CN106582653A - 一种Fe3O4/FeNi纳米链状复合材料的制备方法 - Google Patents
一种Fe3O4/FeNi纳米链状复合材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种Fe3O4/FeNi纳米链状复合材料的制备方法:包括以下步骤:将Fe2(C2O4)3∙5H2O的水溶液和Ni(CH3COO)2∙4H2O的乙二醇溶液溶于乙二醇中,常温条件下超声处理,然后转移至反应釜中加热保温,反应结束,冷却至室温,将样品进行离心,洗涤,真空干燥收集中间产物,将其放进管式炉中,通入氮气气体保护,在一定温度下退火并保温一定时间,得黑色固体粉末。本发明工艺简单,制备条件通用,产物形貌稳定,纯度高,且产物处理简单,适合中等规模工业生产。
Description
技术领域
本发明属于无机纳米材料技术领域,尤其涉及一种Fe3O4/FeNi纳米链状复合材料的制备方法。
背景技术
纳米科学技术是20世纪80年代末产生的一项正在迅猛发展的新技术。所谓纳米技术是指用若干分子或原子构成的单元——纳米微粒,制造材料或微型器件的科学技术。纳米微粒是指尺寸介于1~100 nm之间的金属或半导体的细小颗粒。纳米微粒所具有的特殊结构层次,赋予了它许多特殊的性质和功能,纳米粒子具有大的比表面积,表面原子数、表面能和表面张力随粒径的下降急剧增加,表面效应、小尺寸效应、量子尺寸效应、宏观量子隧道效应及介电限域效应等导致纳米粒子的热、磁、光、敏感特性和表面稳定性等不同于常规粒子,这就使它具有广泛的应用前景。
多级复合结构由于界面效应和多组分的协同作用在生物、光催化、电化学、传感器、太阳能敏化电池以及锂电储能材料等方面都有广阔的应用前景。纳米多级复合结构由于具有小尺寸和较大的比表面积,可以使合金表面暴露出的反应活性位点增加,同时不同金属之间的电子效应可以导致能带位置发生改变,进而降低反应的活化能,这些为它成为高效催化剂提供了条件。
多级金属复合结构材料多是采用沉淀聚合法、电沉积法、溶剂热法得到的多种金属自组装的规则结构。合成策略中通常要使用功能化的高分子链对核进行保护和修饰。由于纳米材料在催化、能源、磁性、环境、生物及传感器等领域的广泛应用,出于降低成本,减少贵金属使用量,开发高效催化剂的考虑,促进了人们对制备贵金属和非贵金属结合的多级异质纳米材料的研究,如PdCu、Co包覆Pt、Ni包覆Au,由于碳具有优良的电子传导性能,这些金属催化剂通常使用碳材料作为载体,如导电炭黑、石墨烯、碳纳米管等,其难题之一是如何同步合成碳分隔的AgCo纳米颗粒材料。目前纳米合金的合成方法主要有:多元醇法、水热法、电化学沉积法、溶胶-凝胶法、微波辐照法等。
发明内容
本发明的目的是提供一种Fe3O4/FeNi纳米链状复合材料的制备方法。
为了实现上述目的,本发明的技术方案如下:
本发明提出的一种Fe3O4/FeNi纳米链状复合材料的制备方法,具体步骤如下:将Fe2(C2O4)3∙5H2O的水溶液和Ni(CH3COO)2∙4H2O的乙二醇溶液溶于乙二醇中,常温条件下超声处理,然后转移至反应釜中加热保温,反应结束,冷却至室温,得到中间产物,真空干燥,将其放进管式炉中,通入氮气气体保护,在300~500℃温度下退火,并保温3小时,得Fe3O4/FeNi纳米链状复合材料;其中:所述Fe2(C2O4)3∙5H2O的水溶液的浓度为0.0075 mol/L,所述Ni(CH3COO)2∙4H2O的乙二醇溶液的浓度为0.03mol/L,所述Fe2(C2O4)3∙5H2O的水溶液与所述Ni(CH3COO)2∙4H2O的乙二醇溶液的体积比为4:1。
本发明中,所述超声处理时间为10分钟。
