CN109516492B - 一种Cu2S微纳米晶的制备方法 - Google Patents
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Abstract
一种Cu2S微纳米晶的制备方法,涉及Cu2S材料制备以及污水处理技术领域。首先,将氯化铜溶于去离子水中配成氯化铜水溶液;然后,将硫脲加入至氯化铜水溶液中,超声和搅拌快速反应后得到白色沉淀,将沉淀抽滤出来便得到铜‑硫脲配合物前驱体;最后,将铜‑硫脲前驱体转入到反应釜中,并加入适量的有机溶剂,密封后进行溶剂热还原反应,即可获得Cu2S产物。在不同溶剂中成功获得了由若干Cu2S纳米结构单元构成的多种形态的Cu2S微纳米晶。该方法具有操作简单、产物形态可控、可见光吸收性能优异和成本低廉等优点。获得Cu2S微纳米晶具有良好的可见光吸收性能,可望用于污染物治理领域。
Description
技术领域
本发明涉及Cu2S材料制备以及污水处理技术领域,具体是涉及一种Cu2S微纳米晶的制备方法。
背景技术
辉铜矿(Cu2S)是自然界中一种重要的矿物,也是一种重要的P型半导体材料(Eg~1.2eV),在太阳能电池、光电器件和光催化等方面应用广泛。通常来说,Cu2S纳米晶的合成及组装是在有机相中进行的。例如,在十二胺、三辛基氧化膦和油酸等高沸点有机相中采用热分解巯基酸铜前驱体可以得到Cu2S纳米盘、纳米球和纳米线等。十二胺、三辛基氧化膦和油酸等高沸点有机相中,采用高温(250~350℃)手段来制备Cu2S纳米晶或量子点,需要在严格的无水和无氧条件下,制备工艺复杂,环境污染严重。
另外,还存在以巯基乙酸、半胱氨酸和青霉胺等为配体水热合成法制备,其具有简单,多功能性、可扩展性、环境友好性和低成本性等优点。但是,通常需要选择短链硫醇作为Cu2S 的稳定剂,环境污染大,且获得的产物尺寸小,不易分离等。
微纳米结构材料由于具有较大尺寸和稳定性,在使用过程中较容易分散和分离。同时,微纳米结构材料中又有若干纳米结构单元,因此又具有一些纳米效应。因此,微纳米结构材料兼具有微米尺寸材料和纳米材料各自的优点。近年来,材料研究者对各种微纳米结构材料研究和报道常采用绿色、环境友好的有机溶剂为反应介质制备。
发明内容
本发明针对已有制备Cu2S微纳米晶中所存在的不足之处,提供一种Cu2S微纳米晶的制备方法。在硫脲-铜配合物前驱体和多元醇介质中通过溶剂热反应快速得到了具有微纳米结构的 Cu2S微纳米晶。通过改变溶剂的种类,可获得不同形态的Cu2S微纳米晶。
为了实现上述目的,本发明所采用的技术方案为:一种Cu2S微纳米晶的制备方法,首先,将氯化铜(CuCl2·2H2O)溶于去离子水中配成氯化铜水溶液;然后,将硫脲(CH4N2S)加入至氯化铜水溶液中,超声和搅拌快速反应后得到白色沉淀,将沉淀抽滤出来便得到铜-硫脲配合物前驱体;最后,将铜-硫脲前驱体转入到反应釜中,并加入适量的有机溶剂,密封后进行溶剂热还原反应,即可获得Cu2S产物。
作为本发明制备方法的优选技术方案,制备铜-硫脲前驱体时氯化铜与硫脲的添加量摩尔比为1.5~3:1,反应时间为1~10min。溶剂热还原反应时向每1g铜-硫脲前驱体加入5~20mL 的乙二醇或丙三醇。有机溶剂为乙二醇时制备产物的微观形态为由纳米片组装而成的微米棒状结构;有机溶剂为丙三醇时制备产物的微观形态为由纳米片组装而成的微米球状结构。溶剂热还原反应的反应温度为180~200℃,反应时间为6~24h。
与现有技术相比,本发明的有益效果表现在:
本发明以铜-硫脲配合物为前驱体,在不同溶剂中成功获得了由若干Cu2S纳米结构单元构成的多种形态的Cu2S微纳米晶。该方法具有操作简单、产物形态可控、可见光吸收性能优异和成本低廉等优点。获得Cu2S微纳米晶具有良好的可见光吸收性能,可望用于污染物治理领域。
附图说明
