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CN117144278A - Preparation method of high-temperature protective coating and coating - Google Patents

Preparation method of high-temperature protective coating and coating Download PDF

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Publication number
CN117144278A
CN117144278A CN202311403964.6A CN202311403964A CN117144278A CN 117144278 A CN117144278 A CN 117144278A CN 202311403964 A CN202311403964 A CN 202311403964A CN 117144278 A CN117144278 A CN 117144278A
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layer
plating
electroplating
coating
mcralx
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CN117144278B (en
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刘建明
黄凌峰
于月光
王帅
郭睿
刘通
吴超
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Bgrimm Advanced Materials Science & Technology Co ltd
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Bgrimm Advanced Materials Science & Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Mechanical Engineering (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The invention belongs to the field of high-temperature protective coatings, and particularly relates to a preparation method of a high-temperature protective coating and the coating, wherein the method comprises the following steps: pre-plating the substrate to obtain a pre-plating layer, performing first electroplating treatment on the substrate plated with the pre-plating layer to obtain a first plating layer, performing second electroplating treatment on the substrate plated with the pre-plating layer and the first plating layer to obtain a second plating layer, performing vacuum heat treatment on the substrate plated with the pre-plating layer, the first plating layer and the second plating layer to obtain an alloy coating, and depositing a ceramic layer on the surface of the alloy coating through atmospheric plasma spraying; the preplating solution, the first electroplating solution and the second electroplating solution are M-based plating solutions, the first electroplating solution and the second electroplating solution contain MCrAlX alloy particles, M is Ni or Co or NiCo, X is selected from Y, ta, hf, si, and the granularity of the alloy particles of the first electroplating solution is smaller than that of the alloy particles of the second electroplating solution. The coating of the invention has strong binding force with the matrix and the ceramic layer, and is not easy to peel off and fail.

Description

Preparation method of high-temperature protective coating and coating
Technical Field
The invention belongs to the technical field of high-temperature protective coatings, and particularly relates to a preparation method of a high-temperature protective coating and the coating.
Background
The high-temperature protective coating is widely applied to the manufacture and maintenance of aviation, aerospace and mechanical equipment, and has the protective functions of heat insulation, oxidation resistance, gas corrosion resistance, water oxygen corrosion resistance, erosion resistance and the like. The high-temperature protective coating is generally composed of an MCrAlX layer and a ceramic surface layer, wherein the MCrAlX layer mainly plays roles of resisting oxidation, resisting corrosion and coordinating the mismatch of the thermal expansion coefficients of the ceramic surface layer and a metal matrix, and the ceramic surface layer mainly plays roles of heat insulation, resisting oxygen corrosion and resisting erosion.
The existing preparation method of the MCrAlX layer mainly comprises supersonic flame spraying, low-pressure plasma spraying, atmospheric plasma spraying, electron beam physical vapor deposition, magnetron sputtering and the like, and the existing preparation method of the ceramic surface layer mainly comprises an atmospheric plasma spraying process and the like. However, when the MCrAlX layer is sprayed by methods such as supersonic flame spraying, low-pressure plasma spraying, atmospheric plasma spraying, electron beam physical vapor deposition, magnetron sputtering and the like, the problem of uneven coating thickness and uneven surface morphology exists when the part with complex shape is coated due to the 'sight' effect, and when the ceramic surface layer is prepared by adopting atmospheric plasma spraying, the bonding force between the ceramic surface layer and the MCrAlX layer is not strong.
The existing high-temperature protective coating formed by the MCrAlX layer and the ceramic surface layer has the defects that the bonding force between the ceramic surface layer and the MCrAlX layer is not strong, the thickness and the surface morphology of the MCrAlX layer are uneven, the local stress is easy to increase, and the local spalling failure is easy to occur between the MCrAlX layer and the substrate and between the MCrAlX layer and the ceramic surface layer.
Disclosure of Invention
The invention aims to overcome the defect that the MCrAlX layer and the ceramic surface layer of the high-temperature protective coating in the prior art are not strong in bonding force, local peeling failure is easy to occur between the MCrAlX layer and the substrate and between the MCrAlX layer and the ceramic surface layer, and provides a preparation method of the high-temperature protective coating and the coating.
In order to achieve the above object, in a first aspect, the present invention provides a method for preparing a high temperature protective coating, comprising the steps of:
placing a substrate into a pre-plating solution for pre-plating treatment to obtain a pre-plating layer, placing the substrate plated with the pre-plating layer into a first electroplating solution for first electroplating treatment to obtain a first plating layer, placing the substrate plated with the pre-plating layer and the first plating layer into a second electroplating solution for second electroplating treatment to obtain a second plating layer, performing vacuum heat treatment on the substrate plated with the pre-plating layer, the first plating layer and the second plating layer, preparing an alloy coating on the substrate, and continuously depositing a ceramic layer on the surface of the alloy coating through atmospheric plasma spraying;
the pre-plating solution, the first plating solution and the second plating solution are M-based plating solutions, the first plating solution and the second plating solution contain MCrAlX alloy particles, M is Ni or Co or NiCo, X is one or more of Y, ta, hf, si, the granularity of the MCrAlX alloy particles in the first plating solution is Dv90=8-15 mu M, dv50=5-10 mu M and Dv10=2-5 mu M, and the granularity of the MCrAlX alloy particles in the second plating solution is Dv90=16-50 mu M, dv50=11-25 mu M and Dv10=2-10 mu M.
In some preferred embodiments, the MCrAlX alloy particles have a concentration of 10g/L to 100g/L in the first and second plating solutions and the M ions have a concentration of 50g/L to 90g/L in the first and second plating solutions.
In some preferred embodiments, the conditions of the first electroplating process include: the current density was 1A/dm 2 ~3A/dm 2 Performing first stirring and suspending electroplating at intervals of a first preset time, wherein the first preset time is 20 s-40 s, and the time of each first stirring and suspending electroplating is 20 s-40 s;
the conditions of the second electroplating process include: the current density was 1A/dm 2 ~3A/dm 2 And performing second stirring and suspending electroplating at intervals of a second preset time, wherein the second preset time is 50 s-70 s, and the time of each second stirring and suspending electroplating is 20 s-40 s.
