CN107311236A - 一种Fe2O3@SnO2核壳结构纳米棒的制备方法 - Google Patents
一种Fe2O3@SnO2核壳结构纳米棒的制备方法 Download PDFInfo
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Abstract
本发明公开了一种Fe2O3@SnO2核壳结构纳米棒的制备方法,包括以下步骤:将锡酸钠加入到硝酸铁水溶液中,混合均匀后,然后在120‑200℃下反应,最后经过离心分离、洗涤和干燥,得到Fe2O3@SnO2核壳结构纳米棒。其中,锡酸钠和硝酸铁的摩尔比为1:10‑1:2,锡酸钠的摩尔浓度为0.020‑0.100 moL/L,硝酸铁的摩尔浓度为0.200moL/L。本发明采用水热方法,制备条件温和,工艺简单节能;本发明制备方法合成的Fe2O3@SnO2核壳结构纳米棒以Fe2O3长度约为100‑200 nm纳米棒为核,SnO2纳米粒子为壳组成;与Fe2O3相比,Fe2O3@SnO2核壳结构纳米棒对乙醇表现出更高的灵敏度。
Description
技术领域
本发明涉及的是新材料领域,具体涉及一种Fe2O3@SnO2核壳结构纳米棒的制备方法。
背景技术
在纳米结构设计中,半导体纳米异质结,由于其含有不同的成分,在光电化学、气敏和催化等领域具有潜在的应用。材料的性能受其成分、形貌和尺寸的影响,因此生长不同成分、形貌和尺寸的纳米异质结引起了人们极大的兴趣。至今为止,国内外的科研工作者合成了大量的纳米异质结。例如Fe2O3/TiO2、Fe2O3/SnO2、CdSe/CdS、ZnO/ZnFe2O4、PPY@CoNi-LDH、AlCo-LDH/MOF等等,并广泛应用于催化、传感等领域,不同的成分和特殊的结构大大提高了材料的性能。与单一的成分相比,不同成分之间的协同效应大大提高了材料的性能。
作为功能氧化物半导体纳米材料,Fe2O3和SnO2在气敏、催化和电池等领域都展现了优异的性能。复合材料相对于单一的成分,某方面性能往往得到提高。Fe2O3@SnO2复合材料纳米异质结在光电化学、催化和气敏等方面显示出更优异的性能。
通常情况下,Fe2O3@SnO2核壳结构的合成采用两步法合成,首先得到Fe2O3纳米结构,然后再在Fe2O3纳米结构上生长SnO2纳米结构,从而得到Fe2O3@SnO2核壳结构。关于一步水热法合成Fe2O3@SnO2核壳结构纳米棒尚未见报道。
综上所述,本发明设计了一种Fe2O3@SnO2核壳结构纳米棒的一步制备方法。
发明内容
针对现有技术上存在的不足,本发明目的是在于提供一种a-Fe2O3@SnO2核壳结构纳米棒的制备方法,该方法采用水热方法,通过一步简单的混合过程合成出Fe2O3@SnO2核壳结构纳米棒,简单易行,避免了传统过程中首先得到Fe2O3再复合SnO2的繁琐处理过程。
为了实现上述目的,本发明是通过如下的技术方案来实现:一种Fe2O3@SnO2核壳结构纳米棒的制备方法,包括以下步骤:首先配制0.2 mol/L的硝酸铁溶液,将一定量的锡酸钠加入到硝酸铁水溶液中,磁力搅拌10-30min,分散均匀得到混合液;然后在120-200℃下反应1-12小时;最后经过离心分离、洗涤和干燥,得到Fe2O3@SnO2核壳结构纳米棒。
作为优选,所述的锡酸钠和硝酸铁的摩尔比为1:10-1:2。
作为优选,所述的混合溶液中锡酸钠的摩尔浓度为0.020-0.100 moL/L。
作为优选,所述的硝酸铁的摩尔浓度为0.200 moL/L。
作为优选,所述洗涤,分别采用水和乙醇对产品洗涤。
作为优选,所述干燥采用烘箱干燥,干燥温度为50-80℃,时间为6-24 h。
本发明具有以下有益效果:1、采用一步水热方法,制备条件温和,工艺简单;
2、本发明制备方法可得到核壳结构的Fe2O3@SnO2纳米棒,制备的Fe2O3@SnO2纳米棒,长度约为100-200 nm;以Fe2O3纳米棒为核, SnO2纳米粒子为壳组成;
3、与Fe2O3相比,Fe2O3@SnO2核壳结构纳米棒对乙醇表现出更高的灵敏度;
4、Fe2O3@SnO2核壳结构纳米棒在气体传感、光电转换、光催化等领域具有大的应用潜力。
附图说明
下面结合附图和具体实施方式来详细说明本发明;
图1本发明实施例锡酸钠和硝酸铁不同摩尔比样品的XRD图谱。
图2本发明实施例1产品的EDX元素分布mappings图。
图3本发明实施例1产品的电镜图,其中,(a,b)为FE-SEM图,(c,d)为TEM图,(e)为单个纳米棒的TEM图,(f)为HRTEM图(内附SAED图)。
图4本发明实施例1产品的XPS图谱。
图5本发明实施例2产品的FE-SEM电镜图。
图6本发明实施例3产品的FE-SEM电镜图。
图7a是本发明实施例1制备的Fe2O3@SnO2核壳结构纳米棒气敏传感器对不同浓度乙醇的响应曲线图;b是Fe2O3气敏传感器对不同浓度乙醇的响应曲线图。
具体实施方式
为使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施方式,进一步阐述本发明。
