Super-high-temperature-resistant nickel-based ceramic composite coating process

Abstract

The invention belongs to the technical field of surface engineering, and particularly relates to a super-high-temperature-resistant nickel-based ceramic composite coating process which comprises the following steps: (1) pretreating an aluminum base material; (2) preparation of a silicon-aluminum transition layer: coating the surface of the pretreated aluminum substrate with silica gel, and performing curing, pore forming and anaerobic high-temperature calcination to form the silicon-aluminum transition layer with a porous structure; (3) nickel-based ceramic layer electroplating: taking the silicon-aluminum transition layer as a substrate, and carrying out electroplating codeposition by adopting a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite coating; and (4) low-temperature annealing is conducted, and the super-high-temperature-resistant nickel-based ceramic composite coating is achieved.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of surface engineering, and in particular, relates to a super-high-temperature-resistant nickel-based ceramic composite coating process. BACKGROUND

[0002] Surface treatment technology is an important guarantee for the service performance and reliability of industrial equipment in extreme environments such as high temperature, high load, and strong corrosion. Among many surface treatment schemes, nickel-based ceramic composite coating technology has attracted widespread attention and application in the industry due to its ability to organically combine the toughness and electrical conductivity of metal matrix with the high hardness, wear resistance, and excellent high-temperature stability of ceramic particles, thus exhibiting excellent comprehensive performance. The core concept of this technology is to build a composite functional coating with nickel or nickel alloy as the continuous phase and high-hardness ceramic particles such as silicon carbide and aluminum oxide as the dispersed reinforcing phase on the surface of metal or non-metal substrates through co-deposition process.

[0003] Specifically, the current mainstream preparation method in the industry is composite electrodeposition technology. In a specific electrolyte system containing nickel salt, conductive salt, pH buffer, and suspended ceramic particles, the workpiece to be processed is used as the cathode, and an external electric field is applied to drive the reduction reaction of nickel ions in the plating solution on the cathode surface, resulting in the deposition and growth of a metal nickel layer. At the same time, under the action of mechanical stirring or ultrasonic dispersion, ceramic particles uniformly suspended in the plating solution are carried to the cathode surface and mechanically embedded or "riveted" into the growing coating layer along with the continuous deposition of nickel metal, ultimately forming a metal matrix composite coating with a dense structure and uniform distribution of ceramic particles. This preparation method has successfully solved the shortcomings of traditional single metal coatings in hardness and wear resistance, and has provided effective surface protection for a large number of engineering parts due to its high process maturity, relatively simple equipment requirements, controllable cost, and ability to achieve rapid deposition of large areas.

[0004] However, with the continuous development of related technologies and the increasingly stringent requirements for performance indicators in application scenarios, especially in the field of lightweight and high-temperature resistance, for example, applying such coatings to lightweight substrates such as aluminum alloys for operation in high-temperature environments, some inherent characteristics of the above-mentioned traditional composite electroplating technology at the principle level gradually reveal its fundamental limitations when facing new challenges. The reason lies in the fact that the successful application of this technology implies a prerequisite that the coating and the substrate have good physical and chemical compatibility. When the substrate is traditional steel, copper, or other materials, the difference in thermal physical properties between the nickel-based coating and the substrate is within a controllable range. However, when the substrate is replaced by aluminum alloy with a very high thermal expansion coefficient (about 23x10 -6 / K), while the thermal expansion coefficient of the nickel matrix (about 13x10 -6 / K) and ceramic particles (such as SiC, about 4x10-6 When the thermal expansion coefficients of the aluminum substrate and the nickel-based ceramic coating (CTE) are much lower than that of the aluminum substrate, a deep internal contradiction is highlighted. Under high-temperature working conditions, especially when experiencing frequent temperature rise and fall cycles, the huge mismatch in thermal expansion coefficients between the substrate and the coating will generate extremely strong alternating thermal stress at the interface. This stress, which is a compressive stress when the temperature rises and a tensile stress when the temperature falls, is extremely prone to inducing the initiation and propagation of microcracks at the fragile physical bonding interface under repeated action, and ultimately leading to peeling, bubbling and even catastrophic peeling failure of the coating. Traditional substrate pretreatment, such as simple mechanical polishing or chemical zinc immersion, although can increase the mechanical locking force of the interface to some extent, does not fundamentally change the sudden change in thermal physical properties of the materials on both sides of the interface, and cannot fundamentally alleviate or release the huge interfacial stress generated by the CTE mismatch, so it has little effect in ultra-high temperature applications.

[0005] Therefore, how to effectively alleviate the interfacial thermal stress generated between the lightweight metal substrate (such as aluminum alloy) and the nickel-based ceramic composite coating due to the significant difference in thermal physical properties (especially the thermal expansion coefficient) under high-temperature working conditions, and construct a stable interfacial structure that can achieve stress relief and gradient transition, thereby fundamentally improving the bonding strength and service life of the composite coating in the working environment of the phosphoric acid industry, has become a key challenge and technical problem to be solved for those skilled in the art. SUMMARY

[0006] To solve the above problems, the present application provides a super-high-temperature-resistant nickel-based ceramic composite coating process. Instead of using a traditional single physical bonding interface, the process constructs a composite interface system with a gradient transition of thermal expansion coefficient and stress dissipation capacity between the aluminum substrate and the final nickel-based ceramic functional coating through the synergistic action of multiple steps and multiple mechanisms, which is composed of an in-situ grown layer, a covalently bonded porous buffer layer and a mechanically locked layer. The system realizes the fundamental improvement of the interfacial bonding force through multiple ways such as chemical bonding, mechanical locking and subsequent diffusion metallurgical bonding formed by heat treatment, and effectively absorbs and relieves the interfacial stress generated during thermal cycling by using the special porous structure of the intermediate layer, thereby ensuring the structural integrity and long-term service reliability of the composite coating in the super-high-temperature environment.

[0007] To achieve the above purpose, the present application provides the following technical scheme: A super-high-temperature-resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: the aluminum substrate is sequentially subjected to surface roughening, anodic oxidation and oxygen ion bombardment activation treatment to obtain a pretreated aluminum substrate with a roughened surface and high activity; Step (2) Preparation of the silicon-aluminum transition layer: Silicon gel is coated on the surface of the pretreated aluminum substrate, and is cured, pore-formed and calcined at high temperature in an oxygen-free atmosphere to form a silicon-aluminum transition layer containing a porous structure; Step (3) Electroplating of the nickel-based ceramic layer: The silicon-aluminum transition layer is used as a substrate, and a nickel-based electroplating solution containing ceramic particles is used for electroplating co-deposition to obtain a nickel-based ceramic composite plating layer. Step (4) Low-temperature annealing: The nickel-based ceramic composite plating layer is annealed in an oxygen-free atmosphere to eliminate internal stress and enhance the interface bonding force, thereby realizing an ultra-high-temperature nickel-based ceramic composite plating layer.

