Slag pulling device used in germanium single crystal production process
By designing a slag extra device for single crystal production, the solid floating residue is directly removed, which solves the problem of excessive time and poor single crystal quality in the traditional slag extraction process, and achieve efficient single crystal preparation.
Patent Information
- Application Number
- CN202411740056.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-29
- Publication Date
- 2025-01-28
AI Technical Summary
During the production process of germanium single crystal, the presence of liquid surface slag impurities leads to an increase in dislocation of the single crystal, affecting the quality of the single crystal. The traditional slag extraction process takes too long, affecting the preparation efficiency.
Design a slag extra device for single crystal production, including seed crystal, seed crystal chip, and slag plug blocks. Through the adhesion of the slag block, the liquid surface is directly removed. Shoulder growth steps.
Effectively shortened the time of the single crystal preparation, significantly improved the efficiency of single crystal preparation, and avoided the quality problem of single crystal quality caused by the traditional slag extraction process.
Smart Images
Figure CN119372765A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of germanium single crystal production, and in particular to a slag removal device used in the production process of germanium single crystal. Background Art
[0002] When using zone melting germanium and blank cuttings as raw materials to pull germanium single crystals, some impurities contained in the raw materials, oxide films on the surface of the raw materials, and oxides produced by the reaction of the raw materials with residual oxygen in the single crystal furnace during heating and melting will float on the surface of the molten germanium melt. The floating objects have a higher melting point than germanium and are insoluble in germanium. They emit a large amount of heat to the outside. When floating on the surface of the melt over a large area, they affect the uniformity of the melt surface temperature and adhere to the solid-liquid interface of the single crystal growth, which can easily cause the single crystal dislocation to increase and cause the single crystal to metamorphose. Therefore, before pulling germanium single crystals, it is necessary to remove the floating slag impurities on the liquid surface.
[0003] The slag removal process starts with constant temperature, seeding, and shouldering to grow a crystal block, and then the slag is lifted and lowered by the principle of condensation of slag when it encounters cold to remove impurities. During the crystal growth process, constant temperature ensures that the raw materials can be kept in a stable temperature range after melting, which is conducive to obtaining a uniform superheated melt. Seeding is the initial step of crystal growth, which involves introducing a tiny crystal seed (or crystal nucleus) under appropriate conditions. The purpose of seeding is to start the crystal growth process and ensure that the crystal can grow in a predetermined direction and morphology. After seeding, the crystal begins to enter the shouldering growth stage. This stage is characterized by the rapid expansion of the crystal in a direction perpendicular to the growth axis to form a larger crystal block.
[0004] However, the above-mentioned slag removal process needs to go through the steps of constant temperature, seeding, and shoulder release to grow a crystal block, which results in a long time consumption and affects the preparation of germanium single crystals. Summary of the invention
[0005] In order to solve or partially solve the problems existing in the related art, the present application provides a slag removal device for use in the production process of germanium single crystals.
[0006] To achieve the above objectives, this application is implemented through the following technical solutions:
[0007] A slag removal device for use in a germanium single crystal production process, the slag removal device for use in a germanium single crystal production process comprising:
[0008] Seed crystal;
[0009] A seed crystal chuck connected to one end of the seed crystal, wherein a screw hole is provided at the end of the seed crystal chuck away from the seed crystal;
[0010] The slag block connected to the other end of the seed crystal through the seed crystal pin is used to attach slag impurities.
[0011] Optionally, a conical necking transition is adopted at the connection between the seed crystal and the seed crystal chuck.
[0012] Optionally, the slag remover block is a hemispherical structure with a circular arc at the bottom.
[0013] Optionally, a connecting tube is provided on the upper end surface of the slag puller block, and a pin hole is provided on the connecting tube for allowing a seed crystal pin to pass through, and the distance between the pin hole and the upper end surface of the slag puller block is not less than 5 mm.
