Furnace tube and method of making and processing equipment therefor
By setting a protective layer on the inner wall of the quartz tube, including a heat-resistant alloy and a metal oxide layer, the problem of quartz furnace tubes being easily corroded by polycrystalline silicon is solved, extending their lifespan and reducing replacement frequency and cost.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JIAGENG (JIANGSU) SPECIAL MATERIALS CO LTD
- Filing Date
- 2024-12-06
- Publication Date
- 2026-06-09
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Figure CN122169051A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of photovoltaic technology, and more specifically, to furnace tubes and their preparation methods and processing equipment. Background Technology
[0002] Chemical vapor deposition (CVD) is typically performed in a high-temperature and vacuum environment. Specifically, within a vacuum furnace, various chemical reactions generate a corresponding vapor material, which is then deposited onto the surface of an object to form a film. During this process, the vapor material deposits on the inner wall of the vacuum furnace tube (usually a quartz tube). Over prolonged contact, this gradually erodes the furnace tube, eventually causing damage. Summary of the Invention
[0003] The first aspect of this application provides a furnace tube. The furnace tube includes a quartz tube, an adhesive layer, and a protective layer. The protective layer includes a stacked heat-resistant alloy layer and a metal oxide layer. The heat-resistant alloy layer is bonded to the inner wall of the quartz tube through the adhesive layer, and the metal oxide layer is located on the surface of the heat-resistant alloy layer opposite to the quartz tube.
[0004] This furnace tube utilizes a protective layer on its inner wall to prevent corrosion from deposits (such as polycrystalline silicon) generated during the chemical vapor deposition process, thus protecting the quartz tube and extending its lifespan. Specifically, the heat-resistant alloy layer provides mechanical strength and stability at high temperatures, while the metal oxide layer further enhances the protective effect, preventing oxidation or corrosion of the heat-resistant alloy layer and extending the furnace tube's service life.
[0005] In some embodiments, the heat-resistant alloy layer is made of any one of nickel-based alloys, molybdenum alloys, and tungsten alloys.
[0006] In some embodiments, the adhesive layer is made of any one of phosphate adhesives, silicate adhesives, and ceramic adhesives.
[0007] In some embodiments, the protective layer is provided with a plurality of through holes spaced apart.
[0008] In some embodiments, the size of each through hole ranges from 2 mm to 8 mm; and / or the distance between adjacent through holes ranges from 30 mm to 150 mm.
[0009] In some embodiments, the thickness of the protective layer ranges from 20 μm to 100 μm.
[0010] A second aspect of this application provides a processing apparatus. This processing apparatus includes the furnace tube described in the first aspect of this application.
[0011] A third aspect of this application provides a method for preparing a furnace tube. The method includes: attaching a heat-resistant alloy layer to the inner wall of a quartz tube using an adhesive to obtain a composite tube; and subjecting the composite tube to heat treatment, causing the adhesive to cure and bond the heat-resistant alloy layer and the inner wall of the quartz tube, and causing the surface of the heat-resistant alloy layer facing away from the quartz tube to be oxidized to form a metal oxide layer.
[0012] In some embodiments, the heat-resistant alloy layer includes an adhesive surface for bonding with the quartz tube. Before attaching the heat-resistant alloy layer to the inner wall of the quartz tube using the adhesive, the method for preparing the furnace tube further includes: roughening the adhesive surface, and / or roughening the inner wall of the quartz tube.
[0013] In some embodiments, the bonding surface is roughened by rubbing it with sandpaper. The inner wall of the quartz tube is roughened by sandblasting.
[0014] In some embodiments, before attaching the heat-resistant alloy layer to the inner wall of the quartz tube using the adhesive, the method for preparing the furnace tube further includes: forming a plurality of spaced through holes on the heat-resistant alloy layer; attaching the heat-resistant alloy layer to the inner wall of the quartz tube using the adhesive includes: discharging air and / or excess adhesive between the heat-resistant alloy layer and the inner wall of the quartz tube through the through holes and the edge of the heat-resistant alloy layer.
