Near infrared spectroscopy for fibre based gas detection

Gas sensing systems based on fibre optic linked near infra red absorption cells are potentially a flexible and effective tool for monitoring accumulations of hazardous and noxious gases in enclosed areas such as tunnels and mines. Additionally the same baseline technology is readily modified to measure concentrations of hydrocarbon fuels - notably but not exclusively methane, and monitoring emissions of greenhouse gases. Furthermore the system can be readily implemented to provide intrinsically safe monitoring over extensive areas at up to ~250 points from a single interrogation unit. In this paper we review our work on fibre coupled gas sensing systems. We outline the basic principles through which repeatable and accurate self calibrating gas measurements may be realised, including the recover of detailed line shapes for non contact temperature and / or pressure measurements in addition to concentration assessments in harsh environments. We also outline our experience in using these systems in extensive networks operating under inhospitable conditions over extended periods extending to several years

Thulium-doped fibre laser in the 2 μm wavelength region for gas sensing

The transition 3F4->3H6 of trivalent Thulium is widely studied for generating lasers at wavelength near 2 μm. For decades, tuneable continuous wave narrow line-width sources in this wavelength region have been proved to be very useful as spectroscopic tools for trace gas detection. Semiconductor lasers are often not readily available at a reasonable cost with the specific wavelengths required to provide a close ‘match’ to the key absorption features of the gases of interest. Well-designed fibre laser-based systems, however, can overcome this limitation by offering potentially much wider wavelength ranges, coupled with their distinctive and valuable features such as stability, narrow linewidth and high tuneability at room temperature. In this work, a compact ‘all-fibre’ laser system has been specifically designed, developed and evaluated, as this type of laser systems is highly desirable for ‘in-the-field’ applications. This takes full advantages of the active fibres based on silica glass host compared to other non-oxide glass hosts in terms of their chemical durability, stability and crucial structural compatibility with readily available telecommunication optical fibres. Ideal host composition for Thulium and efficient pumping scheme posses major challenges restricting the production of commercially deployable efficient ‘all-fibre’ lasers in the 2 μm wavelength region. The aim of the thesis work is to address these challenges. The work presented in this thesis demonstrates a modulated Thulium-doped ‘all-fibre’ tuneable laser in the 2 μm wavelength region suitable for detection of a number of gases of interest. The scope of work includes the fabrication and optimization of the active fibre with the core composition suitable for the creation of an effective Thulium-doped fibre laser. Codoping of Ytterbium is explored to investigate the energy-transfer mechanism from Ytterbium to Thulium and thereby opening up the opportunity of using economic pump laser diodes emitting at around 0.98 μm. In this respect, both Thulium- and Thulium/Ytterbium-doped single-mode single-clad silica optical fibres are designed and fabricated for a systematic analysis before being used as laser gain media. The optical preforms having different host compositions, Thulium-ion concentrations and proportions of Ytterbium to Thulium are fabricated by using the Modified Chemical Vapour Deposition technique coupled with solution doping to enable the incorporation of rareearth ions into the preforms. A thorough investigation of the basic absorption and emission properties of Thulium-doped silica fibres has been performed. The step-wise energy-transfer parameters in Thulium/Ytterbium-doped silica fibre have been determined quantitatively from spectroscopic measurements along with migrationassisted energy-transfer model. A set of tuneable Thulium-doped ‘all-fibre’ lasers, offering a narrow line-width in the 2 μm wavelength region, is created by using fabricated Thulium-and Thulium/Ytterbium-doped fibres as gain media and fibre Bragg grating pairs under in-band pumping at 1.6 μm and/or pumping by an economical laser diode at 0.98 μm, utilizing Ytterbium to Thulium energy- transfer. The host composition and the dopnat concentration in the single-mode single-clad fibre configuration are optimized to achieve maximum lasing efficiency. The tuning of laser wavelength has been achieved by using relaxation/compression mechanism of the fibre Bragg grating pair used to confine the laser cavity. A new set of laser resonators has also been formed by using a combination of a high reflective fibre Bragg grating with a low reflective broadband mirror, fabricated at the end of the fibre through silver film deposition, to enable only one fibre Bragg grating to be tuned. The stability of the laser output power, line-width and shape have been monitored throughout the tuning range. This is followed by the design of a compact, high-Q, narrow line-width and low threshold microsphere laser resonator, operating in the 2 μm wavelength region, by coupling a Thulium-doped silica microsphere to a tapered fibre. In the microsphere, laser emission occurred at wavelengths over the range from 1.9 to 2.0 μm under excitation at a wavelength of around 1.6 μm. The designed modulated tuneable Thulium-doped ‘all-fibre’ laser, operating at a wavelength range centred at a wavelength of 1.995 μm, has been tested for CO2 gas detection. Both the modulation of the fibre laser, through pump source modulation and the ‘locking’ detection mechanism have been utilized to eliminate laser intensity noise and therefore to obtain a compact gas sensor with high sensitivity. The absorption spectrum, the line-strength and the concentration level of CO2, have been monitored using the absorption spectroscopic technique. The measured minimum detectable concentration of CO2 obtained using the system confirms the claim that it is capable of detecting trace gases at the ppm level. The stable laser performance achieved in the sensor system illustrates its potential for the development of practical, compact yet sensitive fibre laser based gas sensor systems

