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Growing Large Size Complex Oxide Single Crystals by Czochralski Technique for Electronic Devices I.M

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Growing Large Size Complex Oxide Single Crystals by Czochralski Technique for Electronic Devices I.M Vol. 124 (2013) ACTA PHYSICA POLONICA A No. 2 Special Anniversary Issue: Professor Jan Czochralski Year 2013 Invited Paper Growing Large Size Complex Oxide Single Crystals by Czochralski Technique for Electronic Devices I.M. Solskiia;∗, D.Yu. Sugaka;b and M.M. Vakiva;b aScientic Research Company Carat, 202, Stryjska st., Lviv, 79031, Ukraine bLviv Polytechnic National University, 12, Bandera st., Lviv, 79013, Ukraine This paper is devoted to the use and further development of the single crystal growing technique invented by Professor Jan Czochralski (18851953). The possibilities of the Czochralski technique are demonstrated. Further improvements were introduced at the Scientic Research Company Carat (Lviv, Ukraine) to grow large size complex oxide single crystals. The paper presents an overview of some single crystals grown with the use of a modied technology. Growth parameters and properties of resulting crystals are summarized to show a high potential of the Czochralski technique as an industrial technology to grow large-size, high quality, and structurally perfect single crystals of complex oxides. DOI: 10.12693/APhysPolA.124.314 PACS: 81.10.−h 1. Introduction in [10]. For example, the paper not only describes routine technologies to grow traditional activated garnet and Since the 1970s the electronic industry has been fac- vanadate crystals, but also considers how the Czochral- ing a strong demand for novel devices based on new ski method can be used to grow complex borate crystals physical principles. Examples are electro- and acousto- doped with rare-earth elements which have both laser -optic modulators and Q-switches, acoustoelectric delay and nonlinear optical properties. lines, surface-acoustic-wave lters (SAW lters); devices In 2003, in Ref. [11] it was reported that the method of nonlinear, integral and polarization optics, new laser was used to grow new laser crystals with the structure of active media, as well as scintillation detectors for environ- olivine and phenacite doped with d-elements. mental monitoring, tomography, and high-energy physics The review [12] is of special interest since it considers [18]. Such devices are mainly based on the use of com- the history of the Czochralski method development and plex oxide single crystals with unique physical properties. its status as of 2004, compares its benets and disadvan- Thus, the development of a reliable technology to grow tages, and indicates the directions of further improve- large size single crystals of oxide compounds has become ment. Thus, a special focus is placed on increasing the a vital task. size of resulting crystals, extending a variety of crystal During the last few decades, new microelectronic com- types, implementing high frequency heating of a crucible, ponents and new-generation processing facilities are able, improving the diameter control of growing crystal. The precisely to operate at melting temperatures up to 2800 K weighing method was considered the most promising one have become available. This makes the stability of among other diameter control methods. growth thermal environment and other processing pa- rameters a true challenge which can be answered through 2. Specics of using the Czochralski technique further improving the Czochralski technique. The Czochralski method has been widely used to grow The principle of this technique implies melting a start- complex oxide single crystals since the 1960s. Over this ing raw material in a platinum or iridium crucible (this period, the technique keeps being improved, and a variety condition is mandatory because the oxide compound of crystals grown by the Czochralski method is extending. melts are aggressive to any substance except refractory The method history is described in a number of review noble metals) and dipping a seed, previously oriented articles. with X-ray method, into the melt followed by pulling out The review [9] was one of the rst publications to dis- a single crystal at a given rate, with the crystal being cuss the general issues and a scope of application of the rotated. method and to consider which types of crystals can be Since the melting temperatures of most oxide com- grown. The Czochralski technique is most used to fabri- pounds exceed 1800 K, the Czochralski process to grow cate laser crystals and laser beam control crystals. The single crystals is performed with the use of high frequency experience of Polish scientists in this eld is summarized heating equipment of GALAXIE type which was specially designed for the SRC Carat by PHYSITERM (France) and then modied by Carat specialists. The single crystal is grown in a sealed chamber with a ∗corresponding author; e-mail: [email protected] water-cooled case. Thermal environment around the cru- cible creates the thermal gradients necessary for growing (314) Growing Large Size Complex Oxide Single Crystals . 