CN114686862B - Chromium oxide and zirconium oxide composite coating and preparation method thereof - Google Patents
Chromium oxide and zirconium oxide composite coating and preparation method thereof Download PDFInfo
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1241—Metallic substrates
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1291—Process of deposition of the inorganic material by heating of the substrate
Abstract
The invention provides a chromium oxide and zirconium oxide composite coating and a preparation method thereof, which are applicable to hydrogen permeation resistance and isotope permeation thereof in various hydrogen-related fields such as fusion reactor cladding module structural materials, hydrogen storage devices and the like. The composite coating is a single-layer composite coating or a multi-layer gradient composite coating, each layerLayers are all made of Cr 2 O 3 And ZrO 2 The composite coating combines the hydrogen/deuterium/tritium permeation resistance characteristics of the zirconium oxide and the chromium oxide, maintains the good toughness of the zirconium oxide coating on the basis of improving the hydrogen/deuterium/tritium permeation resistance of the single-phase zirconium oxide coating, and prolongs the service life of the zirconium oxide coating. The preparation process combining sol-gel with dip-coating can be suitable for coating the surface of a material with a complex structure, and the practical value of the composite coating is greatly improved. The whole process method is simple, healthy and environment-friendly, and is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of material surface protection, in particular to a chromium oxide and zirconium oxide composite coating and a preparation method thereof.
Background
Hydrogen and hydrogen isotopes such as tritium and deuterium are easy to permeate into the metal structure material, so that the strength and plasticity of the structure material are reduced, the performance is deteriorated, the service cycle of the structure material is shortened, and the service safety is damaged. At present, the problems of serious permeation of hydrogen and isotopes thereof exist in cladding module structural materials of fusion reactors, heat collecting tubes for solar thermal power generation, oil pump cylinders, oil pipelines and other hydrogen-related devices, so that a coating material for blocking hydrogen permeation, namely a coating for blocking hydrogen/deuterium/tritium permeation, needs to be prepared on the surface of the structural materials. Among various coating materials, the ceramic has the advantages of low hydrogen permeability and hydrogen dissolution rate, high mechanical hardness, good thermal stability, corrosion resistance and the like, and is considered as a preferred hydrogen/deuterium/tritium permeation resistant material.
Most of the studies on hydrogen permeation-resistant coatings currently carried out are single-component single-layer or multi-layer coating material systems, such as single Cr 2 O 3 、Al 2 O 3 、Er 2 O 3 Coating and Al 2 O 3 /FeAl、Al 2 O 3 /Cr 2 O 3 、Er 2 O 3 The traditional single coating has insufficient permeation resistance to structural materials, poor film-substrate combination and good hydrogen permeation resistance, is the main development direction of the hydrogen permeation resistant coating in the future,
CN104708863A discloses an organic chemical vapor deposition or magnetron sputtering preparationAl of (2) 2 O 3 /Cr 2 O 3 The composite coating combines the hydrogen permeation resistance of the chromium oxide layer and the aluminum oxide layer, but still has the problems of complex preparation process and incapability of completely covering parts with complex shapes.
In summary, the prior art also lacks a composite hydrogen/deuterium/tritium permeation barrier coating which is formed by compounding two phases, has a simple preparation process and meets the covering requirements of complex parts.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the chromium oxide and zirconium oxide composite coating and the preparation method thereof, the composite coating combines the hydrogen permeation resistance characteristics of the chromium oxide and the zirconium oxide, has excellent high-temperature deuterium resistance, and has the advantages of simple preparation process of the coating, capability of covering complex parts with different shapes and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a composite coating of chromium oxide and zirconium oxide is prepared from Cr 2 O 3 And ZrO 2 The two phases are compounded.
Furthermore, the composite coating is a single-layer composite coating or a multi-layer composite coating, and the thickness of the composite coating is 50nm-4um.
Furthermore, the molar ratio of the two elements of chromium and zirconium in the composite coating is 1.