本发明中,所述管式炉升温速率为3℃/min。
本发明中,所述中间产品在真空干燥前进行预处理,具体步骤为:首先分别用去离子水和乙醇洗涤产物各2次,然后以5000 rpm的转速下离心分离出沉淀,弃去离心液,直到离心液无色澄清,收集所需产物。
由于采用上述方案,本发明具有以下有益效果:
1、本发明实现了利用常见的铁盐和镍盐为前驱体,通过溶剂热法和退火首次制备出Fe3O4/FeNi纳米链状复合材料。
2、本发明采用简单无机盐作为反应物,具有很强的通用性。
3、本发明制备的产物对芳香硝基化合物具有良好的降解能力,可以作为高性能催化剂,有较为广阔的发展前景和应用空间。
4、本发明的工艺简单,制备条件通用,产物形貌稳定、纯度高,且产物处理方便简洁,适合于中等规模工业生产。
5、本发明所采用的原材料易得,不需要催化剂和模板,价格低廉。
附图说明
图1为实施例1中在300nm的倍数下得到的Fe3O4/FeNi纳米棒SEM照片。
图2为实施例1中在30nm的倍数下得到的Fe3O4/FeNi纳米棒TEM照片。
图3为实施例1中得到的Fe3O4/FeNi纳米棒HRTEM照片,插图为Fe3O4/FeNi纳米棒的电子衍射图谱。
图4为实施例1中在300nm倍数下得到的Fe3O4/FeNi纳米链状复合材料SEM照片。
图5为实施例1中在50nm倍数下得到的Fe3O4/FeNi纳米链状复合材料SEM照片。
图6为实施例1中在200nm的倍数下得到的Fe3O4/FeNi纳米链状复合材料TEM照片
图7为实施例1中在30nm的倍数下得到的单根Fe3O4/FeNi纳米链状复合材料TEM照片。
图8为实施例1中得到的Fe3O4/FeNi纳米链复合材料HRTEM照片,插图为Fe3O4/FeNi纳米链的电子衍射图谱。
图9为实施例1中Fe3O4/FeNi纳米棒(a)和Fe3O4/FeNi纳米链状复合材料(b)产物的XRD图谱。
图10为实施例1中Fe3O4/FeNi纳米棒(a)和Fe3O4/FeNi纳米链状复合材料(b)产物的EDS图谱。
图11为实施例2中所得Fe3O4/FeNi复合材料的SEM图。
图12为实施例3中所得Fe3O4/FeNi纳米链状复合材料的SEM图。
具体实施方式
下面结合附图所示实施例对本发明作进一步详细的说明。
实施例1
第一步:反应釜用王水浸泡过夜后,再盛满蒸馏水,加热至60℃下保温2 h。然后用蒸馏水清洗,晾干备用;
第二步:准确称取0.87375 g的Fe2(C2O4)3∙5H2O置于烧杯中,加入100 mL去离子水,充分搅拌使其溶解,然后转移至250mL容量瓶中,配置成0.0075 mol/L Fe2(C2O4)3∙5H2O水溶液;
第三步:准确称取0.37326g的Ni(CH3COO)2∙4H2O置于烧杯中,加入10 mL乙二醇,充分搅拌使其溶解,然后转移至50mL容量瓶中,配置成0.03mol/L Ni(CH3COO)2∙4H2O乙二醇溶液;
第四步:准确量取2.4 mL Fe2(C2O4)3∙5H2O水溶液和0.6mLNi(CH3COO)2∙4H2O加入到35mL的聚四氟乙烯反应釜中,再加入18 mL乙二醇。超声10 min后装入釜套,然后在电热恒温鼓风干燥箱中以1℃/min的升温速率升至180℃保温12 h;
