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Optics Express

Optics Express

  • Editor: C. Martijn de Sterke
  • Vol. 19, Iss. 18 — Aug. 29, 2011
  • pp: 16985–16995
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Highly efficient THG in TiO2 nanolayers for third-order pulse characterization

Susanta Kumar Das, Christoph Schwanke, Andreas Pfuch, Wolfgang Seeber, Martin Bock, Günter Steinmeyer, Thomas Elsaesser, and Ruediger Grunwald  »View Author Affiliations


Optics Express, Vol. 19, Issue 18, pp. 16985-16995 (2011)
http://dx.doi.org/10.1364/OE.19.016985


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Abstract

Third harmonic generation (THG) of femtosecond laser pulses in sputtered nanocrystalline TiO2 thin films is investigated. Using layers of graded thickness, the dependence of THG on the film parameters is studied. The maximum THG signal is observed at a thickness of 180 nm. The corresponding conversion efficiency is 26 times larger compared to THG at the air-glass interface. For a demonstration of the capabilities of such a highly nonlinear material for pulse characterization, third-order autocorrelation and interferometric frequency-resolved optical gating (IFROG) traces are recorded with unamplified nanojoule pulses directly from a broadband femtosecond laser oscillator.

© 2011 OSA

1. Introduction

Here we report essential progress in this field. Employing nanocrystalline TiO2 thin films, THG signal enhancement up to 26 times above the value for the air-glass interface is observed. The properties of the THG are discussed, and immediate application for ultrashort-pulse characterization by third-order autocorrelation and interferometric frequency-resolved optical gating (IFROG) is presented.

2. Experimental details

2.1. Preparation and characterization of nanocrystalline layers

Thin TiO2 nanolayers were deposited by reactive dc-sputtering in a vacuum chamber using a two-inch metallic titanium target. Before depositing, the chamber was evacuated to a base pressure below 10−4 Pa. Sputtering was performed in the low pressure region with an argon-oxygen-atmosphere at a partial pressure ratio of 2:1 (argon partial pressure about 1,5*10−3 mbar and an oxygen partial pressure of about 0,7 * 10−3 mbar, respectively) with constant power of 200 W and a target-to-substrate distance of 5 cm. Formerly, the total sputtering pressure was varied to influence the morphology of the growing film as well as the formation and the amount of crystalline phases in the films [12

12. T. Tölke, A. Kriltz, and A. Rechtenbach, “The influence of pressure on the structure and the self-cleaning properties of sputter deposited TiO2 layers,” Thin Solid Films 518(15), 4242–4246 (2010). [CrossRef]

]. The thin films were deposited onto thin glass substrates (microscope slides). Prior to this deposition, a reactively sputtered SiO2 barrier layer was deposited to prevent unwanted alkali migration from the glass into the TiO2-layer. The samples were investigated (a) as-deposited and (b) after annealing at 723 K for one hour in air. As the annealed samples exhibit slightly higher nonlinearities, we focus on their discussion in the following. Film thickness and optical properties were characterized by a mechanical stylus profilometer (Dektak 3 ST, Veeco) and spectral ellipsometry (SE850, Sentech). The first main objective of this work was to experimentally identify the optimum thickness for efficient THG. For a sufficiently large thickness difference over the sputtered area, glass substrates with dimensions of about 70 x 22 mm2 were used. Measurements indicate a well-defined variation in layer thickness ranging from 105 to 420 nm. Thickness data and refractive indices determined at discrete positions (step width 6.25 mm) of the sample are plotted in Fig. 1(a)
Fig. 1 Titanium dioxide nanolayers for highly efficient nonlinear frequency conversion: (a) Measured values of thickness (circles) and refractive indices (squares) at different positions, (b)-(c) Surface morphology of the granular surface at two selected positions corresponding to thicknesses of ~180 and 400 nm, respectively, detected by scanning electron microsopy. Inset of (a): optical image of a graded thin film. The spatially varying thickness is indicated by Newton's rings.
. Over a large thickness range between 150 and 375 nm, the refractive index was found to remain nearly constant, i.e. n ≈2.3, close to the value reported for TiO2 thin films grown by electron beam evaporation [13