[0008] The technical mechanism of the super-high-temperature nickel-based ceramic composite coating scheme is essentially to build a gradient interface system of "aluminum substrate-transition layer-nickel-based ceramic layer" through component design and process coordination. The transition layer plays a key role in subsequent annealing and dynamically adjusts the difference in the expansion coefficient of the two materials. From the component point of view, the high-activity microstructure is formed on the surface of the aluminum substrate after pretreatment (roughening and oxygen ion activation), providing "anchor points" for the mechanical embedding and chemical bonding of the transition layer. The silica gel formula of the silicon-aluminum transition layer mainly uses silica sol, and the chemical bonding of silicon and aluminum is achieved through KH560 coupling agent (-OH and epoxy group reaction). The pore-forming agent PMMA forms a porous SiO2-Al2O3 structure after calcination, and the porosity and elastic modulus are naturally between aluminum (high CTE, low modulus) and the nickel-based ceramic layer (low CTE, high modulus), forming a natural "buffer zone" prototype. From the process point of view, annealing (450-500°C in an oxygen-free atmosphere) is the core link for the transition layer to adjust the expansion coefficient: on the one hand, annealing promotes the diffusion of Al atoms in the aluminum substrate to the transition layer, reacts with the residual SiO2 network of the silica sol to form Al-O bonding, and at the same time, the Ni atoms in the nickel-based ceramic layer migrate to the transition layer, react with SiO2 or the residual PMMA to form Ni-Si bonding. This two-way diffusion makes the structure of the transition layer more dense and the pore distribution more uniform, and the overall thermal expansion coefficient is "flattened" to the intermediate value of aluminum and the nickel-based ceramic layer. On the other hand, the porous structure of the transition layer is partially closed during annealing, reducing the stress concentration points between the interfaces and further relieving the direct mismatch of the high CTE of aluminum and the low CTE of the nickel-based ceramic layer. Finally, the transition layer becomes a "flexible interface" connecting aluminum and the nickel-based ceramic layer through chemical bonding between components and structural optimization after annealing, effectively adjusting the thermal expansion difference between the two, laying the foundation for the overall super-high-temperature and strong bonding performance of the coating. In the nickel-based ceramic layer, the SiC particles (high melting point, low CTE) co-deposited by electroplating are embedded in the nickel matrix, and the composite structure of rigid particles and plastic nickel matrix itself has the ability to resist thermal stress. Annealing further promotes the interfacial diffusion of Ni and SiC (such as the formation of a small amount of Ni-Si solid solution), strengthening the high-temperature stability of the layer. Each component and process is linked, and finally realizes the continuous and coordinated thermal-mechanical matching from the aluminum substrate to the nickel-based ceramic layer, achieving the comprehensive performance of super-high-temperature and corrosion resistance.

[0009] As preferred, the surface roughening in step (1) is performed by anodic oxidation, with the following parameters: electrolyte of 120-150 g / L oxalic acid, voltage of 12-15 V, oxidation at room temperature for 12-15 min, to form a porous Al2O3 layer with a thickness of 25-30 μm and a surface roughness Ra of 3.5-5 μm.

[0010] As preferred, the oxygen ion bombardment activation in step (1) is performed by a plasma device with the following process parameters: working gas Ar / O2 (volume ratio 9:1), power 100-120 W, and processing time 8-10 min.

[0011] As preferred, the formula of the silica gel in step (2) is as follows (mass fraction): Silica sol (SiO2 particle size 20-50 nm, content 30%): 55-60%; Deionized water: 28-35%; γ-glycidoxypropyltrimethoxysilane: 3-4%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10-15%; Toughening agent polydimethylsiloxane: 2-3%.

[0012] As preferred, the wet grinding thickness after coating in step (2) is 90-110 μm, and the curing process is as follows: constant temperature drying at 60°C for 2.5 h, post-curing at 80°C for 1.5 h, and promoting the hydrolysis and condensation of KH560; the pore-forming condition is calcination at 450-500°C for 2 h, and PMMA is decomposed into CO2 and H2O to escape, forming a porous silicon-aluminum transition layer with a porosity of 45-55% and a pore size of 2-6 μm.

[0013] As preferred, the nickel-based electroplating solution in step (3) has the following mass concentration components: Nickel sulfate: 250-280 g / L; Nickel chloride: 45-55 g / L; Boric acid: 35-40 g / L; Sodium dodecyl sulfate: 0.04-0.06 g / L; Leveling agent sodium saccharin: 0.08-0.12 g / L; Ceramic particles (SiC, particle size 1-5 μm, surface treated with silane coupling agent): 20-40 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1-3 g / L (used to improve the dispersibility of SiC).

[0014] As preferred, the electroplating parameters in step (3) are as follows: current density 2.5-3 A / dm 2 , temperature 52-55°C, pH 4.8-5.0 (boric acid buffer), and electroplating time 12-15 min.

[0015] Preferably, the low-temperature annealing process in step (4) is annealing at 450-500°C for 1.5h in a nitrogen / argon mixed atmosphere (oxygen content ≤10ppm) to eliminate the residual stress of electroplating and promote the interface diffusion between the nickel matrix and the SiC particles, while further adjusting the expansion coefficients.

[0016] Compared with the prior art, the present application has the following advantages: 1. The high-temperature service reliability is significantly improved by the gradient buffer mechanism of the silicon-aluminum transition layer. The present application adopts a silicon-aluminum transition layer to form a buffer zone, the thermal expansion coefficient of which is naturally between that of aluminum and the nickel-based ceramic layer, and the pretreatment and annealing process further adjusts the expansion difference between the two, effectively reducing the interface thermal stress and avoiding the interface fracture problem at high temperature.

[0017] 2. The adaptability to strong corrosive environment is strengthened by the dual mechanism of transition layer blocking and composite layer corrosion resistance. The porous SiO2 network of the silicon-aluminum transition layer can physically block the penetration of corrosive medium to the aluminum matrix, while the high-stability Ni matrix in the nickel-based ceramic layer and the SiC particles (chemically inert) cooperate to form a metal-ceramic composite corrosion-resistant layer, significantly reducing the erosion rate of the plating layer by the corrosive medium, thereby realizing long-term stable service in high-temperature strong corrosive environment. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 The boxed area in the figure is the silicon-aluminum transition layer. DETAILED DESCRIPTION

[0019] It should be noted that the embodiments and features in the embodiments can be combined with each other without conflict. In order to enable those skilled in the art to better understand the present application, the technical solutions in the embodiments of the present application will be described clearly and completely below in conjunction with the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor should be within the scope of protection of the present application.

