Development and fabrication of optical biosensors based on biophotonic sensing cells (BICELLs)

El objetivo de esta tesis es el desarrollo y caracterización de biosensores ópticos sin marcado basados en celdas sensoras biofotónicas (BICELLs). Éstas son un nuevo concepto de biosensor desarrollado por el grupo de investigación y consiste en la combinación de técnicas de interrogación vertical, junto a estructuras fotónicas producidas usando métodos de micro- y nanofabricación. Varias conclusiones son extraídas de este trabajo. La primera, que se ha definido una BICELL estándar basada en interferómetros Fabry-Perot (FP). Se ha demostrado su capacidad para la comparación de rendimiento entre BICELLs estructuradas y para la realización de inmunoensayos de bajo coste. Se han estudiado diferentes técnicas de fabricación disponibles para la producción de BICELLs. Se determinó que la litografía de contacto a nivel de oblea produce estructuras de bajo coste, reproducibles y de alta calidad. La resolución alcanzada ha sido de 700 nm. El estudio de la respuesta a inmunoensayos de las BICELLs producidas se ha desarrollado en este trabajo. Se estudió la influencia de BICELLs basadas en diferentes geometrías y tamaños. De aquí resulta un nuevo enfoque para predecir el comportamiento de respuesta para la detección biológica de cualquier biosensor óptico estructurado, relacionando su superficie efectiva y su sensibilidad óptica. También se demostró una técnica novedosa y de bajo coste para la caracterización experimental de la sensibilidad óptica, basada en el depósito de películas ultradelgadas. Finalmente, se ha demostrado el uso de BICELLs desarrolladas en esta tesis, en la detección de aplicaciones reales, tales como hormonas, virus y proteínas. ABSTRACT The objective of this thesis is the development and characterization of optical label-free biosensors based on Bio-Photonic sensing Cells (BICELLs). BICELL is a novel biosensor concept developed by the research group, and it consists of a combination of vertical interrogation optical techniques and photonic structures produced by using micro- and nano-fabrication methods. Several main conclusions are extracted from this work. Firstly, a standard BICELL is defined based on FP interferometers, which demonstrated its capacity for accomplishing performance comparisons among different structured BICELLs, as well as to achieve low-cost immunoassays. Different available fabrication techniques were studied for BICELL manufacturing. It is found that contact lithography at wafer scale produce cost-effective, reproducible and high quality structures. The resolution achieved was 700 nm. Study on the response of developed BICELLs to immunoassays is performed within this work. It is therefore studied the influence of BICELLs based on different geometries and sizes in the immunoassay, which resulted in a new approach to predict the biosensing behaviour of any structured optical biosensor relating to its effective surface and optical sensitivity. Also, it is demonstrated a novel and low-cost characterization technique of the experimental optical sensitivity, based on ultrathin-film deposition. Finally, it is also demonstrated the capability of using the developed BICELLs in this thesis for real applications detection of hormones, virus and proteins.

Characterization of emission regimes in a 1.5 um high brightness MOPA

We present and analyze experimental results on the emission characteristics of a 1.5 ?m distributed feedback tapered master-oscillator power-amplifier in a wide range of steady-state injection conditions, showing different emission regimes under cw operation: stable single frequency emission, multi-frequency Fabry-Perot-like emission, and self-pulsation operation.

Desenvolvimento e caracterização do filtro óptico de interferência variável para detectores de alta resolução espectral e biossensores.