[0015] In some embodiments, an inspection step is included before heat treatment of the composite tube. The inspection step includes allowing the composite tube to stand for a preset time, and then checking whether the composite tube has quality defects such as delamination, separation, and / or bulging. If the composite tube has such quality defects, the composite tube is then re-adhesiveted and compacted, and the inspection step is repeated until the composite tube is free of such quality defects.
[0016] In some embodiments, the composite tube is subjected to heat treatment, including: placing the composite tube in a high-temperature furnace, raising the temperature in the high-temperature furnace from room temperature to 120°C to 180°C over 10 to 30 minutes, and holding the temperature for 1 to 3 hours; then raising the temperature in the high-temperature furnace to 550°C to 600°C over 50 to 80 minutes, and holding the temperature for 1 to 3 hours; then raising the temperature in the high-temperature furnace to 750°C to 830°C, and holding the temperature for 1 to 3 hours; and then cooling the temperature in the high-temperature furnace to room temperature. Attached Figure Description
[0017] Figure 1 This is a schematic diagram of the structure of a furnace tube according to an embodiment of this application.
[0018] Figure 2 for Figure 1 Scanning electron microscope image of the protective layer of the furnace tube.
[0019] Figure 3 for Figure 1 Another scanning electron microscope image of the protective layer of the furnace tube.
[0020] Figure 4 for Figure 1 Another scanning electron microscope image of the protective layer of the furnace tube.
[0021] Figure 5 for Figure 1 Scanning electron microscope image of the interface between the protective layer and the adhesive layer of the furnace tube.
[0022] Figure 6 for Figure 1 A plan view of the protective layer of the furnace tube.
[0023] Explanation of key component symbols: The following detailed description, in conjunction with the accompanying drawings, will further illustrate this application. Detailed Implementation
[0024] The embodiments of this application are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the embodiments of this application, and should not be construed as limiting this application.
[0025] In the description of the embodiments of this application, the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the implementation methods of this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this application.
[0026] In the description of the embodiments of this application, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Therefore, features defined with "first" and "second" may explicitly or implicitly include one or more of the stated features.
[0027] In the description of the embodiments of this application, unless otherwise stated, "a plurality of" means two or more.
[0028] In the description of the embodiments of this application, unless otherwise stated, the terms "installation", "connection" and "linking" should be interpreted broadly. For example, they can be fixed connections, detachable connections, or integral connections; they can be mechanical connections, electrical connections, or connections that can communicate with each other; they can be direct connections or indirect connections through an intermediate medium; they can be internal connections between two components or interactive relationships between two components.
[0029] Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.
[0030] In related technologies, when quartz furnace tubes are used in polycrystalline silicon thin film deposition processes, their lifespan ranges from 60 to 90 days. The core mechanism of quartz furnace tube failure is the erosion of the inner wall of the quartz tube by polycrystalline silicon. As the degree of erosion increases, the strength of the quartz tube continuously decreases, eventually leading to breakage under the influence of external forces such as vacuum, thermal shock, and its own gravity. Therefore, quartz tubes in related technologies have short lifespans, high losses, high costs, and require frequent replacements, each taking 2-3 days, impacting production capacity. Furthermore, quartz tube breakage can cause damage to related equipment and the products themselves.
[0031] In response, this application provides a furnace tube. This furnace tube, by providing a protective layer on the inner wall of a quartz tube, prevents the quartz tube from being eroded by deposits (such as polycrystalline silicon) during the chemical vapor deposition process, thereby protecting the quartz tube and extending its lifespan.
[0032] Figure 1 This is a schematic diagram of a furnace tube according to an embodiment of this application. This furnace tube can be applied in chemical vapor deposition processes, and more specifically, in low-pressure chemical vapor deposition of polycrystalline silicon thin films. Figure 1 As shown, the furnace tube 100 includes a quartz tube 10, an adhesive layer 20, and a protective layer 30. The quartz tube 10 includes an inner wall W1 and an outer wall W2. The protective layer 30 is bonded to the inner wall W1 of the quartz tube 10 via the adhesive layer 20. The adhesive layer 20 is located between the inner wall W1 of the quartz tube 10 and the protective layer 30.
