Sub-100 nanosecond temporally resolved imaging with the Medipix3 direct electron detector

Detector developments are currently enabling new capabilities in the field of transmission electron microscopy (TEM). We have investigated the limits of a hybrid pixel detector, Medipix3, to record dynamic, time varying, electron signals. Operating with an energy of 60keV, we have utilised electrostatic deflection to oscillate electron beam position on the detector. Adopting a pump-probe imaging strategy we have demonstrated that temporal resolutions three orders of magnitude smaller than are available for typically used TEM imaging detectors are possible. Our experiments have shown that energy deposition of the primary electrons in the hybrid pixel detector limits the overall temporal resolution. Through adjustment of user specifiable thresholds or the use of charge summing mode, we have obtained images composed from summing 10,000s frames containing single electron events to achieve temporal resolution less than 100ns. We propose that this capability can be directly applied to studying repeatable material dynamic processes but also to implement low-dose imaging schemes in scanning transmission electron microscopy.Comment: 11 pages, 6 figures; improve ref formatting + revise tex

Measurement of the nonlinear refractive index (n2) and stimulated Raman scattering in optical fibers as a function of germania content, using the photorefractive beam coupling technique

One of the greatest challenges in optical communication is the understanding and control of optical fiber nonlinearities. While these nonlinearites limit the power handling capacity of optical fibers and can cause noise, signal distortion and cross talk in optically amplified transmission systems, they have been equally harnessed for the development of new generations of optical amplifiers and tunable laser sources. The two prominent parameters that characterize the nonlinear properties of an optical fiber are the nonlinear refractive index n2 and the Raman gain coefficient gR. These parameters are related to the third order nonlinear susceptibility [x(3)]. In this work, the photorefractive beam coupling technique, also called induced grating autocorrelation (IGA), has been used to measure the nonlinear refractive index (n2) and the Raman gain coefficient (gR) of short lengths (z ~ 20 m) of optical fibers. In the IGA experiment, a transform limited Gaussian pulse is propagated through a short length of an optical fiber, where it undergoes self-phase modulation (SPM) and other nonlinear distortions, and the output pulse is split into two. The two-excitation pulses are then coupled into a photorefractive crystal, where they interfere and form a photorefractive phase grating. The IGA response is determined by delaying one beam (the probe) and plotting the diffracted intensity of the probe versus the relative delay (τ).Analysis of the IGA response yields information about the nonlinear phase distortions and other calibration parameters of the fiber. Using the IGA technique the author has measured the nonlinear refractive index in several types of fibers, including pure silica, Er-Al-Ge doped fibers, DCF (dispersion compensating fiber) and the recently developed TrueWave Rs fiber, and investigated the dependence of n2 on the doping profiles of Er, Al, and Ge in optical fibers. The standard IGA model for n2 measurements was derived from the solution of the nonlinear wave equation for pulse propagation in the limit of pure self-phase modulation. This model assumed that GVD (group velocity dispersion) and other nonlinear processes such as SRS (stimulated Raman scattering) are negligible. This model has been successfully used to fit the experimental data and determine the n2 of the fiber from the time dependent phase shift. However, SRS has been observed to distort the IGA trace, thus leading to a breakdown of the standard IGA model. A new IGA model has been developed in this study from the solution of the coupled-amplitude nonlinear Schrodinger equation, using both analytical and numerical approaches. This new model successfully accounts for the SRS effects on the IGA trace, in the limit of zero GVD, and allows the direct determination of the Raman gain coefficient from the fit of the SRSdistorted IGA trace. The measured nonlinear refractive index and Raman gain coefficients are in good agreement with published results. It was also shown that in the limit of zero GVD and no Raman, the IGA technique reduces to the widely accepted spectral domain SPM technique pioneered by Stolen and Lin, but is readily applicable to shorter lengths of fiber and is sensitive to smaller phase shifts