[0020] OVERALL EMBODIMENT A super-high-temperature nickel-based ceramic composite plating process, comprising the following steps: Step (1) Pretreatment of aluminum substrate: the aluminum substrate is subjected to surface roughening, anodic oxidation and oxygen ion bombardment activation treatment in sequence to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation, and the specific parameters are as follows: electrolyte is 120-150 g / L oxalic acid, voltage is 12-15 V, and oxidation is performed at room temperature for 12-15 min to form a porous Al2O3 layer with a thickness of 25-30 μm and a surface roughness Ra of 3.5-5 μm; The oxygen ion bombardment activation is performed by a plasma device, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100-120 W, and processing time is 8-10 min; Step (2) preparation of the silicon-aluminum transition layer: the silicon gel is coated on the surface of the pretreated aluminum substrate, and is cured, pore-formed and calcined at high temperature in an oxygen-free atmosphere to form a silicon-aluminum transition layer containing a porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%-60%; Deionized water: 28%-35%; γ-glycidyl ether propyltrimethoxysilane: 3%-4%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%-15%; Toughening agent polydimethylsiloxane: 2%-3%; The wet grinding thickness after coating is 90-110 μm, the curing process is as follows: constant temperature drying at 60 ℃ for 2.5 h, post-curing at 80 ℃ for 1.5 h to promote the hydrolysis and condensation of KH560, and the pore-forming condition is calcination at 450-500 ℃ for 2 h to form a porous silicon-aluminum transition layer with a porosity of 45%-55% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: the silicon-aluminum transition layer is used as a substrate, and nickel-based electroplating solution containing ceramic particles is used for electroplating co-deposition to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 250-280 g / L; Nickel chloride: 45-55 g / L; Boric acid: 35-40 g / L; Sodium dodecyl sulfate: 0.04-0.06 g / L; Leveling agent sodium saccharin: 0.08-0.12 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 20-40 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1-3 g / L; Current density 2.5-3 A / dm 2 , temperature 52-55 ℃, pH 4.8-5.0 (boric acid buffer), and electroplating time 12-15 min; Step (4) Low-temperature annealing: The nickel-based ceramic composite coating is annealed in an oxygen-free atmosphere to eliminate internal stress and enhance interfacial bonding, thereby achieving an ultra-high temperature resistant nickel-based ceramic composite coating; annealing is carried out in a nitrogen / argon mixed atmosphere (oxygen content ≤10ppm) at 450~500℃ for 1.5h to eliminate residual electroplating stress, promote interfacial diffusion between the nickel substrate and SiC particles, and further harmonize the expansion coefficient.

