Crystal growth apparatus
The furnace apparatus with crucible deposition sections and precise temperature control addresses the challenge of growing large, high-quality crystals by enhancing nucleation and growth uniformity, resulting in improved crystal quality and efficiency.
Patent Information
- Application Number
- JP2021528851
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2018-11-22
- Filing Date
- 2019-11-19
- Publication Date
- 2025-01-08
- Estimated Expiration
- 2039-11-19
AI Technical Summary
Existing methods face challenges in providing stable temperature, pressure, and gas conditions for growing large, high-quality single crystals of materials like SiC and Al2O3, leading to difficulties in achieving uniform crystal growth.
A furnace apparatus with a crucible design that includes deposition sections on the sidewalls and top for seed crystals, allowing controlled crystal growth away from the bottom, combined with precise temperature management and reactant injection systems to enhance nucleation and growth.
The apparatus enables the growth of larger, higher-quality crystals by reducing atomic stacking faults and ensuring a uniform temperature gradient, facilitating controlled crystal growth and multiple crystal formation simultaneously.
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Abstract
Description
[Technical field]
[0001] The present invention relates to an apparatus for growing crystals and to a method for growing crystals. [Background technology]
[0002] A single crystal, or monocrystalline solid, is a material in which the crystal lattice throughout the sample is continuous and unbroken all the way to the edges of the sample without grain boundaries. The absence of defects associated with grain boundaries can give single crystals unique properties, particularly mechanical, optical, and electrical, and, depending on the type of crystal structure, may even be anisotropic. These properties, in addition to making some gemstones valuable, are used industrially in technological applications, particularly in optics and electronics.
[0003] Crystal growth is the process by which pre-existing crystals become larger as more molecules or ions are added to their positions in the crystal lattice. A crystal is defined as a crystal lattice that extends in all three spatial dimensions, with atoms, molecules, or ions arranged in a regular repeating pattern. Therefore, crystal growth differs from droplet growth in that, for an ordered crystal to grow, the molecules or ions must fall into the correct lattice positions during growth.
[0004] Crystallization of biopolymers such as proteins is basically performed in the same manner as in the case of general low molecular weight compounds such as inorganic salts, by removing the solvent from an aqueous or anhydrous solution containing the polymer, thereby creating a supersaturated state and growing the crystals. Typical methods for this purpose include, for example, the batch method, the dialysis method, and the gas-liquid correlation diffusion method, and are selected according to the type, amount, properties, etc. of the sample.
[0005] For example, crystal growth can be used to obtain single crystals of semiconductors (eg, silicon, germanium, and gallium arsenide), metals (eg, palladium, platinum, silver, gold), salts, and synthetic gems.
[0006] A further application could be the growth of large cylindrical ingots or boules of single crystal silicon that are used in the electronics industry to manufacture semiconductor devices such as integrated circuits.
[0007] To grow a crystal, a crucible is placed in the chamber of a furnace. To form a crystalline component, a seed crystal is placed in the crucible. The seed crystal is generally made of the desired crystalline material from which the crystalline component is to be formed. The furnace is heated so that the crystalline material in the crucible is provided in a molten and liquid state. The crystalline component is formed by growing the crystalline component starting from the seed crystal at the bottom of the crucible.
[0008] However, it is difficult to provide stable temperature, pressure and gas during the growth process, and therefore it is difficult to grow large, high-quality single crystals made of SiC, Al2O3, etc. Summary of the Invention [Problem to be solved by the invention]
[0009] SUMMARY OF THE PRESENT EMBODIMENT It is therefore an object of the present invention to provide a furnace for growing crystals that has a homogeneous atmosphere for growing large crystals. [Means for solving the problem]
[0010] This object is solved by an apparatus for growing crystals and a method for growing crystals according to the independent claims.
[0011] According to a first aspect of the present invention, an apparatus for growing a crystal is provided. The apparatus comprises a chamber and a crucible disposed in a heatable containment space of the chamber, the crucible comprising an interior volume configured to grow a crystal therein. The crucible comprises a bottom with each sidewall extending to a top of the crucible. The crucible comprises at least one deposition section configured to mount a seed crystal, the deposition section being formed in at least one of the sidewalls and the top of the crucible.
