CN114059116B - Method for preparing FeCoNiCuSn high-entropy alloy through electrodeposition - Google Patents
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
Abstract
The invention discloses a method for preparing FeCoNiCuSn high-entropy alloy by electrodeposition, which belongs to the technical field of electroplating, and comprises the steps of firstly stirring choline chloride, levulinic acid and distilled water at constant temperature to obtain a transparent eutectic solvent, then adding ferrous chloride, cobalt chloride hexahydrate, nickel chloride hexahydrate, copper chloride dihydrate and stannous chloride dihydrate into the eutectic solvent, and then stirring at constant temperature to obtain electroplating solution; graphite is used as an anode, brass sheets and the like are used as cathodes, and the anodes are immersed into electroplating liquid for constant current electroplating.
Description
Technical Field
The invention belongs to the technical field of electroplating, and particularly relates to a method for preparing FeCoNiCuSn high-entropy alloy by electrodeposition.
Background
High entropy alloys are simple solid solutions composed of five or more elements. It was initially found that alloys consisting of more principal elements exhibit a complex microstructure and an undesirable brittle behaviour. However, yeh suggested in 1995 that an alloy system containing five or more metal elements actually had a high mixing entropy, facilitating the formation of a multi-element solid solution phase. In addition to the high entropy effect, the formation of the solid solution phase is also due to the large lattice distortion and slow diffusion of such multi-element mixtures. High entropy alloys exhibit different microstructures and properties depending on their composition or processing technique. The high-entropy alloy coating has excellent properties such as high strength, high hardness, high temperature resistance, wear resistance and corrosion resistance, and is expected to be applied to cutters, dies, aviation military industry and the like. The deposition potential of a metal differs depending on its compositional nature and the state difference in the electrolyte. The high-entropy alloy contains five or more alloy systems, and the deposition potentials of the high-entropy alloy are different, so that codeposition is difficult to realize in common electroplating solution. Soare V et Al prepared Al-Cr-Fe-Mn-Ni and Al-Cr-Cu-Fe-Mn-Ni high entropy alloy coatings by potentiostatic electrodeposition in N, N-dimethylformamide-acetonitrile organic system [ Soare V, burda M, constantin I, et Al, electrochemical deposition and micro structural characterization of Al-Cr-Fe-Mn-Ni and Al-Cr-Cu-Fe-Mn-Ni high entropy alloy coatings [ J ]. Applied Surface Science,2015,358 (15): 533-539 ]. However, acetonitrile belongs to a neutral toxic organic solvent, and causes certain pollution to the environment. The toxicity of the aqueous solution system is low, but the FeCoNiCuSn high-entropy alloy has good corrosion resistance and is difficult to codeposit in the aqueous solution system.
Through retrieval, the preparation method is disclosed as a FeCoNiCuMo high-entropy alloy film with the patent publication number of CN108728876A and the publication date of 2018, 11 and 2, and takes deionized water as a solvent to prepare an electroplating solution, and the FeCoNiCuMo high-entropy alloy film is prepared by an electrochemical deposition method; the method comprises the following steps: s1, taking three parts of deionized water, and dissolving triethanolamine, ammonium molybdate tetrahydrate and copper salt in the first part of deionized water to obtain a solution A; s2, dissolving glycine, ethylene glycol, an antioxidant and additional salt in a second part of deionized water to obtain a solution B; s3, dissolving trisodium citrate, ferrous salt, cobalt salt and nickel salt in third deionized water to obtain a solution C; s4, uniformly mixing the solution A, the solution B and the solution C, aging, adjusting the pH value of the solution to 7-8, heating to 30 ℃, introducing nitrogen to remove oxygen, and obtaining electroplating solution; and S5, electroplating by taking the graphite plate as an anode and taking the copper base as a cathode to obtain the FeCoNiCuMo high-entropy alloy film. The electroplating solution has the defects that various additives are required to be added to realize the codeposition of five alloy elements, and triethanolamine has certain toxicity and does not meet the requirement of green production.
