Method for preparing a protective layer on stainless steel parts of a mocvd reactor chamber

Abstract

The application provides a method for preparing a protective layer on a stainless steel component of a MOCVD reaction cavity, and relates to the technical field of semiconductor devices. The method comprises the following steps: roughening the surface of a stainless steel component to be processed; sequentially forming a MgO-based transition layer and a MgO-based functional layer; the thermal expansion coefficient of the stainless steel component to be processed is CTE1, the thermal expansion coefficient of the MgO-based transition layer is CTE2, and the thermal expansion coefficient of the MgO-based functional layer is CTE3; CTE1>CTE2>CTE3. The MgO-based transition layer and the MgO-based functional layer jointly form a MgO-based protective layer. The method solves the problems of long equipment occupation time, high maintenance cost and unstable coating performance in the prior art, and further improves the adaptability and long-term use stability of the protective layer on stainless steel components of different sizes and curvatures.

Description

Technical Field

[0001] This application relates to the field of semiconductor device technology, and more particularly to a method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber. Background Technology

[0002] Currently, the protective layer is mainly formed by multiple rounds of "in-situ venting" within the MOCVD (Metal-organic Chemical Vapor Deposition) reaction chamber. However, this process is heavily dependent on the equipment itself, taking 2-3 weeks, which is extremely long and occupies core production equipment, significantly reducing equipment uptime. Furthermore, the composition and structure of the formed protective layer are uncontrollable, resulting in low density, weak adhesion, and easy peeling under thermal shock above 1200℃, leading to large fluctuations in metal volatilization and failing to effectively prevent contamination. Moreover, this lengthy process must be repeated every time the top cover is cleaned and maintained, increasing the annual maintenance cost per unit. The root cause of these problems lies in binding the preparation of the protective layer to the core process equipment, lacking an independent, controllable, and efficient offline preparation solution.

[0003] Currently, there are solutions that involve coating the surface of stainless steel components within the MOCVD reaction chamber with a dense protective film. However, these solutions only vaguely mention that the protective film composition may include magnesium nitrides / oxides, without disclosing any pretreatment processes for the stainless steel components or specifying the exact structure and precise preparation parameters of the protective film. This results in weak coating adhesion and unreliable density, making it prone to peeling under high-temperature service environments of 1250°C. Furthermore, these solutions still fall under the core limitation of "relying on online preparation within the MOCVD chamber," failing to address the issue of large fluctuations in metal volatilization and neglecting the compatibility with stainless steel components of different sizes and curvatures. Consequently, they fail to achieve a substantial breakthrough in addressing the core pain points of existing technologies. Summary of the Invention

[0004] In view of the above problems, this application provides a method for preparing a protective layer on stainless steel components of an MOCVD reaction chamber, solving the problems of long equipment occupancy time, high maintenance costs, and unstable coating performance in existing technologies. It also specifically addresses the risk of high-temperature cracking and peeling caused by thermal expansion mismatch between the pure MgO-based protective layer and the stainless steel components, further improving the adaptability and long-term stability of the protective layer on stainless steel components of different sizes and curvatures. The specific solution is as follows:

[0005] This application provides a method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the method comprising:

[0006] Roughen the surface of the stainless steel parts to be treated;

[0007] A MgO-based transition layer is formed on the surface of the stainless steel component to be treated after roughening.

[0008] A MgO-based functional layer is formed on the side of the MgO-based transition layer opposite to the stainless steel component to be treated.

[0009] Wherein, the coefficient of thermal expansion of the stainless steel component to be treated is CTE1, the coefficient of thermal expansion of the MgO-based transition layer is CTE2, and the coefficient of thermal expansion of the MgO-based functional layer is CTE3; CTE1 > CTE2 > CTE3.

[0010] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the roughening treatment of the surface of the stainless steel component to be treated includes:

[0011] The surface of the stainless steel component to be treated is roughened by sandblasting using abrasive grains with a diameter range of 50μm-100μm, including the endpoint values.

[0012] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the roughening treatment of the surface of the stainless steel component to be treated includes:

[0013] Plasma etching is performed on the surface of the stainless steel component to be processed, with a power range of 250W-300W (including the endpoint value) and a processing time range of 5min-15min (including the endpoint value).