A preparation method of a chromium oxide and zirconium oxide composite coating comprises the following steps:
(1) Preparing a chromium-zirconium mixed sol, namely taking zirconium salt, chromium salt, absolute ethyl alcohol, acetone and glacial acetic acid as raw materials, fully stirring and dissolving to form a clear and transparent mixed sol, wherein the mass fraction of the zirconium salt is 2-10%, the mass fraction of the chromium salt is 0.2-30%, the absolute ethyl alcohol is 30-150 ml, the acetone is 2-20 ml, and the glacial acetic acid is 10-180ul;
(2) Uniformly coating the chromium-zirconium mixed sol obtained in the step (1) on a stainless steel substrate by adopting a dipping and pulling method to obtain a precursor coating, namely soaking a stainless steel substrate into the mixed sol, controlling the rising speed of the substrate to be 50-500 um/s, putting the substrate into a drying oven for drying and shaping after the substrate completely emerges from the liquid level, wherein the drying temperature is 40-80 ℃, and the drying time is 1-3 h;
(3) Placing the precursor coating obtained in the step (2) in a muffle furnace at the temperature of 200-400 ℃ for heat preservation for 20-60 min to remove organic matters in the coating, and cooling;
(4) Repeating the steps (1) to (3) for 1 to 20 times, and finally carrying out heat treatment for 0.5 to 5 hours in a muffle furnace at the temperature of between 500 and 800 ℃ under the atmosphere to form the composite coating.
Further, the zirconium salt comprises one of zirconium acetate, zirconium nitrate, zirconium isopropoxide and zirconium oxychloride or a mixture thereof.
Further, the chromium salt comprises one or a mixture of chromium acetate, chromium nitrate, chromium isopropoxide and chromium oxychloride.
The invention has the following beneficial effects:
1. the invention combines the hydrogen permeation resistance of chromium oxide and zirconium oxide to prepare Cr 2 O 3 /ZrO 2 The composite coating has more excellent hydrogen/deuterium/tritium permeation resistance;
2. the invention combines the thermal expansion coefficient of the chromium oxide close to the base material and the good toughness of the zirconium oxide coating, and can adjust the composition proportion of the chromium oxide and the zirconium oxide of the composite coating, improve the thermal compatibility of the coating and the matrix and prolong the service life;
3. the preparation method disclosed by the invention is simple in process flow, capable of meeting the coating requirement of the surface coating of the structural component with the complex shape, strong in repeatability and suitable for large-scale production.
Drawings
FIG. 1 is a graph of deuterium ion permeation current for a high temperature gas phase deuterium inhibition experiment for a pure zirconia coating;
FIG. 2 is a diagram of deuterium ion permeation current in a high temperature gas phase deuterium inhibition experiment with a molar ratio of Cr to Zr of 1 according to an embodiment of the present invention;
FIG. 3 is a deuterium ion permeation current diagram of a deuterium inhibition experiment at a high temperature in which the molar ratio of Cr to Zr is 2;
FIG. 4 is a diagram of deuterium ion permeation current in a high temperature gas phase deuterium inhibition experiment with a molar ratio of Cr to Zr of 3 according to an embodiment of the present invention;
FIG. 5 is an SEM image of a coating with a Cr and Zr molar ratio of 2 according to the example of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
Pure ZrO 2 The hydrogen/deuterium/tritium permeation resistant coating is prepared by the following method:
1. polishing 321L stainless steel to mirror surface, ultrasonic treating with ethanol for 15min, removing ions, and cleaning with acetone.
2. Weighing 3g of zirconium acetate, adding 50ml of absolute ethyl alcohol, 2.5ml of acetone and 50 mu L of glacial acetic acid, placing the mixture in a magnetic stirrer, stirring for about 10 hours until the mixture is fully dissolved to be in a clear transparent state, and standing for 24 hours to obtain the zirconium sol.
