式，本发明的保护范围并不以上述实施方式为限，但凡本领域技术人员根据本发明所述内容所作的等效变化，皆应纳入权利要求书中记载的保护范围内。

Claims (2)

1.一种石墨烯量子点分散液的制备方法，其特征在于包括以下工艺步骤：
(1)以化学气相沉积法制备的石墨烯为原料，将生长有石墨烯薄膜的金属箔放入10倍体积的腐蚀液中腐蚀2-10h以去除金属箔，得到含石墨烯薄膜的腐蚀液；
(2)将步骤(1)中得到的含石墨烯薄膜的腐蚀液在功率50-200W下超声处理10-150min，再用有机溶剂进行萃取以得到石墨烯量子点分散液。
2.根据权利要求1所述的石墨烯量子点分散液的制备方法，其特征在于所述腐蚀液为硝酸铁溶液、硝酸溶液或过硫酸铵溶液；所述金属箔为铜箔或镍箔；所述有机溶剂为极性2-5的有机溶剂，包括环己烷、二氯甲烷、氯仿和三氯甲烷。
CN201710458545.0A 2017-06-16 2017-06-16 一种石墨烯量子点分散液的制备方法 Expired - Fee Related CN107098340B (zh)

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