More preferably, the electroplating time of the first electroplating treatment is 2-6 h, and the electroplating time of the second electroplating treatment is 1-3 h.
In some preferred embodiments, the MCrAlX alloy particles have a composition comprising: m: 0-10wt% of Cr: 50-70 wt%, al: 25-35 wt%, X: 2-15 wt%.
In some preferred embodiments, the conditions of the vacuum heat treatment include: the temperature is 900-1100 ℃ and the time is 1-8 hours.
In some preferred embodiments, the conditions of the vacuum heat treatment include: the vacuum degree is 0.001Pa-0.1 Pa.
In some preferred embodiments, the atmospheric plasma spray conditions include: the current is 500-600A, the main air volume is 1500-2000L/h, the powder feeding rate is 30-50 g/min, the spraying distance is 120-160 mm, and the granularity of the ceramic powder is 140-325 meshes.
In some preferred embodiments, the conditions of the pre-plating treatment include: the current density was 5A/dm 2 ~7A/dm 2 The preplating time is 3 min-5 min, and the concentration of M ions in the preplating liquid is 25 g/L-60 g/L.
In a second aspect, the present invention provides a process as described in the first aspectThe high-temperature protective coating prepared by the method comprises an alloy coating and a ceramic layer, wherein the alloy coating is positioned on a substrate, the ceramic layer is positioned on the alloy coating, the alloy coating is an MCrAlX alloy coating, M is Ni or Co or NiCo, X is one or more of Y, ta, hf, si, the roughness Ra of one side of the alloy coating close to the ceramic layer is 4-8 mu M, one side of the alloy coating close to the ceramic layer is provided with a TGO layer, the thickness of the TGO layer is 0.5-3.5 mu M, and the components of the TGO layer comprise alpha-Al 2 O 3 。
In the preparation process of the high-temperature protective coating, pre-plating treatment is firstly carried out, the pre-plating solution is M-based plating solution, then first electroplating treatment and second electroplating treatment are carried out, the plating solution of the first electroplating treatment and the second electroplating treatment is also M-based plating solution, the plating solution of the first electroplating treatment and the plating solution of the second electroplating treatment contain MCrAlX alloy particles, and metal elements in the pre-plating layer, the first plating layer and the second plating layer are mutually diffused through vacuum heat treatment, so that the MCrAlX alloy coating can be obtained.
According to the preparation method of the high-temperature protective coating, the matrix is subjected to pre-plating treatment to obtain the pre-plating layer, the pre-plating solution is M-based plating solution, the binding force between the first plating layer and the matrix can be improved, the binding force between the matrix and the MCrAlX alloy coating can be improved, and local peeling failure between the MCrAlX alloy coating and the matrix is inhibited in the preparation process of the composite coating; the preparation process of the MCrAlX alloy coating sequentially comprises a pre-plating process, a first electroplating process and a second electroplating process, adopts a non-sight line process, avoids a sight line effect, obtains a pre-plating layer, a first plating layer and a second plating layer with relatively uniform thickness and surface morphology, and obtains the MCrAlX alloy coating with relatively uniform thickness and surface morphology by mutual diffusion of metal elements in the pre-plating layer, the first plating layer and the second plating layer through vacuum heat treatment, so that the local stress in the MCrAlX alloy coating can be reduced, and local spalling failure between the MCrAlX alloy coating and a substrate and between the MCrAlX alloy coating and a ceramic layer can be inhibited; the first electroplating solution contains MCrAlX alloy particles, the grain size of the MCrAlX alloy particles in the first electroplating solution is Dv90=8μm-15 μm, dv50=5μm-10 μm, dv10=2μm-5 μm, the grain size of the MCrAlX alloy particles in the first electroplating solution is finer, the thickness and appearance of the first coating are uniform in the preparation process of the high-temperature protective coating, the local stress is small, the binding force of the first coating and the pre-coating can be improved, the binding force of the first coating and a substrate can be further improved, the binding force of the MCrAlX alloy coating and the substrate can be improved, the grain size of the alloy particles in the second electroplating solution is Dv90=16μm-50 μm, dv50=11μm-25 μm, dv10=2μm-10 μm, the grain size of the MCrAlX alloy particles in the second electroplating solution is coarser, the binding force of the MCrAlX alloy particles after the surface treatment of the second coating is larger than that of the MCrAlX alloy coating is subjected to the high-temperature protective coating is prepared, and the surface roughness of the MCrAlX ceramic coating is larger than the surface roughness of the MCrAlX coating is deposited by the ceramic coating.
According to the vacuum heat treatment process disclosed by the invention, a stable and compact TGO layer (thermal growth oxide layer) is slowly grown on the surface of the MCrAlX alloy coating while metal elements in the pre-plating layer, the first plating layer and the second plating layer are diffused, so that the growth speed of the TGO on the surface of the MCrAlX alloy coating under the service condition of the composite coating can be slowed down, the uniformity of the TGO layer is improved, the internal stress of the TGO is reduced, the binding force between the MCrAlX alloy coating and the ceramic layer is kept, and the service life of the coating is prolonged.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view of the structure of a coating before vacuum heat treatment according to the present invention.
Fig. 2 is a schematic structural view of the high temperature protective coating of the present invention.
Fig. 3 is a cross-sectional profile view of the high temperature protective coating of example 1 of the present invention.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The inventor of the invention researches and discovers that the existing high-temperature protective coating formed by the MCrAlX layer and the ceramic layer has weak bonding force with the MCrAlX layer, the thickness and the surface morphology of the MCrAlX layer are uneven, so that local stress is easy to increase, and local spalling failure is easy to occur between the MCrAlX layer and the substrate and between the MCrAlX layer and the ceramic layer.
