6.3.1 Experiment
The experimental system is depicted in Fig. 6.5. The pump source is a 1.064 µm Nd:YAG laser and the signal source is a β − BaB2O4(BBO)-based OPO. The Nd:YAG fundamental pulses at 1.064 µm had a pulse duration of 20 ps and a rep-etition rate of 10 Hz. The OPO, which was pumped with the 355 nm line from a Nd:YAG/THG(third harmonic generation) laser, can generate an idler with wave-length tunable in the range of 1.1-1.8 µm with a pulse duration of 5 ps. The pulse energy of the Nd:YAG laser is attenuated to 750 µJ and the idler waves of OPO are varied between 35 and 50 µJ for each pulsebefore incidence. The beam spot size for pump beam was measured about 1.6 mm, which corresponds to a maximum peak intensity of 1.7 GW/cm2. The signal beam from the OPO laser was combined par-allel with the pump beam (collinear configuration) using a polarizing beam splitter.
The polarization directions of pump and signal lights were vertical and horizontal, respectively. The temporal overlap of the two incident beams was adjusted using an optical delay line. The GaSe crystal was mounted on a precise rotation stage.
In this part of experiment, we use pure and erbium doped GaSe crystals having a thicknesses of 6.5 mm, and a cleaved ellipsoidal face with the lengths of the major and minor axes to be 15 and 10 mm, respectively, and with no antireflection coatings on them. Different concentration of erbium doped samples were also employed in this study. The generated mid-IR radiation was detected by a cryogenically cooled MCT detector and a bolometer combined with a digital oscilloscope. A Ge filter
Figure 6.5: Experimental system for generation of tunable infrared picosecond pulses.
was used to block near-infrared pump radiations. This filter completely eliminates all the pumping wavelengths without blocking any IR output wavelength. The pulse energies obtained by us are correcting for the Fresnel reflections and the transmittance of Ge filter. The pulse energy of the generated mid-IR radiation was measured by a pyroelectric detector and calibrated a MCT detector.
6.3.2 Results and Discussion
First we examine the tuning curves of the nonlinear crystals GaSe based on DFG. Fig-ure 6.6 shows the external phase matching angle as a function of the idler wavelength for difference frequency with a pump wavelength of λ=1.064 µm. The circle-points indicate the experimental results, and the solid-line is theoretical calculation from refractive index data in Ref.[56]. Meanwhile, azimuthal angle φ is optimized for type I phase matching, which exhibits smaller phase matching angles, walk-off, and higher efficiency than type-II. Tunable and coherent picosecond pulses in the range of 2.4-30 µm are achieved based on type-I DFG in GaSe. Wavelength tuning does not require readjustment of the time delay between pump and signal pulses. We observe good agreement between the experimental data and the theoretical calculation curve. The external angles are between 340 and 800 in z-cut crystals, corresponding to DFG wavelength from 2.5 to 30 µm. The high nonlinearity of GaSe allows an efficient gen-eration of infrared pulses even though the considerable reflection losses from the large angle occur. Besides, the results of tuning curves in 0.2% and 0.5% doped Er:GaSe crystals are also in agreement with the theoretical calculation curve. It significantly appears that the refractive index dose not change dramatically in the erbium doped crystals. Therefore, the dispersion relations of Ref.[56] are still applicable for erbium doped GaSe crystal.
The measured infrared output pulse energies in undoped, 0.2%, and 0.5% Er:GaSe crystals at different infrared wavelength are shown in Fig. 6.7. These values are obtained after correcting for the transmittance of the Ge filter. The pulse energies range between a maximum of about 5 µJ and 0.1 µJ, corresponding to the wavelength of 3.5 µm and 20 µm, respectively. The three GaSe crystals show the almost similar
µ
Figure 6.6: Type-I DFG output wavelength vs external phase-matching(PM) angle
maximum output, which are about 5 µJ around the wavelength of 3.5 µm. The maximum photon conversion efficiency greater than 8% is achieved at a wavelength of 3.5 µm. Our photon conversion efficiency is higher than the Dahinten’s result of 2% [57], but much lower than the maximum efficiency of 50% that was reported by Finsterbusch et al.[58]. Experimentally, we observed the transmittance of about 59%
while the pump beam with the intensity of 1.5 GW/cm2 at 1.064µm through GaSe crystal. After taking out the reflected losses and linear absorption, there are still much losses in GaSe. The reason could be ascribed that the two-photon absorption (TPA) occurs when the laser photon energy is larger than half the band gap of GaSe crystal, and can set the limit to the performance of photon conversion efficiency.
