CN113930838A - Crystal growth device and method - Google Patents

Crystal growth device and method Download PDF

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Publication number
CN113930838A
CN113930838A CN202111205374.3A CN202111205374A CN113930838A CN 113930838 A CN113930838 A CN 113930838A CN 202111205374 A CN202111205374 A CN 202111205374A CN 113930838 A CN113930838 A CN 113930838A
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China
Prior art keywords
growth
crystal growth
crystal
rate
heating
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CN202111205374.3A
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CN113930838B (en
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王宇
顾鹏
梁振兴
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Meishan Boya New Material Co ltd
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Meishan Boya New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/30Mechanisms for rotating or moving either the melt or the crystal

Abstract

An embodiment of the present disclosure provides a crystal growth apparatus and a method, the apparatus including: the growth cavity is used for placing raw materials for crystal growth; the heating assembly is used for heating the growth cavity to provide heat required by crystal growth; the motion assembly comprises a rotating part, and the rotating part is in transmission connection with the growth cavity to drive the growth cavity to rotate eccentrically.

Description

Crystal growth device and method
Technical Field
The specification relates to the technical field of crystal preparation, in particular to a crystal growth device and a crystal growth method.
Background
The growth of the crystal is usually realized by combining a fluxing agent method with a pulling method for a non-uniform molten crystal, a crystal with volatile components at high temperature or a crystal with phase change at high temperature. The crystallization is carried out by slowly reducing the temperature in the crystal growth process, the melt viscosity is increased by the temperature reduction, the mass and heat transfer of solute in the molten raw material are correspondingly influenced, the crystal growth is slowed, even a fluxing agent wrap appears in the crystal, and the crystal quality is reduced. Therefore, there is a need for a crystal growth apparatus and method that improves the mass and heat transfer behavior of the solute and grows larger sized crystals while maintaining crystal quality.
Disclosure of Invention
One of the embodiments of the present specification provides a crystal growth apparatus, including: the growth cavity is used for placing raw materials for crystal growth; the heating assembly is used for heating the growth cavity to provide heat required by crystal growth; the motion assembly comprises a rotating part, and the rotating part is in transmission connection with the growth cavity to drive the growth cavity to rotate eccentrically.
One of the embodiments of the present specification provides a crystal growth method, including: placing the raw material for crystal growth in a growth cavity; heating the growth chamber to provide heat required for the crystal growth; in the crystal growth process, when the preset conditions are met, the rotating part of the moving assembly drives the growth cavity to eccentrically rotate.
Drawings
The present description will be further explained by way of exemplary embodiments, which will be described in detail by way of the accompanying drawings. These embodiments are not intended to be limiting, and in these embodiments like numerals are used to indicate like structures, wherein:
FIG. 1 is a schematic diagram of an exemplary crystal growth apparatus, shown in accordance with some embodiments herein;
FIG. 2 is a schematic structural diagram of an exemplary rotating component shown in accordance with some embodiments herein;
FIG. 3 is a schematic illustration of an eccentric rotation process according to some embodiments herein;
FIG. 4 is a schematic view of a rotatable shaft and sleeve movably coupled according to some embodiments of the present description;
FIG. 5 is a schematic diagram of an exemplary lift member according to some embodiments herein;
FIG. 6 is an exemplary flow chart of a crystal growth method according to some embodiments described herein.
In the figure, 100 is a crystal growth device, 110 is a growth cavity, 120 is a motion component, 121 is a rotating component, 121-1 is a rotating motor, 121-2 is a first transmission element, 121-3 is a rotating rod, 121-4 is a sleeve, 121-5 is an insulating layer, 121-6 is a sliding chute, 122 is a lifting component, 122-1 is a lifting motor, 122-2 is a second transmission element, 122-3 is a screw rod, 122-4 is an annular groove disc, 122-5 is a lifting platform, 122-6 is a lifting guide rail, 130 is a heating component, 140 is a motion device, 150 is a hearth, and 160 is a temperature field.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present disclosure, the drawings used in the description of the embodiments will be briefly described below. It is obvious that the drawings in the following description are only examples or embodiments of the present description, and that for a person skilled in the art, the present description can also be applied to other similar scenarios on the basis of these drawings without inventive effort. Unless otherwise apparent from the context, or otherwise indicated, like reference numbers in the figures refer to the same structure or operation.
It should be understood that "system", "apparatus", "unit" and/or "module" as used herein is a method for distinguishing different components, elements, parts, portions or assemblies at different levels. However, other words may be substituted by other expressions if they accomplish the same purpose.
As used in this specification and the appended claims, the terms "a," "an," "the," and/or "the" are not intended to be inclusive in the singular, but rather are intended to be inclusive in the plural, unless the context clearly dictates otherwise. In general, the terms "comprises" and "comprising" merely indicate that steps and elements are included which are explicitly identified, that the steps and elements do not form an exclusive list, and that a method or apparatus may include other steps or elements.
Flow charts are used in this description to illustrate operations performed by a system according to embodiments of the present description. It should be understood that the preceding or following operations are not necessarily performed in the exact order in which they are performed. Rather, the various steps may be processed in reverse order or simultaneously. Meanwhile, other operations may be added to the processes, or a certain step or several steps of operations may be removed from the processes. In describing the crystal growth related art in the present specification, "crystal growth apparatus" and "crystal preparation apparatus" are equivalent descriptions.
FIG. 1 is a schematic diagram of an exemplary crystal growth apparatus, shown in some embodiments herein.
In some embodiments, crystal growth apparatus 100 may be used to grow crystals that may have a phase change at high temperatures (e.g., LuAG crystals, YAP crystals, LaBO crystals)3Crystal, BaB2O4Crystals, etc.), crystals whose components are volatile at high temperatures (e.g., LiGaO)2Crystal, Ca5 (PO)4)3F crystals, etc.), inconsistent molten compound crystals (e.g., LBO crystals, BBO crystals, etc.), and the like.
In some embodiments, as shown in FIG. 1, crystal growth apparatus 100 can include a growth chamber 110, a motion assembly 120, a heating assembly 130, a motion assembly 140, a furnace 150, and a thermal field 160.
In some embodiments, the furnace 150 may be the site where the crystal is grown. In some embodiments, a grate may be provided outside of the furnace 150. In some embodiments, the movement device 140 can be located above the hearth 150. In some embodiments, the movement device 140 may be drivingly connected to the pull rod to move the pull rod and the seed crystal up and down and/or rotate. In some embodiments, a temperature field 160 may be located within the furnace 150 for providing a temperature environment for crystal growth. In some embodiments, the crystal growth apparatus 100 may further include a vacuum device (not shown) for providing a vacuum environment or an atmospheric pressure environment below standard atmospheric pressure to the interior of the furnace 150 or the thermal field 160.
