CN114250489B - Method for preparing copper-iron alloy based on electrodeposition method - Google Patents
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Abstract
The application discloses a method for preparing copper-iron alloy based on an electrodeposition method, which belongs to the field of electrochemical deposition alloy, and adopts a sulfate aqueous solution system as electrolyte, copper plating on a copper plate or a stainless steel plate is used as a negative electrode, an oxygen-evolving anode is used as a positive electrode, pulse power supply deposition is adopted, pulse voltage is applied, and the circulation speed, pH value, current density, pulse width, deposition temperature, deposition time and positive and negative electrode spacing of the electrolyte are controlled to obtain the copper-iron alloy. The copper-iron alloy prepared by the method has controllable components and thickness, excellent mechanical and corrosion properties, electromagnetic shielding property, compact microstructure, fine crystallization and excellent mechanical, electrical, magnetic and corrosion resistance properties, and can be widely applied to the industrial fields of electronics, medical treatment, electromechanics, communication and the like.
Description
Technical Field
The application belongs to the technical field of electrochemical deposition, and particularly relates to an electrodeposition preparation method of copper-iron alloy.
Background
The copper-iron alloy has high strength, high heat conductivity, high wear resistance, high bending strength and excellent magnetic and electromagnetic shielding performance when the iron content is more than 30 percent. Therefore, the alloy has very broad application prospect, for example, the copper-iron alloy plate and strip can be used for shielding cases, large-size OLED backboard, 5G mobile phone cooling plate, large-size LED display screen cooling plate, air conditioner condenser pipe, wireless charging circuit board and the like; the copper-iron alloy rods, bars, wires and other materials can be used for electromagnetic shielding wires, high-fidelity audio wires, woven electromagnetic shielding nets, mariculture net cages, radio frequency wires and the like; the copper-iron alloy powder can be used for brake pads, wave-absorbing shielding paint, 3D printing, medical antibacterial and other aspects; besides, the copper-iron alloy has wide application in the aspects of electric spark machining, electric soldering tips, motor rotors, injection molds, electrical contacts and the like. Therefore, development and design of a complete and feasible copper-iron alloy preparation process with reliable product performance are imperative.
Copper-iron alloy preparation process is numerous, and CuFe is successfully developed by adopting vacuum consumable technology for the first time in 2017 of Shanxi Rui New Material Co 50 The alloy is independently developed based on a vacuum induction smelting technology, and 8 preparation processes including a vacuum consumable arc smelting process, an upward continuous casting process, a non-vacuum semi-continuous casting process, a vacuum gas atomization powder process, a 3D printing process, a vacuum horizontal continuous casting process and a vacuum downward continuous casting process are included. Based on the above processes, different production processes are adopted for different product types (plates, belts, rods, wires, powder, etc.) to ensure high purity, high uniformity and high consistency of the products. However, copper has a large difference in properties from iron and low mutual solubility, and only about 4% of the iron can be dissolved into the copper matrix to form an alloy. Therefore, when the copper-iron alloy is produced by the preparation process, the problems of high impurity content, complex process, high cost, high alloy segregation degree and the like are unavoidable, and the overall performance of the alloy is seriously affected.
Compared with the traditional copper-iron alloy preparation process, the electrodeposition technology has the advantages of high cost efficiency, simple structure, less element waste, high production speed, easy deposition and the like, and is widely applied to the production of single-layer or alloy films no matter the surface size and the area size of the copper-iron alloy. The crystallization process of electrodeposition is quite different from that of the conventional melting technology, in which alloying is performed at a low temperature, whereas crystals are usually formed by crystallization at a high temperature, which will greatly reduce the influence of stress effects introduced at high temperatures. At present, very few researchers at home and abroad prepare copper-iron alloys with different components and morphologies by using direct current electrolysis or pulse electrolysis, and the influence of various parameters on the alloy performance and structure and the formation process of the alloy are explored by changing relevant parameters such as different component ratios, current density during electroplating, additive components and the like in electrolyte and analyzing the parameters such as XRD, muss Baol spectra and the like.
Disclosure of Invention
In order to solve the defects in the prior art, the application aims to provide a method for preparing copper-iron alloy by an electrodeposition method, which has the advantages of environment-friendly process, simple operation, low cost, controllable thickness and components of the produced alloy, excellent mechanical and corrosion properties and electromagnetic shielding performance; the prepared copper-iron alloy can be applied to the industrial fields of electronics, medical treatment, communication, electromechanics and the like.
The application is realized by the following technical scheme.
