Semiconductor device corrosion-resistant component with gradient functional material and preparation process thereof
By employing a gradient functional material fabrication process that incorporates a high-strength metal layer, a gradient transition layer, and a corrosion-resistant ceramic layer in semiconductor device components, the problems of corrosion resistance, thermal shock resistance, and high structural strength of semiconductor devices under extreme environments have been solved, resulting in a comprehensive improvement in the overall performance of the components.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- ZHONGFENG SEMICONDUCTOR TECHNOLOGY (NANTONG) CO LTD
- Filing Date
- 2026-04-02
- Publication Date
- 2026-06-19
Abstract
Description
Technical Field
[0001] This application relates to the field of semiconductor manufacturing equipment technology, and in particular to a corrosion-resistant component of a semiconductor device with graded functional materials and its manufacturing process. Background Technology
[0002] In semiconductor chip manufacturing, many processes are carried out in high-temperature, highly corrosive atmospheres (such as fluorine-containing chlorine plasma), or acidic / alkaline solutions. As the carriers of these process reactions, the semiconductor equipment chambers and their critical internal components (such as CVD reaction chambers, cleaning machine chambers, and polishing machine plates) are directly exposed to these harsh conditions. Their corrosion resistance, thermal shock resistance, and structural strength directly affect equipment reliability, maintenance cycles, and chip yield. Therefore, developing high-performance component materials capable of long-term stable operation in extreme environments has become a key technological challenge in the semiconductor equipment manufacturing field.
[0003] To address the aforementioned operating conditions, existing technologies mainly employ three approaches: First, components are manufactured as a single piece using ceramics such as yttrium oxide and alumina. While corrosion-resistant, these materials are inherently brittle and have poor resistance to mechanical impact, making it difficult to meet the strength requirements of large-scale, complex structures. Second, a ceramic protective layer is coated onto the surface of a high-strength metal substrate. However, the difference in thermal expansion coefficients between the metal and ceramic can easily cause the coating to crack and peel off during thermal cycling, and once it fails, the substrate will be rapidly corroded. Third, corrosion-resistant ceramics are mechanically spliced with load-bearing metal using bolts or adhesives. However, it is difficult to achieve an airtight seal at the interface, and non-coordinated deformation under thermal cycling can easily lead to loosening and leakage at the joints, resulting in insufficient long-term reliability.
[0004] In summary, existing technical solutions cannot simultaneously meet the comprehensive requirements of semiconductor devices for components in three dimensions: high-temperature corrosion resistance, thermal shock resistance, and high structural strength. They suffer from technical contradictions such as "insufficient corrosion resistance and high strength but poor corrosion resistance" and poor interface bonding reliability. They cannot meet the requirements of advanced processes for long life and high reliability of components, and therefore need to be improved. Summary of the Invention
[0005] To address the aforementioned issues, this application provides a corrosion-resistant component for semiconductor devices with gradient functional materials and its fabrication process.
[0006] This application provides a corrosion-resistant component for semiconductor devices with graded functional materials and its fabrication process, which adopts the following technical solution: In a first aspect, this application provides a fabrication process for corrosion-resistant components of semiconductor devices using graded functional materials, employing the following technical solution: A fabrication process for a corrosion-resistant component of a semiconductor device with graded functional materials includes the following steps: S1. Establish a three-dimensional model of the corrosion-resistant component of the semiconductor device. The corrosion-resistant component of the semiconductor device is provided with a high-strength metal layer, a gradient transition layer and a corrosion-resistant ceramic layer in sequence from the outside to the inside along the thickness direction. Discretize the three-dimensional model into several printing layers and set the material ratio of each layer. S2. Prepare metal powder and ceramic powder; the high-strength metal layer is prepared from metal powder, the corrosion-resistant ceramic layer is prepared from ceramic powder, and the gradient transition layer is prepared from a mixture of metal powder and ceramic powder; place the metal powder and ceramic powder in two independent powder supply systems, adjust the powder feeding ratio of metal powder and ceramic powder through an algorithm, and deposit the high-strength metal layer, gradient transition layer and corrosion-resistant ceramic layer layer by layer to obtain an integrated green body; S3. The integrated green blank is subjected to hot isostatic pressing and surface precision machining to obtain corrosion-resistant components for semiconductor equipment.
[0007] By sequentially depositing a high-strength metal layer, a gradient transition layer, and a corrosion-resistant ceramic layer along the thickness direction of the component from the outside to the inside, and using an independent powder supply system for layer-by-layer cladding deposition, a spatial gradient transition of material components is achieved. The high-strength metal layer serves as the substrate to bear structural loads, improving the tensile strength of the component. The corrosion-resistant ceramic layer directly contacts the corrosive environment, resisting media erosion with its stable chemical properties, thus improving the component's corrosion resistance. The gradient transition layer, through continuous variation in the ratio of metal to ceramic powder, alleviates the thermal stress caused by the difference in thermal expansion coefficients between the metal and ceramic, improving the component's thermal shock resistance under conditions of drastic temperature changes, while eliminating abrupt performance changes between layers. This allows the three-layer structure to form a synergistically reinforced whole, comprehensively improving the component's mechanical strength and environmental stability.
