CN116219504A - Method for preparing bismuth film by electroplating process, bismuth film and application thereof - Google Patents

Method for preparing bismuth film by electroplating process, bismuth film and application thereof Download PDF

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Publication number
CN116219504A
CN116219504A CN202310284863.5A CN202310284863A CN116219504A CN 116219504 A CN116219504 A CN 116219504A CN 202310284863 A CN202310284863 A CN 202310284863A CN 116219504 A CN116219504 A CN 116219504A
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China
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electroplating
bismuth
bismuth film
film
preparing
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Inventor
许哲峰
彭鲁亚
于金库
范长增
祝萌莹
王妍
王慧慧
张辉辉
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Yanshan University
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Yanshan University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/54—Electroplating: Baths therefor from solutions of metals not provided for in groups C25D3/04 - C25D3/50
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • C25D21/14—Controlled addition of electrolyte components
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The invention provides a method for preparing a bismuth film by an electroplating process, the bismuth film and application thereof. The method comprises injecting electroplating solution into electroplating bath, using copper sheet as cathode, stainless steel as anode, and applying current density of 0.5A/dm 2 ～2.5A/dm 2 The temperature of the electroplating solution is 20-40 ℃, the electroplating time is 2-10 min, the direct current power supply is connected under acidic or neutral environment conditions for electroplating, and the film deposited on the surface of the cathode copper sheet is the prepared bismuth film. The invention adopts the electroplating process, and controls the bismuth plating film by regulating and controlling the current density, the plating time and the plating temperature, thus preparing the bismuth film with smooth and bright surface, low porosity, good binding force, easy thickness control and the like.