13. S. Y. Kim, “Simultaneous determination of refractive index, extinction coefficient, and void distribution of titanium dioxide thin film by optical methods,” Appl. Opt. 35(34), 6703–6707 (1996). [CrossRef] [PubMed]

]. The SEM images in Figs. 1(b)1(c) reveal the differences in the surface structure at two different positions of a graded thickness TiO2 thin film. At a thickness of 180 nm, the surface consists of nanograins with an average size of about 20 nm [Fig. 1(b)], whereas the layer appears to be much smoother at a thickness of 400 nm [Fig. 1(c)]. We attribute the higher index of refraction measured for large thickness to this change of morphology. The inset of Fig. 1(a) shows the optical image of a gradient layer sample. The thickness variation is directly visible from the differently colored zones (Newton's rings).

The X-ray diffraction pattern for the sample with 180 nm thickness is shown in Fig. 2
Fig. 2 X-ray diffraction pattern of TiO2 film (thickness 180 nm); the most prominent peak indicates the anatase phase.
. For higher thickness, a nearly identical pattern was observed, indicating anatase (101) as the prevalent phase together with a small amount of the rutile (110) phase. The damage threshold fluence of TiO2 thin film is ~0.3 J/cm2 for a pulse duration of 150 fs [14

14. S. K. Das, A. Rosenfeld, M. Bock, A. Pfuch, W. Seeber, and R. Grunwald, “Scattering-controlled femtosecond-laser induced nanostructuring of TiO2 thin films,” Proc. SPIE 7925, 79251B (2011). [CrossRef]

]. This value is expected to further reduce for the shorter pulses.

2.2. Third-harmonic generation

THG studies were performed by exciting the samples with a Ti:sapphire laser oscillator (Femtosource) capable of emitting linearly polarized 15 fs pulses at a repetition rate of 75.3 MHz, a pulse energy of 4 nJ, and a central wavelength near 800 nm. The experimental setup is schematically shown in Fig. 3
Fig. 3 Experimental setup for detecting the THG signal of nanolayers and performing highly sensitive pulse characterization by third-order autocorrelation and IFROG measurements (schematically). BS = beam splitter; OF = optical fiber, Mono/EMCCD = electron multiplier charge coupled device based spectrometer, L = lens (f = 12 mm) or concave mirror (f = 25 mm), MO = UV microscope objective, IF = 2 interference filters (266 nm, bandwidth 40 nm FWHM), M = HR mirrors (266 nm for comparative pulse characterization only).
. The experiments were done either without the Michelson interferometer (for THG study) or with it (for pulse characterizations). The laser pulses were tightly focused onto the samples under normal incidence. The generated THG signal was collected in transmission direction by a UV transmitting microscope objective. The THG spectrum was mostly separated from residual pump radiation by two interference filters. In some cases one or two additional highly reflecting mirrors at 266 nm were also used. The generated signal was analyzed with a fiber-coupled grating spectrometer (HR 2000, Ocean Optics) and a high-sensitivity electron multiplier charge coupled device (EMCCD) based spectrometer (Newton, Andor Technology). All experiments were carried out at room temperature. The EMCCD detector was thermo-electrically cooled down to −75°C. The input power dependence was studied by varying the intensity with a set of neutral density filters.

2.3. Third-order pulse characterization

To demonstrate the applicability to the characterization of ultrashort pulses, third-order interferometric autocorrelation [6

6. D. Meshulach, Y. Barad, and Y. Silberberg, “Measurement of ultrashort optical pulses by third-harmonic generation,” J. Opt. Soc. Am. B 14(8), 2122–2125 (1997). [CrossRef]

] and frequency-resolved optical gating (IFROG) [15

15. T. Utikal, T. Zentgraf, J. Kuhl, and H. Giessen, “Dynamics and dephasing of plasmon polaritons in metallic photonic crystal superlattices: time- and frequency-resolved nonlinear autocorrelation measurements and simulations,” Phys. Rev. B 76(24), 245107 (2007). [CrossRef]

20

20. I. Amat-Roldán, I. G. Cormack, P. Loza-Alvarez, E. J. Gualda, and D. Artigas, “Ultrashort pulse characterisation with SHG collinear-FROG,” Opt. Express 12(6), 1169–1178 (2004). [CrossRef] [PubMed]

] were implemented experimentally. Using the Michelson interferometer, the input pulses were split into two replicas using a broadband dielectric beam splitter (Venteon). A 25 mm focal length concave mirror or a lens of focal length 12 mm was used to generate the THG, and the EMCCD based spectrometer served for frequency-resolved detection. The total THG signal was deduced from this signal by spectral integration, yielding the autocorrelation signal as a function of temporal delay.

