CN108439486A - 一种形貌可控的Fe3O4纳米材料的制备方法 - Google Patents
一种形貌可控的Fe3O4纳米材料的制备方法 Download PDFInfo
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 20
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Abstract
本发明公开了一种形貌可控的Fe3O4纳米材料的制备方法,属于纳米功能材料技术领域。本发明针对现有的Fe3O4纳米材料在制备特殊形貌的方法中需要加入表面活性剂等方面的不足,提供了一种通过尿素控制的自组装制备方法,通过尿素的加入比例和回流反应的时间可以可控得制备纳米粒子、纳米片与纳米花之间的连续形貌,颗粒尺寸为1~3.5μm,分散性好,溶于水中即可分散;具有良好磁性性能,在室温下,无磁滞现象,无剩磁,无矫顽磁场,饱和磁化强度为60‑80emu/g,使用普通磁铁即可分离,在常温下表现出超顺磁性。
Description
技术领域
本发明属于纳米功能材料技术领域,具体涉及一种由纳米粒子过度到纳米花球形貌的Fe3O4的制备方法。
背景技术
磁性纳米材料的小尺寸效应、量子尺寸效应、表面效应等使它具备常规粗晶粒材料所不具备的异常的磁学性质。在信息存储、传感器、磁流体等传统领域已有相当的发展外,靶向给药、生物分离、医疗诊断、DNA分离和检测领域也有较广应用前景,有着巨大的潜在价值。Fe3O4纳米粒子是磁性纳米粒子材料中研究最热的材料,它的基本性质有一下几个方面:制备Fe3O4纳米粒子原材料便宜;Fe3O4的理论自旋极化率为100%,有磁电阻效应;Fe3O4磁性纳米材料对人体没有毒性,在磁场下可方便的操控,可通过人体降解的方式排泄出体外等优点,因此可对人体使用。Fe3O4颗粒作为一种重要的磁性材料,具有合适的饱和磁化强度、电导率和相对合适的介电常数,保证了其作为吸收体的反射系数和衰减性能。此外,磁性Fe3O4材料具有低毒、生物相容性、居里温度高、半金属性质等优点,在增强磁共振成像、药物靶向载体和磁流体等方面有着广泛的应用。
合成粒径均匀、尺寸可控的磁性纳米颗粒在科学和技术上应用都具及其重要意义,所以关于磁性纳米粒子的制备方法也成为近年研究的热点。目前用于制备磁性Fe3O4纳米材料的方法有很多种:共沉淀法、高温分解法、微乳液法、溶胶凝胶法、溶剂热法、球磨法、超声分解法等。
近年来通过对上述方法的研究,Fe3O4纳米材料的制备取得了明显的进步,但也存在着以下几点不足:(1)制备原料复杂,成本较高,不利于产业化发展;(2)添加表面活性剂或有机物,从而导致潜在的与工艺相关的危害或生产效率低下。因此,开发一种经济、无害环境的方法来合成表面形貌可控的无表面活性剂和模板的新型分层结构,仍然是一个巨大的挑战。
发明内容
针对背景技术存在的上述技术问题,本发明提出了一种形貌可控的Fe3O4纳米材料的制备方法,实现由纳米粒子过渡到纳米花球形貌的可控合成,本发明中以FeCl3·6H2O为铁源,尿素为还原剂,利用自组装法来制备Fe3O4纳米材料,操作简单、可控性强。
本发明提出的形貌可控的Fe3O4纳米材料的制备方法,包括如下步骤:
1)将FeCl3·6H2O和乙二醇按照FeCl3·6H2O和乙二醇的质量体积比30:1mg/mL混合,再加入尿素,然后通过搅拌使FeCl3·6H2O和尿素溶解于乙二醇中,得到混合溶液,
2)将上述混合溶液在190~200℃温度范围内回流加热4~10min或20~25min,回流加热过程中继续通入氮气保护,然后冷却至室温;
3)将步骤2)中所得产物采用乙醇离心清洗,得到Fe3O4前驱体;
4)将Fe3O4前驱体在490~510℃煅烧3h,煅烧过程中通入氮气保护,煅烧完成后得到所述形貌可控的Fe3O4纳米材料;
当混合溶液回流时间为4~10min时,所得Fe3O4纳米材料为纳米颗粒,颗粒粒径为20nm。
当混合溶液回流时间为20~25min时,根据FeCl3·6H2O和尿素的摩尔比在4:(3~60)的范围内不同比例分别得到不同形貌的Fe3O4纳米材料,由低到高可依次得到由纳米片、纳米花到纳米花球逐步过渡的形貌,颗粒尺寸为1~3.5μm。
