取向尖晶石基薄膜的层状前驱体法制备及其磁学性能研究
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摘要
尖晶石铁氧体薄膜材料在高密度存储、电磁波吸收、磁共振等领域有着广泛的应用前景。研发简便的薄膜制备方法,控制薄膜材料的组成、结构及形貌,进而提高薄膜的磁学性能,成为该领域研究的热点问题。本论文围绕尖晶石铁氧体薄膜材料的构筑及其磁学性能开展基础研究。针对目前该领域研究中的关键科学问题,采用层状前驱体技术,以层状双羟基复合金属氢氧化物(layered double hydroxides,简称LDHs,又叫类水滑石)薄膜为前驱体材料,经高温焙烧制得系列取向尖晶石基铁氧体薄膜材料。通过LDHs薄膜前驱体的制备参数调变及焙烧过程控制,实现了相关铁氧体薄膜材料的组成、形貌、取向的可控制备。同时,表征了溶剂蒸发组装成膜过程,探讨了LDHs薄膜的成膜驱动力及组装机制。最后,研究测试了取向尖晶石基铁氧体薄膜材料的磁学性能。研究工作可望为尖晶石基铁氧体薄膜材料在结构设计、构筑过程控制、应用性能等方面的深入进行奠定一定的实验基础。
本论文的创新点和研究结果如下：
首先,针对高密度磁存储领域存在的铁磁性纳米粒子“超顺磁限制”这一关键科学问题,以溶剂蒸发制备得到的(00l)取向CoFe-LDHs薄膜为前驱体,在氦气保护下利用LDHs的结构拓扑效应焙烧制备了(111)取向的系列CoFe2O4/CoO纳米复合薄膜。CoFe2O4和CoO界面间强的铁磁／反铁磁相互作用提高了CoFe2O4磁性纳米粒子的热稳定性。与相同粒径的纯相CoFe2O4粒子相比,CoFe2O4/CoO纳米复合薄膜中CoFe2O4粒子的截止温度(TB)提高了100 K以上。同时发现,该薄膜的磁各向异性导致了平行于膜面方向的交换偏置场(HE)的数值大于垂直于膜面条件下的交换偏置场。
然后,以(00l)取向的NiFe-LDHs薄膜为前驱体,首先利用LDHs的结构拓扑效应焙烧制备了(111)取向的NiFe2O4/NiO纳米复合薄膜。然后,采用硝酸溶蚀的方法将此复合薄膜中的NiO去除,得到了多孔的(111)取向NiFe2O4薄膜。其表面粗糙程度可通过焙烧温度及酸溶蚀时间来进行调控。经过表面有机化处理后,多孔NiFe2O4薄膜显示出了良好的超疏水性能。随其表面粗糙程度的增强,薄膜与水的接触角变大。磁性及表面浸润性的可控调节使得该多孔尖晶石基铁氧体薄膜有可能在苛刻的外界环境中获得应用。
此外,基于LDHs薄膜可控制备的重要意义,通过研究表征溶剂蒸发组装过程,探讨了LDHs薄膜的成膜驱动力及组装机制。在不同晶化温度条件下制备了LDHs纳米粒子。TEM、AFM等表征结果表明,随晶化温度升高LDHs纳米粒子的表观形貌由类球形转变为六方片状,其长厚比(aspect ratio)的增加表明LDHs纳米粒子各向异性程度加强。成膜实验显示,长厚比的大小直接影响溶剂蒸发后最终成膜的连续性及粒子(00l)晶面的取向程度。大的长厚比有利于LDHs纳米粒子间面-面相互作用的增强。在所研究的NiFe-LDHs体系中,发现长厚比大于3时能够制得连续完整的LDHs薄膜。
本论文最后还尝试采用了涂覆技术制备LDHs薄膜前驱体,然后经过焙烧处理分别得到了MgFe2O4/MgO和NiFe2O4/NiO复合铁氧体薄膜以及纯相MgFe2O4薄膜。研究表明,上述复合铁氧体薄膜中组分均匀分布,磁性可调；而纯相MgFe2O4薄膜在室温条件下则显示出了优异的“超顺磁”性能。
Spinel ferrite films are an important class of inorganic functional materials. They have potentially been used in many fields such as high density storage, electromagnetic wave absorbing, and magnetic resonance, because of their excellent structural and physicochemical properties. In order to improve the magnetic properties of ferrite films, increasing interest has been paid to regulate the composition, structure and morphologies of ferrite films with simple preparation methods. In the present thesis, our research mainly focuses on the construction of spinel ferrite film materials and the enhancement of corresponding magnetic properties. Oriented spinel type ferrite films have been fabricated through high temperature calcinations process using layered double hydroxides (LDHs) films as precursors. With changing the preparation parameter of LDHs films precursors and controlling the high temperature calcinations process, we have realized controllable preparation of a series of ferrite film materials with different composition, morphology and orientation. Meanwhile, we have also investigated the solvent evaporation process of LDHs nanoparticles and discussed possible driving force in the LDHs film formation process. Finally, magnetic properties of oriented spinel type ferrite films have been investigated in detail. We think our research work may be regarded as some experimental basis for the further study on structural design, building process control and application performance of spinel type ferrite films.