O presente trabalho está fundamentado no desenvolvimento de uma metodologia e/ou uma tecnologia de obtenção e caracterização de filtros ópticos de interferência de banda passante variável [C.M. da Silva, 2010] e de banda de corte variáveis, constituídos por refletores dielétricos multicamadas de filmes finos intercalados por cavidades de Fabry-Perot não planares com espessuras linearmente variáveis, que apresentam a propriedade do deslocamento linear da transmitância máxima espectral em função da posição, isto é, um Filtro de Interferência Variável (FIV). Este método apresenta novas e abrangentes possibilidades de confecção de filtros ópticos de interferência variável: lineares ou em outras formas desejadas, de comprimento de onda de corte variável (passa baixa ou alta) e filtros de densidade neutra variável, através da deposição de metais, além de aplicações em uma promissora e nova área de pesquisa na deposição de filmes finos não uniformes. A etapa inicial deste desenvolvimento foi o estudo da teoria dos filtros ópticos dielétricos de interferência para projetar e construir um filtro óptico banda passante convencional de um comprimento de onda central com camadas homogêneas. A etapa seguinte, com base na teoria óptica dos filmes finos já estabelecida, foi desenvolver a extensão destes conhecimentos para determinar que a variação da espessura em um perfil inclinado e linear da cavidade entre os refletores de Bragg é o principal parâmetro para produzir o deslocamento espacial da transmitância espectral, possibilitando o uso de técnicas especiais para se obter uma variação em faixas de bandas de grande amplitude, em um único filtro. Um trabalho de modelagem analítica e análise de tolerância de espessuras dos filmes depositados foram necessários para a seleção da estratégia do \"mascaramento\" seletivo do material evaporado formado na câmara e-Beam (elétron-Beam) com o objetivo da obtenção do filtro espectral linear variável de características desejadas. Para tanto, de acordo com os requisitos de projeto, foram necessárias adaptações em uma evaporadora por e-Beam para receber um obliterador mecânico especialmente projetado para compatibilizar os parâmetros das técnicas convencionais de deposição com o objetivo de se obter um perfil inclinado, perfil este previsto em processos de simulação para ajustar e calibrar a geometria do obliterador e se obter um filme depositado na espessura, conformação e disposição pretendidos. Ao final destas etapas de modelagem analítica, simulação e refinamento recorrente, foram determinados os parâmetros de projeto para obtenção de um determinado FIV (Filtro de Interferência Variável) especificado. Baseadas nos FIVs muitas aplicações são emergentes: dispositivos multi, hiper e ultra espectral para sensoriamento remoto e análise ambiental, sistemas Lab-on-Chip, biossensores, detectores chip-sized, espectrofotometria de fluorescência on-chip, detectores de deslocamento de comprimento de onda, sistemas de interrogação, sistemas de imageamento espectral, microespectrofotômetros e etc. No escopo deste trabalho se pretende abranger um estudo de uma referência básica do emprego do (FIV) filtro de interferência variável como detector de varredura de comprimento de ondas em sensores biológicos e químicos compatível com pós processamento CMOS. Um sistema básico que é constituído por um FIV montado sobre uma matriz de sensores ópticos conectada a um módulo eletrônico dedicado a medir a intensidade da radiação incidente e as bandas de absorção das moléculas presentes em uma câmara de detecção de um sistema próprio de canais de microfluidos, configurando-se em um sistema de aquisição e armazenamento de dados (DAS), é proposto para demonstrar as possibilidades do FIV e para servir de base para estudos exploratórios das suas diversas potencialidades que, entre tantas, algumas são mencionadas ao longo deste trabalho. O protótipo obtido é capaz de analisar fluidos químicos ou biológicos e pode ser confrontado com os resultados obtidos por equipamentos homologados de uso corrente.

Synthesis, Modification, and Application of Siloxane Materials for Environmental Sensing

As human populations and resource consumption increase, it is increasingly important to monitor the quality of our environment. While laboratory instruments offer useful information, portable, easy to use sensors would allow environmental analysis to occur on-site, at lower cost, and with minimal operator training. We explore the synthesis, modification, and applications of modified polysiloxane in environmental sensing. Multiple methods of producing modified siloxanes were investigated. Oligomers were formed by using functionalized monomers, producing siloxane materials containing silicon hydride, methyl, and phenyl side chains. Silicon hydride-functionalized oligomers were further modified by hydrosilylation to incorporate methyl ester and naphthyl side chains. Modifications to the siloxane materials were also carried out using post-curing treatments. Methyl ester-functionalized siloxane was incorporated into the surface of a cured poly(dimethylsiloxane) film by siloxane equilibration. The materials containing methyl esters were hydrolyzed to reveal carboxylic acids, which could later be used for covalent protein immobilization. Finally, the siloxane surfaces were modified to incorporate antibodies by covalent, affinity, and adsorption-based attachment. These modifications were characterized by a variety of methods, including contact angle, attenuated total reflectance Fourier transform infrared spectroscopy, dye labels, and 1H nuclear magnetic resonance spectroscopy. The modified siloxane materials were employed in a variety of sensing schemes. Volatile organic compounds were detected using methyl, phenyl, and naphthyl-functionalized materials on a Fabry-Perot interferometer and a refractometer. The Fabry-Perot interferometer was found to detect the analytes upon siloxane extraction by deformation of the Bragg reflectors. The refractometer was used to determine that naphthyl-functionalized siloxanes had elevated refractive indices, rendering these materials more sensitive to some analytes. Antibody-modified siloxanes were used to detect biological analytes through a solid phase microextraction-mediated enzyme linked immunosorbent assay (SPME ELISA). The SPME ELISA was found to have higher analyte sensitivity compared to a conventional ELISA system. The detection scheme was used to detect Escherichia coli at 8500 CFU/mL. These results demonstrate the variety of methods that can be used to modify siloxanes and the wide range of applications of modified siloxanes has been demonstrated through chemical and biological sensing schemes.

