Abstract

Spectroscopy in the molecular fingerprint spectral region (6.7–20 µm) yields critical information on material structure for physical, chemical, and biological sciences. Despite decades of interest and effort, this portion of the electromagnetic spectrum remains challenging to cover with conventional laser technologies. In this paper, we present a simple and robust method for generating super-octave, optical frequency combs in the fingerprint region through intra-pulse difference frequency generation in an orientation-patterned gallium phosphide crystal. The attainable brightness from this tabletop source reaches the same level achievable by infrared synchrotron radiation with a bandwidth spanning from 4 to 12 µm. We demonstrate the utility of this unique coherent light source for high-precision, dual-frequency-comb spectroscopy of methanol and ethanol vapor. These results highlight the potential of laser frequency combs for a wide range of infrared molecular sensing applications from basic molecular spectroscopy to nanoscopic imaging.

© 2018 Optical Society of America under the terms of the OSA Open Access Publishing Agreement

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References

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2018 (4)

G. Ycas, F. R. Giorgetta, E. Baumann, I. Coddington, D. Herman, S. A. Diddams, and N. R. Newbury, “High-coherence mid-infrared dual-comb spectroscopy spanning 2.6 to 5.2 µm,” Nat. Photonics 12, 202–208 (2018).
[Crossref]

A. V. Muraviev, V. O. Smolski, Z. E. Loparo, and K. L. Vodopyanov, “Massively parallel sensing of trace molecules and their isotopologues with broadband subharmonic mid-infrared frequency combs,” Nat. Photonics 12, 209–214 (2018).
[Crossref]

N. Nader, D. L. Maser, F. C. Cruz, A. Kowligy, H. Timmers, J. Chiles, C. Fredrick, D. A. Westly, S. W. Nam, R. P. Mirin, J. M. Shainline, and S. Diddams, “Versatile silicon-waveguide supercontinuum for coherent mid-infrared spectroscopy,” APL Photon. 3, 036102 (2018).
[Crossref]

A. S. Kowligy, A. Lind, D. D. Hickstein, D. R. Carlson, H. Timmers, N. Nader, F. C. Cruz, G. Ycas, S. B. Papp, and S. A. Diddams, “Mid-infrared frequency comb generation via cascaded quadratic nonlinearities in quasi-phase-matched waveguides,” Opt. Lett. 43, 1678–1681 (2018).
[Crossref]

2017 (4)

K. F. Lee, C. J. Hensley, P. G. Schunemann, and M. E. Fermann, “Midinfrared frequency comb by difference frequency of erbium and thulium fiber lasers in orientation-patterned gallium phosphide,” Opt. Express 25, 17411–17416 (2017).
[Crossref]

C. Riek, P. Sulzer, M. Seeger, A. S. Moskalenko, G. Burkard, D. V. Seletskiy, and A. Leitenstorfer, “Subcycle quantum electrodynamics,” Nature 541, 376–379 (2017).
[Crossref]

O. Kara, L. Maidment, T. Gardiner, P. G. Schunemann, and D. T. Reid, “Dual-comb spectroscopy in the spectral fingerprint region using OPGaP optical parametric oscillators,” Opt. Express 25, 32713–32721 (2017).
[Crossref]

A. Dazzi and C. B. Prater, “AFM-IR: technology and applications in nanoscale infrared spectroscopy and chemical imaging,” Chem. Rev. 117, 5146–5173 (2017).
[Crossref]

2016 (6)

2015 (5)

F. C. Cruz, D. L. Maser, T. Johnson, G. Ycas, A. Klose, F. R. Giorgetta, I. Coddington, and S. A. Diddams, “Mid-infrared optical frequency combs based on difference frequency generation for molecular spectroscopy,” Opt. Express 23, 26814–26824 (2015).
[Crossref]

S. Guha, J. O. Barnes, and P. G. Schunemann, “Mid-wave infrared generation by difference frequency mixing of continuous wave lasers in orientation-patterned gallium phosphide,” Opt. Mater. Express 5, 2911–2923 (2015).
[Crossref]