The innovation of this thesis and results are as follows:
First, in order to beat "superparamagnetic limit" of ferromagnetic nanoparticles in high-density storage field, cobalt-iron layered double hydroxides (CoFe-LDHs) film with (00l) orientation has been fabricated through a solvent evaporation method, and (111) oriented CoFe2O4/CoO nanocomposite film formed in a subsequent thermal treatment process in He atmosphere. The resulting product is composed of nano-sized ferromagnetic (FM) CoFe2O4 particles embedded in antiferromagnetic (AFM) CoO matrix. A topotactic transformation from the LDHs precursor film to the CoFe2O4/CoO nanocomposite film was proposed to cause an exchange coupling between the FM CoFe2O4 and AFM CoO phases in the nanocomposite, leading to an enhanced magnetic stability of the CoFe2O4. The blocking temperature of CoFe2O4 nanoparticles in CoFe2O4/CoO nanocomposite film increased more than 100 k than that for pure CoFe2O4 nanoparticles with similar size. Furthermore, the orientation of the CoFe2O4/CoO nanocomposite film is found to be attributed to the magnetic anisotropy when the magnetic field was applied on different directions.
Then, porous oriented NiFe2O4 films have also been prepared using LDH films as precursors. The process mainly involves the formation of (00l) oriented NiFe-LDH film through solvent evaporation, subsequently topotactic transformation from (00l) oriented NiFe-LDH film to (111) oriented NiFe2O4/NiO composite films induced by high-temperature calcination, followed by selective leaching of NiO sacrificial phase from NiFe2O4/NiO composite films. The surface roughness can be tuned by altering calcined temperature or acid treatment time. With hydrophobic treatment, the as-prepared NiFe2O4 film shows stable superhydrophobicity. Furthermore, surface wettability of NiFe2O4 film can be tuned in a wide range through alteration of the surface roughness. The controllable regulations of magnetism and surface wettability make porous oriented NiFe2O4 films could potentially be used in harsh external environments.
Besides, we discussed the possible driving force for film formation through investigating the assembly process of LDHs nanoparticles during solvent evaporation. LDHs nanoparticles were prepared at different aging temperatures conditions. TEM, AFM were used to characterize the products. With increasing the aging temperature, the morphology of LDHs nanoparticles changes from spherelike to hexagonal platelike. The increased aspect ratio can be used as a direct evidence for the enhancement of anisotropic degree of LDHs nanoparticles. The film formation results exhibit the aspect ratio of LDHs nanoparticles can greatly influence the continuity of LDHs film and orientation of (00l) crystal plane. The high aspect ratios is favor to the enhancement of Surface-to-surface interaction of LDHs nanoparticles. In NiFe-LDHs system, it is easy to obtain large continuous LDHs film when aspect ratio is greater than 3.