第五步:将聚四氟乙烯的反应釜内的灰黑色沉淀转移至离心管中,分别用去离子水和乙醇各洗涤2次,以5000rpm的转速下离心分离出沉淀,弃去离心液;直到离心液无色澄清,收集所需产物。将新制得的产物在真空干燥箱中干燥成粉末,密封存于样品管中;该中间产物如图1~3所示,图1为实施例1中在300nm的倍数下得到的Fe3O4/FeNi纳米棒SEM照片,由图可以看出溶剂热法合成出分散性良好的Fe3O4/FeNi纳米棒,Fe3O4/FeNi纳米棒的平均直径为150nm;图2为实施例1中在30nm的倍数下得到的单根Fe3O4/FeNi纳米棒TEM照片; 图3为实施例1中得到的Fe3O4/FeNi纳米棒HRTEM照片, 插图为Fe3O4/FeNi纳米棒的电子衍射图谱,由图2~3可以得出合成的材料为镶嵌式结构,镶嵌的粒子为Fe3O4粒子,粒子直径约15nm,表明Fe3O4/FeNi纳米棒为非晶态纳米合金和Fe3O4组成的复合物。
第六步:取第五步得到的Fe3O4/FeNi纳米棒于瓷舟中,将其一并置于管式炉中,先通入氮气排尽管式炉中的空气,然后再以3℃/min的升温速率升至400℃保温3h,降温至室温,整个过程在氮气气氛保护下。
第七步,将瓷舟取出,收集产物,将其密封存于样品管中。
产物的形貌图如图4~10所示,图4为实施例1中在300nm的倍数下得到的多根Fe3O4/FeNi纳米链的SEM照片,Fe3O4/FeNi纳米链平均直径为100nm;图5为实施例1中在50nm的倍数下得到的Fe3O4/FeNi纳米链的SEM照片;图6为实施例1中在200nm的倍数下得到的Fe3O4/FeNi纳米链的TEM照片;图7为实施例1中在30nm的倍数下得到的单根Fe3O4/FeNi纳米链的TEM照片;图8为实施例1中得到的Fe3O4/FeNi纳米链HRTEM照片,插图为Fe3O4/FeNi纳米链的电子衍射图谱图,证明了Fe3O4/FeNi纳米链由晶态FeNi合金和Fe3O4组成,说明退火将非晶态FeNi合金成分转变成晶态的FeNi合金;图9为实施例1中Fe3O4/FeNi纳米棒(a)和Fe3O4/FeNi纳米链(b)产物的XRD图谱,该图谱分别与电子衍射图相对应,证明了产物的组成成分;图10为实施例1中Fe3O4/FeNi纳米棒(a)和Fe3O4/FeNi纳米链(b)产物的EDS图谱。
实施例2
第一步:反应釜用王水浸泡过夜后,再盛满蒸馏水,加热至60℃下保温2 h。然后用蒸馏水清洗,晾干备用;
第二步:准确称取0.87375 g的Fe2(C2O4)3∙5H2O置于烧杯中,加入100 mL去离子水,充分搅拌使其溶解,然后转移至250mL容量瓶中,配置成0.0075 mol/L Fe2(C2O4)3∙5H2O水溶液;
第三步:准确称取0.37326g的Ni(CH3COO)2∙4H2O置于烧杯中,加入10 mL乙二醇,充分搅拌使其溶解,然后转移至50mL容量瓶中,配置成0.03 mol/L Ni(CH3COO)2∙4H2O乙二醇溶液;
第四步:准确量取2.4 mL Fe2(C2O4)3∙5H2O水溶液和0.6mLNi(CH3COO)2∙4H2O加入到35mL的聚四氟乙烯反应釜中,再加入18 mL乙二醇。超声10 min后装入釜套,然后在电热恒温鼓风干燥箱中以1℃/min的升温速率升至180℃保温12 h;
第五步:将聚四氟乙烯的反应釜内的灰黑色沉淀转移至离心管中,分别用去离子水和乙醇各洗涤2次,以5000rpm的转速下离心分离出沉淀,弃去离心液;直到离心液无色澄清,收集所需产物。将新制得的产物在真空干燥箱中干燥成粉末,密封存于样品管中。
第六步:取第五步得到的Fe3O4/FeNi纳米棒于瓷舟中,将其一并置于管式炉中,先通入氮气排尽管式炉中的空气,然后再以3℃/min的升温速率升至300℃保温3h,降温至室温,整个过程在氮气气氛保护下。
第七步, 将瓷舟取出,收集产物,将其密封存于样品管中。
图11为实施例2中所得产物的SEM图,表明当管式炉中退火保温温度降低到300度时,Fe3O4/FeNi纳米棒表面无明显变化,未形成Fe3O4/FeNi纳米链。
实施例3