[0021] Example 1 A process for ultra-high temperature resistant nickel-based ceramic composite coating includes the following steps: Step (1) Pretreatment of aluminum substrate: The aluminum substrate is subjected to surface roughening, anodizing and oxygen ion bombardment activation treatment in sequence to obtain a surface roughened and highly active aluminum substrate; Surface roughening was achieved by anodic oxidation, with the following parameters: electrolyte 120 g / L oxalic acid, voltage 12 V, oxidation at room temperature for 12 min, resulting in a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm. Oxygen ion bombardment activation was performed using plasma equipment with the following process parameters: working gas was Ar / O2 (volume ratio 9:1), power was 100 W, and processing time was 8 min. Step (2) Preparation of silicon-aluminum transition layer: Silicon gel is coated on the surface of the pretreated aluminum substrate, and then cured, pore-forming and oxygen-free high-temperature calcination is performed to form a silicon-aluminum transition layer with a porous structure. The silicone gel formulation, by mass fraction, is as follows: Silica sol (SiO2 particle size 20~50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidoxypropyltrimethoxysilane: 3%; Pore-forming agent: polymethyl methacrylate, particle size 1~5 μm: 10%; Toughening agent: polydimethylsiloxane: 2%; The wet-milled coating thickness was 90 μm. The curing process was: constant temperature drying at 60℃ for 2.5 h, followed by curing at 80℃ for 1.5 h to promote the hydrolysis and condensation of KH560. The pore-forming condition was calcination at 450℃ for 2 h to form a porous silicon-aluminum transition layer with a porosity of 45% and a pore size of 2~6 μm. Figure 1 The image shows the crystal phase diagram of the ultra-high temperature resistant nickel-based ceramic composite coating at 500×, where the area in the box is the silicon-aluminum transition layer. Step (3) Electroplating of nickel-based ceramic layer: Using the silicon-aluminum transition layer as the substrate, a nickel-based electroplating solution containing ceramic particles is used for electroplating co-deposition to obtain a nickel-based ceramic composite coating; Nickel-based electroplating solutions are composed of the following components by mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent saccharin sodium: 0.08 g / L; Silane coupling agent surface treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52℃, pH 4.8 (boric acid buffer), plating time 12 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance interface bonding force, realizing the super high temperature resistant nickel-based ceramic composite coating; annealing at 450℃ for 1.5 h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate the residual stress of plating, promote the interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0022] Example two A super high temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are as follows: electrolyte is 135 g / L oxalic acid, voltage is 13.5 V, and the porous Al2O3 layer with a thickness of 27 μm is generated by oxidizing at room temperature for 13.5 min, and the surface roughness Ra is 4.0 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are as follows: the working gas is Ar / O2 (volume ratio 9:1), the power is 110 W, and the treatment time is 9 min; Step (2) preparation of silicon-aluminum transition layer: coating silicon gel on the surface of the pretreated aluminum substrate, and forming a silicon-aluminum transition layer containing porous structure through solidification, pore formation and oxygen-free high temperature calcination; The formula of the silicon gel is, by mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 57%; Deionized water: 30%; γ-glycidyl ether propyltrimethoxysilane: 3.5%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 12%; Toughening agent polydimethylsiloxane: 2.5%; The wet grinding thickness after coating is 100 μm, the curing process is: constant temperature drying at 60℃ for 2.5h, post-curing at 80℃ for 1.5h, promoting the hydrolysis and condensation of KH560; the pore forming condition is calcining at 475℃ for 2h, forming a porous silicon-aluminum transition layer with porosity of 50% and pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: taking the silicon-aluminum transition layer as the substrate, electroplating co-deposition is carried out by using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite coating; The nickel-based electroplating solution has the following mass concentration components: Nickel sulfate: 265 g / L; Nickel chloride: 50 g / L; Boric acid: 37 g / L; Sodium dodecyl sulfate: 0.05 g / L; Leveling agent sodium saccharin: 0.10 g / L; Silane coupling agent surface treated ceramic particles with particle size of 1-5 μm: 30 g / L; Dispersant polyethylene glycol (molecular weight 2000): 2 g / L; Current density 2.8 A / dm 2 , temperature 53.5℃, pH 4.9 (boric acid buffer), electroplating time 13.5 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance the interface bonding force, realizing an ultra-high temperature resistant nickel-based ceramic composite coating; annealing at 475℃ for 1.5h in a nitrogen / argon mixed gas atmosphere (oxygen content ≤10 ppm) to eliminate electroplating residual stress, promote the interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0023] Example Three An ultra-high temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with rough surface and high activity; The surface roughening is performed by an anodic oxidation method, and the specific parameters are: electrolyte is 150 g / L oxalic acid, voltage is 15 V, and the aluminum substrate is oxidized at room temperature for 15 min to form a porous Al2O3 layer with a thickness of 30 μm and a surface roughness Ra of 5.0 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are: working gas is Ar / O2 (volume ratio 9:1), power is 120 W, and treatment time is 10 min; Step (2) silicon-aluminum transition layer preparation: coating a silica gel on the surface of the pretreated aluminum substrate, and forming a silicon-aluminum transition layer containing a porous structure through solidification, pore forming and oxygen-free high temperature calcination. The formula of the silica gel is, by mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 60%; Deionized water: 28%; γ-glycidoxypropyltrimethoxysilane: 4%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 15%; Toughening agent polydimethylsiloxane: 3%; The wet grinding thickness after coating is 110 μm, and the curing process is: constant temperature drying at 60°C for 2.5 h, post-curing at 80°C for 1.5 h, and promoting the hydrolysis and condensation of KH560; the pore-forming condition is calcination at 500°C for 2 h, forming a porous silica-aluminum transition layer with a porosity of 55% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silica-aluminum transition layer as the substrate, electroplating co-deposition is performed using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following mass concentration components: Nickel sulfate: 280 g / L; Nickel chloride: 55 g / L; Boric acid: 40 g / L; Sodium dodecyl sulfate: 0.06 g / L; Leveling agent sodium saccharin: 0.12 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 40 g / L; Dispersant polyethylene glycol (molecular weight 2000): 3 g / L; Current density 3 A / dm 2 , temperature 55°C, pH 5.0 (boric acid buffer), electroplating time 15 min; Step (4) low-temperature annealing: annealing the nickel-based ceramic composite plating layer in an oxygen-free atmosphere to eliminate internal stress and enhance the interface bonding force, realizing an ultra-high-temperature nickel-based ceramic composite plating layer; annealing at 500°C for 1.5 h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate electroplating residual stress, promote the interface diffusion of the nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0024] Example Four An ultra-high-temperature nickel-based ceramic composite plating layer process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation, and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation, and the specific parameters are as follows: an electrolyte is 125 g / L oxalic acid, a voltage is 13 V, and the oxidation is performed at room temperature for 14 min to form a porous Al2O3 layer with a thickness of 26 μm and a surface roughness Ra of 3.8 μm; The oxygen ion bombardment activation is performed by using a plasma device, and the process parameters are as follows: the working gas is Ar / O2 (volume ratio 9:1), the power is 105 W, and the processing time is 8.5 min; Step (2) preparation of the silicon-aluminum transition layer: the silicon gel is coated on the surface of the pretreated aluminum substrate, and is cured, pore-formed and calcined at high temperature in an oxygen-free atmosphere to form a silicon-aluminum transition layer containing a porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 56%; Deionized water: 33%; Gamma-glycidoxypropyltrimethoxysilane: 3.2%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 11%; Toughening agent polydimethylsiloxane: 2.3%; The wet grinding thickness after coating is 95 μm, the curing process is as follows: constant temperature drying at 60°C for 2.5 h, post-curing at 80°C for 1.5 h to promote the hydrolysis and condensation of KH560, and the pore-forming condition is calcination at 460°C for 2 h to form a porous silicon-aluminum transition layer with a porosity of 47% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: the silicon-aluminum transition layer is used as a substrate, and nickel-based electroplating solution containing ceramic particles is used for electroplating co-deposition to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 255 g / L; Nickel chloride: 47 g / L; Boric acid: 36 g / L; Sodium dodecyl sulfate: 0.045 g / L; Leveling agent sodium saccharin: 0.09 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 25 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1.5 g / L; Current density 2.6 A / dm 2 , temperature 52.5°C, pH 4.85 (boric acid buffer), and electroplating time 13 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance the interface bonding force, realizing the super high temperature resistant nickel-based ceramic composite coating; annealing at 460℃ for 1.5h in a nitrogen / argon mixed atmosphere (oxygen content ≤10ppm) to eliminate the residual stress of electroplating, promote the interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0025] Example Five A process for preparing a super high temperature resistant nickel-based ceramic composite coating, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are as follows: electrolyte is 145 g / L oxalic acid, voltage is 14 V, and the aluminum substrate is oxidized at room temperature for 14.5 min to form a porous Al2O3 layer with a thickness of 29 μm and a surface roughness Ra of 4.5 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 115 W, and treatment time is 9.5 min; Step (2) preparation of silicon-aluminum transition layer: coating silicon gel on the surface of the pretreated aluminum substrate, and then performing solidification, pore forming and oxygen-free high temperature calcination to form a silicon-aluminum transition layer containing a porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 59%; Deionized water: 29%; γ-glycidyl ether propyltrimethoxysilane: 3.8%; Pore forming agent polymethyl methacrylate, particle size 1-5 μm: 14%; Toughening agent polydimethylsiloxane: 2.8%; The wet grinding thickness after coating is 105 μm, and the solidification process is as follows: constant temperature drying at 60℃ for 2.5h, post-solidification at 80℃ for 1.5h to promote the hydrolysis and condensation of KH560, pore forming conditions are calcination at 490℃ for 2h to form a porous silicon-aluminum transition layer with a porosity of 53% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as a substrate, electroplating co-deposition is performed by using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite coating; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 275 g / L; Nickel chloride: 53 g / L; Boric acid: 39 g / L; Sodium dodecyl sulfate: 0.055 g / L; Leveling agent sodium saccharin: 0.11 g / L; Silane coupling agent surface treated ceramic particles, particle size 1-5 μm: 35 g / L; Dispersant polyethylene glycol (molecular weight 2000): 2.5 g / L; Current density 2.9 A / dm 2 , temperature 54.5℃, pH 4.95 (boric acid buffer), plating time 14 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance interface bonding force, realizing the super high temperature resistant nickel-based ceramic composite coating; annealing at 490℃ for 1.5h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate the residual stress of