The invention discloses a high-entropy alloy porous electrode and a preparation method thereof, wherein the patent publication number is CN112609213A, the publication date is 2021, 4 and 6, and the preparation method of the high-entropy alloy porous electrode comprises the following steps: step S10: preparing a mixed solution containing a plurality of metal ions and hydrogen ions; step S30: and taking the mixed solution obtained in the step S10 as an electrolyte, taking a conductive substrate as a cathode, and carrying out electrodeposition under a negative potential, wherein the negative potential is lower than the reduction potential of the hydrogen ions, and when the multiple metal ions are reduced and deposited on the conductive substrate, the hydrogen ions are synchronously reduced on the surface of the conductive substrate to form hydrogen bubbles so as to obtain the high-entropy alloy electrode with a porous structure. The disadvantages are that concentrated hydrochloric acid, concentrated sulfuric acid, concentrated nitric acid and the like are added into the electroplating solution, and the electroplating solution is difficult to treat.
Disclosure of Invention
1. Solves the technical problem
In order to solve the problem that an additive added into a water-containing system of the high-entropy alloy in the prior art has toxicity and causes environmental pollution, the invention aims to provide a method for preparing FeCoNiCuSn high-entropy alloy by electrodeposition, the electrodeposition process can realize codeposition of FeCoNiCuSn, and is safe, nontoxic, environment-friendly and economical.
2. Technical scheme
In order to achieve the technical purpose, the invention is realized by the following technical scheme:
the invention provides a method for preparing FeCoNiCuSn high-entropy alloy by electrodeposition, which specifically comprises the following steps:
(1) Preparing an electroplating solution: firstly, preparing a eutectic solvent according to a molar ratio, then stirring at a constant temperature until the eutectic solvent is transparent, then respectively weighing a soluble iron source, a soluble cobalt source, a soluble nickel source, a soluble copper source and a soluble tin source according to the molar ratio, adding the soluble iron source, the soluble cobalt source, the soluble nickel source, the soluble copper source and the soluble tin source into the eutectic solvent, stirring at the constant temperature to obtain the eutectic solvent, and taking the eutectic solvent as an electroplating solution;
(2) Electroplating: immersing graphite serving as an anode and a brass sheet serving as a cathode into the electroplating solution obtained in the step (1) for constant-current electroplating;
(3) Cleaning and drying: and after the electroplating is finished, taking out the brass sheet, cleaning and drying.
Further, the eutectic solvent is a mixed solvent of choline chloride, levulinic acid and pure water, and the molar ratio of the choline chloride to the levulinic acid to the pure water is 1:2: (2-4).
Further, the temperature of the constant-temperature stirring is 60-80 ℃ to achieve dissolution and uniform mixing of the eutectic solvent and the metal salt.
Furthermore, the molar ratio of the iron source, the cobalt source, the nickel source, the copper source and the tin source to the choline chloride is 0.025:0.025:0.025:0.025:0.005:1.
Furthermore, the soluble iron source is preferably ferrous chloride, and can also be ferrous sulfate or ferrous nitrate, and the soluble iron source can be dissolved in the eutectic solvent and provides an iron source; the soluble cobalt source is preferably cobalt chloride hexahydrate, and can also be cobalt sulfate or cobalt nitrate, and the soluble cobalt source can be dissolved in a eutectic solvent and can provide a cobalt source; the soluble nickel source is preferably nickel chloride hexahydrate, can also be nickel sulfate or nickel nitrate, can be dissolved in the eutectic solvent and provides the nickel source; the soluble copper source is preferably copper chloride dihydrate, can also be copper sulfate or copper nitrate, can be dissolved in a eutectic solvent and can provide a copper source; the soluble tin source is preferably stannous chloride dihydrate, and can also be tin sulfate or tin nitrate, and the soluble tin source can be dissolved in the eutectic solvent and provide a tin source.
Further, the direct distance between the cathode and the anode is 1-2cm; the electroplating temperature is 50-70 ℃, and the electroplating time is 1-10h.
