摘要
近年来,随着纳米科学技术的发展,一维纳米材料由于其独特的物理和化学性质而在基础研究和技术应用等方面得到人们的广泛关注。磁性纳米纤维和纳米线状材料具有高的长径比、大的比表面积、显著的形状各向异性等一系列优点而备受研究者的青睐。目前制备纳米纤维的方法有许多种,比如：AAO模板法、水热法、相分离法等,虽然这些方法已经能够制备出形貌和磁性良好的磁性纳米纤维,但是它们存在操纵复杂、原料成本高、难以工业化大规模生产的缺点。静电纺丝技术是近年来制备纳米纤维材料的一种新颖方法,它的实验设备和制作工艺简单,能适用于多种聚合物和复合物溶液,制备的纤维直径可在微米和纳米之间调节。
静电纺丝技术已经在组织工程学、生物医学、纺织、能源、环境保护等领域有了实际应用,但是在制备磁性纳米纤维方面研究的较少。本论文利用静电纺丝法分别制备了尖晶石铁氧体、六角铁氧体、金属Fe、Ni内米纤维等,并利用XRD进行物相结构分析、SEM和TEM观察微观形貌和成分、VSM测量静态磁性、SQUID研究高场下的磁性能、矢量网络分析仪进行高频磁性研究。在此基础上系统研究了工艺参数对铁氧体和金属纳米纤维的晶体结构和磁性质的影响,找到了具有较大矫顽力和形状各向异性的制备参数。本论文的主要工作包括以下几个方面：
1、系统地研究了升温速率对CoFe204内米纤维的形貌和晶体结构的影响,发现低的升温速率是保持良好纤维状形貌的关键条件,高的升温速率则会导致纤维形貌破坏,本论文中的升温速率都保持在1-2℃/min。
2、烧结温度会影响磁性纳米纤维的晶体结构、形貌和磁性质。对于CoFe2O4纳米纤维来说,低于900℃的样品能保持纤维表面光滑、连续直的纤维状形貌；而900和1000℃下烧结的纤维表面变的粗糙且发生了弯曲；500℃时样品的矫顽力最大：Hc=773Oe。对于永磁SrFe12O19纳米纤维来说,700℃时样品的矫顽力最大：Hc=5508Oe。这是由于低温下晶粒较小,组成纳米纤维的颗粒表现为单畴结构,随着烧结温度的升高,磁性材料晶粒长大,其畴结构从单畴变为多畴而导致矫顽力降低。
3、系统地研究了Zn2+离子掺杂对CuFe2O4纳米纤维的微观结构、形貌和磁性质的影响,其晶格结构从反尖晶石型向正尖晶石型转变。Zn2+离子掺杂明显改善了CuFe2O4(?)内米纤维的形貌,使其纤维表面光滑和致密化。系统研究了Cu2+离子掺杂对NiFe2O4纳米纤维的微观结构、形貌和磁性质的影响。两种离子掺杂对磁性质的影响都是由于A、B位金属离子种类和数量的改变而导致A-B间超交换作用的改变。对CU0.6Zn0.4Fe2O4纳米纤维,磁场方向平行和垂直于样品表面测量的磁滞回线表明其磁性易轴沿着纤维的长轴方向；而通过对退磁能和形状各向异性场的计算以及系列Cu1-xZnxtFe2O4纳米纤维的穆斯堡尔谱的研究发现,有效各向异性并没有完全沿着纳米纤维的长轴方向,这一结果是由于组成纳米纤维的小颗粒间有偶极相互作用导致的。
4、利用静电纺丝法成功制备出Fe3O4(?)内米纤维,并系统地研究了还原条件对Fe3O4(?)内米纤维晶体结构和形貌的影响。制备出的Fe3O4纳米纤维具有高的矫顽力,HC=188.4Oe;这来自纳米纤维高的长径比导致的形状各向异性。用叉指电极测量了Fe3O4纳米纤维在室温和低温下的磁电阻,导电机理来自组成纳米纤维的临近颗粒间的隧穿。
5、利用静电纺丝法成功制备出具有高磁晶各向异性的FePt(?)内米纤维,在磁晶各向异性和形状各向异性的共同作用下得到高的矫顽力：Hc＝10.27kOe。在Ni纳米纤维的磁导率-频率曲线上观察到两个共振峰,分别是4.0GHz和12.5GHz。第一个共振峰是自然共振峰,通过Kittel公式推算出这个共振峰来自形状各向异性的贡献；第二个共振峰主要归因于交换共振。在匹配厚度为8.4mm、匹配频率为1.3GHz时得到最小的RL值：RL=-35.4dB。
Recently, with the rapid development of nanoscale science and technology, one-dimensional nanomaterials have been paid much attention because of their distinctive physical and chemical properties in basic scientific research and potential technology applications. Magnetic nanofibers-like or nanowires-like materials have attracted a great deal of interest due to their advantages of high aspect ratio, large surface area and remarkable shape anisotropy. There are several methods to prepare nanofibers, such as AAO template, hydrothermal method, phase separation, etc. Although these methods have been able to prepare magnetic nanofibers with good morphology and magnetic properties, there are some disadvantages, such as manipulation complex, high cost of raw materials, difficult of industrial mass production. Electrospinning is a simple and versatile technique for generating a rich variety of nanofibers made of polymers and composites, the diameter of nanofibers can be controlled form micro-to nano scales.
