Cerussite, PbCO 3 - a new Stimulated Raman Scattering (SRS)-active...

Laser Photonics Rev. 7, No. 3, 425–431 (2013) / DOI 10.1002/lpor.201200123

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Abstract Orthorhombic PbCO3, known as natural crystalcerussite, is presented as a new Stimulated Raman Scatter-ing (SRS)-active crystal. With picosecond laser pumping high-order Raman-induced χ (3) generation is observed. All regis-tered Stokes and anti-Stokes sidebands in the visible and near-IR are identified and attributed to the SRS-promoting phononmode A1g of the carbonate group, with ωSRS ≈ 1054 cm−1. Thefirst Stokes steady-state Raman gain coefficient in the visiblespectral range is estimated as well to a value not less than 4.6cm·GW−1.

Cerussite, PbCO3 – a new Stimulated Raman Scattering(SRS)-active crystal with high-order Stokes and anti-StokeslasingOn the 50th anniversary of the discovery of stimulated Raman scattering

Alexander A. Kaminskii1,∗, Ladislav Bohaty2,∗, Hanjo Rhee3, Andre Kaltenbach3, Oliver Lux3,Hans J. Eichler3, Reinhard Ruckamp4, and Petra Becker2

1. Introduction

In the 50 years of history of physics and spectroscopy ofstimulated Raman scattering (SRS) single crystals of min-erals from nature have played a conductive role. Particu-larly, natural crystals of diamond and calcite were two ofthe first crystals, in which SRS was observed in solid statematter [1]. At present, about 150 SRS-active crystallinematerials are characterised and reported in literature (mostof which are compiled in a recent review [2]), includinginorganic and organic single crystals, ceramics and naturalcrystals. Over many years various SRS-active crystals havebeen used successfully for the realization of self-Ramanlasers (based on crystals doped with mainly trivalent lan-thanide dopants, see, e.g., [3]), or Raman laser wavelengthshifters. They can be applied to solve problems of beamcombining of powerful lasers, and occasionally offer theintriguing possibility to use their octave spanning Stokesand anti-Stokes generation combs for Fourier synthesis ofultra-short lasing waveforms (pulses). Also, the study ofthe manifestations of χ (3)- and χ (2)- nonlinear laser effects

1 Institute of Crystallography, Russian Academy of Sciences, Leninsky prospect 59, 119333 Moscow, Russia2 Institute of Crystallography, University of Cologne, Greinstr. 6, 50939 Cologne, Germany3 Institute of Optics and Atomic Physics, Technical University of Berlin, 10623 Berlin, Germany4 II. Institute of Physics, University of Cologne, 50937 Cologne, Germany∗Corresponding authors: e-mail: [email protected]; [email protected]

in many-phonon crystals, including cross-cascaded photon-phonon χ (3)-interactions, are of particular interest in solidstate physics. This emphasizes the relevance of an ongo-ing broad search for new potential SRS-active crystals, in-cluding both, synthetically and naturally grown specimen.Especially among the latter, in recent years an appreciablenumber of suitable SRS-active crystals were discovered,which are listed in Table 1. The present work is devoted tothe investigation of χ (3)-nonlinear laser SRS properties ofanother natural crystal, cerussite, PbCO3. The close struc-tural similarity of cerussite to aragonite (CaCO3), a crystalwhich offers several attractive manifestations of nonlinearlaser interactions [4], motivated our SRS investigation ofPbCO3.

2. Crystallography

Cerussite, PbCO3, is a member of the isomorphic seriesof carbonate compounds, which crystallize with aragonite-type structure. Main features of this structure type are sheets

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426 A. A. Kaminskii et al.: χ (3) nonlinear-lasing in cerussite (PbCO3)

Table 1 Known SRS-active natural crystals and some of their χ (2)- and χ (3)-nonlinear-laser properties

non- SRS-promoting manifestation of nonlinear-

crystal space group linearities mode, cm−1a) laser interaction

Cb) (diamond) O7h − Fd3m (No. 227) χ (3) 1331.8 [1]b) SRS [1]