Recovery of absolute absorption line shapes in tunable diode laser spectroscopy using external amplitude modulation with balanced detection

Accurate recovery of an absorption lineshape is important in many industrial applications for simultaneous measurement of gas concentration and pressure or temperature. Here we demonstrate a method, based on a modification to the Hobbs balanced receiver circuit, for background signal nulling when external amplitude modulation of the laser output is used. Compared with direct or non-nulled detection techniques, we demonstrate that the method significantly improves the signal to noise ratio to a level comparable to that of conventional second harmonic wavelength modulation spectroscopy. Most importantly, normalisation and recovery of the lineshape is straightforward and immune to the difficulties that afflict lineshape recovery with conventional wavelength modulation spectroscopy

Integrated nano-opto-electro-mechanical sensor for spectrometry and nanometrology

Spectrometry is widely used for the characterization of materials, tissues, and gases, and the need for size and cost scaling is driving the development of mini and microspectrometers. While nanophotonic devices provide narrowband filtering that can be used for spectrometry, their practical application has been hampered by the difficulty of integrating tuning and read-out structures. Here, a nano-opto-electro-mechanical system is presented where the three functionalities of transduction, actuation, and detection are integrated, resulting in a high-resolution spectrometer with a micrometer-scale footprint. The system consists of an electromechanically tunable double-membrane photonic crystal cavity with an integrated quantum dot photodiode. Using this structure, we demonstrate a resonance modulation spectroscopy technique that provides subpicometer wavelength resolution. We show its application in the measurement of narrow gas absorption lines and in the interrogation of fiber Bragg gratings. We also explore its operation as displacement-to-photocurrent transducer, demonstrating optomechanical displacement sensing with integrated photocurrent read-out