For this first aspect, the present invention provides a method for preparing a high temperature protective coating, comprising the steps of:
placing a substrate into a pre-plating solution for pre-plating treatment to obtain a pre-plating layer, placing the substrate plated with the pre-plating layer into a first electroplating solution for first electroplating treatment to obtain a first plating layer, placing the substrate plated with the pre-plating layer and the first plating layer into a second electroplating solution for second electroplating treatment to obtain a second plating layer, performing vacuum heat treatment on the substrate plated with the pre-plating layer, the first plating layer and the second plating layer, preparing an alloy coating on the substrate, and continuously depositing a ceramic layer on the surface of the alloy coating through atmospheric plasma spraying;
the pre-plating solution, the first plating solution and the second plating solution are M-based plating solutions, the first plating solution and the second plating solution contain MCrAlX alloy particles, M is Ni or Co or NiCo, X is one or more of Y, ta, hf, si, the granularity of the MCrAlX alloy particles in the first plating solution is Dv90=8μm-15 μm, dv50=5μm-10 μm and Dv10=2μm-5 μm, and the granularity of the MCrAlX alloy particles in the second plating solution is Dv90=16μm-50 μm, dv50=11μm-25 μm and Dv10=2μm-10 μm.
The preparation process of the high-temperature protective coating of the invention refers to fig. 1 and 2, an alloy coating is firstly prepared on a substrate, and then a ceramic layer is deposited on the surface of the alloy coating through atmospheric plasma spraying, wherein the preparation method of the alloy coating comprises the steps of sequentially carrying out pre-plating treatment, first electroplating treatment and second electroplating treatment, carrying out vacuum heat treatment on the substrate plated with the pre-plating layer (not shown), the first plating layer and the second plating layer, and carrying out mutual diffusion of metal elements in the pre-plating layer, the first plating layer and the second plating layer in the vacuum heat treatment process to obtain the alloy coating.
In the preparation process of the alloy coating, the pre-plating treatment, the first electroplating treatment, the second electroplating treatment and the vacuum heat treatment are sequentially carried out, and as the electroplating treatment is a non-sight line process, the pre-plating layer, the first plating layer and the second plating layer with relatively uniform thickness and surface morphology can be obtained, after the vacuum heat treatment, the MCrAlX alloy coating with relatively uniform thickness and surface morphology can be obtained, the local stress in the MCrAlX alloy coating can be reduced, the local peeling failure between the MCrAlX alloy coating and a substrate can be restrained, and the local peeling failure between the MCrAlX alloy coating and the ceramic layer can be restrained after the ceramic layer is deposited on the surface of the alloy coating through atmospheric plasma spraying. The invention adopts the electroplating treatment mode to prepare the alloy coating, has low coating cost, low energy consumption and high coating density, does not need roughening treatment such as sand blowing and the like on the substrate, does not damage the substrate, does not cause recrystallization of the surface of the monocrystalline high-temperature alloy substrate, can obtain bonding strength remarkably higher than that of the traditional spraying coating, and does not cause adverse heat influence on the substrate structure in the process of electroplating preparation of the coating compared with the modes such as supersonic flame spraying and the like.
In the preparation process of the alloy coating, the preplating treatment is carried out firstly, and the preplating solution is M-based plating solution, so that the binding force between the first plating layer and the substrate can be improved, and the binding force between the MCrAlX alloy coating and the substrate can be improved; the first electroplating solution used in the first electroplating treatment contains MCrAlX alloy particles, the granularity of the MCrAlX alloy particles in the first electroplating solution is Dv90=8μm-15 μm, dv50=5μm-10 μm and Dv10=2μm-5 μm, the granularity of the MCrAlX alloy particles in the first electroplating solution is finer, and in the preparation process of the alloy coating, the first coating which has uniform thickness, uniform morphology and small local stress and is compact can be obtained, the binding force of the first coating and the pre-coating can be improved, the binding force of the first coating and a matrix can be further improved, and the binding force of the MCrAlX alloy coating and the matrix can be improved; the second electroplating solution used in the second electroplating treatment contains MCrAlX alloy particles, the granularity of the alloy particles in the second electroplating solution is Dv90=16-50 mu m, dv50=11-25 mu m and Dv10=2-10 mu m, the granularity of the MCrAlX alloy particles in the second electroplating solution is thicker, a second plating layer with higher surface roughness can be obtained in the preparation process of the alloy coating, an MCrAlX alloy coating with higher surface roughness can be obtained after heat treatment, and the mechanical embedding area of the MCrAlX alloy coating and the ceramic layer can be increased in the process of depositing the ceramic layer on the surface of the alloy coating by atmospheric plasma spraying, so that the binding force of the MCrAlX alloy coating and the ceramic layer is improved; the vacuum heat treatment ensures that metal elements in the pre-plating layer, the first plating layer and the second plating layer are mutually diffused to form an alloy coating with uniform and compact structure, and meanwhile, a stable and compact TGO layer (thermal growth oxide layer) is slowly grown on the surface of the MCrAlX alloy coating, so that the growth speed of the TGO on the surface of the MCrAlX alloy coating under the service condition of the high-temperature protective coating can be slowed down, the uniformity of the TGO layer is improved, the internal stress of the TGO is reduced, the bonding force between the MCrAlX alloy coating and the ceramic layer is kept, and the service life of the coating is prolonged.
The inventor researches find that MCrAlX alloy particles with larger granularity (Dv90=16-50 μm, dv50=11-25 μm and Dv10=2-10 μm) in the second electroplating solution can obtain larger composite amount in the plating layer than MCrAlX alloy particles with smaller granularity (Dv90=8-15 μm, dv50=5-10 μm and Dv10=2-5 μm) in the first electroplating solution, wherein the composite amount refers to the mass ratio of the MCrAlX alloy particles based on the total mass of the plating layer. In the heat treatment process, metal elements in the first coating and the second coating are mutually diffused, so that the Cr and Al element contents of the MCrAlX alloy coating on one side close to the substrate can be improved, and the oxidation resistance of the coating can be improved.