Further description of the movement means 140, the furnace 150, the thermal field 160 and the vacuum means can be found in the following applications, the entire contents of which are incorporated herein by reference in their entirety. For example, chinese applications 201980051052.2, 201910772691.X and 202010585048.9 describe a movement apparatus 140, a furnace 150 and a temperature field 160. Also for example, chinese applications 201910772691.X and 202010585048.9 describe vacuum devices. In particular, chinese application 201980051052.2 describes a crystal growth apparatus, which at least comprises a furnace chamber. The furnace chamber comprises a furnace body and a furnace cover, and the furnace cover is arranged at the top of the furnace body. The furnace cover is provided with a first through hole for placing a temperature field. Chinese application 201910772691.X describes a crystal growth apparatus comprising a hearth, a lifting rod, a movement device and a control system. A temperature field and a heat source are arranged in the hearth, at least one part of the lifting rod is positioned in the hearth, and the moving device is in transmission connection with the lifting rod so as to drive the lifting rod to move up and down and/or rotate. The control system is used for controlling the movement direction and/or the movement speed of the movement device. Chinese application 202010585048.9 describes a crystal preparation apparatus comprising: furnace, vacuum apparatus, lifting rod and telecontrol equipment. A temperature field and a heat source are arranged in the hearth, the vacuum device is connected with the temperature field, at least one part of the lifting rod is positioned in the temperature field, and the moving device is in transmission connection with the lifting rod to drive the lifting rod to move up and down and/or rotate.
In some embodiments, growth chamber 110 may be used to place feedstock for growing crystals. In some embodiments, the growth chamber 110 may also be used to place an auxiliary material (e.g., a flux). In some embodiments, the growth chamber 110 may be located inside the thermal field 160, so that crystal growth may be performed under a temperature environment provided by the thermal field 160.
In some embodiments, the growth cavity 110 may be shaped as a cylinder, a cube, a cuboid, a polygonal prism, or the like. In some embodiments, the growth chamber 110 may be a chamber comprised of a bottom and a sidewall. In some embodiments, the growth chamber 110 may be an open chamber. In some embodiments, the growth chamber 110 may be a closed chamber. In some embodiments, the growth chamber 110 may be made of a high temperature resistant material such as graphite, platinum, ceramic, iridium, etc. In some embodiments, for growth chambers 110 that are made of materials that are susceptible to oxidation (e.g., graphite, iridium), an inert gas is introduced into the furnace 150 and the thermal field 160 during the crystal growth process.
In some embodiments, the motion assembly 120 may impart motion to the growth chamber 110.
In some embodiments, motion assembly 120 may include a rotational component 121. In some embodiments, the rotating component 121 may be in driving connection with the growth chamber 110 to rotate the growth chamber 110. In some embodiments, the rotating component 121 may be in driving connection with the growth chamber 110 to rotate the growth chamber 110 eccentrically. For more on the rotating part 121, reference may be made to the description of fig. 2-4, which is not repeated here.
In some embodiments, the motion assembly 120 may also include a lifting member 122. In some embodiments, the lifting member 122 may be in driving connection with the growth chamber 110 to lift or lower the growth chamber 110. For more details of the lifting member 122, reference may be made to the related description of fig. 5, which is not repeated herein.
In some embodiments, heating assembly 130 is used to provide the heat required for crystal growth. For example, heating assembly 130 may be used to heat growth chamber 110 to melt the materials (e.g., raw materials for growing crystals) within growth chamber 110 to form a melt. As another example, heating element 130 may provide a temperature profile required for crystal growth. In the embodiments of the present specification, the temperature field, the temperature distribution, the temperature gradient field, and the temperature information may be used alternatively.
In some embodiments, the heating assembly 130 can be located outside the thermal field 160 and inside the furnace 150. In some embodiments, heating assembly 130 may be located at the periphery of thermal field 160, concentrically disposed with thermal field 160. In some embodiments, heating assembly 130 may be located above and/or below thermal field 160. In some embodiments, the heating assembly 130 may be located outside the furnace 150.
In some embodiments, the heating assembly 130 may include an induction heating component. In some embodiments, the inductive heating component may include an electromagnetic induction coil, a magnetically permeable object, or the like.
In some embodiments, the heating assembly 130 may include a resistive heating element. In some embodiments, the resistive heating elements may include high resistance graphite, silicon molybdenum rods (MoSi)2) Nickel-chromium wires (Ni-Cr), iron-chromium-aluminum wires (Fe-Cr-Al), nickel-iron wires (Ni-Fe), nickel-copper wires (Ni-Cu), silicon carbide rods (SiC) and the like.
In some embodiments, the heating assembly 130 may be segmented, and multiple heating segments may be independently controlled. For example, the heating assembly 130 may include a plurality of heating segments axially spaced along the thermal field 160, such that heating control may be individually performed at different heights in the axial direction of the thermal field 160. For another example, the heating assembly 130 may include a plurality of heating sections spaced along the circumference of the thermal field 160, so that heating control can be individually performed at different positions along the circumference of the thermal field 160. For another example, the heating assembly 130 may include a plurality of heating sections spaced above the thermal field 160, so that heating control can be separately performed at different positions above the thermal field 160. For another example, the heating assembly 130 may include a plurality of heating sections spaced below the thermal field 160, so that heating control can be separately performed at different positions below the thermal field 160. For another example, when the plurality of heating sections of the heating assembly 130 are independently controlled, at least one of the heating sections may be controlled to increase the heating power, and the other heating sections may be controlled to decrease the heating power; or controlling at least one of the heating sections to reduce the heating power, and increasing the heating power of the rest heating sections.
In some embodiments, crystal growth apparatus 100 may further include a monitoring component (not shown) and a control component (not shown).
In some embodiments, a monitoring component can be used to monitor crystal growth parameters. In some embodiments, the crystal growth parameters may include crystal growth rate, crystal growth weight, crystal growth volume, crystal pull height, crystal growth diameter, and the like.
In some embodiments, the monitoring components may include weight sensing components, image acquisition components (e.g., monocular camera, binocular camera, infrared high definition camera, etc.) components, measurement components (e.g., grating scale components), and the like. The weight sensing assembly may monitor the weight of the growing crystal. Description of the weight sensing assembly can be found in chinese applications 201980051052.2, 201910772691.X and 202010585048.9, the entire contents of which are incorporated herein by reference in their entirety. The image acquisition assembly may acquire images of the growing crystal, which may in turn determine crystal appearance, crystal volume, etc. based on the images. For example, binocular images of the crystal may be acquired by a binocular camera, and the crystal volume may be determined by performing preprocessing, image rectification, three-dimensional reconstruction, and volume matching on the binocular images. The measurement assembly may monitor crystal pull height, crystal growth diameter, crystal growth rate, and the like.
In some embodiments, the control assembly may adjust a heating related parameter of the heating assembly 130 and/or a motion related parameter of the motion assembly 120 based on the crystal growth parameter. In some embodiments, the control component may determine the crystal growth rate based on the crystal growth parameter. In some embodiments, the control assembly may adjust the eccentric rotation parameter of rotating component 121 if the crystal growth rate is below a rate threshold. In some embodiments, the control assembly may adjust the lift parameters of the lift member 122 if the crystal growth rate is below a rate threshold. For more about the control component, reference may be made to the related description of fig. 6, which is not repeated herein.
It should be noted that the above description of crystal growth apparatus 100 is for purposes of example and illustration only and is not intended to limit the scope of applicability of the present description. Various modifications and alterations to crystal growth apparatus 100 will become apparent to those skilled in the art in light of this description. However, such modifications and variations are intended to be within the scope of the present description. For example, crystal growing apparatus 100 may also include a display component for displaying crystal growth related parameters. As another example, during the initial stage of crystal growth, the growth chamber 110, the heating assembly 130, the movement device 140, the furnace 150, and the thermal field 160 are concentrically arranged.