3. Results and discussion

3.1. Optimum thickness for efficient THG

The thickness-dependent THG is depicted in Fig. 4(a)
Fig. 4 Analysis of the THG properties: (a) Thickness dependent THG from a graded TiO2 thin film. (b) THG signal as a function of the input power. The slope of ≈3 indicates the third-order process. (c) THG spectrum of a uniform TiO2 nanolayer with a thickness of 180 nm in comparison to the measured THG of a reference air-glass interface. Inset: spectrum of air-glass interface THG at different vertical scale (to improve the visibility).
, clearly illustrating increasing dephasing between fundamental and THG signal for increasing length. From this oscillating curve we deduce a thickness of 180 nm for the strongest THG signal.

In general, the highest frequency conversion efficiency is achieved when the thickness is equal to the coherence length (LC) of the nonlinear optical interaction. For the THG process, this length is defined by
LC=λ6(n3n1),
(1)
wheren1is refractive index of the material at the fundamental wavelength and n3that at THG wavelength. The value of Lc calculated from Eq. (1) was found to be 190 nm, thereby approximately confirming the experimental value of thickness for highest THG. For this calculation the refractive indices were taken from [13

13. S. Y. Kim, “Simultaneous determination of refractive index, extinction coefficient, and void distribution of titanium dioxide thin film by optical methods,” Appl. Opt. 35(34), 6703–6707 (1996). [CrossRef] [PubMed]

], in which the data for the transmission region were similar to our experimental findings for lower thickness. To further verify the result, the thickness dependence was tested with a discrete set of TiO2 nanolayer samples of different, but uniform thickness. As in the first experiment with graded layers, a thickness close to 180 nm is found to exhibit the highest THG efficiency. All details on THG signal analysis and applications to pulse diagnostics reported below refer to this one optimized uniform sample. The appearance of a second peak according to the signal dependence on the coherence length was expected for a larger thickness than 350 nm as it is indicated by the experimental results in Fig. 4(a).

The fast damped oscillation behavior and the appearance of a second peak at 350 nm deviates from the expected ideal characteristics, according to which the THG signal should show a gradual decrease with subsequent gradual increase towards 570 nm position. The fast deviating signal after the peak at 180 nm is explained by a significant contribution the Fabry-Pérot interference of the fundamental in the layer. This was verified by numerical simulations.

The reason for the modified curve at larger thickness, however, may only be understood by assuming a distinct change of the stoichiometry. Indeed, this becomes obvious from Fig. 1(a) in which the refractive index undergoes an extremely steep rise toward higher thickness, and from the corresponding structural change (strongly decreasing roughness, Figs. 1(b) and 1(c)). The local intra-layer variation of stoichiometry, however, is still the subject of investigations by independent physico-chemical analytical techniques.

3.2. Analysis of the THG signal

According to the expectations, the generated THG signal strength scales with third power of the input signal strength (straight line in the logarithmic plot in Fig. 4(b)). The THG spectrum generated from the thin film [Fig. 4(c)] exhibits a FWHM bandwidth of 22 nm and is centered at a wavelength of 272 nm. For comparison, the air-glass interface THG signal detected under the same experimental conditions is displayed in the inset of Fig. 4(c). For the latter case, the spectral properties appeared to be quite similar to those obtained with the TiO2 thin films.

