Single crystals growth and Pechini synthesis of δ-BiB3O6:Pr3+

Maciej J. Chrunik 1Andrzej Majchrowski 1Edward Michalski 2Przemysław Morawiak 1Józef Żmija 2Ivan V. Kityk 3

1. Military University of Technology, Institute of Applied Physics, ul. Kaliskiego 2, Warszawa 00-908, Poland
2. Military University of Technology, Institute of Optoelectronics (IOE), Kaliskiego 2, Warszawa 00-908, Poland
3. Czestochowa University of Technology, Electrical Engineering Department, Armii Krajowej 13/15, Częstochowa 42201, Poland


Monoclinic α-BiB3O6 (α–BIBO) single crystals have excellent nonlinear optical (NLO) properties. They find numerous applications in second harmonic generators (SHG), optical parametric oscillators (OPO) and other NLO devices [1]. In the past there were taken efforts to dope α-BIBO with rare earths (RE) active ions (Nd3+, Yb3+) to create a material joining both NLO and lasing properties. It would lead to self frequency doubling (SFD) applications. Unfortunately it was shown that the level of RE doping of α phase is insufficient [2]. According to Aleksandrovsky et al. [3] another BiB3O6 NLO phase, namely orthorhombic δ-BIBO, can be also crystallized from the stoichiometric melts. Moreover it was shown recently that the δ phase, despite its higher density than in case of α phase, can be efficiently doped with some RE ions such as Nd3+ [4]. It was proved that some RE dopants can stabilize the orthorhombic δ-BIBO phase, probably due to the fact that it is isostructural to REB3O6 [5]. This distinctive feature of δ-BIBO allows to obtain significantly high doping level of some RE3+ cations, reaching up to 15 at.% for La, Pr, Ce and Nd.

Our investigations were devoted to synthesis of δ-BIBO phase doped with Pr3+ ions as a material for photoinduced SHG experiments. To obtain δ-BIBO:Pr3+ samples two approaches were used. Single crystal growth was carried out by Kyropoulos technique from stoichiometric melts under conditions of low temperature gradients, while δ-BIBO powders were synthesized by means of sol-gel Pechini method by citric way [6]. In current work we describe the details of δ-Bi1-xPrxB3O6 samples synthesis (x = 0.025 and 0.075) and their XRD characterization, determining precise lattice parameters of orthorhombic phase using Cohen method [7]. Samples obtained by Pechini method were also characterized by calculating crystallite size and lattice strain using Williamson-Hall method [8] comprised to Scherrer formula. Photoinduced SHG of YAG: Nd3+ 1.064 µm laser radiation in obtained δ-BIBO:Pr3+ samples was investigated similarly to the method described in Ref [9]. Obtained results show that Pr3+ doping increases NLO properties of δ-BIBO.


1. V. Petrov, M. Ghotbi, O. Kokabee, A. Esteban-Martin, F. Noack, A. Gaydardzhiev, I. Nikolov, P. Tzankov, I. Buchvarov, K. Miyata, A. Majchrowski, I.V. Kityk, F. Rotermund, E. Michalski, M. Ebrahim-Zadeh, Laser and Photonic Reviews, 4 (2010) 53.

2. A. Brenier, I.V. Kityk, A. Majchrowski, Opt. Commun., 203 (2002) 125.

3. A.S. Aleksandrovsky, A.D. Vasiliev, A.I. Zaitsev, A.V. Zamkov, J. Cryst. Growth, 310 (2008) 4027.

4. D.A. Ikonnikov, A.V. Malakhovskii, A.L. Sukhachev, A.I. Zaitsev, A.S. Aleksandrovsky, V. Jubera, Opt. Mater., 34 (2012) 1839.

5. R. Cong, T. Yang, Z. Lin, L. Bai, J. Ju, F. Lian, Y. Wang, J. Lin, J. Mater. Chem., 22 (2012) 17934.

6. M.P. Pechini, Method of preparing lead and alkaline earth titanates and niobates and coating method  using the same to form a capacitor, United States Patent Office, USA 1967.

7. M. U. Cohen, Rev. Sci. Instrum. 6 (1935) 68.

8. G.K. Williamson, W.H. Hall, Acta Metallurgica, 1 (1953) 22.

9. A. Majchrowski, J. Ebothe, E. Gondek, K. Ozga, I.V. Kityk, A.H. Reshak, T. Lukasiewicz, J. Alloys Compounds, 485 (2009) 29.

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Presentation: Poster at 17th International Conference on Crystal Growth and Epitaxy - ICCGE-17, Topical Session 7, by Maciej J. Chrunik
See On-line Journal of 17th International Conference on Crystal Growth and Epitaxy - ICCGE-17

Submitted: 2013-04-14 22:32
Revised:   2013-04-17 22:58
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