[0008] Preferably, the metal powder in step S2 comprises the following components by mass percentage: 20-22% Cr, 13-14% Mo, 2-3% W, with the balance being Ni and unavoidable impurities.
[0009] In the metal powder composition, chromium forms a continuous solid solution in the nickel matrix, which improves the corrosion resistance of the component by forming a dense oxide film on the surface. Molybdenum and tungsten dissolve in the nickel matrix, causing lattice distortion, which improves the tensile strength of the metal layer through solid solution strengthening mechanism. At the same time, the high melting point of molybdenum and tungsten ensures that the alloy maintains structural stability at high temperatures, which helps to alleviate thermal stress and thus improves the thermal shock resistance of the component. Nickel, as the matrix element, ensures that the components are evenly distributed and form a stable austenitic structure, giving the metal layer both good toughness and strength, providing basic mechanical support for the overall structure, and comprehensively improving the service performance of the component under corrosive environment and thermo-mechanical coupling conditions.
[0010] Preferably, the metal powder further includes 0.5-1% Nb and 0.3-0.5% Y.
[0011] Niobium introduced into the metal powder partially dissolves in the nickel matrix during laser cladding, resulting in solid solution strengthening, while partially combines with nickel to form a dispersed intermetallic compound precipitate phase. This precipitation strengthening mechanism enhances the tensile strength of the metal layer. Yttrium, as an active element, is enriched at grain boundaries and phase interfaces. By purifying grain boundary impurities and refining the solidification structure, it improves the material's density and interfacial bonding strength. Simultaneously, yttrium preferentially oxidizes to form a thermodynamically stable oxide film, enhancing the adhesion and density of the surface oxide film, thereby improving the component's corrosion resistance. The synergistic effect of niobium and yttrium makes the alloy structure more uniform and refined, improving the grain boundary strengthening effect. This helps to hinder grain boundary slip and crack propagation at high temperatures, allowing the metal layer to maintain structural integrity during temperature changes, thus improving the component's thermal shock resistance.
[0012] Preferably, the cladding deposition conditions for the high-strength metal layer in step S2 are as follows: only the metal powder supply system is turned on, the laser power is 300-400W, the scanning speed is 800-1200mm / s, and the layer thickness is 30-50μm.
[0013] The cladding deposition conditions for high-strength metal layers are achieved by limiting the operation of only the metal powder supply system and matching laser power, scanning speed, and layer thickness to ensure that the metal powder receives appropriate energy input and cooling rate during the cladding process. The synergistic effect of laser power and scanning speed ensures that the powder is fully melted and forms a stable molten pool, enabling metallurgical bonding between the cladding layer and the substrate or adjacent layers. This reduces porosity and incomplete fusion defects, improves the density of the metal layer and the interlayer bonding strength, and thus enhances the tensile strength of the component. The stable molten pool fluidity and moderate cooling rate promote the uniform distribution of alloying elements in the nickel matrix, allowing elements such as chromium, molybdenum, and tungsten to fully exert their solid solution strengthening effect, while avoiding localized corrosion-sensitive areas caused by element segregation, thereby improving the corrosion resistance of the component. Layer thickness control ensures that each cladding layer forms a uniform solidification structure, refining the grain size. The fine grain structure can release thermal stress more evenly during temperature changes, inhibiting crack initiation and propagation, thereby improving the thermal shock resistance of the component.
[0014] Preferably, the ceramic powder in step S2 comprises the following components by mass percentage: 10-20% YOF, 5-15% Al2O3, and the balance being Y2O3.
[0015] Yttrium oxide, as a matrix component in ceramic powder, forms a passivation layer in a fluorine-containing plasma environment due to its stable chemical properties, resisting physical sputtering and chemical erosion by active particles and improving the corrosion resistance of the component. The introduction of yttrium oxyfluoride pre-introduces fluorine into the ceramic phase, reducing the reaction driving force between the fluorine plasma and the material surface, further enhancing the surface layer's resistance to fluorine corrosion. At the same time, yttrium oxyfluoride forms a solid solution with yttrium oxide, maintaining the integrity of the crystal structure and helping to maintain the density of the ceramic layer, thereby improving the corrosion resistance of the component. The addition of alumina modulates the thermal expansion behavior of the ceramic layer, reducing the difference in thermal expansion coefficients between it and the metal layer and gradient transition layer, reducing interfacial thermal stress during temperature changes. Simultaneously, alumina promotes liquid phase sintering during laser cladding, filling the gaps between ceramic particles, improving the density and uniformity of the ceramic layer, and thus improving the component's thermal shock resistance and tensile strength.