TAP, which have been reported the value of β=6.3×10−9 cm/W at the wavelength of 1.064µm, would produce the nonlinear absorption losses in GaSe while intensity of incident beam up to the order of GW/cm2.
Keeping on tuning to shorter infrared wavelengths is limited by two possible rea-sons in this experiment. On the one hand the increasing angle of incidence of the GaSe crystals results in a reduced free aperture and a higher reflection loss. On the other hand the pulse energy of signal wave from OPO system is lower as tuning to the longer signal wave. As tuning to the longer infrared wavelength, the results from using the erbium doped GaSe crystals indicated broader tuning range and slightly higher output pulse energy. According to IR transmission from the undoped and 0.5% Er:GaSe crystals, as shown in Fig. 6.8, the transmittance of the erbium doped GaSe crystal was compared highly with the one of undoped crystal while the out-put wavelength was above 15 µm. Although the difference of outout-put pulse energy between two crystals is not too obvious, therefore, the slightly higher output pulse energy in erbium doped crystal could be ascribed to higher transmittance for longer wavelength. From the results of DFG experiment, unfortunately, the doping effect resulting in variation of effective nonlinear coefficient can’t display. The reason could be that the difference-frequency mixing requirs two input laser source. As aligning two laser beams collinearly, the deviation of two beams, such as misalignment and different divergence angle, always arose in the DFG experiment. The most commonly used method to determine the effective nonlinear coefficient is second-harmonic gen-eration(SHG), because SHG benefits from well-established focused beam theories for type-I and type-II interactions. Subsequently, we will use the picosecond infrared light source generated by our DFG system as a pump beam to achieve the frequency
doubling in the erbium doped GaSe crystals.
We measured the SHG efficiency for erbium doped GaSe samples to determine the effects of doping on the nonlinear coefficient. The previous DFG system tuned to the wavelength of 6 µm was used, as shown in Fig. 6.9. The output of the DFG system had a pulsed width of 5 ps, and the pulse energy was available up to∼1µJ. We determined optimum position by varying the orientation and position of the crystal until maximum SHG output was observed. The pulse energy in both the fundamental beam at 6 µm and the doubled frequency was measured with MCT detector. A 1-mm-thick glass plate was used to separate the two wavelengths, and the absorption of the plate was factored into the efficiency measurement.
Type I phase matching was used with an ordinary wave input and obtained an ex-traordinary output wave. The external phase-matching angle of 30.180 was adjusted by means of dispersion relations of GaSe. As a function of the input pulse energy, the measured efficiencies of undoped and erbium doped GaSe crystals are displayed in Fig. 6.10. The slope of the efficiency data was also used to determined the effective nonlinear optical coefficient for both crystals. The extracted effective nonlinear coef-ficient K, using the focused Gaussian beam theory of Boyd and Kleinman, combined with both focusing and double refraction effects can be determined. The theoretical second-harmonic power P2 is related to K the following equation by
P2 = KP12Lk1h(B, ξ) (6.3)
where P1 is the fundamental input power; L is the interaction length; k1 = 2πn/λ0,
µ
µ
Figure 6.7: Type-I DFG pulse energy vs output wavelength
Figure 6.8: Infrared transmission of undoped and 0.5%Er:GaSe crystals
Figure 6.9: Experimental system for SHG.
Kleinman efficiency factor. The double refraction parameter is B = (ρ/2)(k1L)1/2, where ρ is the off angle between the phase and the power-flow directions. A walk-off angle of 3.40 was used, which is the predicted value when the Sellmeier equations are used at the predicted phase-matching angle. The focusing parameters ξ = L/b, where b is the length for confocal configuration over which the beam diameter is less than 21/2ω0. It is given by b = kiω02, and the efficiency scaling constant in mks units is
K = 8πd2/(c0n3λ20) (6.4)
where 0 is the permittivity of free space, c is the vacuum speed of light, and d is the effective nonlinear coefficient in meters per volt.
The measured nonlinear conversion efficiency is the total energy of second-harmonic signal compared with the fundamental pulsed energy and is given by η =
P2dt/ P1dt, where the integrals are over the temporal duration of the pulse. One can relate this efficiency to the time-independent Boyd and Kleinman theory by measuring the fun-damental pulse shape and integrating Eq. 6.3 over time. The result is
η = KLk1h(B, ξ)
Pλ2dt/
Pλdt (6.5)
so that by measuring the temporal pulse shape of the fundamental we can relate the experimental conversion efficiency to the theoretical.