FIG. 2 is a schematic diagram of an exemplary rotating component shown in accordance with some embodiments of the present description.
In some embodiments, as shown in fig. 2, the rotating member 121 may include a rotating motor 121-1, a first transmission element 121-2, a rotating rod 121-3, and a sleeve 121-4.
In some embodiments, the rotating shaft 121-3 may be driven to rotate by the rotating motor 121-1. In some embodiments, the rotating motor 121-1, the first transmission element 121-2 and the rotating rod 121-3 may be in transmission connection, and the rotating motor 121-1 may drive the rotating rod 121-3 to rotate through the first transmission element 121-2. In some embodiments, the first transmission member 121-2 may be a pulley and a belt. In some embodiments, the output shaft of the rotating motor 121-1 may be connected to a shaft of a pulley, and one or more belts may be sleeved on the pulley and the rotating rod 121-3 to realize the driving connection between the rotating motor 121-1 and the rotating rod 121-3.
In some embodiments, the rotating rod 121-3 may be fixedly connected with the sleeve 121-4. In some embodiments, rotating rod 121-3 may rotate sleeve 121-4. In some embodiments, the axis of rotation of rotating rod 121-3 is not coincident with the central axis of sleeve 121-4, thereby allowing sleeve 121-4 (or growth cavity 110 located therein) to be eccentrically rotated. In some embodiments, the top of the rotating rod 121-3 may be provided with a platform for placing the sleeve 121-4 and fixedly connecting with the sleeve 121-4. In some embodiments, the rotating rod 121-3 may be movably connected with the sleeve 121-4 such that an eccentric distance of the eccentric rotation of the sleeve 121-4 is adjustable. Further details regarding the eccentric rotation of the sleeve 121-4 can be found in the description of fig. 3 and 4, and will not be described herein.
In some embodiments, the sleeve 121-4 may be partially sleeved on the outer circumference of the growth chamber 110. For example, the height of the upper edge of the sleeve 121-4 may be lower than the height of the sidewall of the growth chamber 110. In some embodiments, the sleeve 121-4 may be entirely sleeved on the outer circumference of the growth chamber 110. For example, the height of the upper rim of sleeve 121-4 is equal to or higher than the height of the sidewall of growth chamber 110. In some embodiments, the sleeve 121-4 may include two or more curved side barrel pieces that are spliced into a hollow barrel, with the growth chamber 110 placed in the hollow cavity of the hollow barrel. In some embodiments, the rotating rod 121-3 rotates (e.g., eccentrically rotates) the sleeve 121-4, which may rotate (e.g., eccentrically rotate) the growth chamber 110. For more details about the eccentric rotation of the growth chamber 110, reference may be made to the description of fig. 3 and 4, which are not repeated herein.
In some embodiments, the hollow cavity of the sleeve 121-4 may be in the shape of a cylinder, a cube, a cuboid, a polygonal prism, or the like. In some embodiments, to prevent the growth chamber 110 from moving or sliding in the radial direction when rotating eccentrically, the hollow cavity of the sleeve 121-4 may be shaped according to the outer wall shape of the growth chamber 110. In some embodiments, the shape of the hollow cavity of the sleeve 121-4 may match the shape of the outer wall of the growth chamber 110 such that the sleeve 121-4 wraps around the outer wall of the growth chamber 110. In some embodiments, "matching" may mean that the shape of the hollow cavity of the sleeve 121-4 is the same as or similar to the shape of the outer wall of the growth chamber 110 and that the difference in the cross-sectional dimension (e.g., side length or diameter) of the hollow cavity of the sleeve 121-4 and the cross-sectional dimension of the outer wall of the growth chamber 110 is within a preset threshold range (e.g., 1mm-10 mm). For example, the outer wall of the growth chamber 110 is cylindrical in shape, the hollow cavity of the sleeve 121-4 is also cylindrical in shape, and the cross-sectional dimension (e.g., diameter or area) of the hollow cavity of the sleeve 121-4 is slightly larger than the cross-sectional dimension (e.g., diameter or area) of the outer wall of the growth chamber 110 so that the sleeve 121-4 can wrap around the outer wall of the growth chamber 110. In some embodiments, the shape of the hollow cavity of the sleeve 121-4 may also be different from the shape of the outer wall of the growth chamber 110. For example, the outer wall of the growth chamber 110 is cylindrical in shape, and the hollow cavity of the sleeve 121-4 is also polygonal in shape.
In some embodiments, the outer wall of the sleeve 121-4 may be shaped as a cylinder, a cube, a cuboid, a polygonal prism, or the like. In some embodiments, the shape of the outer wall of the sleeve 121-4 may or may not be the same as the shape of the hollow cavity of the sleeve 121-4. For example, the outer wall of the sleeve 121-4 is shaped as a cylinder, and the hollow cavity of the sleeve 121-4 is shaped as a cylinder. For another example, the outer wall of the sleeve 121-4 is rectangular, and the hollow cavity of the sleeve 121-4 is cylindrical.
In some embodiments, the sleeve 121-4 may be made of a high temperature resistant material. In some embodiments, the sleeve 121-4 may be made of refractory graphite, alumina, zirconia, iridium, platinum, tungsten, tantalum, molybdenum, etc. By using the above-mentioned high temperature resistant material to make the sleeve 121-4, the sleeve 121-4 can be applied to a high temperature environment to grow various types of crystals.
By sleeving the sleeve 121-4 on the outer periphery of the growth cavity 110, the growth cavity 110 can rotate when the rotating rod 121-3 drives the sleeve 121-4 to rotate. Meanwhile, the growth chamber 110 can be prevented from moving or sliding in the radial direction due to the centrifugal action during the rotation process, so that the growth chamber 110 falls. In addition, the phenomenon that the liquid level is unstable and the crystal growth condition is influenced due to the fact that the molten raw materials in the growth cavity 110 are splashed out due to moving oscillation can be avoided.
In some embodiments, the sleeve 121-4 and the outer periphery of the growth chamber 110 may be filled with an insulating layer 121-5.
In some embodiments, insulation layer 121-5 may be a thin sheet having a certain thickness. In some embodiments, insulation layer 121-5 may be pressed into a thin sheet having a certain thickness by a compression molding technique. In some embodiments, the outside of the insulation layer 121-5 may match the inside wall of the sleeve 121-4, and the inside of the insulation layer 121-5 may match the outside wall of the growth chamber 110, such that the insulation layer 121-5 may be disposed in the gap between the sleeve 121-4 and the growth chamber 110. In some embodiments, "matching" may mean that the outer side of the insulation layer 121-5 is the same shape and the same or similar size (e.g., no more than 1mm difference) as the inner wall of the sleeve 121-4, and the inner side of the insulation layer 121-5 is the same shape and the same or similar size (e.g., no more than 1mm difference) as the outer wall of the growth chamber 110. By arranging the outer side of the insulating layer 121-5 to be matched with the inner wall of the sleeve 121-4 and the inner side of the insulating layer 121-5 to be matched with the outer wall of the growth cavity 110, the outer side and the inner side of the insulating layer 121-5 can be well attached between the sleeve 121-4 and the growth cavity 110, and the effect of preventing the growth cavity 110 from sliding or moving is achieved.
In some embodiments, insulation 121-5 may also include bulk insulation, granular insulation, batting insulation, laminated insulation, and the like. In some embodiments, an appropriate insulation layer 121-5 may be selected to fill, depending on the size of the gap between sleeve 121-4 and growth chamber 110, so that growth chamber 110 does not move or slide during rotation.
