CN105905949B - 一种磁性Fe3O4/Fe2O3复合纳米棒的制备方法 - Google Patents
一种磁性Fe3O4/Fe2O3复合纳米棒的制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 239000002073 nanorod Substances 0.000 title claims abstract description 42
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000001354 calcination Methods 0.000 claims abstract description 23
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 31
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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Abstract
本发明属于一维或准一维无机非金属纳米磁性复合材料制备领域技术,具体涉及一种磁性Fe3O4/Fe2O3复合纳米棒的简捷制备方法,本发明以硝酸铁和无水乙醇为原料,且2mmol硝酸铁对应无水乙醇的量为1mL,搅拌溶解制得前驱体溶液,将前驱体溶液在空气中点火燃烧制得凝,将凝胶在升温速率为0.5‑15℃/min条件下,150‑400℃煅烧0.1‑10h,自然冷却至室温即可得磁性Fe3O4/Fe2O3复合纳米棒。本发明制备方法简单、快捷、方便,原料丰富,成本低,设备要求不高,产品形貌均匀。
Description
技术领域
本发明涉及一种磁性Fe3O4/Fe2O3复合纳米棒的简捷制备方法,属于一维或准一维无机非金属纳米复合材料制备技术领域。
背景技术
作为一种环境友好的磁性纳米材料,氧化铁纳米材料具有很多独特的物理化学性质,能在环境条件下稳定存在,这些独特的性质使其被广泛应用于电极材料、催化剂、传感器、磁共振成像等多个领域。由于其成本低,环保,生物相容性好,在生物体中表现出无毒或低毒的特性,因此,氧化铁纳米材料在生物医药领域也得到了广泛的应用,如用于基因和药物传递载体、细胞分离、DNA萃取、热疗等等。
一维或准一维纳米材料对材料科学的研究发挥着重要的作用,并且因其各种各样的应用成为一类很有前景的理想纳米材料。在过去的几十年里,一维纳米结构材料,如纳米棒、纳米管、纳米纤维、纳米片等等,因其独特的特性及其在各个领域广泛的实际应用引起了大量科研人员的兴趣和研究。
目前,关于磁性Fe3O4/Fe2O3复合纳米棒制备的报道很少,虽已有文献资料报道单一成分的Fe2O3纳米棒的制备,但这些方法耗时都较长,且因成分的影响产品的饱和磁化强度较小。当然,有文献(J.Magn.Magn.Mater.,2004,272-276: 1776-1777)报道,将Fe2O3在95%氩气和5%氢气氛围中350℃还原0.5-6h,之后在氦气保护下1100℃煅烧3h,制得磁性Fe3O4/Fe2O3纳米复合颗粒,其制备过程复杂,工艺控制难度大,使用氢气还原,操作控制要求较高,对设备的要求也很高,以确保气体不会泄露,且若操作不当还会带来安全隐患;同时,使用稀有气体保护,污染环境,制备成本高;若采用上述两种方法进行工艺制备磁性Fe3O4/Fe2O3复合纳米棒,工艺过程复杂且不经济,生产安全性不高。
发明内容
发明目的:为解决现有技术中存在的技术问题,本发明一种磁性Fe3O4/Fe2O3复合纳米棒的制备方法,简化了工艺操作程序,生产周期短,真正实现了简捷安全快速生产的优势。
技术方案:为实现上述技术目的,本发明提出一种磁性Fe3O4/Fe2O3复合纳米棒的制备方法,包括如下步骤:
(1)将硝酸铁溶于无水乙醇中,搅拌至完全溶解,制得前驱体溶液;