[0016] Preferably, in step S2, as the number of printed layers increases, the proportion of ceramic powder fed into the gradient transition layer gradually increases, so that the volume fraction of the ceramic phase gradually increases from 0% to 100% with a gradient of 3-5% per layer, while the proportion of metal powder fed into the gradient layer is reduced accordingly.
[0017] The gradient transition layer construction method achieves continuous change of material composition in the thickness direction by increasing the proportion of ceramic powder fed layer by layer, so that the volume fraction of ceramic phase transitions from pure metal to pure ceramic with an increasing gradient in each layer. The gradual increase of the ceramic phase allows for a smooth transition in the coefficient of thermal expansion along the thickness direction, avoiding the concentration of interfacial thermal stress caused by abrupt changes in the coefficient of thermal expansion when metals and ceramics are directly bonded. This ensures that thermal stress is evenly distributed and released within the gradient layer during temperature changes, reducing the risk of crack initiation and propagation, and improving the component's thermal shock resistance. Simultaneously, the gradual change in composition allows the metallic and ceramic phases to form an interlocking network structure within the transition layer. The metallic phase provides a tough framework to bear the load, while the ceramic phase provides rigid support. Their synergistic effect gives the transition layer both strength and toughness, preventing interlayer delamination caused by abrupt changes in performance and improving the component's tensile strength. The gradual introduction of the ceramic phase gradually enriches the surface of the transition layer with ceramic components, forming a continuous microstructure when it connects with the pure ceramic layer. This eliminates interfacial porosity and microcracks caused by abrupt changes in material composition, blocks the penetration path of corrosive media along the interface, and improves the component's corrosion resistance.
[0018] Preferably, the cladding deposition conditions of the gradient transition layer in step S2 are as follows: the laser power increases linearly from 300-400W to 400-500W as the ceramic content increases, the scanning speed decreases linearly from 800-1200mm / s to 400-800mm / s, and the layer thickness is 30-50μm.
[0019] The cladding deposition conditions of the gradient transition layer are matched with the changes in material composition by synergistic regulation of laser power increasing linearly with increasing ceramic content and scanning speed decreasing linearly. As the proportion of ceramic powder increases, the material's reflectivity to laser decreases and its melting point increases. The linearly increasing laser power ensures the full melting of the high-melting-point ceramic phase, avoiding the generation of incomplete fusion defects, improving the density of the transition layer and the interlayer bonding strength, thereby enhancing the tensile strength of the component. The linearly decreasing scanning speed prolongs the molten pool existence time, allowing the metal and ceramic phases to flow and mix fully within the molten pool, forming a microstructure with uniform compositional transition. This eliminates micropores and elemental segregation caused by abrupt changes in composition, blocks the penetration channels of corrosive media along the interlayer, and improves the corrosion resistance of the component. The linear change in power and speed allows the heat input of the molten pool to be smoothly adjusted with the ceramic content, avoiding local overheating or overcooling caused by abrupt energy changes. This allows thermal stress to be uniformly released within the gradient layer, inhibiting the initiation of hot cracks. At the same time, the uniform microstructure allows the thermal expansion behavior to change continuously along the thickness direction, further alleviating the concentration of thermal stress during temperature changes, thereby improving the thermal shock resistance of the component.
[0020] Preferably, the cladding deposition conditions for the corrosion-resistant ceramic layer in step S2 are as follows: the metal powder supply system is turned off, only the ceramic powder supply system is turned on, the laser power is 400-500W, the scanning speed is 400-800mm / s, and the layer thickness is 20-40μm.
[0021] The cladding deposition conditions for corrosion-resistant ceramic layers are achieved by shutting down the metal powder supply system and turning on only the ceramic powder supply system, and by matching the laser power, scanning speed and layer thickness, so that the ceramic powder can be completely melted and uniformly spread under sufficient energy input. The high laser power and moderate scanning speed ensure the full melting of the high-melting-point ceramic phase. The molten pool expels internal gases within an appropriate time and achieves metallurgical bonding between ceramic particles, reducing porosity and incomplete fusion defects, improving the density and cohesive strength of the ceramic layer, and thus enhancing the tensile strength of the component. The dense ceramic structure makes it difficult for corrosive media to penetrate inward along pores or grain boundaries. At the same time, the passivation layer formed by yttrium oxide-based ceramics in a fluorine-containing environment remains intact and continuous, enhancing the surface's resistance to chemical erosion, thereby improving the component's corrosion resistance. The thinner layer thickness allows each ceramic layer to obtain a fine grain structure during solidification. The fine grain structure can release thermal stress more uniformly under drastic temperature changes, reducing the initiation and propagation of microcracks. Meanwhile, the continuity of the ceramic layer and the gradient transition layer ensures a smooth transition in thermal expansion behavior, further alleviating interfacial thermal stress, thereby improving the component's thermal shock resistance.
