摘要
铁电材料具有自发极化强度,其极化方向在外加电场的作用下可以在两个稳态之间翻转,基于这一机理的铁电存储器已得到了商业化的应用。本论文主要对在高密度存储领域有应用潜力的无机铁电材料铁酸铋和适用于低成本RFID存储的有机铁电材料偏二氟乙烯-三氟乙烯共聚物P(VDF-TrFE)进行了薄膜制备和性能研究。针对两种材料在应用中的问题,一方面研究如何提高由薄膜应力导致的具有高度择优取向的铁酸铋薄膜的极化保持性能,另一方面研究如何提高P(VDF-TrFE)有机铁电薄膜存储器的擦写速度,降低擦写电压。本论文主要内容如下：
一、使用脉冲激光沉积系统(PLD)制备了氧空位掺杂的半导体铁酸铋薄膜,使用原子力显微镜对薄膜的电畴结构进行了微观表征,检验薄膜质量。采用分离铁电畴极化翻转电流和薄膜漏电流的方法获得半导体铁电薄膜的电滞回线,并对结果进行分析。主要结果如下：
1、使用脉冲激光沉积和射频磁控溅射方法,制备了平整的氧化物底电极薄膜及不同化学配比的铁酸铋薄膜。原子力显微镜结果显示,在原子级平整的底电极表面生长的铁酸铋薄膜具有矩形规则排列的晶粒。运用原子力显微镜分析了不同组分薄膜的电畴结构及微观的电畴弛豫特性,测量结果与宏观电学性能吻合。
2、对有较大漏电流的半导体铁酸铋薄膜的测量技术进行了研究,通过将铁电薄膜的电畴翻转电流与薄膜漏电流分离并转换为电滞回线的方法,得到了半导体薄膜的矫顽电压及极短时间内的印刻效应和极化保持特性,弥补了以往的测试技术仅能够表征绝缘薄膜的局限性。实验数据证明了该技术测试结果的可靠性,并且发现半导体铁酸铋薄膜的矫顽电场在外加电压增大的情况下基本保持在320kV/cm左右,远高于绝缘薄膜的矫顽电场,证明了半导体薄膜具有与绝缘薄膜不同的电畴翻转机制。
3、为了研究漏电流对铁酸铋薄膜电学性能的影响,解决应力薄膜保持性能较差的科学难题,分别对三种铁含量的薄膜进行了电学测试。提出运用电荷注入机制改善以上薄膜的保持性能的方案,为应力超薄膜在铁电器件中的应用探索出一条新的解决途径。结果表明,在膜厚下降时由应力造成的薄膜内固定电荷形成的退极化电场使得薄膜的极化保持性能(Retention)普遍下降,但是随薄膜中铁含量的增加情况逐渐有所好转。实验中使用的外加负向电压脉冲对薄膜进行电荷注入的方法,可明显改善薄膜的极化保持性能。得出了薄膜漏电流密度的大小可显著影响电荷补偿作用和极化保持性能的结论,证明了通过电荷注入机制来改善薄膜保持性能的科学性。
二、为了提高P(VDF-TrFE)有机铁电薄膜存储器的擦写速度、降低擦写电压。我们采用Spin-coating方法制备了P(VDF-TrFE)薄膜,采用串联等效电容电路模型对薄膜的电畴翻转特性进行了分析,从电畴微观极化翻转过程提出问题的解决方案。主要结果如下：
1、发现P(VDF-TrFE)薄膜较高的矫顽电压很大程度上是薄膜中非铁电相及界面层形成的等效非铁电电容分压的结果。串联等效电容模型的方法可以排除薄膜中非铁电相和界面层的干扰因素,得到薄膜的等效铁电电容和本征的矫顽电压。通过分析不同速度的电畴翻转过程,证明了等效非铁电电容会随测试脉冲频率的增大而减小,从而导致了使用高频电压脉冲测量时薄膜矫顽电压的增大和剩余极化的减小
2、在采用等效电路提取薄膜等效铁电电容的基础上,通过平行板电容器模型在无需求得等效铁电层厚度的情况下得到计算薄膜本征矫顽电场的方法,通过比较不同厚度的P(VDF-TrFE)薄膜本征矫顽电场得到了与理论计算相近的结果。
以上模型能够定量地分析铁电薄膜中非铁电成分的含量及其对薄膜电学性能的影响,解决了现有测试分析手段无法定量表征界面非铁电层电容的困难。
A ferroelectric material exhibits reversible spontaneous polarization in which direction can be switched by an applied electrical field. The switchable polarization in two "up" and "down" states has achieved commercial application in FeRAMs. In this thesis, the ferroelectric thin films of bismuth ferrite and Poly(vinylidene fluoride-trifluoroethylene) were fabricated. The former has a large prospect in the application of high-density memory, and the latter can be used in low-cost RFID chips. To address their obstacle driven by rapidly growing application, we emphasized on the enhancement of retention time of bismuth ferrite thin films with preferred domain orientations and the improvement of writing/reading performance of P(VDF-TrFE) copolymer thin films.