315 and annealing the single crystal after the growth is com- A special feature of the Czochralski growth facilities pleted. at SRC Carat is that they were originally designed to The crucible is heated up by 24 kHz high frequency produce large size single crystals up to 40 kg and up to generator radiation. The computer-assisted weighing 110 mm in diameter. This imposes special requirements method is used to control the crystal diameter during to the thermal environment since large size crystals re- the growth. A tensoresistive bridge placed on a rod with quire large size crucibles, with the ratio of a resulting a seed is a measuring element. The software ensures the crystal diameter to a crucible diameter (and the diame- process of PC visualization at all stages to begin from ter of melt surface) being about 1:2. We should also note the time of nucleation and up to separation of the crys- that the diameter of an inductive coil in growth units at tal. Figure 1 shows a control PC screenshot presenting the SRC Carat allows installing a crucible of 250 mm the real process parameters and the growth stages of a external diameter inside the coil. This makes it possible lithium niobate crystal. to grow complex oxide crystals up to 125 mm in diameter. Fig. 1. Process parameters and the growth stages of a lithium niobate crystal on a control PC screenshot. The pulling rate, depending on the crystal type and the growing stage, can vary within 0100 mm/h, and the rotation rate within 0100 rpm. The equipment is shown in Fig. 2. Fig. 3. A typical thermal unit: 13 parts made of special corundum and yttrium-zirconium ceramics, 4 iridium or platinum screen, 5 quartz tube, 6 ori- ented seed, 7 iridium or platinum crucible, 8 in- ductor coil. Thus, for each type of single crystals, in order to ensure their optical quality and structural perfection, the growth interface should be made as at as possible through con- trolling radial thermal gradients as well as crystal pulling and rotational rates. In addition, in each specic case a small overcooling is necessary for maintaining the speci- ed vertical thermal gradients to ensure the reliable crys- tal growth and gradual cooling of a crystal part above a melt. For the large size crystals, designing a thermal unit of a growth chamber becomes a special problem. Fig- ure 3 presents a typical thermal unit, with elements 13 being made of special corundum and yttrium-zirconium ceramics to ensure refractory and thermal insulation and maintain the thermal radial gradient, 4 an iridium or platinum screen, its dimension and position relative to the crucible edge allow inuencing the thermal environ- ment above the melt, 5 a quartz tube which is both Fig. 2. Crystal growth equipment. 316 I.M. Solskii, D.Yu. Sugak, M.M. Vakiv an additional thermal insulator and an electric one, 6 and tableted. a properly oriented seed, 7 an iridium or platinum Then the tablets are placed into the crucible where crucible, 8 an inductor coil to induce whirling cur- the raw material is deposited, and the melt is further rents which heat the crucible up to a required temper- homogenized at the temperature that exceeds the raw ature. This typical design is customized to each single material melting temperature. In fact, the growth starts crystal. at this moment. Another important factor inuencing the quality of sin- 3. Application and properties of resulting gle crystals is the purity of starting raw materials. There- single crystals fore they are prepared in the form of ne powders with Several manufacturing processes were developed to a controlled amount of impurities and 99.9999.999% of grow a large range of complex oxide single crystals us- the main phase. At the rst stage (charge preparation) ing the technology described above. these powders are mixed in stoichiometric proportions, Growth parameters are summarized in the following subjected to high temperature synthesis in a solid phase Table. TABLE Growth parameters. Melting Crystallographic Content Crystal growth Crystal of activator Crystal temperature growth direction in a crystal and rotational rates dimensions −1 −1 [K] [hkl] [at.%] [mm h /rev min ] [mm] Gd3Ga5O12 2013 [111] 7/1522 Ø = 82−85, L ≤ 350 Gd3Ga5O12:Nd 2013 [111] 1.7 7/1522 Ø = 60, L ≤ 100 LiNbO3 1523 [0001] 5/68 Ø = 96, L = 110 YAlO3:Nd 2140 [010], Pbnm set 1.4 3/1518 Ø = 65, L ≤ 140 YAlO3:Tm 2140 [010], Pbnm set 4.2 3/1518 Ø = 60, L ≤ 110 CaWO4 1849 [110] 3/1518 Ø = 60−65, L = 140 CdWO4 1643 [100] or [010] 3/1518 Ø = 60−65, L ≤ 170 CaMoO4 1703 [100] or [010] 3/1822 Ø = 55−60, L = 140 The values of growth and rotational rates presented in should be very good because substrate structural defects Table were determined in the course of numerous tech- are reproduced in monocrystalline thin lms during the nological experiments followed by testing the optical and epitaxial growth.
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