[0012] According to a further aspect of the present invention, a method for growing a crystal is provided, in which a seed crystal is attached to a deposition section of a crucible, the deposition section being formed in at least one of a sidewall and an upper portion of the crucible, and the crystal is grown within an interior volume of the crucible, the interior volume being disposed within a heatable accommodation space of a chamber.
[0013] The apparatus may be a furnace with a chamber providing a heatable containment space for the crucible. The apparatus and the crucible each heat the interior volume of the crucible until a desired temperature is reached. The temperature that may be provided within the interior volume may be from 100° C. to 1400° C., preferably about 2100° C. or higher. The chamber may include insulation such that the interior volume of the crucible is thermally isolated from the environment surrounding the enclosure, i.e., the intermediate volume.
[0014] The crucible comprises an internal volume in which crystal growth occurs. A seed element may be disposed within the crucible. The seed element is made of a desired single crystal material, such as sapphire. Further, a reactive fluid, e.g., a reactive liquid or gas, such as a desired crystal material, e.g., high purity alumina crackle, is placed within the internal volume of the crucible. As the temperature within the crucible increases, the desired material within the reactive liquid / gas grows on the surface of the seed crystal. The crucible comprises a cylindrical shape with a circular, elliptical or rectangular base.
[0015] The aim is to provide a desired temperature gradient within the interior volume of the crucible to control the growth of the crystal, however, due to convection it is difficult to provide, for example, a higher temperature in the bottom region than in other regions of the interior volume of the crucible.
[0016] Thus, according to the inventive approach, the deposition of seed crystals is placed in a deposition section defined on the side wall or on the top of the crucible. The seed crystals may be attached to the deposition section, for example, by means of a specific adhesive. Furthermore, the deposition section may form a step on the inner wall of the crucible, so that the seed crystals can be placed on the step forming the deposition section without any adhesive.
[0017] Thus, the crystal growth occurs in the region of the internal volume away from the bottom, where temperature control may be more accurate. When the deposition section is located on the side wall or on the top of the crucible, the crystal growth from each seed crystal is directed laterally from the side wall of the crucible to the center of the crucible, or upside down from the top to the bottom of the crucible. Based on the lateral growth and top-to-bottom growth directions, the nucleation on the deposition section is appropriately controlled so that atomic stacking faults can be reduced. Thus, the crystal growth occurs in the desired growth atmosphere inside the internal volume of the crucible, and larger crystals can be grown.
[0018] According to an exemplary embodiment of the present invention, the bottom does not have a deposition section for the seed crystal, so the temperature near the bottom inside the internal volume does not affect uniform crystal growth inside the middle and top of the crucible.
[0019] According to a further exemplary embodiment, the crucible extends along a vertical direction between a bottom and a top, in other words a bottom at the bottom of the crucible and a top at the top of the crucible.
[0020] According to a further exemplary embodiment of the present invention, the crucible comprises a plurality of deposition sections, each configured to receive a seed crystal, the deposition sections being spaced apart from one another and formed on at least one of a sidewall and an upper portion of the crucible, such that a plurality of crystals can be grown from different lateral and upper portions of the crucible in a direction toward the center of the crucible.
[0021] According to a further exemplary embodiment, the crucible comprises at least one protrusion extending from an inner surface, in particular from a side wall or an upper portion of the crucible, into the interior volume, and the deposition section is formed on the protrusion. Thus, the deposition section can be formed with a step on the inner wall of the crucible, such that the seed crystal can be placed on the step forming the deposition section without any adhesive.
[0022] According to a further exemplary embodiment, the crucible includes a plurality of protrusions extending from an inner surface of the crucible into the interior volume, the protrusions being spaced apart from one another.
[0023] According to a further exemplary embodiment, the crucible includes at least one nozzle configured to inject a reactive fluid (eg, a reactive liquid or a reactive gas) into the interior volume of the crucible.