The application provides a method for preparing copper-iron alloy based on an electrodeposition method, which comprises the following steps:
the method comprises the steps of adopting a sulfate aqueous solution system as electrolyte, adopting electroplated copper on a copper plate or a stainless steel plate as a negative electrode, adopting an oxygen-evolving anode as a positive electrode, adopting pulse power supply deposition, applying pulse voltage, controlling the circulation speed and pH value of the electrolyte to be 2.5-4, and controlling the distance between the positive electrode and the negative electrode to be 1-4 cm, thus obtaining the copper-iron alloy.
In the scheme, the sulfate aqueous solution electrolyte comprises the following components in mass volume concentration g/L:
in the above scheme, the ferrous salt is Fe (NH) 4 ) 2 (SO 4 ) 2 ·6H 2 O、FeSO 4 ·7H 2 O or FeCl 2 。
In the above scheme, the sodium complexing agent is sodium gluconate or sodium citrate.
In the scheme, when the pulse power supply is adopted for deposition, the low potential range is-3 to-5V, and the high potential range is-3.5 to-5.5V.
In the scheme, when pulse voltage is applied, the corresponding cathode current density is 80-200 mA/cm 2 The pulse width ranges from 1ms to 100ms, the deposition temperature ranges from 45 ℃ to 50 ℃ and the deposition time ranges from 15 to more120min。
In the scheme, the prepared copper-iron alloy comprises 0.84-86 wt% of Fe and 5.10-95 wt% of Cu.
In the scheme, the electrolyte adopts a circulating system, and the circulating speed is 700-1400 mL/min.
The application provides another way for preparing the copper-iron alloy by adopting an electrochemical electrolysis technology. A thicker uniform coating can be grown at a faster deposition rate using electrochemical electrolysis at atmospheric pressure, and the properties of the alloy can be achieved by adjusting the electrolyte composition, electrolysis temperature, pH, and plating parameters (stirring mode and rate, current density, etc.).
Due to the adoption of the technical scheme, the application has the following beneficial effects:
(1) The electrodeposited copper-iron alloy electrolyte disclosed by the application does not contain sulfuric acid, sodium dodecyl sulfate and other toxic components harmful to the environment and human health, and belongs to a green and environment-friendly formula.
(2) Compared with the alloy prepared by a physical method, the alloy prepared by electrodeposition has lower cost, and the crystal grains obtained by pulse electrodeposition are fine and compact, belong to the category of nanocrystals, have excellent corrosion resistance and uniform coating thickness, can be electrodeposited at normal temperature, saves energy and is suitable for large-scale industrial production.
(3) The composition and thickness of the alloy can be adjusted by changing the concentration of metal ions and the input amount of complexing agent, etc., and changing the process parameters (temperature, pH, pulse voltage, electrodeposition time, etc.).
Electrochemical reduction of Fe in an electrolyte at pH 2+ And Cu 2+ The activity is greater than H + Thus Fe can be realized 2+ And Cu 2+ Is formed into an alloy by electrochemical co-deposition. But Fe is 2+ The reduction potential is much lower than Cu 2+ Therefore, the electrode potential of the metal ions needs to be balanced as much as possible, the application starts from the formula, and selects the sodium gluconate complexing agent with strong complexing ability to the copper ions and weak complexing ability to the ferrous ions, so that the resistance of copper ion reduction is increased, and the ferrous ions and the copper ions are co-deposited; secondly, boric acid is used as a buffering agent to stabilize the solutionThe pH value of the alloy is reduced, so that the hydrolysis reaction of ferrous ions is facilitated, and meanwhile, the higher electrodeposition temperature is adopted, so that the internal stress of the alloy can be obviously reduced, the continuity of the alloy is ensured, and cracks are not easy to generate.
(4) The application adopts the pulse voltage codeposition alloy method, the obtained alloy is better pure phase, the appearance is compact, the pulse voltage avoids the problem of large deposition voltage difference between copper and iron, the components, the appearance and other microscopic features of the film are improved, the controllable preparation of the copper-iron alloy is realized, and the large-area preparation can be realized.