Entanglement and the Einstein-Podolsky-Rosen paradox with coupled intracavity optical down-converters

We show that two evanescently coupled χ((2)) parametric down-converters inside a Fabry-Perot cavity provide a tunable source of quadrature squeezed light, Einstein-Podolsky-Rosen (EPR) correlations and quantum entanglement. Analyzing the operation in the below threshold regime, we show how these properties can be controlled by adjusting the coupling strengths and the cavity detunings. As this can be implemented with integrated optics, it provides a possible route to rugged and stable EPR sources.

Wavelength-division and spatial multiplexing using tandem interferometers for Bragg grating sensor networks

We present a new method for the interrogation of large arrays of Bragg grating sensors. Eight gratings operating between the wavelengths of 1533 and 1555 nm have been demultiplexed. An unbalanced Mach—Zehnder interferometer illuminated by a single low-coherence source provides a high-phase-resolution output for each sensor, the outputs of which are sequentially selected in wavelength by a tunable Fabry-Perot interferometer. The minimum detectable strain measured was 90 ne-vHz at 7 Hz for a wavelength of 1535 nm.

Interferometric sensor interrogation using an arrayed waveguide grating

We experimentally investigate the use of an arrayed waveguide grating (AWG) to interrogate interferometric sensors. A single broad-band light source is used to illuminate the system. Reflected spectral information is directed to an AWG with integral photodetectors providing 40 electrical outputs. We show that using the dual-wavelength technique we can measure the length of a Fabry-Perot cavity by determining the optical phase changes of the scanned interferometric pattern, which produced a maximum unambiguous range of 1440 mum with an active sensor and a maximum unambiguous range of 300 mum with the introduction of a second processing interferometer, which allows the sensor to be passive.

Optical in-fiber Bragg grating sensor systems for medical applications

Two in-fiber Bragg grating (FBG) temperature sensor systems for medical applications are demonstrated: (1) an FBG flow-directed thermodilution catheter based on interferometric detection of wavelength shift that is used for cardiac monitoring; and (2) an FBG sensor system with a tunable Fabry-Perot filter for in vivo temperature profiling in nuclear magnetic resonance (NMR) machines. Preliminary results show that the FBG sensor is in good agreement with electrical sensors that are widely used in practice. A field test shows that the FBG sensor system is suitable for in situ temperature profiling in NMR machines for medical applications.

Fabrication and applications of fibre Bragg gratings

The consequences of fabricating Bragg gratings in various fibres, with or without hydrogen loading, and with varying laser power levels are explored. Three new techniques for fabricating chirped gratings are presented. Beams with dissimilar wavefront curvatures are interfered to give chirped gratings. With the same aim techniques of writing gratings on tapered fibres and on deformed fibres are also covered. With these techniques, a wide variety of gratings has been fabricated from the 'superbroad' (with bandwidths of up to 180 nm), small to medium bandwidth gratings with linear chirp profiles and quadratic chirped gratings. It is demonstrated that chirped grating can be concatenated to form all-fibre Fabry-Perot and Moiré resonators. These are further concatenated with chirped gratings to produce filters with narrow passbands and very broad stopbands. A number of other applications are also addressed. The use of chirped fibre gratings for dispersion compensation and femtosecond chirped pulse amplification is demonstrated. Chirped gratings are used as dispersive elements in modelocked fibre lasers producing ultrashort pulses. A chirped fibre grating Fabry-Perot transmission filter is used in a continuous wave laser that exhibits eleven simultaneously lasing wavelengths. Finally, the use of grating-coupler devices as variable reflectivity mirrors for laser optimisation and gain clamping is considered.

Stabilization of self-coherent OFDM with injection locked laser

With the rebirth of coherent detection, various algorithms have come forth to alleviate phase noise, one of the main impairments for coherent receivers. These algorithms provide stable compensation, however they limit the DSP. With this key issue in mind, Fabry Perot filter based self coherent optical OFDM was analyzed which does not require phase noise compensation reducing the complexity in DSP at low OSNR. However, the performance of such a receiver is limited due to ASE noise at the carrier wavelength, especially since an optical amplifier is typically employed with the filter to ensure sufficient carrier power. Subsequently, the use of an injection-locked laser (ILL) to retrieve the frequency and phase information from the extracted carrier without the use of an amplifier was recently proposed. In ILL based system, an optical carrier is sent along with the OFDM signal in the transmitter. At the receiver, the carrier is extracted from the OFDM signal using a Fabry-Perot tunable filter and an ILL is used to significantly amplify the carrier and reduce intensity and phase noise. In contrast to CO-OFDM, such a system supports low-cost broad linewidth lasers and benefits with lower complexity in the DSP as no carrier frequency estimation and correction along with phase noise compensation is required.