In some embodiments, insulation layer 121-5 may be a high temperature resistant insulation material. In some embodiments, the insulation layer 121-5 may comprise a high temperature resistant material such as metal, alumina, zirconia, silica, tempered aluminum, carbide, nitride, silicide, and the like. By adopting the high-temperature resistant material, the high-temperature resistant material can be made into a slice with a certain thickness by a compression molding technology, and can also be made into a granular or flocculent heat-insulating material by a crushing technology, so that the process is simple and the operation is convenient.
The heat preservation layer 121-5 is arranged in the gap between the sleeve 121-4 and the growth cavity 110, so that the heat preservation effect on the growth cavity 110 can be achieved, the close degree of the fit between the sleeve 121-4 and the growth cavity 110 can be improved, the growth cavity 110 is prevented from sliding or moving in the radial direction in the sleeve 121-4 due to the centrifugal effect in the eccentric rotation process, and the growth cavity 110 is prevented from being collided or even damaged; the phenomenon that the liquid level is unstable and the crystal growth condition is influenced due to oscillation and splashing of the molten raw material in the growth cavity 110 caused by sliding or moving can also be avoided.
In some embodiments, an insulation layer (not shown) may be disposed outside the rotating member 121, on the upper portion of the rotating member 121, and/or at the bottom of the rotating member 121. In some embodiments, the rotary member insulation may comprise bulk insulation, granular insulation, batting insulation, laminated insulation, or the like. In some embodiments, the material of the heat insulating layer of the rotating component may include metals, alumina, zirconia, silica, tempered aluminum, carbides, nitrides, silicides, and other high temperature resistant materials.
Through set up the rotary part heat preservation outside rotary part 121, rotary part 121 upper portion and/or rotary part 121 bottom, can keep apart the raw materials and melt and the heat radiation in the crystal growth process to avoid rotary part 121 to lead to the high temperature and be damaged because of the heat radiation.
FIG. 3 is a schematic illustration of an eccentric rotation process, shown in accordance with some embodiments herein.
In some embodiments, eccentric rotation refers to the central axis of rotation of the eccentric rotating component (e.g., sleeve 121-4, growth chamber body 110) not coinciding with its own actual central axis (or thermal field central axis, or lift pin central axis). The eccentric rotation process is described below in a specific embodiment, as shown in fig. 3, which illustrates the case where the eccentric rotation member (e.g., the sleeve 121-4 or the growth chamber 110) rotates clockwise in one cycle (only 4 positions P1-P4 are shown by way of example), where Z represents the growing crystal (or pulling rod, or seed crystal), a represents the actual central axis of the sleeve 121-4 or the growth chamber 110, and 121-3 is the rotation rod (or the rotation axis thereof). The position of the crystal Z is fixed and the sleeve 121-4 or growth chamber 110 rotates clockwise eccentrically around the rotating rod 121-3.
When the crystal is grown by the Czochralski method, the temperature of the molten raw material near the intersection point of the central axis of the thermal field (or the actual central axis A of the growth chamber 110) and the molten liquid level is the lowest (also called as "cold spot") at the initial stage of crystal growth, and the seed crystal is positioned at the cold spot; the temperature of the molten raw material can be reduced to be within a preset range (for example, 3-8 ℃ higher than the saturation temperature) above the saturation temperature by adjusting the temperature (for example, adjusting the heating power of the heating assembly 130) and keeping the temperature for a period of time; further, the temperature is adjusted again so that the temperature of the molten raw material is slowly lowered to cause the raw material to precipitate from the flux, thereby realizing crystal growth on the surface of the seed crystal. However, when the temperature of the molten raw material is lowered to a certain degree, the viscosity of the molten raw material increases sharply, the mass and heat transfer of the solute in the molten raw material is slowed down, the crystal growth is slowed down, and even flux inclusions appear inside the crystal, reducing the crystal quality. Accordingly, in the embodiment of the specification, the heat and mass transfer behaviors of the solute can be improved through eccentric rotation, and further growth of the crystal is promoted to improve the quality of the crystal.
As shown in fig. 3, at position P1, crystal Z and actual central axis a coincide; at the position P2-P4, the position of the crystal Z is not changed actually, but because the sleeve 121-4 or the growth cavity 110 rotates eccentrically around the rotating rod 121-3, the position of the actual central axis A of the growth cavity 110 is changed continuously, so that the position of the crystal Z relative to the actual central axis A of the growth cavity 110 is changed continuously, the crystal Z can deviate from the cold point of the molten raw material during the eccentric rotation of the sleeve 121-4 or the growth cavity 110, and the flow capacity of the molten raw material around the crystal Z is improved due to the centrifugal effect of the eccentric rotation, namely the heat and mass transfer behaviors of the molten raw material around the crystal Z are improved, the growth of the crystal Z is further promoted, the occurrence of flux inclusions in the crystal can be reduced, and the quality of the crystal is improved.
In some embodiments, the eccentric rotation may also be achieved by tilting the bottom of the sleeve 121-4. For example, the angle formed by the sleeve 121-4 (or the growth chamber 110) and the horizontal plane can be adjusted to make the position of the crystal Z relative to the actual central axis a of the growth chamber 110 change constantly, so that the crystal Z can deviate from the cold spot of the molten raw material, and the eccentric rotation can also improve the flow capability of the molten raw material around the crystal Z, i.e., improve the heat and mass transfer behavior of the molten raw material around the crystal Z, thereby promoting the growth of the crystal Z, and can also reduce the occurrence of flux inclusions in the crystal, thereby improving the crystal quality.
In order to avoid overflow of the molten material in the growth chamber 110 and to ensure the eccentric rotation effect, the angle formed by the sleeve 121-4 (or the growth chamber 110) and the horizontal plane should be within a predetermined range. In some embodiments, sleeve 121-4 (or growth chamber body 110) may be at an angle in the range of 1-30 degrees from horizontal. In some embodiments, sleeve 121-4 (or growth chamber body 110) may be at an angle in the range of 3-27 from horizontal. In some embodiments, sleeve 121-4 (or growth chamber body 110) may be at an angle in the range of 5-25 degrees from horizontal. In some embodiments, sleeve 121-4 (or growth chamber body 110) may be at an angle in the range of 7-23 degrees from horizontal. In some embodiments, sleeve 121-4 (or growth chamber body 110) may be at an angle in the range of 10-20 degrees from horizontal. In some embodiments, sleeve 121-4 (or growth chamber body 110) may be at an angle in the range of 12-18 degrees from horizontal. In some embodiments, sleeve 121-4 (or growth chamber body 110) may be at an angle in the range of 15-16 degrees from horizontal.
FIG. 4 is a schematic view of a rotatable shaft and sleeve movably coupled according to some embodiments of the present disclosure.
In some embodiments, the rotating rod 121-3 is movably connected to the bottom of the sleeve 121-4 so that the eccentric distance of the eccentric rotation of the growth chamber 110 is adjustable. In some embodiments, the movable connection means that the rotating rod 121-3 is connected to the bottom of the sleeve 121-4, and the relative position of the two can be changed or moved. In some embodiments, the movable connection of the rotating rod 121-3 and the sleeve 121-4 may be achieved by a sliding slot 121-6 and a locking member (not shown in fig. 4). In some embodiments, the eccentric distance of the eccentric rotation (e.g., "d" shown in fig. 4) may be the distance of the actual central axis a of the sleeve 121-4 from the central axis of the rotating rod 121-3.
