CN101830515B - 一种制备四氧化三铁纳米片的方法 - Google Patents
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Abstract
本发明公开的制备四氧化三铁纳米片的方法,步骤包括:将可溶性的亚铁离子盐溶解于去离子水中;将强碱溶解于去离子水中,然后加入表面活性剂;超声条件下将上述两种溶液混合,反应得悬浊液,提取悬浊液中的固相,用蒸馏水和无水乙醇反复洗涤后,120℃下真空干燥,得Fe3O4纳米片。本发明具有反应温度低,工艺简单,生产周期短,成本低的特点,产品纯度高,本发明所得到的纳米片为Fe3O4单相,形貌为二维片状,平均厚度在5nm以下。
Description
技术领域
本发明涉及制备四氧化三铁纳米片的方法。
背景技术
随着科学技术的不断进步,纳米技术取得了不断的发展。纳米材料由于其不同于普通块材的独特性能,越来越受到人们的关注。纳米结构的铁磁性材料由于其广泛的应用,比如作为铁磁流体、先进磁性材料、催化剂原料、高密度磁存储设备和生物医学及生物药学等方面,吸引了很多研究者的兴趣。
Fe3O4具有一定的磁性,在外磁场下能定向移动,粒径小到一定范围之内具有超顺磁性。纳米Fe3O4的用途广泛,在生物医药方面,磁性纳米颗粒被广泛用作抗癌药物载体,能形成一种磁靶向给药系统;用磁性纳米材料制成的磁性微球还可应用于磁性免疫细胞分离,核磁共振造影等方面。表面改性后的纳米Fe3O4粉体,能分散于介质中成为磁性液体;利用纳米Fe3O4的磁性和颜色,可制作磁记录材料,高梯度磁分离器,微波吸收材料以及静电复印显影剂等。片状磁性金属及合金纳米颗粒具有高的饱和磁化强度,同时具有纳米颗粒的小尺寸效应和强的形状各向异性,可以得到非常广泛的应用。
Fe3O4纳米颗粒的制备方法可以分为物理法和化学法。物理法一般采用物理粉碎法、机械球磨法等,但是产品一般厚度分布不均匀,易被氧化,很难制备出5nm以下的纳米片状颗粒。化学法主要包括共沉淀法、溶胶-凝胶法、微乳液法、水热法等,但一般包括的步骤工艺较多,生产周期较长。在较低的温度下,以较低的能耗和制备周期获得Fe3O4纳米片能够明显降低产品成本,本发明提供了一种在较低温度下快速制备片状Fe3O4纳米颗粒的方法,具有生产周期短,成本低,颗粒一维尺寸小的特点。
发明内容
本发明的目的是提供一种工艺简单,生产成本低,生产周期短的四氧化三铁纳米片的方法。
本发明的制备四氧化三铁纳米片的方法,其特征包括以下步骤:
1)搅拌下,将可溶性亚铁盐和去离子水配制成Fe2+摩尔浓度为0.01~0.5mol/L的水溶液;
2)将强碱试剂加入去离子水中,充分搅拌,配制成OH-摩尔浓度为0.02~1.2mol/L的水溶液,溶液中OH-与步骤1)中Fe2+摩尔比为1~5;然后,向搅拌着的强碱水溶液中加入表面活性剂,表面活性剂与步骤1)中亚铁盐的质量比为1~5;
3)用超声波处理器处理步骤2)混合溶液的同时,将步骤1)中的水溶液逐滴地加入到步骤2)的混合溶液中,滴加完后,继续超声波处理0.5~2小时,得悬浊液,控制超声波功率在80~240W,频率在20~40KHz范围内;
4)用滤纸过滤出步骤3)悬浊液中的固相,用蒸馏水和无水乙醇反复洗涤,并在120℃以下真空干燥,即得四氧化三铁纳米片。
本发明中对可溶性的亚铁离子盐没有特殊要求,只要完全溶解于水中能得到Fe2+的化合物都符合要求。可溶性的Fe2+化合物可以是FeSO4或FeCl2。
上述的强碱试剂可以选择LiOH、NaOH和KOH中的一种或混合物。表面活性剂可以是醋酸钠、聚乙烯吡烙烷酮、油酸钠、聚乙二醇、丙烯酸钠和油酸中的任意一种或几种。
本发明制备步骤2)中,优选OH-与步骤1)中Fe2+的摩尔比为2。
本发明制备四氧化三铁纳米片具有以下优点:
(1)制备四氧化三铁的原料成本低廉,工艺简单。
(2)制备温度低,能耗少,制备周期短,产品成本低。
(3)所得到的纳米片为Fe3O4单相,成品厚度保持在5nm以下。
附图说明
图1实施例1的Fe3O4的TEM照片
图2实施例2的Fe3O4的TEM照片。
具体实施方式
实施例1
1)搅拌下,将2.3353g FeSO4·7H2O和120mL去离子水充分混合;
