Single crystal growth device capable of regulating and controlling crystallization solid-liquid interface in real time and use method

Abstract

The invention relates to a single crystal growth device capable of regulating and controlling a crystallization solid-liquid interface in real time and a use method. The device comprises a crucible, a growth mold and a transmission system. Through the synergistic effect of the transmission system and the growth mold, the function that the height of the growth mold can be adjusted up and down under different growth conditions in the crystal growth process is achieved, the problem that a solid-liquid interface is unstable in beta-Ga2O3 single crystal growth is effectively solved, andby using a traditional crystal growth technique such as edge-defined film-fed crystal growth, the stability of the large-size beta-Ga2O3 single crystal in the growth process and the integrity of the single crystal are greatly improved. The invention overcomes the problems of crystal spiral growth, quality fluctuation, high defect density, crystal cracking and the like caused by solid-liquid interface instability in the crystal growth process, and the single crystal length and the crystal quality are improved.

Description

technical field

[0001] The invention relates to a single crystal growth device capable of real-time regulation and control of the solid-liquid interface of crystallization and its use method, in particular to the process of growing a gallium oxide single crystal by a guided mode method, and belongs to the technical field of crystal growth. Background technique

[0002] β-Ga 2 o 3 It is a transparent semiconductor oxide material with an ultra-wide bandgap (4.9eV). It is a monoclinic crystal system. Its melting point is as high as 1820°C and its breakdown electric field strength is as high as 8MV / cm. It is the second generation of the third-generation semiconductor materials SiC and GaN. To three times, the appropriate bandgap width makes it a natural sun-blind deep ultraviolet detection material (ultraviolet cut-off wavelength 254nm, located in the sun-blind band), the excellent performance of this semiconductor material makes it suitable for power semiconductor devices, opt...

Examples

Embodiment 1

[0035] Such as figure 1 As shown, a single crystal growth device capable of real-time regulation and control of the solid-liquid interface of crystallization includes an iridium crucible 6, an iridium growth mold 7, and a transmission system; the iridium crucible 6 is surrounded by radio frequency coils 8, and the iridium The growth mold 7 is positioned in the iridium gold crucible 6; the center of the iridium gold growth mold 7 is provided with a through hole 9 vertically penetrating, and the through hole 9 top is provided with a seed rod 4; the iridium gold growth mold 7 Both ends are equipped with a transmission system;

[0036]The transmission system includes four iridium clamping plates 5, four iridium gold transmission rods 3, two platinum horizontal linkage rods 2 and a lifting control system 1; the iridium gold clamping plates 5 are symmetrically arranged on the iridium gold growth mold On both sides of 7, the end of the iridium clamping plate 5 away from the iridium ...

Embodiment 2

[0040] The method for growing a single crystal using the single crystal growth device provided in Example 1 capable of real-time regulation and control of the solid-liquid interface of crystallization includes the following steps:

[0041] (1) Selection and processing of raw materials

[0042] Vacuum-dry gallium oxide raw material powder with a purity ≥ 99.99% at 200°C to remove the adsorbed water in the raw material, and press the dried raw material into a cake shape with a hydraulic press to obtain gallium oxide polycrystalline material;

[0043] (2) Selection of seed crystal

[0044] Select β-Ga with [010] orientation 2 o 3 The seed crystal is cut, ultrasonically cleaned and dried for later use;

[0045] (3) Crystal growth

[0046] Put the gallium oxide polycrystalline material in step (1) into the iridium crucible, and then place the iridium growth mold, transmission system, iridium afterheater and insulation material in sequence. The insulation material should be plac...