[0014] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the formation of a MgO-based transition layer on the surface of the roughened stainless steel component includes:

[0015] The surface of the roughened stainless steel component has a thermal expansion coefficient ranging from 13 × 10⁻⁶. -6 K -1 -17×10 -6 K -1 Including endpoint values, MgO-based transition layers.

[0016] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the step of forming a MgO-based functional layer on the side of the MgO-based transition layer opposite to the stainless steel component to be treated includes:

[0017] A thermal expansion coefficient ranging from 10 × 10⁻⁶ is formed on the side of the MgO-based transition layer opposite to the stainless steel component to be treated. -6 K -1 -12×10 -6 K -1Including endpoint values, MgO-based functional layers.

[0018] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the formation of a MgO-based transition layer on the surface of the roughened stainless steel component includes:

[0019] The sol-gel method is used to coat the surface of the roughened stainless steel component with MgO-NiO composite sol to form the MgO-based transition layer.

[0020] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the step of forming a MgO-based functional layer on the side of the MgO-based transition layer opposite to the stainless steel component to be treated includes:

[0021] The MgO-based functional layer is formed by coating magnesium isopropoxide sol or MgO-Al2O3 composite sol onto the side of the MgO-based transition layer away from the stainless steel component to be treated using the sol-gel method.

[0022] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the sol-gel method is used to coat the surface of the roughened stainless steel component with a MgO-NiO composite sol to form the MgO-based transition layer, comprising:

[0023] Using the sol-gel method, MgO-NiO composite sol is coated on the surface of the roughened stainless steel part to be treated at a dipping speed in the range of 2 mm / s-5 mm / s including the endpoint value to form the MgO-based transition layer.

[0024] The process employs a sol-gel method, coating the MgO-based transition layer on the side facing away from the stainless steel component to be treated with magnesium isopropoxide sol or MgO-Al2O3 composite sol to form the MgO-based functional layer, including:

[0025] Using the sol-gel method, magnesium isopropoxide sol or MgO-Al2O3 composite sol is applied to the side of the MgO-based transition layer away from the stainless steel component to be treated at a dipping speed in the range of 2 mm / s-5 mm / s, including the endpoint value, to form the MgO-based functional layer.

[0026] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the method further includes:

[0027] Sintering treatment is performed.

[0028] Preferably, in the above method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, the sintering process includes:

[0029] Sintering is performed with a heating rate of 3℃ / min-5℃ / min, including the endpoint value, a heating temperature of 450℃-550℃, including the endpoint value, and a holding time of 1h-3h, including the endpoint value.

[0030] By means of the above technical solution, this application provides a method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber includes: roughening the surface of the stainless steel component to be treated; forming an MgO-based transition layer on the roughened surface of the stainless steel component to be treated; and forming an MgO-based functional layer on the side of the MgO-based transition layer away from the stainless steel component to be treated. The coefficient of thermal expansion of the stainless steel component to be treated is CTE1, the coefficient of thermal expansion of the MgO-based transition layer is CTE2, and the coefficient of thermal expansion of the MgO-based functional layer is CTE3; CTE1 > CTE2 > CTE3.

[0031] Before preparing the protective layer, the technical solution of this application first roughens the surface of the stainless steel component to be treated, thereby increasing the bonding force between the protective layer and the stainless steel component, and fundamentally solving the problem of thermal shock peeling of the protective layer.

[0032] The gradient structure of the MgO-based transition layer and the MgO-based functional layer formed in sequence achieves a smooth transition of thermal expansion coefficients when CTE1 > CTE2 > CTE3. This allows the final protective layer to withstand ≥50 thermal shock cycles (air cooling) at 1250℃ without cracking, making it suitable for stainless steel parts of different sizes and curvatures, such as 8-inch and 12-inch, thus breaking through the limitations of traditional single-coating application scenarios.

[0033] Furthermore, the preparation of the protective layer in this application is not tied to the core process equipment. The entire process is completed outside the MOCVD equipment and does not occupy its production time. That is, after the protective layer is prepared on the stainless steel component, it can be installed on the MOCVD reaction chamber. It is an independent, controllable, and efficient offline preparation solution.

