CN109943872B - Preparation method of composite coating for protecting Cr-containing stainless steel in molten fluoride salt - Google Patents
Preparation method of composite coating for protecting Cr-containing stainless steel in molten fluoride salt Download PDFInfo
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Abstract
The invention discloses a preparation method of a composite coating for protecting Cr-containing stainless steel in molten fluoride salt, which comprises the following steps: 1) selecting stainless steel as a cathode substrate and selecting a nickel sheet as an anode substrate; 2) placing the cathode and anode base materials in a nano composite electroplating bath, and carrying out nano composite pulse electroplating while stirring to prepare a Ni (NiO) transition layer; 3) stirring the base material in a bright nickel plating bath for nickel plating; 4) placing the base material into a container filled with inert gas for heat treatment, wherein the temperature of the heat treatment is 850-900 ℃, the time is 8 hours, the Cr in the base material reacts with the NiO in the transition layer, and then the Cr grows out in situ on the surface2O3A diffusion barrier. The method has the advantages of simple and convenient operation, high coating controllability, good corrosion prevention effect, reduced electroplating time, less additives of the plating solution, reduced cost, contribution to reducing the pollution to the environment, and good compactness and bonding force of the prepared coating.
Description
Technical Field
The invention belongs to the technical field of metal material surface treatment, and particularly relates to a preparation method of a Cr-containing stainless steel protective composite coating used in molten fluoride salt.
Background
The fused fluoride salt is a novel high-temperature and high-heat-flow-density heat transfer and storage medium, has unique thermophysical and thermochemical properties such as high heat capacity, high melting point, high heat conductivity, high radiation stability, low neutron capture cross section, low saturated vapor pressure, low viscosity and the like, and is widely applied to the field of high-temperature industry at present. However, molten fluorides are very corrosive at high temperatures. When corresponding equipment or a corresponding system is used, the active dissolution of metal elements of the metal-based structural material is easy to occur in fluoride in a high-temperature molten state, the service life of the material is obviously shortened, and the method is also one of main obstacles for restricting the industrial application of the molten fluoride salt. In recent years, with the development of techniques such as molten salt galvanic reactors, post-processing of spent fuels, molten salt heat storage materials, and the like, the problem of molten fluoride corrosion has received much attention. Mo-containing low Cr nickel-based alloys, represented by Hastelloy N alloys (mainly comprising Ni-7Cr-16Mo-5Fe), are generally considered to have good fluoride corrosion resistance, but such alloys still have unavoidable formation of chromium-poor regions and pores due to selective corrosion of active elements during long-term operation.
At present, a method of applying a diffusion barrier between a Ni coating and a matrix alloy is generally adopted to inhibit the outward diffusion of elements such as Cr and the like in the matrix alloy, so that the molten fluoride corrosion resistance of the Ni coating can be obviously improved. The ceramic diffusion barrier has certain advantages in inhibiting the out-diffusion of elements. The oxide ceramic diffusion barrier is generally prepared by a pre-oxidation thermal growth method, an in-situ growth method and the like. The existing researchers use an in-situ growth method to prepare an oxide diffusion barrier between a cold spraying coating and a substrate, but find that the bonding force between the coating and the substrate under the cold spraying process is poor, so that the microscopic defects of the subsequently prepared diffusion barrier cannot be avoided, and the mutual diffusion of elements cannot be completely blocked in the long-term service process of the coating.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a composite coating for protecting Cr-containing stainless steel in molten fluoride salt, which adopts pulse composite electroplating to prepare a Ni (NiO) transition layer, then pulse electroplating the Ni coating, and finally growing Cr on the surface of a matrix alloy in situ through proper high-temperature vacuum treatment2O3Diffusion barrier to obtain continuous compact Cr with good combination with the matrix2O3the/Ni composite coating.
