Research Collection. Optical parametric oscillator pumped mid-infrared laser sources for photoacoustic trace gas spectroscopy.
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1 Research Collection Doctoral Thesis Optical parametric oscillator pumped mid-infrared laser sources for photoacoustic trace gas spectroscopy Author(s): Bohren, Andreas Markus Publication Date: 1997 Permanent Link: Rights / License: In Copyright - Non-Commercial Use Permitted This page was generated automatically upon download from the ETH Zurich Research Collection. For more information please consult the Terms of use. ETH Library
2 Dtea Eth <2x.?> Diss. ETH No Optical Pumped Mid-Infrared Laser Sourcesfor Photoacoustic Trace Gas Spectroscopy Parametric Oscillator A dissertation submitted to the Swiss Federal Institute of Technology ETH Zürich for the degree of Doctor of Natural Sciences presented by Andreas Markus Bohren Dipl. Phys. ETH born September 6, 1965 Citizen of Grindelwald (BE) date of examination February 7, 1997 accepted on the recommendation of Prof. Dr. M.W. Sigrist, ETH Zürich, referee Prof. Dr. F.K. Kneubühl, ETH Zürich, co-referee Prof. Dr. G. Guekos, ETH Zürich, co-referee Zürich, January
3 Zusammenfassung Messsysteme für die Erfassung von atmosphärischen Spurengasen, für die industrielle Prozessüberwachung, für die medizinische Diagnostik und für ähnliche Anwendungen erfordern sehr empfindliche und selektive Sensoren mit einer hohen Zeitauflösung. Verschiedene Untersuchungen belegen die vielfältigen Anwendungsmöglichkeiten der laser-photoakustischen Spektroskopie (PAS) im Infraroten für diese Zwecke. Die meisten dieser PAS-Systeme, darunter auch einige an unserem Institut entwickelte, basieren auf diskret bzw. kontinuierlich abstimmbaren C02-Lasern, die im Wellenlängenbereich um 10 im Strahlung emittieren. Andere Wellenlängen, die von speziellem Spurengasanalyse sind, beispielsweise der Bereich von 3-5 (im, begrenzt mit konventionellen Lasern erzeugt werden. Interesse für die können nur sehr Der erst seit kurzem erhältliche schmalbandige, nanosekunden-gepulste Optisch Parametrische Oszillator (OPO) stellt eine der vielversprechendsten Entwicklungen im Hinblick auf einen möglichst grossen Wellenlängenabstimmbereich dar. Einer der ersten kommerziellen OPOs bildet die Basis für diese Arbeit. Der OPO ist eine passive, Nd:YAG-Laser gepumpte Strahlungsquelle, deren Wellenlängenabstimmbarkeit auf einem nichtlinearen Frequenzmischprozess beruht. Mit dem von uns verwendeten System wird der ganze sichtbare Bereich und ein Teil des Infraroten bis 2 im mit Energien von bis zu 100 mj pro Puls abgedeckt. Das Ziel dieser Arbeit ist die Erweiterung dieses Abstimmbereichs bis etwa 5 im und der Einsatz dieses Systems in photoakustischen Spurengasmessungen. Zwei Methoden der Wellenlängenumwandlung, die beide auf nichtlinearer Frequenzmischung beruhen, wurden studiert: Differenzfrequenzerzeugung (DFG) und Stimulierte Raman Streuung (SRS). Systeme dieser Art wurden hier zum ersten Mal auf ihre Eignung für Spurengasanalyse untersucht. Vergleichbare Experimente lasern anstelle des hier verwendeten OPOs durchgeführt. wurden bereits mit Farbstoff Die Differenzfrequenz wird erzeugt durch Mischen der OPO Strahlung, abgestimmt zwischen 1.4 (im und 1.85 u.m, mit restlicher Strahlung des Nd:YAG-Pumplasers bei (im in einem LiNbÜ3 Kristall. Mit diesem Aufbau konnten Energien bis zu 500 uj im Wellenlängenbereich zwischen 2.5 und 4.5 Jim erreicht werden. Um die Eignung dieser Quelle für die Spurengasanalyse zu testen, wurden photoakustische Absorptionsspektren einzelner Gase (Methan, Methanol, Ethanol, Isopentan, Benzol und Toluol) bei einer Konzentration von 100 ppm im Bereich um 3 Jim aufgenommen. Zusätzlich wurden Mischungen der erwähnten Gase mit teilweise überlappender spektraler Absorption analysiert. Für die nachträgliche Kalibration der Wellenlängenskala der gemessenen Spektren, enthalten alle diese Mischungen Methan, dessen
4 4.5 Absorptionsspektrum sehr genau bekannt ist. Dieses Vorgehen ist notwendig, da kein geeigneter Monochromator für diesen Laser zur Verfügung stand. Mit dem vorgestellten DFG-Spektrometer können die meisten flüchtigen organischen Substanzen in Konzentrationen bis wenige ppm und Methan sogar bis zu etwa 60 ppb nachgewiesen werden. Verschiedene mögliche Verbesserungen des photoakustischen Messsystems und auch des DFG-Lasers deuten auf eine mögliche Reduktion der Nachweisgrenzen um bis zu drei Grössenordnungen hin. Ein zweiter Ansatz für die Wellenlängenumwandlung der OPO Strahlung beruht auf Stimulierter Raman Streuung (SRS) in Wasserstoffgas. Der angestrebte Abstimmbereich von fim wird durch einen OPO-gepumpten Wellenleiter SRS-Laser (betrieben in der zweiten Stokes Ordnung) abgedeckt. Die damit erzeugten Energien liegen allerdings noch im uj-bereich. Der geringe Wirkungsgrad ist hauptsächlich auf die Krümmung der verwendeten Wellenleiter und auf die eher mangelhafte Strahlqualität der OPO-Strahlung zurückzuführen. Aufgrund der beobachteten Reduktion der Emissionsbreite und des einfacheren experimentellen Aufbaus, könnten SRS-Laser aber trotzdem eine Alternative zu den DFG-Quellen werden. Mit der Verwendung verbesserter Wellenleiter und zusätzlicher Raman-Verstärker sollten ausserdem Energien im Bereich der DFG-Quelle erzeugbar sein. Im Hinblick auf eine mögliche kommerzielle Anwendung eines Luftanalysesystems, welches auf abstimmbaren Lasern basiert, ist die Analyse der gemessenen Spektren von grosser Wichtigkeit. Eines der Hauptprobleme ist dabei eine falsch kalibrierte oder nicht genügend genau bekannte Wellenlängenskala. Die kontinuierliche Messung der Wellenlänge eines gepulsten Lasers ist mit grossem Aufwand und hohen Kosten verbunden. Als Alternative wurde ein Algorithmus entwickelt, der die Wellenlängenskala eines gemessenen Spektrums aufgrund von bekannten Absorptionsspektren von Substanzen bestimmt, die sicher in der analysierten Probe vorhanden sind. Mit dieser Prozedur, die auf einem genetischen Algorithmus basiert, wird die experimentelle Bestimmung der Wellenlänge bei Spurengasanalysen überflüssig.