3. The dipping and pulling process is completed by a pulling machine, the pulling speed is uniform in the whole process, the pulling speed is set to be 400 mu m/s, the wet sol and the base material after pulling are placed at 80 ℃ for drying for 1h, the temperature is kept at 400 ℃ for 30min, the second layer is pulled after the wet sol and the base material are cooled, the previous operations are repeated, the pulling is carried out for three times, finally, the heat treatment is carried out, the temperature is kept at 600 ℃ for 1h, and the temperature rising rate is 5 ℃/min.
Example 2
Cr and Zr molar ratio of 1 2 O 3 /ZrO 2 The composite hydrogen/deuterium/tritium permeation resistant coating is prepared by the following method:
1. polishing 321L stainless steel to mirror surface, ultrasonic treating with ethanol for 15min, removing ions, and cleaning with acetone.
2. Weighing 3g of zirconium acetate, adding 50ml of absolute ethyl alcohol, 2.5ml of acetone and 50 mul of glacial acetic acid, placing the mixture in a magnetic stirrer, stirring for about 10 hours until the mixture is fully dissolved to be in a clear and transparent state, and standing for 24 hours to obtain zirconium sol; then 1.23g of chromium acetate is added into the mixture, and the mixture is stirred for about 1 hour by ultrasonic wave for 0.5 hour or magnetic force to obtain mixed sol.
3. The dipping and pulling process is completed by a pulling machine, the pulling speed is uniform in the whole process, the pulling speed is set to be 400 mu m/s, the wet sol and the base material after pulling are placed at 80 ℃ for drying for 1h, the temperature is kept at 400 ℃ for 30min, the second layer is pulled after the wet sol and the base material are cooled, the previous operations are repeated, the pulling is carried out for three times, finally, the heat treatment is carried out, the temperature is kept at 600 ℃ for 1h, and the temperature rising rate is 5 ℃/min.
Example 3
Cr and Zr with a molar ratio of 2 2 O 3 /ZrO 2 The composite hydrogen/deuterium/tritium permeation resistant coating is prepared by the following method:
1. polishing 321L stainless steel to mirror surface, ultrasonic treating with ethanol for 15min, removing ions, and cleaning with acetone.
2. Weighing 3g of zirconium acetate, adding 50ml of absolute ethyl alcohol, 2.5ml of acetone and 50 mul of glacial acetic acid, placing the mixture in a magnetic stirrer, stirring for about 10 hours until the mixture is fully dissolved to be in a clear and transparent state, and standing for 24 hours to obtain zirconium sol; then 2.46g of chromium acetate is added into the mixed sol, and the mixed sol is obtained by ultrasonic stirring for 0.5h or magnetic stirring for about 1 h.
3. The dip-coating process is completed by a coating machine, the coating speed in the whole process is uniform, the coating speed is set to be 400 mu m/s, the wet sol after coating and the substrate are dried for 1h at 80 ℃, the temperature is kept for 30min at 400 ℃, the second layer is coated after the wet sol is cooled, the previous operations are repeated, coating and coating are carried out for three times, finally, heat treatment is carried out, the temperature is kept for 1h at 600 ℃, and the heating rate is 5 ℃/min.
Example 4
Cr and Zr at a molar ratio of 3 2 O 3 /ZrO 2 The composite hydrogen/deuterium/tritium permeation resistant coating is prepared by the following method:
1. polishing 321L stainless steel to mirror surface, ultrasonic treating with ethanol for 15min, removing ions, and cleaning with acetone.
2. Weighing 3g of zirconium acetate, adding 50ml of absolute ethyl alcohol, 2.5ml of acetone and 50 mul of glacial acetic acid, placing the mixture in a magnetic stirrer, stirring for about 10 hours until the mixture is fully dissolved to be in a clear and transparent state, and standing for 24 hours to obtain zirconium sol; then 3.69g of chromium acetate is added into the mixed sol, and the mixed sol is obtained after ultrasonic stirring for 0.5h or magnetic stirring for about 1 h.