C. Riek, D. V. Seletskiy, A. S. Moskalenko, J. F. Schmidt, P. Krauspe, S. Eckart, S. Eggert, G. Burkard, and A. Leitenstorfer, “Direct sampling of electric-field vacuum fluctuations,” Science 350, 420–423 (2015).
[Crossref]

B. Pollard, F. C. B. Maia, M. B. Raschke, and R. O. Freitas, “Infrared vibrational nanospectroscopy by self-referenced interferometry,” Nano Lett. 16, 55–61 (2015).
[Crossref]

I. Pupeza, D. Sanchez, J. Zhang, N. Lilienfein, M. Seidel, N. Karpowicz, T. Paasch-Colberg, I. Znakovskaya, M. Pescher, W. Schweinberger, V. Pervak, E. Fill, O. Pronin, Z. Wei, F. Krausz, A. Apolonski, and J. Biegert, “High-power sub-two-cycle mid-infrared pulses at 100 MHz repetition rate,” Nat. Photonics 9, 721–724 (2015).
[Crossref]

2014 (1)

2013 (2)

T. Ideguchi, S. Holzner, B. Bernhardt, G. Guelachvili, N. Picqué, and T. W. Hänsch, “Coherent Raman spectro-imaging with laser frequency combs,” Nature 502, 355–358 (2013).
[Crossref]

L. S. Rothman, I. E. Gordon, Y. Babikov, A. Barbe, D. C. Benner, P. F. Bernath, M. Birk, L. Bizzocchi, V. Boudon, L. R. Brown, A. Campargue, K. Chance, E. A. Cohen, L. H. Coudert, V. M. Devi, B. J. Drouin, A. Fayt, J.-M. Flaud, R. R. Gamache, J. J. Harrison, J.-M. Hartmann, C. Hill, J. T. Hodges, D. Jacquemart, A. Jolly, J. Lamourouxk, R. J. LeRoy, G. Li, D. A. Long, O. M. Lyulin, C. J. Mackie, S. T. Massie, S. Mikhailenko, H. S. P. Müller, O. V. Naumenko, A. V. Nikitin, J. Orphal, V. Perevalov, A. Perrin, E. R. Polovtseva, C. Richard, M. A. H. Smith, E. Starikova, K. Sung, S. Tashkun, J. Tennyson, G. C. Toon, V. G. Tyuterev, and G. Wagner, “The HITRAN2012 molecular spectroscopic database,” J. Quant. Spectrosc. Radiat. Transfer 130, 4–50 (2013).
[Crossref]

2012 (3)

J. J. Harrison, N. D. C. Allen, and P. F. Bernath, “Infrared absorption cross sections for methanol,” J. Quant. Spectrosc. Radiat. Transfer 113, 2189–2196 (2012).
[Crossref]

A. Schliesser, N. Picqué, and T. W. Hänsch, “Mid-infrared frequency combs,” Nat. Photonics 6, 440–449 (2012).
[Crossref]

A. Hugi, G. Villares, S. Blaser, H. C. Liu, and J. Faist, “Mid-infrared frequency comb based on a quantum cascade laser,” Nature 492, 229–233 (2012).
[Crossref]

2010 (3)

B. Bernhardt, A. Ozawa, P. Jacquet, M. Jacquey, Y. Kobayashi, T. Udem, R. Holzwarth, G. Guelachvili, T. W. Hänsch, and N. Picqué, “Cavity-enhanced dual-comb spectroscopy,” Nat. Photonics 4, 55–57 (2010).
[Crossref]

F. Adler, P. Maslowski, A. Foltynowicz, K. C. Cossel, T. C. Briles, I. Hartl, and J. Ye, “Mid-infrared Fourier transform spectroscopy with a broadband frequency comb,” Opt. Express 18, 21861–21872 (2010).
[Crossref]

M. Conforti, F. Baronio, and C. D. Angelis, “Nonlinear envelope equation for broadband optical pulses in quadratic media,” Phys. Rev. A 81, 053841 (2010).
[Crossref]