In the invention, when the Dv90 of the MCrAlX alloy particles in the first electroplating solution is lower than 8 mu m, the Dv50 is lower than 5 mu m, the Dv10 is lower than 2 mu m, and when the Dv90 of the MCrAlX alloy particles in the second electroplating solution is lower than 16 mu m, the Dv50 is lower than 11 mu m and the Dv10 is lower than 2 mu m, the composite amount of the MCrAlX alloy particles in the electroplating process is lower, the Cr and Al element contents in the MCrAlX alloy coating are too low, the oxidation resistance of the coating is influenced, and when the Dv90 of the MCrAlX alloy particles in the first electroplating solution is higher than 15 mu m, the Dv50 is higher than 10 mu m and the Dv10 is higher than 5 mu m, the bonding force between the MCrAlX alloy coating and a matrix is influenced.
The Dv90 of the MCrAlX alloy particles in the first plating solution in the invention may be, for example, specifically 8 μm, 10 μm, 12 μm and 15 μm, the Dv50 may be, for example, specifically 5 μm, 6 μm, 7 μm, 8 μm, 9 μm and 10 μm, and the Dv10 may be, for example, specifically 2 μm, 3 μm, 4 μm and 5 μm; the Dv90 of the MCrAlX alloy particles in the second plating solution may be, for example, 16 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm and 50 μm, the Dv50 may be, for example, 11 μm, 14 μm, 17 μm, 20 μm and 25 μm, and the Dv10 may be, for example, 2 μm, 4 μm, 6 μm, 8 μm and 10 μm.
In some preferred embodiments, the composition of the ceramic layer comprises one or more of partially or fully stabilized zirconia, rare earth zirconate, rare earth silicate, magnesia alumina spinel, and the like.
In some preferred embodiments, the MCrAlX alloy particles have a concentration of 10g/L to 100g/L in the first and second plating solutions and the M ions have a concentration of 50g/L to 90g/L in the first and second plating solutions. Under the preferred scheme, the concentration of MCrAlX alloy particles in the first electroplating solution is 10 g/L-100 g/L, the concentration of M ions is 50 g/L-90 g/L, the plating layer with uniform structure, low roughness and high binding force is more favorable for obtaining, the concentration of MCrAlX alloy particles in the first electroplating solution is not lower than 10g/L, the content of the alloy particles in the first plating layer is higher, the rapid oxidation failure of the plating layer is more favorable for avoiding, the growth of an effective TGO layer is more favorable, the concentration of MCrAlX alloy particles in the second electroplating solution is 10 g/L-100 g/L, the concentration of M ions is 50 g/L-90 g/L, and the alloy plating layer with uniform structure and high alloy particle compound amount is more favorable for obtaining. Further preferably, the concentration of MCrAlX alloy particles in the first electroplating solution is 20 g/L-30 g/L, the concentration of M ions is 70 g/L-90 g/L, and the plating layer with uniform tissue, low roughness and high binding force is more easily obtained, and the concentration of MCrAlX alloy particles in the second electroplating solution is 20 g/L-30 g/L, and the concentration of M ions is 70 g/L-90 g/L, so that the alloy plating layer with uniform tissue and high alloy particle composite amount is more easily obtained.
In some preferred embodiments, the conditions of the first electroplating process include: the current density was 1A/dm 2 ~3A/dm 2 Performing first stirring and suspending electroplating at intervals of a first preset time, wherein the first preset time is 20 s-40 s, and the time of each first stirring and suspending electroplating is 20 s-40 s;
the conditions of the second electroplating process include: the current density was 1A/dm 2 ~3A/dm 2 And performing second stirring and suspending electroplating at intervals of a second preset time, wherein the second preset time is 50 s-70 s, and the time of each second stirring and suspending electroplating is 20 s-40 s.
In the process of stirring suspension electroplating, a stirring paddle is used for mechanically stirring the plating solution.
Under the preferred scheme, stirring suspension plating is carried out at intervals of preset time in the first plating treatment and the second plating treatment, and as the plating solution contains MCrAlX alloy particles, the stirring suspension plating is more beneficial to promoting the plating of Ni or Co or NiCo, and the stirring suspension plating is carried out at intervals of preset time, so that the MCrAlX alloy particles are more beneficial to embedding in the plating growth process, and the MCrAlX particles are compounded in the Ni or Co or NiCo plating; the interval between each stirring suspension plating of the first plating treatment is 20 s-40 s, because the grain size of MCrAlX alloy particles in the first plating solution is smaller, the small particles MCrAlX are not beneficial to the passing of the plating solution after being covered on the surface of a substrate, the first preset time is not higher than 40s, the concentration polarization caused by the failure of the passing of the plating solution is more beneficial to preventing the concentration polarization from easily causing cathodic hydrogen evolution, the internal defect of a plating layer is increased, the growth efficiency of the plating layer is influenced, the binding force between the plating layer and the substrate is reduced, the grain size of the MCrAlX alloy particles is smaller, and the MCrAlX alloy particles can be effectively embedded even if the interval between each stirring suspension plating is shorter and not higher than 40s; the interval between each stirring and suspending electroplating of the second electroplating treatment is 50 s-70 s, and as the grain size of MCrAlX alloy particles in the second electroplating solution is larger, the passing capacity of the plating solution is stronger after the MCrAlX alloy particles with large grain size are covered on the surface of the substrate, the interval time between each stirring and suspending electroplating is not less than 50s, thereby being more beneficial to preventing the large-size MCrAlX particles from being washed away from the plating layer by the stirring plating solution, promoting the embedding of the MCrAlX alloy particles and ensuring the compound quantity of the MCrAlX alloy particles in the second plating layer.
