Proceedings of the Korea Association of Crystal Growth Conference (한국결정성장학회:학술대회논문집)
The Korea Association of Crystal Growth
- Semi Annual
Domain
- Earth Science(Earth/Atmosphere/Marine/Astronomy) > Geological Science
1997.06a
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Synthesis of ammonium aluminum hydrogen carbonate(AAHC) via reaction of aluminum bicarbonate and aluminum salt and thermal decomposition is oner of the important processes for preparation of high pure and ultra fine alumina. Kato and coworkers[1] developed this process, at same time Von Erdos and Altorfe[2] found AAHC in the corrosive products of aluminum in the atmosphere of carbon dioxide and ammonia. Murase and Iga[3] synthesized acicular AAHC in a autoclave under 60 to 12
$0^{\circ}C$ Hayashi[4] optimized the conditions for preparation of AAHC and alumina. Attemp has been made in this paper to reveal the conditions affect the morphology of the synthesized AAHC and the consequently produced alumina. -
SiC/C functionally gradient material (FGMs) were formed on graphite substrates by hot-wall chemical vapor deposition (CVD) technique using the SiCl
$_4$ -C$_3$ H8-H$_2$ chemistry. Thermochemical equilibrium calculations were carried out to investigate the deposition process. The effect of process variables on the deposition yield and the SiC/C ratio in deposited layers was studied in detail. Calculated results showed a reasonable agreement with the experiment in a qualitative sense. SiC/C FGMs with excellent mechanical and thermal properties could be successfully formed on graphite substrates by carefully controlling the compositions in the deposited layers. -
The densification of
$Al_2$ O$_3$ /15v/o ZrO$_2$ (Zirconia Toughened Alumina: ZTA) to the 99% of theoretical density was attempted by controlling the processing parameters affecting the each processing step i.e., milling, spray-drying, forming and pressureless sintering. The ZTA processed under the identical conditions showed a large variation in the green and sintered densities, and the mechanical properties. The deviation of 4-point bending strength was more than 100MPa for the ZTA with ~99% of theoretical density. Moreover, the relative green and sintered densities were deviated greatly from the average value. This low reproducibility could be caused by the variation of spray-dried granule properties. Thus, the effect of yield strength and morphology of spray-dried ZTA granule on the green and sintered densities and the mechanical properties needs to be studied in detail. The objective of this work is to fine out the optimum condition of compaction pressure and compaction method depending on the properties of spray-dried granules. -
The surface modificaion of alumina by
$Al_2$ O$_3$ /SiC nanocomposite coating was studied in terms of processing and microstructure. A powder slurry of 5 vol% SiC composition was dipcoated onto presintered alumina bodies and pressurelessly sintered at 1$700^{\circ}C$ for 2 h in$N_2$ . The used of organic binder and plasticizer in the slurry preparation, and the control of the density of presintered alumina body were found to be necessary to avoid cracking and warping during processing. The nanocomposite coating well bonded to the alumina body with thickness about 110${\mu}{\textrm}{m}$ . The average grain size of coating (2${\mu}{\textrm}{m}$ ) was much finer than that of alumina body (13${\mu}{\textrm}{m}$ ). Fracture surface observations revealed mostly transgranular fracture for the coating, whereas intergranular fracture for the alumina body. Some pores (about 6%) were observed in the coating layer, although the alumina body showed fully dense microstructure. -
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Dispersion and flocculation behaviors of clay-ash powders in a slurry state were examined, and we have systematically investigated the effects of colloid/interfaces variables on slip properties and the rheological behavior of ash-clay slurry. Ash-clay slurries have been characterized on the basis of the time dependent rheology which was done out by the gel-curve test. Gel-curve for the coagulated slip shows interesting rheological behavior which was caused by the formation of the new network structure and the readsoption of the polysilicon hydroxo species on the particle surfaces.