The movable connection between the rotating rod 121-3 and the sleeve 121-4 is described in an exemplary manner with reference to fig. 4: as shown in fig. 4, the sliding groove 121-6 is fixedly installed on the sleeve 121-4, and the upper end of the rotating rod 121-3 is installed in a sliding rail of the sliding groove 121-6 and can horizontally move along the sliding groove 121-6; when the rotating rod 121-3 moves to a designated position, the locking member can lock, so that the rotating rod 121-3 is fixedly connected with the sleeve 121-4. The rotating rod 121-3 can be locked at any position on the sliding groove 121-6 as required, thereby adjusting the eccentric distance d of the eccentric rotation of the growth chamber 110.
If the eccentric distance d is too small, the eccentricity is too small, and the distance of the crystal Z from a cold point in the molten raw material is too small, so that the flowing capability of the molten raw material around the crystal Z is weaker, the heat and mass transfer behaviors of the molten raw material around the crystal Z are not obviously improved, and the effect of promoting the growth of the crystal Z is not obvious; if the eccentric distance d is too large, the eccentricity is too large, which may cause the crystal Z to collide with the growth cavity 110 during the eccentric rotation process, and may also cause the asymmetry of the thermal field to be more pronounced, the crystal growth shape to be uneven, and the crystal quality to be reduced. Therefore, it is necessary to select an appropriate eccentric distance d.
In some embodiments, the eccentricity is within a preset percentage of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 1% to 20% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 2% to 19% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 3% to 18% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 4% to 17% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 5% to 16% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 6% to 15% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 7% to 14% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 8% to 13% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 9% to 12% of the diameter of the growth chamber 110. In some embodiments, the eccentric distance may be in the range of 10% to 11% of the diameter of the growth chamber 110.
Through the movable connection between the rotating rod 121-3 and the sleeve 121-4, the eccentric rotating eccentric distance of the growth cavity can be adjusted, and then the eccentric distance is adjusted to be located within the preset percentage range of the diameter of the growth cavity 110, so that the proper eccentricity is determined, the distance of the crystal deviating from a cold point in the molten raw material is proper, the flowing capacity of the molten raw material around the crystal is strong, and the crystal cannot collide with the growth cavity 110, and the crystal with uniform shape and high quality is prepared while the crystal growth is promoted.
FIG. 5 is a schematic diagram of an exemplary lift feature according to some embodiments herein.
In some embodiments, as shown in FIG. 5, the lifting member 122 may include a lifting motor 122-1, a second transmission element 122-2, a screw 122-3, a ring groove disk 122-4, and a lifting platform 122-5.
In some embodiments, lift motor 122-1 may drive screw 122-3 to rotate. In some embodiments, the lifting motor 122-1, the second transmission element 122-2 and the screw 122-3 may be in transmission connection, and the lifting motor 122-1 may drive the screw 122-3 to rotate through the second transmission element 122-2.
In some embodiments, a circular groove disk 122-4 may be provided at the bottom of the screw 122-3. In some embodiments, the size of the inner ring of the ring-groove disk 122-4 matches the size of the screw 122-3. In some embodiments, "matching" may be that the inner ring of the annular groove disk 122-4 is the same shape and the same or similar size as the outer wall of the screw 122-3, e.g., the difference between the cross-sectional diameter of the inner ring of the annular groove disk 122-4 and the cross-sectional diameter of the outer wall of the screw 122-3 is within a predetermined threshold range (e.g., 1mm-3 mm). In some embodiments, the ring-groove disk 122-4 may be drivingly connected to the second driving element 122-2, and accordingly the ring-groove disk 122-4, and thus the screw 122-3, may be driven by the lifting motor 122-1.
In some embodiments, the lifting platform 122-5 may be disposed on the screw 122-3 and rotatably connected to the screw 122-3. When the screw 122-3 is driven by the lifting motor 122-1 to rotate, the lifting platform 122-5 can be driven to move up and down.
In some embodiments, the lifting platform 122-5 may be disposed below the rotating component 121, and accordingly, the lifting platform 122-5 and the rotating component 121 may be driven to move up and down (and correspondingly the growth chamber 110 may be driven to move up and down) by the rotation of the screw 122-3.
In some embodiments, the lifting member 122 may also include a lifting rail 122-6. In some embodiments, the lifting platform 122-5 may be disposed on the lifting rail 122-6, which further increases the stability of the lifting platform 122-5 when the rotating member 121 (or the growth chamber 110) is driven to move up and down.
In some embodiments, the outer side of the lifting member 122, the upper portion of the lifting member 122, and/or the bottom of the lifting member 122 may be provided with a lifting member insulating layer (not shown). In some embodiments, the lifting member insulation may include bulk insulation, granular insulation, batting insulation, sheet insulation, and the like. In some embodiments, the material of the heat insulating layer of the lifting member may include metal, alumina, zirconia, silica, tempered aluminum, carbide, nitride, silicide, and other high temperature resistant materials.
By arranging the lifting part heat-insulating layer outside the lifting part 122, on the upper part of the lifting part 122 and/or at the bottom of the lifting part 122, the heat radiation generated by the crucible in the raw material melting and crystal growth processes can be isolated, so that the lifting part 122 is prevented from being damaged due to overhigh temperature caused by the heat radiation.
Because there is a temperature gradient within the thermal field 160, and there is a difference in the magnitude of the temperature gradient at different heights. The lifting platform 122-5 can be moved up and down to drive the rotating part 121 to move up and down, so that the vertical position of the growth cavity 110 in the temperature field 160 is changed, and the temperature gradient of the molten raw materials in the growth cavity is adjusted. For example, increasing the temperature gradient in the molten feedstock promotes mass transfer behavior in the molten feedstock, promoting crystal growth.
When the growth cavity 110 is driven to ascend and descend by the ascending and descending of the ascending and descending component 122, the temperature gradient in the growth cavity 110 can be changed, the spontaneous nucleation of crystals caused by the sudden temperature drop is prevented, the quality of the crystals is influenced, the ascending and descending speed of the ascending and descending component 122 can be controlled, and the cooling speed is maintained within a certain range.
In some embodiments, the lift rate may be in the range of 0.05mm/h to 0.2 mm/h. In some embodiments, the lift rate may be in the range of 0.08mm/h to 0.18 mm/h. In some embodiments, the lift rate may be in the range of 0.1mm/h to 0.15 mm/h. In some embodiments, the lift rate may be in the range of 0.12mm/h to 0.14 mm/h.
In some embodiments, the cooling rate may be in the range of 10 ℃/min to 20 ℃/min. In some embodiments, the cooling rate may be in the range of 10.5 ℃/min to 19.5 ℃/min. In some embodiments, the cooling rate may be in the range of 11 ℃/min to 19 ℃/min. In some embodiments, the cooling rate may be in the range of 11.5 ℃/min to 18.5 ℃/min. In some embodiments, the cooling rate may be in the range of 12 ℃/min to 18 ℃/min. In some embodiments, the cooling rate may be in the range of 12.5 ℃/min to 17.5 ℃/min. In some embodiments, the cooling rate may be in the range of 13 ℃/min to 17 ℃/min. In some embodiments, the cooling rate may be in the range of 13.5 ℃/min to 16.5 ℃/min. In some embodiments, the cooling rate may be in the range of 14 ℃/min to 16 ℃/min. In some embodiments, the cooling rate may be in the range of 14.5 ℃/min to 15.5 ℃/min.