plating, promote the interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0026] Comparative Example One The difference from Example One is that there is no transition layer: A super high temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and the surface is oxidized at room temperature for 12 min to generate a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by a plasma equipment, and the process parameters are: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and treatment time is 8 min, the surface energy is increased to ≥60 mN / m, and the contact angle is ≤35°; Step (2) preparation of silicon-aluminum transition layer: no silicon-aluminum transition layer is prepared, and this step is directly skipped; Step (3) nickel-based ceramic layer plating: taking the aluminum substrate as the substrate, performing electroplating co-deposition by using a nickel-based plating solution containing ceramic particles to obtain a nickel-based ceramic composite coating; The nickel-based plating solution has the following components by mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 Temperature 52℃, pH 4.8 (boric acid buffer), plating time 12 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance interface bonding force, realizing the ultra-high temperature resistant nickel-based ceramic composite coating; annealing at 450℃ for 1.5 h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate residual stress of plating, promote interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0027] Comparative example two The difference from example one is that the transition layer is too thick: An ultra-high temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and oxidation is performed at room temperature for 12 min to generate a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and treatment time is 8 min, so that the surface energy is increased to ≥60 mN / m and the contact angle is ≤35°; Step (2) silicon-aluminum transition layer preparation: coating silicon gel on the surface of the pretreated aluminum substrate, and then performing solidification, pore formation and oxygen-free high temperature calcination to form a silicon-aluminum transition layer containing porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether propyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 120 μm, the curing process is: constant temperature drying at 60℃ for 2.5h, post-curing at 80℃ for 1.5h, promoting the hydrolysis and condensation of KH560; the pore forming condition is calcination at 450℃ for 2h, forming a porous silicon-aluminum transition layer with porosity of 45% and pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: taking the silicon-aluminum transition layer as the substrate, electroplating co-deposition is carried out by using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite coating; The nickel-based electroplating solution has the following mass concentration components: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent saccharin sodium: 0.08 g / L; Silane coupling agent surface treated ceramic particles with particle size of 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52℃, pH 4.8 (boric acid buffer), electroplating time 12 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance the interfacial bonding force, realizing an ultra-high temperature resistant nickel-based ceramic composite coating; annealing at 450℃ for 1.5h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate electroplating residual stress, promote the interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0028] Comparative Example Three The difference from Example One is that the aluminum substrate surface is not subjected to oxygen ion bombardment treatment: An ultra-high temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening and anodic oxidation treatment on the aluminum substrate, omitting oxygen ion bombardment activation, to obtain an aluminum substrate with roughened surface but low activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and oxidation is carried out at room temperature for 12 min to form a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; Step (2) silicon-aluminum transition layer preparation: coating a silica gel on the surface of the pretreated aluminum substrate, and forming a silicon-aluminum transition layer containing a porous structure through solidification, pore forming and oxygen-free high temperature calcination; The formula of the silica gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidoxypropyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, and the curing process is: constant temperature drying at 60℃ for 2.5h, post-curing at 80℃ for 1.5h, promoting the hydrolysis and condensation of KH560; the pore-forming condition is calcination at 450℃ for 2h, forming a porous silicon-aluminum transition layer with porosity 45% and pore size 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as the substrate, electroplating co-deposition is carried out using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following mass concentration components: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52℃, pH 4.8 (boric acid buffer), electroplating time 12 min; Step (4) low-temperature annealing: annealing the nickel-based ceramic composite plating layer in an oxygen-free atmosphere to eliminate internal stress and enhance the interface bonding force, realizing an ultra-high-temperature nickel-based ceramic composite plating layer; annealing at 450℃ for 1.5h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate electroplating residual stress, promote the interface diffusion of the nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0029] Comparative Example Four The difference from Example One is that the calcination temperature is too high, being 700℃: An ultra-high-temperature nickel-based ceramic composite plating layer process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, oxidation is performed at room temperature for 12 min, a porous Al2O3 layer with a thickness of 25 μm is generated, and the surface roughness Ra is 3.5 μm; The oxygen ion bombardment activation is performed by using a plasma device, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, processing time is 8 min, the surface energy is increased to ≥60 mN / m, and the contact angle is ≤35°; Step (2) preparation of the silicon-aluminum transition layer: the silicon gel is coated on the surface of the pretreated aluminum substrate, and is cured, pore-formed and calcined at high temperature in an oxygen-free atmosphere to form a silicon-aluminum transition layer containing a porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether propyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, the curing process is as follows: constant temperature drying at 60°C for 2.5 h, post-curing at 80°C for 1.5 h to promote the hydrolysis and condensation of KH560, the pore-forming condition is calcination at 700°C for 2 h, and a porous silicon-aluminum transition layer with a porosity of 45% and a pore size of 2-6 μm is formed; Step (3) nickel-based ceramic layer electroplating: the silicon-aluminum transition layer is used as a substrate, and nickel-based electroplating solution containing ceramic particles is used for electroplating co-deposition to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52°C, pH 4.8 (boric acid buffer), electroplating time 12 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance the interface bonding force, realizing the super high-temperature resistant nickel-based ceramic composite coating; annealing at 450℃ for 1.5h in a nitrogen / argon mixed atmosphere (oxygen content ≤10ppm) to eliminate the residual stress of electroplating, promote the interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0030] Comparative Example Five The difference from Example One is that no pore-forming agent is added: A super high-temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and oxidation is performed at room temperature for 12 min to generate a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and treatment time is 8 min, so that the surface energy is increased to ≥60 mN / m and the contact angle is ≤35°; Step (2) preparation of silicon-aluminum transition layer: coating silicon gel on the surface of the pretreated aluminum substrate, and then performing solidification, pore formation and oxygen-free high-temperature calcination to form a silicon-aluminum transition layer containing a porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether propyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 0%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, and the solidification process is as follows: constant temperature drying at 60℃ for 2.5h and post-solidification at 80℃ for 1.5h to promote the hydrolysis and condensation of KH560; the pore-forming conditions are calcination at 450℃ for 2h to form a porous silicon-aluminum transition layer with a porosity of 45% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as a substrate and using a nickel-based electroplating solution containing ceramic particles for electroplating co-deposition to obtain a nickel-based ceramic composite coating; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent saccharin sodium: 0.08 g / L; Silane coupling agent surface treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52℃, pH 4.8 (boric acid buffer), plating time 12 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance interface bonding force, realizing the ultra-high temperature resistant nickel-based ceramic composite coating; annealing at 450℃ for 1.5 h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate the residual stress of plating, promote the interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0031] Comparative example six The difference from example one is that too much pore-forming agent is added: An ultra-high temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and the oxidation is performed at room temperature for 12 min to generate a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and treatment time is 8 min, and the surface energy is increased to ≥60 mN / m and the contact angle is ≤35°; Step (2) preparation of silicon-aluminum transition layer: coating silicon gel on the surface of the pretreated aluminum substrate, and forming a silicon-aluminum transition layer containing a porous structure through solidification, pore formation and oxygen-free high temperature calcination; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether propyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 18%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, the curing process is: constant temperature drying at 60℃ for 2.5h, post-curing at 80℃ for 1.5h, promoting the hydrolysis and condensation of KH560; the pore-forming condition is calcination at 450℃ for 2h, forming a porous silicon-aluminum transition layer with porosity of 45% and pore size of 2~6 μm; Step (3) nickel-based ceramic layer electroplating: taking the silicon-aluminum transition layer as the substrate, electroplating co-deposition is carried out by using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following mass concentration components: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface treated ceramic particles with particle size of 1~5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52℃, pH 4.8 (boric acid buffer), electroplating time 12 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite plating layer in an oxygen-free atmosphere to eliminate internal stress and enhance interface bonding force, realizing an ultra-high temperature resistant nickel-based ceramic composite plating layer; annealing at 450℃ for 1.5h in a nitrogen / argon mixed gas atmosphere (oxygen content ≤10 ppm) to eliminate electroplating residual stress, promote interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0032] Comparative Example Seven The difference from Example One is that the pH control is not within the range: An ultra-high temperature resistant nickel-based ceramic composite plating layer process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and oxidation is carried out at room temperature for 12 min to generate a porous Al2O3 layer with thickness of 25 μm and surface roughness Ra of 3.5 μm; Oxygen ion bombardment activation uses a plasma device, and the process parameters are as follows: the working gas is Ar / O2 (volume ratio 9:1), the power is 100 W, the processing time is 8 min, the surface energy is increased to ≥60 mN / m, and the contact angle is ≤35°; Step (2) preparation of the silicon-aluminum transition layer: the silicon gel is coated on the surface of the pretreated aluminum substrate, and is cured, pore-formed and calcined at high temperature in an oxygen-free atmosphere to form a porous silicon-aluminum transition