Development and Characterization of Polymer-based Magnetoelectric Nanofibers

With the rapid development of bionics, where biological systems meet electronics, there is an interest in polymer-based electrode systems that are soft, flexible, easily processed and fabricated. In this research area, magnetoelectric (ME) composites bring new and exciting opportunities, including contactless or “wireless” electrical stimulation, less-invasive integration in the form of dispersible, injectable nanoelectrodes, and applications as biodegradable sensors and bioenergy harvesters in the biomedical field. When ME composites are exposed to a magnetic field, a magnetostrictive (MS) component transfers strain to a piezoelectric (PE) component that generates an output voltage. In doing so, ME composites have the ability to enable magnetic-to-electrical conversion and thus can be utilized to power devices or electrically stimulate tissues or cells from a remote magnetic stimulus. To date, ceramic materials have mostly been applied in nanostructured ME composites, however, these may become fragile and cause deleterious reactions at the interface regions, leading to low electrical resistivity and high dielectric losses and ultimately low output voltage. To overcome these shortcomings, polymer-based ME composites offer new solutions to develop softer, contactless electrodes, without electrical connections, for easier and unique fabrication approaches (e.g. incorporation into soft gels). Their strain-mediated ME effect in large scale devices has been thoroughly studied both experimentally and theoretically. Polymer-based ME composites have almost exclusively used the PE polymer, poly (vinylidene fluoride) (PVDF), due to its high PE coefficient and as such developments in exploring other types of PE polymers have not been forthcoming. For example, other PE polymers such as poly (vinylidene fluoride-co-hexafluoropropylene) (P(VDF-HFP)) and poly (lactic acid) (PLA) have yet to be investigated though have the potential to bring added-value and function to polymer-based ME composites. Compared to PVDF and its copolymer P(VDF-TrFE), the piezoelectricity of another copolymer, P(VDF-HFP), is less-well understood. As a biocompatible polymer, PLA has been extensively investigated for applications in drug delivery and tissue engineering. Instead of being used only as a biodegradable and bioactive thermoplastic material, PLA is promising as a PE polymer, which has potential to mimic PE functions of tissues. Thus, in addition to PVDF, the thesis investigates the PE properties of P(VDF-HFP) and PLA and aims to develop ME composite nanofibers based on these polymers

Untersuchung von Magnetostriktiven und Piezotronischen Mikrostrukturen und Materialien für biomagnetische Sensoren mittels Röntgenstrahlen

Detecting electric potential differences from the human physiology is an established technique in medical diagnosis, e.g., as electrocardiogram. It arises from a changing electrical polarization of living cells. Simultaneously, biomagnetism is induced and can be utilized for medical examinations, as well. Benefits in using magnetic signals are, no need for direct skin contact and an increased spatial resolution, e.g., for mapping brain activity, especially in combination with electrical examinations. But biomagnetic signals are very weak and, thus, highly sensitive devices are necessary. The development of small and easy to use biomagnetic sensors, with a sufficient sensitivity, is the goal of the Collaborative Research Centre 1261 - Magnetoelectric Sensors: From Composite Materials to Biomagnetic Diagnostics. This thesis was written as part of this collaboration, with the main focus on the investigation of crystalline structures and structure related properties of piezotronic and magnetostrictive materials by utilizing a selection of X-ray techniques, i.e., X-ray diffraction (XRD), X-ray reflectivity (XRR) and coherent X-ray diffraction imaging (CXDI). Piezotronics, realized by combining piezoelectricity and Schottky contacts in one structure, provides a promising path to enhance sensor sensitivity. A first study investigated the crystalline structure of three piezotronic ZnO rods, spatially resolved by scanning nano XRD and combined with electrical examinations of their Schottky contact properties. It is found that the crystalline quality has a clear impact on the electrical properties of the related Schottky contact, probably due to crystalline defects. A complementary transmission electron microscopy (TEM) and XRD study performed on hybride vapor phase epitaxy (HVPE) grown GaN showed a slight, photoelectrochemical etching related relaxion of strain originating from crystal growth. In a separate study, CXDI was utilized for three-dimensional visualization of strain in a gold coated ZnO rod, with spatial resolution below 30 nm. A distinct strain distribution was found inside the rod, denoted to depletion and screening effects occurring in bent piezotronic structures, and a high strain at the interface may be related to Schottky contact formation. This interface strain agrees with results obtained from TEM. A succeeding CXDI study was conducted on a ZnO rod coated with magnetostrictive FeCoSiB and the possibility for the investigation of the Schottky contacts electrical properties. It was found that FeCoSiB sputtered on ZnO results in an ohmic contact and that an external magnetic field causes a change of the electrical properties, probably due to a strain change, visualized by CXDI. In a fifth study, magnetostrictive FeCo/TiN multilayer structures were investigated by a combined TEM and XRD/XRR approach, showing a relaxation of the structure due to an annealing process and a cube-on-cube structure of the FeCo and TiN layers

