METHOD FOR GROWING SINGLE CRYSTALS OF TRINARY COMPOUND OF ZINC, GERMANIUM AND PHOSPHORUS Russian patent published in 2024 - IPC C30B29/10 C30B11/02 C30B11/14 

FIELD: semiconductors.

SUBSTANCE: used in the manufacture of semiconductor materials. First, a single-crystalline ZnGeP₂ seed with a user-defined orientation and polycrystalline ZnGeP₂ seed are loaded into a boron nitride crucible. The crucible with the load is placed in a quartz ampoule, a phosphorus additive is also placed there to create excess pressure in the ampoule when heated, preventing the formation of zinc vapours and their diffusion into the cold part of the ampoule. At the quartz blowing station, a lid with a process quartz tube is welded to the ampoule, the ampoule is connected to a vacuum system and pumped out to 10^-7-10^-8 Torr to minimize traces of residual atmospheric oxygen, and to remove water, it is heated to a temperature of 400 K and held for one hour. Then the ampoule is sealed off from the vacuum system and installed in a growing oven, which is a thermal device that provides axial temperature profiles with two independently adjustable temperature “shelves.” In the transition-gradient section of the furnace, a smooth continuous temperature distribution is ensured, and by means of diametrically opposed heaters a radial temperature difference of 20 K is formed, which allows the formation of a radial component of the temperature gradient in the melt zone. The oven is brought to the “standard” temperature distribution: (1260-1280) K in the “cold” zone and (1325-1330) K in the “hot” zone. To melt a polycrystalline ZnGeP₂ seed, the melting-crystallization temperature of which is approximately 1300 K, the temperature of the “cold zone” is chosen 20-30 K lower than the crystallization temperature to ensure a guaranteed transition from the liquid phase to the solid, and the temperature of the “hot zone” is 20-30 K above the melting point to ensure melting of polycrystalline ZnGeP₂ seed. The ampoule with loading is installed in the “hot zone” of the oven and held until the polycrystalline ZnGeP₂ seed is completely melted and fused. At the end of the stage of bringing the oven to the crystallization mode, including homogenization curing of the melt, directed cooling of the ampoule with loading is carried out in order to form a single-crystalline ingot of the ZnGeP₂ compound by mechanical moving it from the “hot zone” to the “cold zone”. At the end of the crystallization process, the ampoule is slowly cooled to room temperature. The crucible is removed from the ampoule, and the ZnGeP₂ single crystal is removed from the crucible after complete cooling.

EFFECT: invention makes it possible to push defects in the crystalline lattice of the ingot from the central part to the periphery and increase the threshold of optical breakdown of the crystal.

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