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Tunable Far Infrared Laser Spectrometers G REVIEW ARTICLE Tunable far infrared laser spectrometers G. A. Blake,a) K. B. Laughlin,b, R C. Cohen, K. L. Busarow, D-H. Gwo,~) C. A. Schmuttenmaer, D. W. Steyert, and R. J. Saykally Department of Chemistry, University of California, and Materials and Chemical Sciences Division, Lawrence Berkeley Laboratory, Berkeley, California 94720 (Received 24 September 1990; acceptedfor publication 10 March 1991) The state of the art in far infrared (FIR) spectroscopyis reviewed. The development of tunable, coherent FIR radiation sources is discussed. Applications of tunable FIR laser spectrometersfor measurementof rotational spectra and dipole moments of molecular ions and free radicals, vibration-rotation-tunneling (VRT) spectra of weakly bound complexes, and vibration-rotation spectra of linear carbon clusters are presented.A detailed description of the Berkeley tunable FIR laser spectrometersis presentedin the following article. I. INTRODUCTION sub-Doppler resolution, and have certainly produced a considerable number of important results, they are, how- Defined most conveniently in terms of modern tech- ever, applicable only to paramagnetic or polar molecules, nology, the far infrared (FIR) region of the spectrum ex- and yield spectra that are more difficult to interpret. tends from the frequencieswhere “standard” submillime- There are numerous systems and phenomenaof great ter techniques begin to fail ( - 10 cm - ’ = 0.3 THz) to current interest in chemistry, physics, and biology, which those where lead-salt infrared diode laser technology be- could be very effectively studied by high resolution spec- comes operative ( -350 cm- ’ = 10.5 THz). In this fre- troscopy in the FIR. These include the determination of quency range, pure rotational spectra of light molecules intermolecular potential surfaces,studies of hydrogen bond and torsional (hindered rotation) spectra of nonrigid mol- tunneling dynamics, vibrational spectroscopyof metal and eculeshave been studied for many years. In terms of wave- covalent clusters, and studies of reactive molecular com- length, this spectral region (30-1000 ,um) is centerednear plexes. In order to addressthese systemsin a general way, the peak of the room temperature (3-300 K) blackbody tunable coherent sourcesof FIR radiation are required. In emission spectrum, and has accordingly been of great im- this review article we describe the development of such portance in the development of modern physics. In terms tunable FIR laser systemsand discusstheir employment in of energy, photons in this region (0.03-1.0 kcal/mole) are several of the contexts discussedabove. We begin with a less energetic than essentially all known hydrogen bond brief review of recent technological evolution that has (and, of course, chemical bond) strengths, but are about made these new experiments possible. the same magnitude as typical van der Waals bond strengths. II. A BRIEF HISTORY OF SPECTROSCOPY IN THE The extremely high resolution ( > 1 x 106) tradition- FAR INFRARED ally associatedwith microwave spectroscopy has been ex- tended throughout the mid-IR and into the far UV with A. Broadband spectroscopy the continued development and exploitation of modern la- As was the case for other spectral regions before the ser techniques.In contrast, the FIR is still often referred to invention of lasers, initial work in the FIR was performed as “the gap in the electromagneticspectrum, ” and remains with the use of the dispersive elements,such as diffraction relatively unexplored with high resolution techniques. In- gratings, or with Fourier transform spectrometers. Since stead, incoherent blackbody sources and dispersive or in- the throughput of Fourier transform instruments is so terferometric spectrometers have traditionally been em- large when compared with gratings (no small advantagein ployed in the FIR, yielding vastly lower sensitivity and a region where simply producing suitably intense radiation resolution than is now routinely achieved in other regions is difficult), Fourier transform spectroscopy (FTS) has of the spectrum. Exceptions to this scenario are the laser beenconsiderably more popular for spectral line work. The magnetic resonance”’ and laser stark spectroscopy3exper- earliest FTS spectrometersutilized stretched sheetsof plas- iments carried out over the last 15 years with line-tunable tic materials for beamsplitters, which accordingly produce FIR gas lasers. While these intracavity resonanceexperi- large gaps, or “nulls,” in the spectrum. In 1969, Martin ments have demonstrated extremely high sensitivity and and Puplett4 proposed and demonstrated a novel polariza- *‘Division of Geological and Planetary Science, California Institute of Technology, MS-170-25, Pasadena, CA 91125. “Research Laboratories, 727 Norristown Road, Rohm & Haas Company, Spring House, PA 19477. “Department of Physics, Hansen Laboratory (GP-B, MS-4085), Stanford University, Stanford, CA 94035. 