2007 (1)

2006 (1)

P. Roy, M. Rouziéres, Z. Qi, and O. Chubar, “The AILES infrared beamline on the third generation synchrotron radiation facility SOLEIL,” Infrared Phys. Technol. 49, 139–146 (2006).
[Crossref]

2004 (2)

2000 (3)

R. A. Bosch, “Computed flux and brightness of infrared edge and synchrotron radiation,” Nucl. Instrum. Methods Phys. Res. Sect. A 454, 497–505 (2000).
[Crossref]

D. D. S. Hale, M. Bester, W. C. Danchi, W. Fitelson, S. Hoss, E. A. Lipman, J. D. Monnier, P. G. Tuthill, and C. H. Townes, “The Berkeley infrared spatial interferometer: a heterodyne stellar interferometer for the mid-infrared,” Astrophys. J. 537, 998–1012 (2000).
[Crossref]

R. Huber, A. Brodschelm, F. Tauser, and A. Leitenstorfer, “Generation and field-resolved detection of femtosecond electromagnetic pulses tunable up to 41 THz,” Appl. Phys. Lett. 76, 3191–3193 (2000).
[Crossref]

1997 (1)

1995 (1)

A. Bonvalet, M. Joffre, J. L. Martin, and A. Migus, “Generation of ultrabroadband femtosecond pulses in the mid-infrared by optical rectification of 15 fs light pulses at 100 MHz repetition rate,” Appl. Phys. Lett. 67, 2907–2909 (1995).
[Crossref]

Adler, F.

Allen, N. D. C.

J. J. Harrison, N. D. C. Allen, and P. F. Bernath, “Infrared absorption cross sections for methanol,” J. Quant. Spectrosc. Radiat. Transfer 113, 2189–2196 (2012).
[Crossref]

Allison, T. K.

Angelis, C. D.

M. Conforti, F. Baronio, and C. D. Angelis, “Nonlinear envelope equation for broadband optical pulses in quadratic media,” Phys. Rev. A 81, 053841 (2010).
[Crossref]

Apolonski, A.

I. Pupeza, D. Sanchez, J. Zhang, N. Lilienfein, M. Seidel, N. Karpowicz, T. Paasch-Colberg, I. Znakovskaya, M. Pescher, W. Schweinberger, V. Pervak, E. Fill, O. Pronin, Z. Wei, F. Krausz, A. Apolonski, and J. Biegert, “High-power sub-two-cycle mid-infrared pulses at 100 MHz repetition rate,” Nat. Photonics 9, 721–724 (2015).
[Crossref]

Babikov, Y.

L. S. Rothman, I. E. Gordon, Y. Babikov, A. Barbe, D. C. Benner, P. F. Bernath, M. Birk, L. Bizzocchi, V. Boudon, L. R. Brown, A. Campargue, K. Chance, E. A. Cohen, L. H. Coudert, V. M. Devi, B. J. Drouin, A. Fayt, J.-M. Flaud, R. R. Gamache, J. J. Harrison, J.-M. Hartmann, C. Hill, J. T. Hodges, D. Jacquemart, A. Jolly, J. Lamourouxk, R. J. LeRoy, G. Li, D. A. Long, O. M. Lyulin, C. J. Mackie, S. T. Massie, S. Mikhailenko, H. S. P. Müller, O. V. Naumenko, A. V. Nikitin, J. Orphal, V. Perevalov, A. Perrin, E. R. Polovtseva, C. Richard, M. A. H. Smith, E. Starikova, K. Sung, S. Tashkun, J. Tennyson, G. C. Toon, V. G. Tyuterev, and G. Wagner, “The HITRAN2012 molecular spectroscopic database,” J. Quant. Spectrosc. Radiat. Transfer 130, 4–50 (2013).
[Crossref]

Barbe, A.

