• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.3 no.1
• /
• pp.1-11
• /
• 1993

A suppression of turbulent fluid motion and a control of oxygen and dopants could be improved by application of magnetic field in Czochralski growth of silicon. The effect of an axial magnetic field on Czochralski system was numerically calculated. The fluid motions induced by temperature gradients and by crystal and crucible rotations were suppressed by magnetic force. The S/L interface was gradually flattened in proportion to the increase of magnetic field due to a reduced ascending velocity in the vicinity of center line. The t.emperature distributions in the melt at 8=0.3 Tesla were similar to those analyzed by the conduction heat transfer only. The dissipated amounts of heat flux from melt and crystal surfaces by Ar gas blowing was Jess than 3 %.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1999.06a
• /
• pp.187-207
• /
• 1999

The thermal distributions near the growth interface of 150mm CZ crystals were measured by three thermocouples installed at the center, middle (half radius) and edge (10m from surface) of the crystals. The results show that larger growth rates produced smaller thermal gradients. This contradicts the widely used heat flux balance equation. Using this fact, it si confirmed in CZ crystals that the type of point defects created is determined by the value of the thermal gradient (G) near the interface during growth, as already reported for FZ crystals. Although depending on the growth systems the effective lengths of the thermal gradient for defect generation are varied, were defined the effective length as 10mm from the interface in this experiment. If the G is roughly smaller than 20C/cm, vacancy rich CZ crystals are produced. If G is larger than 25C/cm, the species of point defects changes dramatically from vacancies to interstitial. The experimental results which FZ and CZ crystals are detached from the melt show that growth interfaces are filled with vacancy. We propose that large G produces shrunk lattice spacing and in order to relax such lattice excess interstitial are necessary. Such interstitial recombine with vacancies which were generated at the growth interface, next occupy interstitial sites and residuals aggregate themselves to make stacking faults and dislocation loops during cooling. The shape of the growth interface is also determined by the distributions of G across the interface. That is, the small G and the large G in the center induce concave and convex interfaces to the melt, respectively.

• Journal of the Korean Ceramic Society
• /
• v.27 no.5
• /
• pp.698-701
• /
• 1990

The necessary conditions for the growth of high quality Bi12SiO20 single crystals by the Czochralski method have been determined. The interface of melt and crystal was transformed convex to concave above 7 rpm. For growth <001> and <111> directions, facet morphology exhibited 4-fold and 6-fold symmetry. When the crystal of <001> growth direction was broadened, minor facet {110} was developed outstandingly.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1996.06a
• /
• pp.179-200
• /
• 1996

The intrinsic instabilities of fluid flow occurred in the melt of the Czochralski crystal growth system Czochralski method, asymmetric flow patterns and temperature profiles in the melt have been studied by many researchers. The idea that the non-symmetric structure of the growing equipment is responsible for the asymmetric profiles is usually accepted at the first time. However further researches revealed that some intrinsic instabilities not related to the non-symmetric equipment structure in the melt could also appear. Ristorcelli had pointed out that there are many possible causes of instabilities in the melt. The instabilities appears because of the coupling effects of fluid flow and temperature profiles in the melt. Among the instabilities, the B nard type instabilities with no or low crucible rotation rates are analyzed by the visualizing experiments using X-ray radiography and the 3-D numerical simulation in this study. The velocity profiles in the Silicon melt at different crucible rotation rates were measured using X-ray radiography method using tungsten tracers in the melt. The results showed that there exits two types of fluid flow mode. One is axisymmetric flow, the other is asymmetric flow. In the axisymmetric flow, the trajectory of the tracers show torus pattern. However, more exact measurement of the axisymmetrc case shows that this flow field has small non-axisymmetric components of the velocity. When fluid flow is asymmetric, the tracers show random motion from the fixed view point. On the other hand, when the observer rotates to the same velocity of the crucible, the trajectory of the tracer show a rotating motion, the center of the motion is not same the center of the melt. The temperature of a point in the melt were measured using thermocouples with different rotating rates. Measured temperatures oscillated. Such kind of oscillations are also measured by the other researchers. The behavior of temperature oscillations were quite different between at low rotations and at high rotations. Above experimental results means that the fluid flow and temperature profiles in the melt is not symmetric, and then the mode of the asymmetric is changed when rotation rates are changed. To compare with these experimental results, the fluid flow and temperature profiles at no rotation and 8 rpm of crucible rotation rates on the same size of crucible is calculated using a 3-dimensional numerical simulation. A finite different method is adopted for this simulation. 50×30×30 grids are used. The numerical simulation also showed that the velocity and flow profiles are changed when rotation rates change. Futhermore, the flow patterns and temperature profiles of both cases are not axisymmetric even though axisymmetric boundary conditions are used. Several cells appear at no rotation. The cells are formed by the unstable vertical temperature profiles (upper region is colder than lower part) beneath the free surface of the melt. When the temperature profile is combined with density difference (Rayleigh-B nard instability) or surface tension difference (Marangoni-B nard instability) on temperature, cell structures are naturally formed. Both sources of instabilities are coupled to the cell structures in the melt of the Czochralski process. With high rotation rates, the shape of the fluid field is changed to another type of asymmetric profile. Because of the velocity profile, isothermal lines on the plane vertical to the centerline change to elliptic. When the velocity profiles are plotted at the rotating view point, two vortices appear at the both sides of centerline. These vortices seem to be the main reason of the tracer behavior shown in the asymmetric velocity experiment. This profile is quite similar to the profiles created by the baroclinic instability on the rotating annulus. The temperature profiles obtained from the numerical calculations and Fourier transforms of it are quite similar to the results of the experiment. bove esults intend that at least two types of intrinsic instabilities can occur in the melt of Czochralski growing systems. Because the instabilities cause temperature fluctuations in the melt and near the crystal-melt interface, some defects may be generated by them. When the crucible size becomes large, the intensity of the instabilities should increase. Therefore, to produce large single crystals with good quality, the behavior of the intrinsic instabilities in the melt as well as the effects of the instabilities on the defects in the ingot should be studied. As one of the cause of the defects in the large diameter Silicon single crystal grown by the

