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Growth of Oxide Laser Crystals by Czochralski Method E.V

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Growth of Oxide Laser Crystals by Czochralski Method E.V Vol. 124 (2013) ACTA PHYSICA POLONICA A No. 2 Special Anniversary Issue: Professor Jan Czochralski Year 2013 Invited Paper Growth of Oxide Laser Crystals by Czochralski Method E.V. Zharikov∗, D.A. Lis, K.A. Subbotin, V.B. Dudnikova and O.N. Zaitseva A.M. Prokhorov General Physics Institute of Russian Academy of Sciences Vavilova St. 38, 119991 Moscow, Russia The growth of series of actual laser crystals belonging to dierent structural types by the Czochralski method is presented. The primary attention is given to single crystalline compounds and their solid solutions with garnet structure (scandium-containing rare-earth garnets with general formula fLnScg3[ScMe]2Me3O12, Me = Al, Ga) as well as with olivine (forsterite Mg2SiO4) and scheelite structure (double tungstates and molybdates with formula NaLn(TO4)2, where T = Mo or W). The broad bands of luminescence and absorption produced by activator ions in these laser hosts that appear either as a result of structural disorder (garnets, scheelites) or due to the doping by transition metal ions (chromium in forsterite) join together these representatives of dierent structural classes and determine their application in photonics. The paper considers the problems of growing of large crystals with uniform distribution of components and dopants, determination of congruently melting composition, especially in compounds with complex isomorphism. The mutual inuence of components and dopants, redistribution of ions along crystallographically non-equivalent sites in the structure, alteration of valency of transition metal ions accompanied with the change of their segregation coecients under variation of redox conditions is discussed. DOI: 10.12693/APhysPolA.124.274 PACS: 81.10.Fq, 42.70.Hj 1. Introduction However, one important feature pools them together. Proposed by Jan Czochralski method of crystal pulling There is a broadband absorption and uorescence. Use from melt in 1918 [1], becomes now one of the most of laser materials with broadband uorescence gives the widely used methods for growth of dielectric and semi- possibility to create the tunable solid-state lasers and conductor crystals. Today, after 95 years Czochralski lasers emitting ultra-short pulses in mode-locking regime. technique continues to progress and get replenished; the On the other hand, the broad absorption band results today's status of the method is presented in Ref. [2] and in essential enhancement of overall eciency of diode- last advances and developments are given in Ref. [3]. -pumped solid state lasers, since the power consumption of diode coolers for temperature control of laser diode The rst reported oxide material (CaWO4) was grown using the Czochralski technique in 1960 [4]. Since then wavelength now is not required, because the temperature- the many tens of other oxide laser crystals appeared, and -induced uctuations of the radiation wavelength of the majority of them were growed by Czochralski method. pumping diode become noncritical. Extensive collection of papers devoted to laser crystal The materials under study demonstrate the broad ab- growth was published recently in Ref. [5]. sorption and uorescence due to the dierent reasons. The present paper considers some aspects of the In case of doping by transition metal ions (in particu- Czochralski growth technology of a number of actual lar, chromium-doped forsterite and garnets) the broad laser crystals belonging to dierent structural types. and intensive absorption and uorescence bands arise The primary attention will be given to single crys- from vibronic transitions of particular ion in the laser talline compounds and solid solutions with structures of medium. Another reason is in case of garnets and scheel- garnet (Ln Me O and {LnSc} [ScMe] Me O , Me = ites doped by rare-earth ions. This is the structural 3 5 12 3 2 3 12 disorder originating from the isomorphic substitution. Al, Ga), olivine (forsterite Mg2SiO4) and scheelite (double tungstates and molybdates with general for- The large isomorphic capacity and possibility of incor- poration of high concentrations of neodymium and other mula NaLn(TO4)2, where Ln = Y, Bi, La, Gd, Lu; T = Mo or W). rare-earth ions without substantial quenching are the at- Crystals belonging to all above mentioned structural tractive features of both of these structures. Statistical types are essentially dierent in physico-chemical prop- (or quasi-statistical) distribution of ions of dierent type erties that is necessary to take into account at develop- among identical crystallographic sites produces a partial ment of technology of their growing [6, 7]. They are also structural disorder in such materials that leads to