The spectral characteristics corroborate that the TiO2 thin films are, in fact, a viable alternative for obtaining reliable THG over the full bandwidth of a broadband Ti:sapphire laser oscillator. From Fig. 4(c) an enhancement factor of about 26 (ratio between the THG from 180 nm TiO2 nanolayers and the value for the air-glass interface) was found. The estimation of third-order nonlinearity from a comparison of THG signals in the presence and absence of the thin film is a proven standard method [10

10. R. Barille, L. Canioni, L. Sarger, and G. Rivoire, “Nonlinearity measurements of thin films by third-harmonic-generation microscopy,” Phys. Rev. E Stat. Nonlin. Soft Matter Phys. 66(6), 067602 (2002). [CrossRef] [PubMed]

]. For focused Gaussian beams, the THG intensities without and with film can be expressed by Eqs. (2) and (3), respectively:

I(3ω)sub=HIω3|χsubJ(b,Δksub)|2,
(2)
I(3ω)sub+tf=HIω3|χsubJ(b,Δksub)χtfJ(b,Δktf)|2.
(3)

3.3. Application to third-order ultrashort pulse characterization

Figure 5(a)
Fig. 5 Third-order pulse characterization experiments with optimized TiO2 nanolayers: (a) THG autocorrelation and (b) IFROG trace of a 15-fs pulse, (c) Retrieved spectral signal (blue rectangles) and spectral phase (red circles) from IFROG algorithm (including a marginal test of the retrieved signal with the reference signal, see the retrieved spectrum).
shows a third-order interferometric autocorrelation trace recorded for with a pulse energy of 0.6 nJ (EMCCD detector exposure time 10 ms, gain = 0). For generating this trace, the concave mirror of f = 25 mm was used, and only interference filters were employed to suppress the residual fundamental. In accordance with theory [7

7. T. Tsang, M. A. Krumbügel, K. W. Delong, D. N. Fittinghoff, and R. Trebino, “Frequency-resolved optical-gating measurements of ultrashort pulses using surface third-harmonic generation,” Opt. Lett. 21(17), 1381–1383 (1996). [CrossRef] [PubMed]

], the peak-to-background ratio is found to be close to 32:1. Figure 5(b) shows a spectrally resolved representation of the same measurement, yielding a high-contrast third-order IFROG trace. IFROG is a collinear variant of FROG that is particularly suited for few-cycle pulses [16

16. G. Stibenz and G. Steinmeyer, “Interferometric frequency-resolved optical gating,” Opt. Express 13(7), 2617–2626 (2005). [CrossRef] [PubMed]

18

18. A. Anderson, K. S. Deryckx, X. G. Xu, G. Steinmeyer, and M. B. Raschke, “Few-femtosecond plasmon dephasing of a single metallic nanostructure from optical response function reconstruction by interferometric frequency resolved optical gating,” Nano Lett. 10(7), 2519–2524 (2010). [CrossRef] [PubMed]

]. IFROG offers two independent ways of retrieving pulse shapes and offers added internal consistency checks, in particular for calibrating the delay axis. Here we restrict ourselves to analyzing the unmodulated dc part of the trace that we extract by Fourier filtering. The resulting THG-FROG trace can then directly be processed by a standard pulse retrieval software (Femtosoft Technologies, FROG 3.0).The retrieved spectral signal and spectral phase are shown in Fig. 5(c). The corresponding pulse duration is determined as 22 fs. The spectral phase information [red circles, Fig. 5(c)] indicates the presence of a positive quadratic chirp. Due to this chirp, the measured pulse duration is found to be larger than the input duration of 15 fs, which we attribute mostly to the beam splitters used in this study.

We performed a marginal test, comparing the retrieved and an independently measured fundamental spectrum [dashed line Fig. 5(c)]. Even though the agreement may not be perfect, there are no indications of a major loss of bandwidth. As the retrieved spectrum appears enhanced on the short wavelength side, the deviations are indicative of an increase of nonlinearity with shorter wavelength, which may be explained by resonant enhancement of the nonlinearity in the vicinity of the bandgap. A certain influence may also come from the relatively strong filtering required for rejection of the fundamental in collinear techniques. Considering the challenges of measuring oscillator pulses with third-order FROG methods [19

19. G. Ramos-Ortiz, M. Cha, S. Thayumanavan, J. Mendez, S. R. Marder, and B. Kippelen, “Ultrafast-pulse diagnostic using third-order frequency-resolved optical gating in organic films,” Appl. Phys. Lett. 85(16), 3348–3350 (2004). [CrossRef]

], we therefore believe that nanocrystalline TiO2 thin films provide a viable alternative for characterizing ultrashort pulses, with the added advantage of time-symmetry disambiguation.