Methodology of ZnO Based 1D Microstructures : from Synthesis to Application

ZnO is among the most studied materials in the past decades. A large number of synthesis routes and a unique combination of properties offer a wide range of possible applications. This work focuses on the development of applications using 1D ZnO micro- and nanostructures. The development starts with the introduction of a new synthesis process, flame transport synthesis (FTS). The FTS allows the fabrication of various metal oxide micro- and nanostructures. Depending on the used parameter set the structural type can be modified leading to different morphologies, e.g., interconnected net- works, core spike particles or large 1D single crystals. These resulting structures were characterized by state of the art methods to determine their crystalline, electric and piezoelectric properties. X-ray diffraction analysis revealed excellent crystalline properties and the absence of pre-strain in 1D ZnO microrods. TEM investigations showed the existence of twin boundaries in the spikes of core spike particles. Electromechanical measurements were used to demonstrate the pre- strain in ZnO microrods when attached to a plane substrate. Electromechanical measurements inside SEM allowed the precise measurement of the piezoresistive properties of individual ZnO microrods. The hydrophobic and hydrophilic wetting states of ZnO are discussed and a theoretical model is introduced which expands the common wetting theory and explains the wetting of superhydrophobic surfaces. Magnetoelectric sensors based on ZnO microrods are realized and investigated. The new concept of piezotronic measurements is applied for the sensors and is compared to the classical piezoelectric measurement concept. The comparison revealed a lower limit of detection for the piezotronic sensor, which makes it a promising candidate for new applications

Emerging versatile two-dimensional MoSi2_2N4_4 family

The discovery of two-dimensional (2D) layered MoSi$_2$N$_4$ and WSi$_2$N$_4$ without knowing their 3D parents by chemical vapor deposition in 2020 has stimulated extensive studies of 2D MA$_2$Z$_4$ system due to its structural complexity and diversity as well as versatile and intriguing properties. Here, a comprehensive overview on the state-of-the-art progress of this 2D MA$_2$Z$_4$ family is presented. Starting by describing the unique sandwich structural characteristics of the emerging monolayer MA$_2$Z$_4$, we summarize and anatomize their versatile properties including mechanics, piezoelectricity, thermal transport, electronics, optics/optoelectronics, and magnetism. The property tunability via strain engineering, surface functionalization and layered strategy is also elaborated. Theoretical and experimental attempts or advances in applying 2D MA$_2$Z$_4$ to transistors, photocatalysts, batteries and gas sensors are then reviewed to show its prospective applications over a vast territory. We further discuss new opportunities and suggest prospects for this emerging 2D family. The overview is anticipated to guide the further understanding and exploration on 2D MA$_2$Z$_4$.Comment: 29 pages, 21 figure

Investigation of the factors influencing magnetic flux leakage and magnetic Barkhausen noise

