Hybrid technique for growing homogeneous single crystals of semiconductor solid solutions from melt

A concept and fundamentals of a hybrid technique for growing homogeneous single crystals of semiconductor solid solutions (SSs) from melt are presented. The growth consists of two stages. In the first stage, a single crystal with a specified concentration of the more refractory component is grown by an innovative method of directional constitutional supercooling of a melt in the steady-state mode. In the second stage, the melt is fed with the second component. Using an example of the classical Ge-Si system, the concentration profiles of the components along the crystal axis are calculated and the SS growth dynamics ensuring single crystallinity over the entire ingot length is determined. An analysis of the results yields the optimal technological parameters and conditions for growing homogeneous single crystals of SSs of a specified composition and size.     

Growth of cobalt single crystals by the Electron beam floating-zone method

Co single crystals of striation-free were grown easily by the electron-beam floating-zone melting. For these crystals, observations on dislocations were carried out. Slight preferred direction of grown crystals were discussed on the basis of the local step structure on the crystal surface.     

Growth and study of single crystals of the (Na,Li)Nbo3 solid solutions

Plateletlike transparent (Na,Li)NbO₃ (NLN) single crystals with up to 7 mol % LiNbO₃ possessing a perovskite structure are synthesized by the method of spontaneous crystallization from NaBO₂ flux. Based on the X-ray diffraction data and dielectric measurements of these single crystals, the phase x-T diagram of these solid solutions is constructed in the vicinity of the NaNbO₃ composition. It differs from the x-T diagrams established for the Na_{1 ? x} Li_xNbO₃ ceramic.     

Growth of p-type InP single crystals by the temperature gradient method

P-type InP single crystals doped with zinc or cadmium have been prepared from a solution using indium as a solvent in which a temperature gradient was maintained for the transport of the InP solute. The average growth rate was between 1.1 and 3.0 mm/week. The room temperature hole concentration of the crystals obtained was in a range of 10¹⁷ to 10¹⁸ cm^-3. The distribution coefficients of zinc and cadmium were 0.8 and 0.004, respectively. The temperature gradient method makes it possible to dope the crystals with volatile impurities in a controlled manner.     

Growth of high-purity ZnTe single crystals by the sublimation travelling heater method

A travelling heater method (THM) was developed to grow high-purity ZnTe from the vapor phase. This crystal growth method is called the “sublimation THM”. The temperature of the sublimation interface was set at 815°C and the temperature of the growth interface was varied from 785 to 800°C. The growth rate was 3 mm/day. Under these conditions, it was found that the growth process was mainly due to surface nucleation. Characteristics of the crystals were compared with those of solution-THM and vapor phase epitaxially grown crystals. The free-exciton line at 2.381 eV strongly appears and a doublet structure in neutral- acceptor bound exciton at 2.375 eV is clearly resolved with splitting energy of about 0.7 meV. We thus conclude that the THM from the vapor phase is suitable for preparing ZnTe single crystals which have excellent luminescent properties.     

Growth of semiconductor silicon crystals

This paper focuses on the recent developments in Czochralski (CZ) crystal growth of silicon for large-scale integrated circuits (LSIs) and multi-crystalline silicon growth using a directional solidification method for solar cells. Growth of silicon crystals by the CZ method currently allows the growth of high-quality crystals that satisfy the device requirements of LSIs or power devices for electric cars. This paper covers how to obtain high-quality crystals with low impurity content and few point defects. It also covers the directional solidification method, which yields crystals with medium conversion efficiency for photovoltaic applications. We discuss the defects and impurities that degrade the efficiency and the steps to overcome these problems.     

