CN101274751B - 单分散银、硫化银及硒化银纳米晶的制备方法 - Google Patents
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Abstract
本发明涉及一种单分散银纳米晶的制备方法,其包括以下步骤:(1)将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中反应1至10分钟;(2)将反应沉淀物以乙醇洗涤后烘干,即得到单分散银纳米晶。该制备方法中的步骤(1)可通过进一步将硫粉放入上述反应体系后继续反应8至12分钟,获得单分散硫化银纳米晶或通过进一步将硒粉放入上述反应体系后继续反应8至12分钟,获得单分散硒化银纳米晶。本发明所提供的单分散银、硫化银及硒化银纳米晶的制备方法适于大规模工业生产,具有极为广阔的市场前景。
Description
技术领域
本发明涉及一种银、硫化银及硒化银的制备方法,尤其涉及单分散银、硫化银及硒化银纳米晶的制备方法。
背景技术
纳米尺寸的金属银颗粒由于具有独特的光学、电学及催化性质而广泛地应用于传感器、催化、纳米器件、光学开关等方面。例如,纳米银颗粒具有极强的增强表面拉曼光谱(SERS)的能力而被广泛地应用于拉曼光谱技术原位检测催化反应方面。
硫化银和硒化银是化学稳定性较高的半导体材料,具有较好的光电及热电性能,现已被广泛地应用于光电池、光电导元件、红外检测器及快离子导体等制造业。当硫化银和硒化银的颗粒尺寸降为纳米量级时,由于较大的比表面积和显著的量子尺寸效应,与体相材料相比,其会具有特殊的光吸收、传感及催化性能。例如,近年来人们发现纳米硫化银具有很强的杀菌能力,使其在生物、医学及环境治理等方面有着重要的潜在应用。
因此,银、硫化银及硒化银纳米材料的合成和性质的研究已成为广泛研究的热点。近年来,化学法在单分散纳米晶控制合成方面已经取得了很大的进展,例如,以金属有机物为反应前驱物,通过控制合成条件,能获得具有规则多面体外形的银纳米晶;采用液相-固相-溶液(LSS)反应机制成功合成单分散银及硫化银纳米晶,并能有效地控制其粒径大小。然而这些方法工艺复杂、耗时、反应毒性大、难于批量生产,且其产品的质量稳定性也较差,因而难于实现工业应用。
有鉴于此,提供一种工艺简便、耗时少、反应毒性小、易于批量生产,且产品质量稳定的银、硫化银及硒化银单分散纳米晶的制备方法是必要的。
发明内容
一种单分散银纳米晶的制备方法,其包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中,在160℃至300℃温度下反应1至10分钟;将反应沉淀物以乙醇洗涤后,于40℃至80℃温度下烘干,即得到粒径为6至12纳米的单分散银纳米晶。
一种单分散硫化银纳米晶的制备方法,其包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中,在160℃至300℃温度下反应1至10分钟;将硫粉放入上述反应体系后继续反应8至12分钟;将反应沉淀物以乙醇洗涤后,于40℃至80℃温度下烘干,即得到粒径为6至12纳米的单分散硫化银纳米晶。其中,硫粉与硝酸银的摩尔比为1∶2。
一种单分散硒化银纳米晶的制备方法,其包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中,在160℃至300℃温度下反应1至10分钟;将硒粉放入上述反应体系后继续反应8至12分钟;将反应沉淀物以乙醇洗涤后,于40℃至80℃温度下烘干,即得到粒径为6至12纳米的单分散硒化银纳米晶。其中,硒粉与硝酸银的摩尔比为1∶2。
与现有技术相比,本发明所提供的制备方法具有如下优点:采用无机物为原料,该制备方法的反应毒性小,原料更为经济;采用十八胺为溶剂,具有毒性小、价格便宜的特点,且十八胺通过简单的过滤、分离即可重复利用;所得的产物颗粒小、粒径尺寸分布均匀;反应时间短,为该制备方法应用于工业化生产奠定了基础。因此,本发明所提供的单分散银、硫化银及硒化银纳米晶的制备方法适于大规模工业生产,具有极为广阔的市场前景。
附图说明
图1是本发明实施例制备的单分散银纳米晶的透射电子显微镜(TEM)照片。
图2是本发明实施例制备的单分散硫化银纳米晶的TEM照片。
图3是本发明实施例制备的单分散硒化银纳米晶的TEM照片。
图4是本发明实施例制备的单分散银、硫化银及硒化银纳米晶的粉末X射线衍射(XRD)图。
具体实施方式
下面将结合附图对本发明实施例作进一步的详细说明。
一种单分散银纳米晶的制备方法,其具体包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中,在160℃至300℃温度下反应1至10分钟;将反应沉淀物以乙醇洗涤后,于40℃至80℃温度下烘干,即得到粒径为6至12纳米的单分散银纳米晶。
上述反应的化学方程式如下:
请参阅图1为本发明实施例制备的单分散银纳米晶的透射电子显微镜(TEM)照片。
一种单分散硫化银纳米晶的制备方法,其包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中,在160℃至300℃温度下反应1至10分钟;将硫粉放入上述反应体系后继续反应8至12分钟;将反应沉淀物以乙醇洗涤后,于40℃至80℃温度下烘干,即得到粒径为6至12纳米的单分散硫化银纳米晶。其中,硫粉与硝酸银的摩尔比为1∶2。
上述反应的化学方程式如下:
请参阅图2为本发明实施例制备的单分散硫化银纳米晶的TEM照片。