In the preferred embodiment, the current density of the first electroplating treatment is not less than 1A/dm 2 The plating layer with higher composite amount of MCrAlX alloy particles is more favorable to be obtained, and the current density of the first electroplating treatment is not higher than 3A/dm 2 The plating layer with compact structure, low roughness and high binding force with the matrix is more favorable for obtaining the plating layer with high tissue density and low roughness, the first preset time of the first plating treatment is not less than 20s, the MCrAlX alloy particles are embedded in the first plating layer, the high-temperature oxidation resistance of the plating layer is improved, the time of each first stirring and suspending plating is not less than 20s, the plating of Ni or Co or NiCo is more favorable for preventing from being influenced due to concentration polarization caused by the unsmooth passing of plating solution, the time of each first stirring and suspending plating is not more than 40s, the MCrAlX alloy particles are embedded in the first plating layer, and the current density of the second plating treatment is not less than 1A/dm 2 The plating layer with high MCrAlX alloy particle composite and high roughness is more favorable to be obtained, and the current density of the second electroplating treatment is not higher than 3A/dm 2 The plating layer with compact structure and high binding force with the first plating layer is more favorable to be obtained. The second preset time of the second electroplating treatment is not higher than 70s, so that concentration polarization caused by the fact that the plating solution cannot smoothly pass through is prevented from influencing electroplating of Ni or Co or NiCo, the time of each second stirring and suspending electroplating is not lower than 20s, electroplating of Ni or Co or NiCo is facilitated, the time of each second stirring and suspending electroplating is not higher than 40s, and MCrAlX alloy particles are facilitated to be embedded in the second plating layer.
More preferably, the current density of the first electroplating treatment is 1A/dm 2 ~1.5A/dm 2 The current density of the second electroplating treatment was 1.5A/dm 2 ~2A/dm 2 The current density of the first electroplating treatment is not less than 1A/dm 2 The composite amount of MCrAlX alloy particles is more favorably improved, and the current density of the first electroplating treatment is not higher than 1.5A/dm 2 Is more beneficial to obtaining compact structure, low roughness and basePlating layer with high binding force of body, and current density of second electroplating treatment is not less than 1.5A/dm 2 The method is more favorable for obtaining a plating layer with high composite quantity and high roughness of MCrAlX alloy particles, and the current density of the second electroplating treatment is not higher than 2A/dm 2 The plating layer with compact structure and high binding force with the first plating layer is more favorable to be obtained.
According to the invention, the conditions of stirring suspension electroplating comprise that a substrate is positioned at the center of a plating tank, mechanical stirring paddles are positioned at two sides of the plating tank, the rotating speed of the mechanical stirring paddles is 500-700 r/min, the plating tank is provided with an arc-shaped tank bottom, the arc-shaped tank bottom is provided with a ventilation pipeline with air holes, the distance between circle centers of adjacent air holes along the ventilation pipeline is 7-13 mm, and the pressure of gas in the ventilation pipeline is 0.5-0.7 MPa.
In some preferred embodiments, the first electroplating process has an electroplating time of 2h to 6h, and the second electroplating process has an electroplating time of 1h to 3h. The current density in the first plating treatment was 1A/dm 2 ~3A/dm 2 When the electroplating time of the first electroplating treatment is not less than 2 hours, the electroplating time of the first electroplating treatment is not more than 6 hours, the first plating layer with proper thickness is more beneficial to obtaining, and the current density of the second electroplating treatment is 1A/dm 2 ~3A/dm 2 And when the electroplating time of the second electroplating treatment is not less than 1h, the electroplating time of the second electroplating treatment is not more than 3h, and the second plating layer with proper thickness is more beneficial to obtaining.
In some preferred embodiments, the MCrAlX alloy particles have a composition comprising: m: 0-10wt% of Cr: 50-70 wt%, al: 25-35 wt%, X: 2-15 wt%. Under the preferred scheme, the contents of Cr and Al in the MCrAlX alloy particles are respectively 50-70 wt% and 25-35 wt%, so that the high-temperature oxidation resistance of the high-temperature protective coating is improved, the contents of one or more elements such as Y, ta, hf and Si are 2-15 wt%, the high-temperature oxidation resistance of the MCrAlX alloy coating is further improved, and the slow growth of a stable and compact TGO layer in the heat treatment process is facilitated. The content of M element may be 0wt%, 1wt%, 3wt%, 5wt%, 7wt% and 9wt%.
In some preferred embodiments, the conditions of the vacuum heat treatment include: the temperature is 900-1100 ℃ and the time is 1-8 hours. Under the preferred scheme, the temperature of vacuum heat treatment is not lower than 900 ℃, so that the mutual diffusion of metal elements in the pre-plating layer, the first plating layer and the second plating layer is facilitated, a uniform and compact MCrAlX alloy coating with a uniform structure is formed, the continuous TGO layer grows on the surface of the MCrAlX alloy coating, the temperature of vacuum heat treatment is not higher than 1100 ℃, the compact and stable TGO layer grows, the thickness of the TGO layer is controlled to be proper, the bonding force of the ceramic layer and the alloy layer is improved, the time of vacuum heat treatment is not lower than 1h, the mutual diffusion of metal elements in the pre-plating layer, the first plating layer and the second plating layer is facilitated, the formation of a continuous TGO layer is facilitated, the time of vacuum heat treatment is not higher than 8h, and the production efficiency is improved.
In some preferred embodiments, the conditions of the vacuum heat treatment include: the vacuum degree is 0.001Pa-0.1 Pa. Under the preferred scheme, the vacuum degree is not lower than 0.001Pa, the generation of a TGO layer is facilitated, the vacuum degree is not higher than 0.1Pa, the slow growth of the TGO layer is facilitated, the compactness and the stability of the TGO layer are improved, the thickness of the TGO layer is controlled to be proper, and the binding force of the ceramic layer and the alloy layer is improved.
