CN106086820B - 一种负载有纳米银的氟化石墨烯复合材料的制备方法 - Google Patents
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Abstract
本发明公开了一种负载有纳米银的氟化石墨烯复合材料的制备方法,包括如下步骤:1)将石墨烯薄膜至于PECVD反应室中,设压力为5×10‑4‑10‑3Pa,温度为200‑600℃,等离子体产生的微波功率为300‑500W,以氩气为载体,通入氟气,反应1‑20h,得到氟化石墨烯薄膜;2)将得到的氟化石墨烯薄膜转移至原子沉积腔室中,采用惰性气体除气20min‑30min,调节超真空反应腔的真空度为10‑6‑10‑7Pa,调节温度为400℃‑700℃;3)以银为靶材,通过电子束轰击蒸发形成银反应气源,通入到沉积腔室中,时间为20‑100ns,再通入惰性载气50‑200ns,重复步骤5‑20min,交替通入银反应气源和惰性载气,在氟化石墨烯薄膜上生长形成纳米银,得到负载有纳米银的氟化石墨烯复合材料。本发明得到的复合材料具有优良性能。
Description
技术领域
本发明涉及到复合材料制备的技术领域,特别涉及到一种负载有纳米银的氟化石墨烯复合材料的制备方法。
背景技术
随着城市化和工业化的进程越来越快,特别是改革开放以来,城市化和工业化都进入了一个高潮,而随之而来的是一系列导致城市不可持续发展的环境污染问题,特别是空气污染和水污染已经成为人类生存的重大威胁,成为人类健康、经济和社会可持续发展的重大障碍。特别是近些年来,人们对家居环境的追求,对室内装潢的要求越来越高,但是装修材料中的甲苯甲醛及其他挥发性有机物质,使室内空气污染严重,引发呼吸道疾病与生理机能障碍,以及眼鼻等粘膜组织受到刺激而患病等危害。
现有技术中因为活性炭呈毛细结构,具有很强的吸附能力,所以多采用竹炭等活性炭包吸附污染气体,净化空气,保持空气清新。但由于活性炭在使用过程中,常会过量的吸附污染气体,转换成吸附物质,覆在活性炭表面,使活性炭失活。
纳米银具有优良的比表面积活性及催化性能,对抗菌及光催化吸附污染气体等领域都起到了极其广泛的应用。墨烯是单原子厚度的二维碳原子晶体具有独特的电子,物理和化学性质。其独特的二维结构,使得石墨烯成为一个非常理想的纳米粒子的载体来制备石墨烯基的复合材料,用石墨烯负载纳米银粒子,存在于石墨烯层间的纳米银粒子可以起到分离邻近石墨烯片层,防止石墨烯发生团聚的作用。专利201410540914.7公开了一种石墨烯负载纳米银复合材料的制备方法,利用氧化石墨烯、银氨为原料,直接采用市面上可以出售的芦荟胶作为还原剂,在不添加任何稳定剂/分散剂的条件下,一步法制得纳米银负载石墨烯复合材料,具有工艺简单、原料来源广泛、反应温和、绿色环保等优点。但是该方法的到纳米银很难均匀充分的分布在石墨烯片的表面,石墨烯片表面部分区域团聚有大量的纳米颗粒,部分区域又没有纳米颗粒分布,从而导致复合材料的催化活性的有效比表面积降低。
发明内容
本发明的目的在于提出一种负载有纳米银的氟化石墨烯复合材料的制备方法,利用氟掺杂功能化石墨烯,能够诱导更多带正电的纳米银负载在石墨烯表面,提高了石墨烯对纳米银的负载率,同时形成稳定的复合材料,具有高活性和高吸附性,并能保持吸附稳定性和长久性,且制备成本低,无污染,符合绿色环保的目的。
为此,本发明采用以下技术方案:
一种负载有纳米银的氟化石墨烯复合材料的制备方法,包括如下步骤:
1)将石墨烯薄膜置于PECVD反应室中,设压力为5×10-4-10-3Pa,温度为200-600℃,等离子体产生的微波功率为300-500W,以氩气为载体,通入氟气,反应1-20h,得到氟化石墨烯薄膜;
2)将得到的氟化石墨烯薄膜转移至原子沉积腔室中,采用惰性气体除气20min-30min,调节超真空反应腔的真空度为10-6-10-7Pa,调节温度为400℃-700℃;
3)以银为靶材,通过电子束轰击蒸发形成银反应气源,通入到沉积腔室中,时间为20-100ns,再通入惰性载气50-200ns,重复步骤5-20min,交替通入银反应气源和惰性载气,在氟化石墨烯薄膜上生长形成纳米银,得到负载有纳米银的氟化石墨烯复合材料。
优选的,所述石墨烯薄膜的厚度为0.34-3.5nm,即1-10层。
优选的,所述通入氟气的流量为10-50sccm。
优选的,所述氟化石墨烯的氟的质量分数为0.1%-10%。
优选的,所述惰性气体为氦气或者氩气,其通入流量为10-100sccm。
优选的,所述电子束束流70-150mA。
优选的,所述银反应气源的通入流量为1-10sccm。
优选的,所述方法还包括将得到的负载有纳米银的氟化石墨烯复合材料在真空腔中以小于10℃/min的速率降温至室温后取出。