L. S. Rothman, I. E. Gordon, Y. Babikov, A. Barbe, D. C. Benner, P. F. Bernath, M. Birk, L. Bizzocchi, V. Boudon, L. R. Brown, A. Campargue, K. Chance, E. A. Cohen, L. H. Coudert, V. M. Devi, B. J. Drouin, A. Fayt, J.-M. Flaud, R. R. Gamache, J. J. Harrison, J.-M. Hartmann, C. Hill, J. T. Hodges, D. Jacquemart, A. Jolly, J. Lamourouxk, R. J. LeRoy, G. Li, D. A. Long, O. M. Lyulin, C. J. Mackie, S. T. Massie, S. Mikhailenko, H. S. P. Müller, O. V. Naumenko, A. V. Nikitin, J. Orphal, V. Perevalov, A. Perrin, E. R. Polovtseva, C. Richard, M. A. H. Smith, E. Starikova, K. Sung, S. Tashkun, J. Tennyson, G. C. Toon, V. G. Tyuterev, and G. Wagner, “The HITRAN2012 molecular spectroscopic database,” J. Quant. Spectrosc. Radiat. Transfer 130, 4–50 (2013).
[Crossref]

Barnes, J. O.

Baronio, F.

M. Conforti, F. Baronio, and C. D. Angelis, “Nonlinear envelope equation for broadband optical pulses in quadratic media,” Phys. Rev. A 81, 053841 (2010).
[Crossref]

Baumann, E.

G. Ycas, F. R. Giorgetta, E. Baumann, I. Coddington, D. Herman, S. A. Diddams, and N. R. Newbury, “High-coherence mid-infrared dual-comb spectroscopy spanning 2.6 to 5.2 µm,” Nat. Photonics 12, 202–208 (2018).
[Crossref]

G. B. Rieker, F. R. Giorgetta, W. C. Swann, J. Kofler, A. M. Zolot, L. C. Sinclair, E. Baumann, C. Cromer, G. Petron, C. Sweeney, P. P. Tans, I. Coddington, and N. R. Newbury, “Frequency-comb-based remote sensing of greenhouse gases over kilometer paths,” Optica 1, 290–298 (2014).
[Crossref]

Benner, D. C.

L. S. Rothman, I. E. Gordon, Y. Babikov, A. Barbe, D. C. Benner, P. F. Bernath, M. Birk, L. Bizzocchi, V. Boudon, L. R. Brown, A. Campargue, K. Chance, E. A. Cohen, L. H. Coudert, V. M. Devi, B. J. Drouin, A. Fayt, J.-M. Flaud, R. R. Gamache, J. J. Harrison, J.-M. Hartmann, C. Hill, J. T. Hodges, D. Jacquemart, A. Jolly, J. Lamourouxk, R. J. LeRoy, G. Li, D. A. Long, O. M. Lyulin, C. J. Mackie, S. T. Massie, S. Mikhailenko, H. S. P. Müller, O. V. Naumenko, A. V. Nikitin, J. Orphal, V. Perevalov, A. Perrin, E. R. Polovtseva, C. Richard, M. A. H. Smith, E. Starikova, K. Sung, S. Tashkun, J. Tennyson, G. C. Toon, V. G. Tyuterev, and G. Wagner, “The HITRAN2012 molecular spectroscopic database,” J. Quant. Spectrosc. Radiat. Transfer 130, 4–50 (2013).
[Crossref]

Bernath, P. F.

L. S. Rothman, I. E. Gordon, Y. Babikov, A. Barbe, D. C. Benner, P. F. Bernath, M. Birk, L. Bizzocchi, V. Boudon, L. R. Brown, A. Campargue, K. Chance, E. A. Cohen, L. H. Coudert, V. M. Devi, B. J. Drouin, A. Fayt, J.-M. Flaud, R. R. Gamache, J. J. Harrison, J.-M. Hartmann, C. Hill, J. T. Hodges, D. Jacquemart, A. Jolly, J. Lamourouxk, R. J. LeRoy, G. Li, D. A. Long, O. M. Lyulin, C. J. Mackie, S. T. Massie, S. Mikhailenko, H. S. P. Müller, O. V. Naumenko, A. V. Nikitin, J. Orphal, V. Perevalov, A. Perrin, E. R. Polovtseva, C. Richard, M. A. H. Smith, E. Starikova, K. Sung, S. Tashkun, J. Tennyson, G. C. Toon, V. G. Tyuterev, and G. Wagner, “The HITRAN2012 molecular spectroscopic database,” J. Quant. Spectrosc. Radiat. Transfer 130, 4–50 (2013).
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Supplementary Material (2)

NameDescription
» Supplement 1       Supplemental material
» Visualization 1       Experimental demonstration of molecular fingerprinting with the longwave infrared frequency combs using dual comb spectroscopy.