[0024] In particular, according to a further exemplary embodiment, at least one nozzle is configured to emit a reactive fluid / liquid in a direction towards one of the deposition sections. The reactive fluid / liquid may be a gas, vapor or liquid medium. In particular, the reactive fluid / liquid may be a gas or vapor mixture having a single or mixture of C-, H-, CH- solutions or vapors.
[0025] According to a further exemplary embodiment, the crucible comprises an ejection column element that extends partially between the bottom and the top of the crucible and comprises at least one nozzle. The ejection column element has a rod shape and can be fixed, for example, to the bottom of the crucible. The ejection column element can be, for example, a kind of shower head with a number of nozzles, each nozzle being directed towards a respective deposition side. In particular, the ejection column element extends, for example, along the central axis of the cylindrical shape of the crucible. Thus, each nozzle arranged on the ejection column element is directed from the center of the crucible towards the side wall of the crucible. Furthermore, the upper end of the ejection column element can be arranged at a distance from the top of the crucible. At the upper end of the ejection column element, each nozzle can be arranged that is directed towards the deposition section arranged at the top of the crucible.
[0026] According to a further exemplary embodiment, the discharge column element is connected to a reaction liquid interface formed at the bottom of the crucible, the discharge column element is thus formed, for example, as a hollow column or pillar, and gas lines extend from the bottom of the column to respective nozzles arranged on the discharge column element.
[0027] According to a further exemplary embodiment, the crucible comprises an injection interface for injecting an injection fluid, for example an injection liquid or an injection gas, which can be connected to a pressure regulating valve for adjusting the pressure in the internal volume. For example, the injection interface comprises one or more openings, for example, arranged at the top of the crucible. In particular, the injection interface may be arranged at a position opposite the crucible with respect to the reaction liquid interface. In particular, a pressure regulating valve is provided for adjusting the pressure of the injection liquid, for example, between 1 millibar (100 Pa) and 10 bar (1 MPa). The injection liquid may be injected in liquid and / or gaseous state. The injection liquid may be reacted with the reaction liquid. For example, the reaction liquid may be a first component and the injection liquid may be a second component. After the reaction of the first component with the second component, a raw material that can be sublimated on the seed crystal and a crystal layer already formed on the seed crystal are generated, respectively.
[0028] A pressure regulating valve for regulating the pressure in the internal volume and an injection interface are connected for injecting liquid / gas and for flowing liquid / gas to reduce the pressure in the crucible.
[0029] According to a further exemplary embodiment, the chamber comprises a number of heating elements for providing thermal energy to the crucible, in particular surrounding the outer wall of the chamber. The heating elements may also be arranged in the accommodation space between the outer wall of the chamber and the side wall of the crucible. The heating elements may for example be tubes surrounding the chamber and the crucible, respectively, the tubes containing a heating medium, such as a hot liquid or a hot gas. For example, the heating elements may surround the side wall and further surround the top and bottom of the crucible.
[0030] According to a further exemplary embodiment, the plurality of heating elements are configured to heat the interior volume to a temperature between 1350°C and 1450°C.
[0031] According to a further exemplary embodiment, the plurality of heating elements are selected from one of a RF (radio frequency) heater, a resistive heater, and a heat generator.
[0032] According to a further exemplary embodiment, there is provided a thermal insulator disposed in the containment space between the crucible and the walls of the chamber, the thermal insulator maintaining a temperature gradient in the space and protecting the chamber walls.
[0033] According to a further exemplary embodiment, the crucible is made of a material selected from one of the group including metal-based, oxide-based, nitride-based, carbon-based, and dense graphite.
[0034] According to a further exemplary embodiment, the device comprises a growth enhancement device for enhancing the nucleation of crystals on the deposition section, the growth enhancement device being selected from one of the group consisting of a plasma source, a microwave source, and a laser source. The growth enhancement device increases the temperature inside the crucible so that the growth rate of the crystals increases. The temperature inside the crucible can be controlled more precisely by the growth enhancement device than, for example, by a heating element surrounding the crucible. Thus, the base temperature can be controlled by the heating element, and the temperature change or more detailed temperature profile in the crucible can be controlled by the growth enhancement device.