Description

Method for preparing bismuth film by electroplating process, bismuth film and application thereof
Technical Field
The invention relates to the technical field of electroplating, in particular to a method for preparing a bismuth film by an electroplating process, the bismuth film and application thereof.
Background
Electroplating is an effective method for obtaining a metal protective layer, and the metal coating obtained by electroplating has fine crystallization, high chemical purity (referred to as single metal) and good binding force. According to the actual needs, the metal plating method can have different electroplating purposes, such as improving the corrosion resistance, the light reflection property, the electrical conductivity, the magnetic conductivity and the brazability of the metal, increasing the surface hardness and the wear resistance, repairing the worn parts, preventing local carburization, nitridation and the like. The plating metal is generally a metal (such as nickel, chromium, zinc, copper) and alloy (such as copper zinc alloy, copper tin alloy, etc.) which is not easy to change in air and solution and has larger hardness. Electroplating is an electrochemical process, and is also a redox process.
Bismuth is a transitional orthorhombic metal, which has both covalent bond and metal bond, and the structure makes the bismuth have a series of special physical and chemical characteristics, and the bismuth metal has the characteristics of no toxicity, no carcinogenicity and no pollution to the environment, so that the bismuth is used as a green metal which can be safely used, and is widely applied to the fields of semiconductors, superconductors, flame retardants, pigments, cosmetics, chemical reagents, electronic ceramics and the like besides being used in the pharmaceutical industry, and has the tendency of substituting toxic elements such as lead, antimony, cadmium mercury and the like. In recent years, along with the development of bismuth industry and the importance of people on environmental protection, the trend of green and environment protection and lead free will provide good development prospect for the deep processing of bismuth series products. Therefore, research on preparing the bismuth film has important significance on development and application of 'green metal' bismuth and research on new materials.
Disclosure of Invention
The invention aims to control the bismuth plating film by regulating and controlling the current density, the plating temperature and the plating time, and prepare the bismuth plating film with the characteristics of smooth and bright surface, low porosity, good binding force and the like.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the invention provides a method for preparing a bismuth film by an electroplating process, which comprises the following steps: injecting the electroplating solution into an electroplating bath, taking a copper sheet as a cathode and stainless steel as an anode, and setting the current density to be 0.5A/dm 2 ～2.5A/dm 2 The temperature of the electroplating solution is 20-40 ℃, the electroplating time is 2-10 min, and the direct current power supply is switched on for electroplating under the acidic or neutral environment condition to obtain the bismuth film deposited on the surface of the copper sheet; wherein the electroplating solution comprises the following components in parts by mass: 15-65 parts of bismuth nitrate, 5-55 parts of complexing agent, 10-70 parts of stabilizer, 3-30 parts of sensitizer and 1100 parts of solvent; the stainless steel is steel with a chromium content of at least 10.5% and a carbon content of not more than 1.2%.
Further, the acidic or neutral environmental condition is specifically pH 6.5.
Further, the complexing agent comprises one or two of citric acid and tartaric acid; the stabilizer comprises one or two of mannitol and polyethylene glycol; the sensitizer is nickel chloride; the solvent is dimethyl sulfoxide.
Further, the complexing agent is citric acid, and the stabilizer is mannitol.
Further, in the plating tank, a distance between the copper sheet and the stainless steel is 8cm.
The second aspect of the invention provides a bismuth film prepared by the method for preparing the bismuth film by the electroplating process.
Further, the thickness of the bismuth film is 5 μm to 80 μm.
The third aspect of the invention provides the application of the bismuth film in the medicine field and the electronic device field.
Compared with the prior art, the technical scheme provided by the invention has at least the following advantages:
compared with chemical plating, the electroplating process has simple operation, fast plating speed and low cost, and the thickness of the film is controlled by changing the parameters of the electroplating process, so that the bismuth film material with bright plating layer, good binding force and thickness of 5-80 μm can be obtained. By increasing the plating time, the film thickness is increased without changing other process parameters.
Drawings
One or more embodiments are illustrated by way of example and not limitation in the figures of the accompanying drawings, which are not to be construed as limiting the embodiments unless specifically indicated otherwise.
FIG. 1 is an XRD pattern of an electroplated bismuth film of the present invention;
FIG. 2 is an SEM image of an electroplated bismuth film of the present invention;
FIG. 3 is a schematic view of an electroplating apparatus for electroplating to prepare a bismuth film according to the present invention.
Detailed Description
The first aspect of the invention provides a method for preparing a bismuth film by an electroplating process, which comprises the following steps: injecting the electroplating solution into an electroplating bath, taking a copper sheet as a cathode and stainless steel as an anode, and setting the current density to be 0.5A/dm 2 ～2.5A/dm 2 The temperature of the electroplating solution is 20-40 ℃, the electroplating time is 2-10 min, and the direct current power supply is switched on for electroplating under the acidic or neutral environment condition to obtain the bismuth film deposited on the surface of the copper sheet; wherein the electroplating solution comprises the following components in parts by mass: 15-65 parts of bismuth nitrate, 5-55 parts of complexing agent, 10-70 parts of stabilizer, 3-30 parts of sensitizer and 1100 parts of solvent; the stainless steel is steel with a chromium content of at least 10.5% and a carbon content of not more than 1.2%.
The second aspect of the invention provides a bismuth film prepared by the method for preparing the bismuth film by the electroplating process.
The third aspect of the invention provides the application of the bismuth film in the medicine field and the electronic device field.
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
In this embodiment 1, the bismuth thin film plating using the plating solution includes the steps of:
preparing electroplating solution; the prepared bismuth plating electroplating solution comprises the following reagent components: 30g of bismuth nitrate, 20g of citric acid, 23g of mannitol, 15g of nickel chloride and 1L of dimethyl sulfoxide to prepare an electroplating solution.
And (5) electroplating preparation process.
The copper matrix is pretreated, in particular polished, degreased and activated.