Further, the electroplating power supply in the step (2) is a direct current power supply, and the current density is 3-10mA/cm 2 。
Furthermore, the electroplating power supply in the step (2) is a pulse power supply, the duty ratio is 1 (3-4), the current frequency is 100-1000Hz, and the current density is 3-10mA/cm 2 。
The main difficulty of preparing the high-entropy alloy film by adopting an electrochemical deposition method is to find a proper complexing agent, so that various ions are simultaneously dissolved in a solution, and then metal ions are subjected to electron emission in a cathode discharge mode to be deposited into the film. In addition, as the high-entropy alloy FeCoNiCuSn contains five different elements,the difference of reduction potentials of different metal atoms is large, how to realize the Co-deposition of Fe, co, ni, cu and Sn is also the difficulty of preparing a uniform high-entropy alloy film by using an electrochemical deposition technology. The electroplating solution for preparing the high-entropy alloy by the electrodeposition method is divided into an aqueous solution system and a non-aqueous solution system, but the electrochemical window of water in the aqueous solution system is small, part of metal has negative potential in the aqueous solution and is difficult to reduce, and in addition, hydrogen evolution reaction and hydroxide generation exist on a cathode. The non-aqueous solution system has a wide electrochemical window, but the solution has poor conductivity, the dissolving capacity for metal salts is not ideal, the solution also has certain toxicity, and in addition, the coordination capacity of common non-aqueous systems (such as a dimethylformamide-DMF system, a dimethyl sulfoxide-DMSO system and an ethylene diamine tetraacetic acid-EDTA system) for metal ions is too strong, so that the migration of ions between electrodes is not facilitated. Therefore, the invention takes the mixed solvent of choline chloride, levulinic acid and pure water as the eutectic solvent to dissolve soluble iron source, soluble cobalt source, soluble nickel source, soluble copper source and soluble tin source to prepare the electroplating solution, and the single Fe 2+ (Standard deposition potential: -0.447V), co 2+ (standard deposition potential: -0.28V), ni 2+ (Standard deposition potential: -0.257V), cu 2 + (Standard deposition potential: 0.3419V) and Sn 2+ (Standard deposition potential: -0.138V) the standard potential difference is large, codeposition cannot be realized, and after the eutectic solvent is added, fe in the solution 3+ 、Co 2+ 、Ni 2+ 、Cu 2+ And Sn 2+ With choline chloride, levulinic acid to form [ NiCl 3 ] - 、[CuCl 4 ] - 、[SnCl 3 ] - The isocoordination structure can realize the adjustment of the deposition potential. The eutectic solvent adopted by the invention has a higher electrochemical window, and the induced codeposition of the five elements can be realized without additional additives. Furthermore, in the prior art (Xc A, lx A, ys B, et al, electrochemical scanner and electrochemical position of cobalt from chlorine-urea future electrolytic solution [ J]Electrochimica Acta,2019,295)In order to realize the coprecipitation of five metals, the system is more complex, and the difference of the deposition potential is larger, so that the preparation of the electrolyte is more difficult.
3. Advantageous effects
Compared with the prior art, the invention has the following technical effects:
(1) The electroplating liquid is prepared by adding metal salt into a eutectic solvent consisting of choline chloride-levulinic acid-pure water, and Fe 3+ 、Co 2+ 、Ni 2+ 、Cu 2+ And Sn 2+ With choline chloride, levulinic acid to form [ NiCl 3 ] - 、[CuCl 4 ] - 、[SnCl 3 ] - The equal coordination structure is adopted to adjust the deposition potential, so that the codeposition of FeCoNiCuSn is realized, and the prepared FeCoNiCuSn meets the ideal high-entropy alloy equal atomic ratio requirement;
(2) The invention is realized by introducing Sn 2+ Potential gradient is formed between the Cu and other more negative metal potentials, the potential difference is reduced, and the co-deposition of five-element FeCoNiCuSn is realized;
(3) Compared with the system in the prior art, the system of the invention does not need to add extra additives, and the codeposition of the multi-component alloy can be obtained by directly electroplating metal anions formed by metal ions and the eutectic solvent, and the process is safe, nontoxic, environment-friendly and economical.
