Correlation between the crystal size and crystal growth rate of KDP and Rochelle salt crystals
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A newly developed nonlinear optical crystal, LiRbB 6 O 10 , has been successfully grown by the Czochralski (CZ) method. The major problem in growing this crystal is that it becomes pulverized during cooling after growth. Growth conditions that would allow us to avoid such pulverization have been investigated in association with the hydrous reaction between a grown crystal and the water in it or in the growth atmosphere. The optical properties of a grown crystal are also investigated and compared with those of Li 2 B 4 O 7 .
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Characterization
Czochralski method
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Micro-pulling-down
Interface (matter)
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In the industrial crystallization process, it is known that impurities in the mother liquor inhibit the crystal growth or decrease the crystal purity. It is important to investigate the influence of each impurity on the crystal growth and the crystal purity in the presence of admixture impurities assuming a real process. In this study, the influences of impurities on the crystal growth and the crystal purity have been simultaneously evaluated for the growth of crystalline particles in a real process solution in which admixture impurities are present. An operation method is proposed in order to increase the productivity while maintaining a certain crystal purity. The crystal growth rate is increased by masking Ca2+, an impurity that inhibits the crystal growth, EDTA to the real industrial process solution. This means that the initial supersaturation σi necessary to achieve a certain crystal growth rate can be lowered. Moreover, when the same crystal growth rate is established in two systems, the crystal purity in both systems is found to be very similar. It is found that Ca2+ has no influence on the crystal purity, even though Ca2+ inhibits the crystal growth rate. This study makes it clear that the driving force of the crystal growth, required for maintaining a certain crystal purity, can be lowered by preventing impurities from inhibiting the crystal growth. Therefore, the proposed operation method can be used in order to improve the productivity while maintaining a certain crystal purity when the crystalline particles are produced in the presence of admixture impurities.
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Supersaturation
Seed crystal
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Supercooling
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Free surface
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On the basis of the analysis of dramatical history of development of the concepts of building units in crystal growth we discuss the genesis of non-classical concepts of crystal growth. We show that in the 21st century the competent advantage in the theory of crystal growth transits to notions about building units larger than individual atoms and molecules. New experimental data, testifying to a stable life of prenuclear clusters-quatarons or other organized groups of atoms in crystal-forming environments and their participation in crystal growth and also already formed crystalline particles, allow not only solving the old “Kossel vs. Balarev” problem, but also proving non-classical mechanisms of crystal growth.
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A new growth system, which allows in situ monitoring of the crystal-solution interface, was developed and applied to grow Si x Ge 1- x ( x \fallingdotseq0.15) bulk crystal with uniform composition by the multicomponent zone-melting method. By utilizing the system, the dynamical change of the growth rate was evaluated from the nonlinear upward shift of the interface as a function of the growth time. Based on the monitoring, an attempt was made to balance the pulling rate of the ampoule with the growth rate of the crystal, which led to the suppression of the upward shift of the growth interface. Consequently, the compositional uniformity of the crystal in the growth direction was markedly improved.
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Ampoule
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This paper deals with the mechanism of crystal growth of layered octosilicate, called ilerite, in the hydrothermal synthesis in the presence of seed crystals. The seed crystals grew efficiently at the initial period of the crystallization process; however, the crystal growth rate decreased with an increase in their size. In addition, the seeding promoted the production of crystal nuclei and their growth, resulting in an increase in the formation of finer particles. The pH value of the solution increased as the progress of the synthesis reaction, resulting in inhibition of the crystal growth. In order to enhance the crystal growth, the hydrothermal synthesis with controlling the pH value was carried out. By decreasing the pH value to the initial one, the yield of ilerite reached over 80%, however, the particle size of products increased slightly because of the production of crystal nuclei and their growth.
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Seed crystal
Hydrothermal Synthesis
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The characteristics of crystal's macroscopic and micro morphology are mirrors of the mechanism of crystal growth.The study of macroscopic and micro morphology of the crystal is not only an aid to find the truth of the crystal growth,but also some help to improve the quality of the grown crystals.Some unusual crystal faces with large indices and the spiral growth striations on {100} in hydrothermal grown KTP crystal were reported and the causes were discussed,such as,lower concentration of supersaturated solution and the directions of seed crystal.Some suggestions on improving the technics of the crystal growth of KTP were given.
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Supersaturation
Morphology
Seed crystal
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In the case of evaporation crystallization, the density of ε-hexanitrohexaazaisowurtzitane (ε-HNIW, C6H6N12O12) crystals was controlled using the evaporation rate, initial HNIW concentration, and temperature as the operating parameters. When crystal growth was promoted, the crystal density was found to deviate from the theoretical density, probably due to the inclusion of voids in the crystals that amplified the decrease in the crystal density. Thus, the crystal density was significantly reduced when the evaporation rate and initial HNIW concentration were increased. The influence of the evaporation rate on the crystal density was also found to be much stronger than that of the initial HNIW concentration. However, the crystal density was enhanced when the temperature was increased, due to a retardation of the crystal growth process. It was also interesting to find that the β-form of HNIW crystals was obtained with a high evaporation rate above 0.125 mL/h at 70 °C.
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