[0014] Optionally, the seed crystal and the seed crystal pin are made of tungsten steel, tungsten, molybdenum, tantalum, osmium or iridium.
[0015] Optionally, the seed crystal chuck is made of graphite, carbon-carbon composite material, tungsten steel or molybdenum material.
[0016] Optionally, the slag stripping block is made of tungsten, molybdenum, tantalum, osmium or iridium.
[0017] The beneficial effects of the present application are as follows: the present application removes the slag on the liquid surface through the adhesion of the slag pulling block, omits the time-consuming steps of traditional constant temperature, crystal induction, and shoulder growth of crystal blocks, and directly uses the slag pulling device to perform efficient slag pulling in the initial stage of pulling, effectively shortening the time and thus avoiding affecting the preparation of germanium single crystals.
[0018] It should be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the present application. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The above and other objects, features and advantages of the present application will become more apparent through a more detailed description of exemplary embodiments of the present application in conjunction with the accompanying drawings, wherein the same reference numerals generally represent the same components in the exemplary embodiments of the present application.
[0020] Figure 1 It is a schematic diagram of the structure of a slag removal device used in the production process of germanium single crystals shown in an embodiment of the present application.
[0021] Reference numerals: 1 seed crystal, 2 seed crystal chuck, 3 screw hole, 4 seed crystal pin, 5 slag puller block, 6 connecting tube. DETAILED DESCRIPTION
[0022] In the description of the present invention, it is to be understood that the terms “center”, “longitudinal”, “lateral”, “length”, “width”, “thickness”, “up”, “down”, “front”, “back”, “left”, “right”, “vertical”, “horizontal”, “top”, “bottom”, “inside”, “outside”, “clockwise”, “counterclockwise”, “axial”, “radial”, “circumferential”, etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.
[0023] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In the description of the present invention, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.
[0024] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral one; it can be a mechanical connection, an electrical connection, or communication with each other; it can be a direct connection, or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to the specific situation.
[0025] In the present invention, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediate medium. Moreover, a first feature being "above", "above" or "above" a second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is higher in level than the second feature. A first feature being "below", "below" or "below" a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.
[0026] In the present invention, the terms "one embodiment", "some embodiments", "examples", "specific examples" or "some examples" etc. mean that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, unless they are contradictory.
[0027] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and vary the above embodiments within the scope of the present invention.
[0028] The above description is only an optional embodiment of the present application and is not intended to limit the present application. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.
[0029] In order to make the purpose, technical solutions and beneficial effects of the present application clearer, the preferred embodiments of the present application will be described in detail below in conjunction with the accompanying drawings to facilitate understanding by technical personnel.
[0030] Embodiment 1:
[0031] See also Figure 1 , a slag removal device for use in a germanium single crystal production process, the slag removal device for use in a germanium single crystal production process comprising:
[0032] Seed crystal 1;
[0033] A seed crystal chuck 2 connected to one end of the seed crystal 1, wherein a screw hole 3 is formed at one end of the seed crystal chuck 2 away from the seed crystal 1;
[0034] The slag removal block 5 connected to the other end of the seed crystal 1 through the seed crystal plug 4 is used to attach slag impurities.
[0035] Specifically, the seed crystal 1 is cylindrical, one end of which is connected to the seed crystal chuck 2, and the other end is provided with a through hole allowing the seed crystal plug 4 to pass through. After the seed crystal 1 is connected to the slag extraction block 5, the seed crystal plug 4 is inserted into the through hole to fix the seed crystal 1 and the slag extraction block 5, and limit blocks are provided at both ends of the seed crystal plug 4. A screw hole 3 is provided at one end of the seed crystal chuck 2 away from the seed crystal 1, and is threadedly connected to the weight of the single crystal furnace through the screw hole 3, so that the slag extraction device can be detachably installed in the single crystal furnace equipment.