FIG. 6 is an exemplary flow chart of a crystal growth method according to some embodiments described herein. In some embodiments, the process 600 may be performed by one or more components in the crystal growth apparatus 100. In some embodiments, the process 600 may be performed automatically by a control system (e.g., a control component). For example, the process 600 may be implemented by control instructions, based on which the control system controls various components to perform various operations of the process 600. In some embodiments, process 600 may be performed semi-automatically. For example, one or more operations of the process 600 may be performed manually by an operator. In some embodiments, one or more additional operations not described may be added and/or one or more operations discussed herein may be deleted upon completion of process 600. Additionally, the order of the operations shown in FIG. 6 is not limiting. As shown in fig. 6, the process 600 includes the following steps.
Step 610, placing the raw material for crystal growth in the growth chamber.
In some embodiments, the starting material for crystal growth may be the starting material required to grow the target crystal. In some embodiments, the starting material for growing the crystals may be a powder, a cake, a granule, or the like.
In some embodiments, the purity of the starting material for growing the crystal may be greater than or equal to 90.00%. In some embodiments, the purity of the starting material for growing the crystal may be greater than or equal to 92.00%. In some embodiments, the purity of the starting material for growing the crystal may be greater than or equal to 95.00%. In some embodiments, the purity of the starting material for growing the crystal may be greater than or equal to 99.00%. In some embodiments, the purity of the starting material for growing the crystal may be greater than or equal to 99.9%. In some embodiments, the purity of the raw material for growing the crystal may be greater than or equal to 99.99%. In some embodiments, the raw material purity of the growing crystal may be greater than or equal to 99.999%.
In some embodiments, the raw materials for crystal growth and the auxiliary materials (e.g., flux) for crystal growth may be mixed uniformly and then placed in the growth chamber 110. In some embodiments, flux may refer to a material capable of lowering the melting temperature of a substance (e.g., a source material from which crystals are grown). In some embodiments, the flux may include, but is not limited to, fluorides (e.g., lithium fluoride, sodium fluoride, aluminum fluoride, bismuth fluoride, lead fluoride, barium fluoride), chlorides (e.g., potassium chloride, calcium chloride), oxides (lead oxide, boron oxide, sodium oxide, molybdenum oxide, bismuth oxide), and the like.
Step 620, heating the growth chamber to provide the heat required for crystal growth.
In some embodiments, the growth chamber may be heated by a heating assembly to provide the heat required for crystal growth. In some embodiments, the heating assembly may be arranged in segments, and the plurality of heating segments may be independently controlled to heat the growth chamber. For more details on the heating manner of the heating element, reference may be made to the description of the heating element 130 in fig. 1, which is not repeated herein.
In step 630, in the process of crystal growth, when a preset condition is met, the rotating part (e.g., the rotating part 121) of the moving component (e.g., the moving component 120) drives the growth cavity to eccentrically rotate.
In some embodiments, the predetermined condition may be that the crystal growth rate is below a rate threshold.
In some embodiments, the crystal growth rate may include a crystal weight growth rate, a crystal volume growth rate, a crystal diameter growth rate, a crystal pulling rate, a liquid level lowering rate, and the like.
In some embodiments, the control component may determine the crystal growth rate based on the crystal growth parameter. In some embodiments, the crystal growth parameters may be monitored by a monitoring component. In some embodiments, the crystal growth parameters may include crystal growth weight, crystal growth volume, crystal pulling height, crystal growth diameter, and the like. In some embodiments, the control component may determine the crystal growth rate based on a plurality of crystal growth parameters. For example, the control component may determine the crystal growth rate based on a plurality of crystal growth weights over a period of time. As another example, the control component may determine the crystal growth rate based on a plurality of crystal growth heights over a period of time.
In some embodiments, the rate threshold may be a system default or a manual preset. In some embodiments, different crystal types or different growth environments may correspond to different rate thresholds.
In some embodiments, the control component may also determine the velocity threshold based on a crystal growth model. In some embodiments, the control component can construct a crystal growth model based on crystal growth size, crystal growth weight, melt level height, and the like, which can characterize theoretical growth of the crystal throughout the growth process. In some embodiments, the crystal growth process includes multiple stages (e.g., seeding stage, shouldering stage, isodiametric stage, ending stage). In some embodiments, the velocity thresholds are different for the various stages of the crystal growth process. In some embodiments, a crystal growth model may be used to determine a time-varying velocity threshold.
As described in connection with fig. 3, when the temperature of the molten raw material is lowered to a certain degree, the viscosity of the molten raw material increases sharply, and mass and heat transfer of the solute in the molten raw material are slowed down, resulting in slow crystal growth, and even flux inclusion inside the crystal. Correspondingly, when the crystal growth rate is lower than the rate threshold, the rotating component of the moving component can drive the growth cavity to eccentrically rotate so as to improve the heat and mass transfer behaviors of the solute and promote the further growth of the crystal to improve the crystal quality.
In some embodiments, the control assembly may adjust the eccentric rotation parameter of rotating component 121 if the crystal growth rate is below a rate threshold. In some embodiments, the eccentric rotation parameters include an eccentric distance, a rotation rate, and the like. For example, if the crystal growth rate is below a rate threshold, the eccentricity distance may be increased and/or the rotation rate may be increased. As another example, the eccentricity distance and/or the rotation rate may be adjusted separately under different circumstances (e.g., different crystal types, different crystal growth rates). Also for example, the eccentricity distance and/or the rotation rate, etc. may be dynamically adjusted according to the crystal growth rate.
When the crystal growth rate is lower than the rate threshold value, the eccentric distance between the rotating rod and the sleeve or the rotating speed of the rotating rod is adjusted through the control assembly, so that the distance of the crystal from a cold point in the molten raw material is proper, the flowing capacity of the molten raw material around the crystal is enhanced on the premise that the crystal is not collided with the growth cavity, and the crystal with uniform shape and high quality is prepared while the crystal growth is promoted.
In some embodiments, the control component may also cause the growth chamber to ascend or descend by controlling the lifting component (e.g., lifting component 122) of the motion component (e.g., motion component 120) if the crystal growth rate is below the rate threshold.
In some embodiments, the control assembly may adjust the lifting parameters of the lifting member if the crystal growth rate is below a rate threshold. In some embodiments, the lift parameters may include lift rate, lift distance, and the like. For example, if the crystal growth rate is below a rate threshold, the lift rate may be increased and/or the lift distance may be increased. As another example, the lift rate and/or lift distance may be adjusted separately under different circumstances (e.g., different crystal types, different crystal growth rates). Also for example, the lifting rate and/or lifting distance, etc. may be dynamically adjusted based on the crystal growth rate.
When the crystal growth rate is lower than the rate threshold, the lifting rate or the lifting distance of the lifting component is adjusted through the control assembly, so that the vertical position of the growth cavity in a temperature field can be changed, the temperature gradient of the molten raw material is adjusted, the mass transfer behavior in the molten raw material is promoted, and the crystal growth is promoted.