The invention solves the technical problems by the following technical scheme:
the invention relates to a preparation method of a composite coating for protecting Cr-containing stainless steel in molten fluoride salt, which comprises the following steps:
1) pretreatment of a base material: selecting stainless steel as a cathode substrate, a nickel sheet as an anode substrate, wherein the size of the nickel sheet is equivalent to that of the stainless steel cathode substrate, and pretreating the cathode substrate and the anode substrate, wherein the pretreatment refers to polishing, chamfering, oil removal, water washing, activation and water washing treatment again on the surface of the substrate;
2) preparing a Ni (NiO) transition layer by nano composite electroplating: placing the pretreated cathode and anode base materials in a nano composite electroplating bath, and carrying out nano composite pulse electroplating on a Ni (NiO) transition layer in a stirring process, wherein each 1L of the needed electroplating solution contains the following components: 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 20-100 g of nickel oxide powder and the balance of deionized water; the pulse plating conditions were: the average current density is 6-8A/dm2The pH value of the plating solution is 3.5, the temperature during electroplating is 50-55 ℃, the frequency is 100-500 Hz, the total duty ratio is 70-80%, and the electroplating time is 300 s;
3) electroplating outer nickel: stirring and nickel plating the base material treated by the nano composite electroplated Ni (NiO) transition layer in a bright nickel plating bath, wherein each 1L of the required plating solution contains the following components: 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 1g of saccharin sodium and the balance of deionized water; electroplating conditions are as follows: the average current density is 3.5A/dm2The pH value of the plating solution is 4.5, the temperature during electroplating is 45 ℃, the frequency is 50Hz, the total duty ratio is 40 percent, wherein the forward duty ratio is 36 percent, and the electroplating time is 300 s;
4) and (3) heat treatment: placing the base material subjected to the nickel treatment on the outer electroplating layer into a container protected by inert gas for heat treatment at 850-900 ℃ for 8 hours to enable Cr in the base material to react with NiO in the transition layer, and growing Cr on the surface in situ2O3Diffusion barrier, namely Cr for protecting Cr-containing stainless steel in molten fluoride salt2O3the/Ni composite coating.
In the step 1), 316L stainless steel is selected as the stainless steel, and the stainless steel is cut into sheets with the thickness of 15 multiplied by 10 multiplied by 2 mm.
In the step 1), the oil removal in the pretreatment is to put the substrate into an acetone solution and perform ultrasonic cleaning in an ultrasonic cleaner for 3-5 minutes, wherein the temperature of the ultrasonic cleaning is room temperature.
In the step 1), the activating solution adopted in the activating treatment in the pretreatment is prepared by mixing hydrochloric acid, sulfuric acid and deionized water according to the mass ratio of 2:4:2, the activating temperature is room temperature, the activating time is 15 seconds, the activated substrate is washed by the deionized water again, and then the substrate is quickly placed in an electroplating bath.
In the step 1), the grinding and chamfering in the pretreatment are respectively performed by 150-mesh and 600-mesh sandpaper.
In the step 2), the particle size of the nickel oxide powder adopted in the nano composite electroplating is 50 nm.
In the step 2), the inert gas adopted in the heat treatment process is high-purity argon, and the container is a quartz tube.
In the step 2), the stirring mode adopted in the nano composite electroplating is a magnetic stirring mode, and the rotating speed is 550 rpm.
In the step 2), the electroplating solution is prepared and then subjected to ultrasonic dispersion for 24 hours to obtain a nano powder electroplating solution with uniform dispersion.
The method of the invention has the following beneficial effects:
1) NiO nano-particles are adopted in the composite electroplating solution, and the nano-particles are added into the electroplating solution to be co-deposited with metal, so that a Ni (NiO) composite coating is obtained. Because of the higher controllability of the pulse plating on the plating layer, a fine crystal structure is formed, the porosity of the plating layer is reduced, and the surface of the plating layer is smooth and compact; and the plating time is greatly reduced while the required plating thickness is achieved.
2) When the bright nickel plating process is adopted, the method has the advantages of fewer additive types, reduced manual operation intensity, short electroplating time, improved production efficiency, reduced environmental pollution to a certain extent and green production.
3) The reverse pulse composite electroplating technology adopted by the invention has the advantages of high deposition efficiency, uniform and compact deposited layer, low internal stress, capability of being prepared at low temperature and normal pressure and simple and convenient operation. When the nano composite coating is plated, the microstructure, phase composition, thickness and the like of the coating and the nickel layer can be accurately controlled by adjusting pulse deposition parameters. When nickel plating is carried out, higher current density can be adopted, plating efficiency is improved, and a plating layer with better performance is obtained.
4) The high current density of the pulse composite electroplating adopted by the invention accelerates the deposition speed, and simultaneously, because the duty ratio exists, namely a certain on-off time, sufficient particles are provided for the cathode, the nickel deposition speed on the cathode is equivalent to the deposition speed of nano particles, and the Ni-NiO composite coating with uniformity, compactness and fine particles can be obtained.
5) The Ni (NiO) pulse composite coating prepared by the invention can react with the base material in situ through the subsequent heat treatment process, so that Cr grows in situ between the base material and the Ni coating2O3The composite coating prepared by the method has good bonding force with a substrate.
Drawings
FIG. 1 is a scanning electron micrograph of the surface of a composite coating according to example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of the surface of the composite coating of example 2 of the present invention.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings.