layer; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether oxypropyl trimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, the curing process is as follows: constant temperature drying at 60°C for 2.5 h, post-curing at 80°C for 1.5 h, and promoting the hydrolysis and condensation of KH560; the pore-forming condition is calcination at 450°C for 2 h to form a porous silicon-aluminum transition layer with a porosity of 45% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as a substrate, nickel-based electroplating solution containing ceramic particles is used for electroplating co-deposition to obtain a nickel-based ceramic composite coating; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52°C, pH 4.7 (boric acid buffer), electroplating time 12 min; Step (4) low-temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance the interfacial bonding force, so as to realize the super-high-temperature nickel-based ceramic composite coating; annealing at 450°C for 1.5 h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate the residual stress of electroplating, promote the interfacial diffusion of the nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0033] Comparative Example Eight The difference from Example One is that the electroplating conditions are out of range: A super-high-temperature-resistant nickel-based ceramic composite plating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and oxidation is performed at room temperature for 12 min to generate a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and treatment time is 8 min, so that the surface energy is increased to ≥60 mN / m and the contact angle is ≤35°; Step (2) preparation of silicon-aluminum transition layer: coating silicon gel on the surface of the pretreated aluminum substrate, and then performing solidification, pore formation and oxygen-free high-temperature calcination to form a silicon-aluminum transition layer containing a porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether propyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, and the solidification process is as follows: constant temperature drying at 60°C for 2.5 h, post-solidification at 80°C for 1.5 h, and promotion of hydrolysis and condensation of KH560; the pore formation condition is calcination at 450°C for 2 h to form a porous silicon-aluminum transition layer with a porosity of 45% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as a substrate, performing electroplating co-deposition by using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 3.5 A / dm 2 Temperature 52℃, pH 4.8 (boric acid buffer), plating time 12 min; Step (4) low-temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance interface bonding force, realizing the ultra-high-temperature nickel-based ceramic composite coating; annealing at 450℃ for 1.5 h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate residual stress of plating, promote interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0034] Comparative Example Nine The difference from Example One is that the annealing environment has an oxygen atmosphere: An ultra-high-temperature nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and the surface is oxidized at room temperature for 12 min to form a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by a plasma equipment, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and treatment time is 8 min, so that the surface energy is increased to ≥60 mN / m and the contact angle is ≤35°; Step (2) preparation of silicon-aluminum transition layer: coating silicon gel on the surface of the pretreated aluminum substrate, and then performing solidification, pore formation and oxygen-free high-temperature calcination to form a silicon-aluminum transition layer containing a porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether propyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, and the solidification process is as follows: constant temperature drying at 60℃ for 2.5 h and post-solidification at 80℃ for 1.5 h to promote hydrolysis and condensation of KH560; the pore formation condition is calcination at 450℃ for 2 h to form a porous silicon-aluminum transition layer with a porosity of 45% and a pore size of 2-6 μm; Step (3) Nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as the substrate, electroplating co-deposition is carried out by using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite coating; The nickel-based electroplating solution has the following components by mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface treated ceramic particles with a particle size of 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52℃, pH 4.8 (boric acid buffer), electroplating time 12 min; Step (4) Low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-containing atmosphere to eliminate internal stress and enhance the interfacial bonding force, realizing an ultra-high temperature resistant nickel-based ceramic composite coating; annealing at 450℃ for 1.5 h in an air atmosphere (oxygen content about 21%) to eliminate electroplating residual stress, promote the interface diffusion of the nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0035] Comparative Example Ten The difference from Example One is that the annealing temperature is too high: An ultra-high temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) Aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by an anodic oxidation method, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and oxidation is performed at room temperature for 12 min to generate a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and treatment time is 8 min, the surface energy is increased to ≥60 mN / m, and the contact angle is ≤35°; Step (2) Silicon-aluminum transition layer preparation: coating a silica gel on the surface of the pretreated aluminum substrate, and performing solidification, pore formation and oxygen-free high temperature calcination to form a silicon-aluminum transition layer containing a porous structure; The formula of the silica gel is as follows by mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidoxypropyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, and the curing process is: constant temperature drying at 60℃ for 2.5h, post-curing at 80℃ for 1.5h, promoting the hydrolysis and condensation of KH560; the pore-forming condition is calcination at 450℃ for 2h, forming a porous silicon-aluminum transition layer with porosity 45% and pore size 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as the substrate, electroplating co-deposition is carried out using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following mass concentration components: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52℃, pH 4.8 (boric acid buffer), electroplating time 12 min; Step (4) low-temperature annealing: annealing the nickel-based ceramic composite plating layer in an oxygen-free atmosphere to eliminate internal stress and enhance the interfacial bonding force, realizing an ultra-high-temperature nickel-based ceramic composite plating layer; annealing at 550℃ for 1.5h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate electroplating residual stress, promote the interfacial diffusion of the nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0036] Comparative Example XI The difference from Example I is that the calcination temperature is too low, being 400℃: An ultra-high-temperature nickel-based ceramic composite plating layer process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and oxidation is performed at room temperature for 12 min to form a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by using a plasma device, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and processing time is 8 min, so that the surface energy is increased to ≥60 mN / m and the contact angle is ≤35°; Step (2) preparation of the silicon-aluminum transition layer: a silica gel is coated on the surface of the pretreated aluminum substrate, and is cured, pore-formed and calcined at high temperature in an oxygen-free atmosphere to form a silicon-aluminum transition layer containing a porous structure; The formula of the silica gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether propyltrimethoxysilane: 3%; Pore-forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, and the curing process is as follows: constant temperature drying at 60°C for 2.5 h, post-curing at 80°C for 1.5 h to promote the hydrolysis and condensation of KH560, pore-forming at 400°C for 2 h to form a porous silicon-aluminum transition layer with a porosity of 45% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as a substrate, a nickel-based electroplating solution containing ceramic particles is used for electroplating co-deposition to obtain a nickel-based ceramic composite plating layer; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent sodium saccharin: 0.08 g / L; Silane coupling agent surface-treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52°C, pH 4.8 (boric acid buffer), and electroplating time 12 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance the interface bonding force, realizing the super high temperature resistant nickel-based ceramic composite coating; annealing at 450℃ for 1.5h in a nitrogen / argon mixed atmosphere (oxygen content ≤10ppm) to eliminate the residual stress of electroplating, promote the interface diffusion of nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0037] Comparative example twelve The difference from example one is that the annealing temperature is too low: A super high temperature resistant nickel-based ceramic composite coating process, comprising the following steps: Step (1) aluminum substrate pretreatment: sequentially performing surface roughening, anodic oxidation and oxygen ion bombardment activation treatment on the aluminum substrate to obtain an aluminum substrate with roughened surface and high activity; The surface roughening is performed by anodic oxidation method, and the specific parameters are as follows: electrolyte is 120 g / L oxalic acid, voltage is 12 V, and oxidation is performed at room temperature for 12 min to generate a porous Al2O3 layer with a thickness of 25 μm and a surface roughness Ra of 3.5 μm; The oxygen ion bombardment activation is performed by using a plasma equipment, and the process parameters are as follows: working gas is Ar / O2 (volume ratio 9:1), power is 100 W, and treatment time is 8 min, so that the surface energy is increased to ≥60 mN / m and the contact angle is ≤35°; Step (2) preparation of silicon-aluminum transition layer: coating silicon gel on the surface of the pretreated aluminum substrate, and performing solidification, pore formation and oxygen-free high temperature calcination to form a silicon-aluminum transition layer containing a porous structure; The formula of the silicon gel is as follows in terms of mass fraction: Silica sol (SiO2 particle size 20-50 nm, content 30%): 55%; Deionized water: 35%; γ-glycidyl ether propyltrimethoxysilane: 3%; Pore forming agent polymethyl methacrylate, particle size 1-5 μm: 10%; Toughening agent polydimethylsiloxane: 2%; The wet grinding thickness after coating is 90 μm, and the solidification process is as follows: constant temperature drying at 60℃ for 2.5h, post-solidification at 80℃ for 1.5h to promote the hydrolysis and condensation of KH560; and the pore formation condition is calcination at 450℃ for 2h to form a porous silicon-aluminum transition layer with a porosity of 45% and a pore size of 2-6 μm; Step (3) nickel-based ceramic layer electroplating: using the silicon-aluminum transition layer as a substrate, electroplating co-deposition is performed by using a nickel-based electroplating solution containing ceramic particles to obtain a nickel-based ceramic composite coating; The nickel-based electroplating solution has the following components in terms of mass concentration: Nickel sulfate: 250 g / L; Nickel chloride: 45 g / L; Boric acid: 35 g / L; Sodium dodecyl sulfate: 0.04 g / L; Leveling agent saccharin sodium: 0.08 g / L; Silane coupling agent surface treated ceramic particles, particle size 1-5 μm: 20 g / L; Dispersant polyethylene glycol (molecular weight 2000): 1 g / L; Current density 2.5 A / dm 2 , temperature 52°C, pH 4.8 (boric acid buffer), plating time 12 min; Step (4) low temperature annealing: annealing the nickel-based ceramic composite coating in an oxygen-free atmosphere to eliminate internal stress and enhance interface bonding force, realizing the super high-temperature nickel-based ceramic composite coating; annealing at 400°C for 1.5 h in a nitrogen / argon mixed atmosphere (oxygen content ≤10 ppm) to eliminate the residual stress of plating, promote the interface diffusion of the nickel matrix and SiC particles, and further harmonize the expansion coefficient.