[0022] Preferably, the hot isostatic pressing treatment in step S3 is performed at 1100-1300℃ and 150-200MPa for 2-4 hours.
[0023] By applying isotropic pressure to the integrally formed green compact under high temperature and pressure, the residual pores inside the material undergo plastic collapse and metallurgical bonding, improving the material's density and microstructure uniformity. This eliminates microscopic defects that may remain from the laser cladding process, transforming the interfacial bonding between the high-strength metal layer, gradient transition layer, and corrosion-resistant ceramic layer from mechanical interlocking to diffusion bonding. The increased interfacial bonding strength makes the component less prone to interlayer delamination under tensile loads, thereby improving the component's tensile strength. The densified microstructure also creates channels for corrosive media to penetrate along grain boundaries or pores. The components are effectively sealed, and the high temperature and pressure promote the uniform distribution of alloying elements and the purification of ceramic phase grain boundaries, thus maintaining the integrity of the oxide film on the surface of the metal layer and the passivation film on the ceramic layer, thereby improving the corrosion resistance of the components. The high temperature treatment releases the residual stress inside the material and alleviates the concentration of micro-stress caused by the difference in thermal expansion in the gradient transition layer. At the same time, the dense and uniform structure makes the heat conduction and thermal expansion behavior more coordinated, and the distribution of thermal stress inside the material becomes more uniform when the temperature changes drastically, which inhibits the initiation and propagation of hot cracks, thereby improving the thermal shock resistance of the components.
[0024] Secondly, this application provides a corrosion-resistant component for semiconductor devices using graded functional materials, employing the following technical solution: A process for fabricating corrosion-resistant semiconductor device components with gradient functional materials.
[0025] The corrosion-resistant semiconductor device components prepared according to the above-described process exhibit a continuously varying ratio of metallic and ceramic phases within the gradient transition layer. This allows for a smooth transition in the coefficient of thermal expansion along the thickness direction, resulting in uniform release of thermal stress during temperature changes. This reduces the risk of crack initiation and propagation, thereby improving the component's thermal shock resistance. The solid solution strengthening of alloying elements in the high-strength metal layer and the gradient bonding between the metal and ceramic layers enable effective load transfer between layers, preventing interface delamination and enhancing the component's tensile strength. The corrosion-resistant ceramic layer covers the inner surface of the component, resisting fluorine-containing plasma erosion due to the chemical inertness of yttrium oxide-based ceramics. Simultaneously, the dense gradient transition layer blocks the penetration path of corrosive media into the metal substrate, protecting the interface between the metal and ceramic layers from erosion and further enhancing the component's corrosion resistance.
[0026] In summary, this application includes at least one of the following beneficial technical effects: By sequentially depositing a high-strength metal layer, a gradient transition layer, and a corrosion-resistant ceramic layer along the thickness direction of the component from the outside to the inside, and using an independent powder supply system for layer-by-layer cladding deposition, a spatial gradient transition of material components is achieved. The high-strength metal layer serves as the substrate to bear structural loads, improving the tensile strength of the component. The corrosion-resistant ceramic layer directly contacts the corrosive environment, resisting media erosion with its stable chemical properties, thus improving the component's corrosion resistance. The gradient transition layer, through continuous variation in the ratio of metal to ceramic powder, alleviates the thermal stress caused by the difference in thermal expansion coefficients between the metal and ceramic, improving the component's thermal shock resistance under conditions of drastic temperature changes, while eliminating abrupt performance changes between layers. This allows the three-layer structure to form a synergistically reinforced whole, comprehensively improving the component's mechanical strength and environmental stability.