[0033] In some embodiments, the adhesive layer 20 is made of any one of phosphate adhesives, silicate adhesives, and ceramic adhesives. Thus, the adhesive layer 20 uses a high-temperature resistant adhesive material, ensuring that the adhesive layer 20 will not decompose or fail under high-temperature conditions, maintaining a strong bond between the protective layer 30 and the quartz tube 10, and improving the overall structural stability of the furnace tube 100.
[0034] Figure 2 for Figure 1 Scanning electron microscope image of the protective layer of the furnace tube. Figure 3 for Figure 1 Another scanning electron microscope image of the protective layer of the furnace tube. (See image below.) Figure 2 and Figure 3 As shown, the protective layer 30 includes a stacked heat-resistant alloy layer 31 and a metal oxide layer 32. The side of the protective layer 30 containing the heat-resistant alloy layer 31 is used for bonding to the quartz tube 10 via the adhesive layer 20. In the furnace tube 100, the metal oxide layer 32 is located on the surface of the heat-resistant alloy layer 31 facing away from the quartz tube 10.
[0035] In some embodiments, the heat-resistant alloy layer 31 is made of any one of nickel-based alloys, molybdenum alloys, and tungsten alloys. Therefore, selecting high-temperature alloy materials such as nickel-based, molybdenum, or tungsten alloys for the heat-resistant alloy layer 31 can significantly improve its high-temperature resistance and corrosion resistance, ensuring that the furnace tube 100 maintains stable physical and chemical properties even under extreme temperatures.
[0036] Specifically, when the material of the heat-resistant alloy layer 31 is a nickel-based alloy, the material of the metal oxide layer 32 may include nickel oxide; when the material of the heat-resistant alloy layer 31 is a nickel-chromium-based alloy, the material of the metal oxide layer 32 may include nickel oxide and / or chromium oxide.
[0037] In some embodiments, the thickness of the protective layer 30 ranges from 20 μm to 100 μm (e.g., 20 μm to 30 μm, 30 μm to 40 μm, 4 μm to 50 μm, 50 μm to 60 μm, 60 μm to 70 μm, 70 μm to 80 μm, 80 μm to 90 μm, 90 μm to 100 μm, etc.).
[0038] Specifically, an excessively thick protective layer 30 may lead to thermal stress concentration, especially under conditions of significant temperature variations. This could cause the protective layer 30 to crack or peel off, affecting its protective effect. Furthermore, an excessively thick protective layer 30 will reduce heat transfer efficiency, resulting in uneven temperatures inside and outside the furnace tube 100, affecting the stability and uniformity of the chemical vapor deposition process. Moreover, an excessively thick protective layer 30 requires more material, which increases manufacturing costs and resource consumption.
[0039] Furthermore, an excessively thin protective layer 30 may not provide sufficient protection and is easily penetrated by high temperatures, oxidizing agents, and corrosive gases, leading to damage to the quartz tube 10. Moreover, an excessively thin protective layer 30 has low mechanical strength and is prone to cracking or wear under mechanical stress. It is also difficult to adhere to the inner wall of the quartz tube 10 or it may deform or fall off the wall W1 of the quartz tube 10, affecting its protective effect.
[0040] Therefore, the thickness of the protective layer 30 is in the range of 20μm to 100μm, which can provide sufficient protection without being too thick and causing a decrease in heat conduction efficiency or an increase in cost. This helps to ensure its stability and reliability in complex environments such as high temperature, oxidation and mechanical stress.
[0041] In one specific embodiment, such as Figure 2 As shown, the thickness of the heat-resistant alloy layer 31 ranges from 60 μm to 65 μm. Figure 3 As shown, the thickness of the metal oxide layer 32 ranges from 7 μm to 8 μm.
[0042] Figure 4 for Figure 1 Another scanning electron microscope image of the protective layer of the furnace tube. (See image below.) Figure 4 As shown, the metal oxide layer 32 has a dendritic texture structure.
[0043] Specifically, the dendritic textured metal oxide layer 32 can significantly improve the oxidation resistance of the heat-resistant alloy layer 31. As a protective layer, the metal oxide layer 32 can effectively block oxygen and other corrosive gases from directly contacting the heat-resistant alloy layer 31, thereby slowing down the oxidation and corrosion rate of the heat-resistant alloy layer 31.