SiO2 (α-quartz) D43 − P3121c) (No. 152) χ (2) +χ (3) 465.5 [5] SRS, SHG, THG, self-SFG(SRS),

χ (3)-comb [5, 6]

CaCO3 (calcite) D63d − R3c (No. 167) χ (3) 1086.5 [7] ≈ 282 [8] SRS, SHGd), THGe), FiHGf),

self-SFG(SRS)g), χ (3)-comh),χ (3)-cr-casci) [1, 8–13]

CaCO3 (aragonite) D162h − Pmcnj) (No. 62) χ (3) 1087(≈1096), ≈152 (≈157),

≈205 [4]SRS, THG-SFGk), self-SFG(SRS),

χ (3)-comb, χ (3)-cr-casc [4]

PbCO3 (cerussite)present work

D162h − Pmcn (No. 62) χ (3) ≈1054 SRS, χ (3)-comb

SrSO4 (celestine) D162h − Pnma (No. 62) χ (3) ≈999 [14] SRS, THG-SFG, self-SFG(SRS),

χ (3)-comb [14, 15]

BaSO4 (barite) D162h − Pnma (No. 62) χ (3) ≈985 [15] SRS, THG-SFG, self-SFG(SRS),

χ (3)-comb [15]

PbSO4 (anglesite) D162h − Pnma (No. 62) χ (3) ≈977 [15] SRS, χ (3)-comb [15]

α-KAl(SO4)2·12H2O(potassium alum)

T 6h − Pa3 (No. 205) χ (3) ≈990 [16] SRS, χ (3)-comb [16]

Al2(F1-x(OH)x)2SiO4

(topaz)D16

2h − Pbnm (No. 62) χ (3) ≈265(≈268), ≈238(≈239),≈503(≈507), ≈27(≈29) [17]

SRS, THG-SFG, self-SFG(SRS),χ (3)-comb, χ (3)-cr-casc,com-phonl) [17]

a)In parentheses SRS-promoting vibration modes measured at ≈9 K are given.b)Most probably natural crystals of diamond and calcite were used in this study [1].c)Or D6

3 − P3221(No. 154).d)In [11] bulk electric-field induced second harmonic generation (SHG) was observed.e)THG: Third harmonic generation.f)FiHG: Fifth harmonic generation.g)Self-SFG(SRS): Sum-frequency generation arising from SRS lasing components and pumping radiation.h)χ (3)-comb: Spectrum of Stokes and anti-Stokes laser frequency components that span at least one octave (i.e. the highest frequency(energy) component must be least double the lowest frequency component).i)χ (3)-cr-casc: Cascade of one or many-step χ (3)-lasing with the involvement of the interaction of different SRS-promoting vibrationmodes of the crystal in the photon-phonon generation of high-order Stokes and anti-Stokes components.j)For aragonite a non-standard setting bca, corresponding to the space group symbol Pmcn, is frequently used in literature.k)THG-SFG: Third harmonic generation arising via parametric four-wave mixing (generation) under collinear coherent pumping at twofundamental wavelengths λf1 = 1.06415 μm and λf2 = 0.53207 μm (externally generated SHG of the fundamental wavelength λf1) ofa picosecond Nd3+:Y3Al5O12 laser.l)Com-phon: Combined SRS-active phonon vibration arising as an interaction of two original SRS-promoting modes of crystal.

of isolated coplanar carbonate groups [CO3], that alternatewith sheets of nine-fold coordinated MII cations, where theMII site can be occupied by rather large cations CaII, SrII,BaII, RaII, PbII or EuII, SmII, YbII [18–20]. The orthorhom-bic (space groupPmcn − D16

2h) structure of cerussite wasfirst determined in 1928 by W.H. Zachariasen (as cited in[21]) and re-determined shortly later by [22]. In the follow-ing, several refinements of the cerussite structure, basedon X-ray diffraction measurements [23–25] and on neutrondiffraction [26], were published. In [25] also a pressure-induced structural phase transition of cerussite at approx.8.7 GPa with a symmetry change to monoclinic P21/c isreported. In the present work we use structural data taken

from [26] (a = 5.179(1) A, b = 8.492(3) A, c = 6.141(2)A) with the usual non-standard setting bca, correspondingto the space group Pmcn (see also Table 2) that is gener-ally given for cerussite in literature. In Fig. 1 a view of thecrystal structure of cerussite is presented.