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ZrO
$_2$ coated flake graphite powders were prepared by the controlled hydrolysis of zirconium oxichloride. The stirring process plays an important role in the coating process. There are two types of coated ZrO$_2$ particles: (a)primary particles with few nm size were obtained by the direct formation of the shell by precipitation of the surface of the graphite and (b) Secondary particles of ZrO$_2$ with ∼0.1$\mu\textrm{m}$ size were obtained by the independent formation of primary particles ZrO$_2$ and subsequent heterocoagulation at the graphites surface. -
New complex perovskite compounds (Na0.5Sr0.5)(Ti0.5Nb0.5)O3, (Na0.5Sr0.5)(Zr0.5Ti0.5)O3 and (Na0.5Sr0.5)(Ti0.5Ta0.5)O3 have been prepared. The crystal structures of these compounds were determined by powder X-ray Rietveld analysis. The crystal structure of (Na0.5Sr0.5)(Ti0.5Nb0.5)O3 and (Na0.5Sr0.5)(Zr0.5Ta0.5)O3 was Pmmn, and that of (Na0.5Sr0.5)(Ti0.5Nb0.5)O3 was I4/mmm. All these compounds showed the superstructure due to the oxygen octahedron distortion. The selected bond distances and bond angles were calculated by the OFFER. The octahedron distortion for each sample, which was measured from the bond distances and bond angles, showed the following order: (Na0.5Sr0.5)(Z0.5Ta0.5)O3> (Na0.5Sr0.5)(Ti0.5Nb0.5)O3 > (Na0.5Sr0.5)(Ti0.5Ta0.5)O3. Dielectric properties were measured for the samples. In this study, the crystal structure and dielectric properties of the new complex perovskite structures and discussed.
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The roasting of pyrite with a cyclone reactor have been studied in terms of investigating the reaction behavior of pyrite. The development of a fundamental model for pyrite oxidation and lime sulfation in a vertical cyclone reactor. The model assumes a chemical control shrinking core behavior for the pyrite and a fluid film control shrinking core behavior for the lime. The oxygen and sulphur dioxide concentrations and the energy balance for the gas, pyrite and lime particles are solved. The model was solved and characterized numerically. Experiments have been performed to study the influence of reaction parameters such as reactor temperatures, pyrite particle sizes, air flow rates, feeding rates, and mixing ratio of pyrite and lime. The oxidation and sulfation products were characterized chemically and physically.
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Activated carbons are the microporous carbonaceous adsorbents which are prepared from carbon-containing source materials such as wood, coal, lignite, peteroleum and sometimes synthetic high polymers. [1-2] Activated carbons shows an ability to adsorbe hydrocarbons of the gas phase. Activated carbons are used in the purification of many kinds of gas phases like hexane, benzene, toluene, gasoline, phenol etc.[3] In this study, cokes from bitminous coal were activated for the purpose of preparing the activated carbons by steam activation. The effect of the activation temperature, time, steam concentration and flow rate on the n-butane adsorption, burn off, surface area and average pore size of the activated carbons, were investigated. The adsorption characteristics of the activated carbons for gasoline are indirectly estimated by n-butane adsorption.
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Fe
$_2$ O$_3$ thin films were prepared on$Al_2$ O$_3$ substrate by PECVD(Plasma-Enhanced Chemical Vapor Deposition) process. The phase transformation of iron oxide film was determined as the substrate temperature and reduction-oxidation process.$\alpha$ -Fe$_2$ O$_3$ was stable in deposition temperature ranges of 80~15$0^{\circ}C$ . Fe$_3$ O$_4$ phase was obtained by the reduction process of$\alpha$ -Fe$_2$ O$_3$ phase in H$_2$ ambient. Fe$_3$ O$_4$ phase was transformed into a${\gamma}$ -Fe$_2$ O$_3$ thin film under controlled oxidation conditions at 280~30$0^{\circ}C$ . -
One of the general properties of adsorption on multilayer is that the amount of adsorbing particles is not saturated. As another important property, in many cases, the amount of adsorbed particles is linearly proportional to the pressure of gases above the layers, at sufficiently low pressure, which is known to be Henry's experimental law. A purpose of this paper is to show qualitatively, in terms of a theory, that an adsorption on multilayer lbeys Henry's law at the region of low pressure. For this, we introduce a simple multilayer adsorption model and establish an adsorption isotherm for the given model, which is analyzed in the limit of low pressure.
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We have developed new algorithms for solution of the three-dimensional, time-dependent Navier-Stokes equations that utilize massively parallel supercomputing implemented on the Connection Machine 5. Here, we apply these techniques to analyze he fluid flows that occur during the growth of the tow nonlinear optical crystals-potassium dihydrogen phosphate (KDP), which is producted in a novel rapid growth system under development by the Lawrence Livermore National Laboratory Laser Division, and Potassium titanyl phosphate(KTP), which is grown from a high-temperature aqueous solution.