[0035] The growth enhancement device can be located directly inside the crucible (e.g., if the growth enhancement device is a laser source) or outside the crucible (e.g., if the growth enhancement device is a microwave source). For example, the laser source can be located at the top or bottom of the crucible.
[0036] According to a further exemplary embodiment of the method, a source material is provided in the crucible, the source material being selected from one of the group consisting of a solid phase material, a liquid phase material, and a mixed phase material.
[0037] According to a further exemplary embodiment of the method, a reactive fluid / liquid is injected into the interior volume of the crucible, the reactive fluid / liquid being selected from one of the group consisting of gases or vapors having a single or mixture of C-, H-, CH- solutions or vapors.
[0038] According to a further exemplary embodiment, a source material is provided that is one of a reactant gas / liquid and an injectant gas / liquid in a crucible, the source material being selected from one of the group consisting of a solid phase material, a liquid phase material, a gas phase material comprising a C-, H-, CH- solution, and a mixed phase material. The reactant gas / liquid and the injectant gas / liquid may comprise methylsilicochloroform (MTS) and a precursor nucleus, for example, -C5H5 or CxHy.
[0039] It should be noted that the embodiments of the present invention have been described with reference to different subject matters. In particular, some embodiments have been described with reference to device type claims, while other embodiments have been described with reference to method type claims. However, unless otherwise known, a person skilled in the art will understand that in addition to any combination of features belonging to one type of subject matter, any combination between features relating to different subject matters, in particular any combination between features of device type claims and features of method type claims that are considered to be disclosed in this application, is also considered to be disclosed along with this application.
[0040] The above defined aspects and further aspects of the invention are apparent from and will be elucidated with reference to the exemplary embodiments described hereinafter. The invention is explained in more detail below with reference to exemplary embodiments, but the invention is not limited thereto. [Brief description of the drawings]
[0041] [Figure 1]FIG. 1 shows a schematic diagram of an apparatus for growing crystals according to an exemplary embodiment of the invention. [Diagram 2] FIG. 2 shows polycrystalline pieces formed in the upper deposition section of the apparatus according to an exemplary embodiment of the invention. [Diagram 3] FIG. 3 shows multiple crystals in a lateral deposition section of an apparatus according to an exemplary embodiment of the invention. [Figure 4] FIG. 4 shows a number of unoriented crystals produced on the lower side of a lateral deposition section of an apparatus according to an exemplary embodiment of the invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0042] The figures of the drawings are intended to be schematic and it should be noted that in different figures, similar or identical elements are provided with the same reference symbols.
[0043] 1 shows a schematic diagram of an apparatus 100 for growing crystals according to an exemplary embodiment of the invention. The apparatus comprises a chamber 101 and a crucible 102 disposed within a heatable containment space 103 of the chamber 101, the crucible 102 comprising an interior volume 104 configured to grow a crystal therein. The crucible 102 comprises a bottom 105 with each sidewall 106 extending to a top 107 of the crucible 102. The crucible 102 comprises at least one deposition section configured to mount a seed crystal 108, the deposition section being formed on at least one of the sidewalls 106 and the top 107 of the crucible 102.
[0044] The chamber 101 provides a heatable containment space 103 for the crucible 102. The apparatus 100 and the crucible 102 each heat the inner volume 104 of the crucible until a desired temperature is reached. The temperature that can be provided inside the inner volume 104 can be from 100° C. to 1400° C., preferably about 2100° C. or higher. The chamber 101 includes insulation 121 so that the inner volume 104 of the crucible is thermally isolated from the environment surrounding the chamber 101, i.e., the intermediate volume.
[0045] The crucible 102 comprises an interior volume 104 in which crystal growth takes place. A seed element 108 is disposed within the crucible 104. The seed element 108 is made of a desired single crystal material, such as sapphire. Additionally, a reaction gas / liquid 111 of the desired crystal material, e.g., high purity alumina crackle, is injected into the interior volume 104 of the crucible 102. As the temperature within the crucible 102 increases, the desired material within the reaction gas / liquid grows on the surface of the seed crystal 108. The crucible 102 may comprise a cylindrical shape with a circular, elliptical, or rectangular base.