[0036] When in use, the device is installed at the weight inside the single crystal furnace. After the gas replacement process and the temperature rise and material processing process, the slag gathers in the center of the liquid surface. The control system controls the length of the seed crystal rope of the single crystal furnace, and indirectly controls the lifting and lowering of the weight and the slag removal structure, so that the lower part of the slag removal block 5 is immersed in the melt for 1-10 seconds, and then the slag removal block 5 is raised to 50-300mm above the liquid surface, cooled for 1-10 minutes, and the above operation is repeated until the slag on the liquid surface is cleared. By detachably installing the slag removal device in the single crystal furnace equipment, it is convenient to replace the device with ordinary seed crystals after the slag removal is completed.
[0037] In this embodiment, the slag on the liquid surface is cleaned by the adhesion of the slag removal block 5, and the traditional time-consuming steps of constant temperature, crystal induction, and shoulder growth of the crystal block are omitted. The slag removal device is directly used to perform efficient slag removal in the initial stage of pulling, which effectively shortens the time and avoids affecting the preparation of the germanium single crystal.
[0038] Actual application effect: Before using this device, the traditional steps of constant temperature, seeding, and shouldering to grow crystal blocks take 4 to 5 hours. After using this device to remove slag and impurities, the whole process time is shortened to about 2 hours, significantly improving the efficiency of single crystal preparation.
[0039] Embodiment 2:
[0040] See also Figure 1 Based on the first embodiment, optionally, a conical necking transition is adopted at the connection between the seed crystal 1 and the seed crystal chuck 2 .
[0041] Specifically, the conical necking design makes the connection part tighter and increases the stability of the connection. Through the conical necking process, the bearing capacity of a specific part can be increased while maintaining the overall strength of the material, ensuring that the seed crystal 1 has sufficient bearing capacity and ensuring that the structure remains stable when subjected to external forces.
[0042] Optionally, the slag stripping block 5 is a hemispherical structure with a circular arc at the bottom.
[0043] Specifically, the bottom of the slag stripping block 5 adopts a semi-spherical structure with an arc-shaped design, which is conducive to the attachment of slag impurities to the slag stripping block 5.
[0044] Optionally, a connecting tube 6 is provided on the upper end surface of the slag stripping block 5 , and a pin hole is provided on the connecting tube 6 for allowing the seed crystal pin 4 to pass through, and the distance between the pin hole and the upper end surface of the slag stripping block 5 is not less than 5 mm.
[0045] Specifically, the lower end of the connecting tube 6 is fixedly connected to the upper end surface of the slag stripping block 5, and the pin hole provided on the connecting tube 6 corresponds to the through hole provided on the seed crystal 1, so that the seed crystal pin 4 can be inserted therethrough to connect the connecting tube 6 and the seed crystal 1.
[0046] The distance between the pin hole and the upper end surface of the slag stripping block 5 is not less than 5 mm to prevent the liquid level from overflowing the slag stripping block 5 and pouring into the connection, making it impossible to remove the seed crystal 1 and the slag stripping block 5.
[0047] Optionally, the seed crystal 1 and the seed crystal pin 4 are made of tungsten steel, tungsten, molybdenum, tantalum, osmium or iridium.
[0048] Specifically, tungsten steel, tungsten, molybdenum, tantalum, osmium or iridium materials have good thermal stability and chemical inertness, and their melting points are higher than those of germanium, which can prevent the materials from dissolving and sticking together in a high-temperature environment. At the same time, after being immersed in the germanium melt, the above materials will not introduce new impurities that affect a series of parameters such as the conductivity type, resistivity, and carrier concentration of the germanium single crystal.
[0049] Optionally, the seed crystal chuck 2 is made of graphite, carbon-carbon composite material, tungsten steel or molybdenum material.
[0050] Specifically, graphite, carbon-carbon composite materials, tungsten steel or molybdenum materials all have a high melting point, good thermal conductivity, certain hardness and strength, and are suitable for use in single crystal furnaces.