其中,当FeCl3·6H2O和尿素的摩尔比在4:(3~5)时得到Fe3O4纳米材料的颗粒尺寸为3.5μm,形貌为纳米片状。
当FeCl3·6H2O和尿素的摩尔比在4:(10~12)时得到Fe3O4纳米材料的颗粒尺寸为2.5μm,形貌为纳米类花状。
当FeCl3·6H2O和尿素的摩尔比在4:(17~19)时得到Fe3O4纳米材料的颗粒尺寸为2.5μm,形貌为纳米花状。
当FeCl3·6H2O和尿素的摩尔比在4:(58~60)时得到Fe3O4纳米材料的颗粒尺寸为1μm,形貌为纳米花球状。
当FeCl3·6H2O和尿素的摩尔比在以上范围之间时或的为两种形貌之间的过渡形貌。
回流时间中间10~20min之间可获得纳米粒子与纳米花之间的过渡形貌。
优选地,步骤2)中的回流温度为195℃。
优选地,步骤4)中的煅烧温度为500℃
本发明方法具有以下优点和积极效果:
1)本发明提供了一种制备Fe3O4纳米材料的方法。该方法以氯化铁和尿素为起始原料,制备过程中无任何表面活性剂的添加,且所需生产设备简单,成本低,易于实现工业化生产的Fe3O4纳米花;
2)本发明通过对自组装法中尿素的控制,实现合成Fe3O4从纳米粒子到纳米花,再到纳米花球的变化。相对于以前报道的合成类似的纳米复合结构,本发明所制备的Fe3O4纳米材料,形貌可控,分散性好,溶于水中即可分散;
3)本发明的Fe3O4纳米材料具有良好磁性性能,在室温下,无磁滞现象,无剩磁,无矫顽磁场,饱和磁化强度为60-80emu/g,使用普通磁铁即可分离,在常温下表现出超顺磁性;
4)本发明所制备的Fe3O4纳米材料为多孔结构,有较高的比表面积,易于其它材料的负载;
5)本发明所制备的Fe3O4纳米材料磁性强,本发明方法简单,成本低,重复性好,可用于大规模制备。
附图说明
图1是本发明实施例1中合成的Fe3O4纳米粒子的SEM图像;
图2是本发明实施例2合成的Fe3O4纳米片的SEM图像;
图3是本发明实施例3合成的Fe3O4纳米类花的SEM图像
图4是本发明实施例4合成的Fe3O4纳米花的SEM图像;
图5是本发明实施例5合成的Fe3O4纳米花球的SEM图像;
图6是本发明合成的Fe3O4前驱体的XRD谱图;
图7是本发明合成的Fe3O4纳米材料的XRD谱图;
图8是本发明实施例4合成的Fe3O4纳米花的VSM谱图;
具体实施方式
下面通过具体实施例对本发明的技术方案进行详细说明。
实施例1
FeCl3·6H2O和乙二醇置于烧杯内,FeCl3·6H2O和乙二醇的质量体积比(mg/mL)30:1,再加入尿素,FeCl3·6H2O和尿素的摩尔比为(mol)4:17,然后机械搅拌烧杯中的混合物使上述原料混合均匀,倒入三颈烧瓶中回流加热,回流加热的温度为195℃,回流加热的时间为5min,回流加热过程中继续通入氮气,然后冷却至室温,采用乙醇离心清洗,得到Fe3O4前驱体。图1是本发明在回流加热的时间为5min时得到的Fe3O4前驱体的SEM图像。最后将前驱体纳米片放在高温炉中煅烧,温度在500℃保持3h,并通入氮气保护。
最终产物为尺寸为20nm的Fe3O4纳米粒子,产物形貌如图1所示,饱和磁化强度为69emu/g,剩磁、矫顽力近似为零。
实施例2
FeCl3·6H2O和乙二醇置于烧杯内,FeCl3·6H2O和乙二醇的质量体积比(mg/mL)30:1,再加入尿素,FeCl3·6H2O和尿素的摩尔比为(mol)4:3,然后机械搅拌烧杯中的混合物使上述原料混合均匀,倒入三颈烧瓶中回流加热,回流加热的温度为195℃,回流加热的时间为20min,回流加热过程中继续通入氮气,然后冷却至室温,采用乙醇离心清洗,得到Fe3O4前驱体纳米片。最后将前驱体纳米片放在高温炉中煅烧,温度在500℃保持3h,并通入氮气保护。
最终产物为尺寸为3.5μm的Fe3O4纳米片,产物形貌如图2所示,饱和磁化强度为70emu/g,剩磁、矫顽力近似为零。
实施例3
本实施例与实施例2的不同之处在于,FeCl3·6H2O和尿素的摩尔比为(mol)4:11,其余与实施例2相同。