[0044] In addition, the dendritic texture structure increases the specific surface area of the surface, which helps to improve the stability and durability of the metal oxide layer 32. Moreover, the larger surface area can more effectively disperse stress and reduce the formation and propagation of cracks in the quartz tube 10.
[0045] Furthermore, when the furnace tube 100 is used in a chemical vapor deposition apparatus, the dendritic textured surface structure of the metal oxide layer 32 helps to promote the uniform deposition of reactants on the protective layer 30 during the chemical vapor deposition process.
[0046] Furthermore, the dendritic textured metal oxide layer 32 can improve the thermal shock resistance of the heat-resistant alloy layer 31. In environments with rapid temperature changes, the dendritic structure can effectively alleviate thermal stress and reduce thermal fatigue and crack formation.
[0047] Figure 5 for Figure 1 Scanning electron microscope (SEM) image of the interface between the protective layer and the adhesive layer of the furnace tube. (See image for reference.) Figure 5 As shown, the adhesive layer 20 comprises multiple granular structures of uniform size and shape. The interface between the protective layer 30 and the adhesive layer 20 has an uneven texture to ensure a tight bond with the adhesive layer 20.
[0048] Figure 6 for Figure 1 A plan view of the protective layer of the furnace tubes. (See attached image.) Figure 6As shown, the protective layer 30 has multiple through holes H spaced apart. These through holes H are used to expel air and / or excess adhesive between the inner wall W1 of the quartz tube 10 and the protective layer 30 during the process of attaching the protective layer 30 to the inner wall W1 of the quartz tube 10, preventing the protective layer 30 from bulging, cracking, or detaching, thus enhancing the reliability and safety of the furnace tube 100. Furthermore, the multiple through holes H also facilitate the discontinuity of the film layer formed during chemical vapor deposition, reducing stress transmission.
[0049] In some embodiments, the size of each through-hole H ranges from 2mm to 8mm (e.g., 2mm to 3mm, 3mm to 5mm, 5mm to 6mm, 6mm to 8mm, etc.). In this embodiment, the multiple through-holes H are equally spaced circular holes of equal size. The size of the through-hole H refers to its diameter. In other embodiments, the size of the through-hole H refers to the size at its smallest position. In other embodiments, the shape, size, and arrangement of the through-holes H are not limited.
[0050] Specifically, if the size of the through-hole H is too small, the following problems may occur: First, poor venting: Too small a through-hole may not effectively expel air and excess adhesive, leading to air bubble residue and affecting the adhesion and overall performance of the protective layer. Second, risk of clogging: Small through-holes are more easily clogged by adhesive or other tiny particles, further reducing venting efficiency. Third, increased manufacturing difficulty: Manufacturing very small through-holes in the protective layer may require more precise processing techniques, increasing manufacturing difficulty and cost.
[0051] Furthermore, if the size of the through-hole H is too large, the following problems may arise: First, structural integrity may be compromised: an excessively large through-hole weakens the structural integrity of the protective layer, reducing its mechanical strength and durability. Second, thermal stress concentration may occur: a large through-hole may lead to thermal stress concentration, increasing the risk of the protective layer cracking or peeling off in high-temperature environments. Third, the protective effect may be weakened: an excessively large through-hole reduces the effective area of the protective layer, decreasing its protective effect on the quartz tube, especially in high-temperature and corrosive environments.
[0052] In summary, the through-hole H size ranges from 2mm to 8mm, which can effectively expel air and excess adhesive, ensuring good adhesion between the protective layer 30 and the quartz tube 10, while maintaining the structural integrity and mechanical strength of the protective layer 30.
[0053] In some embodiments, the distance between adjacent through holes ranges from 30 mm to 150 mm (e.g., 30 mm to 50 mm, 50 mm to 70 mm, 70 mm to 100 mm, 100 mm to 150 mm, etc.).