The plating solution is moved into a plating bath, the copper sheet is placed in the plating solution to serve as a cathode, the stainless steel is placed in the plating solution to serve as an anode, and the interval distance between the cathode and the anode is 8cm. The power supply for electroplating is a direct current power supply, electroplating is carried out, and a film deposited on the surface of the copper matrix is the prepared bismuth film; washing the bismuth-plated copper sheet with deionized water and absolute ethyl alcohol, and drying with a blower to obtain the bismuth film.
The electroplating process conditions were a current density of 1.0A/dm 2 The temperature of the electroplating solution is 25 ℃, the electroplating time is 2min, the electroplating mode adopts a direct current power supply method for electroplating, and the electroplating process is started.
A bismuth film having a thickness of about 13 μm was obtained.
In this embodiment 2, the bismuth thin film plating using the plating solution includes the steps of:
preparing electroplating solution; the prepared bismuth plating electroplating solution comprises the following reagent components: 30g of bismuth nitrate, 20g of citric acid, 23g of mannitol, 15g of nickel chloride and 1L of dimethyl sulfoxide to prepare an electroplating solution.
And (5) electroplating preparation process.
The copper matrix is pretreated, in particular polished, degreased and activated.
The plating solution is moved into a plating bath, the copper sheet is placed in the plating solution to serve as a cathode, the stainless steel is placed in the plating solution to serve as an anode, and the interval distance between the cathode and the anode is 8cm. The power supply for electroplating is a direct current power supply, electroplating is carried out, and a film deposited on the surface of the copper matrix is the prepared bismuth film; washing the bismuth-plated copper sheet with deionized water and absolute ethyl alcohol, and drying with a blower to obtain the bismuth film.
The electroplating process conditions were a current density of 1.0A/dm 2 The temperature of the electroplating solution is 25 ℃, the electroplating time is 6min, the electroplating mode adopts a direct current power supply method for electroplating, and the electroplating process is started.
A bismuth film having a thickness of about 17 μm was obtained.
In this embodiment 3, the bismuth thin film plating using the plating solution includes the steps of:
preparing electroplating solution; the prepared bismuth plating electroplating solution comprises the following reagent components: 30g of bismuth nitrate, 20g of citric acid, 23g of mannitol, 15g of nickel chloride and 1L of dimethyl sulfoxide to prepare an electroplating solution.
And (5) electroplating preparation process.
The copper matrix is pretreated, in particular polished, degreased and activated.
The plating solution is moved into a plating bath, the copper sheet is placed in the plating solution to serve as a cathode, the stainless steel is placed in the plating solution to serve as an anode, and the interval distance between the cathode and the anode is 8cm. The power supply for electroplating is a direct current power supply, electroplating is carried out, and a film deposited on the surface of the copper matrix is the prepared bismuth film; washing the bismuth-plated copper sheet with deionized water and absolute ethyl alcohol, and drying with a blower to obtain the bismuth film.
The electroplating process conditions were a current density of 1.0A/dm 2 The temperature of the electroplating solution is 25 ℃, the electroplating time is 10min, the electroplating mode adopts a direct current power supply method for electroplating, and the electroplating process is started.
A bismuth film having a thickness of about 42 μm was obtained.
In embodiment 4, the bismuth thin film plating using the plating solution includes the steps of:
preparing electroplating solution; the prepared bismuth plating electroplating solution comprises the following reagent components: 15g of bismuth nitrate, 5g of tartaric acid, 10g of polyethylene glycol, 3g of nickel chloride and 1L of dimethyl sulfoxide to prepare an electroplating solution.
And (5) electroplating preparation process.
The copper matrix is pretreated, in particular polished, degreased and activated.
The plating solution is moved into a plating bath, the copper sheet is placed in the plating solution to serve as a cathode, the stainless steel is placed in the plating solution to serve as an anode, and the interval distance between the cathode and the anode is 8cm. The power supply for electroplating is a direct current power supply, electroplating is carried out, and a film deposited on the surface of the copper matrix is the prepared bismuth film; washing the bismuth-plated copper sheet with deionized water and absolute ethyl alcohol, and drying with a blower to obtain the bismuth film.
The electroplating process conditions were a current density of 0.5A/dm 2 The temperature of the electroplating solution is 20 ℃, the electroplating time is 2min, the electroplating mode adopts a direct current power supply method for electroplating, and the electroplating process is started.
A bismuth film having a thickness of about 8 μm was obtained.
In this embodiment 5, the bismuth thin film plating using the plating solution includes the steps of:
preparing electroplating solution; the prepared bismuth plating electroplating solution comprises the following reagent components: 65g of bismuth nitrate, 55g of tartaric acid, 70g of polyethylene glycol, 30g of nickel chloride and 1L of dimethyl sulfoxide to prepare an electroplating solution.
And (5) electroplating preparation process.
The copper matrix is pretreated, in particular polished, degreased and activated.
The plating solution is moved into a plating bath, the copper sheet is placed in the plating solution to serve as a cathode, the stainless steel is placed in the plating solution to serve as an anode, and the interval distance between the cathode and the anode is 8cm. The power supply for electroplating is a direct current power supply, electroplating is carried out, and a film deposited on the surface of the copper matrix is the prepared bismuth film; washing the bismuth-plated copper sheet with deionized water and absolute ethyl alcohol, and drying with a blower to obtain the bismuth film.
The electroplating process conditions were a current density of 2.5A/dm 2 The temperature of the electroplating solution is 40 ℃, the electroplating time is 2min, the electroplating mode adopts a direct current power supply method for electroplating, and the electroplating process is started.
A bismuth film having a thickness of about 7 μm was obtained.
Through the data of examples 1-5, as shown in fig. 1 and fig. 2, the bismuth plating electroplating process parameters can prepare the bismuth film material with compact and flat surface, low porosity, good binding force and film thickness of between 5 and 80 mu m. The bismuth film is prepared by controlling the current density, the plating time and the plating temperature and has the characteristics of smooth and bright surface, low porosity, good binding force, easy thickness control and the like.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples of implementing the present application and that various changes in form and details may be made therein without departing from the spirit and scope of the present application. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention, and the scope of the invention shall be defined by the appended claims.