5 Summary Trace gas detection Systems for air pollution monitoring, industrial process monitoring, medical diagnostics and similar applications require very sensitive and selective sensors with a high temporal resolution. Numerous investigations document the versatility of laser photoacoustic spectroscopy (PAS) in the infrared for these purposes. However, most of the implemented PAS devices, including also Systems developed at our institute, are based on line tunable or continuously tunable CO2 lasers that operate in the 10 (im wavelength ränge. Other wavelength ranges that are of special interest for trace gas detection, especially the 3-5 (im ränge, are difficult to access with conventional laser Systems. The only recently available narrowband nanosecond pulsed Optical Parametric Oscillator (OPO) is one of the most promising developments concerning widely tunable laser Systems. One of the first commercial OPOs builds the basis for this work. The OPO is a passive, Nd:YAG laser pumped source, whose wavelength tunability is based on a nonlinear frequency mixing process. With the present Systems the whole visible and part of the infrared spectrum up to 2 (im is covered with laser radiation at energies of up to 100 mj per pulse. The subject of this work is to further extend this tuning ränge to access wavelengths up to approximately 5 {im and to implement this system in a photoacoustic device for trace gas detection. Two possible wavelength conversion processes are investigated: Difference Frequency Generation (DFG) and Stimulated Raman Scattering (SRS), which both are ruled by nonlinear optical frequency mixing principles. To our knowledge it is for the first time that Systems of such a kind are investigated with respect to their aptitude for trace gas monitoring. Previous experiments that are comparable make use of dye lasers instead of the OPO implemented for this work. Difference Frequency Generation is done by mixing the OPO radiation tuned between 1.4 (im and 1.85 im with residual fundamental radiation of the Nd:YAG pump laser at (im in a LiNbOß crystal. With this device a tunability from 2.5 to 4.5 (im at energies of up to 500 uj per pulse is achieved. The suitability of the source for trace gas detection is tested by recording PAS absorption spectra of individual gases (methanol, ethanol, isopentane, benzene and toluene at concentrations of 100 ppm) in the 3 (im ränge. Furthermore, mixtures of up to six gases with interfering spectral absorption signatures are analyzed. These mixtures always contain methane with an exactly known absorption spectrum that allows the wavelength calibration posterior to the recording of the spectra. This is necessary because no suitable monochromator for the implemented laser sources was available. With this DFG-spectrometer most organic substances are
6 detectable in concentrations down to a few ppm and methane even down to about 60 ppb. Several possible modifications of the detection system and of the DFG laser point to a possible improvement of these detection limits by up to three Orders of magnitude. A second approach to extend the tuning ränge of the OPO is based on Stimulated Raman Scattering (SRS) in hydrogen gas. The anticipated mid IR tuning ränge from 2.5 to 4.5 (im is covered with an OPO-pumped second order Stokes waveguide SRS laser. However, the generated energies are found in the uj-range. The poor conversion efficiency is mainly caused by the curvature of the implemented capillaries and by the rather bad beam quality of the OPO emission. Some interesting results such as the narrowing of the laser linewidth connected with the rather simple experimental setup required for a large tuning ränge indicate that OPO pumped SRS lasers may become a valid alternative to DFG sources. It is expected that the implementation of improved waveguides and Raman amplifiers will result in energies that are comparable generated with the DFG source. to those In view of a possible commercial implementation of an air pollution monitoring system based on continuously tunable lasers the analysis of the measured absorption spectra is of fundamental importance. Here one of the major problems arises from a miscalibrated or only inaccurately known wavelength scale. The measuring of the wavelength of a pulsed tunable laser is connected with considerable experimental efforts and expenses. As an alternative, a Computer algorithm is developed that recalibrates the wavelength scale of a measured spectrum on the basis of the spectrum of a well-known substance that is assumed to be part of the investigated sample. With this algorithm, which is based on a genetic code, the experimental tracking of the wavelength for trace gas spectroscopic purposes becomes obsolete.
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