实施例1:一种Fe2O3@SnO2核壳结构纳米棒的制备方法,包括以下步骤:
(1)将0.2 mmoL锡酸钠加入到10 mL 0.200 moL/L硝酸铁水溶液中,采用磁力搅拌30min,得到悬浊液;
(2)将悬浊液倒入聚四氟乙烯内衬的不锈钢高压反应釜中,升温至160℃,反应6 h,反应完后随炉冷却;
(3 )将反应产物离心分离,得到固体粉末,接着依次用蒸馏水、乙醇洗涤,然后在60℃下干燥24 h,得到Fe2O3@SnO2核壳结构纳米棒。
采用X射线粉末衍射(XRD)、场发射扫描电子显微镜(FE-SEM)和透射电子显微镜(TEM)对产品进行分析。
图1(b)是实施例1产品的XRD图,结果表明本实施例产品是六方晶型的Fe2O3相;SnO2为无定型相,XRD图谱上看不到其衍射峰。图2为实施例1产品的EDX 元素分布mappings图,由图可以看到产品为Fe2O3纳米棒为核, SnO2纳米粒子为壳组成的核壳结构。
图3(a)(b)为实施例1产品的SEM图,图3(c,d)为实施例1产品的TEM图,图3(e)为单个纳米棒的TEM图,图3(f)为单个纳米棒的高分辨透射电镜图和选区电子衍射图。从图中可以看出,实施例1产品的长度约为100-200 nm,大小均匀;晶格条文清晰,结晶良好,为多晶结构。
图4为实施例1产品的XPS图,由于XPS只能检测样品表面1-10nm厚度的元素。由图可以看到产品的外壳为SnO2。
实施例2:
(1)将0.4 mmoL锡酸钠加入到10 mL 0.200 moL/L硝酸铁水溶液中,采用磁力搅拌20min,得到悬浊液;
(2)将悬浊液倒入聚四氟乙烯内衬的不锈钢高压反应釜中,升温至160℃,反应6 h,反应完后随炉冷却;
(3 )将反应产物离心分离,得到固体粉末,接着依次用蒸馏水、乙醇洗涤,然后在70℃下干燥16 h,得到Fe2O3@SnO2核壳结构纳米棒。
制得的产品与实施例1基本一致,棒的直径略微加大,其XRD如图1(c)和扫瞄电镜图如图5(a)(b)所示。
实施例3:
(1)将1 mmoL锡酸钠加入到10 mL 0.200 moL/L硝酸铁水溶液中,采用磁力搅拌10min,得到悬浊液;
(2)将悬浊液倒入聚四氟乙烯内衬的不锈钢高压反应釜中,升温至200℃,反应12h,反应完后随炉冷却;
(3 )将反应产物离心分离,得到固体粉末,接着依次用蒸馏水、乙醇洗涤,然后在80℃下干燥12h,得到Fe2O3@SnO2核壳结构纳米棒。
制得的产品与实施例1基本一致,棒的直径变大,与棒上生长的SnO2纳米粒子变多有关。其XRD如图1(d),扫瞄电镜图如图6(a)(b)所示。
实施例4:
以实施例1制备的Fe2O3@SnO2核壳结构纳米棒测试其气敏性能。具体为:Fe2O3@SnO2核壳结构纳米棒和Fe2O3样品与一定量的无水乙醇混合成糊状。将糊均匀致密地涂在有四个Pt电极的Al2O3微米管上后,将其焊接在基座上。气敏性测试在昆明贵研金峰科技有限公司生产的 JF02E系统上进行。测试浓度范围100–500 ppm,温度180°C,控温系统的压强:2.0–5.0V。
图7为实施例1制备的Fe2O3@SnO2核壳结构纳米棒气敏传感器对不同浓度乙醇的响应曲线图。当乙醇浓度为100 ppm时,Fe2O3@SnO2核壳结构纳米棒对乙醇的灵敏度为14.3。随着乙醇浓度从100 ppm增加到500 ppm时,Fe2O3@SnO2核壳结构纳米棒的灵敏度分别从14.3增加到 58.7。而Fe2O3样品的灵敏度从9.6增加到 29.3。Fe2O3@SnO2核壳结构纳米棒表现出比Fe2O3样品更高的灵敏度。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (6)
1.一种Fe2O3@SnO2核壳结构纳米棒的制备方法,其特征在于,包括以下步骤:首先配制0.2 mol/L的硝酸铁溶液,将一定量的锡酸钠加入到硝酸铁水溶液中,磁力搅拌10-30min,分散均匀得到混合液;然后在120-200℃下反应1-12小时;最后经过离心分离、洗涤和干燥,得到a-Fe2O3@SnO2核壳结构纳米棒。
2.根据权利要求1所述的一种Fe2O3@SnO2核壳结构纳米棒的制备方法,其特征在于,所述的锡酸钠和硝酸铁的摩尔比为1:10-1:2。
3.根据权利要求1所述的一种Fe2O3@SnO2核壳结构纳米棒的制备方法,其特征在于,所述的混合溶液中锡酸钠的摩尔浓度为0.020-0.100 moL/L。
4.根据权利要求1所述的一种Fe2O3@SnO2核壳结构纳米棒的制备方法,其特征在于,所述的硝酸铁的摩尔浓度为0.200 moL/L。
5.根据权利要求1所述的一种Fe2O3@SnO2核壳结构纳米棒的制备方法,其特征在于,所述洗涤,分别采用水和乙醇对产品洗涤。
6.根据权利要求1所述的一种Fe2O3@SnO2核壳结构纳米棒的制备方法,其特征在于,所述干燥采用烘箱干燥,干燥温度为50-80℃,时间为6-24 h。
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