The invention relates to a preparation method of a composite coating for protecting Cr-containing stainless steel in molten fluoride salt, which comprises the following specific process flows of:
1) pretreatment of a base material: stainless steel is selected as a cathode substrate, a nickel sheet is selected as an anode substrate, the size of the nickel sheet is equivalent to that of the stainless steel cathode substrate, and the cathode substrate and the anode substrate are pretreated, wherein the pretreatment refers to the treatment of polishing, chamfering, oil removal, water washing, activation and water washing again on the surface of the substrate.
The stainless steel is 316L stainless steel and is cut into 15X 10X 2mm sheets.
The base material is polished and chamfered by 150-mesh sand paper and 600-mesh sand paper to obtain a continuous and flat base material surface, so that the binding force between the base material and the coating can be improved during subsequent electroplating.
The activating solution adopted in the activating treatment in the pretreatment is prepared by mixing hydrochloric acid, sulfuric acid and deionized water according to the mass ratio of 2:4:2, the activating temperature is room temperature, the activating time is 15 seconds, the activated substrate is washed by the deionized water again, and then the substrate is quickly placed into an electroplating bath.
And the oil removal in the pretreatment is to put the substrate into an acetone solution and perform ultrasonic cleaning in an ultrasonic cleaner for 3-5 minutes at room temperature.
2) Nanocomposite plating of ni (nio) transition layer: the cathode material and the anode material are fixed in an electroplating bath which is placed in parallel with a moderate distance, the electroplating bath can be replaced by a 200ml beaker, then the nano composite pulse electroplating is carried out in the stirring process, and each 1L of the needed electroplating solution contains the following components: 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 20-100 g of nickel oxide powder and the balance of deionized water; the pulse plating conditions were: the average current density is 6-8A/dm2The pH value of the plating solution is 3.5, the temperature during electroplating is 50-55 ℃, the frequency is 100-500 Hz, the total duty ratio is 70-80%, and the electroplating time is 300 s.
The particle size of the nickel oxide powder adopted in the nano composite electroplating is 50nm, and the nano powder can greatly improve the performance of a composite coating due to the unique physical and chemical properties of the nano powder.
The stirring mode adopted in the nano composite electroplating is a magnetic stirring mode, the rotating speed is 550rpm, the uniform dispersion of nano particles in the plating solution during electroplating is ensured, and the uniform deposition of the nano particles in the plating layer is also ensured.
The prepared electroplating solution needs to be subjected to ultrasonic dispersion for 24 hours to obtain a nano powder electroplating solution with uniform dispersion.
3) Electroplating outer nickel: stirring and nickel plating the base material treated by the nano composite electroplated Ni (NiO) transition layer in a bright nickel plating bath, wherein each 1L of the required plating solution contains the following components: 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 1g of saccharin sodium and the balance of deionized water; electroplating conditions are as follows: the average current density is 3.5A/dm2The pH value of the plating solution is 4.5, the temperature during electroplating is 45 ℃, the frequency is 50Hz, the total duty ratio is 40 percent, wherein the forward duty ratio is 36 percent, and the electroplating time is 300 s;
and (3) washing the coating by using deionized water after the electroplating is finished, and drying by using an electric hair drier after the washing (blowing by using cold air to avoid water stains on the surface of the coating) so as to obtain a clean coating surface.
4) And (3) heat treatment: sealing and placing the substrate subjected to the nickel treatment on the outer layer of the electroplating layer in a container protected by inert gas, then placing the substrate in a muffle furnace for heat treatment, or placing the substrate in a vacuum tube furnace, then introducing inert gas for heat treatment, wherein the temperature of the heat treatment is 850-900 ℃, and the time is 8 hours, so that Cr grows on the surface of the substrate2O3And (4) diffusion barrier, namely obtaining the composite coating for protecting the Cr-containing stainless steel in the molten fluoride salt.
The inert gas adopted in the heat treatment process is high-purity argon, and the container is a quartz tube.
The preparation of a continuous and compact diffusion barrier with good bonding performance with a matrix alloy and a corrosion-resistant Ni layer on the surface of stainless steel is the key point for preparing a melting-resistant fluoride coating, and the chemical bonding between an oxide coating and a matrix can obviously improve the adhesion between the oxide and the matrix. The invention adopts pulse composite plating to prepare a Ni-NiO transition layer, then pulse plating a Ni coating, and growing Cr on the surface of the matrix alloy in situ by proper high-temperature vacuum treatment2O3Diffusion barrier to obtain continuous compact Cr with good combination with the matrix2O3the/Ni composite coating.