[0054] Specifically, if the via spacing H is too close, the following problems may arise: First, an excessively close via spacing will weaken the structural integrity of the protective layer, reducing its mechanical strength and durability. Second, a dense via layout may lead to thermal stress concentration, increasing the risk of the protective layer cracking or peeling off under high-temperature conditions. Third, an overly dense via layout may increase manufacturing complexity and cost, as more precise processing techniques are required to ensure the uniform distribution of vias.
[0055] Furthermore, if the distance between the through holes (H) is too great, the following problems may arise: First, an excessively large through hole spacing may prevent the effective expulsion of air and excess adhesive between the inner wall of the quartz tube and the protective layer, leading to air bubble residue and affecting the adhesion and overall performance of the protective layer. Second, a large through hole spacing may cause adhesive to accumulate in localized areas, preventing uniform distribution and thus affecting the adhesion quality of the protective layer. Third, an excessively large through hole spacing may result in uneven thermal stress distribution, increasing the risk of thermal stress concentration in localized areas.
[0056] In summary, the through-hole H distance ranges from 30mm to 150mm, which can effectively expel air and excess adhesive, ensuring good adhesion between the protective layer and the quartz tube, while maintaining the structural integrity and mechanical strength of the protective layer.
[0057] This application also provides a processing apparatus. This processing apparatus includes the furnace tube of any of the above embodiments of this application. For example, this processing apparatus is a chemical vapor deposition apparatus.
[0058] This application also provides a method for preparing a furnace tube. The method includes steps S10 to S20 as described below. This method can be used to prepare furnace tubes according to any of the above embodiments.
[0059] Depending on different needs, the order of some steps or sub-steps in the preparation method of the furnace tube can be changed, and some steps or sub-steps can be omitted or combined.
[0060] Step S10: Form a plurality of through holes spaced apart on the heat-resistant alloy layer.
[0061] In some embodiments, the heat-resistant alloy layer is a nickel thin film. The specifications of the nickel thin film can be, but are not limited to: nickel content > 99.99%, thickness 60 μm, and width 400 mm. In other embodiments, other heat-resistant alloy materials can be selected for the heat-resistant alloy layer.
[0062] In some embodiments, the nickel sheet is cut into rectangles of a certain size, the length of which is 0.5 cm to 1 cm longer than the inner circumference of the quartz tube (e.g., the nickel sheet is cut to a length of 1360 mm). Then, a stamping machine is used to create multiple circular through-holes on the surface of the nickel sheet. The diameter of the circular through-holes can be, but is not limited to, 3.5 mm. The gap between adjacent through-holes can be, but is not limited to, 80 mm.
[0063] The pre-formation of through holes and the venting design help prevent air and adhesive from being trapped during the subsequent bonding process, avoid the generation of bubbles or voids, ensure the density and uniformity of the adhesive layer, and improve the quality of the furnace tube.
[0064] Step S20: Roughen the heat-resistant alloy layer.
[0065] Specifically, the heat-resistant alloy layer includes an adhesive surface for bonding to the inner wall of the quartz tube. Roughening the heat-resistant alloy layer involves rubbing the adhesive surface with sandpaper. This effective roughening method improves processing efficiency and bonding quality, ensures uniformity and appropriate roughness of the adhesive surface, and further enhances bond strength.
[0066] In some embodiments, the bonding surface of the heat-resistant alloy layer is rubbed with 400-800 grit sandpaper (e.g., 400-500, 500-600, 600-800, etc.) until a matte finish is achieved. This roughening treatment of the heat-resistant alloy layer increases the surface area of the bonding surface, which is beneficial for improving the adhesion of the adhesive in subsequent steps, enhancing the bond strength between the heat-resistant alloy layer and the quartz tube, and preventing separation at high temperatures.
[0067] Step S30: Roughen the inner wall of the quartz tube.
[0068] Specifically, step S30 includes sandblasting the inner wall of the quartz tube.
[0069] In some embodiments, the abrasive used for sandblasting is corundum with a particle size between 100 and 200 mesh (e.g., 100 to 120 mesh, 120 to 150 mesh, 150 to 180 mesh, 180 to 200 mesh). This roughens the inner wall of the quartz tube, increasing its surface area, which is beneficial for improving the adhesion of the adhesive in subsequent steps, enhancing the bond strength between the heat-resistant alloy layer and the quartz tube, and preventing separation at high temperatures.