Ultra-high-resolution optical imaging for silicon integrated-circuit inspection

This thesis concerns the development of novel resolution-enhancing optical techniques for the purposes of non-destructive sub-surface semiconductor integrated-circuit (IC) inspection. This was achieved by utilising solid immersion lens (SIL) technology, polarisation-dependent imaging, pupil-function engineering and optical coherence tomography (OCT). A SIL-enhanced two-photon optical beam induced current (TOBIC) microscope was constructed for the acquisition of ultra-high-resolution two- and three-dimensional images of a silicon flip-chip using a 1.55μm modelocked Er:fibre laser. This technology provided diffraction-limited lateral and axial resolutions of 166nm and 100nm, respectively - an order of magnitude improvement over previous TOBIC imaging work. The ultra-high numerical aperture (NA) provided by SIL-imaging in silicon (NA=3.5) was used to show, for the first time, the presence of polarisation-dependent vectorialfield effects in an image. These effects were modelled using vector diffraction theory to confirm the increasing ellipticity of the focal-plane energy density distribution as the NA of the system approaches unity. An unprecedented resolution performance ranging from 240nm to ~100nm was obtained, depending of the state of polarisation used. The resolution-enhancing effects of pupil-function engineering were investigated and implemented into a nonlinear polarisation-dependent SIL-enhanced laser microscope to demonstrate a minimum resolution performance of 70nm in a silicon flip-chip. The performance of the annular apertures used in this work was modelled using vectorial diffraction theory to interpret the experimentally-obtained images. The development of an ultra-high-resolution high-dynamic-range OCT system is reported which utilised a broadband supercontinuum source and a balanced-detection scheme in a time-domain Michelson interferometer to achieve an axial resolution of 2.5μm (in air). The examination of silicon ICs demonstrated both a unique substrate profiling and novel inspection technology for circuit navigation and characterisation. In addition, the application of OCT to the investigation of artwork samples and contemporary banknotes is demonstrated for the purposes of art conservation and counterfeit prevention

THE DEVELOPMENT OF A NOVEL ELECTRO-MAGNETIC FORCE MICROSCOPE

This thesis describes the development of a new type of Magnetic Force Microscope (MFM) probe based on a unique electromagnetic design. In addition the design, construction and testing of a new MFM system, complete in both hardware and software, is also described. The MFM allowed initial tests on prototypes of the new probe, and is to provide a base for future new probe integration. The microscope uses standard MFM micro-cantilever probes in static modes of imaging. A new computer hosted DSP control system, software, and its various interfaces with the MFM have been integrated into the system. The system has been tested using standard probes with various specimens and satisfactory results have been produced. A novel probe has been designed to replace the standard MFM magnetic coated tip with a field generated about a sub-micron aperture in a conducting film. The field from the new probe is modelled and its imaging capability investigated, with iterative designs analysed in this way. The practical construction and potential problems therein, of the probe are also considered. Test apertures have been manufactured, and an image of the field produced when operating is provided as support to the theoretical designs. Future methods of using the new probe are also discussed, including the examination of the probe as a magnetic write mechanism. This probe, integrated into the MFM, can provide a new method of microscopic magnetic imaging, and in addition opens a new potential method of magnetic storage that will require further research

Dynamic Measurements with Scanning Probe Microscopy: Surface Studies Using Nanostructured Test Platforms of Metalloporphyrins, Nanoparticles and Amyloid Fibrils