[0034] In summary, the technical solution of this application solves the problems of long equipment occupancy time, high maintenance cost and unstable coating performance in the prior art. At the same time, it specifically addresses the risk of high-temperature cracking and peeling caused by thermal expansion mismatch between MgO-based protective layer and stainless steel parts, and further improves the adaptability and long-term stability of the protective layer on stainless steel parts of different sizes and curvatures. Attached Figure Description

[0035] The above and other features, advantages, and aspects of the embodiments of this disclosure will become more apparent from the accompanying drawings and the following detailed description. Throughout the drawings, the same or similar reference numerals denote the same or similar elements. It should be understood that the drawings are schematic, and the originals and elements are not necessarily drawn to scale.

[0036] Figure 1 This is a schematic flowchart illustrating a method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, as provided in an embodiment of the present invention.

[0037] Figure 2 A schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, provided in an embodiment of the present invention.

[0038] Figure 3 A schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, provided in an embodiment of the present invention.

[0039] Figure 4 A schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, provided in an embodiment of the present invention.

[0040] Figure 5 A schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, provided in an embodiment of the present invention.

[0041] Figure 6 This is a schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, provided in an embodiment of the present invention. Detailed Implementation

[0042] The embodiments of this application are described below with reference to the accompanying drawings. The terminology used in the implementation section of this application is only for explaining specific embodiments and is not intended to limit the application. Those skilled in the art will recognize that, with technological advancements and the emergence of new scenarios, the technical solutions provided in the embodiments of this application are also applicable to similar technical problems.

[0043] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0044] It should be noted that the directional terms appearing in this invention are based on the relative positional relationships shown in the accompanying drawings and should not be taken as absolute limitations on this application.

[0045] Various modifications and variations can be made to this invention without departing from its spirit or scope, as will be apparent to those skilled in the art. Therefore, this invention is intended to cover modifications and variations falling within the scope of the corresponding claims (the claimed technical solutions) and their equivalents. It should be noted that the embodiments provided in this invention can be combined with each other without contradiction.

[0046] refer to Figure 1 , Figure 1 This is a schematic flowchart illustrating a method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, as provided in an embodiment of the present invention. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, as provided in this embodiment of the present invention, includes:

[0047] S101: Roughen the surface of the stainless steel parts to be treated.

[0048] S102: A MgO-based transition layer is formed on the surface of the roughened stainless steel component.

[0049] S103: An MgO-based functional layer is formed on the side of the MgO-based transition layer away from the stainless steel component to be treated; wherein the coefficient of thermal expansion of the stainless steel component to be treated is CTE1, the coefficient of thermal expansion of the MgO-based transition layer is CTE2, and the coefficient of thermal expansion of the MgO-based functional layer is CTE3; CTE1 > CTE2 > CTE3.

[0050] Optionally, a surface with a thermal expansion coefficient ranging from 13 × 10⁻⁶ is formed on the roughened stainless steel component. -6 K -1 -17×10 -6 K -1 A MgO-based transition layer is formed on the side of the MgO-based transition layer opposite to the stainless steel component to be treated, with a thermal expansion coefficient ranging from 10 × 10⁻⁶. -6 K -1 -12×10 -6 K -1 MgO-based functional layers. Among them, 13 × 10 -6 K -1 -17×10 - 6 K -1 This parameter range includes endpoint values, 10×10 -6 K -1 -12×10 -6 K -1 This parameter range includes endpoint values.

[0051] For example, a surface with a thermal expansion coefficient of 15 × 10⁻⁶ is formed on the surface of the roughened stainless steel part. - 6 K -1 A MgO-based transition layer is formed on the side of the MgO-based transition layer opposite to the stainless steel component to be treated, with a coefficient of thermal expansion of 10.8 × 10⁻⁶. -6 K -1 MgO-based functional layer.

[0052] Specifically, in this embodiment of the invention, the stainless steel component to be processed includes, but is not limited to, the top cover, spray head, and sidewalls of the MOCVD reaction chamber. The MgO-based transition layer and the MgO-based functional layer together form the MgO-based protective layer covering the stainless steel component.