[0051] Optionally, the slag stripping block 5 is made of tungsten, molybdenum, tantalum, osmium or iridium.
[0052] Specifically, the melting points of tungsten, molybdenum, tantalum, osmium or iridium materials are higher than that of germanium, which can prevent the materials from dissolving and sticking together in a high temperature environment. At the same time, the above materials can be immersed in the germanium solution without introducing new impurities that affect a series of parameters such as the conductivity type, resistivity, and carrier concentration of the germanium single crystal. The materials are optional and can allow the germanium solution to adhere to them.
[0053] In addition, in the traditional technology, the output slag needs to be returned to the germanium tetrachloride section for chlorination combustion and then go through the entire zone melting germanium metal preparation process before it can be put into the single crystal furnace again for single crystal pulling. There are problems such as high slag processing costs and long processing processes; in the slag pulling process, the crystal block needs to be broken by external force, which may cause the seed crystal to tilt, increase the seed crystal stress, destroy the seed crystal orientation, and cause the problem of failure to crystallize during formal crystal pulling. After using this device, the generation of slag is reduced, the subsequent processing cost is directly reduced, and the recovery rate of the germanium single crystal section is increased by 0.5%, including the recovery of slag, chlorination combustion and re-preparation process, while improving the recovery rate of germanium single crystals. The use of this device can also avoid the operation of breaking the crystal block by force, fundamentally eliminating the problems of increased stress in the seed crystal, increased dislocation and crystal orientation shift caused by knocking, ensuring the stability of the seed crystal and the crystallization rate of the pulled crystal.
[0054] It should be noted that structures and / or installation methods not described in detail in this application are known to those skilled in the art in combination with common knowledge and / or prior art, and are not the focus of disclosure in this application and will not be further elaborated herein.
[0055] Finally, it should be noted that the above preferred embodiments are only used to illustrate the technical solution of the present application rather than to limit it. Although the present application has been described in detail through the above preferred embodiments, those skilled in the art should understand that various changes can be made in form and details without departing from the scope defined by the claims of the present application; the dimensions of the drawings are not related to the specific objects, and the dimensions of the objects can be changed arbitrarily.
Claims
1. A slag removal device used in the production process of germanium single crystals, characterized in that: The slag removal device used in the production process of germanium single crystals comprises: Seed crystal (1); A seed crystal chuck (2) connected to one end of the seed crystal (1), wherein a screw hole (3) is provided at one end of the seed crystal chuck (2) away from the seed crystal (1); A slag removal block (5) connected to the other end of the seed crystal (1) via a seed crystal plug (4) is used to attach slag impurities.
2. The slag removal device for use in the production process of germanium single crystals according to claim 1, characterized in that: The connection between the seed crystal (1) and the seed crystal chuck (2) adopts a conical necking transition.
3. The slag removal device for germanium single crystal production process according to claim 1, characterized in that: The slag removing block (5) is a hemispherical structure with a circular arc at the bottom.
4. The slag removal device for use in the production process of germanium single crystals according to claim 1 or 3, characterized in that: The upper end surface of the slag stripping block (5) is provided with a connecting tube (6), and the connecting tube (6) is provided with a pin hole for allowing the seed crystal pin (4) to pass through, and the distance between the pin hole and the upper end surface of the slag stripping block (5) is not less than 5 mm.
5. The slag removal device for use in the production process of germanium single crystals according to claim 1, characterized in that: The seed crystal (1) and the seed crystal pin (4) are made of tungsten steel, tungsten, molybdenum, tantalum, osmium or iridium.
6. The slag removal device for use in the production process of germanium single crystals according to claim 1, characterized in that: The seed crystal chuck (2) is made of graphite, carbon-carbon composite material, tungsten steel or molybdenum material.
7. The slag removal device for use in the production process of germanium single crystals according to claim 4, characterized in that: The slag stripping block (5) is made of tungsten, molybdenum, tantalum, osmium or iridium.