The following are examples of the present invention:
example 1
Taking stainless steel (the components are shown in table one) containing 16 wt.% of Cr as a cathode substrate, cutting the stainless steel cathode substrate into 15 x 10 x 2mm slices, taking a nickel sheet as an anode substrate, wherein the size of the nickel sheet is equivalent to that of the stainless steel cathode substrate, pretreating the cathode substrate and the anode substrate, namely polishing and chamfering, ultrasonically removing oil by using acetone, washing by using deionized water, acidifying, and finally washing. Then the nickel oxide powder is put into a well-dispersed plating solution containing NiO nano particles (50nm), wherein each 1L of the plating solution contains 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 20g of nickel oxide powder and the balance of deionized water for electroplating. The power supply being adjustable double pulsesThe power supply adopts a pulse frequency of 100Hz and an average current density of 6A/dm2The temperature of the plating solution is 50 ℃, the total duty ratio is 70%, the stirring speed in the electroplating process is 550rpm, the pH value of the plating solution is 3.5, and the electroplating time is 300 s. Putting a sample with a nano composite coating with the thickness of 1 micron to be electroplated into Ni electroplating solution to carry out outer layer Ni electroplating, wherein each 1L of the plating solution contains the following components: 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 1g of saccharin sodium and the balance of deionized water. The power supply is an adjustable double-pulse power supply, and the average current density adopted is 3.5A/dm2The pH value of the plating solution is 4.5, the temperature during electroplating is 45 ℃, the frequency is 50Hz, the total duty ratio is 40 percent, wherein the forward duty ratio is 36 percent, and the electroplating time is 300 s. Washing the electroplated sample, drying, sealing the sample in a quartz tube filled with high-purity argon, putting the quartz tube into a muffle furnace, and performing heat treatment at 900 ℃ for 8 hours to obtain the Cr-containing sample2O3A diffusion barrier and an oxide composite coating of the corrosion resistant Ni layer. The cross-sectional morphology of the resulting oxide diffusion barrier is shown in fig. 1. The inner and outer interfaces of the heat treated corrosion resistant layer disappear and a continuous oxide with an average thickness of about 1 micron is generated at the inner and outer interfaces. The sample was scanned by using an energy spectrum, and the main components of the obtained oxide composite coating are shown in table two (marked part in fig. 1). The results of the elemental line scan and elemental distribution analysis are combined to obtain an oxide diffusion barrier consisting mainly of Cr-rich oxides.
Watch 1
Watch two
Example 2
Using stainless steel (composition shown in table one) containing Cr in an amount of about 16 wt.% as a cathode substrate, the stainless steel cathode substrate was cut into 15X 10X 2mm thin pieces, and nickel pieces were used as an anode substrateThe size of the nickel sheet is equal to that of the stainless steel cathode substrate, and the cathode substrate and the anode substrate are pretreated, namely, after polishing and chamfering, acetone ultrasonic degreasing is carried out, deionized water is washed and then acidified, and finally washing is carried out. Then the nickel oxide powder is put into a well-dispersed plating solution containing NiO nano particles (50nm), wherein each 1L of the plating solution contains 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 100g of nickel oxide powder and the balance of deionized water for electroplating. The power supply is an adjustable double-pulse power supply, the adopted pulse frequency is 500Hz, and the average current density is 8A/dm2The temperature of the plating solution is 55 ℃, the total duty ratio is 80%, the stirring speed in the electroplating process is 550rpm, the pH of the plating solution is 3.5, and the electroplating time is 300 s. Putting a sample with a 2-micron-thick nano composite coating in a Ni plating solution for plating outer Ni, wherein each 1L of the plating solution contains the following components: 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 1g of saccharin sodium and the balance of deionized water. The power supply is an adjustable double-pulse power supply, and the average current density adopted is 3.5A/dm2The pH value of the plating solution is 4.5, the temperature during electroplating is 45 ℃, the frequency is 50Hz, the total duty ratio is 40 percent, wherein the forward duty ratio is 36 percent, and the electroplating time is 300 s. Washing the electroplated sample, drying, placing the sample in a vacuum tube furnace, introducing inert gas, and performing heat treatment at 850 deg.C for 8 hr to obtain the final product containing Cr2O3A diffusion barrier and an oxide composite coating of the corrosion resistant Ni layer. The cross-sectional morphology of the resulting oxide diffusion barrier is shown in fig. 2. The inner and outer interfaces of the heat treated corrosion resistant layer disappear and a continuous oxide with an average thickness of about 1 micron is generated at the inner and outer interfaces. The sample was scanned by using an energy spectrum, and the main components of the obtained oxide composite coating are shown in table three (marked part in fig. 2). The results of the elemental surface scan and elemental distribution analysis are combined to obtain an oxide diffusion barrier consisting mainly of Cr-rich oxides.