Crystal growth attempts of PbCO3 by hydrothermalsynthesis (e.g. [27, 28]) and gel growth (e.g. [28]) are re-ported in literature. The crystals, which could be obtainedfrom these efforts, do not meet the requirements in dimen-sions and crystal quality of our SRS experiments, though.Fortunately however, large single crystals with parts of op-tical quality of sufficient size have been found occasion-ally in nature, particularly at the famous locality Tsumeb

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Laser Photonics Rev. 7, No. 3 (2013) 427

Table 2 Some known physical properties at room temperature of cerussite, PbCO3, single crystals

characteristic

space group [26]a) Pmcn − D162h (No. 62)

unit cell parameters, A [26]a) a = 5.179(1); b = 8.492(3); c = 6.141(2)

formula units per unit cell Z = 4

fractional coordinates, site symmetry (SS) andcoordination number (CN) of atoms [26]a)

x y z SS CN

Pb 0.25 0.41702(7) 0.24560(12) Cs 9

C 0.25 0.76221(11) 0.08718(15) Cs 3

O1 0.25 0.91299(14) 0.09649(20) Cs

O2 0.46445(14) 0.68597(9) 0.08893(14) C1

density, g·cm−3 6.571b)

hardness (Mohs scale) [29] 3–3.5

cleavage [29] {110} and {021} good

linear optical character biaxial negative

optical transparency range, μmc) ≈0.26 – ≈2.6d) (see Fig. 3)

refractive indices for selected wavelengths λ [30] 0.527 μm 0.589 μm 0.687 μm

nα (‖ c) 1.8164 1.8037 0.7915

nβ (‖ b) 2.0919 2.0763 2.0595

nγ (‖ a) 2.0934 2.0780 2.0613

nonlinearity χ (3)

energy of SRS-promoting vibration mode, cm−1 ωSRS ≈ 1054

FWHM linewidth for the Raman shifted line relatedto SRS-promoting vibration mode, cm−1

�νR ≈ 1.2

steady-state Raman gain coefficient for the firstStokes lasing wavelength, cm·GW−1

gSt1ss R ≥ 4.6e) (for λSt1 = 0.5637 μm, see Fig. 5)

phonon spectra extension, cm−1f) ≈1477

a)The non-standard setting bca given here as well as in [26] is generally used in literature concerning the structure of cerussite. Itcorresponds to the classical morphological setting of cerussite crystals.b)Calculated from X-ray structure data [26].c)For a polished (100) plate of ≈0.99 mm thickness.d)In the estimation the IR border of PbCO3 transmission lies in the region of ≈2.6 μm.e)Measured in consideration of the limited optical quality of the used sample.f)From spontaneous Raman scattering (see Fig. 6).

mine in Namibia. Crystals of cerussite usually are coarselytwinned on {110} and (less common) on {130} [29], butcan show also large un-twinned regions. The contact twinscan easily be distinguished in polarized light and sep-arated mechanically. In the present work we used twocolourless single crystals from the Tsumeb mine with largeun-twinned regions for sample preparation. The crystalswere of plate-shaped morphology with faces {001}, {010},{021}, {110} and {111}. In Fig. 2a, one of the crystalsthat were used for sample preparation is given, togetherwith one of the polished samples for our SRS investiga-tions. The surface of the natural crystals are crusted overby a second growth generation of small cerussite crystals,while the bulk is of sufficient optical quality in large parts.Figure 2b represents the morphology of the used cerussitecrystals with indicated face indices. A sample of cerus-site of parallel-epipedal shape was prepared for the present

SRS study. The face normals of the sample are e1, e2 ande3, with e1 = a

|a| , e2 = b|b| , e3 = c

|c| . The dimensions of

the sample are 15.7 × 9.7 × 6.9 mm3. The sample facesare polished but without anti-reflection coating. Selectedphysical properties of cerussite crystals are summarized inTable 2.