(2)将前驱体溶液直接点火燃烧至火自然熄灭,制得其凝胶;
(3)将凝胶置于程序控温炉中,升温并保温煅烧,热处理后自然冷却至室温得磁性Fe3O4/Fe2O3复合纳米棒。
优选地,步骤(1)中,硝酸铁和无水乙醇的用量为每2mmol硝酸铁对应无水乙醇的量为1mL。
优选地,步骤(3)中,所述保温煅烧的条件为:煅烧温度150-400℃,升温速率为0.5-15℃/min。
优选地,步骤(3)中,所述保温煅烧时间为0.1-10h。
有益效果:与现有技术相比,本发明首次采用溶液燃烧—凝胶煅烧法制备出磁性Fe2O3/Fe3O4纳米棒。采用本方法制备磁性Fe2O3/Fe3O4纳米棒,只需要硝酸铁和无水乙醇为原料,原料种类少,具有过程易控制,装置和工艺简单,无还原过程,操作方便,成本低,无污染,所需设备要求不高,制备周期短,煅烧温度低,产品形貌均匀、收率高,制备时间短等优点,可通过控制前驱体溶液中无水乙醇与硝酸铁的比例以及煅烧的机制有效地控制目标产物的组成、微观结构和性能。
附图说明
图1为实施例1制备的磁性Fe3O4/Fe2O3复合纳米棒的扫描电镜照片,图中标尺大小为100nm;
图2为实施例1制备的磁性Fe3O4/Fe2O3复合纳米棒的透射电镜照片全景图,图中标尺大小为100nm;
图3为实施例1制备的磁性Fe3O4/Fe2O3复合纳米棒的透射电镜照片放大图,图中标尺大小为20nm;
图4为实施例1制备的磁性Fe3O4/Fe2O3复合纳米棒的X射线衍射谱与Fe2O3标准PDF卡片(JCPDS No.33-0664)和Fe3O4标准PDF卡片(JCPDS No.03-0863) 对比图;
图5为实施例1制备的磁性Fe3O4/Fe2O3复合纳米棒的X射线能谱图;
图6为实施例1制备的磁性Fe3O4/Fe2O3复合纳米棒的磁滞回线图。
具体实施方式
下面结合具体实施例和附图内容对本发明作进一步的阐述,以使本领域技术人员更好的理解本发明的技术方案。
实施例1磁性Fe3O4/Fe2O3复合纳米棒的制备。
向15mL无水乙醇中加入12.12g硝酸铁,磁力搅拌溶解2h制得前驱体溶液,将溶液置于坩埚中,点火燃烧,待到火尽,得到凝胶,将凝胶置于程序控温炉中,以10.0℃/min的升温速率升温至250℃,在250℃下保温煅烧0.1h,自然冷却至室温后取出,研磨得磁性Fe3O4/Fe2O3复合纳米棒。
图1~3为本实施例制备的磁性Fe3O4/Fe2O3复合纳米棒的扫描电镜照片、透射电镜照片全景图和透射电镜照片放大图,从电镜图可以看出,磁性Fe3O4/Fe2O3复合纳米棒平均直径约10nm,长度约为50nm。
图4为本实施例所述条件下制备的磁性Fe3O4/Fe2O3复合纳米棒的X射线衍射谱与Fe2O3标准PDF卡片(JCPDS No.33-0664)和Fe3O4标准PDF卡片(JCPDS No.03-0863)对比图;从图中可以看出,产物的绝大部分衍射峰位置和Fe2O3标准PDF卡片衍射峰位置对应,在30°和43°衍射角度上出现了Fe3O4特征衍射峰,表明了Fe3O4成分的存在;同时,磁性Fe2O3/Fe3O4复合纳米棒在33°和35.6°两个衍射角度处的衍射峰比例明显比标准Fe2O3的衍射强度比例小,说明了33.5°处存在Fe3O4的衍射峰。
图5为本实施例所述条件下制备的磁性Fe3O4/Fe2O3复合纳米棒的X射线能谱图。从其EDX图可以看到所得磁性Fe3O4/Fe2O3复合纳米棒元素比例。
图6为本实施例所述条件下制备的磁性Fe3O4/Fe2O3复合纳米棒的磁滞回线图;其磁滞回线显示,磁性Fe3O4/Fe2O3复合纳米棒具有典型的软磁特性,其饱和磁化强度高达142.6Am2/kg。
实施例2磁性Fe3O4/Fe2O3复合纳米棒的制备。