• Journal of Mechanical Science and Technology
• /
• v.15 no.8
• /
• pp.1188-1195
• /
• 2001

A numerical analysis has been carried out to investigate the influences of thermosolutal convection on the heat and mass transfer and solute segregation in crystals grown by the vertical Bridgman technique. The governing equations are solved by a finite-volume method using the power law scheme and the SIMPLE algorithm in which body-fitted coordinate system has been used. A primary convective cell driven by thermal gradients forms in the bulk of the domain, while a secondary convective cell driven by solutal gradients forms near interface. As the solutal Rayleigh number increases, secondary cell becomes to be stronger and has a great influence on the radial concentration along the interface.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1996.06a
• /
• pp.522-522
• /
• 1996

An investigation of the effects of transverse magnetic field and Peltier effect on melt convection and macrosegregation in vertical Bridgman crystal grosth of Te doped InSb was been carried out by means of microstructure observation, Hall measurement, electrical resistivity measurement and X-ray analysis. Before the experiments, Interface stability, convective instability and suppression of convection by magnetic field were calculated theoretically. After doping 1018, 1019 cm-3 Te in InSb, the temperature of Bridgman furnace was set up at $650^{\circ}C$. The samples were grown in I.D. 11mm, 100mm high quartz tube. The velocity of growth was about 2${\mu}{\textrm}{m}$/sec. In order to obtain the suppression of convection by magnetic field in the middle of growth, 2-4KG magnetic field was set on the melt. For searching of the shape of solid-liquid interface and the actual velocity of crystal growth, let 2A current flow from solid to liquid for 1second every 50seconds repeatedly (Peltier effect). The grown InSb was polycrystal, and each grain was very sharp. There was no much difference between the sample with and without magnetic field at a point of view of microstructure. For the sample with Peltier effect, the Peltier marks(striation) were observed regularly as expected. Through these marks, it was found that the solid-liquid interface was flat and the actual growth velocity was about 1-2${\mu}{\textrm}{m}$/sec. On the ground of theoretical calculation, there is thermosolutal convection in the Te doped InSb melt without magnetic field in this growth condition. and if there is more than 1KG magnetic field, the convection is suppressed. Through this experiments, the effective distribution coefficients, koff, were 0.35 in the case of no magnetic field, and 0.45 when the magnetic field is 2KG, 0.7 at 4KG. It was found that the more magnetic field was applied, the more convection was suppressed. But there was some difference between the theoretical calculation and the experiment, the cause of the difference was thought due to the use of some approximated values in theoretical calculation. In addition to these results, the sample with Peltier effect showed unexpected result about the Te distribution in InSb. It looked like no convection and no macrosegregation. It was thought that the unexpected behavior was due to Peltier mark. that is, when the strong current flew the growing sample, the mark was formed by catching Te. As a result of the phenomena, the more Te containing thin layer was made. The layer ruled the Hall measurement. The values of resistivity and mobility of these samples were just a little than those of other reference. It was thought that the reason of this result was that these samples were due to polycrystal, that is, grain boundaries had an influence on this result.

• Journal of the Korean Ceramic Society
• /
• v.25 no.1
• /
• pp.78-82
• /
• 1988

Good quality LiNbO3 single crystals which can be applied to SAW devices, were grown by Czochralski method. It was observed that the gas-bubbles were concentrated in ring shape at the outer part of grown crystals, and this anomaly was illustrated by modeling the mechanism of gas-bubble entrapment according to the melt flow pattern in the crucible. And this mechanism was also encertained by observation of solid-liquid interface shape of grown crystals. The optimal condition for good quality crystals was known that the solid-liquid interface shape was slightly concave.