In order to demonstrate the performance of the TiO2 THG based pulse characterization system relative to STHG at the air-glass interface, we did the comparative study of linear chirp measurements. For these measurements, we employed tighter focusing with the 4 mm thick flint glass lens (f = 12 mm), which exhibits a group-delay dispersion of 500 fs2. In the case of air-glass STHG, it was considerably more difficult to suppress residual fundamental light. Therefore an additional filter (HR at 266 nm) was used, and the same condition was maintained for THG of TiO2 to ensure equal experimental conditions in both cases. The interferometric autocorrelation trace measured with STHG (exposure time = 200 ms) and THG in TiO2 (exposure time = 10 ms) are shown in Figs. 6(a)
Fig. 6 Interferometric autocorrelation of a chirped pulse taken with air-glass STHG (a) and THG of TiO2 thin film. (b) exposure times were 200 and 10 ms, respectively. Abscissas are scaled in relative units to demonstrate the 1:32 signal ratio of ideal third-order interferometric autocorrelations as well as in absolute units to enable a comparison of efficiencies.
and 6(b), respectively. Both traces exhibit a nearly perfect 32:1 peak to background ratio, with clear indications of somewhat elevated noise levels on the STHG trace. Despite a 20 times lower integration time, the absolute signal levels (shown as lefthand ordinates) are 1.2 times higher for THG in TiO2, yielding a ratio of ~24 between the THG of our TiO2 thin film and STHG at the air-glass interface, which is very close to the value reported in section 3.2.

Extracting the unmodulated dc part from the IFROG traces in Figs. 7(a)
Fig. 7 Interferometric FROG trace of a chirped pulse taken with air-glass STHG (a) and THG of TiO2 thin film (c). Exposure times are 200 and 10 ms, respectively. Retrieved pulses from the unmodulated kernel of the IFROG trace are shown in (b) and (d), respectively. The intensity profiles are indicated by solid lines (left axis); the phases as dashed lines (right axis).
and 7(c), we retrieved the pulse shapes shown in Figs. 7(b) and 7(d), respectively. The FROG errors observed in the retrieval are in the range of 0.01 to 0.02. Regardless of the nonlinear material used, similar slightly asymmetric pulse shapes with 150 fs pulse duration are retrieved [Figs. 7(b) and 7(d)]. In the spectral representation, the phase curvature is indicative of a group delay dispersion of 500-600 fs2, which agrees well with the additional dispersion introduced by the 4 mm thick lens.

4. Conclusions

Acknowledgments

The authors thank Dr. M. Albrecht, A. Kwasniewski and M. Schmidbauer (IKZ Berlin), M. Tischer, and C. Poppe (MBI Berlin) and Prof. Rüssel (OSI, FSU Jena) for stimulating discussions and support. The work was in part financially supported by DFG (projects no. GR 1782/12-1 and GR 1782/13-1).

References and links

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R. Trebino, K. W. DeLong, D. N. Fittinghoff, J. N. Sweetser, M. A. Krumbügel, B. A. Richman, and D. J. Kane, “Measuring ultrashort laser pulses in the time-frequency domain using frequency-resolved optical gating,” Rev. Sci. Instrum. 68(9), 3277–3295 (1997). [CrossRef]

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T. Y. F. Tsang, “Optical third-harmonic generation at interfaces,” Phys. Rev. A 52(5), 4116–4125 (1995). [CrossRef] [PubMed]

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T. Tsang, M. A. Krumbügel, K. W. Delong, D. N. Fittinghoff, and R. Trebino, “Frequency-resolved optical-gating measurements of ultrashort pulses using surface third-harmonic generation,” Opt. Lett. 21(17), 1381–1383 (1996). [CrossRef] [PubMed]

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D. N. Fittinghoff, J. A. der Au, and J. Squier, “Spatial and temporal characterizations of femtosecond pulses at high-numerical aperture using collinear, background-free, third-harmonic autocorrelation,” Opt. Commun. 247(4-6), 405–426 (2005). [CrossRef]

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D. S. Stoker, J. Baek, W. Wang, D. Kovar, M. F. Becker, and J. W. Keto, “Ultrafast third-harmonic generation from textured aluminum nitride-sapphire interfaces,” Phys. Rev. A 73(5), 053812 (2006). [CrossRef]