3. Stokes and anti-Stokes lasing

For the excitation of single pass (cavity-free) Raman-induced Stokes and anti-Stokes χ (3)-lasing of cerussite sin-gle crystals in the visible, near- and mid-IR range, weused a SRS-setup based on a home-made Xe-flashlamppumped picosecond Nd3+:Y3Al5O12 laser. Details of thesetup and the methods of measurements are described in

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Figure 1 Structure plot of cerussite, PbCO3, viewed approxi-mately along the c-axis. Pb atoms are marked with large greenspheres, carbon is represented by orange spheres, oxygen atomsby blue spheres. The carbonate groups [CO3] are marked by or-ange triangles. The unit cell is indicated.

several recent publications (see, e.g., [4, 8, 31]). The usedpump laser can emit at two fundamental wavelengths,λf1 = 1.06415 μm with pulse duration τ f1 ≈ 80 ps, orλf2 = 0.53207 μm with τ f2 ≈ 60 ps. Selected χ (3)-lasingspectra of orthorhombic PbCO3, recorded at room temper-ature with excitation geometry e2[(e1 + e3)(e1 + e3)]e2,and the results of their analysis are presented in Fig. 4 andFig. 5 (for the used notation of the excitation geometry seefootnote a) of Table 3). The spectral components and theirprobable attributions are summarized in Table 3. It shouldbe noted that, due to the limited optical quality of the crys-tal samples, only rather low pump power could be applied.So, the comparatively narrowband spectra of the Stokes andanti-Stokes lasing do not reflect the full SRS potential of thetitle crystal, which could be enhanced with the availabilityof more flawless crystal samples.

Due to the applied steady-state (ss) pumping conditionswe could roughly estimate the Raman gain coefficient gSt1

ss Rfor the first Stokes lasing component at the wavelength λSt1= 0.5637 μm (see Fig. 5 and Table 3) for the used cerussitecrystal. For this purpose the sufficiently tested method (see,

Figure 3 Optical transmission spectrum of cerussite (PbCO3),recorded at room temperature using a polished (100) plate of ca.0.99 mm thickness and a spectrophotometer PerkinElmer, modelLambda 19 UV/VIS/NIR. In the inset, the UV part of the spectrumis magnified and the transmission border (in μm) is indicated byan arrow.

e.g., [35,36]), based on the well known relation gSt1ssR I thr

f lSRS

≈ 30 [37] and a comparative measurement under similarpumping conditions of the “threshold” pump intensity (I thr

f )of the confidently detectable first-Stokes lasing signal ofcerussite and GdVO4 (taken as reference crystal), was used.We found that the measured threshold for PbCO3 (in pump-ing geometry e2[(e1 + e3)(e1 + e3)]e2) is approximately 3.5times higher than for the reference crystal GdVO4. Note,that in [38] the equality of the corresponding gain coef-ficients for GdVO4 and YVO4 was found; for YVO4 therather reliable determined value of the steady state Ra-man gain coefficient gSt1

ssR is ≈16 cm·GW−1 at λSt1 = 0.5583 μm [39]. This results in a value of the steady-stateRaman gain coefficientgSt1

ssR for cerussite of not less than4.6 cm·GW−1.

The assignment of the single SRS-promoting vibrationmode in cerussite was evaluated from spontaneous Ramanspectroscopy. Cerussite, as an aragonite-type compound,

Figure 2 (a) Example of one of the usednatural single crystals of cerussite fromthe locality Tsumeb mine, Namibia, to-gether with one of the samples preparedfor our SRS investigations. The lengthof the polished sample is 15.7 mm. (b)Morphology of the used cerussite crys-tals, face indices are indicated. The axesand indices refer to the cell setting givenin Table 2.