3. The dipping and pulling process is completed by a pulling machine, the pulling speed is uniform in the whole process, the pulling speed is set to be 400 mu m/s, the wet sol and the base material after pulling are placed at 80 ℃ for drying for 1h, the temperature is kept at 400 ℃ for 30min, the second layer is pulled after the wet sol and the base material are cooled, the previous operations are repeated, the pulling is carried out for three times, finally, the heat treatment is carried out, the temperature is kept at 600 ℃ for 1h, and the temperature rising rate is 5 ℃/min.
Referring to FIGS. 1-4, cr can be seen from the deuterium ion permeation current diagrams of the high temperature vapor deuterium inhibition experiments of the coatings prepared in comparative example 1 and examples 2, 3 and 4 2 O 3 /ZrO 2 Pure ZrO when high-temperature gas phase deuterium ion permeation current of composite coating reaches steady state at 500 DEG C 2 The deuterium permeation reduction factor of the alloy is calculated to be 25, 140, 256 and 58 respectively for 321L stainless steel, which indicates that Cr is lower by one order of magnitude 2 O 3 /ZrO 2 ZrO of composite coating with deuterium permeation resistance ratio of single system 2 The performance of the coating is improved by nearly 10 times.
Comparing examples 2, 3 and 4, the influence of Cr and Zr contents with different molar ratios on the performance of the coating is relatively large, and when the molar ratio is 2.
FIG. 5 shows Cr and Zr molar ratios of 2 2 O 3 /ZrO 2 SEM image of the surface of the composite coating shows that the coating is compact and has no defects, and the matrix phase of the coating is very fine ZrO 2 Crystal grains and white Cr precipitated on the surface 2 O 3 Second phase grains. With mono-ZrO 2 In contrast, cr 2 O 3 Has better hydrogen/deuterium/tritium permeation resistance, so that the permeation retardation of the composite coating to hydrogen and isotopes can be further improved.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. A preparation method of a chromium oxide and zirconium oxide composite coating is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing a chromium-zirconium mixed sol, namely taking zirconium salt, chromium salt, absolute ethyl alcohol, acetone and glacial acetic acid as raw materials, and fully stirring and dissolving the raw materials to form a clear and transparent mixed sol, wherein the mass fraction of the zirconium salt is 2-10%, the mass fraction of the chromium salt is 0.2-30%, the mass fraction of the absolute ethyl alcohol is 30-150 ml, the mass fraction of the acetone is 2-20 ml, and the mass fraction of the glacial acetic acid is 10-180 mu l;
(2) Uniformly coating the chromium-zirconium mixed sol obtained in the step (1) on a stainless steel substrate by adopting a dipping and pulling method to obtain a precursor coating, namely soaking a stainless steel substrate into the mixed sol, controlling the rising speed of the substrate to be 50-500 mu m/s, putting the substrate into an oven for drying and shaping after the substrate completely emerges from the liquid surface, wherein the drying temperature is 40-80 ℃, and the drying time is 1-3 hours;
(3) Placing the precursor coating obtained in the step (2) in a muffle furnace at 200-400 ℃ for heat preservation for 20-60 min to remove organic matters in the coating, and cooling;
(4) Repeating the steps (1) to (3) for 1 to 20 times, and finally performing heat treatment for 0.5 to 5 hours in a muffle furnace at the temperature of 500 to 800 ℃ under the atmospheric atmosphere to form the composite coating;
the composite coating consists of Cr 2 O 3 And ZrO 2 The coating is characterized by being formed by compounding two phases, wherein the thickness of the composite coating is 50nm-4 mu m, and the molar ratio of two elements of chromium to zirconium in the composite coating is 1.
2. The method of preparing a chromium oxide and zirconium oxide composite coating according to claim 1, wherein: the zirconium salt comprises one or a mixture of zirconium acetate, zirconium nitrate, zirconium isopropoxide and zirconium oxychloride.
3. The method of preparing a chromium oxide and zirconium oxide composite coating according to claim 1, wherein: the chromium salt comprises one or a mixture of chromium acetate, chromium nitrate, chromium isopropoxide and chromium oxychloride.
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