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Figures (4)

Fig. 1.
Fig. 1. Experimental layout for intra-pulse DFG comb generation. (a) Conceptually, in the time domain (top panel) a few-cycle pulse undergoes intra-pulse DFG within a quasi-phase-matched, nonlinear crystal, leading to the generation of radiation with a longer optical period than the pump pulse. In the frequency domain (bottom panel), the various comb modes within the few-cycle pulse spectrum mix within the crystal, leading to the generation of down-converted light lying within the molecular fingerprint window. (b) Experimentally, the output of a Er mode-locked laser (MLL) is amplified using an Er-doped fiber amplifier (EDFA) and undergoes nonlinear broadening within a normal dispersion highly nonlinear fiber (ND-HNLF). The positive chirp accumulated within the ND-HNLF is compensated for using a pair of fused silica wedges, resulting in a few-cycle pump pulse. The spectrum of this few-cycle driver is shown in (c). The inset of (c) displays the measured intensity profile of the pump pulse, corresponding to a pulse duration of 10.6 fs. (d) When the pump pulse is focused into an OP-GaP crystal, we generate super-octave LWIR spectra containing up to 0.25 mW of power. This spectrum is well reproduced by simulation.
Fig. 2.
Fig. 2. Brightness comparison between broadband infrared sources. The brightness of the experimental and simulated intra-pulse DFG spectrum is plotted in comparison to more conventional broadband infrared sources. This experimental source is significantly brighter than a blackbody lamp and on par with the maximum brightness attainable from a synchrotron infrared user facility.
Fig. 3.
Fig. 3. Dual-comb spectroscopy of methanol and ethanol. (a) In the time domain, the multi-heterodyne signal from two LWIR frequency combs results in a periodic interferogram with a recurrence period of 1/δfrep=20  ms. A sequence of 5 interferograms is shown in the inset (top) for the acquisition of comb-tooth resolved spectra. The free-induction decay signature of molecular absorption is shown in the bottom inset, highlighting the high temporal resolution of a complete absorption cycle. (b) The measured DCS absorbance spectrum of methanol at low pressure (blue curve) compared against the methanol spectrum from the HITRAN2012 reference model [34] (red, reflected about origin). The overlaying black curves are the experimental and modeled spectra for methanol acquired at atmospheric pressure. (c) To demonstrate the resolution and agreement, we plot a 2  cm1 subset of the spectrum around 993.5  cm1. (d) The DCS spectrum arising from the phase-coherent acquisition of multiple interferograms resolves the individual 100 MHz comb modes, represented as open circles. (e) We also collect an ethanol DCS spectrum (blue) spanning a 700  cm1 window around 1050  cm1 to demonstrate the broadband acquisition capabilities of the LWIR frequency comb. The experimental spectrum agrees well with the PNNL reference model [35].
Fig. 4.
Fig. 4. Time-series analysis of methanol evaporation. (a) A time series of DCS spectra collected during the evaporation of methanol within the absorption gas cell. (b) The measured average absorbance demonstrates the ability of LWIR-based DCS in detecting transient changes in a reaction occurring on a few-second time scale. (c) Spectral line outs of the time series taken along the lines denoted by (i), (ii), and (iii) in (a). Even with a short averaging time of 2 s per time step, we can achieve simultaneous high spectral resolution (7 GHz) and high signal-to-noise ratio (SNR=67  Hz1/2).

Equations (1)

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A(ω)=ln[|I˜A(ω)||I˜o(ω)|],

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