Drawings
FIG. 1 is an SEM image of a FeCoNiCuSn plating layer obtained in example 1 of the present invention;
FIG. 2 is an EDS spectrum of an electroplated FeCoNiCuSn layer obtained in example 1 of the present invention, in which the ordinate represents the number d in cps, and the abscissa represents the energy in keV;
FIG. 3 is an XRD pattern of an electroplated FeCoNiCuSn layer obtained in example 1 of the present invention, wherein the ordinate is intensity and the abscissa is a double angle;
FIG. 4 is a polarization curve of a plating layer FeCoNiCuSn obtained in example 1 of the present invention;
FIG. 5 is an EDS spectrum of the electroplated FeCoNiCuSn obtained in example 2 of the present invention;
FIG. 6 is an EDS spectrum of the plated CuNi film obtained in comparative example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples.
Wherein, table 1 is the experimental parameters of each embodiment of the present invention; table 2 shows the atomic percentages of the elements of the products produced by the examples of the present invention.
Example 1
Respectively weighing 0.2mol of choline chloride, 0.4mol of levulinic acid and 0.4mol of distilled water, placing the materials into a beaker, sealing the beaker by using a preservative film, stirring the materials at a constant temperature of 70 ℃ to obtain a transparent eutectic solvent, then respectively adding 0.05mol of ferrous chloride, 0.05mol of cobalt chloride hexahydrate, 0.05mol of nickel chloride hexahydrate, 0.05mol of copper chloride dihydrate and 0.01mol of stannous chloride dihydrate, and stirring the materials at a constant temperature of 70 ℃ to obtain the electroplating solution.
Immersing graphite plate as anode and brass sheet as cathode in electroplating solution heated to 70 deg.C in water bath for 1 hr constant current electroplating, wherein the power supply is selected from DC power supply, the direct distance between cathode and anode is 1cm, and the current density is 10mA/cm 2 。
And after the electroplating is finished, taking out the brass sheet, washing the brass sheet for 2 times by using water, and finally drying the brass sheet by using hot air.
The morphology and the structure of the prepared electroplated layer are characterized, as shown in figures 1-3, SEM image results show that the prepared electroplated layer has uniform particle size and 1-2 mu m size, the electroplated layer simultaneously contains five elements of Fe, co, ni, cu and Sn measured in an EDS energy spectrogram, and characteristic diffraction peaks in an XRD image correspond to face-centered cubic crystals, which indicates that the FeCoNiCuSn electroplated layer is prepared, is a single solid solution and accords with the characteristics of high-entropy alloy. As shown in FIG. 4, the results of the polarization curves show that the corrosion potential of the electroplated layer is-0.263V and the self-corrosion current is 1.493X 10 -5 And A, the electroplated layer has better corrosion resistance.
Example 2
Respectively weighing 0.2mol of choline chloride, 0.4mol of levulinic acid and 0.6mol of distilled water, placing the choline chloride, the levulinic acid and the distilled water in a beaker, sealing the beaker by using a preservative film, stirring the mixture at a constant temperature of 60 ℃ to obtain a transparent eutectic solvent, then respectively adding 0.05mol of ferrous chloride, 0.05mol of cobalt chloride hexahydrate, 0.05mol of nickel chloride hexahydrate, 0.05mol of copper chloride dihydrate and 0.01mol of stannous chloride dihydrate, and stirring the mixture at a constant temperature of 60 ℃ to obtain the electroplating solution.
The graphite plate is used as an anode, the brass sheet is used as a cathode, the graphite plate is immersed into electroplating solution heated to 50 ℃ in water bath for 1-hour constant current electroplating, the power supply is selected as a pulse power supply, wherein the direct distance between the cathode and the anode is 1.5cm, the duty ratio is 1 & lt 3 & gt, the current frequency is 100Hz, and the current density is 10mA/cm 2 。
And after the electroplating is finished, taking out the brass sheet, washing the brass sheet for 2 times by using water, and finally drying the brass sheet by using hot air.
As shown in FIG. 5, the obtained plating film contained five elements of Fe, co, ni, cu and Sn in combination.