最终产物为尺寸为2.5μm的Fe3O4纳米类花状颗粒,产物形貌如图3所示,饱和磁化强度为73emu/g,剩磁、矫顽力近似为零。
实施例4
本实施例与实施例2的不同之处在于,FeCl3·6H2O和尿素的摩尔比为(mol)4:17,其余与实施例2相同。
最终产物为尺寸为2.5μm的Fe3O4纳米花,产物形貌如图4所示,饱和磁化强度为72emu/g,剩磁、矫顽力近似为零。
实施例5
本实施例与实施例2的不同之处在于,FeCl3·6H2O和尿素的摩尔比为(mol)4:59,其余与实施例2相同。
最终产物为尺寸为1μm的Fe3O4纳米花球,产物形貌如图5所示,饱和磁化强度为65emu/g,剩磁、矫顽力近似为零。
图6是本发明在FeCl3·6H2O和尿素的摩尔比为(mol)4:17,回流加热时间为20min时得到的Fe3O4纳米花前驱体的XRD谱图,图7是本发明得到的Fe3O4纳米材料的XRD谱,从本发明所得样品的XRD图谱可以看到,样品为纯相Fe3O4,无任何杂质。
图8是本发明得到的Fe3O4纳米花的VSM谱图,从本发明所制得样品的磁滞回线可以看到,样品具有亚铁磁性,并且有较高的饱和磁化强度。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种形貌可控的Fe3O4纳米材料的制备方法,包括如下步骤:
1)将FeCl3·6H2O和乙二醇按照FeCl3·6H2O和乙二醇的质量体积比30:1mg/mL混合,再加入尿素,然后通过搅拌使FeCl3·6H2O和尿素溶解于乙二醇中,得到混合溶液,
2)将上述混合溶液在190~200℃温度范围内回流加热4~25min,回流加热过程中继续通入氮气保护,然后冷却至室温;
3)将步骤2)中所得产物采用乙醇离心清洗,得到Fe3O4前驱体;
4)将Fe3O4前驱体在490~510℃煅烧3h,煅烧过程中通入氮气保护,煅烧完成后得到所述形貌可控的Fe3O4纳米材料;
其中,当混合溶液回流时间为4~10min时,所得Fe3O4纳米材料为纳米颗粒,颗粒粒径为20nm;
当混合溶液回流时间为20~25min时,根据FeCl3·6H2O和尿素的摩尔比在4:(3~60)的范围内不同比例分别得到不同形貌的Fe3O4纳米材料,由低到高可依次得到由纳米片、纳米花到纳米花球逐步过渡的形貌,颗粒尺寸为1~3.5μm。
2.根据权利要求1所述的形貌可控的Fe3O4纳米材料的制备方法,其特征在于,当FeCl3·6H2O和尿素的摩尔比在4:(3~5)时得到Fe3O4纳米材料的颗粒尺寸为3.5μm,形貌为纳米片状。
3.根据权利要求1所述的形貌可控的Fe3O4纳米材料的制备方法,其特征在于,当FeCl3·6H2O和尿素的摩尔比在4:(10~12)时得到Fe3O4纳米材料的颗粒尺寸为2.5μm,形貌为纳米类花状。
4.根据权利要求1所述的形貌可控的Fe3O4纳米材料的制备方法,其特征在于,当FeCl3·6H2O和尿素的摩尔比在4:(17~19)时得到Fe3O4纳米材料的颗粒尺寸为2.5μm,形貌为纳米花状。
5.根据权利要求1所述的形貌可控的Fe3O4纳米材料的制备方法,其特征在于,当FeCl3·6H2O和尿素的摩尔比在4:(58~60)时得到Fe3O4纳米材料的颗粒尺寸为1μm,形貌为纳米花球状。
6.根据权利要求1~5中任意一项所述的形貌可控的Fe3O4纳米材料的制备方法,其特征在于,步骤2)中的回流温度为195℃。
7.根据权利要求1~5中任意一项所述的形貌可控的Fe3O4纳米材料的制备方法,其特征在于,步骤4)中的煅烧温度为500℃。
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CN115028206A (zh) * | 2022-06-21 | 2022-09-09 | 中海石油(中国)有限公司 | 一种Janus二维磁性纳米颗粒及其制备方法与应用 |
CN115028206B (zh) * | 2022-06-21 | 2023-10-31 | 中海石油(中国)有限公司 | 一种Janus二维磁性纳米颗粒及其制备方法与应用 |
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