The electrochemical electrolysis preparation process is simple, high temperature is not needed, the production cost is low, the impurity content of the product is low, the grain size and orientation of the iron phase are easy to control, the porosity is low, and the preparation method is an alloy preparation technology with wide application prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and constitute a part of this specification, are incorporated in and constitute a part of this specification and do not limit the application in any way, and in which:
FIG. 1 shows the microscopic morphology of the copper-iron alloy of 20.16wt% Fe and 76.38wt% Cu prepared in example 2, at high to low magnification, in FIGS. 1a, 1b and 1 c;
FIGS. 2a, 2b and 2c show the microscopic morphology of the copper-iron alloy of composition 42.45wt% Fe, 42.81wt% Cu, from high to low magnification, prepared in example 4;
FIG. 3 is a graph of the microscopic morphology and alloy composition detection energy spectrum of sample 1 prepared in example 1;
FIG. 4 is a graph of the microscopic morphology and alloy composition detection energy spectrum of sample 2 prepared in example 2;
FIG. 5 is a graph of the microscopic morphology and alloy composition detection energy spectrum of sample 3 prepared in example 3;
FIG. 6 is a graph of the microscopic morphology and alloy composition detection energy spectrum of sample 4 prepared in example 4;
FIG. 7 is a graph of the microscopic morphology and alloy composition detection energy spectrum of sample 5 prepared in example 5;
FIG. 8 is an XRD pattern for a Cu-Fe alloy having a composition of 20.16wt% Fe, 76.38wt% prepared in example 2.
Detailed Description
The present application will now be described in detail with reference to the drawings and the specific embodiments thereof, wherein the exemplary embodiments and descriptions of the present application are provided for illustration of the application and are not intended to be limiting.
The embodiment of the application provides a copper-iron alloy electrodeposition preparation method, which comprises the following steps:
adopting a sulfate aqueous solution system as electrolyte, electroplating copper on a copper plate or a stainless steel plate as a negative electrode, an oxygen-evolving anode as a positive electrode, adopting a pulse power supply for deposition, wherein the low potential range is-3 to-5V, and the high potential range is-3.5 to-5.5V; applying pulse voltage with corresponding cathode current density of 80-200 mA/cm 2 The pulse width range is 1-100 ms, the electrolyte circulation speed is controlled to be 700-1400 mL/min, the pH value is controlled to be 2.5-4, the deposition temperature is 45-50 ℃, and the deposition time is 15-120 min; the distance between the positive electrode and the negative electrode is 1-4 cm, and the obtained copper-iron alloy contains Fe0.84-86 wt% and Cu 5.10-95 wt%.
Wherein the sulfate aqueous system electrolyte comprises the following components in mass volume concentration g/L:
100-400 parts of ferrous salt; 8-80 parts of copper sulfate; boric acid 10-30; 1 to 5 portions of o-benzoyl-sulfonyl imide; 20-120 parts of sodium complexing agent. The ferrous salt is Fe (NH) 4 ) 2 (SO 4 ) 2 ·6H 2 O or FeSO 4 ·7H 2 O or FeCl 2 . The sodium complexing agent is sodium gluconate or sodium citrate.
Electrochemical electrolytic preparation of CuFe alloy is realized by introducing an organic complex, circulating an electrolytic tank and adopting a pulse power supply method. Due to Fe during electrochemical reduction in electrolyte with certain pH 2+ And Cu 2+ Are all greater than H + Thus Fe can be realized 2+ And Cu 2+ Is formed into an alloy by electrochemical co-reduction. But Fe is 2+ The reduction potential is much lower than Cu 2+ Therefore, the preparation of the copper-iron alloy is realized by balancing the electrode potential of the metal ions.
The application is further illustrated by the following examples.
Example 1
(1) Taking an oxygen-evolving anode as a positive electrode, taking copper plating on a stainless steel plate as a negative electrode, and carrying out sulfate aqueous solution electrolyte:
Fe(NH 4 ) 2 (SO 4 ) 2 ·6H 2 o200 g/L; 80g/L copper sulfate; boric acid 20g/L; 3g/L of phthalylsulfonyl imide; 100g/L of sodium gluconate.
Depositing by adopting a pulse power supply, wherein the low potential range is-3.5V, and the high potential range is-4V; applying pulse voltage with corresponding cathode current density of 120mA/cm 2 The pulse width range is 80ms, the circulation speed of the electrolyte is controlled to be 1000mL/min, the pH value is 3, and the deposition temperature is 50 ℃; and (3) electrodepositing for 30min at a distance of 3cm between the positive electrode and the negative electrode to produce the iron-copper alloy.
The electrochemical deposition method of the embodiment is adopted to continuously prepare the iron-copper alloy with the components of 9.97wt% of Fe and 87.24wt% of Cu, uniform coating and low impurity content.
Example 2
Taking an oxygen-separating anode as an anode, plating copper on a stainless steel plate as a cathode, and adopting sulfate aqueous solution electrolyte:
Fe(NH 4 ) 2 (SO 4 ) 2 ·6H 2 o300 g/L; 30g/L copper sulfate; boric acid 20g/L; 5g/L of phthalylsulfonyl imide; sodium citrate 80g/L.