in- dierent in the structure, cations arrangement as well as homogeneous broadening of spectral lines of rare-earth in symmetry and coordination of crystallographic sites activators. Wide ranges of homogeneity in garnets and which oers the possibility to incorporate quite various scheelites easily allow to vary the structural disorder and dopants [8]. create the desirable disordered crystalline media. Growth of crystals of solid solutions give the additional possibil- ities in this respect. Growth of crystals by the Czochralski method oered ∗corresponding author; e-mail: [email protected] the possibility to vary in wide range the conditions of growth (oxidizing-reducing character of ambient atmo- (274) Growth of Oxide Laser Crystals by Czochralski Method 275 sphere, temperature gradients, stirring in melt, etc.). sites, the brackets octahedral sites and the parentheses The paper considers the problems of growing of large tetrahedral sites. crystals, with uniform distribution of components and Redistribution of Sc3+ on sublattices of garnet struc- dopants along and across the crystal. There are discussed ture depends on initial garnet composition, in particular such aspects of problem of composition constancy as de- on Sc3+ concentration, as well as on temperature. The al- termination of congruently melting composition, mutual teration of initial content of scandium essentially changes inuence of components and dopants, redistribution of its distribution on crystallographic nonequivalent sites of ions along crystallographically non-equivalent positions the lattice. At small concentrations scandium ions oc- in the structure etc. Inuence of above-mentioned factors cupy only octahedral sites in RESG. The increase of ini- on spectral-luminescent characteristics and defect forma- tial Sc3+ content leads to the entry of scandium also into tion in crystals are discussed. dodecahedral sites that results in the break of straight- Further improvement of crystal quality and intensi- forward dependence of lattice parameter on crystal com- cation of growth kinetics brings the use in growth tech- position [24]. The replacement by scandium a part of the nology the phenomenon of vibrational convection [9, 10] rare-earth ions in the dodecahedral sites leads to main- arising in the liquid under applied to the growth sys- taining in this way a necessary average size proportion of tem the axial low-frequency vibrations of small ampli- coordination polyhedra in the structure. tude. The controlled axial vibrations in the growth sys- The increase of temperature leading to general exten- tem eciently aect distribution of the temperature and sion of the lattice and increase of eective sizes of coor- composition in liquid near front of crystallization, as well dination polyhedra causes the partial transition of Sc3+ as on the shape of the interface. They can also drasti- ions from dodecahedral sites to octahedral ones, the so- cally aect surface tension driven ows (the Marangoni -called C ! A transition [22]. Such cation redistribution convection) and smooth or completely eliminate temper- is thermally reversible and this process becomes easier in ature uctuations at the interface resulting in essential the presence of oxygen and cation vacancies. reduction of intensity of growth striation leading to ob- The dependence of positional redistribution of scan- taining the crystals of high perfection. dium on the composition is demonstrated by congruently 2. Rare-earth scandium garnets melting compositions of RESG, which are presented in The rst publications devoted to rare-earth scandium Table I. It is seen that the congruently melting compo- garnets (RESG) appeared rather long ago, however, these sitions of RESG, indicating the structural disorder, are laser crystals remain actual matter today due to their re- quite dierent from stoichiometric ones that is unlike to markable spectral-luminescent and laser properties. Rep- YAG as well as to GGG. The data demonstrate that with resentatives of RESG are included in a short list of laser the change of initial composition of garnet both the to- crystals used in practice nowadays. Commercial produc- tal content of Sc3+ in RESG, and the grade of lling of tion of RESG single crystals continues today (see, for octahedral sites by scandium as well as quantity of its instance, [11]), novel ecient diode-pumped lasers emit- entry in dodecahedral sites of garnet structure change. ting on practically important wavelengths [12, 13], as The type of cations occupying the tetrahedral and do- well as high-average power femtosecond lasers are de- decahedral sublattices renders the substantial inuence veloping on their base [14, 15]; more and more widely on these processes. RESG solid state lasers are used in medicine [16, 17]. It should be stressed that the congruently melting com- Recently a new
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