2)将0.64g NaOH试剂加入80mL去离子水中,充分搅拌使其完全溶解,然后,向搅拌着的强碱水溶液中加入6.89g醋酸钠;
3)用超声波处理器处理步骤2)混合溶液的同时,将步骤1)中的水溶液逐滴地加入到步骤2)的混合溶液中,滴加完后,继续超声波反应1小时,得悬浊液,超声波功率控制在80W,频率在25KHz;
4)用滤纸过滤出步骤3)悬浊液中的固相,用蒸馏水和无水乙醇分别洗涤四次,并在60℃下真空干燥,即得四氧化三铁纳米片。形貌如图1所示,为二维片状,平均厚度在5nm以下。
实施例2
1)搅拌下,将1.6701g FeCl2·4H2O和120mL去离子水充分混合;
2)将0.7093g KOH试剂加入80mL去离子水中,充分搅拌使其完全溶解,然后,向搅拌着的强碱水溶液中加入3.3402g聚乙烯吡烙烷酮;
3)用超声波处理器处理步骤2)混合溶液的同时,将步骤1)中的水溶液逐滴地加入到步骤2)的混合溶液中,滴加完后,继续超声波反应0.5小时,得悬浊液,超声波功率控制在120W,频率在25KHz;
4)用滤纸过滤出步骤3)悬浊液中的固相,用蒸馏水和无水乙醇分别洗涤四次,并在100℃下真空干燥,即得四氧化三铁纳米片。形貌如图2所示,为二维片状,平均厚度在5nm以下。
Claims (4)
1.一种制备四氧化三铁纳米片的方法,包括以下步骤:
1)搅拌下,将可溶性亚铁盐和去离子水配制成Fe2+摩尔浓度为0.01~0.5mol/L的水溶液;
2)将强碱试剂加入去离子水中,充分搅拌,配制成OH-摩尔浓度为0.02~1.2mol/L的水溶液,溶液中OH-与步骤1)中Fe2+摩尔比为1~5;然后,向搅拌着的强碱水溶液中加入表面活性剂,表面活性剂与步骤1)中亚铁盐的质量比为1~5;
3)用超声波处理器处理步骤2)混合溶液的同时,将步骤1)中的水溶液逐滴地加入到步骤2)的混合溶液中,滴加完后,继续超声波处理0.5~2小时,得悬浊液,控制超声波功率在80~240W,频率在20~40KHz范围内;
4)用滤纸过滤出步骤3)悬浊液中的固相,用蒸馏水和无水乙醇反复洗涤,并在120℃以下真空干燥,即得四氧化三铁纳米片。
2.根据权利要求1所述的制备四氧化三铁纳米片的方法,其特征在于所述的可溶性亚铁盐是FeSO4和FeCl2。
3.根据权利要求1所述的制备四氧化三铁纳米片的方法,其特征在于所述的强碱试剂选择LiOH、NaOH和KOH中的一种或混合物。
4.根据权利要求1所述的制备四氧化三铁纳米片的方法,其特征在于所述的表面活性剂是醋酸钠、聚乙烯吡咯烷酮、油酸钠、聚乙二醇、丙烯酸钠和油酸中的任意一种或几种。
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US20080299047A1 (en) * | 2003-07-31 | 2008-12-04 | National Cheng Kung University | Method for preparation of water-soluble and dispersed iron oxide nanoparticles and application thereof |
CN1557725A (zh) * | 2004-01-13 | 2004-12-29 | 上海大学 | 纳米四氧化三铁的制造方法 |
US20060141149A1 (en) * | 2004-12-29 | 2006-06-29 | Industrial Technology Research Institute | Method for forming superparamagnetic nanoparticles |
CN101113022A (zh) * | 2007-07-06 | 2008-01-30 | 哈尔滨工业大学 | 壳聚糖水凝胶诱导原位合成超顺磁性纳米四氧化三铁颗粒 |
CN101423258A (zh) * | 2008-11-25 | 2009-05-06 | 江苏大学 | 液相化学氧化法制备反尖晶石四氧化三铁纳米片 |
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