In some embodiments, the control assembly may cause the growth chamber to rotate and ascend eccentrically simultaneously, or both, by controlling the rotation member and the lift member of the motion assembly simultaneously if the crystal growth rate is below a rate threshold. In some embodiments, the control assembly may simultaneously adjust the eccentric rotation parameter of the rotating member and the lift parameter of the lift member to promote crystal growth if the crystal growth rate is below a rate threshold.
In some embodiments, if the crystal growth rate is lower than the rate threshold, the control component may control the rotating component to drive the growth chamber to eccentrically rotate, and then control the lifting component to drive the growth chamber to ascend or descend. In some embodiments, if the crystal growth rate is lower than the rate threshold, the control component may control the lifting component to drive the growth chamber to ascend or descend, and then control the rotating component to drive the growth chamber to eccentrically rotate.
In some embodiments, the control assembly may also adjust a heating related parameter of the heating assembly during the crystal growth process. In some embodiments, the heating-related parameters of the heating assembly may include heating power, current, voltage, rate of change of power, and the like. In some embodiments, the control assembly may decrease the heating power of the heating assembly to increase the crystal growth rate if the crystal growth rate is below the speed threshold. In some embodiments, if the crystal growth rate is above the speed threshold, the control assembly may increase the heating power of the heating assembly such that the crystal growth rate is at or below the speed threshold. In some embodiments, if the crystal growth rate is below or above the speed threshold, the control assembly may increase the heating power of at least one heating segment in the heating assembly and decrease the heating power of the remaining at least one heating segment in the heating assembly such that the crystal growth rate is equal to or similar to the speed threshold. By adjusting the heating related parameters of the heating assembly, crystals with uniform size and good weight can be grown.
It should be noted that the above description of the flow 600 is for illustration and description only, and does not limit the scope of the application of the present disclosure. Various modifications and changes to flow 600 will be apparent to those skilled in the art in light of this description. However, such modifications and variations are intended to be within the scope of the present description. For example, the crystal growth parameter may be a crystal growth volume, and the control component may determine the crystal growth rate based on a plurality of crystal growth volumes over a period of time. For another example, the process 600 may further include: in the process of crystal growth, when a preset condition is met, the lifting component of the movement component drives the growth cavity to ascend or descend. For another example, the control assembly may cross-control the lifting member and the rotating member to cross-adjust the eccentric rotation parameter of the rotating member and the lifting parameter of the lifting member if the crystal growth rate is below a rate threshold.
Examples
Example 1: and (3) growing a beta-BBO nonlinear optical crystal.
Step 1: barium carbonate, boric acid and NaCl fluxing agent which are raw materials required by crystal growth are mixed according to the mass ratio of 1: (0.6-0.8): (0.1-0.3) weighing, fully mixing, pressing into blocks, and filling into a platinum crucible. The platinum crucible filled with the raw material is placed in a ceramic sleeve in a crystal growth device, and a gap between the platinum crucible and the ceramic sleeve is filled with high-temperature refractory cotton. And adjusting the platinum crucible, the temperature field and the heating assembly to be positioned at the same axis, so that the platinum crucible is positioned in symmetrical temperature field distribution.
Step 2: and (3) starting heating and melting, and determining the saturation temperature point of the molten raw materials by using a trial contact method when the heating power is increased to 4200W, wherein the saturation temperature point is in the range of 800-850 ℃. After the saturation temperature point is determined, slowly immersing part of beta-BBO seed crystals into the molten raw materials and keeping the temperature for 1 h.
And step 3: and setting the crystal to grow according to the growth rate of the crystal weight of 30-35 g/day, and monitoring the crystal growth weight monitored by the weight sensing assembly in the process. In the initial stage of crystal growth, because the temperature of the molten raw material is higher, the viscosity of the molten raw material is lower, and the mass transfer behavior is obvious, the temperature reduction rate is automatically adjusted by the control assembly in the stage, and the rotation rate and/or the up-and-down movement rate of the pulling rod and the seed crystal or the crystal are driven by the control movement device, so that the crystal growth rate meets the rate threshold. Generally, the process can be maintained for 10-15 days.
And 4, step 4: when the crystal growth process is continued, the viscosity of the molten raw material is sharply increased due to the reduction of the temperature of the molten raw material, the mass transfer behavior of the solute is hindered at the moment, and the crystal growth rate is difficult to continuously maintain within the rate threshold range, possibly causing crystal pull-off. And starting the rotating part to make the central axis of the platinum crucible deviate from the central axis of the crystal, keeping the eccentric distance within the range of 1-20% of the diameter of the platinum crucible, driving the platinum crucible to rotate, increasing the mass transfer speed of the solute and continuing to grow the crystal. During this phase, the control assembly may control the rotation rate of the rotating member and/or adjust the eccentric distance of the platinum crucible based on the crystal growth weight monitored by the weight sensing assembly such that the crystal growth rate is within a rate threshold.
And 5: when the crystal growth process is continued, if the rotating component drives the platinum crucible to eccentrically rotate and the crystal growth rate is difficult to keep meeting the rate threshold, the lifting component is started to drive the platinum crucible to ascend or descend, the lifting rate is in the range of 0.05 mm/h-0.2 mm/h, the temperature gradient of the molten raw materials in the platinum crucible is changed, the transfer rate of solute and the crystal growth rate are further accelerated, and the crystal growth rate is in the range of the rate threshold.
Through the above-mentioned a series of control step flows: the moving device drives the lifting rod and the seed crystal or the crystal to move up and down and/or rotate so as to grow the crystal → the rotating part drives the platinum crucible to rotate eccentrically so as to improve the mass transfer behavior, so that the crystal growth is continued → the lifting part drives the platinum crucible to ascend or descend, and the temperature gradient in the molten raw material is changed so as to realize the growth of the crystal with larger size.
The beneficial effects that may be brought by the embodiments of the present description include, but are not limited to: (1) the rotating part drives the growth cavity to eccentrically rotate, so that the crystal can deviate from a cold spot of a molten raw material, the flowing capacity of the molten raw material around the crystal is improved, namely, the heat and mass transfer behaviors of the molten raw material around the crystal are improved, the growth of the crystal is further promoted, a fluxing agent inclusion in the crystal can be reduced, and the quality of the crystal is improved; (2) the sleeve and the heat insulation layer are arranged on the periphery of the growth cavity, so that the growth cavity is prevented from moving or sliding along the radial direction due to centrifugal action in the eccentric rotation process, the growth cavity is prevented from falling or colliding, the molten raw material in the growth cavity is prevented from splashing due to the radial movement and oscillation of the growth cavity, the liquid level of the molten raw material is ensured to be stable, and the growth quality of the crystal is ensured; (3) the rotating rod is movably connected with the bottom of the sleeve, so that the eccentric distance of the eccentric rotation of the growth cavity can be adjusted, and the proper eccentric distance can be determined according to different conditions, so that the distance of the crystal from a cold point in the molten raw material is proper, the flowing capability of the molten raw material around the crystal is strong, and the crystal cannot collide with the growth cavity, and the crystal with uniform shape and high quality is prepared while the growth of the crystal is promoted; (4) through setting up the lifting unit, can change the high position of growth cavity in the temperature field, and then can adjust the temperature gradient in the melt, promote the transmission action of solute, promote the growth of crystal.