In some preferred embodiments, the atmospheric plasma spray conditions include: the current is 500-600A, the main air volume is 1500-2000L/h, the powder feeding rate is 30-50 g/min, the spraying distance is 120-160 mm, and the granularity of the ceramic powder is 140-325 meshes. Under the preferred scheme, the granularity of the ceramic powder sprayed by the atmosphere plasma is 140-325 meshes, the powder forms good fluidity to obtain good powder feeding characteristics during spraying, the powder is prevented from blocking a powder feeding pipe during spraying, the current is 500-600A, the main air quantity is 1500L/h-2000L/h, the good melting state of the spraying surface of the ceramic powder is ensured, a ceramic layer with uniform structure is obtained, the bonding force of the ceramic layer and an alloy coating is improved, the powder feeding rate is not lower than 30g/min, the ceramic powder overmelting is prevented, the stress of the ceramic layer is reduced, the bonding force of the ceramic layer and the alloy coating is improved, the powder feeding rate is not higher than 50g/min, the ceramic powder melting degree is prevented from being insufficient, the deposition uniformity is improved, the spraying distance is not lower than 120mm, the flame flow impact is prevented from being excessive, the ceramic powder kinetic energy is difficult to deposit, the spraying distance is not higher than 160mm, and the ceramic powder is prevented from being completely cooled and solidified in the air from being unable to deposit. In some preferred embodiments, the thickness of the ceramic layer is 0.05 mm-4 mm, and under the preferred embodiment, the heat insulation effect of the high-temperature protective coating and the bonding strength of the ceramic layer and the MCrAlX alloy coating are improved more favorably.
In some preferred embodiments, the conditions of the pre-plating process include: the current density was 5A/dm 2 ~7A/dm 2 The preplating time is 3 min-5 min, and the concentration of M ions in the preplating liquid is 25 g/L-60 g/L. Under the preferred scheme, the current density of the pre-plating treatment is not lower than 5A/dm 2 Is more beneficial to improving the binding force between the preplating layer and the matrix, and the current density is not higher than 7A/dm 2 The method is more beneficial to preventing the excessive hydrogen evolution of the cathode from influencing the binding force between the pre-plating layer and the matrix, the pre-plating time is 3-5 min, the pre-plating layer with proper thickness is more beneficial to being obtained, the situation that the pre-plating layer is too thin or too thick to cause too large internal stress, the effect of improving the binding force between the first plating layer and the matrix can not be achieved, and the concentration of M ions in the pre-plating solution is 25-60 g/L, so that the quality of the plating layer is improved.
In a second aspect, the present invention provides a high temperature protective coating prepared by the preparation method of the first aspect, the coating comprises an alloy coating and a ceramic layer, the alloy coating is positioned on a substrate, the ceramic layer is positioned on the alloy coating, the alloy coating is an MCrAlX alloy coating, M is Ni or Co or NiCo, X is one or more of Y, ta, hf, si, the roughness Ra of the alloy coating on the side close to the ceramic layer is 4 μm to 8 μm, the alloy coating on the side close to the ceramic layer has a TGO layer, the thickness of the TGO layer is 0.5 μm to 3.5 μm, and the composition of the TGO layer comprises α -Al 2 O 3。
According to the high-temperature protective coating disclosed by the invention, the roughness Ra of one side of the alloy coating close to the ceramic layer is 4-8 mu m, the bonding strength of the MCrAlX alloy coating and a substrate is greater than 30MPa, the bonding strength of the MCrAlX alloy coating and the ceramic layer is greater than 18MPa, and local spalling failure is not easy to occur between the MCrAlX alloy coating and the substrate and between the MCrAlX alloy coating and the ceramic layer. The side of the alloy coating, which is close to the ceramic layer, is provided with a micron-sized compact continuous TGO layer, so that the growth speed of the TGO on the surface of the MCrAlX alloy coating of the high-temperature protective coating under the service condition can be slowed down, the uniformity of the TGO layer is improved, the internal stress of the TGO is reduced, the binding force between the MCrAlX alloy coating and the ceramic layer is maintained, and the service life of the coating is prolonged.
The invention will be further described in detail with reference to specific examples.
Example 1
Step one: immersing a GH4169 metal wafer in acetone for ultrasonic cleaning for 5min, immersing the GH4169 wafer in deionized water for ultrasonic cleaning for 3min, taking out and drying, placing the dried GH4169 wafer in a preplating solution containing nickel chloride and boric acid, wherein the concentration of nickel ions in the preplating solution is 29.63g/L (nickel ions are added in the form of nickel chloride hexahydrate), the concentration of boric acid is 40g/L, and the concentration of boric acid is 6A/dm 2 Performing impact nickel preplating treatment for 4min under the current density of (2) to obtain a metal wafer plated with a nickel preplating layer, taking out the metal wafer and washing the metal wafer with deionized water;
step two: the metal wafer plated with the nickel preplating layer obtained in the step one is placed into a first electroplating solution containing nickel sulfate, nickel chloride, boric acid and CrAlY alloy particles at 1.5A/dm 2 Carrying out first electroplating treatment for 2 hours to obtain a metal wafer plated with a nickel pre-plating layer and a first plating layer, then taking out and washing the metal wafer with deionized water, wherein the concentration of CrAlY alloy particles in the first electroplating solution is 30g/L, the concentration of nickel ions is 79.3g/L, the concentration of boric acid is 36g/L, the content of Cr in the CrAlY alloy particles is 65.67wt%, the content of Al is 31.90wt%, the content of Y is 2.43wt%, the particle size distribution of the CrAlY alloy particles is Dv90 is 12.5 mu m, dv50 is 6.94 mu m and Dv10 is 3.55 mu m, and in the first electroplating treatment process, stirring and suspending electroplating is carried out every 30s, and each stirring and suspending electroplating lasts for 30s;
step three: the metal wafer plated with the nickel preplating layer and the first plating layer obtained in the second step is placed into a second electroplating solution containing nickel sulfate, nickel chloride, boric acid and CrAlY alloy particles at the speed of 2A/dm 2 Performing a second electroplating treatment for 1h to obtain a metal wafer plated with a nickel preplating layer, a first plating layer and a second plating layer, and then taking out andwashing with deionized water, wherein the concentration of CrAlY alloy particles in the second electroplating solution is 30g/L, the concentration of nickel ions is 79.3g/L, the concentration of boric acid is 36g/L, the content of Cr in the CrAlY alloy particles is 63.80wt%, the content of Al is 33.13wt%, the content of Y is 3.07wt%, the particle size distribution of the CrAlY alloy particles is Dv90 of 30.5 mu m, dv50 of 18.0 mu m and Dv10 of 8.03 mu m, and in the second electroplating treatment process, stirring and suspending electroplating is carried out every 60 seconds, and each stirring and suspending electroplating lasts for 30 seconds;
step four: placing the metal wafer plated with the nickel preplating layer, the first plating layer and the second plating layer obtained in the third step into a vacuum sintering furnace, and pumping the air pressure in the furnace to 8 multiplied by 10 -3 Pa is maintained, the temperature in the furnace is raised to 1100 ℃ and kept for 2 hours, and the metal wafer plated with the alloy coating is obtained after natural cooling along with the furnace in a vacuum environment.