[0046] The seed crystal 108 is placed on the side wall 106 of the crucible 102 or on the deposition sections D1-D7 defined in the top 107 of the crucible 102. The seed crystal 108 is attached to the deposition sections D1-D7, for example, by means of a specific adhesive. Furthermore, the deposition sections D1-D7 form steps on the inner wall 106 of the crucible 102, such that the seed crystal 108 can be placed on the steps forming the deposition sections D1-D7 without adhesive.
[0047] Thus, the crystal growth takes place in the region of the internal volume 104 away from the bottom 105, allowing for more accurate temperature control. If the deposition sections D1-D7 are arranged on the side walls 106 of the crucible or on its top 107, the crystal growth from the various crystals 108 is directed laterally from the side walls 106 of the crucible 102 towards the center of the crucible 102, or upside down from the top 107 of the crucible 102 to the bottom 105 of the crucible 102. Based on the lateral growth and the growth direction from the top 107 to the bottom 105, the nucleation on the deposition sections D1-D7 is appropriately controlled so as to reduce atomic stacking faults. As can be seen from FIG. 1, the bottom 105 does not include deposition sections D1-D7 for the seed crystals 108. Therefore, the temperature near the bottom 105 within the interior volume 104 does not affect uniform crystal growth inside the center and top of the crucible 102 .
[0048] 1, the crucible 102 comprises a number of deposition sections D1-D7 configured to mount various crystals 108. The deposition sections D1-D7 are spaced apart from one another and formed on at least one of the side walls 106 and the top 107 of the crucible 102. Thus, multiple crystals can be grown from different lateral and top positions of the crucible 100 in a direction towards the center of the crucible 100.
[0049] The deposition sections D1-D7 are formed by protrusions extending from an inner surface, in particular from a side wall 106 or a top 107 of the crucible 102, into the interior volume 104.
[0050] Further shown is a nozzle 110 of the crucible 102 configured to inject a reactant gas / liquid into the interior volume 104 of the crucible 102. The nozzle 110 is configured to inject the reactant gas / liquid in a direction towards the deposition sections D1-D7. The reactant gas / liquid 111 may be a gas, vapor or liquid medium. In particular, the reactant gas / liquid may be a gas or vapor mixture having a single or mixture of C-, H-, CH- solutions or vapors.
[0051] The nozzle 110 is disposed inside an exhaust column element 112 extending from the bottom 105 of the crucible 102 to at least partially the top 107. The exhaust column element 112 has a rod shape and is fixed to the bottom 105 of the crucible 102. The exhaust column element 112 is, for example, a kind of shower head having a plurality of nozzles 110, each of which is directed to each of the deposition sections D1-D7. Specifically, the exhaust column element 112 extends, for example, along the central axis of the cylindrical shape of the crucible 102. Thus, each of the nozzles 110 is disposed on the exhaust column element 112 from the center of the crucible 102 toward the side wall 106. Furthermore, the upper end of the exhaust column element 112 is spaced apart from the top 107 of the crucible 102. At the upper end of the discharge column element 112 is a nozzle 110 that is directed towards a deposition section D 1 located in the upper portion 107 of the crucible 102 .
[0052] The exhaust column element 112 is coupled to a reactant gas / reactant liquid interface 113 formed in the bottom 105 of the crucible 102. The exhaust column element 112 includes gas lines extending from the bottom 105 of the column 102 to each nozzle 110 disposed in the exhaust column element 112.
[0053] The crucible 102 includes an inlet liquid / inlet gas interface 116 for injecting an inlet liquid / inlet gas 115, the inlet liquid interface 116 being connectable to a pressure regulating valve 114 for regulating the pressure within the internal volume 104. For example, the inlet liquid interface 116 includes a number of openings, for example, located in the top 107 of the crucible 102. The inlet liquid interface 116 is located on an opposite side of the crucible 102 to the reactant liquid interface 113.