[0038] Performance detection: Coating bonding strength: reference ASTM C633; Coating Vickers hardness: ASTM E384; Coating bonding strength and coating Vickers hardness under high-temperature phosphoric acid industrial working conditions: high-temperature phosphoric acid immersion corrosion, retesting the coating bonding strength and Vickers hardness: medium: 50% H3PO4(simulating industrial concentration) temperature: 100±2°C time: 168 h (7 days); Thermal expansion coefficient test standard ASTM E831.

[0039] The detection results are shown in Table 1.

[0040] Table 1 The embodiment of the present scheme realizes the stable combination of aluminum base material and nickel-based ceramic coating under severe working conditions through stepwise interface construction and multi-component synergistic effect: the porous alumina layer formed by anodic oxidation constructs a micro-mechanical anchoring foundation, and the significantly improved surface energy after oxygen ion bombardment activation ensures the full infiltration and spreading of the silica sol precursor; the nano-silica sol and micron-sized pore-forming agent in the silicon-aluminum transition layer form a buffer structure with gradient porosity under controlled calcination, the pore size distribution of which forms a topological match with the size of the subsequent electroplated ceramic particles, while the covalent network constructed by the silane coupling agent and the toughening agent endow the interlayer with deformation coordination ability; the dispersant and buffer system in the electroplating process ensure the uniform embedding of ceramic particles in the nickel matrix, and the precise temperature control of oxygen-free annealing optimizes the continuity of the thermal expansion coefficient through interfacial element interdiffusion, establishing a gradual transition between the high expansion characteristics of the aluminum base material and the low expansion characteristics of the nickel coating, thereby maintaining the interface integrity under thermal-mechanical-chemical coupling loads. This multi-level design from micro-roughness control to macro-stress coordination enables the coating to form a self-adaptive protection mechanism that protects the main interface by forming sacrificial pores in the high-temperature corrosion environment.