Finally, we attempt to prepare LDHs films precursors by coating techniques. MgFe2O4/MgO, NiFe2O4/MgO composite films and pure MgFe2O4 film were obtained after calcinations of corresponding LDHs film precursors. The analysis results show the two phases in the composite films are uniformly interdispersed. At the same time, the magnetization of composite films can be tuned by alterating the M(Ⅱ)/Fe(Ⅲ) molar ratio of LDHS precursors. Moreover, the pure MgFe2O4 film exhibits a promising superparamagnetic behavior under room temperature condition.
本论文的创新点和研究结果如下：
首先,针对高密度磁存储领域存在的铁磁性纳米粒子“超顺磁限制”这一关键科学问题,以溶剂蒸发制备得到的(00l)取向CoFe-LDHs薄膜为前驱体,在氦气保护下利用LDHs的结构拓扑效应焙烧制备了(111)取向的系列CoFe2O4/CoO纳米复合薄膜。CoFe2O4和CoO界面间强的铁磁／反铁磁相互作用提高了CoFe2O4磁性纳米粒子的热稳定性。与相同粒径的纯相CoFe2O4粒子相比,CoFe2O4/CoO纳米复合薄膜中CoFe2O4粒子的截止温度(TB)提高了100 K以上。同时发现,该薄膜的磁各向异性导致了平行于膜面方向的交换偏置场(HE)的数值大于垂直于膜面条件下的交换偏置场。
然后,以(00l)取向的NiFe-LDHs薄膜为前驱体,首先利用LDHs的结构拓扑效应焙烧制备了(111)取向的NiFe2O4/NiO纳米复合薄膜。然后,采用硝酸溶蚀的方法将此复合薄膜中的NiO去除,得到了多孔的(111)取向NiFe2O4薄膜。其表面粗糙程度可通过焙烧温度及酸溶蚀时间来进行调控。经过表面有机化处理后,多孔NiFe2O4薄膜显示出了良好的超疏水性能。随其表面粗糙程度的增强,薄膜与水的接触角变大。磁性及表面浸润性的可控调节使得该多孔尖晶石基铁氧体薄膜有可能在苛刻的外界环境中获得应用。
此外,基于LDHs薄膜可控制备的重要意义,通过研究表征溶剂蒸发组装过程,探讨了LDHs薄膜的成膜驱动力及组装机制。在不同晶化温度条件下制备了LDHs纳米粒子。TEM、AFM等表征结果表明,随晶化温度升高LDHs纳米粒子的表观形貌由类球形转变为六方片状,其长厚比(aspect ratio)的增加表明LDHs纳米粒子各向异性程度加强。成膜实验显示,长厚比的大小直接影响溶剂蒸发后最终成膜的连续性及粒子(00l)晶面的取向程度。大的长厚比有利于LDHs纳米粒子间面-面相互作用的增强。在所研究的NiFe-LDHs体系中,发现长厚比大于3时能够制得连续完整的LDHs薄膜。
本论文最后还尝试采用了涂覆技术制备LDHs薄膜前驱体,然后经过焙烧处理分别得到了MgFe2O4/MgO和NiFe2O4/NiO复合铁氧体薄膜以及纯相MgFe2O4薄膜。研究表明,上述复合铁氧体薄膜中组分均匀分布,磁性可调；而纯相MgFe2O4薄膜在室温条件下则显示出了优异的“超顺磁”性能。
Spinel ferrite films are an important class of inorganic functional materials. They have potentially been used in many fields such as high density storage, electromagnetic wave absorbing, and magnetic resonance, because of their excellent structural and physicochemical properties. In order to improve the magnetic properties of ferrite films, increasing interest has been paid to regulate the composition, structure and morphologies of ferrite films with simple preparation methods. In the present thesis, our research mainly focuses on the construction of spinel ferrite film materials and the enhancement of corresponding magnetic properties. Oriented spinel type ferrite films have been fabricated through high temperature calcinations process using layered double hydroxides (LDHs) films as precursors. With changing the preparation parameter of LDHs films precursors and controlling the high temperature calcinations process, we have realized controllable preparation of a series of ferrite film materials with different composition, morphology and orientation. Meanwhile, we have also investigated the solvent evaporation process of LDHs nanoparticles and discussed possible driving force in the LDHs film formation process. Finally, magnetic properties of oriented spinel type ferrite films have been investigated in detail. We think our research work may be regarded as some experimental basis for the further study on structural design, building process control and application performance of spinel type ferrite films.