Magnetic Nondestructive methods, including Magnetic Flux Leakage (MFL) and Magnetic Barkhausen Noise (MBN), are widely used to evaluate the structural integrity, mechanical properties, and microstructures of ferromagnetic materials. The MFL method is commonly applied to nondestructively evaluate the damage in ferromagnetic materials due to its reliability, high efficiency, and cost-saving. The MBN method is applicable in nondestructive evaluation (NDE) of mechanical and material properties due to the high sensitivity of Barkhausen jumps to residual (or applied) stress and microstructure of ferromagnetic material. The recognized research and successful applications helped these methods to be feasible NDE tools. However, there are still several important factors that may have noticeable influences on the experimental results of these NDE methods and usually are ignored in applications. In this thesis, the effects of the factors of stress and temperature on the MFL method, as well as the influences of temperature and microstructure on the MBN method are analysed via analytical and numerical modelling. A new finite element model for evaluating the effect of stress on the MFL amplitude is proposed and validated in defective steel under various stresses. Moreover, the new models describing the direct effect of temperature and the combined effects of temperature and thermal stress on the MFL signals are presented. The direct and combined effects are verified in an environmental temperature range from -40℃ to 60℃ by experimental results of a single lamination steel and multilayer structure, respectively. A set of newly derived equations modelling the effect of temperature on the MBN signals are given. Both the direct effect of temperature and the combined effects of temperature and thermal stress are considered in these equations, which are further simplified to linear functions consistent with the measured results in an environmental temperature range from -40℃ to 40℃. Furthermore, the microstructure factors, including the microstructure induced anisotropy in non-oriented silicon steel and the metallographic phases changing with carbon content in steel, are theoretically and experimentally investigated, respectively. For the factor of anisotropy, a new model II describing the dependency of Barkhausen emission on the angle between measurement and rolling directions is proposed. It allows the deduction of a trigonometric function to evaluate the effect of directional anisotropy. The agreement of simulated and measured results of MBN signals indicates the feasibility of the presented model. In the investigation of the influence of carbon content in steel on MBN signals, an optimisation method for MBN pick-up coil is proposed, and a multifunctional measurement system is presented. The correlations of the MBN signals and hysteresis loops related to the carbon content in steel are experimentally observed. The method for the quantitative evaluation of the carbon content using MBN signals and hysteresis loops are discusse

DEVELOPMENT OF A NOVEL Z-AXIS PRECISION POSITIONING STAGE WITH MILLIMETER TRAVEL RANGE BASED ON A LINEAR PIEZOELECTRIC MOTOR

Piezoelectric-based positioners are incorporated into stereotaxic devices for microsurgery, scanning tunneling microscopes for the manipulation of atomic and molecular-scale structures, nanomanipulator systems for cell microinjection and machine tools for semiconductor-based manufacturing. Although several precision positioning systems have been developed for planar motion, most are not suitable to provide long travel range with large load capacity in vertical axis because of their weights, size, design and embedded actuators. This thesis develops a novel positioner which is being developed specifically for vertical axis motion based on a piezoworm arrangement in flexure frames. An improved estimation of the stiffness for Normally Clamped (NC) clamp is presented. Analytical calculations and finite element analysis are used to optimize the design of the lifting platform as well as the piezoworm actuator to provide maximum thrust force while maintaining a compact size. To make a stage frame more compact, the actuator is integrated into the stage body. The complementary clamps and the amplified piezoelectric actuators based extenders are designed such that no power is needed to maintain a fixed vertical position, holding the payload against the force of gravity. The design is extended to a piezoworm stage prototype and validated through several tests. Experiments on the prototype stage show that it is capable of a speed of 5.4 mm/s, a force capacity of 8 N and can travel over 16 mm

Micro motion amplification – A Review

Many motion-active materials have recently emerged, with new methods of integration into actuator components and systems-on-chip. Along with established microprocessors, interconnectivity capabilities and emerging powering methods, they offer a unique opportunity for the development of interactive millimeter and micrometer scale systems with combined sensing and actuating capabilities. The amplification of nanoscale material motion to a functional range is a key requirement for motion interaction and practical applications, including medical micro-robotics, micro-vehicles and micro-motion energy harvesting. Motion amplification concepts include various types of leverage, flextensional mechanisms, unimorphs, micro-walking /micro-motor systems, and structural resonance. A review of the research state-of-art and product availability shows that the available mechanisms offer a motion gain in the range of 10. The limiting factor is the aspect ratio of the moving structure that is achievable in the microscale. Flexures offer high gains because they allow the application of input displacement in the close vicinity of an effective pivotal point. They also involve simple and monolithic fabrication methods allowing combination of multiple amplification stages. Currently, commercially available motion amplifiers can provide strokes as high as 2% of their size. The combination of high-force piezoelectric stacks or unimorph beams with compliant structure optimization methods is expected to make available a new class of high-performance motion translators for microsystems