[0054] A pressure regulator 120 is connected to the inlet liquid / inlet gas interface 116. The pressure regulator 120 for regulating the pressure within the internal volume and the inlet liquid / inlet gas interface 116 are connected to inject and flow liquids / gases to control, i.e., increase or decrease, the pressure inside the crucible.
[0055] The chamber 102 includes, inter alia, a number of heating elements 119 surrounding the outer wall of the chamber 102 for providing thermal energy to the crucible 102 .
[0056] The apparatus 100 further includes a growth enhancement device 117 for enhancing nucleation of crystals in the deposition sections D1-D7, the growth enhancement device 117 being selected from one of the group consisting of a plasma source, a microwave source, and a laser source.
[0057] At the bottom 105, unused reactant gas / liquid 111 is collected. Therefore, the deposition side D1-D7 is spaced from the bottom 105, and since there are no deposition parts D1-D7 at the bottom 105, the seed crystal 108 is not in contact with the reactant liquid 111 collected at the bottom region of the crucible 102. Therefore, the reactant liquid 111 and the injected liquid 115 already injected into the deposition parts D1-D7 from the nozzle 110 and the liquid interface 116, respectively, react with the raw material 118 and flow down to the bottom 105. The raw material 118 collected at the bottom 105 of the crucible 102 no longer affects the growth of the crystal.
[0058] Figure 2 shows a piece of polycrystal 200 formed in the upper deposition section D1 of the crucible 102 shown in Figure 1. To provide sufficient space for the grown crystal, the exhaust column element 112 may be movable along the central (vertical) axis of the crucible 102 so that the distance from the upper nozzle 110 of the exhaust column element 112 to the proximal point of the grown crystal can be kept constant.
[0059] Figure 3 shows multiple crystals in each lateral deposition section D2-D7 of the crucible 102 shown in Figure 1. As can be seen from Figure 3, multiple crystals can be formed simultaneously using one common crucible 102.
[0060] Figure 4 shows a number of randomly oriented crystals that have developed on the underside of a lateral deposition section (e.g., the underside of deposition sections D2-D7) of the crucible 102 shown in Figure 1. The randomly oriented crystals may be collected and melted to receive injection and reaction liquids again.
[0061] It should be noted that the term "comprising" does not exclude other elements or steps, and "a" or "an" does not exclude a plurality. Also, elements described in association with different embodiments may be combined. It should also be noted that reference signs in the claims shall not be construed as limiting the scope of the claims. According to an aspect (1), there is provided an apparatus (100) for growing crystals, the apparatus (100) comprising: A chamber (101); a crucible (102) disposed in a heatable receiving space (103) of the chamber (101); the crucible (102) having an interior volume (104) configured to grow a crystal therein; The crucible (102) has a bottom (105) with side walls (106) extending to a top (107) of the crucible (102); the crucible (102) comprises at least one deposition section (D1-D7) configured to receive a seed crystal (108); The deposition sections (D1-D7) are formed in at least one of the sidewall (106) and the top (107) of the crucible (102). According to embodiment (2), the bottom part (105) does not include a deposition section (D1-D7) for a seed crystal (108). According to embodiment (3), the crucible (102) extends vertically between the bottom (105) and the top (107). According to aspect (4), the crucible (102) comprises a plurality of deposition sections (D1-D7), each configured to receive a seed crystal (108); The deposition sections (D1-D7) are spaced apart from one another and are formed in at least one of the sidewall (106) and the top (107) of the crucible (102). According to aspect (5), the crucible (102) includes at least one protrusion (109) extending from an inner surface into the interior volume (104); The accumulation sections (D1-D7) are formed in the projection (109). According to aspect (6), the projection (109) extends from the sidewall (106) or the top (107) of the crucible (102) into the interior volume (104). According to aspect (7), the crucible (102) includes a plurality of protrusions (109) extending from the inner surface of the crucible (102) into the interior volume (104); The projections (109) are spaced apart from one another. According to aspect (8), the crucible (102) is provided with at least one nozzle (110), The nozzle (110) is configured to inject a reactant gas / liquid (111) into the interior volume (104) of the crucible (102). According to aspect (9), at least one of the nozzles (110) is configured to discharge a reactant gas / liquid (111) in a direction towards one of the deposition sections (D1-D7). According to aspect (10), the crucible (102) includes a discharge column element (112) extending partially between the bottom (105) and the top (107) of the crucible (102); The discharge pillar element (112) includes at least one of the nozzles (110). According to embodiment (11), the exhaust column element (112) is coupled to a reactant gas / reactant liquid interface (113) formed in the bottom (105) of the crucible (102). According to embodiment (12), the crucible (102) comprises an injection interface (116) for injecting an injection gas / liquid. According to aspect (13), the injection interface (116) is connectable to a pressure regulating valve (120) for regulating pressure within the interior volume (104). According to aspect (14), the chamber (101) includes a plurality of heating elements (119) for providing thermal energy to the crucible (102). According to aspect (15), the plurality of heating elements (119) surround an outer wall of the chamber (101). According to aspect (16), the plurality of heating elements (119) are configured to heat the interior volume (104) to a temperature between 1350°C and 1450°C. According to aspect (17), the plurality of heating elements (119) are selected from one of an RF heater, a resistive heater, and a heat generator. According to aspect (18), the apparatus further includes a thermal insulator (121) disposed in the storage space (103) between the crucible (102) and a wall of the chamber (101). According to an embodiment (19), the crucible (102) is made of a material selected from one of the group including metal-based, oxide-based, nitride-based, carbon-based, and dense graphite. According to aspect (20), the method further comprises a growth enhancement device (117) for enhancing nucleation of crystals in the deposition section, The growth enhancement device (117) is selected from one of the group consisting of a plasma source, a microwave source, and a laser source. According to an aspect (21), a method for growing a crystal is provided, the method comprising the steps of attaching a seed crystal (108) to a deposition section (D1-D7) of a crucible (102), the deposition section (D1-D7) being formed in at least one of a sidewall (106) and a top (107) of the crucible (102); , and growing a crystal within an internal volume (104) of the crucible (102) disposed in a heatable accommodation space (103) of a chamber (101). According to an aspect (22), the method further includes providing a source material (118) in the crucible (102) comprising one of a reaction fluid and an injection fluid, the source material (118) being selected from the group consisting of a solid phase material, a liquid phase material, a gas phase material, and a mixed phase material including C-, H-, and CH- solutions. According to aspect (23), the reaction fluid is a liquid (111) and the injection fluid is a liquid (116). [Explanation of symbols]
[0062] 100 devices 101 Chamber 102 Crucible 103 Containment Space 104 Internal volume 105 Bottom 106 Side wall 107 Top 108 Seed Crystal 109 Protrusion 110 Nozzle 111 Reactive gas / liquid 112 Discharge column element 113 Reactive Liquid Interface 114 Control valve 115 Injection gas / injection liquid 116 Injection Interface 117 Growth power enhancement device 118 Raw materials 119 Heating element 120 Pressure Regulating Valve 121 Insulation 200 Piece of polycrystal 300 Polycrystalline 400 Unoriented Crystals D1-D7 Sedimentation Section
Claims
1. An apparatus (100) for growing crystals, said apparatus (100) comprising: A chamber (101); a crucible (102) disposed in a heatable accommodation space (103) of the chamber (101); The crucible (102) comprises an interior volume (104) configured to grow a crystal therein; The crucible (102) has a bottom (105) with side walls (106) extending to a top (107) of the crucible (102); the crucible (102) comprises a plurality of deposition sections (D2-D7), each of the plurality of deposition sections (D2-D7) being configured to receive a seed crystal (108); Each of the deposition sections (D2-D7) is formed in the side wall (106) or the top (107) of the crucible (102); the crucible (102) includes a plurality of projections (109) extending from an inner surface into the interior volume (104); said accumulation sections (D2-D7) are formed in said projection (109); The device (100), wherein the projections (109) are spaced apart from one another.