[0041] Compared with Example One, Comparative Example One has no transition layer, and the gradient buffer of the silicon-aluminum transition layer is missing. The aluminum base material (23x10 -6 / ℃) and the nickel-based ceramic layer (~13x10 -6 / ℃) have a direct mutation in the thermal expansion coefficient, and the interface thermal stress is concentrated at high temperatures. The pre-soaking bond strength is only 9.6 MPa, and it decreases to 4.2 MPa after phosphoric acid corrosion, and the coating is prone to peeling. -6 / ℃) and the nickel-based ceramic layer (~13x10 0.3In Comparative Example 6, the pore-forming agent was excessive, with PMMA accounting for 18%, exceeding the 10%~15% range. The transition layer had excessively high porosity, resulting in a loose structure unable to withstand stress. The bonding strength was only 13.5 MPa. After corrosion, the pores became channels for the corrosive medium, causing the hardness to drop to 365 HV. 0.3 Comparative Example 7: The electroplating pH was outside the acceptable range (pH=4.7, below 4.8-5.0), resulting in uneven nickel ion reduction rate, a rough coating, and disordered SiC particle distribution. The bonding strength was 16.4 MPa, but after corrosion, the coating defects eroded the coating, reducing the strength to 9.2 MPa. Comparative Example 8: The current density was too high (3.5 A / dm³). 2 The current caused the coating to deposit too quickly, resulting in cracks and pinholes. The SiC particles were unevenly embedded, and the bonding strength was only 10.8 MPa. After corrosion, the defective areas were preferentially eroded, reducing the strength to 5.6 MPa. Comparative Example 9 involved annealing in an oxygen atmosphere. Annealing in air caused the nickel-based coating and transition layer to oxidize, forming NiO and Al2O3. The interfacial bonding strength decreased to 12.7 MPa due to the oxide layer barrier, and the oxidation products reduced hardness, further deteriorating performance after corrosion. Comparative Example 10 involved annealing at too high a temperature (550℃), leading to excessive diffusion of aluminum and nickel, destroying the transition layer structure, and causing the nickel-based coating to have coarse grains, reducing its hardness to 380 HV. 0.3 The initial bonding strength was 17.5 MPa, but after corrosion, the strength decreased to 11.8 MPa due to increased brittleness of the diffusion layer. Comparative Example 11 had an excessively low calcination temperature; calcination at 400℃ resulted in incomplete decomposition of residual carbon impurities in the PMMA, leading to an incomplete porous structure in the transition layer and an increase in the coefficient of thermal expansion to 21.8 × 10⁻⁶. -6 / ℃, the bonding strength was 13.1 MPa. After corrosion, impurities accelerated interface erosion, and the strength dropped to 6.9 MPa. The annealing temperature of the comparative example was too low. Annealing at 400℃ failed to effectively eliminate the residual stress of electroplating (>30 MPa). The internal stress of the coating resulted in a bonding strength of only 19.2 MPa. Moreover, the diffusion of nickel and SiC interface was insufficient. After corrosion, the coating cracked due to stress release, and the strength dropped to 14.5 MPa.

[0042] In summary, the comparative examples failed to achieve stress buffering and multiple bonding at the gradient interface due to the disruption of the process synergy between pretreatment, transition layer, electroplating, and annealing, or deviation from the ratio range of key components. As a result, their performance in high-temperature and highly corrosive environments was significantly inferior to that of the examples.

Claims

1. A process for ultra-high temperature resistant nickel-based ceramic composite coating, characterized in that, Includes the following steps: Step (1) Pretreatment of aluminum substrate: The aluminum substrate is subjected to surface roughening, anodizing and oxygen ion bombardment activation treatment in sequence to obtain the pretreated aluminum substrate; Step (2) Preparation of silicon-aluminum transition layer: Silicon gel is coated on the surface of the pretreated aluminum substrate, and then cured, pore-forming and oxygen-free high-temperature calcination is performed to form a silicon-aluminum transition layer with a porous structure. Step (3) Electroplating of nickel-based ceramic layer: Using the silicon-aluminum transition layer as the substrate, a nickel-based electroplating solution containing ceramic particles is used for electroplating co-deposition to obtain a nickel-based ceramic composite coating; Step (4) Low-temperature annealing: The nickel-based ceramic composite coating is annealed in an oxygen-free atmosphere to obtain an ultra-high temperature resistant nickel-based ceramic composite coating.

2. The ultra-high temperature resistant nickel-based ceramic composite coating process as described in claim 1, characterized in that, The surface roughening in step (1) is performed by anodic oxidation. The specific parameters are: electrolyte is 120~150 g / L oxalic acid, voltage is 12~15 V, and oxidation is performed at room temperature for 12~15 min.

3. The ultra-high temperature resistant nickel-based ceramic composite coating process as described in claim 1, characterized in that, In step (1), the process parameters for oxygen ion bombardment activation are: working gas is Ar / O2 with a volume ratio of 9:1, power is 100~120 W, and processing time is 8~10 min.

4. The ultra-high temperature resistant nickel-based ceramic composite coating process as described in claim 1, characterized in that, The formulation of the silicone gel mentioned in step (2) is as follows, by mass fraction: Silica sol: 55%~60%; the silica sol contains 30% SiO2 particles with a particle size of 20~50 nm. Deionized water: 28%~35%; γ-glycidoxypropyltrimethoxysilane: 3%~4%; Pore-forming agent: polymethyl methacrylate, particle size 1~5 μm: 10%~15%; Toughening agent: polydimethylsiloxane: 2%~3%.

5. The ultra-high temperature resistant nickel-based ceramic composite coating process as described in claim 1, characterized in that, The wet grinding thickness after coating in step (2) is 90~110 μm, and the curing process is: constant temperature drying at 60℃ for 2.5h, followed by curing at 80℃ for 1.5h.

6. The ultra-high temperature resistant nickel-based ceramic composite coating process as described in claim 1, characterized in that, The conditions for creating the pores in step (2) are calcination at 450~500℃ for 2 hours.

7. The ultra-high temperature resistant nickel-based ceramic composite coating process as described in claim 1, characterized in that, The nickel-based electroplating solution described in step (3) has the following composition by mass concentration: Nickel sulfate: 250~280 g / L; Nickel chloride: 45~55 g / L; Boric acid: 35~40 g / L; Sodium dodecyl sulfate: 0.04~0.06 g / L; Leveling agent sodium saccharin: 0.08~0.12 g / L; Ceramic particles: 20~40 g / L; Dispersant: polyethylene glycol: 1~3 g / L.

8. The ultra-high temperature resistant nickel-based ceramic composite coating process as described in claim 1, characterized in that, The electroplating parameters mentioned in step (3) are: current density 2.5~3 A / dm³. 2 Temperature 52~55℃, pH 4.8~5.0, electroplating time 12~15min.

9. The ultra-high temperature resistant nickel-based ceramic composite coating process as described in claim 1, characterized in that, The low-temperature annealing process described in step (4) is as follows: annealing at 450~500℃ for 1.5h in a nitrogen / argon mixed atmosphere.

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