Stress monitoring of cylindrical structures using guided waves

This thesis presents some approaches for guided wave based stress monitoring as a part of Structural Health Monitoring (SHM). SHM systems include different levels, from damage detection to prognosis, however, this work is focused on detection and on an estimation of the actual stress. The proposed stress monitoring strategies are based on different statistical and signal processing approaches such as Principal Component Analysis and Residuals. These techniques are applied on signals of elastic guided waves generated and sensed via Piezoelectrical (PZT) or Magnetostrictive transducers. Transducer devices are chosen in this work to generate longitudinal, flexural and torsional guided waves in cylindrical specimens, since their high performance, low energy consumption, weight and reasonable price. In order to guarantee the efficacy of the proposed techniques, they are tested in laboratory by emulating real installations and abnormal conditions. Experimental tests revealed that temperature and bonding layer between the PZT and the specimen influence on the performance of the monitoring scheme by changes in the guided wave propagation. Thus, the temperature effect on guided wave propagation was examined by checking the sensitivity of the PCA-based proposed approach. Then, a temperature compensation strategy is applied to improve stability and robustness of the scheme for structures subjected temperature changes. On the other hand, since the acoustoelasticity effect is predominant in the propagation of stressed guided waves, it was observed its incidence on the dispersion curves by using a SAFE method (Semi-Analytical Finite Element) to generate stressed dispersion curves via Effective Elastic Constants (EEC). Finally, as a consequence of some observations in the experimentation stage, it is proposed a scheme for monitoring the supports rigidity in pipelines based on a guided waves energy leakage perspective. The proposed approaches may promise the ability and capability of being implemented in different fields such as aerospace and gas/oil industry.En esta tesis se presentan algunos enfoques para el monitoreo de esfuerzos usando ondas guiadas como parte de un sistema de evaluación de integridad. Estos sistemas incluyen diferentes niveles de monitoreo que van desde la detección de daños hasta su predicción; sin embargo este trabajo se enfoca solo en la detección y estimación de un valor probable de esfuerzo. La estrategia de monitoreo propuesta se basa en diferentes enfoques estadísticos y de procesamiento de señales tales como Análisis de Componentes Principales y Residuos. Estas técnicas se aplican en señales que corresponden a ondas guiadas generadas por transductores piezoelectricos (PZT) o magnetostrictivos. Estos elementos tienen la capacidad de generar ondas guiadas longitudinales, de flexión y torsionales en especímenes cilíndricos, con alto desempeño, bajo consumo de energía, bajo peso y a un costo razonable. Para garantizar la efectividad de las técnicas propuestas, estas se prueban en laboratorio emulando una instalación real y bajo condiciones anormales de esfuerzo. Los resultados experimentales revelaron que la temperatura de los alrededores y la capa adhesiva entre el piezoelectrico y el espécimen influyen en el desempeño del esquema de monitoreo debido a los cambios que se producen en la propagación de onda . Por lo tanto, se estudia el efecto desde una perspectiva analítica el efecto de la temperatura en la propagación de la onda guiada y en consecuencia en el desempeño del enfoque de monitoreo propuesto. Basado en lo anterior, se aplica una estrategia de compensación del efecto de la temperatura para mejorar la estabilidad y la robustez del esquema propuesto ante escenarios de cambios de temperatura. Por otro lado, debido a que el efecto predominante en la propagación de ondas guiadas bajo esfuerzo es el efecto acoustoelastico, se estudia su influencia en las curvas de dispersión usando un método semi-analitico basado en elementos finitos (SAFE del inglés) en combinación con las Constantes Elásticas Efectivas (EEC del inglés) para estimar las curvas de dispersión de ondas guiadas bajo esfuerzo. Finalmente, como un resultados de la experimentación, se propone un esquema de monitoreo de rigidez de soportes de tubería cilíndrica basado en un perspectiva de energía de ultrasonido transferida al entorno vía contacto de superficies. El enfoque propuesto puede ser extendido al monitoreo de rigidez o contacto en otros sistemas en campos tales como el aeroespacial y en la industria del Gas/Petróle