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Figure 4 SRS- and RFWM-lasing spectrum of a PbCO3 (cerus-site) single crystal, recorded at room temperature with excitationgeometry e2[(e1 + e3)(e1 + e3)]e2 under picosecond pumping atthe wavelength λf1 = 1.06415 μm (for the used notation of theexcitation geometry see footnote a) of Table 3, RFWM abbrevi-ates Raman induced four wave mixing). The wavelengths of alllines (pump line is asterisked) are given in μm. Their intensitiesare shown without correction for the spectral sensitivity of theused recording spectrometer system, which is equipped with aSi-CCD (see part (a)), and with an InGaAs-CCD sensor (see part(b)). The spectral spacing between Stokes and anti-Stokes linesof the cascaded χ (3)-lasing is related to the single SRS-promotingvibration mode with ωSRS ≈ 1054 cm−1 of the studied crystal.

Figure 5 SRS- and RFWM-lasing spectrum of a PbCO3 (cerus-site) single crystal, recorded at room temperature with excitationgeometry e2[(e1 + e3)(e1 + e3)]e2 under picosecond pumping atthe wavelength λf2 = 0.53207 μm. All used notations are similarto those used in Fig. 4.

Table 3 Spectral composition of the χ (3)-nonlinear lasing in a cerussite (PbCO3) single crystal, related to its single SRS-promotingvibration mode ωSRS ≈ 1054 cm−1. Data were collected at room temperature under pumping at the fundamental wavelengths λf1 =1.06415 μm or λf2 = 0.53207 μm (externally generated SHG of λf1) of a picosecond Nd3+:Y3Al5O12-laser in excitation geometry e2[(e1

+ e3)(e1 + e3)]e2a)

Stokes and anti-Stokes lasing

λf, μm wavelength, μmb) line attributionc)

1.06415 0.7346 ASt4{λf1} *ωf1 + 4ωSRS = [ωf1 + (ωf1 + 3ωSRS) − (ωf1 − ωSRS)] = [ωf1 + ωASt3 − ωSt1] = ωASt4

(Fig. 4) 0.7962 ASt3{λf1} *ωf1 + 3ωSRS = [ωf1 + (ωf1 + 2ωSRS) − (ωf1 − ωSRS)] = [ωf1 + ωASt2 − ωSt1] = ωASt3

0.8692 ASt2{λf1} *ωf1 + 2ωSRS = [ωf1 + (ωf1 + ωSRS) − (ωf1 − ωSRS)] = [ωf1 + ωASt1 − ωSt1] = ωASt2

0.9385 Y3Al5O12:Nd3 + luminescenced)

0.9460

0.9568 ASt1{λf1} *ωf1 + ωSRS = [ωf1 + ωf1 − (ωf1 − ωSRS)] = [ωf1 + ωf1 − ωSt1] = ωASt1

1.06415 λf1 ωf1

1.1986 St1{λf1} ωf1 − ωSRS = ωSt1

1.3719 St2{λf1} *ωf1 − 2ωSRS = (ωf1 − ωSRS) − ωSRS = ωSt1 − ωSRS = ωSt2

0.53207 0.5038 ASt1{λf2} *ωf2 + ωSRS = [ωf2 + ωf2 − (ωf2 − ωSRS)] = [ωf2 + ωf2 − ωSt1] = ωASt1

(Fig. 5) 0.53207 λf2 ωf2

0.5637 St1{λf2} ωf2 − ωSRS = ωSt1

0.5993 St2{λf2} *ωf2 − 2ωSRS = (ωf2 − ωSRS) − ωSRS = ωSt1 − ωSRS = ωSt2

0.6397 St3{λf2} *ωf2 − 3ωSRS = (ωf2 − 2ωSRS) − ωSRS = ωSt2 − ωSRS = ωSt3

a)Notation is used in analogy to that in [32]. The characters to the left and to the right of the square brackets give the direction of thewave normal of the incident and the generated wave, respectively, while the characters between the square brackets indicate (from leftto right) the polarization direction of the incident and of the generated wave, respectively.b)Measurement accuracy ±0.0003 μm.c)Frequencies related to the cascaded χ (3)-lasing acts are asterisked. In square brackets are given three possibilities for nonlinear-lasercomponents of the RFWM process.d)Lines at 0.9385 μm and 0.9460 μm (see Fig. 4a) are scatter emission from the Nd3 + :Y3Al5O12 double-pass amplifier of the usedpicosecond laser pump source [4,8,31], they correspond to the Nd3 + -ion inter-Stark luminescence transitions 11507 cm−1 4F3/2→4I9/2

852 cm−1 and 11423 cm−1 4F3/2→4I9/2 852 cm−1, respectively (see [33, 34]).