Depositing by adopting a pulse power supply, wherein the low potential is-3V, and the high potential is-3.8V; applying pulse voltage with cathode current density of 80mA/cm 2 The pulse width range is 1ms, the circulation speed of the electrolyte is controlled to be 1200mL/min, the pH value is 2.5, and the deposition temperature is 45 ℃; and (3) electrodepositing for 30min at a distance of 1cm between the positive electrode and the negative electrode to produce the iron-copper alloy.
The electrochemical deposition method of the embodiment is adopted to continuously prepare the copper-iron alloy with the components of 20.16wt percent of Fe, 76.38wt percent of Cu, uniform coating and low impurity content.
Example 3
(1) Taking an oxygen-evolving anode as an anode, taking copper plating on a stainless steel plate as a cathode, and adopting sulfate aqueous solution electrolyte:
Fe(NH 4 ) 2 (SO 4 ) 2 ·6H 2 o300 g/L; 50g/L copper sulfate; boric acid 10g/L; 1g/L of phthalylsulfonyl imide; 120g/L of sodium gluconate.
Depositing by adopting a pulse power supply, wherein the low potential range is-4.5V, and the high potential range is-5V; applying pulse voltage with cathode current density of 200mA/cm 2 The pulse width range is 30ms, the circulation speed of the electrolyte is controlled to 1400mL/min, the pH value is 4, and the deposition temperature is 45 ℃; and (3) electrodepositing for 30min at a distance of 2cm between the positive electrode and the negative electrode to produce the iron-copper alloy.
The electrochemical deposition method of the embodiment is adopted to continuously prepare the copper-iron alloy with the components of 32.71wt percent of Fe and 56.42wt percent of Cu, uniform coating and low impurity content.
Example 4
(1) Taking an oxygen-evolving anode as an anode, taking copper plating on a stainless steel plate as a cathode, adopting an electrolyte adopting a sulfate aqueous solution:
FeSO 4 ·7H 2 o400 g/L; 60g/L copper sulfate; boric acid 30g/L; 4g/L of phthalylsulfonyl imide; 60g/L sodium citrate.
Depositing by adopting a pulse power supply, wherein the low potential range is-3.8V, and the high potential range is-4.5V; applying pulse voltage with cathode current density of 150mA/cm 2 The pulse width range is 50ms, the circulation speed of the electrolyte is controlled to be 700mL/min, the pH value is 3.5, and the deposition temperature is 50 ℃; and (3) electrodepositing for 30min at a distance of 4cm between the positive electrode and the negative electrode to produce the iron-copper alloy.
The electrochemical deposition method of the embodiment is adopted to continuously prepare the copper-iron alloy with the components of 42.45wt percent of Fe and 42.81wt percent of Cu, uniform coating and low impurity content.
Example 5
(1) Taking an oxygen-evolving anode as an anode, taking copper plating on a stainless steel plate as a cathode, adopting an electrolyte adopting a sulfate aqueous solution:
FeCl 2 100g/L; copper sulfate 8g/L; boric acid 20g/L; 2g/L of phthalylsulfonyl imide; sodium gluconate 20g/L。
Depositing by adopting a pulse power supply, wherein the low potential range is-4V, and the high potential range is-5.5V; applying pulse voltage with cathode current density of 100mA/cm 2 The pulse width range is 100ms, the circulation speed of the electrolyte is controlled to be 1100mL/min, the pH value is 4, and the deposition temperature is 50 ℃; and (3) electrodepositing for 30min at a distance of 3cm between the positive electrode and the negative electrode to produce the iron-copper alloy.
The electrochemical deposition method of the embodiment is adopted to continuously prepare the copper-iron alloy with the components of 75.45wt percent of Fe, 15.80wt percent of Cu, uniform coating and low impurity content.
As can be seen from the above examples 1 to 5, the iron-copper alloy having different compositions, uniform plating, dense crystal grains and low impurity content was obtained by changing the composition of the electrolyte, adjusting the pH value, and applying different pulse voltage sets.
As can be seen from fig. 1a, 1b, 1 c: FIGS. 1a-1c are copper-iron alloys having a composition of 20.16wt% Fe, 76.38wt% Cu. The microscopic morphology of the alloy is formed by stacking dense irregular spherical grains. From fig. 1a, a high magnification scanning electron micrograph shows dendritic dendrite growth in the interstices between the spherical particles. From FIG. 1c, the scanning electron micrograph of the alloy at low magnification shows that the overall microstructure is a cauliflower-like morphology of small spherical particles packed, indicating that these spherical particles are continually converging and growing during electrodeposition. As can be seen from fig. 2a, 2b, 2 c: FIGS. 2a-2c are copper-iron alloys having a composition of 42.45wt% Fe, 42.81wt% Cu. The alloy has slight cracks in microscopic morphology, and is also piled up into a cauliflower-like morphology from irregular spherical grains. Comparing fig. 1a and fig. 2a, it can be seen that dendrite growth is seen in fig. 1a, whereas only spheroidal grains are grown in fig. 2a, whereby we can get a growth trend that dendrite is copper. Comparing fig. 1b with fig. 2b, it can be seen that the alloy with high iron content has finer and denser grains.