图1为实施例1中制备两种形态微纳米晶产物的XRD图;
图2a、b为实施例1中以乙二醇为有机溶剂制备微纳米晶产物的形态和化学组成;图2c、 d为实施例1中以丙三醇为有机溶剂制备微纳米晶产物的形态和化学组成;
图3为实施例1中以乙二醇、丙三醇作为有机溶剂所得到的微纳米晶的波长与带隙大小的关系曲线;
图4为实施例2中不同反应时间制备微纳米晶产物的形态。
具体实施方式
以下结合实施例和附图对本发明的Cu2S微纳米晶的制备方法作出进一步的详述。本发明方法所得产物的结构、形态性能分别采用场发射扫描电子显微镜(FE-SEM,SU8010)、X射线粉末衍射(XRD,D3500)和紫外-可见光谱仪(Vb300)来表征和分析。
实施例1:
一种Cu2S微纳米晶的制备方法,步骤如下:
1)、将17g的氯化铜(CuCl2·2H2O)溶于100mL的去离子水中配成氯化铜水溶液。
2)、将4g的硫脲(CH4N2S)加入至上述氯化铜水溶液中,超声和搅拌快速5min反应后得到白色沉淀,将沉淀抽滤出来便得到铜-硫脲配合物前驱体。
3)、取10g的铜-硫脲前驱体转入到反应釜中,并加入100mL的有机溶剂,密封后进行溶剂热还原反应(180℃、18h),即可获得Cu2S产物。
上述有机溶剂分别选择乙二醇和丙三醇,通过选择不同反应介质种类观察对Cu2S结构、形态和光学性能的影响。
图1为实施例1中制备两种形态微纳米晶产物的XRD图(a、b分别对应有机溶剂选择乙二醇、丙三醇制备产物),与标准XRD谱图相比较可以看出,两种形态的产物均为高纯的Cu2S 物相。
图2a、b为实施例1中以乙二醇为有机溶剂制备微纳米晶产物的形态和化学组成,通过图可以看出,采用乙二醇作为溶剂进行溶剂热还原反应制备产物的微观形态为由纳米片组装而成的微米棒状结构,每个片层厚度为60nm左右。图2b是取局部分布,Cu和S在标准谱的衍射峰之比为2:1。
图2c、d为实施例1中以丙三醇为有机溶剂制备微纳米晶产物的形态和化学组成,通过图可以看出,采用丙三醇作为溶剂进行溶剂热还原反应制备产物的微观形态为由纳米片组装而成的微米球状结构,粒径比较均一。图2d是取局部分布,Cu和S在标准谱的衍射峰之比为2: 1。
图3为实施例1中以乙二醇、丙三醇作为有机溶剂所得到的微纳米晶的波长与带隙大小的关系曲线,通过图3可以看出棒状和球状Cu2S的最大吸收波长差不多都在500nm,进一步可以估算出两者的带隙都约为1.24eV。
实施例2:反应时间对Cu2S微纳米晶形态的影响。
制备方法同实施例1,在以丙三醇作为反应溶剂前提下,分别反应6h、12h、18h、24h,得到与之对应的图4a、图4b、图4c、图4d四种不同形貌的Cu2S微纳米晶产物。
通过图4可以看出,反应6h和12h时所得产物(图4a、b)形状各异;当反应到18h左右时所得到的产物(图4c)的分布形态由最初的形状大小不一、形状各异逐渐变为球状分布;当反应24h后所得产物(图4d)球形度较高,分布较均匀。但反应时间过长下,纳米层片堆积Cu2S微球时会出现空心现象。
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (1)
1.一种Cu2S微纳米晶的制备方法,其特征在于,步骤如下:
1)、将17 g的氯化铜CuCl2▪2H2O溶于100 mL的去离子水中配成氯化铜水溶液;
2)、将4 g的硫脲CH4N2S加入至上述氯化铜水溶液中,超声和搅拌快速5 min反应后得到白色沉淀,将沉淀抽滤出来便得到铜-硫脲配合物前驱体;
3)、取10 g的铜-硫脲前驱体转入到反应釜中,并加入100 mL的乙二醇,密封后进行溶剂热还原反应,反应温度为180℃,反应时间为18 h,即可获得Cu2S产物,制备产物的微观形态为由纳米片组装而成的微米棒状结构。
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