2. The apparatus (100) of claim 1, wherein the bottom (105) does not include the deposition section (D2-D7) for the seed crystal (108).
3. 3. The apparatus (100) of claim 1 or claim 2, wherein the crucible (102) extends along a vertical direction between the bottom (105) and the top (107).
4. An apparatus (100) described in any one of claims 1 to 3, wherein the deposition sections (D2-D7) are arranged spaced apart from each other and formed on at least one of the side wall (106) and the top (107) of the crucible (102).
5. the projection (109) extends from the sidewall (106) or the top (107) of the crucible (102) into the interior volume (104); 2. The apparatus (100) of claim 1, wherein an additional protrusion (109) extends from the top (107) of the crucible (102) into the interior volume (104), the additional protrusion (109) forming an additional deposition section (D1) and configured to mount an additional seed crystal (108).
6. The crucible (102) is provided with at least one nozzle (110); The apparatus (100) of any one of claims 1 to 5, wherein the nozzle (110) is configured to inject a reactant gas / liquid (111) into the internal volume (104) of the crucible (102).
7. The apparatus (100) of claim 6, wherein at least one of the nozzles (110) is configured to discharge a reactant gas / liquid (111) in a direction towards one of the deposition sections (D2-D7).
8. the crucible (102) includes a discharge column element (112) extending partially between the bottom (105) and the top (107) of the crucible (102); The apparatus (100) of claim 6 or claim 7, wherein the exhaust column element (112) comprises at least one of the nozzles (110).
9. 9. The apparatus (100) of claim 8, wherein the exhaust column element (112) is coupled to a reactant gas / reactant liquid interface (113) formed in the bottom (105) of the crucible (102).
10. The apparatus (100) of any one of claims 1 to 9, wherein the crucible (102) comprises an injection interface (116) for injecting an injection gas / liquid.
11. 11. The apparatus (100) of claim 10, wherein the injection interface (116) is connectable to a pressure regulating valve (120) for regulating pressure within the internal volume (104).
12. The apparatus (100) of any one of claims 1 to 11, wherein the chamber (101) comprises a plurality of heating elements (119) for providing thermal energy to the crucible (102).
13. The apparatus (100) of claim 12, wherein the plurality of heating elements (119) surround an outer wall of the chamber (101).
14. The apparatus (100) of claim 12 or claim 13, wherein the plurality of heating elements (119) are configured to heat the interior volume (104) to a temperature between 1350°C and 1450°C.
15. The apparatus (100) of any one of claims 12 to 14, wherein the plurality of heating elements (119) are selected from one of an RF heater, a resistive heater, and a heat generator.
16. 16. The apparatus (100) of any one of claims 1 to 15, further comprising a thermal insulation material (121) disposed in the containing space (103) between the crucible (102) and a wall of the chamber (101).
17. 17. The apparatus (100) of any one of claims 1 to 16, wherein the crucible (102) is made of a material selected from one of the group consisting of metal-based, oxide-based, nitride-based, carbon-based and dense graphite.
18. a growth enhancement device (117) for enhancing nucleation of crystals in the deposition section; 18. The apparatus (100) of any one of claims 1 to 17, wherein the growth enhancement device (117) is selected from one of the group consisting of a plasma source, a microwave source, and a laser source.
19. 13. A method for growing crystals using the apparatus of claim 1, the method comprising: attaching a seed crystal (108) to the deposition section (D2-D7) of the crucible (102), the deposition section (D2-D7) being formed on at least one of the sidewall (106) and the top (107) of the crucible (102); growing a crystal within the internal volume (104) of the crucible (102) disposed in a heatable containment space (103) of the chamber (101); A method comprising:
20. 20. The method of claim 19, further comprising providing a source (118) of one of a reaction fluid and an injection fluid in the crucible (102), the source (118) being selected from one of the group consisting of a solid phase material, a liquid phase material, a gas phase material, and a mixed phase material including C-, H-, and CH- solutions.
21. 21. The method of claim 20, wherein the reactant fluid is a liquid (111) and the injector fluid is a liquid (116).
Citation Information
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