[0053] Before preparing the protective layer, the technical solution of this application first roughens the surface of the stainless steel component to be treated, thereby increasing the bonding force between the protective layer and the stainless steel component, and fundamentally solving the problem of thermal shock peeling of the protective layer.

[0054] Subsequently, the gradient structure of the MgO-based transition layer and the MgO-based functional layer, which are formed sequentially, achieves a smooth transition of the coefficient of thermal expansion under the condition that CTE1 > CTE2 > CTE3. This allows the final protective layer to withstand ≥50 thermal shock cycles (air cooling) at 1250℃ without cracking, making it suitable for stainless steel parts of different sizes and curvatures, such as 8 inches and 12 inches, thus breaking through the limitations of traditional single-coating application scenarios.

[0055] Furthermore, the preparation of the protective layer in this application is not tied to the core process equipment. The entire process is completed outside the MOCVD equipment and does not occupy its production time. That is, after the protective layer is prepared on the stainless steel component, it can be installed on the MOCVD reaction chamber. It is an independent, controllable, and efficient offline preparation solution.

[0056] In summary, the technical solution of this application solves the problems of long equipment occupancy time, high maintenance cost and unstable coating performance in the prior art. At the same time, it specifically solves the risk of high temperature cracking and peeling caused by thermal expansion mismatch between pure MgO-based protective layer and stainless steel parts, and further improves the adaptability and long-term stability of the protective layer on stainless steel parts of different sizes and curvatures.

[0057] In an optional embodiment of the present invention, reference is made to... Figure 2 , Figure 2 This is a schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component in an MOCVD reaction chamber, provided by an embodiment of the present invention. In this embodiment, one possible implementation of step S101, "roughening the surface of the stainless steel component to be treated," is as follows:

[0058] S1011: The surface of the stainless steel component to be treated is roughened by sandblasting using abrasive grains with a diameter range of 50μm-100μm. The parameter range of 50μm-100μm includes the endpoint values.

[0059] Specifically, compared to the simple cleaning steps in existing technologies, in this embodiment of the invention, sandblasting is performed on the surface of the stainless steel component to be treated with abrasive particles with a diameter range of 50μm-100μm to achieve deep cleaning and activation of the surface of the stainless steel component to be treated. This maximizes the bonding force between the subsequently prepared film layer and the stainless steel component, fundamentally solving the problem of thermal shock peeling of the subsequently prepared protective layer.

[0060] Optionally, the surface roughness range of the roughened stainless steel part can be Ra1.5μm-Ra2.0μm.

[0061] In an optional embodiment of the present invention, reference is made to... Figure 3 , Figure 3 This is a schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component in an MOCVD reaction chamber, provided by an embodiment of the present invention. In this embodiment, one possible implementation of step S101, "roughening the surface of the stainless steel component to be treated," is as follows:

[0062] S1012: Plasma etching is performed on the surface of the stainless steel component to be processed, with a power range of 250W-300W and a processing time range of 5min-15min. The 250W-300W and 5min-15min parameter ranges include both endpoints.

[0063] Specifically, compared to the simple cleaning steps in existing technologies, in this embodiment of the invention, plasma etching is performed on the surface of the stainless steel component to be treated under a power range of 300W and a processing time range of 10 minutes to achieve deep cleaning and activation of the surface of the stainless steel component. This maximizes the bonding force between the subsequently prepared film layer and the stainless steel component, fundamentally solving the problem of thermal shock peeling of the subsequently prepared protective layer.

[0064] In an optional embodiment of the present invention, reference is made to... Figure 4 , Figure 4 This is a schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component in an MOCVD reaction chamber, provided by an embodiment of the present invention. In this embodiment, one possible implementation of step S101, "roughening the surface of the stainless steel component to be treated," is as follows:

[0065] S1011: The surface of the stainless steel component to be treated is roughened by sandblasting using abrasive grains with a diameter range of 50μm-100μm. The parameter range of 50μm-100μm includes the endpoint values.

[0066] S1012: Plasma etching is performed on the surface of the stainless steel component to be processed, with a power range of 250W-300W and a processing time range of 5min-15min. The 250W-300W and 5min-15min parameter ranges include both endpoints.