[0027] Niobium introduced into the metal powder partially dissolves in the nickel matrix during laser cladding, resulting in solid solution strengthening, while partially combines with nickel to form a dispersed intermetallic compound precipitate phase. This precipitation strengthening mechanism enhances the tensile strength of the metal layer. Yttrium, as an active element, is enriched at grain boundaries and phase interfaces. By purifying grain boundary impurities and refining the solidification structure, it improves the material's density and interfacial bonding strength. Simultaneously, yttrium preferentially oxidizes to form a thermodynamically stable oxide film, enhancing the adhesion and density of the surface oxide film, thereby improving the component's corrosion resistance. The synergistic effect of niobium and yttrium makes the alloy structure more uniform and refined, improving the grain boundary strengthening effect. This helps to hinder grain boundary slip and crack propagation at high temperatures, allowing the metal layer to maintain structural integrity during temperature changes, thus improving the component's thermal shock resistance. Detailed Implementation
[0028] This application discloses a corrosion-resistant component for semiconductor devices with graded functional materials and its fabrication process. Unless otherwise specified, all raw materials used in this application are commercially available. The following detailed description, in conjunction with embodiments, further illustrates this application: Example
[0029] S1. Establish a three-dimensional model of the corrosion-resistant component of the semiconductor equipment. The corrosion-resistant component of the semiconductor equipment is set with a high-strength metal layer, a gradient transition layer and a corrosion-resistant ceramic layer from the outside to the inside along the thickness direction. Discretize the three-dimensional model into several printing layers and set the material ratio of each layer. S2. Prepare metal powder and ceramic powder; the metal powder comprises the following components by mass percentage: 20% Cr, 14% Mo, 3% W, with the balance being Ni and unavoidable impurities; the ceramic powder comprises the following components by mass percentage: 10% YOF, 15% Al2O3, with the balance being Y2O3; the high-strength metal layer is prepared from the metal powder, the corrosion-resistant ceramic layer is prepared from the ceramic powder, and the gradient transition layer is prepared from a mixture of metal powder and ceramic powder; the metal powder and ceramic powder are placed in two independent powder feeding systems, and the powder feeding ratio of metal powder to ceramic powder is adjusted by an algorithm, and the high-strength metal layer, gradient transition layer, and corrosion-resistant ceramic layer are deposited layer by layer to obtain an integrated green body; the cladding deposition conditions for the high-strength metal layer are: only the metal powder is turned on. The system uses a powder feeding system with a laser power of 300W, a scanning speed of 800mm / s, and a layer thickness of 30μm. For the gradient transition layer, as the number of printed layers increases, the proportion of ceramic powder gradually increases, causing the ceramic phase volume fraction to gradually rise from 0% to 100% in a 3% increment per layer. Simultaneously, the proportion of metal powder is correspondingly reduced. The cladding deposition conditions for the gradient transition layer are: laser power linearly increases from 300W to 400W with increasing ceramic content, scanning speed linearly decreases from 800mm / s to 400mm / s, and layer thickness is 30μm. The cladding deposition conditions for the corrosion-resistant ceramic layer are: the metal powder feeding system is turned off, only the ceramic powder feeding system is turned on, laser power is 400W, scanning speed is 400mm / s, and layer thickness is 20μm.
[0030] S3. The integrally formed green blank is subjected to hot isostatic pressing. The hot isostatic pressing conditions are to hold the temperature and pressure at 1100℃ and 150MPa for 4 hours, and then perform surface precision machining to make the surface roughness Ra≤0.4μm of the part, so as to obtain the corrosion-resistant part of the semiconductor equipment. Example
[0031] S1. Establish a three-dimensional model of the corrosion-resistant component of the semiconductor equipment. The corrosion-resistant component of the semiconductor equipment is set with a high-strength metal layer, a gradient transition layer and a corrosion-resistant ceramic layer from the outside to the inside along the thickness direction. Discretize the three-dimensional model into several printing layers and set the material ratio of each layer. S2. Prepare metal powder and ceramic powder; the metal powder comprises the following components by mass percentage: 22% Cr, 13% Mo, 2% W, with the balance being Ni and unavoidable impurities; the ceramic powder comprises the following components by mass percentage: 20% YOF, 5% Al2O3, with the balance being Y2O3; the high-strength metal layer is prepared from the metal powder, the corrosion-resistant ceramic layer is prepared from the ceramic powder, and the gradient transition layer is prepared from a mixture of metal powder and ceramic powder; the metal powder and ceramic powder are placed in two independent powder feeding systems, and the powder feeding ratio of metal powder to ceramic powder is adjusted by an algorithm, and the high-strength metal layer, gradient transition layer, and corrosion-resistant ceramic layer are deposited layer by layer to obtain an integrated green body; the cladding deposition condition of the high-strength metal layer is that only the metal powder is turned on. The final powder supply system has a laser power of 400W, a scanning speed of 1200mm / s, and a layer thickness of 50μm. For the gradient transition layer, as the number of printed layers increases, the proportion of ceramic powder gradually increases, causing the ceramic phase volume fraction to gradually rise from 0% to 100% in increments of 5% per layer. Simultaneously, the proportion of metal powder is correspondingly reduced. The cladding deposition conditions for the gradient transition layer are: laser power linearly increases from 400W to 500W with increasing ceramic content, scanning speed linearly decreases from 1200mm / s to 800mm / s, and layer thickness is 50μm. The cladding deposition conditions for the corrosion-resistant ceramic layer are: the metal powder supply system is turned off, only the ceramic powder supply system is turned on, laser power is 500W, scanning speed is 800mm / s, and layer thickness is 40μm.