[0070] Step S40: The heat-resistant alloy layer is attached to the inner wall of the quartz tube with an adhesive to obtain a composite tube.
[0071] In some embodiments, the inner wall of the quartz tube is sandblasted and then rinsed with distilled water. After the quartz tube dries, a prepared adhesive is sprayed onto the inner wall of the quartz tube at a speed of 20 rpm. Then, a pre-cut heat-resistant alloy layer is laid along the circumference of the inner wall of the quartz tube. Then, using a silicone scraper, air and / or excess adhesive between the heat-resistant alloy layer and the inner wall of the quartz tube are expelled through the through-holes and the edges of the heat-resistant alloy layer by squeezing and scraping, ensuring a tight fit between the heat-resistant alloy layer and the inner wall of the quartz tube.
[0072] The adhesive can be, but is not limited to, an adhesive made by combining a phosphate-based curing agent with silicate powder.
[0073] Step S50: Check the steps.
[0074] In some embodiments, the inspection steps include: after the composite tube has been left to stand for a preset time, checking whether the composite tube has quality defects such as degumming, separation and / or bulging; if the composite tube has quality defects, then the composite tube is re-glued and compacted, and the inspection steps are repeated until the composite tube is free of quality defects.
[0075] Therefore, by setting up quality control procedures, it is beneficial to promptly identify and repair defects in the bonding process, avoid the generation of substandard products, and improve the yield and reliability of furnace tubes.
[0076] Specifically, after bonding the composite tubes, let them stand for a preset time (e.g., 8 hours). Check for problems such as delamination, separation, or bulging. If problems are found, apply additional adhesive or compact the affected areas. Then let them stand for another preset time (e.g., 8 hours) to ensure the composite tubes are free of quality defects.
[0077] Step S60: Heat-treat the composite tube to cure the adhesive and bond the heat-resistant alloy layer and the inner wall of the quartz tube, and oxidize the surface of the heat-resistant alloy layer away from the quartz tube to form a metal oxide layer.
[0078] In some embodiments, heat treatment of the composite tube specifically includes the following steps S61 to S64.
[0079] Step S61: Place the composite tube into a high-temperature furnace and raise the temperature of the furnace from room temperature to 120°C to 180°C (e.g., 120°C to 130°C, 130°C to 150°C, 150°C to 160°C, 160°C to 180°C) over a period of 10 to 30 minutes (e.g., 10 to 15 minutes, 15 minutes to 2 hours, 2 hours to 3 hours).
[0080] Step S62: Raise the temperature inside the high-temperature furnace to 550℃ to 600℃ (e.g., 550℃ to 565℃, 565℃ to 585℃, 585℃ to 600℃) over 50min to 80min (e.g., 50min to 60min, 60min to 70min, 70min to 80min) and hold it at that temperature for 1h to 3h.
[0081] Step S63: Raise the temperature inside the high-temperature furnace to 750°C to 830°C (e.g., 750°C to 780°C, 780°C to 810°C, 810°C to 830°C) and keep it at that temperature for 1 hour to 3 hours.
[0082] Step S64: Turn off the heat source and allow the composite tube to cool down naturally to room temperature along with the furnace (e.g., after 16 hours).
[0083] Therefore, by controlling the temperature and time during the heat treatment process, it is beneficial to ensure the complete curing of the adhesive and the uniform oxidation of the heat-resistant alloy layer surface, forming a stable metal oxide layer and optimizing the physical and chemical properties of the furnace tube.
[0084] In some embodiments, the heat-resistant alloy layer in the protective layer of the furnace tube is a nickel-based alloy. The heat-resistant alloy layer can stably adhere to the inner wall of the quartz tube and will not fall off under thermal shock at 100°C. In actual use, it does not have a negative impact on the vacuum environment, and the chemical vapor deposition process of polycrystalline silicon can be produced normally with stable quality. The furnace tube life is increased by more than 78%. When the furnace tube is taken off the production line, only cracks exist, and the entire tube can be removed, avoiding damage to the machine and products caused by the quartz tube exploding.