Embodiment 3

[0049] A method for growing a single crystal using a single crystal growth device provided in Example 1 that can regulate the solid-liquid interface of crystallization in real time, the specific steps are the same as in Example 1, the difference is that step (3) uses the guided mode method to grow the crystal. To: adjust the iridium growth mold and the upper edge of the iridium crucible to be at the same level, lower the gallium oxide seed crystal through the seed rod and gradually approach the melt, lower the gallium oxide seed crystal and close the neck, when the diameter of the gallium oxide seed crystal shrinks Shoulder and equal-diameter growth are carried out when the diameter reaches 2mm. The crystal pulling speed is 15mm / h. When the equal-diameter growth stage is not completed, use a high-resolution CCD observation system with a resolution of 0.01mm to observe the solid-liquid growth during the crystal growth process. The interface area was monitored, and it was observe...

technical field

[0001] The invention relates to a single crystal growth device capable of real-time regulation and control of the solid-liquid interface of crystallization and its use method, in particular to the process of growing a gallium oxide single crystal by a guided mode method, and belongs to the technical field of crystal growth. Background technique

[0002] β-Ga 2 o 3 It is a transparent semiconductor oxide material with an ultra-wide bandgap (4.9eV). It is a monoclinic crystal system. Its melting point is as high as 1820°C and its breakdown electric field strength is as high as 8MV / cm. It is the second generation of the third-generation semiconductor materials SiC and GaN. To three times, the appropriate bandgap width makes it a natural sun-blind deep ultraviolet detection material (ultraviolet cut-off wavelength 254nm, located in the sun-blind band), the excellent performance of this semiconductor material makes it suitable for power semiconductor devices, opt...

Examples

Embodiment 1

[0035] Such as figure 1 As shown, a single crystal growth device capable of real-time regulation and control of the solid-liquid interface of crystallization includes an iridium crucible 6, an iridium growth mold 7, and a transmission system; the iridium crucible 6 is surrounded by radio frequency coils 8, and the iridium The growth mold 7 is positioned in the iridium gold crucible 6; the center of the iridium gold growth mold 7 is provided with a through hole 9 vertically penetrating, and the through hole 9 top is provided with a seed rod 4; the iridium gold growth mold 7 Both ends are equipped with a transmission system;

[0036]The transmission system includes four iridium clamping plates 5, four iridium gold transmission rods 3, two platinum horizontal linkage rods 2 and a lifting control system 1; the iridium gold clamping plates 5 are symmetrically arranged on the iridium gold growth mold On both sides of 7, the end of the iridium clamping plate 5 away from the iridium ...

Embodiment 2

[0040] The method for growing a single crystal using the single crystal growth device provided in Example 1 capable of real-time regulation and control of the solid-liquid interface of crystallization includes the following steps:

[0041] (1) Selection and processing of raw materials

[0042] Vacuum-dry gallium oxide raw material powder with a purity ≥ 99.99% at 200°C to remove the adsorbed water in the raw material, and press the dried raw material into a cake shape with a hydraulic press to obtain gallium oxide polycrystalline material;

[0043] (2) Selection of seed crystal

[0044] Select β-Ga with [010] orientation 2 o 3 The seed crystal is cut, ultrasonically cleaned and dried for later use;

[0045] (3) Crystal growth

[0046] Put the gallium oxide polycrystalline material in step (1) into the iridium crucible, and then place the iridium growth mold, transmission system, iridium afterheater and insulation material in sequence. The insulation material should be plac...

Embodiment 3

[0049] A method for growing a single crystal using a single crystal growth device provided in Example 1 that can regulate the solid-liquid interface of crystallization in real time, the specific steps are the same as in Example 1, the difference is that step (3) uses the guided mode method to grow the crystal. To: adjust the iridium growth mold and the upper edge of the iridium crucible to be at the same level, lower the gallium oxide seed crystal through the seed rod and gradually approach the melt, lower the gallium oxide seed crystal and close the neck, when the diameter of the gallium oxide seed crystal shrinks Shoulder and equal-diameter growth are carried out when the diameter reaches 2mm. The crystal pulling speed is 15mm / h. When the equal-diameter growth stage is not completed, use a high-resolution CCD observation system with a resolution of 0.01mm to observe the solid-liquid growth during the crystal growth process. The interface area was monitored, and it was observe...

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