Sensing properties of germanate and tellurite glass optical fibres

Strain and thermal sensitivities of germanate and tellurite glass fibres were measured using a fibre Fabry-Perot (FFP) interferometer and fibre Bragg gratings (FBG). The strain phase sensitivity for germanate and tellurite fibre were 5900×103 rad/m and 5600×103 rad/m respectively at a central wavelength of 1540nm using FFP interferometer, which is consistent with the value of 1.22pm/µepsilon obtained for a germanate fibre FBG. The Young's modulus for germanate and tellurite fibre were also measured to be 58GPa and 37GPa. The thermal responses of germanate fibre were examined as 24.71 and 16.80 pm/°C at 1540nm and 1033nm wavelength using the FBG.

Acoustic emission detection using optical fibre sensors for aerospace applications

Structural Health Monitoring (SHM) ensures the structural health and safety of critical structures covering a wide range of application areas. This thesis presents novel, low-cost and good-performance fibre Bragg grating (FBG) based systems for detection of Acoustic Emission (AE) in aircraft structures, which is a part of SHM. Importantly a key aim, during the design of these systems, was to produce systems that were sufficiently small to install in an aircraft for lifetime monitoring. Two important techniques for monitoring high frequency AE that were developed as a part of this research were, Quadrature recombination technique and Active tracking technique. Active tracking technique was used extensively and was further developed to overcome the limitations that were observed while testing it at several test facilities and with different optical fibre sensors. This system was able to eliminate any low frequency spectrum shift due to environmental perturbation and keeps the sensor always working at optimum operation point. This is highly desirable in harsh industrial and operationally active environments. Experimental work carried out in the laboratory has proved that such systems can be used for high frequency detection and have capability to detect up to 600 kHz. However, the range of frequency depends upon the requirement and design of the interrogation system as the system can be altered accordingly for different applications. Several optical fibre configurations for wavelength detection were designed during the course of this work along with industrial partners. Fibre Bragg grating Fabry-Perot (FBG-FP) sensors have shown higher sensitivity and usability than the uniform FBGs to be used with such system. This was shown experimentally. The author is certain that further research will lead to development of a commercially marketable product and the use of active tracking systems can be extended in areas of healthcare, civil infrastructure monitoring etc. where it can be deployed. Finally, the AE detection system has been developed to aerospace requirements and was tested at NDT & Testing Technology test facility based at Airbus, Filton, UK on A350 testing panels.

Grating based devices in polymer optical fibre

We describe recent research into devices based on fibre Bragg gratings in polymer optical fibre. Firstly, we report on the inscription of gratings in a variety of microstructured polymer optical fibre: single mode, few moded and multimoded, as well as fibre doped with trans-4-stilbenmethanol. Secondly, we describe research into an electrically tuneable filter using a metallic coating on a polymer fibre Bragg grating. Finally we present initial results from attempts to produce more complex grating structures in polymer fibre: a Fabry-Perot cavity and a phase-shifted grating.

Optical in-fiber Bragg grating sensor systems for medical applications

Two in-fiber Bragg grating (FBG) temperature sensor systems for medical applications are demonstrated: (1) an FBG flow-directed thermodilution catheter based on interferometric detection of wavelength shift that is used for cardiac monitoring; and (2) an FBG sensor system with a tunable Fabry-Perot filter for in vivo temperature profiling in nuclear magnetic resonance (NMR) machines. Preliminary results show that the FBG sensor is in good agreement with electrical sensors that are widely used in practice. A field test shows that the FBG sensor system is suitable for in situ temperature profiling in NMR machines for medical applications.

Intracavity generation of 610nm light by periodically poled near-stoichiometric lithium tantalate

Intracavity frequency doubling of an optically pumped GaInNAs semiconductor disk laser by a periodically poled near-stoichiometric lithium tantalate crystal has been investigated. Stable second-harmonic generation at 610nm has been achieved with an output power of 730mW, limited only by the spectral acceptance range and Fresnel losses of the crystal. Spectral tuning of 8nm was realised with a Fabry-Pérot etalon. © The Institution of Engineering and Technology.