Step five: clamping the metal wafer plated with the alloy coating on a spraying tool, depositing ceramic powder with granularity of 140-325 meshes on the alloy coating by adopting an atmospheric plasma spraying method, wherein the atmospheric plasma spraying current is 580A, the main gas quantity is 1800L/h, the powder feeding rate is 40g/min, the spraying distance is 150mm, and the ceramic powder comprises ZrO 2 ：94 wt.%，Y 2 O 3 :6, wt percent, and finishing spraying when the average thickness of the ceramic surface layer reaches 200 mu m, thereby obtaining the metal wafer with the high-temperature protective coating. The appearance of the high-temperature protective coating in the embodiment 1 is shown in fig. 3, the uppermost layer is a ceramic layer, the lowermost layer is a substrate, the MCrAlX alloy coating is tightly combined with the substrate and the ceramic layer respectively, one side of the MCrAlX alloy coating close to the substrate is smoother, one side of the MCrAlX alloy coating close to the ceramic layer is rougher, the MCrAlX alloy coating is formed by electroplating twice, one side of the MCrAlX alloy coating close to the substrate and one side of the MCrAlX alloy coating close to the ceramic layer are different in appearance due to different phase distribution, phase proportion and uniformity, but no obvious interface exists between the two sides, in the embodiment 1, after heat treatment, a TGO layer grows on the surface of the MCrAlX alloy coating, the thickness of the TGO layer is 1 mu m, and the thickness of the TGO layer is measured to obtain the average value of the thickness of more than 5 positions.
Example 2
Reference example 1 was conducted, except that in the second step, the concentration of CrAlY alloy particles in the first plating solution was 5g/L.
Example 3
Reference example 1 was made, except that in step three, the concentration of CrAlY alloy particles in the second plating solution was 5g/L.
Example 4
Reference example 1, which differs in that in step two, 0.5A/dm 2 Is subjected to a first plating process.
Example 5
Reference example 1, which differs in that in step three, the ratio was 0.5A/dm 2 And (3) performing a second electroplating treatment at the current density.
Example 6
Reference example 1 was made, except that in the second step, the suspension plating was performed with stirring every 50 s.
Example 7
Reference example 1 was made, except that in step three, the suspension plating was performed with stirring every 40s.
Example 8
Reference example 1 was made, except that in step four, the furnace was warmed to 1200 ℃ and held for 2 hours. After heat treatment, a TGO layer grows on the surface of the MCrAlX alloy coating, and the thickness of the TGO layer is 3 mu m.
Example 9
Reference example 1 was made, except that in step four, the temperature in the furnace was raised to 800℃and kept at that temperature for 2 hours. After heat treatment, no continuous TGO layer was formed on the MCrAlX alloy coating surface.
Example 10
Reference example 1 was made, except that in step four, the gas pressure in the furnace was drawn to 0.2Pa and maintained. After heat treatment, a TGO layer grows on the surface of the MCrAlX alloy coating, and the thickness of the TGO layer is 3.5 mu m.
Example 11
Reference example 1 was made, except that in step five, the spray distance of the atmospheric plasma spray was 250mm.
Comparative example 1
Reference example 1 was made, except that step three was not performed, and in step two, the first plating treatment was performed for 3h20min. The MCrAlX alloy coating is tightly combined with the matrix, the combination between the MCrAlX alloy coating and the ceramic layer is not tight enough, the side of the MCrAlX alloy coating close to the ceramic layer is smoother, the content of Cr and Al elements in the coating is reduced, and the high-temperature oxidation resistance of the coating is reduced.
Comparative example 2
Reference example 1 was made, except that step two was not performed, and in step three, the second plating treatment was performed for 2h30min. The MCrAlX alloy coating is not tightly combined with the matrix, and is tightly combined with the ceramic layer, so that the uniformity and compactness of the internal structure of the coating are reduced.
Test case
The roughness of the side of the MCrAlX alloy coating of examples 1-11 and comparative examples 1-2, which is close to the ceramic layer, and the bonding strength of the MCrAlX alloy coating to the substrate were examined, and the examination results are shown in Table 1. Roughness was measured using a coarser machine and bond strength was measured using the adhesive tensile method (GB/T8642-2002). The bonding strength of the alloy layer and the matrix is measured after the alloy coating is obtained after heat treatment, and the bonding strength of the alloy layer and the ceramic layer is measured after the ceramic layer is prepared. In general, the bonding strength between the alloy layer and the substrate is far greater than that between the ceramic layer and the alloy layer, so that the ceramic layer is bonded to the measuring joint on the back surface of the substrate, the upper surface of the ceramic layer is bonded to the measuring joint, and when the bonding strength between the alloy layer and the ceramic layer is measured by an adhesive stretching method, fracture occurs between the alloy coating and the ceramic layer.