一种单分散硒化银纳米晶的制备方法,其包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中,在160℃至300℃温度下反应1至10分钟;将硒粉放入上述反应体系后继续反应8至12分钟;将反应沉淀物以乙醇洗涤后,于40℃至80℃温度下烘干,即得到粒径为6至12纳米的单分散硒化银纳米晶。其中,硒粉与硝酸银的摩尔比为1∶2。
上述反应的化学方程式如下:
请参阅图3为本发明实施例制备的单分散硒化银纳米晶的TEM照片。
请参阅图4为本发明实施例制备的单分散银、硫化银及硒化银纳米晶的粉末X射线衍射(XRD)图。
下面例举实施例对本发明予以进一步说明:
实施例一:
取10毫升(ml)十八胺加热到200℃,将1克(g)硝酸银固体加入其中,保持在200℃温度下反应10分钟后,将反应所得的沉淀物以乙醇洗涤,在40℃至80℃温度下干燥,即得到粒径为4.7纳米的单分散银纳米晶。
实施例二:
取10ml十八胺加热到200℃,将0.85g硝酸银固体加入其中,保持在200℃温度下反应10分钟后,再加入0.08g硫粉反应10分钟。将反应所得的沉淀物以乙醇洗涤,在40℃至80℃温度下干燥,即得到粒径为7.3纳米的单分散硫化银纳米晶。
实施例三:
取10ml十八胺加热到200℃,将0.85g硝酸银固体加入其中,保持在200℃温度下反应10分钟后,再加入0.198g硒粉反应10分钟。将反应所得的沉淀物以乙醇洗涤,在40℃至80℃温度下干燥,即得到粒径为8.5纳米的单分散硒化银纳米晶。
与现有技术相比,本发明所提供的制备方法具有如下优点:采用无机物为原料,该制备方法的反应毒性小,原料更为经济;采用十八胺为溶剂,具有毒性小、价格便宜的特点,且十八胺通过简单的过滤、分离即可重复利用;所得的产物颗粒小、粒径尺寸分布均匀;反应时间短,为该制备方法应用于工业化生产奠定了基础。因此,本发明所提供的单分散银、硫化银及硒化银纳米晶的制备方法适于大规模工业生产,具有极为广阔的市场前景。
另外,本领域技术人员还可在本发明精神内做其它变化。当然,这些依据本发明精神所做的变化,都应包含在本发明所要求保护的范围之内。
Claims (11)
1.一种单分散银纳米晶的制备方法,其包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中在160℃至300℃温度下反应1至10分钟;将反应沉淀物以乙醇洗涤后烘干,即得到单分散银纳米晶。
2.如权利要求1所述的单分散银纳米晶的制备方法,其特征在于,单分散银纳米晶的粒径为6至12纳米。
3.如权利要求1所述的单分散银纳米晶的制备方法,其特征在于,烘干温度为40℃至80℃。
4.一种单分散硫化银纳米晶的制备方法,其包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中在160℃至300℃温度下反应1至10分钟;将硫粉放入上述反应体系后继续反应8至12分钟;将反应沉淀物以乙醇洗涤后烘干,即得到单分散硫化银纳米晶。
5.如权利要求4所述的单分散硫化银纳米晶的制备方法,其特征在于,硫粉与硝酸银的摩尔比为1∶2。
6.如权利要求4所述的单分散硫化银纳米晶的制备方法,其特征在于,单分散硫化银纳米晶的粒径为6至12纳米。
7.如权利要求4所述的单分散硫化银纳米晶的制备方法,其特征在于,烘干温度为40℃至80℃。
8.一种单分散硒化银纳米晶的制备方法,其包括以下步骤:将0.1克至1克的硝酸银放入10毫升的十八胺溶剂中在160℃至300℃温度下反应1至10分钟;将硒粉放入上述反应体系后继续反应8至12分钟;将反应沉淀物以乙醇洗涤后烘干,即得到单分散硒化银纳米晶。
9.如权利要求8所述的单分散硒化银纳米晶的制备方法,其特征在于,硒粉与硝酸银的摩尔比为1∶2。
10.如权利要求8所述的单分散硒化银纳米晶的制备方法,其特征在于,单分散硒化银纳米晶的粒径为6至12纳米。
11.如权利要求8所述的单分散硒化银纳米晶的制备方法,其特征在于,烘干温度为40℃至80℃。
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US20050199094A1 (en) * | 2003-09-09 | 2005-09-15 | Noble Fiber Technologies, Inc. | Method of producing metal-containing particles |
KR100621309B1 (ko) * | 2004-04-20 | 2006-09-14 | 삼성전자주식회사 | 황 전구체로서 싸이올 화합물을 이용한 황화 금속나노결정의 제조방법 |
US7288134B2 (en) * | 2004-09-10 | 2007-10-30 | International Business Machines Corporation | Dumbbell-like nanoparticles and a process of forming the same |
KR100690360B1 (ko) * | 2005-05-23 | 2007-03-09 | 삼성전기주식회사 | 도전성 잉크, 그 제조방법 및 도전성 기판 |
KR100711967B1 (ko) * | 2005-08-08 | 2007-05-02 | 삼성전기주식회사 | 금속 나노 입자의 제조방법 및 도전성 잉크 |
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