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Emergence of advanced materials has been realized by the great demands for sophisticated state devices in high technology industry. It is the ear of speedy evolution of science and technology, in particular, materials processing technology, which enables us to synthesize any materials with respect to its purity and its perfection of crystal structure and shape (form) that have, heretofore not been available. The availability of ultra pure, fine raw materials, single crystals and thick/thin film materials has been largely responsible for such startling progresses that have been made in the realization of unforeseen, functional devices for high technology industry. Of the functional devices such as passive as active devices, non-silicon devices are mostly passive. Piezoelectric, electro-optic, magneto-optic devices, etc. are some of the examples. In this paper, magneto-optic materials for Faraday device, which is little known, are reviewed including its processing toward practical applications.
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The effects of the moisture and thermal annealing on CLBO crystal have been investigated. CLBO has hydrated at high humidity condition, resulting in 5B
$_2$ O$_3$ $.$ Cs$_2$ O$.$ 8H$_2$ O. The surface hydration seems to induce the cracking and the refractive index change in CLBO. The thermal annealing is effective to restore the changed index. -
Ishii, M.;Kobayashi, M.;Hara, K.;Tanaka, M.;Yamaga, I.;Miwa, K.;Ishibashi, H.;Usuki, Y.;Hirose, Y. 131
Scintillation crystals for industrial field are used in fundamental physics i.e. nuclear and high energy physics experiments besides the medical imaging, process control and gauging, container inspection, mineral process etc. For the reason of limited marketability, there are not so many studies with emphasis paced on the crystal growth. The scintillation crystal is an important theme in the studies in the fundamental physics and researchers for crystal growth are expected participate it. The present work is partly supported by a Grant-in-Aid from the Japanese Ministry of Education, Science and Culture. -
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The doping effects of Mg and/or Fe ions on congruent LiNbO
$_3$ single crystal growth were studied in order to clarify the roles of MgO in Fe doped LiNbO$_3$ single crystals. The effective distribution coefficienct of Fe was found decreased drastically from 0.85 to 0.5 by the addition of MgO into the LiNbO$_3$ melt. M ssbauer spectra revealed that the addition of MgO reduces the occurrence of Fe2+ ions during growth in air. Therefore, it is likely that there would be two important roles of MgO in Fe doped LiNbO$_3$ . One is to suppress the incorporation of all Fe ions, and the other is to reduce the concentration of Fe2+ ions among the total Fe ions. -
Recent progress of electric technology requires new piezoelectric crystals having superior properties such as zero temperature coefficients and large electromechanical coupling factors. We have developed a series of new leading chandidates, La
$_3$ Ga5SiO14(langasite, LGS), La3Nb0.5Ga5.5O14(LNG), La3Ta0.5O14(LTG), to satisfy those requirements. High quality LGS, LNG and LTG single crystals, with dimensions of 2 inches in diameter, were successfully grown by the Czochralski method at a pulling rate of 1mm/h. Since no variation of chemical composition was observed when whole melt in a crucible was crystallized, congruency of these compositions was confirmed. Physical constants such as elastic constants, dielectric constants and piezoelectric constants were measured. Filters and oscillators made of grown LGS, LNG and LTG single crystals showed superior properties such as three times wider passband than that of quartz, low insertion loss and easy processing, Langasite family crystals were shown to be superior materials to other known materials such as quartz, LiTaO$_3$ ,$\alpha$ -AlPO$_4$ and Li$_2$ B$_4$ O7. -
We have successfully grown colorless and transparent Rb-doped potassium niobate (KRN) single crystals using the top seeded solution growth(TSSG) technique. In our crystal growth experiments, the Rb doping concentrations within the melt range from 2-15 mol% relative to that of Nb
$_2$ O5. Atomic absorption measurements indicate that the Rb content in the KRN solid solution is rather low; the Rb segregation coefficient is found to be on the order of 0.05. It is believed that this is due to the relatively much larger Rb+ ionic radius compared to that of K+, rendering it more difficult for Rb to replace K in the KNbO$_3$ (KN) host lattice. Preliminary single-pass second harmonic generation (SHG) experimental results indicate that there exists marginal improvement in the phase-matching temperature tolerance of KRN compared to that of pure Kn single crystals. -
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The MgO-doped LiNbO
$_3$ single crystals were grown along c-axis by the Czochralski method with the pulling rate of 3mm/h and the rotation of 10rpm. The MgO contents were form 1 to 4 mole%. The SHG properties were investigated with the pulsed Nd:YAG laser, and thermo-optic coefficient, electro-optic coefficient of birefringence and curie temperature were measured. Phase matching temperature and Curie temperature increase similarly with MgO content until 4 mole%. -
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When grown the oxide single crystal including Li-ion, optimum oxygen condition is needed. Color and crack are caused in single crystal according too the change in the condition of the oxygen. LiTaO₃ crystals grown from off-composition of congruent melt composition under oxygen deficieny condition didn't generate any crack. LiNbO₃. LiTaO₃ crystals grown from congruent melt composition under optimum oxygen condition caused pale yellow color or colorless with no crack. Color gradually became colorless and generated cracks according to Oxygen excess.