本发明采用以上技术方案,利用气相沉积法制备氟化石墨烯,得到的氟化石墨烯掺杂均匀,能够诱导更多带正电的纳米银负载在石墨烯表面,提高了石墨烯对纳米银的负载率,采用原子沉积法在氟化石墨烯表面沉积纳米银,可以避免纳米银在氟化石墨烯表面发生团聚,可形成稳定的复合材料,具有高活性和高吸附性,并能保持吸附稳定性和长久性,且制备成本低,无污染,符合绿色环保的目的。
附图说明
图1为本发明负载有纳米银的氟化石墨烯复合材料的制备方法流程示意图。
图2为本发明银反应气源和惰性载气通入方式示意图。
具体实施方式
为了使本发明的目的、特征和优点更加的清晰,以下结合附图及实施例,对本发明的具体实施方式做出更为详细的说明,在下面的描述中,阐述了很多具体的细节以便于充分的理解本发明,但是本发明能够以很多不同于描述的其他方式来实施。因此,本发明不受以下公开的具体实施的限制。
一种负载有纳米银的氟化石墨烯复合材料的制备方法,如图1所示,包括如下步骤:
1)将石墨烯薄膜置于PECVD反应室中,设压力为5×10-4-10-3Pa,温度为200-600℃,等离子体产生的微波功率为300-500W,以氩气为载体,通入氟气,反应1-20h,得到氟化石墨烯薄膜;
2)将得到的氟化石墨烯薄膜转移至原子沉积腔室中,采用惰性气体除气20min-30min,调节超真空反应腔的真空度为10-6-10-7Pa,调节温度为400℃-700℃;
3)以银为靶材,通过电子束轰击蒸发形成银反应气源,通入到沉积腔室中,时间为20-100ns,再通入惰性载气50-200ns,重复步骤5-20min,交替通入银反应气源和惰性载气,如图2所示,在氟化石墨烯薄膜上生长形成纳米银,得到负载有纳米银的氟化石墨烯复合材料。
其中,所述石墨烯薄膜的厚度为0.34-3.5nm,即1-10层。
其中,所述通入氟气的流量为10-50sccm。
其中,所述氟化石墨烯的氟的质量分数为0.1%-10%。
其中,所述惰性气体为氦气或者氩气,其通入流量为10-100sccm。
其中,所述电子束束流70-150mA。
其中,所述银反应气源的通入流量为1-10sccm。
其中,所述方法还包括将得到的负载有纳米银的氟化石墨烯复合材料在真空腔中以小于10℃/min的速率降温至室温后取出。
本发明利用气相沉积法制备氟化石墨烯,得到的氟化石墨烯掺杂均匀,能够诱导更多带正电的纳米银负载在石墨烯表面,提高了石墨烯对纳米银的负载率,采用原子沉积法在氟化石墨烯表面沉积纳米银,可以避免纳米银在氟化石墨烯表面发生团聚,可形成稳定的复合材料,具有高活性和高吸附性,并能保持吸附稳定性和长久性,且制备成本低,无污染,符合绿色环保的目的。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种负载有纳米银的氟化石墨烯复合材料的制备方法,其特征在于:包括如下步骤:
1)将石墨烯薄膜置于PECVD反应室中,设压力为5×10-4-10-3Pa,温度为200-600℃,等离子体产生的微波功率为300-500W,以氩气为载体,通入氟气,反应1-20h,得到氟化石墨烯薄膜;
2)将得到的氟化石墨烯薄膜转移至原子沉积腔室中,采用惰性气体除气20min-30min,调节超真空反应腔的真空度为10-6-10-7Pa,调节温度为400℃-700℃;
3)以银为靶材,通过电子束轰击蒸发形成银反应气源,通入到沉积腔室中,时间为20-100ns,再通入惰性载气50-200ns,重复步骤5-20min,交替通入银反应气源和惰性载气,在氟化石墨烯薄膜上生长形成纳米银,得到负载有纳米银的氟化石墨烯复合材料。
2.根据权利要求1所述的一种负载有纳米银的氟化石墨烯复合材料的制备方法,其特征在于,所述石墨烯薄膜的厚度为0.34-3.5nm,即1-10层。
3.根据权利要求1所述的一种负载有纳米银的氟化石墨烯复合材料的制备方法,其特征在于,所述通入氟气的流量为10-50sccm。
4.根据权利要求1所述的一种负载有纳米银的氟化石墨烯复合材料的制备方法,其特征在于,所述氟化石墨烯的氟的质量分数为0.1%-10%。
5.根据权利要求1所述的一种负载有纳米银的氟化石墨烯复合材料的制备方法,其特征在于,所述惰性气体为氦气或者氩气,其通入流量为10-100sccm。
6.根据权利要求1所述的一种负载有纳米银的氟化石墨烯复合材料的制备方法,其特征在于,所述电子束束流70-150mA。
7.根据权利要求1所述的一种负载有纳米银的氟化石墨烯复合材料的制备方法,其特征在于,所述银反应气源的通入流量为1-10sccm。
8.根据权利要求1所述的一种负载有纳米银的氟化石墨烯复合材料的制备方法,其特征在于,所述方法还包括将得到的负载有纳米银的氟化石墨烯复合材料在真空腔中以小于10℃/min的速率降温至室温后取出。
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