Having thus described the basic concept, it will be apparent to those skilled in the art that the foregoing detailed disclosure is to be regarded as illustrative only and not as limiting the present specification. Various modifications, improvements and adaptations to the present description may occur to those skilled in the art, although not explicitly described herein. Such modifications, improvements and adaptations are proposed in the present specification and thus fall within the spirit and scope of the exemplary embodiments of the present specification.
Also, the description uses specific words to describe embodiments of the description. Reference throughout this specification to "one embodiment," "an embodiment," and/or "some embodiments" means that a particular feature, structure, or characteristic described in connection with at least one embodiment of the specification is included. Therefore, it is emphasized and should be appreciated that two or more references to "an embodiment" or "one embodiment" or "an alternative embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, some features, structures, or characteristics of one or more embodiments of the specification may be combined as appropriate.
Additionally, the order in which the elements and sequences of the process are recited in the specification, the use of alphanumeric characters, or other designations, is not intended to limit the order in which the processes and methods of the specification occur, unless otherwise specified in the claims. While various presently contemplated embodiments of the invention have been discussed in the foregoing disclosure by way of example, it is to be understood that such detail is solely for that purpose and that the appended claims are not limited to the disclosed embodiments, but, on the contrary, are intended to cover all modifications and equivalent arrangements that are within the spirit and scope of the embodiments herein. For example, although the system components described above may be implemented by hardware devices, they may also be implemented by software-only solutions, such as installing the described system on an existing server or mobile device.
Similarly, it should be noted that in the preceding description of embodiments of the present specification, various features are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure aiding in the understanding of one or more of the embodiments. This method of disclosure, however, is not intended to imply that more features than are expressly recited in a claim. Indeed, the embodiments may be characterized as having less than all of the features of a single embodiment disclosed above.
Numerals describing the number of components, attributes, etc. are used in some embodiments, it being understood that such numerals used in the description of the embodiments are modified in some instances by the use of the modifier "about", "approximately" or "substantially". Unless otherwise indicated, "about", "approximately" or "substantially" indicates that the number allows a variation of ± 20%. Accordingly, in some embodiments, the numerical parameters used in the specification and claims are approximations that may vary depending upon the desired properties of the individual embodiments. In some embodiments, the numerical parameter should take into account the specified significant digits and employ a general digit preserving approach. Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the range are approximations, in the specific examples, such numerical values are set forth as precisely as possible within the scope of the application.
For each patent, patent application publication, and other material, such as articles, books, specifications, publications, documents, etc., cited in this specification, the entire contents of each are hereby incorporated by reference into this specification. Except where the application history document does not conform to or conflict with the contents of the present specification, it is to be understood that the application history document, as used herein in the present specification or appended claims, is intended to define the broadest scope of the present specification (whether presently or later in the specification) rather than the broadest scope of the present specification. It is to be understood that the descriptions, definitions and/or uses of terms in the accompanying materials of this specification shall control if they are inconsistent or contrary to the descriptions and/or uses of terms in this specification.
Finally, it should be understood that the embodiments described herein are merely illustrative of the principles of the embodiments of the present disclosure. Other variations are also possible within the scope of the present description. Thus, by way of example, and not limitation, alternative configurations of the embodiments of the specification can be considered consistent with the teachings of the specification. Accordingly, the embodiments of the present description are not limited to only those embodiments explicitly described and depicted herein.

Claims (10)

1. A crystal growth apparatus, comprising:
the growth cavity is used for placing raw materials for crystal growth;
the heating assembly is used for heating the growth cavity to provide heat required by crystal growth;
the motion assembly comprises a rotating part, and the rotating part is in transmission connection with the growth cavity to drive the growth cavity to rotate eccentrically.
2. The crystal growth apparatus of claim 1, wherein the rotating component comprises:
the sleeve is at least partially sleeved on the periphery of the growth cavity;
and the rotating rod is connected with the sleeve and drives the growth cavity to eccentrically rotate.
3. The crystal growth apparatus of claim 2, wherein the rotating rod is movably coupled to a bottom of the sleeve such that an eccentric distance of the eccentric rotation of the growth chamber is adjustable.
4. The crystal growth apparatus of claim 1, wherein the eccentric distance of the eccentric rotation of the growth chamber is in the range of 1% to 20% of the diameter of the growth chamber.
5. The crystal growth apparatus of claim 1, wherein the motion assembly further comprises a lifting member drivingly connected to the growth chamber to move the growth chamber up or down.
6. The crystal growth apparatus of claim 5, further comprising:
a monitoring component for monitoring crystal growth parameters;
a control assembly that adjusts a heating related parameter of the heating assembly and/or a motion related parameter of the motion assembly based on the crystal growth parameter.
7. The crystal growth apparatus of claim 6, wherein to adjust the heating related parameter of the heating assembly and/or the motion related parameter of the motion assembly based on the crystal growth parameter, the control assembly:
determining a crystal growth rate based on the crystal growth parameters;
the crystal growth rate is below a rate threshold, and an eccentric rotation parameter of the rotating component is adjusted, the eccentric rotation parameter comprising at least one of an eccentric distance or a rotation rate.
8. The crystal growth apparatus of claim 6, wherein to adjust the heating related parameter of the heating assembly and/or the motion related parameter of the motion assembly based on the crystal growth parameter, the control assembly:
determining a crystal growth rate based on the crystal growth parameters;
the crystal growth rate is below a rate threshold, and a lift parameter of the lift member is adjusted, the lift parameter comprising at least one of a lift rate or a lift distance.
9. A crystal growth method, characterized by comprising:
placing the raw material for crystal growth in a growth cavity;
heating the growth chamber to provide heat required for the crystal growth;
in the crystal growth process, when the preset conditions are met, the rotating part of the moving assembly drives the growth cavity to eccentrically rotate.
10. The method of claim 9, wherein the crystal growth method further comprises:
determining a crystal growth rate based on the crystal growth parameters;
the crystal growth rate is below a rate threshold, and an eccentric rotation parameter of the rotating component is adjusted, the eccentric rotation parameter comprising at least one of an eccentric distance or a rotation rate.
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CN115044964A (en) * 2022-07-19 2022-09-13 眉山博雅新材料股份有限公司 Crystal preparation device
CN117187944A (en) * 2022-10-25 2023-12-08 浙江晶盛机电股份有限公司 Adjusting mechanism and single crystal furnace
CN117187944B (en) * 2022-10-25 2024-04-19 浙江晶盛机电股份有限公司 Adjusting mechanism and single crystal furnace

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CN109576778A (en) * 2018-12-25 2019-04-05 内蒙古中环光伏材料有限公司 A method of reducing the impurity content that CZ method prepares monocrystalline

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CN105603503A (en) * 2016-01-13 2016-05-25 重庆大学 Planet type rotational solution process crystal growth apparatus
CN109576778A (en) * 2018-12-25 2019-04-05 内蒙古中环光伏材料有限公司 A method of reducing the impurity content that CZ method prepares monocrystalline

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CN115044964A (en) * 2022-07-19 2022-09-13 眉山博雅新材料股份有限公司 Crystal preparation device
CN117187944A (en) * 2022-10-25 2023-12-08 浙江晶盛机电股份有限公司 Adjusting mechanism and single crystal furnace
CN117187944B (en) * 2022-10-25 2024-04-19 浙江晶盛机电股份有限公司 Adjusting mechanism and single crystal furnace

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