Using Equations. (6.3)-(6.5), along with the measured pulse shape, we calculated the effective deff coefficient by matching the theory to the data. The nonlinear coefficient deff values of 44.5 pm/V and 55.3 pm/V were determined for the undoped and erbium doped crystals, respectively. The variation in deff value could be ascribed to crystal quality[51] and impurity doping effect[50]. According to the structural analysis, both the GaSe crystals that were used in this experiment showed the similar crystal quality. It means that the erbium doped in GaSe did not strikingly improve crystal quality like the case of indium doping. But the effective nonlinear coefficient
Figure 6.10: SHG in GaSe crystals with the measured deff values.
deff is obviously enhanced due to doping erbium elements. The reason has been speculated that the substitution of one Er3+ atom for one pair of Ga2+ atoms or Er3+ ions interstitial at interlayer sites in the unit cell possibly led to the variation in structural symmetry.
6.4 Conclusions
We have reported on the operation of a Nd:YAG-pumped periodically poled LiNbO3 OPO and on difference frequency mixing of the OPO output waves to produce tunable mid-IR from 4.35 to 14.25 mm. The oscillation threshold and slope efficiency of the OPO were 0.65 mJ and 25%, respectively. Because there was no linewidth-narrowing
element in the OPO cavity, the linewidths of the signal and idler wave were large, especially close to the point of degeneracy. The difference-frequency-mixing efficiency was less than the calculated value, mainly due to high reflection loss, poor surface quality, and OPO beam divergence. As the OPO output beam linewidth becomes wider near the degenerate point, the acceptance linewidth will lead to a significant further reduction in the efficiency for longer wavelengths. The effect of OPO output beam divergence plays a less important role regarding the conversion efficiency than do the reflection loss and surface quality, because the GaSe crystal was only 3 mm long.
Besides, we also report an all-solid-state laser system which generate picosecond infrared pulses with duration 5 ps tunable in the range of 2.4-30 µm. Generally, energies of several microjoule are obtained with a maximum of∼5 µJ at wavelength of 3.5 µm, corresponding to photon conversion efficiency of 8%, in undoped and erbium doped GaSe crystals. The conversion efficiency is limited by TPA resulting in mainly internal losses. The infrared picosecond light source were also used to measure the nonlinear coefficient deff values of GaSe crystals based on SHG technique. GaSe doped erbium showed a deff coefficient of 55.3 pm/V, which is larger than the one of undoped crystal. The improvement of deff coefficient could be due to he substitution of one Er3+ atom for one pair of Ga2+ atoms or Er3+ ions interstitial at interlayer sites.
Chapter 7 Conclusions
The central interest of this work was the investigation on the growth of centimeter size GaSe crystals and the characteristics of erbium doped GaSe crystals. The ma-jor studies are taken concern of the optical and electrical properties of the erbium doped GaSe. Additionally, using GaSe crystal to generate mid-infrared coherent source based on parametric interaction process was demonstrated. All the results and discussions are summarized as follows:
The centimeter size GaSe single crystals were grown by means of the non-stoichiometric mixture and quartz tube with a capillary, which were used to overcome the volatiliza-tion of selenium and reduce the number of nucleavolatiliza-tion, respectively. According to structural analysis, the pure and erbium doped GaSe crystals showed good crystal quality. In the analysis of component, the erbium concentration were three order magnitude lower than the initial erbium concentration. The result was not clear that the remaining amounts of erbium were incorporated into the crystal or segregated during crystal growth.
From the analysis of optical properties, the luminescence spectra of Er-doped GaSe appear to be affected by the dopant of erbium. The impurity level at ∼2.064 eV is
observed and located at ∼64 meV above the valence band in both the as-grown and the annealed Er doped GaSe crystal. The emission band at 2.032 eV might be due to the one-LO-phonon replica of the band-impurity recombination at 2.064 eV. The emission bands at 2.103 eV and 2.093 eV are ascribed to structural defects based on the luminescence intensities varying as temperature. Additionally, the infrared lumi-nescence and transmission spectra which have arisen from the intracenter transitions of erbium ions have been observed at ∼0.81, 0.99, and 1.54 µm, respectively. The annealing process under excess Se atmosphere at 600 oC for 72 hours can enhance the crystal to have more active erbium ions. The deep accepter level that located at 162 meV above the valence band was believed to involve the thermal quenching of Er-related luminescence.
In the case of electrical analysis, Hall measurement results show the room tem-perature hole concentration of order of 1017 in Er-doped GaSe samples while their mobility is in the range of 22-34 cm2/V · s. Two acceptors model, in which one acceptor level is found to locate at about 65 meV above the valence band and the other one is at ∼158 meV, was explained. Furthermore, the shallow acceptor level plays the role both in contributing free hole carriers and acting as a radiative cen-ter and the deep one is a nonradiative cencen-ter which is responsible for the quenching behavior of Er related luminescence. The temperature dependence of hole mobility can be interpreted by combining the homopolar optical phonon and ionized impurity scatterings.