1693Downloaded Rev. 08Sci. Mar Instrum. 2006 to62 131.215.225.174. (7), July 1991 Redistribution00346746/91/071693-08$02.00 subject to AIP license or copyright,@ 1991 American see http://rsi.aip.org/rsi/copyright.jsp institute of Physics 1693 tion interferometer that has found widespread application ple, with an input power of 200 mW from a klystron at 100 ever since, especially in our own work. By employing GHz, Rothermel, Phillips, and Keene’ report the genera- beamsplitters consisting of a finely spaced set of parallel tion of 1 mW (200 GHz), 3OpW (300 GHz), 1 PW (600 wires’ to transmit and reflect beams of opposite polariza- GHz), and 100 nW (900 GHz) on the various harmonics. tion, interferograms may be collected from nearly dc to For such systems, the crossover frequency for the achiev- frequencies as large as c/2d, whlered is the wire spacing. In able output power, as compared to typical laser sideband addition, sample and background data can be taken simul- generation spectrometers, is in the range 300-400 GHz. taneously, thereby producing interferograms which oscil- In higher efficiency multipliers, bandwidth is sacrificed late about the true zero level, allowing complex refractive for efficiency as tuning is used to optimize a given output indices and relative permittivicies to be measured across frequency. This can be particularly useful for analytical or the full FIR with a single device. The most modem polar- remote sensing applications where only a few particular ization FTS instruments use a folded optical configuration fequencies are required. For example, the optimized 350 to double the effective resolution, which is ultimately lim- GWz triplers offered by Millitech Corporation produce ap- ited to about 45-60 MHz.’ If cooled filters are used to proximately 1.5 mW over a 50 GHz range with an input restrict the bandwidths of the detectors, sensitivities as power of 40 mW. For operation at higher frequencies, the high as lo- I4 W/HZ”~ can be reached, enabling some tripler can be cascadedwith a 600 GHz doubler to provide reactive intermediates to be studied. a specified output power of 0.7 mW over a 100 GHz range The principal drawbacks of the Fourier transform with 10 mW input. Thus, a single tripler-doubler combi- technique, as compared to the use of narrowband radiation nation would produce 150 pctwof narrowband radiation at sources, are the much lower resolution and sensitivity lim- 600 GHz. Tunable radiation at frequencies below 650 GHz its obtained. For a single detector covering the entire far- can thus be produced at higher levels in narrow frequency infrared, FTS instruments become background limited un- bands using frequency multiplication methods than can be less the optics and chamber are cryogenically cooled. That generated with laser sideband radiation. These sources are is, under normal conditions the multiplex advantage of difficult to employ in general broadband applications, how- FTS instruments is lost unless narrowband detector arrays ever. are used. To date, however far-infrared detector arrays GaAs diodes have recently been fabricated with I-V have not advanced to a sufficient degree to warrant their curves specifically tailored to generate predominantly a sin- use. The current state of the art of FIR-FTS is depicted by gle high-order harmonic with increased efficiency. Selective the work of Johns,6 who has measured the absorption spec- enhancement of both the ninth harmonic as well as the fifth tra of several isotopes of water and many other species harmonic have been demonstrated.” This simplifies the from 20-350 cm - ’ using a Bomem DA3.002 spectrome- harmonic generation process, as stacks of multipliers can ter. The resolution of the instrument is 0.004 cm - ’ ( 120 be replaced to some extent by the diode fabrication process. MHz) with a frequency accuracy of 0.0002 cm - ’ (6 The major drawback at the moment is the large parasitic MHz), using calibration gasessuch as HF, HCl, and H,G. capacitance of the tailored diodes, which limits their use By averaging spectra over limited frequency intervals for above 300 GHz. the entire hold time of the cryogenic detectors (approxi- mately one full day), a noise level of approximately 1% is C. Backward wave oscillators and laser diodes reached. The use of currently available Ge detector arrays Spectroscopic methods having potentially high sensi- could lower this noise limit by a.factor of 10, although the tivity throughout the 300-1500 GHz region have been minimum attainable linewidth would still remain one or demonstrated by Krupnov and his colleagues in the two orders
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