The electrospinning method has been applied in many fields, such as tissue engineering, biomedical, spinning, energy, environmental protection. However, only a little attention is paid to the application of magnetic nanofibers prepared by electrospinning. In this paper, spinel ferrite, hexagonal ferrite, metal Fe and Ni nanofibers were fabricated by electrospinning. The phase strucure, morphology, composition, magnetic properties of static and high field, high frequency characteristics were investigated by XRD, SEM, TEM, VSM and vector network analyzer, and the effect of process parameters on crystal structure and magnetic properties was studied.
1. The effect of heating rate on morphology and crystal structure of CoFe2O4naofibers was systematically studied. The results show that low heating rate is a key condition for maintaining good fibrous morphology, however, a destroyed ones is attributed to higher heating rate. All heating rate retain at1-2℃/min in this article.
2. Sintering temperature can affect the crystal structure, morphology and magnetic properties of magnetic nanofibers. For CoFe2O4naofibers, the morphology changes from a smooth surface and continuous straight fibers when sintering temperature is lower than900℃to a rough surface and winding ones when the sintering temperature increases to900and1000℃; the nanofibers calcined at500℃has the largest coercivity value, Hc=772.8Oe. For permanent magnets SrFe12O19nanofibers, the ones calcined at700℃has the largest coercivity value, Hc=5508Oe. This is attributed to single domain for magnetic nanofibers calcined at lower temperature. With the sintering temperature increasing, the magnetic crystal will grow and the domain structure will transform from a single domain to a multi domain state.
3. The effects of Zn2+and Cu2+ions substitution on crystal structure, morphology and magnetic properties of CuFe2O4and NiFe2O4nanofiber were systematically studied, and the lattice structure changes from inverse spinel structure to normal spinel structure, or changes from inverse spinel structure to the other inverse ones. Zn2+ions substitution significantly improves the morphology of CuFe2O4nanofibers. The surface of Cu1-xZnxFe2O4with x greater than0clearly becomes smoother and denser. The effects of Zn2+and Cu2+ions substitution on magnetic properties are due to the change of species and quantity of metal ions on A and B sites, which results in the change of super-exchange interaction between A and B sites. For Cu0.6Zn0.4Fe2O4nanofibers, hystersis loops of the nanofibers measured with magnetic field parallel and perpendicular to sample plane exhibit that the magnetic easy axis along the long axis of the nanofibers. However, it is found that the shape anisotropy of nanofibers is not domination the effective anisotropy according to results of calculation for the demagnetization energy and effective anisotropy field. In other words, the easy magnetization direction is not perfectly along the long axis of the nanofibers, which is evidenced by Mossbauer spectra of Cu1-xZnxFe2O4samples. This is due to the dipolar interaction between nanoparticles of which the nanofibers are composed.
4. Fe3O4nanofbers were fabricated by electrospinning, and the effect of reduction conditions on the crystal structure and morphology of Fe3O4nanofbers is systematically studied. The obtained Fe3O4nanofbers have a high coercivity,Hc=188.4Oe, which is attributed to the shape anisotropy come from the high aspect ratio of nanofibers samples. The magnetoresistances (MR) at room and low temperatures of Fe3O4nanofbers were measured by interdigitated electrodes, and the conductive mechanism is explained in terms of the tunneling of adjacent grain boundary.
5. High magnetocrystalline anisotropy FePt nanofibers were fabricated by electrospinning, and the high coercivity is attributed to the combined interaction of magnetocrystalline anisotropy and shape anisotropy, Hc=10.27kOe. The double-resonance behavior of microwave magnetic permeabiligy is observed,4.0GHz and12.5GHz. The natural resonance peak happens at4.0GHz for the contribution of shape anisotropy according to Kittel formula projections, and the second resonance peak originates from exchange resonance effect. A minimum RL reaches-35.4dB at the matching thickness of8.4mm and the matching frequency of1.3GHz.
引文
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