Example 3
2mol of choline chloride, 4mol of levulinic acid and 4mol of distilled water are respectively weighed and placed in a beaker, the beaker is sealed by a preservative film, then the temperature is kept constant at 70 ℃, a transparent eutectic solvent is obtained by stirring, then 0.5mol of ferrous chloride, 0.5mol of cobalt chloride hexahydrate, 0.5mol of nickel chloride hexahydrate, 0.5mol of copper chloride dihydrate and 0.1mol of stannous chloride dihydrate are respectively added, and the electroplating solution is obtained by stirring at the constant temperature of 70 ℃.
Immersing graphite plate as anode and brass sheet as cathode in electroplating solution heated to 60 deg.C in water bath for 10 hr constant current electroplating, wherein the direct distance between cathode and anode is 1cm, and the current density is 5mA/cm 2 。
And after the electroplating is finished, taking out the brass sheet, washing the brass sheet for 2 times by using water, and finally drying the brass sheet by using hot air.
Example 4
Respectively weighing 0.2mol of choline chloride, 0.4mol of levulinic acid and 0.6mol of distilled water, placing the materials into a beaker, sealing the beaker by using a preservative film, stirring the materials at a constant temperature of 80 ℃ to obtain a transparent eutectic solvent, then respectively adding 0.05mol of ferrous chloride, 0.05mol of cobalt chloride hexahydrate, 0.05mol of nickel chloride hexahydrate, 0.05mol of copper chloride dihydrate and 0.01mol of stannous chloride dihydrate, and stirring the materials at a constant temperature of 80 ℃ to obtain the electroplating solution.
The graphite plate is used as an anode, the brass sheet is used as a cathode,immersing in electroplating solution heated to 70 deg.C in water bath for 10 hr for constant current electroplating, wherein the direct distance between cathode and anode is 2cm, and the current density is 3mA/cm 2 。
And after the electroplating is finished, taking out the brass sheet, washing the brass sheet for 2 times by using water, and finally drying the brass sheet by using hot air.
Comparative example 1
Respectively weighing 0.2mol of choline chloride, 0.4mol of levulinic acid and 0.6mol of distilled water, placing the choline chloride, the levulinic acid and the distilled water in a beaker, sealing the beaker by using a preservative film, stirring the mixture at a constant temperature of 80 ℃ to obtain a transparent eutectic solvent, then respectively adding 0.05mol of ferrous chloride, 0.05mol of cobalt chloride hexahydrate, 0.05mol of nickel chloride hexahydrate and 0.05mol of copper chloride dihydrate, and stirring the mixture at a constant temperature of 80 ℃ to obtain the electroplating solution.
Immersing graphite plate as anode and brass sheet as cathode in electroplating solution heated to 70 deg.C in water bath for 1 hr constant current electroplating, wherein the direct distance between cathode and anode is 1cm, and the current density is 10mA/cm 2 。
And after the electroplating is finished, taking out the brass sheet, washing the brass sheet for 2 times by using water, and finally drying the brass sheet by using hot air.
The choline chloride-levulinic acid-pure water selected by the invention belongs to eutectic solvents, and the electrochemical window of the solvents is 2.4V, which is higher than 1.2V of aqueous solution, so that more metals can be deposited. However, it was found by experiment that the co-deposition of metals in the eutectic solvent can be achieved without random combination of metals, as shown in comparative example 1, which has the same process parameters as example 1 except that no tin salt is added, and when trying to deposit FeCoNiCu, the inventors found that co-deposition of two elements, i.e., ni and Cu, can be achieved, and that no conceivable alloy system can be obtained, the atomic contents of the elements are shown in fig. 6, and the surface of the coating has coarse particles and large size difference. The reason is that the potential of Cu is positive, while the potential of other metals is negative, but Cu and Ni can form an infinitely miscible solid solution, so that a binary CuNi alloy is obtained by deposition. However, when a small amount of Sn is added, as in example 1, by introducing Sn 2+ (Standard deposition potential: -0.138V), which is between the potentials of Cu and other more negative metals, and which can form a potential gradientAnd reducing the potential difference, thereby obtaining the codeposition of the five-element high-entropy alloy FeCoNiCuSn.