Thulium-doped fibre laser in the 2 μm wavelength region for gas sensing

The transition 3F4->3H6 of trivalent Thulium is widely studied for generating lasers at wavelength near 2 μm. For decades, tuneable continuous wave narrow line-width sources in this wavelength region have been proved to be very useful as spectroscopic tools for trace gas detection. Semiconductor lasers are often not readily available at a reasonable cost with the specific wavelengths required to provide a close ‘match’ to the key absorption features of the gases of interest. Well-designed fibre laser-based systems, however, can overcome this limitation by offering potentially much wider wavelength ranges, coupled with their distinctive and valuable features such as stability, narrow linewidth and high tuneability at room temperature. In this work, a compact ‘all-fibre’ laser system has been specifically designed, developed and evaluated, as this type of laser systems is highly desirable for ‘in-the-field’ applications. This takes full advantages of the active fibres based on silica glass host compared to other non-oxide glass hosts in terms of their chemical durability, stability and crucial structural compatibility with readily available telecommunication optical fibres. Ideal host composition for Thulium and efficient pumping scheme posses major challenges restricting the production of commercially deployable efficient ‘all-fibre’ lasers in the 2 μm wavelength region. The aim of the thesis work is to address these challenges. The work presented in this thesis demonstrates a modulated Thulium-doped ‘all-fibre’ tuneable laser in the 2 μm wavelength region suitable for detection of a number of gases of interest. The scope of work includes the fabrication and optimization of the active fibre with the core composition suitable for the creation of an effective Thulium-doped fibre laser. Codoping of Ytterbium is explored to investigate the energy-transfer mechanism from Ytterbium to Thulium and thereby opening up the opportunity of using economic pump laser diodes emitting at around 0.98 μm. In this respect, both Thulium- and Thulium/Ytterbium-doped single-mode single-clad silica optical fibres are designed and fabricated for a systematic analysis before being used as laser gain media. The optical preforms having different host compositions, Thulium-ion concentrations and proportions of Ytterbium to Thulium are fabricated by using the Modified Chemical Vapour Deposition technique coupled with solution doping to enable the incorporation of rareearth ions into the preforms. A thorough investigation of the basic absorption and emission properties of Thulium-doped silica fibres has been performed. The step-wise energy-transfer parameters in Thulium/Ytterbium-doped silica fibre have been determined quantitatively from spectroscopic measurements along with migrationassisted energy-transfer model. A set of tuneable Thulium-doped ‘all-fibre’ lasers, offering a narrow line-width in the 2 μm wavelength region, is created by using fabricated Thulium-and Thulium/Ytterbium-doped fibres as gain media and fibre Bragg grating pairs under in-band pumping at 1.6 μm and/or pumping by an economical laser diode at 0.98 μm, utilizing Ytterbium to Thulium energy- transfer. The host composition and the dopnat concentration in the single-mode single-clad fibre configuration are optimized to achieve maximum lasing efficiency. The tuning of laser wavelength has been achieved by using relaxation/compression mechanism of the fibre Bragg grating pair used to confine the laser cavity. A new set of laser resonators has also been formed by using a combination of a high reflective fibre Bragg grating with a low reflective broadband mirror, fabricated at the end of the fibre through silver film deposition, to enable only one fibre Bragg grating to be tuned. The stability of the laser output power, line-width and shape have been monitored throughout the tuning range. This is followed by the design of a compact, high-Q, narrow line-width and low threshold microsphere laser resonator, operating in the 2 μm wavelength region, by coupling a Thulium-doped silica microsphere to a tapered fibre. In the microsphere, laser emission occurred at wavelengths over the range from 1.9 to 2.0 μm under excitation at a wavelength of around 1.6 μm. The designed modulated tuneable Thulium-doped ‘all-fibre’ laser, operating at a wavelength range centred at a wavelength of 1.995 μm, has been tested for CO2 gas detection. Both the modulation of the fibre laser, through pump source modulation and the ‘locking’ detection mechanism have been utilized to eliminate laser intensity noise and therefore to obtain a compact gas sensor with high sensitivity. The absorption spectrum, the line-strength and the concentration level of CO2, have been monitored using the absorption spectroscopic technique. The measured minimum detectable concentration of CO2 obtained using the system confirms the claim that it is capable of detecting trace gases at the ppm level. The stable laser performance achieved in the sensor system illustrates its potential for the development of practical, compact yet sensitive fibre laser based gas sensor systems.EThOS - Electronic Theses Online ServiceGBUnited Kingdo

In-situ cure monitoring of epoxy resin systems

This thesis was submitted for the degree of Doctor of Philosophy and awarded by Brunel University.This thesis describes the work carried out at Brunel University to develop novel optical fibre sensors capable of monitoring the cure state of an epoxy/amine resin system. The sensors were of simple construction, consisting of an optical fibre from which the silicone cladding layer had been removed over a short length. This stripped length was embedded into the curing resin system. The sensor was successfully used in two ways: i) as an evanescent absorption sensor to monitor specific absorption bands of the resin system. The absorption of energy from the evanescent wave of the optical fibre by absorbing media allows evanescent absorption spectra to be obtained. Absorption spectra were obtained from sensors embedded in a model curing resin system over narrow wavelength ranges. These wavelength ranges corresponded to positions of known absorptions in the spectra of active components in epoxy/amine systems. By monitoring the change in these absorptions it was possible to obtain information about concentration of the amine hardener functional group throughout cure; ii) as a refractive index sensor capable of monitoring the changes in the refractive index of the resin system during cure. A laser diode was used to launch light into the sensor and the intensity of light emerging from the other end of the fibre was monitored. Changes in the resin system refractive index caused changes in the guiding properties of this the sensor. This resulted in a significant change in the intensity of light recorded by the detector and allowed the cure process to be followed. This sensor was also embedded into a unidirectional pre-preg system and was able to follow the cure of the system. The results from the two sensing methods have been compared with data obtained using FTIR spectroscopy and Abbe refractometry during the resin system cure. A theoretical model of sensor response has been developed and compared with the experimental data obtained. The sensor response has also been compared to predictions made by several models of evanescent sensor systems obtained from the literature. These models have been modified so that they can be applied to a sensor embedded into a curing resin system. An analysis of the correspondence between theory and experiment is presented

Development of gas detection systems based on microstructured optical fibres

Estágio realizado no INESC e orientado pelo Prof. Doutor Luís Alberto de Almeida FerreiraTese de mestrado integrado. Engenharia Electrotécnica e de Computadores. Faculdade de Engenharia. Universidade do Porto. 200