I. The oxygen vacancy-defected bismuth ferrite films deposited by PLD were systematically characterized by atomic force microscopy and pulsed voltage measurement. We can justify the domain switching current from the leakage of the films. The main results are summarized as following.
Firstly, Atomic force microscopy micrograph of bismuth ferrite films with Fe excess deposited on bottom oxide electrodes reveals the flat film surface of square-like grains. Piezoresponse microscope images illuminated the domain polarization relaxation properties of different components of thin film, in consistence with the macroscopic electrical measurements.
Secondly, we developed a technique to transfer ferroelectric domain switching currents under the pulses into polarization-voltage (P-V) hysteresis loops. With this transformation, it is doable to derive the remanent polarization and coercive voltage from domain switching current after the shortest imprint and retention time of35ns. After an identification of domain switching component from film leakage current, we measured the P-V hysteresis loop in a semiconducting BiFeO3leaky thin film, where the apparent coercive field highly reaches320kV/cm, implying a domain switching mechanism different from other insulators.
Thirdly, in order to assess the leakage current effects on the electrical performance of the films and to improve the retention property of highly strained films, three Fe-enriched films were fabricated. Charge injection proved to be an effective way to enhance the retention time, which paves a way to expand the application for ultra-thin films in ferroelectric devices. The results present that the retention worsens when the film thickness decreases due to a strong depolarization field. The field weakens when the Fe content increases. Under a negative field stressing, the polarization was enhanced approaching up to a theoretical value via charge injection, which supplies an effective way to symmetrize the P-E loop of a highly strained ferroelectric thin film.
Ⅱ. In order to improve the writing/reading performance of the devices, the P (VDF-TrFE) films with various thicknesses prepared by spin coating were modeled using the equivalent in-series capacitance to analyze the electrical domain switching current. The main results are presented.
Firstly, the results display the high coercive voltage mainly due to the interfacial layer and non-ferroelectric phase in the P(VDF-TrFE) films. Through an electrical equivalent in-series capacitance circuit, the intrinsic capacitance and coercive voltage can be derived from either domain switching current transient or voltage dependence of the switched polarization. Interestingly, the non-ferroelectric capacitance reduces with the enhancement of domain switching speed while the continuous reduction of the remanent polarization, which suggests the thickening of the preceding capacitive layers with enhanced domain switching speed.
Secondly, on a basis of the equivalent-circuit description of the films and parallel plate capacitor model, we extract the intrinsic coercive field across the ferroelectric layer in the films with unknown thickness of the ferroelectric layer. The derived intrinsic coercive field of different thickness P(VDF-TrFE) thin-films consists with the theoretical prediction reported previously.
The equivalent in-series capacitance model offers an effective way to quantify the non-ferroelectric capacitor of interfacial layers and its effects on the ferroelectric properties of both organic and inorganic ferroelectric thin-films.
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