The innovation of this thesis and results are as follows:
First, in order to beat "superparamagnetic limit" of ferromagnetic nanoparticles in high-density storage field, cobalt-iron layered double hydroxides (CoFe-LDHs) film with (00l) orientation has been fabricated through a solvent evaporation method, and (111) oriented CoFe2O4/CoO nanocomposite film formed in a subsequent thermal treatment process in He atmosphere. The resulting product is composed of nano-sized ferromagnetic (FM) CoFe2O4 particles embedded in antiferromagnetic (AFM) CoO matrix. A topotactic transformation from the LDHs precursor film to the CoFe2O4/CoO nanocomposite film was proposed to cause an exchange coupling between the FM CoFe2O4 and AFM CoO phases in the nanocomposite, leading to an enhanced magnetic stability of the CoFe2O4. The blocking temperature of CoFe2O4 nanoparticles in CoFe2O4/CoO nanocomposite film increased more than 100 k than that for pure CoFe2O4 nanoparticles with similar size. Furthermore, the orientation of the CoFe2O4/CoO nanocomposite film is found to be attributed to the magnetic anisotropy when the magnetic field was applied on different directions.
Then, porous oriented NiFe2O4 films have also been prepared using LDH films as precursors. The process mainly involves the formation of (00l) oriented NiFe-LDH film through solvent evaporation, subsequently topotactic transformation from (00l) oriented NiFe-LDH film to (111) oriented NiFe2O4/NiO composite films induced by high-temperature calcination, followed by selective leaching of NiO sacrificial phase from NiFe2O4/NiO composite films. The surface roughness can be tuned by altering calcined temperature or acid treatment time. With hydrophobic treatment, the as-prepared NiFe2O4 film shows stable superhydrophobicity. Furthermore, surface wettability of NiFe2O4 film can be tuned in a wide range through alteration of the surface roughness. The controllable regulations of magnetism and surface wettability make porous oriented NiFe2O4 films could potentially be used in harsh external environments.
Besides, we discussed the possible driving force for film formation through investigating the assembly process of LDHs nanoparticles during solvent evaporation. LDHs nanoparticles were prepared at different aging temperatures conditions. TEM, AFM were used to characterize the products. With increasing the aging temperature, the morphology of LDHs nanoparticles changes from spherelike to hexagonal platelike. The increased aspect ratio can be used as a direct evidence for the enhancement of anisotropic degree of LDHs nanoparticles. The film formation results exhibit the aspect ratio of LDHs nanoparticles can greatly influence the continuity of LDHs film and orientation of (00l) crystal plane. The high aspect ratios is favor to the enhancement of Surface-to-surface interaction of LDHs nanoparticles. In NiFe-LDHs system, it is easy to obtain large continuous LDHs film when aspect ratio is greater than 3.
Finally, we attempt to prepare LDHs films precursors by coating techniques. MgFe2O4/MgO, NiFe2O4/MgO composite films and pure MgFe2O4 film were obtained after calcinations of corresponding LDHs film precursors. The analysis results show the two phases in the composite films are uniformly interdispersed. At the same time, the magnetization of composite films can be tuned by alterating the M(Ⅱ)/Fe(Ⅲ) molar ratio of LDHS precursors. Moreover, the pure MgFe2O4 film exhibits a promising superparamagnetic behavior under room temperature condition.
引文
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