[0067] Specifically, compared to the simple cleaning steps in existing technologies, in this embodiment of the invention, sandblasting is performed on the surface of the stainless steel component to be treated using abrasive particles with a diameter range of 50μm-100μm; and plasma etching is performed on the surface of the stainless steel component to be treated with a power range of 250W-300W and a processing time range of 5min-15min, in order to achieve the purpose of deep cleaning and activation of the surface of the stainless steel component to be treated to the greatest extent, thereby maximizing the bonding force between the subsequently prepared film layer and the stainless steel component, fundamentally solving the problem of thermal shock peeling of the subsequently prepared protective layer.

[0068] Experiments have shown that this design can ensure that the bonding strength between the subsequently prepared protective layer and the stainless steel component is greater than or equal to 40 MPa, which is much higher than the 25 MPa of the traditional in-situ venting method. This effectively solves the problem of Fe, Cr, Ni and other metal elements volatilizing and contaminating the epitaxial wafer due to thermal shock spalling of the protective layer.

[0069] It should be noted that when the roughening treatment of the surface of the stainless steel part to be treated includes both steps S1011 and S1012, the order of steps S1011 and S1012 is not explicitly limited and can be determined according to the actual situation.

[0070] In an optional embodiment of the present invention, reference is made to... Figure 5 , Figure 5 This is a schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component in an MOCVD reaction chamber, provided by an embodiment of the present invention. In this embodiment, one possible implementation of step S102, "forming a MgO-based transition layer on the surface of the roughened stainless steel component," is as follows:

[0071] S1021: Using the sol-gel method, MgO-NiO composite sol is coated on the surface of the roughened stainless steel part to be treated to form the MgO-based transition layer.

[0072] In an embodiment of the present invention, one possible way to implement step S103, "forming an MgO-based functional layer on the side of the MgO-based transition layer away from the stainless steel component to be treated," is as follows:

[0073] S1031: Using the sol-gel method, magnesium isopropoxide sol or MgO-Al2O3 composite sol is coated on the side of the MgO-based transition layer away from the stainless steel component to be treated, to form the MgO-based functional layer.

[0074] Specifically, compared to the uncontrollable in-situ degassing method used in existing technologies to deposit a protective layer, this invention employs a two-step dip-coating process. The first step involves coating the roughened stainless steel component with a MgO-NiO composite sol to form the MgO-based transition layer. The second step involves coating the side of the MgO-based transition layer away from the stainless steel component with either magnesium isopropoxide sol or MgO-Al2O3 composite sol to form the MgO-based functional layer. The molar ratio of the MgO-NiO composite sol is in the range of 3:7-7:3, i.e., MgO:NiO is 3:7. -7:3; the concentration range of magnesium isopropoxide sol is 0.3mol / L-0.6mol / L; the molar ratio range of MgO-Al2O3 composite sol is 9:1, that is, MgO:Al2O3 is 9:1; this technical solution not only achieves precise control of coating thickness and uniformity, but also adapts to the thermal expansion difference between stainless steel parts and MgO-based functional layers through gradient composition design, specifically solving the risk of high-temperature cracking and peeling caused by thermal expansion mismatch between MgO-based protective layer and stainless steel parts, further improving the adaptability and long-term stability of MgO-based protective layer on stainless steel parts of different sizes and curvatures.

[0075] Optionally, using the sol-gel method, a MgO-NiO composite sol is coated onto the surface of the roughened stainless steel component to be treated at a dipping speed ranging from 2 mm / s to 5 mm / s to form the MgO-based transition layer. Then, using the sol-gel method, on the side of the MgO-based transition layer opposite to the stainless steel component to be treated, a magnesium isopropoxide sol or a MgO-Al₂O₃ composite sol is coated at a dipping speed ranging from 2 mm / s to 5 mm / s to form the MgO-based functional layer. The parameter range of 2 mm / s to 5 mm / s includes endpoint values.

[0076] Optionally, the dipping speed for forming the MgO-based transition layer can be the same as or different from the dipping speed for forming the MgO-based functional layer, depending on the actual situation. The purpose of the adjustment is to achieve precise control of the coating thickness and uniformity.