TABLE 1
Sequence number Roughness of the alloy layer on the side close to the ceramic layer Bonding strength of alloy layer to substrate Bonding strength of alloy layer and ceramic layer
Example 1 Ra 7.3μm ＞75MPa 43.2MPa
Example 2 Ra 7.0μm ＞75MPa 39.7MPa
Example 3 Ra 4.2μm ＞75MPa 23.8MPa
Example 4 Ra 7.1μm ＞75MPa 39.3MPa
Example 5 Ra 3.9μm ＞75MPa 18.8MPa
Example 6 Ra 7.6μm 35.9Mpa Because the bonding force between the alloy layer and the matrix is limited, the measurement cannot be carried out
Example 7 Ra 5.9μm ＞75MPa 27.0MPa
Example 8 Ra 7.4μm ＞75MPa 22.7MPa
Example 9 Ra 7.6μm ＞75MPa 38.5MPa
Example 10 Ra 7.3μm ＞75MPa 25.9MPa
Example 11 Ra 7.2μm ＞75MPa 18.9MPa
Comparative example 1 Ra 2.7μm ＞75MPa 12.0MPa
Comparative example 2 Ra 7.7μm 19.7MPa Because the binding force between the alloy layer and the matrix is poor, the alloy layer falls off and cannot be measured
As can be seen from comparative examples 1 and 1 to 2, the first plating using a plating solution containing MCrAlX alloy particles having a small particle size and the second plating using a plating solution containing MCrAlX alloy particles having a large particle size are sequentially advantageous in simultaneously obtaining high bonding strength between the alloy layer and the substrate and between the alloy layer and the ceramic layer, and comparative examples 1 and 3, in which the concentration of MCrAlX alloy particles in the second plating solution is not less than 10g/L, the compounding amount of alloy particles is more advantageous, the bonding strength between the alloy layer and the ceramic layer is improved, and comparative examples 1 and 5, the current density of the second plating treatment is not less than 1A/dm 2 The method is more favorable for improving the compounding amount of alloy particles, improving the bonding strength between an alloy layer and a ceramic layer, comparing the example 1 and the example 6, wherein the interval between each stirring suspension plating of the first plating treatment is not higher than 40s, more favorable for improving the bonding strength between the alloy layer and a matrix, comparing the example 1 and the example 7, the interval between each stirring suspension plating of the second plating treatment is not lower than 50s, more favorable for embedding MCrAlX particles, improving the roughness of the alloy layer close to the ceramic layer side, improving the bonding strength between the alloy layer and the ceramic layer, comparing the example 1, the example 8 and the example 9, and the vacuum heat treatment at 900-1100 ℃, more favorable for improving the bonding strength between the alloy layer and the ceramic layer, comparing the example 1 and the example 10, wherein the vacuum degree of the vacuum heat treatment is not higher than 0.1Pa, the spraying distance of atmospheric plasma is not higher than 160mm, and more favorable for improving the bonding strength between the alloy layer and the ceramic layer.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (10)

1. The preparation method of the high-temperature protective coating is characterized by comprising the following steps of:
placing a substrate into a pre-plating solution for pre-plating treatment to obtain a pre-plating layer, placing the substrate plated with the pre-plating layer into a first electroplating solution for first electroplating treatment to obtain a first plating layer, placing the substrate plated with the pre-plating layer and the first plating layer into a second electroplating solution for second electroplating treatment to obtain a second plating layer, performing vacuum heat treatment on the substrate plated with the pre-plating layer, the first plating layer and the second plating layer, preparing an alloy coating on the substrate, and continuously depositing a ceramic layer on the surface of the alloy coating through atmospheric plasma spraying;
the pre-plating solution, the first plating solution and the second plating solution are M-based plating solutions, the first plating solution and the second plating solution contain MCrAlX alloy particles, M is Ni or Co or NiCo, X is one or more of Y, ta, hf, si, the granularity of the MCrAlX alloy particles in the first plating solution is Dv90=8-15 mu M, dv50=5-10 mu M and Dv10=2-5 mu M, and the granularity of the MCrAlX alloy particles in the second plating solution is Dv90=16-50 mu M, dv50=11-25 mu M and Dv10=2-10 mu M.
2. The method according to claim 1, wherein the concentration of the MCrAlX alloy particles in the first plating solution and the second plating solution is 10g/L to 100g/L, and the concentration of M ions in the first plating solution and the second plating solution is 50g/L to 90g/L.
3. The method of claim 1, wherein the conditions of the first electroplating process include: the current density was 1A/dm 2 ~3A/dm 2 Performing first stirring and suspending electroplating at intervals of a first preset time, wherein the first preset time is 20 s-40 s, and the time of each first stirring and suspending electroplating is 20 s-40 s;
the conditions of the second electroplating process include: the current density was 1A/dm 2 ~3A/dm 2 Performing second stirring and suspending electroplating at intervals of second preset time, wherein the second preset time is 50 s-70 s, and each time the second stirring and suspending electroplating is performedThe time is 20 s-40 s.
4. The method according to claim 2, wherein the first electroplating treatment has an electroplating time of 2h to 6h and the second electroplating treatment has an electroplating time of 1h to 3h.
5. The method of claim 1, wherein the MCrAlX alloy particles have a composition comprising: m: 0-10wt% of Cr: 50-70 wt%, al: 25-35 wt%, X: 2-15 wt%.
6. The method according to claim 1, wherein the conditions of the vacuum heat treatment include: the temperature is 900-1100 ℃ and the time is 1-8 hours.
7. The method according to claim 1, wherein the conditions of the vacuum heat treatment include: the vacuum degree is 0.001Pa-0.1 Pa.
8. The method of claim 1, wherein the atmospheric plasma spraying conditions comprise: the current is 500-600A, the main air volume is 1500-2000L/h, the powder feeding rate is 30-50 g/min, the spraying distance is 120-160 mm, and the granularity of the ceramic powder is 140-325 meshes.
9. The method according to claim 1, wherein the conditions of the pre-plating treatment include: the current density was 5A/dm 2 ~7A/dm 2 The preplating time is 3 min-5 min, and the concentration of M ions in the preplating liquid is 25 g/L-60 g/L.
10. The high temperature protective coating prepared by the preparation method according to any one of claims 1 to 9, wherein the coating comprises an alloy coating and a ceramic layer, the alloy coating is positioned on a substrate, the ceramic layer is positioned on the alloy coating, the alloy coating is an MCrAlX alloy coating, M is Ni or Co or NiCo, and X is selected from Y, ta and HfOne or more of Si, wherein the roughness Ra of one side of the alloy coating close to the ceramic layer is 4-8 mu m, one side of the alloy coating close to the ceramic layer is provided with a TGO layer, the thickness of the TGO layer is 0.5-3.5 mu m, and the composition of the TGO layer comprises alpha-Al 2 O 3 。
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