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R. Barille, L. Canioni, L. Sarger, and G. Rivoire, “Nonlinearity measurements of thin films by third-harmonic-generation microscopy,” Phys. Rev. E Stat. Nonlin. Soft Matter Phys. 66(6), 067602 (2002). [CrossRef] [PubMed]

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J. W. Nicholson, M. Mero, J. Jasapara, and W. Rudolph, “Unbalanced third-order correlations for full characterization of femtosecond pulses,” Opt. Lett. 25(24), 1801–1803 (2000). [CrossRef] [PubMed]

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T. Tölke, A. Kriltz, and A. Rechtenbach, “The influence of pressure on the structure and the self-cleaning properties of sputter deposited TiO2 layers,” Thin Solid Films 518(15), 4242–4246 (2010). [CrossRef]

13.

S. Y. Kim, “Simultaneous determination of refractive index, extinction coefficient, and void distribution of titanium dioxide thin film by optical methods,” Appl. Opt. 35(34), 6703–6707 (1996). [CrossRef] [PubMed]

14.

S. K. Das, A. Rosenfeld, M. Bock, A. Pfuch, W. Seeber, and R. Grunwald, “Scattering-controlled femtosecond-laser induced nanostructuring of TiO2 thin films,” Proc. SPIE 7925, 79251B (2011). [CrossRef]

15.

T. Utikal, T. Zentgraf, J. Kuhl, and H. Giessen, “Dynamics and dephasing of plasmon polaritons in metallic photonic crystal superlattices: time- and frequency-resolved nonlinear autocorrelation measurements and simulations,” Phys. Rev. B 76(24), 245107 (2007). [CrossRef]

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19.

G. Ramos-Ortiz, M. Cha, S. Thayumanavan, J. Mendez, S. R. Marder, and B. Kippelen, “Ultrafast-pulse diagnostic using third-order frequency-resolved optical gating in organic films,” Appl. Phys. Lett. 85(16), 3348–3350 (2004). [CrossRef]

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OCIS Codes
(190.4400) Nonlinear optics : Nonlinear optics, materials
(320.7090) Ultrafast optics : Ultrafast lasers

ToC Category:
Nonlinear Optics

History
Original Manuscript: June 29, 2011
Revised Manuscript: August 4, 2011
Manuscript Accepted: August 4, 2011
Published: August 15, 2011

Citation
Susanta Kumar Das, Christoph Schwanke, Andreas Pfuch, Wolfgang Seeber, Martin Bock, Günter Steinmeyer, Thomas Elsaesser, and Ruediger Grunwald, "Highly efficient THG in TiO2 nanolayers for third-order pulse characterization," Opt. Express 19, 16985-16995 (2011)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-19-18-16985


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References

  1. R. Trebino, K. W. DeLong, D. N. Fittinghoff, J. N. Sweetser, M. A. Krumbügel, B. A. Richman, and D. J. Kane, “Measuring ultrashort laser pulses in the time-frequency domain using frequency-resolved optical gating,” Rev. Sci. Instrum. 68(9), 3277–3295 (1997). [CrossRef]
  2. P. Langlois and E. P. Ippen, “Measurement of pulse asymmetry by three-photon-absorption autocorrelation in a GaAsP photodiode,” Opt. Lett. 24(24), 1868–1870 (1999). [CrossRef] [PubMed]
  3. V. N. Ginzburg, N. V. Didenko, A. V. Konyashchenko, V. V. Lozhkarev, G. A. Luchinin, G. A. Lutsenko, S. Yu. Mironov, E. A. Khazanov, and I. V. Yakovlev, “Third-order correlator for measuring the time profile of petawatt laser pulses,” Quantum Electron. 38(11), 1027–1032 (2008). [CrossRef]
  4. T. Y. F. Tsang, “Optical third-harmonic generation at interfaces,” Phys. Rev. A 52(5), 4116–4125 (1995). [CrossRef] [PubMed]
  5. T. Tsang, “Third- and fifth-harmonic generation at the interfaces of glass and liquids,” Phys. Rev. A 54(6), 5454–5457 (1996). [CrossRef] [PubMed]
  6. D. Meshulach, Y. Barad, and Y. Silberberg, “Measurement of ultrashort optical pulses by third-harmonic generation,” J. Opt. Soc. Am. B 14(8), 2122–2125 (1997). [CrossRef]
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