[0077] In an optional embodiment of the present invention, a sol-gel method is used to form multiple MgO-based transition layers. The multiple MgO-based transition layers have different coefficients of thermal expansion. In the direction from the stainless steel component to the MgO-based functional layer, the coefficient of thermal expansion of the multiple MgO-based transition layers gradually decreases. The maximum coefficient of thermal expansion of the multiple MgO-based transition layers is less than the coefficient of thermal expansion of the stainless steel component to be treated, and the minimum coefficient of thermal expansion of the multiple MgO-based transition layers is greater than the coefficient of thermal expansion of the MgO-based functional layer. This achieves a more refined and smooth transition of the coefficient of thermal expansion, and minimizes the risk of high-temperature cracking and detachment caused by thermal expansion mismatch between the MgO-based protective layer and the stainless steel component. This further improves the adaptability and long-term stability of the MgO-based protective layer on stainless steel components of different sizes and curvatures.

[0078] In an optional embodiment of the present invention, reference is made to... Figure 6 , Figure 6 This is a schematic flowchart illustrating another method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, provided by an embodiment of the present invention. In this embodiment, the method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber further includes:

[0079] S104: Sintering treatment is performed.

[0080] Specifically, in this embodiment of the invention, after the MgO-based transition layer and the MgO-based functional layer are sequentially formed using the sol-gel method, sintering is performed. Optionally, sintering is performed at a heating rate of 3°C / min-5°C / min, a temperature of 450°C-550°C, and a holding time of 1h-3h. This promotes the complete transformation of the sol into a dense MgO ceramic layer with a density ≥95%, further achieving interfacial fusion between the MgO-based transition layer, the MgO-based functional layer, and the stainless steel components, ultimately forming a gradient structure MgO-based protective layer with a density ≥95%, ensuring that its metal volatilization at 1250°C is stably ≤0.001 mg / cm³. 2 The performance is far superior to that of traditional solutions. Specifically, the parameter ranges 3℃ / min-5℃ / min, 450℃-550℃, and 1h-3h all include endpoint values.

[0081] The technical solution of this application will be further explained below by comparison.

[0082] Example 1:

[0083] A 316L stainless steel top cover was sandblasted with 80μm diameter white corundum to obtain a component with a surface roughness Ra of 1.8μm. It was then placed in a plasma cleaner and treated with 300W Ar plasma for 10 minutes. Subsequently, in a Class 100 cleanliness coating machine, a MgO-based transition layer was first coated with a 0.5mol / L MgO-NiO composite sol (molar ratio 5:5) at a dipping speed of 3mm / s, and allowed to stand at room temperature for 10 minutes. The second step involved dipping a MgO-based functional layer with a 0.5mol / L magnesium isopropoxide sol at a dipping speed of 3mm / s. After removal, the component was heated to 500℃ in a programmed furnace at a heating rate of 4℃ / min and held for 2 hours. Testing showed that the adhesion between the MgO-based protective layer and the stainless steel component was 42MPa, and the metal volatilization at 1250℃ was 0.0008mg / cm³. 2 .

[0084] Example 2:

[0085] The only difference from Example 1 is that the step of "placing the component in a plasma cleaner and treating it with Ar plasma at a power of 300W for 10 minutes" is omitted. Testing revealed that the adhesion between the MgO-based protective layer and the stainless steel component was 32 MPa, and localized peeling occurred after three thermal shocks.

[0086] Comparative example:

[0087] Simulating the traditional in-situ venting method, a top cover of the same specifications as in Example 1 was subjected to a standard venting process for six rounds within the MOCVD reaction chamber. Testing revealed a coating adhesion of 24 MPa and a metal volatilization rate of 0.012 mg / cm³ at 1250°C. 2 .

[0088] As can be seen from the above description, the method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber provided by this application solves the problems of long equipment occupancy time, high maintenance costs, and unstable coating performance in the prior art. At the same time, it specifically addresses the risk of high-temperature cracking and peeling caused by thermal expansion mismatch between the MgO-based protective layer and the stainless steel component, further improving the adaptability and long-term stability of the protective layer on stainless steel components of different sizes and curvatures.

[0089] The above provides a detailed description of a method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber. Specific examples have been used to illustrate the principle and implementation of the invention. The description of the above embodiments is only for the purpose of helping to understand the method and core idea of ​​the invention. At the same time, for those skilled in the art, there will be changes in the specific implementation and application scope based on the idea of ​​the invention. Therefore, the content of this specification should not be construed as a limitation of the invention.