Growth of CdSiP2 single crystals by self-seeding vertical Bridgman method

Using a high purity CdSiP₂ polycrystalline charge synthesized in a single-temperature zone furnace, a CdSiP₂ single crystal with dimensions of 8 mm in diameter and 40 mm in length was successfully grown by the vertical Bridgman method. The quality of the crystal was characterized by high resolution X-ray diffraction and the full width at half maximum (FWHM) of the rocking curve for the (200) face is 33″. Thermal property measurements show that: the mean specific heat of CdSiP₂ between 300 and 773 K is 0.476 J g^?1 K^?1; the thermal conductivity of the crystal along the a- and c-axes is 13.6 W m^?1 K^?1 and 13.7 W m^?1 K^?1 at 295 K, respectively; and the thermal expansion coefficient measured along the a- and c-axes is 8.4×10^?6 K^?1 and ?2.4×10^?6 K^?1, respectively. The optical transparency range of the crystal is 578–10,000 nm, and there is no absorption loss in the spectrum from 0.7 to 2.5 μm, as often exists with ZnGeP₂ crystals grown from the melt.     

Distribution of aluminum and indium impurities in crystals of Ge-Si solid solutions grown from the melt

The problem regarding the distribution of aluminum and indium impurities in bulk crystals of solid solutions with a variable composition Ge_1−x Si _x (0 ≤ x ≤ 0.3) is solved in order to establish regularities of the changes in the segregation coefficients of impurities with variations in the composition of the host lattice in the germanium-silicon system. Aluminum-and indium-doped crystals of Ge_1−x Si _x (0 ≤ x ≤ 0.3) solid solutions with a silicon content decreasing along the crystallization axis are grown by a modified Bridgman method with the use of a silicon seed. The concentration distribution of impurities over the length of the crystals is determined from Hall measurements. It is demonstrated that the experimental data on the concentration distribution of impurities in the crystals are in good agreement with the results obtained from the theory according to which the equilibrium segregation coefficients of impurities vary linearly with a change in the composition of Ge-Si solid solution crystals.

     

Effect of the growth rate on thermal conditions during the growth of single crystals with melt feeding

An attempt is made to establish a correlation between the radial and axial growth rates and the change in the conditions of heat transfer from a growing crystal to the atmosphere of the water-cooled vacuum furnace for the growth of large alkali halide single crystals. It is found experimentally that an increase in the growth rate leads to an increase in the automatic compensation of the melt temperature by the main heater. In this case, the thickness of the layer of melt condensate on the end face and the lateral surface of the crystal decreases. It is revealed that the possibility of growing infinitely long ingots in the presence of intense melt evaporation is restricted by the possibilities of the heat transport through the boundary between the furnace atmosphere and the cooled furnace walls, onto which melt condensate deposits.     

Pulling CsI(Na) single crystals from melt by continuous method without plastic deformation

It is established that bromine impurity in CsI(Na) crystals not only facilitates the homogeneous incorporation of an activator into the lattice and prevents complex activator clusters from forming, but it also significantly hinders (at certain concentrations) the action of the primary and secondary dislocation slip systems. It is shown that the automatic pulling of large CsI-based crystals can be provided by the introduction of a single Br impurity into the charge; this impurity, to a large extent, strengthens only the top part of the crystal. The absence of plastic deformation in CsI-CsBr(Na) crystals with a diameter Ø300 mm and height h = 600 mm (grown by the continuous method) and Ø500 mm and h = 200 mm (grown by the automatic Kiropulos method) has been experimentally confirmed.     

Automated growing of large single crystals controlled by melt level sensor

The process of single crystal pulling is considered with simultaneous starting material make-up into the melt and heater temperature control in response to a signal generated by the electronic contact melt level sensor, viz.: (i) conditions ensuring the radial broadening steadiness; (ii) effect of melt level displacement, melt temperature changes, changes of solid/liquid interface shape, melt evaporation on the growing crystal diameter; (iii) conditions of crystal purification from impurities and uniform distribution of dopant.     