A novel laser diode wavelength stabilisation technique for use in high resolution spectroscopy

Tuneable diode laser absorption spectroscopy (TDLAS) based gas sensors are widely used for trace gas detection for their high selectivity and sensitivity. The laser source used in TDLAS requires a narrow line width in the order of 10s of MHz, with a wavelength stability multiple orders lower than the molecular absorption line width, which is, for example, 4.1GHz (38pm) for an air broadened methane line. TDLAS requires the use of a laser diode with a long term wavelength stability of better than 10% of the absorption line width of the target gas species. The wavelength stability of the laser is highly temperature dependent as the wavelength increases with increasing temperature. Therefore, control of the temperature of the laser diode is vital for stabilising the laser emission wavelength. In this thesis, a novel method has been proposed to measure and stabilise the temperature of a laser diode. The laser diode emission wavelength was stabilised by using its measured junction voltage in a control feedback loop. In order to determine the junction voltage, a series resistance correction term was identified, which was the novel part of this wavelength stabilisation technique. The laser diode junction and forward voltages were calculated from the forward voltage drop of the laser diode at measured at various operating temperatures. The laser diode series resistance was measured dynamically and was subtracted from the forward voltage to calculate the junction voltage. Both the forward voltage and series resistances were found to be temperature dependent. This method was investigated for its short term (~ 5minute) and long term (~ 1 hour) wavelength stability and was compared with other available methods. The laser diode wavelength stability attained using this method has been also investigated at various ambient temperatures (10-40 °C). ...[cont.

Wavelength Tuneable Frequency Domain Photon Migration Spectrometer for Tissue-like Media

Frequency domain spectrometers use intensity modulated light to quantitatively interrogate turbid media. The modulation frequencies employed are in the radiofrequency range. Intensity modulated light launched into a turbid medium generates photon density fluctuations with wave like character that oscillates at the modulation frequency. These density fluctuations are named diffuse photon density waves, and it has been shown that the amplitude and phase of the photon density wave inside the medium depends on its optical properties. Hence by measuring the amplitude and phase of the photon density wave the optical properties of the medium can be estimated. This is the basic working principle of a frequency domain photon migration spectrometer. Frequency domain spectrometers fabricated with laser diodes are limited to discrete wavelengths thereby making compromises on the information about the media under test. In this research a wavelength tuneable frequency domain spectrometer was constructed by modulating the output intensity of a titanium: sapphire laser using an acousto-optic modulator. A low noise avalanche photodiode module in conjunction with a lock-in amplifier was used to measure the amplitude attenuation and phase lag inside a turbid sample. The frequency domain spectrometer was tested for accuracy and precision by estimating the optical properties of an important tissue simulation phantom, Intralipid , at a representative wavelength 790 nm. The results indicated that the spectrometer estimates absorption with an accuracy of 10%. The instrument estimates the absorption and reduced scattering coefficients with a precision of 3% and 6%, respectively. Optical properties of Intralipid were measured from 710-850 nm in the therapeutic window. The results were compared with published data measured by other methods and similar frequency domain techniques. The absorption coefficient agrees within 10% with results from a time domain measurement. The reduced scattering coefficient was within the error limits of other reported measurements. At 750 nm the reduced scattering agrees within 5% with the results from a continuous wave, time domain and within 1% from another frequency domain measurement, and at 811 and 849 nm this agreement is within 9%. A Mie theory prediction of the reduced scattering coefficient based on a measurement of the particle size distribution by a Mastersizer 2000 is larger than the frequency domain results by 6%. The spectrometer was used to determine the optical temperature coefficient of Intralipid , exploring its potential as a non invasive temperature monitoring device. The measured minute change in the absorption coefficient suggests a minimum observable temperature change of 4'C, which for most practical applications means that the precision needs to improve. The effect of glucose on the optical properties of Intralipid indicates that the absorption coefficient decreases steadily at 730 nm up to 1000mg/dL. The reduced scattering coefficient decreases with increasing glucose concentration at most of the wavelengths. This work quantified the absorption and reduced scattering of Intralipid over a larger wavelength range (in the therapeutic window) than before. This is the first time the effects of temperature on the optical properties of a turbid medium monitored with a frequency domain spectrometer. Specific information about the precision and accuracy which can be achieved with the current technology is documented. Current precision is not sufficient for many applications that would benefit from separation of absorption and scattering