Watch III
Claims (9)
1. A preparation method of a composite coating for protecting stainless steel containing Cr in molten fluoride salt is characterized by comprising the following steps:
1) pretreatment of a base material: selecting stainless steel as a cathode substrate, a nickel sheet as an anode substrate, wherein the size of the nickel sheet is equivalent to that of the stainless steel cathode substrate, and pretreating the surfaces of the cathode substrate and the anode substrate, wherein the pretreatment refers to polishing, chamfering, oil removal, washing, activation and washing treatment again of the surfaces of the cathode substrate and the anode substrate;
2) nano composite electroplating of a Ni-NiO transition layer: placing the pretreated cathode and anode base materials in a nano composite electroplating bath, and carrying out nano composite pulse electroplating while stirring to prepare a Ni-NiO transition layer, wherein each 1L of the needed electroplating solution contains the following components: 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 20-100 g of nickel oxide powder and the balance of deionized water; the pulse plating conditions were: the average current density is 6-8A/dm2The pH value of the plating solution is 3.5, the temperature during electroplating is 50-55 ℃, the frequency is 100-500 Hz, the total duty ratio is 70-80%, and the electroplating time is 300 s;
3) electroplating outer nickel: stirring and nickel plating the base material treated by the nano composite electroplated Ni-NiO transition layer in a bright nickel plating bath, wherein each 1L of the required plating solution contains the following components: 250g of hydrated nickel sulfate, 40g of hydrated nickel chloride, 40g of boric acid, 0.3g of sodium dodecyl sulfate, 1g of saccharin sodium and the balance of deionized water; electroplating conditions are as follows: the average current density is 3.5A/dm2The pH value of the plating solution is 4.5, the temperature during electroplating is 45 ℃, the frequency is 50Hz, the total duty ratio is 40 percent, wherein the forward duty ratio is 36 percent, and the electroplating time is 300 s;
4) and (3) heat treatment: placing the base material subjected to the nickel treatment on the outer electroplating layer into a container filled with inert gas for heat treatment at 850-900 ℃ for 8 hours to enable Cr in the base material to react with NiO in the transition layer, and growing Cr on the surface in situ2O3Diffusion barrier, namely Cr for protecting Cr-containing stainless steel in molten fluoride salt2O3the/Ni composite coating.
2. The method for preparing a composite coating for protecting a stainless steel containing Cr in molten fluoride salt according to claim 1, wherein the stainless steel is 316L stainless steel and cut into 15 x 10 x 2mm thin pieces in step 1).
3. The method for preparing the composite coating for protecting the stainless steel containing Cr in the molten fluoride salt according to the claim 1, wherein in the step 1), the degreasing in the pretreatment is to put the substrate into an acetone solution and perform ultrasonic treatment in an ultrasonic cleaner for 3-5 minutes, and the temperature of the ultrasonic cleaning is room temperature.
4. The method for preparing the composite coating for protecting the stainless steel containing Cr in the molten fluoride salt according to claim 1, wherein in the step 1), the activating solution adopted in the activating treatment in the pretreatment is prepared by mixing hydrochloric acid, sulfuric acid and deionized water according to a mass ratio of 2:4:2, the activating temperature is room temperature, and the activating time is 15 seconds.
5. The method for preparing a composite coating for protecting stainless steel containing Cr in molten fluoride salt according to claim 1, wherein the polishing and chamfering in the pretreatment of step 1) are performed with 150-mesh and 600-mesh sandpaper, respectively.
6. The method for preparing a composite coating for protecting stainless steel containing Cr in molten fluoride according to claim 1, wherein the particle size of the nickel oxide powder used in the nano-composite plating in step 2) is 50 nm.
7. The method for preparing a composite coating for protecting stainless steel containing Cr in molten fluoride salt according to claim 1, wherein the inert gas used in the heat treatment process in step 4) is high-purity argon, and the container is a quartz tube.
8. The method for preparing the composite coating for protecting the stainless steel containing Cr in the molten fluoride salt according to claim 1, wherein in the step 2), the stirring mode adopted in the nano composite electroplating is a magnetic stirring mode, and the rotating speed is 550 rpm.
9. The method for preparing the composite coating for protecting the stainless steel containing Cr in the molten fluoride salt according to claim 1, wherein in the step 2), the electroplating solution is prepared and then ultrasonically dispersed for 24 hours to obtain the nano-powder electroplating solution with uniform dispersion.
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