Figure 6 Polarized spontaneous Raman scattering spectrumtaken with a crystal sample, which was prepared from the samecrystal of cerussite, PbCO3, as the used SRS sample. The spec-trum was recorded at room temperature with excitation geometryb(cc)b, using a MonoVista 500 spectrometer and an entrance slitwidth of 10 μm. The line width �ν (FWHM) of the SRS-promotingvibration mode at ωSRS ≈ 1054 cm−1 is indicated.

was already investigated in the early days of Raman spec-troscopy [40]. Later, several Raman studies of various min-erals, that include also Raman spectra of cerussite, see, e.g.[41–44], were published. A detailed Raman spectroscopystudy including mode assignment and factor group analy-sis, particularly concerning cerussite, is found in [45]. Usinga single crystal sample which was prepared from the samenatural cerussite crystal, that had been used for SRS-samplepreparation, polarized spontaneous Raman scattering spec-tra were recorded at room temperature in backscatteringgeometry. A spectrometer MonoVista 500 (2400 G·mm−1,incident laser wavelength of 0.532 μm) with a resolution of0.33 cm−1 in the energy region of the dominant Raman line(at ≈1055 cm−1) and an entrance slit width of 10 μm wasused. In Fig. 6 an example of a spectrum taken with exci-tation geometry b(cc)b is presented. The observed Ramanshifted lines agree well with the data given in [45]. Accord-ing to [45] the SRS-promoting vibration mode with ωSRS

≈ 1054 cm−1 corresponds to the fully symmetric A1g (ν1)mode of the carbonate group. The linewidth (FWHM) ofthis line was determined (by Lorentz-type function fitting)to be ≈1.2 cm−1.

4. Conclusion

The results of the present investigation in cerussite, PbCO3,show, that the SRS properties of this crystal in general fol-low those of the isomorphic Ca compound aragonite. In thelatter case, the fully symmetric A1g vibrational mode of thecarbonate groups [CO3] is the dominating mode for SRSgeneration. While in aragonite two further lower energySRS-promoting modes are active, in cerussite, however,using the same excitation geometry as in the correspond-

ing SRS experiments in aragonite [4], the A1g(ν1) vibrationis found to be the singly occurring SRS-promoting mode.Cerussite turned out to be an attractive material for SRSwith a steady state Raman gain (of the first Stokes com-ponent), which amounts about twice the value of that ofaragonite. The promising SRS properties of the carbonatecompounds, that have been studied so far, calcite [1,7–13],aragonite [4] and cerussite, stimulate an extension of SRSinvestigations to further members of the carbonates family.

Acknowledgments. The authors wish to note that this work wasconsiderably enhanced through mutual scientific help within the“Joint Open Laboratory for Laser Crystals and Precise Laser Sys-tems”, and was stimulated by research programs of the Instituteof Crystallography of the Russian Academy of Sciences, by theInstitute of Optics and Atomic Physics of the Technical Universityof Berlin, and by the Institute of Crystallography of the Universityof Cologne. One of us (A.A.K.) is grateful to the Russian Founda-tion for Basic Research and the Program “Extreme light fields andtheir applications” of the Presidium of Russian Academy of Sci-ences, as well as to the Alexander von Humboldt Foundation forencouragement of many years of cooperation with the TechnicalUniversity of Berlin in the field of laser physics, nonlinear opticsand solid state physics. By the present work and our further con-tributions published or submitted in 2012 on SRS-spectroscopyof crystals, which are dedicated to the 50th anniversary of the dis-covery of stimulated Raman scattering, we express our respectto this discovery [46,47].

Received: 26 December 2012, Accepted: 30 January 2013

Published online: 28 February 2013

Key words: Lead carbonate, cerussite (PbCO3), stimulated Ra-man scattering (SRS), Stokes and anti-Stokes lasing comb, cen-trosymmetric crystal.

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