[0032] S3. The integrally formed green blank is subjected to hot isostatic pressing. The hot isostatic pressing conditions are to hold the temperature and pressure at 1300℃ and 200MPa for 2 hours, and then perform surface precision machining to make the surface roughness Ra≤0.4μm of the part, so as to obtain the corrosion-resistant part of the semiconductor equipment. Example
[0033] S1. Establish a three-dimensional model of the corrosion-resistant component of the semiconductor equipment. The corrosion-resistant component of the semiconductor equipment is set with a high-strength metal layer, a gradient transition layer and a corrosion-resistant ceramic layer from the outside to the inside along the thickness direction. Discretize the three-dimensional model into several printing layers and set the material ratio of each layer. S2. Prepare metal powder and ceramic powder; the metal powder comprises the following components by mass percentage: 21% Cr, 13.5% Mo, 2.5% W, with the balance being Ni and unavoidable impurities; the ceramic powder comprises the following components by mass percentage: 15% YOF, 10% Al2O3, with the balance being Y2O3; the high-strength metal layer is prepared from the metal powder, the corrosion-resistant ceramic layer is prepared from the ceramic powder, and the gradient transition layer is prepared from a mixture of metal powder and ceramic powder; the metal powder and ceramic powder are placed in two independent powder feeding systems, and the powder feeding ratio of metal powder to ceramic powder is adjusted by an algorithm, and the high-strength metal layer, gradient transition layer, and corrosion-resistant ceramic layer are deposited layer by layer to obtain an integrated green body; the cladding deposition condition of the high-strength metal layer is only turned on. The metal powder supply system has a laser power of 350W, a scanning speed of 1000mm / s, and a layer thickness of 40μm. For the gradient transition layer, as the number of printed layers increases, the proportion of ceramic powder gradually increases, causing the ceramic phase volume fraction to gradually rise from 0% to 100% in a 4% increment per layer. Simultaneously, the proportion of metal powder is correspondingly reduced. The cladding deposition conditions for the gradient transition layer are: laser power linearly increases from 350W to 450W with increasing ceramic content, scanning speed linearly decreases from 1000mm / s to 600mm / s, and layer thickness is 40μm. The cladding deposition conditions for the corrosion-resistant ceramic layer are: the metal powder supply system is turned off, only the ceramic powder supply system is turned on, laser power is 450W, scanning speed is 600mm / s, and layer thickness is 30μm.
[0034] S3. The integrally formed green blank is subjected to hot isostatic pressing (HIP) treatment. The HIP treatment conditions are to hold the temperature and pressure at 1200℃ and 175MPa for 3 hours, and then perform surface precision machining to make the surface roughness Ra≤0.4μm of the part, so as to obtain the corrosion-resistant part of the semiconductor equipment. Example
[0035] Example 4 is based on Example 3. The only difference between Example 4 and Example 3 is that in step S2 of Example 4, the proportion of ceramic powder fed into the gradient transition layer gradually increases with the increase of the number of printing layers, so that the volume fraction of ceramic phase gradually increases from 0% to 100% in a gradient of 10% per layer, while the proportion of metal powder fed into the gradient is reduced accordingly. Example
[0036] Example 5 is based on Example 3. The only difference between Example 5 and Example 3 is that in Example 5, the cladding deposition conditions of the gradient transition layer in step S2 are a laser power of 350W and a scanning speed of 1000mm / s. Example
[0037] Example 6 is based on Example 3. The only difference between Example 6 and Example 3 is that in Example 6, the cladding deposition conditions of the gradient transition layer in step S2 are a laser power of 450W and a scanning speed of 600mm / s. Example
[0038] Example 7 is based on Example 3. The only difference between Example 7 and Example 3 is that in Example 7, the metal powder also includes 0.5% Nb and 0.3% Y. The metal powder includes the following components in mass percentage: 21% Cr, 13.5% Mo, 2.5% W, 0.5% Nb, 0.3% Y, with the balance being Ni and unavoidable impurities. Example
[0039] Example 8 is based on Example 3. The only difference between Example 8 and Example 3 is that the metal powder in Example 8 also includes 1% Nb and 0.5% Y. The metal powder includes the following components in mass percentage: 21% Cr, 13.5% Mo, 2.5% W, 1% Nb, 0.5% Y, with the balance being Ni and unavoidable impurities. Example
[0040] Example 9 is based on Example 3. The only difference between Example 9 and Example 3 is that in Example 9, the metal powder also includes 0.75% Nb and 0.4% Y. The metal powder includes the following components in mass percentage: 21% Cr, 13.5% Mo, 2.5% W, 0.75% Nb, 0.4% Y, with the balance being Ni and unavoidable impurities. Example
[0041] Example 10 is based on Example 3. The only difference between Example 10 and Example 3 is that in Example 10, the metal powder also includes 0.75% Nb. The metal powder includes the following components in mass percentage: 21% Cr, 13.5% Mo, 2.5% W, 0.75% Nb, with the balance being Ni and unavoidable impurities. Example
[0042] Example 11 is based on Example 3. The only difference between Example 11 and Example 3 is that in Example 11, the metal powder also includes 0.4% Y. The metal powder includes the following components by mass percentage: 21% Cr, 13.5% Mo, 2.5% W, 0.4% Y, with the balance being Ni and unavoidable impurities.
[0043] Comparative Example 1 No gradient transition layer is set in Comparative Example 1.