• Journal of the Korean Ceramic Society
• /
• v.31 no.1
• /
• pp.39-46
• /
• 1994

LiTaO3 single crystals were growth without cracking using Pt-Rh crucible and Ir crucible. The starting composition to get the melt of congruent melting composition, which has been dependent upon the experimental procedure, was taken after fixing the total growing process by the result of preliminary experiments. The Rh contamination from the Pt-Rh crucible was to be neglected if the crystal had been grown under inert atmosphere, which resulted in the crystal color being slightly yellow. This color was decolored after 24 hour's annealing at 1200℃ under air atmosphere. The optimum conditions for the crystal growing and the diameter control were so dependent upon the crucible material in spite of using the crucible of the same size. The liquid-solid interface of LiTaO3 crystal of 1" diameter has been flat if the rotation speed was 45rpm.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.7 no.4
• /
• pp.610-618
• /
• 1997

$Al_2O_3$/Al composite was produced by the infiltration of molten Al Into $Al_2$O$_3$ preform at 900-$1200^{\circ}C$, The process was accelerated by spreading borosilicate glass powder onto the interface between Al powder compact and $Al_2O_3$ preform. Melt infiltration initialed after incubation period, and the growth of infiltration was observed to be linearly propotional with time. The major components of the composite are $Al_2O_3$ and Al with a trace of Si which is remained from borosilicate, the reaction accelerator. Relative density of the composite increased with the particle size of $Al_2O_3$ but decreased with infiltration temperature. As infiltration temperature increases from room to $950^{\circ}C$ higher strength and fracture toughness were obtained.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1996.06a
• /
• pp.258-292
• /
• 1996

In the last year great interest appears to YBCO thin films preparation on different substrate materials. Preparation of epitaxial film is a very difficult problem. There are many requirements to substrate materials that must be fullfilled. Main problems are lattice mismatch (misfit) and similarity of structure. From paper [1] or follows that difference in interatomic distances and angles of substrate and film is mire important problem than similarity of structure. In this work we present interatomic distances and angle relations between substrate materials belonging to ABCO4 group (where A-Sr or Ca, B-rare earth element, C-Al or Ga) of different orientations and YBCO thin films. There are many materials used as substrates for HTsC thin films. ABCO4 group of compounds is characterized by small dielectric constants (it is necessary for microwave applications of HTsC films), absence of twins and small misfit [2]. There most interesting compounds CaNdAlO4, SrLaAlO4 and SrLaGaO4 were investigated. All these compounds are of pseudo-perovskite structure with space group 14/mmm. This structure is very similar to structure of YBCO. SLG substrate has the lowest misfit (0.3%) and dielectric constant. For preparation of then films of substrates of this group of compound plane of <100> orientation are mainly used. Good quality films of <001> orientations are obtained [3]. In this case not only a-a misfit play role, but c-3b misfit is very important too. Sometimes, for preparation of thin films substrates of <001> and <110> orientations were manufactured [3]. Different misfits for different YBCO faces have been analyzed. It has been found that the mismatching factor for (100) face is very similar to that for (001) face so there is possibility of preparation of thin films on both orientations. SrLaAlO4(SLA) and SrLaGaO4(SLG) crystals of general formula ABCO4 have been grown by the Czochralski method. The quality of SLA and SLG crystals strongly depends on axial gradient of temperature and growth and rotation rates. High quality crystals were obtained at axial gradient of temperature near crystal-melt interface lower than 50℃/cm, growth rate 1-3 mm/h and the rotation rate changing from 10-20pm[4]. Strong anisotropy in morphology of SLA and SLG single crystals grown by the Czochralski method is clearly visible. On the basics of our considerations for ABCO4 type of the tetragonal crystals there can appear {001}, {101}, and {110} faces for ionic type model [5]. Morphology of these crystals depend on ionic-covalent character of bonding and crystal growth parameters. Point defects are observed in crystals and they are reflected in color changes (colorless, yellow, green). Point defects are detected in directions perpendicular to oxide planes and are connected with instability of oxygen position in lattice. To investigate facets formations crystals were doped with Cr3+, Er3+, Pr3+, Ba2+. Chromium greater size ion which is substituted for Al3+ clearly induces faceting. There appear easy {110} faces and SLA crystals crack even then the amount of Cr is below 0.3at.% SLG single crystals are not so sensitive to the content of chromium ions. It was also found that if {110} face appears at the beginning of growth process the crystal changes its color on the plane {110} but it happens only on the shoulder part. The projection of {110} face has a great amount of oxygen positions which can be easy defected. Pure and doped SLA and SLG crystals measured by EPR in the<110> direction show more intensive lines than in other directions which allows to suggest that the amount of oxygen defects on the {110} plane is higher. In order to find the origin of colors and their relation with the crystal stability, a set of SLA and SLG crystals were investigated using optical spectroscopy. The colored samples exhibit an absorption band stretching from the UV absorption edge of the crystal, from about 240 nm to about 550 m. In the case of colorless sample, the absorption spectrum consists of a relatively weak band in the UV region. The spectral position and intensities of absorption bands of SLA are typical for imperfection similar to color centers which may be created in most of oxide crystals by UV and X-radiation. It is pointed out that crystal growth process of polycomponent oxide crystals by Czochralski method depends on the preparation of melt and its stoichiometry, orientation of seed, gradient of temperature at crystal-melt interface, parameters of growth (rotation and pulling rate) and control of red-ox atmosphere during seeding and growth (rotation and pulling rate) and control of red-ox atmosphere during seeding and growth. Growth parameters have an influence on the morphology of crystal-melt interface, type and concentration of defects.