Claims (8)

1. A method for preparing a bismuth film by an electroplating process, which is characterized by comprising the following steps: injecting the electroplating solution into an electroplating bath, taking a copper sheet as a cathode and stainless steel as an anode, and setting the current density to be 0.5A/dm 2 ～2.5A/dm 2 The temperature of the electroplating solution is 20-40 ℃, the electroplating time is 2-10 min, and the direct current power supply is switched on for electroplating under the acidic or neutral environment condition to obtain the bismuth film deposited on the surface of the copper sheet;
wherein the electroplating solution comprises the following components in parts by mass: 15-65 parts of bismuth nitrate, 5-55 parts of complexing agent, 10-70 parts of stabilizer, 3-30 parts of sensitizer and 1100 parts of solvent;
the stainless steel is steel with a chromium content of at least 10.5% and a carbon content of not more than 1.2%.
2. The method for preparing a bismuth film by electroplating process according to claim 1, wherein the acidic or neutral environmental condition is a specific pH of 6.5.
3. The method for preparing a bismuth film by an electroplating process according to claim 1, wherein the complexing agent comprises one or a combination of citric acid and tartaric acid;
the stabilizer comprises one or two of mannitol and polyethylene glycol;
the sensitizer is nickel chloride;
the solvent is dimethyl sulfoxide.
4. The method for preparing a bismuth film by electroplating process according to claim 3, wherein the complexing agent is citric acid and the stabilizer is mannitol.
5. The method of preparing a bismuth film by electroplating according to claim 1, wherein the copper sheet is spaced apart from the stainless steel by a distance of 8cm in the electroplating bath.
6. A bismuth film produced by the method for producing a bismuth film by the plating process as claimed in any one of claims 1 to 5.
7. The bismuth film according to claim 6, wherein the thickness of the bismuth film is 5 μm to 80 μm.
8. Use of the bismuth film as claimed in claim 6 or 7 in the medical field, in the field of electronic devices.
CN202310284863.5A 2023-03-22 2023-03-22 Method for preparing bismuth film by electroplating process, bismuth film and application thereof Pending CN116219504A (en)

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CN116219504A true CN116219504A (en) 2023-06-06

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