[0044] S1. Establish a three-dimensional model of the corrosion-resistant component of the semiconductor equipment. The corrosion-resistant component of the semiconductor equipment is set with a high-strength metal layer and a corrosion-resistant ceramic layer from the outside to the inside along the thickness direction. Discretize the three-dimensional model into several printing layers and set the material ratio of each layer. S2. Prepare metal powder and ceramic powder; the metal powder includes the following components by mass percentage: 21% Cr, 13.5% Mo, 2.5% W, with the balance being Ni and unavoidable impurities; the ceramic powder includes the following components by mass percentage: 15% YOF, 10% Al2O3, with the balance being Y2O3; the high-strength metal layer is prepared from the metal powder, and the corrosion-resistant ceramic layer is prepared from the ceramic powder; the metal powder and ceramic powder are placed in two independent powder supply systems, and the powder feeding ratio of the metal powder and ceramic powder is adjusted by an algorithm, and the high-strength metal layer and the corrosion-resistant ceramic layer are deposited layer by layer to obtain an integrated green body; the cladding deposition conditions for the high-strength metal layer are: only the metal powder supply system is turned on, the laser power is 350W, the scanning speed is 1000mm / s, and the layer thickness is 40μm; the cladding deposition conditions for the corrosion-resistant ceramic layer are: the metal powder supply system is turned off, only the ceramic powder supply system is turned on, the laser power is 450W, the scanning speed is 600mm / s, and the layer thickness is 30μm.
[0045] S3. The integrally formed green blank is subjected to hot isostatic pressing (HIP) treatment. The HIP treatment conditions are to hold the temperature and pressure at 1200℃ and 175MPa for 3 hours, and then perform surface precision machining to make the surface roughness Ra≤0.4μm of the part, so as to obtain the corrosion-resistant part of the semiconductor equipment.
[0046] (1) Select GB / T 10125-2021 Artificial Atmosphere Corrosion Test Salt Spray Test as the standard, prepare a flat sample with a size of 50mm×50mm×5mm, and record the weight; test solution: 5% NaCl solution, pH adjusted to 7.0, spray continuously for 2h at 35℃, spray pressure 0.1MPa; dry for 4h at a relative humidity below 60%; wet for 2h at a relative humidity above 95%, the total test duration is 480h, take out the sample, rinse with deionized water to remove corrosion products, dry and weigh again, calculate the mass loss per unit area (mg / cm²), and record the results in Table 1.
[0047] (2) Using GB / T 37246-2018 Test Method for Thermal Shock Resistance of Fine Ceramics as the standard, 10 standard bending specimens of 3mm×4mm×40mm were prepared. First, the room temperature bending strength of 5 specimens was measured as the initial strength σ0. Then, the other 5 specimens were placed in a high temperature furnace and heated to 400℃ at 10℃ / min and kept at that temperature for 15min. They were then quickly taken out and placed in a flowing water bath at 20℃ for quenching and kept for 5min. After drying, the bending strength σ after thermal shock was measured, and the strength retention rate (σ / σ0×100%) was calculated. The average value was taken after measurement, and the results were recorded in Table 1.
[0048] (3) Select GB / T 228.1 Metallic materials, tensile testing - Part 1: Test method at room temperature as the standard, and apply tensile force continuously on an electronic universal testing machine at an ambient temperature of 23℃, a yield strain rate of 0.00025 s⁻¹, and a tensile strain rate of 0.0067 s⁻¹ until fracture. Record the tensile strength. Prepare three samples for each specimen, and take the average value after measurement. Record the results in Table 1.
[0049] Table 1. Test results of corrosion resistance, thermal shock resistance, and tensile strength. Test results <![CDATA[Mass loss (mg / cm 2 )]]> Strength retention rate (%) Tensile strength (MPa) Example 1 0.68 86.5 485 Example 2 0.72 85.2 472 Example 3 0.61 88.3 512 Example 4 1.25 72.6 398 Example 5 1.08 80.1 425 Example 6 0.95 82.4 448 Example 7 0.48 90.2 538 Example 8 0.45 91.5 545 Example 9 0.42 92.8 558 Example 10 0.55 89.6 528 Example 11 0.52 90.1 522 Comparative Example 1 1.56 65.4 312 As shown in Table 1, the mass loss in Examples 1-3 was 0.72 mg / cm³. 2 The strength retention rate is above 85.2%, and the tensile strength is above 472 MPa, which shows that the corrosion-resistant parts prepared in this application have good corrosion resistance, thermal shock resistance and tensile strength.
[0050] As shown in Table 1, the only difference between Example 4 and Example 3 is that the gradient step size in Example 4 is too large, which leads to thermal stress concentration, resulting in microcracks, a significant decrease in thermal shock resistance and strength, and an increase in corrosion paths.