A hybrid imaging mode for characterization of magnetic nanomaterials has been developed, using atomic force microscopy (AFM) combined with electromagnetic sample actuation. Instead of using a coated AFM probe as a magnetic sensor; our strategy is to use a nonmagnetic probe with contact mode AFM to characterize the vibration of magnetic and superparamagnetic nanomaterials responding to the flux of an AC electromagnetic field. We refer to the hybrid imaging mode as magnetic sample modulation (MSM-AFM). An oscillating magnetic field is produced by applying an AC current to a wire coil solenoid placed under the sample stage for tuning selected parameters of driving frequency and strength of the magnetic field. When the AC field is on, the AFM probe is scanned in contact with the sample to sense periodic changes in the force and motion of vibrating nanomaterials. With MSM, responses of both the amplitude and phase signal along with spatial maps of the topography channel can be collected simultaneously. A requirement for MSM is that the samples can be free to vibrate, yet remain attached to the surface. Particle lithography was used to prepare well-defined test platforms of ring structures of magnetic or superparamagnetic nanomaterials. Capillary filling of polydimethylsiloxane (PDMS) molds was applied to generate stripes of FeNi3 nanoparticles with microscale dimensions as test platforms. The MSM-AFM imaging mode was used successfully to characterize nanomaterials of FeNi3 nanoparticles, cobalt nanoparticles, octa-substituted porphyrin nanocrystals and ionic liquid nanoGUMBOS with dimensions ranging from 1 to 200 nm. Dynamic MSM-AFM measurements can be obtained by placing the tip on a vibrating nanoparticle and sweeping the frequency or field strength. Changes in frequency spectra and vibrational amplitude can be mapped for nanoparticles of different sizes, shapes and composition. The MSM-AFM imaging mode provides a useful tool for investigating changes in size dependent magnetic properties of materials at the nanoscale. Samples of designed amyloid proteins were characterized ex situ using scanning probe microscopy. The progressive growth and fibrillization of amyloid â over extended time intervals was visualized with high resolution using AFM

Electrospun polymer nanofibers for electromechanical transduction investigated by scanning probe microscopy

Negli ultimi anni, il copolimero ferroelettrico P(VDF-TrFE), ha suscitato un grande interesse nella ricerca scientifica per le potenziali applicazioni elettroniche come ad esempio l’energy harvesting per la produzione di dispositivi indossabili e autoalimentabili, sensori biocompatibili e memorie non volatili. Molti sforzi si sono concentrati nello sviluppo di procedure di fabbricazione che possano migliorare le performance elettromeccaniche di questi materiali. Una delle soluzioni proposte è un processo chiamato elettrofilatura, una tecnica efficiente e a basso costo che sarebbe in grado di realizzare nanofibre polimeriche già polarizzate e pronte per l’integrazione nei dispositivi. Dalle analisi microscopiche svolte in questa tesi, utilizzando tecniche di microscopia a scansione di sonda, è stato scoperto che in realtà l’elettrofilatura non provoca polarizzazione nelle fibre, bensì induce un processo di iniezione di cariche all’interno del materiale che, se testato a livello macroscopico, mostra un’apparente risposta ferroelettrica dovuta però alle cariche intrappolate, come in un elettrete. Nonostante ciò, dopo la dissipazione delle cariche spaziali, ho potuto dimostrare, grazie al’implementazione della Switching Spectroscopy PFM ad alto potenziale, che le nanofibre elettrofilate possono essere polarizzate e mostrano proprietà piezoelettriche simili a quelle del film sottile. Quindi, inducendo la completa polarizzazione del network dopo la deposizione, è auspicabile un miglioramento delle proprietà elettromeccaniche dei dispositivi basati su nano-fibre elettrofilate

Modeling and Control of MEMS-based Multi-layered Prestressed Piezoelectric Cantilever Beam