[0085] The above embodiments are only used to illustrate the technical solutions of this application and are not intended to limit it. Although this application has been described in detail with reference to the above preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions to the technical solutions of this application should not depart from the spirit and scope of the technical solutions of this application.
Claims
1. A furnace tube, characterized in that, It includes a quartz tube, an adhesive layer, and a protective layer. The protective layer includes a stacked heat-resistant alloy layer and a metal oxide layer. The heat-resistant alloy layer is bonded to the inner wall of the quartz tube through the adhesive layer. The metal oxide layer is located on the surface of the heat-resistant alloy layer opposite to the quartz tube.
2. The furnace tube as described in claim 1, characterized in that, The material of the heat-resistant alloy layer is any one of nickel-based alloys, molybdenum alloys, and tungsten alloys.
3. The furnace tube as described in claim 1, characterized in that, The adhesive layer is made of any one of phosphate adhesives, silicate adhesives, and ceramic adhesives.
4. The furnace tube as described in any one of claims 1 to 3, characterized in that, The protective layer has multiple through holes spaced apart.
5. The furnace tube as described in claim 4, characterized in that, The size of each of the through holes ranges from 2 mm to 8 mm; and / or the distance between adjacent through holes ranges from 30 mm to 150 mm.
6. The furnace tube as described in any one of claims 1 to 3, characterized in that, The thickness of the protective layer ranges from 20 μm to 100 μm.
7. A processing equipment, characterized in that, Including furnace tubes as claimed in any one of claims 1 to 6.
8. A method for preparing a furnace tube, characterized in that, include: A heat-resistant alloy layer is attached to the inner wall of a quartz tube using an adhesive to obtain a composite tube. as well as The composite tube is subjected to heat treatment to cure the adhesive and bond the heat-resistant alloy layer and the inner wall of the quartz tube, and to oxidize the surface of the heat-resistant alloy layer away from the quartz tube to form a metal oxide layer.
9. The method for preparing the furnace tube as described in claim 8, characterized in that, The heat-resistant alloy layer includes an adhesive surface for bonding with the quartz tube; Before attaching the heat-resistant alloy layer to the inner wall of the quartz tube using the adhesive, the method for preparing the furnace tube further includes: roughening the bonding surface, and / or roughening the inner wall of the quartz tube.
10. The method for preparing the furnace tube as described in claim 9, characterized in that, The bonding surface is roughened by rubbing it with sandpaper; The inner wall of the quartz tube is roughened, including sandblasting the inner wall of the quartz tube.
11. The method for preparing the furnace tube as described in claim 8, characterized in that, Before attaching the heat-resistant alloy layer to the inner wall of the quartz tube using the adhesive, the method for preparing the furnace tube further includes: forming a plurality of spaced through holes on the heat-resistant alloy layer; Attaching the heat-resistant alloy layer to the inner wall of the quartz tube using the adhesive includes: expelling air and / or excess adhesive between the heat-resistant alloy layer and the inner wall of the quartz tube through the through-hole and the edge of the heat-resistant alloy layer.
12. The method for preparing the furnace tube as described in claim 8, characterized in that, Before heat treatment of the composite tube, the process further includes: Inspection steps: After the composite tube has been left to stand for a preset time, check whether the composite tube has quality defects such as delamination, separation and / or bulging; if the composite tube has such quality defects, then apply glue and compact the composite tube, and repeat the inspection steps until the composite tube is free of such quality defects.
13. The method for preparing a furnace tube according to any one of claims 8 to 12, characterized in that, The composite tube is subjected to heat treatment, comprising: placing the composite tube in a high-temperature furnace, raising the temperature in the high-temperature furnace from room temperature to 120°C to 180°C over 10 to 30 minutes, and holding the temperature for 1 to 3 hours; then raising the temperature in the high-temperature furnace to 550°C to 600°C over 50 to 80 minutes, and holding the temperature for 1 to 3 hours; then raising the temperature in the high-temperature furnace to 750°C to 830°C, and holding the temperature for 1 to 3 hours; and finally cooling the temperature in the high-temperature furnace to room temperature.