向10mL无水乙醇中加入8.08g硝酸铁,磁力搅拌溶解2h制得前驱体溶液,将溶液置于坩埚中,点火燃烧,待到火尽,得到凝胶,将得到的凝胶置于程序控温炉中,以3.0℃/min的升温速率升温至400℃,在400℃下保温煅烧2h,自然冷却至室温后取出,研磨得磁性Fe3O4/Fe2O3复合纳米棒。制备的磁性 Fe3O4/Fe2O3复合纳米棒的饱和磁化强度高达99.3Am2/kg。
实施例3
向20mL无水乙醇中加入16.16g硝酸铁,磁力搅拌溶解4h制得前驱体溶液,将溶液置于坩埚中,点火燃烧,待到火尽,得到凝胶,将凝胶置于程序控温炉中,以0.5℃/min的升温速率升温至150℃,在150℃下保温煅烧10h,自然冷却至室温后取出,研磨得磁性Fe3O4/Fe2O3复合纳米棒。制备的磁性Fe3O4/Fe2O3复合纳米棒的饱和磁化强度高达90.8Am2/kg。
实施例4
向30mL无水乙醇中加入24.24g硝酸铁,磁力搅拌溶解5h制得前驱体溶液,将溶液置于坩埚中,点火燃烧,待到火尽,得到凝胶,将凝胶置于程序控温炉中,以1.0℃/min的升温速率升温至200℃,在200℃下保温煅烧8h,自然冷却至室温后取出,研磨得磁性Fe3O4/Fe2O3复合纳米棒。制备的磁性Fe3O4/Fe2O3复合纳米棒的饱和磁化强度高达111.5Am2/kg。
实施例5
向20mL无水乙醇中加入16.16g硝酸铁,磁力搅拌溶解4h制得前驱体溶液,将溶液置于坩埚中,点火燃烧,待到火尽,得到凝胶,将凝胶置于程序控温炉中,以5.0℃/min的升温速率升温至300℃,在300℃下保温煅烧1h,自然冷却至室温后取出,研磨得磁性Fe3O4/Fe2O3复合纳米棒。制备的磁性Fe3O4/Fe2O3复合纳米棒的饱和磁化强度高达129.4Am2/kg。
实施例6
向15mL无水乙醇中加入12.10g硝酸铁,磁力搅拌溶解3h制得前驱体溶液,将溶液置于坩埚中,点火燃烧,待到火尽,得到凝胶,将凝胶置于程序控温炉中,以1.0℃/min的升温速率升温至250℃,在250℃下保温煅烧0.5h,自然冷却至室温后取出,研磨得磁性Fe3O4/Fe2O3复合纳米棒。制备的磁性Fe3O4/Fe2O3复合纳米棒的饱和磁化强度高达141.0Am2/kg。
实施例7
向10mL无水乙醇中加入8.08g硝酸铁,磁力搅拌溶解2h制得前驱体溶液,将溶液置于坩埚中,点火燃烧,待到火尽,得到凝胶,将凝胶置于程序控温炉中,以15.0℃/min的升温速率升温至350℃,在350℃下保温煅烧5h,自然冷却至室温后取出,研磨得磁性Fe3O4/Fe2O3复合纳米棒。制备的磁性Fe3O4/Fe2O3复合纳米棒的饱和磁化强度高达120.3Am2/kg。
本发明首次采用溶液燃烧一凝胶煅烧法制备出磁性Fe2O3/Fe3O4纳米棒。采用本方法制备磁性Fe2O3/Fe3O4纳米棒,只需要硝酸铁和无水乙醇为原料,原料种类少,具有过程易控制,装置和工艺简单,无还原过程,操作方便,成本低,无污染,所需设备要求不高,制备周期短,煅烧温度低,产品形貌均匀、收率高,制备时间短等优点,可通过控制煅烧的机制有效地控制目标产物的组成、微观结构和性能。
Claims (3)
1.一种磁性Fe3O4/Fe2O3复合纳米棒的制备方法,其特征在于,包括如下步骤:
(1)将硝酸铁溶于无水乙醇中,搅拌至完全溶解,制得前驱体溶液,其中,硝酸铁和无水乙醇的用量为每2 mmol硝酸铁对应无水乙醇的量为1 mL;
(2)将前驱体溶液直接点火燃烧至火自然熄灭,制得其凝胶;
(3)将凝胶置于程序控温炉中,升温并保温煅烧,热处理后自然冷却至室温得磁性Fe3O4/Fe2O3复合纳米棒。
2.根据权利要求1所述的磁性Fe3O4/Fe2O3复合纳米棒的制备方法,其特征在于,步骤(3)中,所述保温煅烧的条件为:煅烧温度150-400℃,升温速率为0.5-15℃/min。
3. 根据权利要求1所述的磁性Fe3O4/Fe2O3复合纳米棒的制备方法,其特征在于步骤(3)中,所述保温煅烧时间为0.1-10 h。
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