Growth and characterization of CdSe single crystals by modified vertical vapor phase method

Good quality, large single crystals of CdSe were grown by the modified growth method (i.e., vertical unseeded vapor phase growth with multi-step purification of the starting material in the same quartz ampoule without any manual transfer between the steps). Lower temperature gradients (8–9°C/cm) at the growth interface were used for the crystal growth. As-grown CdSe crystals was characterized by X-ray diffraction, scanning electron microscopy, energy dispersive analyzer of X-rays, high-resistance instrument measurement, and etch-pit observation. It is found that there are two cleavage faces of (1 0 0) and (1 1 0) orientations on the crystal, the resistivity is about 10⁸ Ω cm, and the density of etch pits is about 10^3–4/cm². The crystal was cut into wafers and was fabricated into detectors. The detectors were tested using an ²⁴¹Am radiation source. γ-ray spectra at 59.5 keV were obtained. The results demonstrated that the quality of the as-grown crystals was good. The crystals were useful for fabrication of room-temperature-operating nuclear radiation detectors. Therefore, the modified growth technique is a promising, convenient, new method for the growth of high-quality CdSe single crystals.     

Growth of single crystals and optimization of anionic transport in La1-x NdxF3 solid solutions with tysonite-type structure by isovalent substitutions

The study of the effect of isomorphous isovalent substitution on the fluoride-ion conductivity in La_1-x Nd_xF₃ solid solutions was aimed at optimizing the anionic transport in solid electrolytes with the tysonite-type (LaF₃) structure. A series of La_1-x Nd_xF₃ single crystals with 0.1 ≤ x ≤ 0.9 was grown for the first time by the Bridgman-Stockbarger method in the fluorinating atmosphere. The ionic conductivity was measured at frequencies ranging from 5 to 500 kHz by the method of impedance spectroscopy (with the use of graphite contacts). The conductivity is maximal at the composition La_0.37Nd_0.63F₃.     

Growth of Eu(OH)3 large single crystals by solid KOH assisted hydrothermal method and luminescent and magnetic properties

Large single crystals of lanthanide hydroxides [Ln(OH)₃ (Ln = La, Pr, Nd, Sm, Eu and Tb)] up to several millimeters have been grown by using solid KOH assisted hydrothermal method. Eu(OH)₃ samples, as a representative of the Ln(OH)₃ crystals, were characterized by X‐ray diffraction (XRD), 4‐circle single‐crystal diffraction, Fourier transform infrared (FTIR) spectroscopy and X‐ray photoelectron spectroscopy (XPS). FESEM image shows hexagonal prism morphology for the Eu(OH)₃ large crystals. Research on the photoluminescence and magnetic properties of Eu(OH)₃ species was conducted.     

The melt growth of oxide and related single crystals

This article reviews the principle changes which have occured during the last three years in the techniques used to produce single crystals of oxide and similar single crystals from the melt. The technological demands created by device applications are emphasized and the current state of knowledge upon the major crystalline defects is discussed. The role of accurate phase diagram analysis, the importance now attached to the atmosphere in which a crystal grows and the relevance of looking at crystals with greater resolution are stressed particularly.     

Effect of ultrasound on the growth of semiconductor single crystals

Crystallography Reports - The influence of ultrasound on striations in InSb, GaAs, and Bi-Sb single crystals grown by the modified Czochralski method was studied. Ultrasonic waves with a frequency...     

X-ray crystal orientation determination for semiconductor single crystals

An improved method to measu reorientation angles of flat single crystals was developed taking Buerger precession technique. The method is described and compared with Laue- and goniometer techniques. Advantages are low costs and short measuring time. An easy evaluation of the records allows to take this method as a routine angle determination for semiconductor manufacturing.     

Growth of equiaxed dendritic crystals settling in an undercooled melt,Part 2: Internal solid fraction

Experiments are conducted to measure the internal solid fraction evolution of equiaxed dendritic crystals that are freely growing and settling in an undercooled melt using the transparent model alloy succinonitrile–acetone. The internal solid fraction is determined from the measured settling speed and crystal envelope shape and size. Depending on the melt undercooling and acetone concentration, the internal solid fraction is found to vary between 0.55 and 0.1. In all experiments, the internal solid fraction decreases continually during settling. Based on heat and solute balances, a model is developed for predicting the internal solid fraction evolution under convective conditions. Nusselt and Sherwood number correlations are obtained that allow for the calculation of the thermal and solutal boundary layer thicknesses at the crystal envelope. The measured and predicted internal solid fraction evolutions are found to be in good agreement.