TABLE 1 Experimental parameters for various embodiments of the invention
TABLE 2 atomic percent of elements of the product prepared by the examples of the invention
| Element content | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 |
| Fe | 19.11 | 20.02 | 15.06 | 10.17 | - |
| Co | 12.66 | 8.34 | 8.28 | 10.17 | - |
| Ni | 31.23 | 24.62 | 24.08 | 16.42 | 15.89 |
| Cu | 35.33 | 45.78 | 50.97 | 64.83 | 84.11 |
| Sn | 0.24 | 1.24 | 1.61 | 0.31 | - |
Comparing example 1 with example 2, it can be seen that co-deposition of five elements can be obtained by using both dc power supply and pulse power supply, but when deposition is performed by using pulse power supply, the Cu content is high because the pulse power supply is used in the electroplating process, when the current is conducted, the pulse (peak) current is several times or even tens of times of the common dc current, and the metal ions are reduced under extremely high overpotential due to the instantaneous high current density. Comparing example 1 with example 3, it can be seen that, at a lower current density, the corresponding deposition voltage is lower, the standard potential of Cu is the most positive, and deposition is preferred, and at this time, the atomic percentages of the elements are greatly different, which does not meet the ideal atomic ratio requirements of high-entropy alloys and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (7)
1. A method for preparing FeCoNiCuSn high-entropy alloy by electrodeposition is characterized by comprising the following steps:
(1) Preparing an electroplating solution: firstly, preparing a eutectic solvent according to a molar ratio, then stirring at a constant temperature until the eutectic solvent is transparent, then respectively weighing a soluble iron source, a soluble cobalt source, a soluble nickel source, a soluble copper source and a soluble tin source according to the molar ratio, adding the soluble iron source, the soluble cobalt source, the soluble nickel source, the soluble copper source and the soluble tin source into the eutectic solvent, stirring at the constant temperature to obtain the eutectic solvent, and taking the eutectic solvent as an electroplating solution, wherein the eutectic solvent is a mixed solvent of choline chloride, levulinic acid and water, and the molar ratio of the choline chloride to the levulinic acid to the water is 1:2: (2-4);
(2) Electroplating: immersing graphite serving as an anode and a brass sheet serving as a cathode into the electroplating solution obtained in the step (1) for constant-current electroplating;
(3) Cleaning and drying: and after the electroplating is finished, taking out the brass sheet, cleaning and drying.
2. The method for preparing FeCoNiCuSn high-entropy alloy through electrodeposition according to claim 1, wherein the molar ratio of the iron source to the cobalt source to the nickel source to the copper source to the tin source to the choline chloride is 0.025:0.025:0.025:0.025:0.005:1.
3. The method for preparing the FeCoNiCuSn high-entropy alloy in the electro-deposition mode according to claim 2, wherein the soluble iron source is ferrous chloride, ferrous nitrate or ferrous sulfate; the soluble cobalt source is cobalt chloride hexahydrate, cobalt nitrate or cobalt sulfate; the soluble nickel source is nickel chloride hexahydrate, nickel nitrate or nickel sulfate; the soluble copper source is copper chloride dihydrate, copper nitrate or copper sulfate; the soluble tin source is stannous chloride dihydrate, stannic nitrate or stannic sulfate.
4. A method for preparing FeCoNiCuSn high entropy alloy by electrodeposition as claimed in claim 3, wherein the temperature of constant temperature stirring in step (1) is 60-80 ℃.
5. The method for preparing the FeCoNiCuSn high-entropy alloy in the electro-deposition mode according to claim 4, wherein the direct distance between the cathode and the anode in the step (2) is 1-2cm; the electroplating temperature is 50-70 ℃, and the electroplating time is 1-10h.
6. The method for preparing FeCoNiCuSn high-entropy alloy through electrodeposition as claimed in claim 5, wherein the electroplating power supply in the step (2) is a direct current power supply, and the current density is 3-10mA/cm 2 。
7. The method for preparing FeCoNiCuSn high-entropy alloy through electrodeposition according to claim 5, wherein the electroplating power supply in the step (2) is a pulse power supply, the duty ratio is 1 (3-4), the current frequency is 100-1000Hz, and the current density is 3-10mA/cm 2 。
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