As can be seen from fig. 3, the prepared alloy sample 1 has a uniform surface, a compact microstructure and a cauliflower shape, and has more copper content in the alloy, so that cracks are more obvious, because the growth trend of copper is dendritic dendrite growth; the composition of the alloy prepared was 9.97wt% Fe, 87.24wt% Cu.
As can be seen from fig. 4, the prepared alloy sample 2 has a uniform surface, a compact microstructure and a cauliflower shape, and the alloy has a high copper content, but the cracks are not obvious compared with fig. 3; the composition of the alloy prepared was 20.16wt% Fe, 76.38wt% Cu.
As can be seen from fig. 5, the prepared alloy sample 3 has a uniform surface, a compact microstructure and a cauliflower shape, and the copper content in the alloy is high, but compared with fig. 3, cracks are not obvious; the composition of the alloy prepared was 32.71wt% Fe, 56.42wt% Cu.
As can be seen from fig. 6, the prepared alloy sample 4 has a uniform surface, a compact microstructure and a cauliflower shape, and the alloy has equivalent copper and iron content and only slight cracks; the composition of the alloy prepared was 42.45wt% Fe, 42.81wt% Cu.
As can be seen from fig. 7, the prepared alloy sample 5 has a uniform surface, a compact microstructure, a cauliflower shape, and contains more iron in the alloy, and almost no cracks exist; compared with the figures 3-6, the alloy with more iron content can be obtained with more compact and finer morphology; the composition of the alloy prepared was 75.45wt% Fe, 15.80wt% Cu.
As can be seen from fig. 8: the peaks of the samples of example 2 are all between the peaks of the elemental standard iron and the elemental standard copper, and it can be obtained that the synthesized samples are alloys.
The application is not limited to the above embodiments, and based on the technical solution disclosed in the application, a person skilled in the art may make some substitutions and modifications to some technical features thereof without creative effort according to the technical content disclosed, and all the substitutions and modifications are within the protection scope of the application.
Claims (3)
1. A method for preparing copper-iron alloy based on electrodeposition method, which is characterized by comprising the following steps:
adopting a sulfate aqueous solution system as electrolyte, electroplating copper on a copper plate or a stainless steel plate as a negative electrode, adopting an oxygen-evolving anode as a positive electrode, adopting pulse power deposition, applying pulse voltage, controlling the circulation speed and pH value of the electrolyte to be 2.5-4, and controlling the distance between the positive electrode and the negative electrode to be 1-4 cm to obtain copper-iron alloy;
when the pulse power supply is adopted for deposition, the low potential range is-3 to-5V, and the high potential range is-3.5 to-5.5V;
when pulse voltage is applied, the corresponding cathode current density is 80-200 mA/cm 2 The pulse width ranges from 1 to 100ms, the deposition temperature ranges from 45 to 50 ℃, and the deposition time ranges from 15 to 120min;
the electrolyte adopts a circulating system, and the circulating speed is 700-1400 mL/min;
the sulfate aqueous solution electrolyte comprises the following components in mass volume concentration g/L:
ferrous salt 100-400; 8-80 parts of copper sulfate; boric acid 10-30; 1-5 parts of o-benzoyl-sulfonyl imide; 20-120 parts of sodium complexing agent; the sodium complexing agent is sodium gluconate or sodium citrate.
2. The method for preparing copper-iron alloy based on electrodeposition method according to claim 1, wherein the ferrous salt is Fe (NH 4 ) 2 (SO 4 ) 2 ·6H 2 O、FeSO 4 ·7H 2 O or FeCl 2 。
3. The method for preparing copper-iron alloy based on electrodeposition method according to claim 1, wherein the prepared copper-iron alloy comprises 0.84-86 wt% of Fe and 5.10-95 wt% of Cu.
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| Structural and Magnetic Properties of Electrodeposited CoPt and FeCu Nanowires Embedded in Polycarbonate Membranes;A. Kazadi Mukenga Bantu et al.;《The African Review of Physics》;20151231;第487-496页 * |
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