Piezoelectric materials are the preferred smart materials for sensing and actuation in the form of micro and nano-engineering structures like beams and plates. Cantilever beams play a significant role as key components in atomic force microscopy and bio and chemical sensors. Adding an active layer such as lead zirconate titanate (PZT) thin-film to form smart cantilever beams with sensing and actuation capabilities is highly desirable to facilitate miniaturization, enhance performance and functionali- ties such as enabling on-chip high-speed parallel AFM. During the micro-fabrication process, residual stresses develop in the different layers of the cantilever beam, causes initial deflection. The residual stress in the different layers of the cantilever beam and the application of voltage to the PZT thin-film affects their dynamics. This the- sis investigates the dynamic behaviour and develops a control technique and a novel charge readout circuit to improve the performance of a micro-fabricated multi-layer prestressed piezoelectric cantilever beam as an actuator and a deflection sensor. Firstly, the fabrication process of a unimorph PZT cantilever beam is explained. A low thermal budget Ultra-high vacuum e-beam evaporated polysilicon thin-film (UHVEEpoly) process is used for the fabrication of multi-layered PZT cantilever beam in d31 mode. The sharp peaks at resonant frequencies in the frequency response of the PZT cantilever beam show very little damping and a large settling time of the cantilever beam. Secondly, the dynamic behaviour of the prestressed PZT cantilever beam is in- vestigated subjected to change in driving voltage. Experimental investigations show a shift in resonant frequencies of a PZT cantilever beam. However, there is no reported mathematical model that predicts the shift in resonance frequencies of a multi-layered prestressed piezoelectric cantilever beam subjected to a change in driving voltage. This work developed a mathematical model with experimental val- idation to estimate the shift in resonance frequencies of such cantilever beams with the change in the driving voltage. A very good agreement between the model predic- tions and experimental measurements for the frequency response of the cantilever beam at different driving voltages has been obtained. A novel linear formulation has been developed to predict the shift in resonance frequencies of the PZT can- i tilever beam for a wide range of driving voltages. The formulation shows that the shift in resonance frequencies of a multi-layered prestressed piezoelectric cantilever beam per unit of applied voltage is dependent on geometric parameters and material properties. Thirdly, a robust resonant controller has been designed and implemented to re- duce the settling time of a highly vibrating PZT cantilever beam. The controller design is based on a mixed negative-imaginary, passivity, and a small-gain approach. The motivation to design a resonant controller using the above-mentioned analyti- cal framework is its bandpass nature and the use of velocity feedback, as the charge collected from a vibrating PZT cantilever beam gives the velocity information of the beam. The proposed controller design results in finite gain stability for a pos- itive feedback interconnection between two stable linear systems with a large gain and phase margin. Experimental results demonstrate that the designed resonant controller is able to effectively damp the first resonant mode of a cantilever, signifi- cantly reducing settling time from 528 ms to 32 ms. The robustness of the designed resonant controller is tested against changes in the cantilever beam dynamics due to residual stress variation and or stress variation due to driving voltage. Finally, to facilitate the miniaturization of on-chip sensors and parallel high- speed AFM, a single layer of a PZT thin-film in a cantilever beam is used as a deflection sensor and an actuator instead of bulky optical deflection sensors. A novel charge readout circuit is designed for deflection sensing by capturing the electrical charge generated due to the vibration of the PZT beam. The signal-to-noise ratio and sensitivity analysis of the readout circuit shows similar results compared to the commercially available optical deflection sensors. Our work highlights very important aspects in the dynamic behaviour and perfor- mance of a multi-layered prestressed piezoelectric cantilever beam. The agreement between the proposed theoretical formulation and experimental investigations in modeling, control design, and a novel readout circuit will provide the platform for further the development and miniaturization of microcantilever-based technologies, including on-chip parallel HS-AFM

Time domain measurement of the nonlinear refractive index in optical fibers and semiconductor film

A new technique to measure the nonlinear refractive index n2 in optical fibers and semiconductor films has been developed. It is based on the time delay two-beam coupling of very intense picosecond laser pulses that have been self-phase modulated in the nonlinear optical medium. The two beams are coupled in a slow responding medium that is sensitive to time dependent phase distortions. We determine that the amount of phase distortion experienced by the pulse is proportional to the nonlinear refractive index of the medium, This time domain approach can also be applied to optical fiber amplifiers in the presence of gain and to semiconductor films. Because the technique is base on pure refraction the measurement of n2 is insensitive to nonlinear absorption, thermal effects, and surface roughness. With this technique we have measured n2 in 20-m. length of Silica-glass, Ytterbium-doped, and Erbium-doped optical fibers at 1.064-µm. Also we have measured the change of n2 at 1.064-µm in the presence of a 980-nm pump laser in Yb3+ -doped and Er3+ -doped fibers. Finally we have extended the technique to measure n_2 in 2-mm thick samples of GaAs, CdTe and ZnTe semiconductors. In the language of ultrafast spectroscopist, if the best tool to characterize an ultrashort optical pulse is the pulse itself, then the best tool to characterize an optical nonlinear medium is a pulse that has been modified by the medium