[0090] It should be noted that each embodiment in this specification focuses on the differences from other embodiments, and the same or similar parts between the embodiments can be referred to each other.

[0091] It should also be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that elements inherent to a process, method, article, or apparatus that comprises a list of elements, or elements inherent to such processes, methods, articles, or apparatus, are also included. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0092] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber, characterized in that, The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber includes: Roughen the surface of the stainless steel parts to be treated; A MgO-based transition layer is formed on the surface of the stainless steel component to be treated after roughening. A MgO-based functional layer is formed on the side of the MgO-based transition layer opposite to the stainless steel component to be treated. Wherein, the coefficient of thermal expansion of the stainless steel component to be treated is CTE1, the coefficient of thermal expansion of the MgO-based transition layer is CTE2, and the coefficient of thermal expansion of the MgO-based functional layer is CTE3; CTE1 > CTE2 > CTE3.

2. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 1, characterized in that, The surface roughening treatment of the stainless steel component to be treated includes: The surface of the stainless steel component to be treated is roughened by sandblasting using abrasive grains with a diameter range of 50μm-100μm, including the endpoint values.

3. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 1 or 2, characterized in that, The surface roughening treatment of the stainless steel component to be treated includes: Plasma etching is performed on the surface of the stainless steel component to be processed, with a power range of 250W-300W (including the endpoint value) and a processing time range of 5min-15min (including the endpoint value).

4. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 1, characterized in that, The process of forming a MgO-based transition layer on the surface of the roughened stainless steel component includes: The surface of the roughened stainless steel component has a thermal expansion coefficient ranging from 13 × 10⁻⁶. -6 K -1 -17×10 -6 K -1 Including endpoint values, MgO-based transition layers.

5. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 1, characterized in that, The formation of a MgO-based functional layer on the side of the MgO-based transition layer opposite to the stainless steel component to be treated includes: A thermal expansion coefficient ranging from 10 × 10⁻⁶ is formed on the side of the MgO-based transition layer opposite to the stainless steel component to be treated. -6 K -1 -12×10 -6 K -1 Including endpoint values, MgO-based functional layers.

6. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 1, characterized in that, The process of forming a MgO-based transition layer on the surface of the roughened stainless steel component includes: The sol-gel method is used to coat the surface of the roughened stainless steel component with MgO-NiO composite sol to form the MgO-based transition layer.

7. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 6, characterized in that, The formation of a MgO-based functional layer on the side of the MgO-based transition layer opposite to the stainless steel component to be treated includes: The MgO-based functional layer is formed by coating magnesium isopropoxide sol or MgO-Al2O3 composite sol onto the side of the MgO-based transition layer away from the stainless steel component to be treated using the sol-gel method.

8. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 7, characterized in that, The process employs a sol-gel method, coating the surface of the roughened stainless steel component with a MgO-NiO composite sol to form the MgO-based transition layer, comprising: Using the sol-gel method, MgO-NiO composite sol is coated on the surface of the roughened stainless steel part to be treated at a dipping speed in the range of 2 mm / s-5 mm / s including the endpoint value to form the MgO-based transition layer. The process employs a sol-gel method, coating the MgO-based transition layer on the side facing away from the stainless steel component to be treated with magnesium isopropoxide sol or MgO-Al2O3 composite sol to form the MgO-based functional layer, including: Using the sol-gel method, magnesium isopropoxide sol or MgO-Al2O3 composite sol is applied to the side of the MgO-based transition layer away from the stainless steel component to be treated at a dipping speed in the range of 2 mm / s-5 mm / s, including the endpoint value, to form the MgO-based functional layer.

9. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 7, characterized in that, The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber further includes: Sintering treatment is performed.

10. The method for preparing a protective layer on a stainless steel component of an MOCVD reaction chamber according to claim 9, characterized in that, The sintering process includes: Sintering is performed with a heating rate of 3℃ / min-5℃ / min, including the endpoint value, a heating temperature of 450℃-550℃, including the endpoint value, and a holding time of 1h-3h, including the endpoint value.

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