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Oxygen transfer in silicon melts during crystal growth under vertical magnetic fields is investigated numeriaclly and experimentally. A three-dimensional numerical simulation, including melt convection and oxygen transport, is carried out to understand how oxygen transfers in the melt under magnetic fields. Oxygen concentrations in single silicon crystals grown from the melt under these magnetic fields are experimentally measured by using an infrared absoption technique. The rusults obtained are compared to results from a numerical simualtion. An anomalous increase is observed in the oxygen concentration of the grown crystals under a magnetic field of about 0/03 tesla. The cause of this anomaly is identified as Benard instability, since the temperature at the bottom of the crucible is higher than that at interface. When the temperature at the bottom is decreased, the Benard cell can be removed, and a monotonical decrease in the oxygen concentration in the single crystals can be observed.
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The momentum, heat and mass trasfer phenomena in the silicon melt of the Czochralki crystal growth system are calculated using a three dimensional numerical simulation thechnique. Even though axisymmetrical boundary conditions are imposed to all calculations in a 3cm diameter crucible, several types of non-axisymmetric profiles of velocities, temperature and oxygen concentration appeared in the melt. Because of the non-axisymmetric profiles of velocities, temperature and oxygen concentration appeared in the melt. Because of the non-axisymmetric profiles and rotations of fluid induced by the crucible rotation, temperatures and oxygen concentrations in the silicon melt fluctuate. The rotating velocity of the profile is calculated from the phase shift of the data of temperature or oxygen at two different points which have same radius from center but 90 degree angular difference. From this calculation, it is found that the rotating veolocity of the oxygen and temperature is different from the crucible rotation rates. Therefore the frequencies of the oscillating temperature and oxygen concentrations are not same to the frequencies of the crucible rotations. Futhermore, the components of the frequencies of the temperature and oxygen concentration at the same point are not same. The fluctuation behaviors of the temperature or oxygen themselves are also different when the points are different. The calculation show that the temperature and the oxygen concentration near the interface also fluctuate. The results suggest that the striation pattern found in the grown silicon single crystals may ben generated by the oxygen concentration and the temperature oscillations of the melt occurred near the interface.
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Influences of boron addition on the oxygen solubiligy in silicon melt and the amount of evaporation loss from the melt surface were investigated. It has been found the oxygen concentration increases from 2
${\times}$ 1018 to 4${\times}$ 1018 atoms/㎤. The amount of evaporation loss was found to vary widely depending on the melt temperature. The amount of SiO evaporating form boron doped (∼102121 atoms/㎤) silicon melt at 1550$^{\circ}C$ is about twice as much as the value of non-doped melt. -
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The principle of dark field imaging is comprehensively discussed using real images of dislocations, stacking faults and gettering phenomena due to defects obtained by Cz Si wafers and LEC semi-insulating GaAs crystals. Resulution of dark field imaging is improved by Fourier transformation of Fraunhofer diffraction pattern obtained at an out-of focusing position of an objective lens.