[0051] As shown in Table 1, the only difference between Examples 5 and 6 and Example 3 is that in Example 5, the gradient layer is fixed at low power and high speed, and the ceramic part has insufficient energy, resulting in unfused defects, reduced density and bonding strength; in Example 6, the gradient layer is fixed at high power and low speed, and the metal part is overheated, resulting in coarse grains and decreased performance.
[0052] As shown in Table 1, the difference between Examples 7-11 and Example 3 is only that: in Examples 7-9, Nb and Y are synergistically compounded, and the effects of fine grain strengthening and anti-oxidation improve the overall performance; Examples 10 and 11 use only a single element, lack synergistic effect, and the performance improvement effect is reduced.
[0053] As shown in Table 1, the only difference between Comparative Example 1 and Example 3 is that there is no transition layer in Comparative Example 1, and the metal and ceramic are directly bonded. The mismatch in thermal expansion coefficients leads to large interfacial stress, weak bonding, and the worst overall performance.
[0054] This specific embodiment is merely an explanation of this application and is not intended to limit it. Based on the above description, those skilled in the art can make various changes and modifications without departing from the technical concept of this application. The technical scope of this application is not limited to the contents of the specification but must be determined according to the scope of the claims.
Claims
1. A fabrication process for corrosion-resistant components of semiconductor devices using graded functional materials, characterized in that: Includes the following steps: S1. Establish a three-dimensional model of the corrosion-resistant component of the semiconductor device. The corrosion-resistant component of the semiconductor device is provided with a high-strength metal layer, a gradient transition layer and a corrosion-resistant ceramic layer in sequence from the outside to the inside along the thickness direction. Discretize the three-dimensional model into several printing layers and set the material ratio of each layer. S2. Prepare metal powder and ceramic powder; the high-strength metal layer is prepared from metal powder, the corrosion-resistant ceramic layer is prepared from ceramic powder, and the gradient transition layer is prepared from a mixture of metal powder and ceramic powder; place the metal powder and ceramic powder in two independent powder supply systems, adjust the powder feeding ratio of metal powder and ceramic powder through an algorithm, and deposit the high-strength metal layer, gradient transition layer and corrosion-resistant ceramic layer layer by layer to obtain an integrated green body; S3. The integrated green blank is subjected to hot isostatic pressing and surface precision machining to obtain corrosion-resistant components for semiconductor equipment.
2. The fabrication process of a corrosion-resistant component for a semiconductor device with graded functional materials according to claim 1, characterized in that: The metal powder in step S2 comprises the following components by mass percentage: 20-22% Cr, 13-14% Mo, 2-3% W, with the balance being Ni and unavoidable impurities.
3. The fabrication process of a corrosion-resistant component for a semiconductor device with graded functional materials according to claim 2, characterized in that: The metal powder also includes 0.5-1% Nb and 0.3-0.5% Y.
4. The fabrication process of a corrosion-resistant component for a semiconductor device with graded functional materials according to claim 1, characterized in that: The cladding deposition conditions for the high-strength metal layer in step S2 are as follows: only the metal powder supply system is turned on, the laser power is 300-400W, the scanning speed is 800-1200mm / s, and the layer thickness is 30-50μm.
5. The fabrication process of a corrosion-resistant component for a semiconductor device with graded functional materials according to claim 4, characterized in that: The ceramic powder in step S2 comprises the following components by mass percentage: 10-20% YOF, 5-15% Al2O3, and the balance being Y2O3.
6. The fabrication process of a corrosion-resistant component for a semiconductor device with graded functional materials according to claim 5, characterized in that: In step S2, as the number of printed layers increases, the proportion of ceramic powder fed into the gradient transition layer gradually increases, so that the volume fraction of the ceramic phase gradually rises from 0% to 100% with a gradient of 3-5% per layer, while the proportion of metal powder fed into the gradient layer is reduced accordingly.
7. The fabrication process of a corrosion-resistant component for a semiconductor device with graded functional materials according to claim 6, characterized in that: In step S2, the cladding deposition conditions for the gradient transition layer are as follows: the laser power increases linearly from 300-400W to 400-500W as the ceramic content increases, the scanning speed decreases linearly from 800-1200mm / s to 400-800mm / s, and the layer thickness is 30-50μm.
8. The fabrication process of a corrosion-resistant component for a semiconductor device with graded functional materials according to claim 7, characterized in that: In step S2, the cladding deposition conditions for the corrosion-resistant ceramic layer are as follows: the metal powder supply system is turned off, only the ceramic powder supply system is turned on, the laser power is 400-500W, the scanning speed is 400-800mm / s, and the layer thickness is 20-40μm.
9. The fabrication process of a corrosion-resistant component for a semiconductor device with graded functional materials according to claim 1, characterized in that: The hot isostatic pressing (HIP) treatment in step S3 is performed at 1100-1300℃ and 150-200MPa for 2-4 hours.
10. A corrosion-resistant component for a semiconductor device, prepared by the process described in any one of claims 1-9, using a graded functional material.