An optical parametric oscillator(OPO) based on periodically poled lithium niobate pumped by a Nd:YAG laser was demonstrated. Combined signal and idler pulse output from OPO with a maximum energy of 2.7 mJ, which corresponds to a slope
efficiency of 25% have been achieved. The tuning range is 1.71 to 1.98 µm for the signal wave and 2.81 to 2.30 µm for the idler wave. The signal and the idler waves are tuned and difference-frequency mixed in a GaSe crystal to produce tunable mid-IR from 4.35 to 14.25 µm. The DFG efficiency was less than the calculated value, mainly due to high reflection loss, poor surface quality, and OPO beam divergence.
Finally, we also demonstrated the infrared light source that provides picosecond pulses on microjoule energy level, widely tunable in the 2.4-30 µm wavelength range with pulse durations ∼5 ps. The energies of several microjoule are obtained with a maximum of ∼5 µJ at wavelength of 3.5 µm, corresponding to photon conversion efficiency of 12%. This picosecond light source was applied to evaluate the nonlin-ear coefficient (deff) of crystals GaSe doped with erbium based on second harmonic generation. The variation in the deff values between undoped and erbium doped GaSe could be probably ascribed to the effect of erbium doping, which resulted in substitution or interstitial of Er atom in GaSe unit cell.
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Publications List:
(A) 期刊論文
1. Y.K. Hsu, J.J. Wang, C.S. Chang, and S.C. Wang, 2002, “Synthesis of Bulk Beta-FeSi2 Crystal”, Japanese Journal of Applied Physics, Vol.41 (2002) pp.3854-3859.
2. S. Haidar, Y.K. Hsu, C.S.Chang, S.C. Wang, and H. Ito, “Difference Frequency Mixing of Periodically Poled Lithium Niobate OPO Output Waves in GaSe Crystal”, Optical Engineering, Vol.41 (2002) pp.1932-1935.
3. Y.K. Hsu, C.S. Chang, and W.F. Hsieh,“Photoluminescence study of GaSe doped with Er”, Japanese Journal of Applied Physics Vol.42, (2003) pp4222-4225.
4. S.H. Lee, Y.K. Hsu, H.C. Hsu, C.S. Chang, and W.F. Hsieh, “Fabrication and Optical Property of GaSe Thin Films Growth by Pulsed Laser Deposition”, Japanese Journal of Applied Physics Vol.42 (2003) pp.5217-5221.
5. Y.K. Hsu, W.C. Huang, and C.S. Chang, “Electrical properties of GaSe doped with Er”, Journal of Applied Physics Vol.96, (2004) pp1563-1567.
(B) 研討會論文
1. S. Haidar, T. Usami, Y.K. Hsu, C.S. Chang, S.C.Wang, and H. Ito, “Difference frequency mixing of periodically poled lithium niobate (PPLN) OPO output waves in GaSe crystal”, Technical Digest. Conference on Lasers and Electro-Optics, 2002.
2. C.Y. Lee, C.H. Lin, Y.K. Hsu, C.S. Chang, W.F. Hsieh, “Nonlinear optical characteristics of GaSe crystal by Z-scan measurement” Optics and Photonics Taiwan 02, Taipei, Taiwan, 2002.
3. M.D. Lee, H.C. Hsu, Y.K. Hsu, C.S. Chang, and W.F. Hsieh “Van der Waals epitaxy of GaSe thin film on hydrogen-terminated Si(111) surfaces by pulsed laser deposition”, Annual Meeting of ROC Physics Society, Taiwan, 2002.
4. C.Y. Lu, Y.K. Hsu, and W.F. Hsieh, “Investigation of electro-optical
semiconductor GaSe on different substrates by pulsed laser deposition”, Annual Meeting of ROC Physics Society, Taiwan, 2003.
5. P.J. Jiang, Y.K. Hsu, and C.S. Chang “Mid-infrared generation by difference frequency conversion in the GaSe crystal doped with Er and In” Annual Meeting of ROC Physics Society, Taiwan, 2004.
6. Y.H. Lin, J.H. Lin, Y.K. Hsu, C.S. Chang, W.F. Hsieh “Femtosecond Z-scan measurement of GaSe” Optics and Photonics Taiwan 04, Taiwan, 2004.
候選人簡歷
♦ 姓名：徐裕奎
性別：男
出生年月日：民國 64 年 7 月 12 日
出生年月日：民國 64 年 7 月 12 日