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The gas dynamics in a stagnation point upflow OMVPE reactor were studied by Raman spectroscopy. The gas temperature was measured as a function of inlet gas velocity and aspect ratio for both H
$_2$ and N$_2$ carrier gases. The centerline temperature gradient was latger at higher inlet velocities and with the use of N$_2$ , and only weakly dependent on the aspect ratio. a tracer molecule, CH$_4$ , was used to investigate the steady state behavior of reactants in the reactor, and the use of a sweeping flow was found to be a suitable method for preventing wall deposition. The transient switching response of the gas manifold was also investigated. Under certain conditions (low velocities, unmatched flows) recirculation flows were apparent. Numerical calculations of the reactor gas dynamics gave reasonable agreement with experimental results when detailed thermal boundary conditions were included. -
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To improve electrical properties and uniformity of high-low doped n-type GaAs, new ohmic contacts with a low-resistance and the superior uniformity was developed using a concept of hybrid ohmic contact. The hybrid ohmic contact displayed good surface and interface morphology and had minimum contact resistivity of 3
${\times}$ 10-6$\Omega$ $\textrm{cm}^2$ in a wide annealing temperature ranged from 340$^{\circ}C$ to 420$^{\circ}C$ , which was much wider than that of conventional ohmic contacts. The microstructural analysis showed that the Pd/Ge ohmic contact at low annealing temperature (∼300$^{\circ}C$ ) and also annealing temperature (∼400$^{\circ}C$ ), resulting ij hybrid ohmic contacts. -
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A new technique for low temperature crystallization of amorphous silicon, called field aided lateral crystallization(FALC) was attempted. To demonstrate the concept of FALC, thin layer of nickel(30
${\AA}$ ) was deposited on top of amorphous silicon film and the electric field was applied during the crystallization. The effects of electric field on the crystallization behavior of amorphous silicon film were investigated. -
GaN films were grown on three differently oriented sapphire substates; (0001), (11-20), and (1-20). GaN films on the (0001) and (11-20) substates have a haxagonal structure and their growth rate was 0.6
$\mu\textrm{m}$ /hr in both case. The film on the (1-102) substrate was too thin to identify its crystalline state. Growth rate was about the half of the others. Substrate orientation is one of the factor determining growth rate. The adhesion between GaN film and alumina substrate seems to be very good judging from the fractography. -
The iron doped GaAs single crystals were grown by liquid phase epitaxial method and its some physical properties were evaluated with a view to investigate the crystal quality and emission property. The isomer shift of 0.303mm/sec is calculated from low-temperature M ssbauer spectroscopy and we know that charge state of iron ion is 3+ in GaAs crystal. In low temperature photoluminescence, the deep emission bands with wide-line width have been observed at 0.99eV and 1.15eV in addition to sharp excitonic peaks. We attributed that these deep emissions are originated from substitutional Fe-acceptor which has charge state of 3+ and 2+, respectively.
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6H-SiC single crystals were successfully grown by the self-designed sublimation apparatus and the optimum growth condition was established. The grown SiC crystals were about 33mm in diameter and 10mm in length. Carrier concentration and doping type of undopped 6H-SiC wafer grown by sublimation method were 1016∼1017/㎤ and n-type Crystallinity of grown 6H-SiC wafer was better than of Acheson seed by data of Raman spectroscopy and Double Crystal XRD. We continue to characterize the grown 6H-SiC wafer in more detail and so we will grow the high-quality 6H-SiC single crystal wafer.
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Silicon carbide(SiC) epilayers were grown by a thermal CVD(chemical vapor deposition) process, and their crystalline properties were investigated. Especially, the growth conditions of 6H-Sic homoepitaxial layers were obtained using a SiC-uncoated graphite susceptor that utilized Mo-plates. In order to investigate the crystallinity of grown layers, Nomarski photograph, transmittance, XRD, Raman, PL and TEM measurements were used. The best quality of 6H-SiC epilayers was obtained in conditions of growth temperature 1500
$^{\circ}C$ and C/Si ratio 2.0. -
We have investigated the deposition characteristics of (Ni0.8Fe0.2)20Ag80 thin films as a function of chamber pressure and nitrogen flow rate with scanning electron microscopy(SEM), atomic force microscopy(AFM), XRD and
$\alpha$ -step. The deposition rate of these film is decreased with increasing the chamber pressure and the nitrogen flow rate. With raising the chamber pressure, the growth mode of thin film is changed from island growth to columnar one, which is probably due to energy of atom. Contrary, the nitrogen flow rate is raised, growth mode is changed from columnar to island one. According to the XRD patterns, the preferred orientation is inhibited as the nitrogen flow rate is kept above 10 sccm, but that is nearly independent on the chamber pressure. When the chamber pressure decrease or the nitrogen flow rate increase, phase separation into permoally and silver is occured.