第一步:反应釜用王水浸泡过夜后,再盛满蒸馏水,加热至60℃下保温2 h。然后用蒸馏水清洗,晾干备用;
第二步:准确称取0.87375 g的Fe2(C2O4)3∙5H2O置于烧杯中,加入100 mL去离子水,充分搅拌使其溶解,然后转移至250mL容量瓶中,配置成0.0075 mol/L Fe2(C2O4)3∙5H2O水溶液;
第三步:准确称取0.37326g的Ni(CH3COO)2∙4H2O置于烧杯中,加入10 mL乙二醇,充分搅拌使其溶解,然后转移至50mL容量瓶中,配置成0.03 mol/L Ni(CH3COO)2∙4H2O乙二醇溶液;
第四步:准确量取2.4 mL Fe2(C2O4)3∙5H2O水溶液和0.6mLNi(CH3COO)2∙4H2O加入到35mL的聚四氟乙烯反应釜中,再加入18 mL乙二醇。超声10 min后装入釜套,然后在电热恒温鼓风干燥箱中以1℃/min的升温速率升至180℃保温12 h;
第五步:将聚四氟乙烯的反应釜内的灰黑色沉淀转移至离心管中,分别用去离子水和乙醇各洗涤2次,以5000rpm的转速下离心分离出沉淀,弃去离心液;直到离心液无色澄清,收集所需产物。将新制得的产物在真空干燥箱中干燥成粉末,密封存于样品管中。
第六步:取第五步得到的Fe3O4/FeNi纳米棒于瓷舟中,将其一并置于管式炉中,先通入氮气排尽管式炉中的空气,然后再以3℃/min的升温速率升至500℃保温3h,降温至室温,整个过程在氮气气氛保护下。
第七步, 将瓷舟取出,收集产物,将其密封存于样品管中。
图12为实施例3中所得产物的SEM图,表明当管式炉中退火保温温度升高到500度时,Fe3O4/FeNi纳米棒表面发生明显变化,相对实施例1所得的材料,本实施例形成的Fe3O4/FeNi纳米链中所含粒子平均尺寸更大。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改,并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此,本发明不限于这里的实施例,在不脱离本发明的范畴的情况下所做出的修改都在本发明的保护范围之内。
Claims (4)
1.一种Fe3O4/FeNi纳米链状复合材料的制备方法,其特征在于具体步骤如下:将Fe2(C2O4)3∙5H2O的水溶液和Ni(CH3COO)2∙4H2O的乙二醇溶液溶于乙二醇中,常温条件下超声处理,然后转移至反应釜中加热保温,反应结束,冷却至室温,得到中间产物,真空干燥,将其放进管式炉中,通入氮气气体保护,在300~500℃温度下退火,并保温3小时,得Fe3O4/FeNi纳米链状复合材料;其中:所述Fe2(C2O4)3∙5H2O的水溶液的浓度为0.0075 mol/L,所述Ni(CH3COO)2∙4H2O的乙二醇溶液的浓度为0.03mol/L,所述Fe2(C2O4)3∙5H2O的水溶液与所述Ni(CH3COO)2∙4H2O的乙二醇溶液的体积比为4:1。
2.根据权利要求1所述的Fe3O4/FeNi纳米链状复合材料的制备方法,其特征在于:所述超声处理时间为10分钟。
3.根据权利要求1所述的Fe3O4/FeNi纳米链状复合材料的制备方法,其特征在于:所述管式炉升温速率为3℃/min。
4.根据权利要求1所述的Fe3O4/FeNi纳米链状复合材料的制备方法,其特征在于:所述中间产物在真空干燥前进行预处理,具体步骤为:首先分别用去离子水和乙醇洗涤产物各2次,然后以5000 rpm的转速下离心分离出沉淀,弃去离心液,直到离心液无色澄清,收集所需产物。
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