CN108866594B - Electroplating solution for uranium foil nickel plating and electroplating method thereof - Google Patents

Electroplating solution for uranium foil nickel plating and electroplating method thereof Download PDF

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CN108866594B
CN108866594B CN201810951085.XA CN201810951085A CN108866594B CN 108866594 B CN108866594 B CN 108866594B CN 201810951085 A CN201810951085 A CN 201810951085A CN 108866594 B CN108866594 B CN 108866594B
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plating
nickel
electroplating
uranium
electroplating solution
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CN108866594A (en
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于宁文
罗志福
邓新荣
沈亦佳
向学琴
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China Institute of Atomic of Energy
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/06Wires; Strips; Foils
    • C25D7/0614Strips or foils
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt
    • C25D3/14Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
    • C25D3/16Acetylenic compounds

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Abstract

The invention belongs to the technical field of chemical plating, and relates to an electroplating solution for uranium foil nickel plating and an electroplating method thereof, wherein the electroplating solution contains 500 g/L of metal ion salt 400, 3-8 g/L of conductive salt, 10-50 mg/L of brightener and 5-20 g/L of leveling agent, and the pH of the electroplating solution is 3.5-4.5.

Description

Electroplating solution for uranium foil nickel plating and electroplating method thereof
Technical Field
The invention belongs to the technical field of chemical plating, and relates to an electroplating solution for uranium foil nickel plating and an electroplating method thereof.
Background
A low uranium enrichment target L EU (23519.75 percent of U by mass or a high-concentration uranium target HEU (235U content of more than 90.0% by mass) producing fission molybdenum99Mo, but the low enriched uranium target L EU uranium core differs from the high enriched uranium target HEU uranium core since the low enriched uranium target L EU uranium core uses the pure metal L EU (23519.75 percent of U by mass), so that very thin uranium foils can be rolled and clamped in two concentric aluminum tube interlayers, so that an outer aluminum tube, a uranium foil and an inner aluminum tube are tightly attached, and a fission reflection protective layer is required to cover the surface of the low-concentration uranium target L EU in order to prevent fission fragment damage during reactor irradiation.
Generally, nickel is selected as a material of the fission reflective protective layer, and the fission reflective protective layer is prepared by electroplating a nickel layer on the surface of uranium. In order to facilitate the target to release heat generated by the uranium foil in the irradiation process, the nickel coating on the surface of the uranium foil is required to be tightly combined with the uranium foil and have uniform thickness. In addition, the quality of the nickel plating solution, the plating time, the ease of plating operations, and the like have an important influence on the quality of the nickel plating layer on the surface of the uranium foil, depending on the requirements for producing the uranium target.
Therefore, the selection of an electroplating solution with a proper formula is the key for ensuring the high quality of the uranium foil coating. The ideal electroplating solution should deposit metal ions with larger cathodic reduction polarization so as to obtain a plating layer with small grain size, small gaps, compactness and good adhesive force; should be stable and have good conductivity; the metal electrodeposition speed is stable, and the loading capacity is large; low cost and low toxicity.
Disclosure of Invention
The invention aims to provide an electroplating solution for uranium foil nickel plating, which has more ideal performance and can be better used for uranium foil nickel plating, so that the performance of a prepared plating layer is better.
In order to achieve the purpose, in a basic embodiment, the invention provides an electroplating solution for uranium foil nickel plating, the electroplating solution contains 500 g/L of metal ion salt 400-8 g/L, 10-50 mg/L of brightener and 5-20 g/L of leveling agent, and the pH value of the electroplating solution is 3.5-4.5.
The principle of the invention is as follows:
in order to facilitate the conduction and the release of heat generated by the uranium foil during the irradiation process of the target, the thickness of the nickel coating on the surface of the uranium foil is required to be uniform. The uranium metal is very easy to oxidize in the air and can adsorb impurities such as oil stains and the like; and uranium is also easy to oxidize in aqueous solution, so that the obtained common direct current plating layer has coarser crystallization and obvious plating layer pores, thereby directly influencing the quality of the nickel plating layer. The throwing power of the plating solution has a very important influence on the quality of the plating layer.
The general formula for calculating the throwing power is shown in formula (1). The product of the reciprocal of the resistivity of the plating solution (bath conductivity) and the ratio of the change in the cathodic overvoltage and current density (the magnitude of cathodic polarization) determines the throwing power. The higher the conductivity of the plating solution, the greater the cathodic polarization, and the higher the throwing power.
Equal plating ability is 1/rho.DELTA.n/DELTA.i (1)
In the formula, P is resistivity of the plating liquid, Δ i is change in current density, and Δ n is change in concentration.
From the formula (1), it is important to select an appropriate electrodeposition inhibitor (polymer) and leveling agent in order to improve the throwing power of the nickel layer on the surface of the uranium foil. In addition, the throwing power also depends on the cathode current density, and care should be taken to control the current density during operation.
The metal ion salt, i.e., the primary salt, in the plating bath formulation of the present invention is used to deposit the coating at a concentration that has an effect on the roughness, current density, and plating rate of the coating.
The conductive salt in the electroplating solution formulation of the present invention can promote anodic dissolution. Too low a concentration of anions (e.g., chloride ions) in the conductive salt can lead to passivation of the anode; too high concentration can increase the internal stress of the coating and influence the quality of the coating.
The brightener in the formula of the electroplating solution of the invention endows the micronized precipitated particle plating with brightness and flexibility, and simultaneously levels the plating. When the uranium foil is immersed in the plating solution, the brightener is uniformly adsorbed on the surface of the uranium foil, and the surface of the coating is reduced along with the growth of the coating in the plating process, so that the electrodeposition reaction can be promoted.
The leveling agent in the formula of the electroplating solution can reduce the liquid-gas and liquid-solid interfacial tension, so that hydrogen bubbles are difficult to stay on the surface of a cathode, and the formation of pinholes is reduced. Under the action of the leveling agent, anions specifically adsorbed on the surface of the uranium foil form a monomolecular film under the action of static electricity, and local current concentration is relieved, so that the effect of eliminating stress is achieved, and the uniform plating capacity is improved.
In a preferred embodiment, the invention provides an electroplating solution for uranium foil nickel plating, wherein the metal ion salt is selected from one or more of nickel sulfamate, nickel methylsulfonate and nickel sulfate.
In a preferred embodiment, the invention provides an electroplating solution for uranium foil nickel plating, wherein the conductive salt is selected from nickel chloride and/or nickel bromide.
In a preferred embodiment, the invention provides an electroplating solution for plating nickel on uranium foil, wherein the brightener is selected from silicon dioxide and/or sodium vinyl sulfonate.
In a preferred embodiment, the invention provides an electroplating solution for plating nickel on uranium foil, wherein the brightener has an average particle size of 0.01-1 μm.
In a preferred embodiment, the invention provides an electroplating solution for plating nickel on uranium foil, wherein the leveling agent is selected from sodium dodecyl sulfate and/or N, N-diethyl propyne amine sulfate.
A second object of the present invention is to provide a method for uranium foil nickel plating using the plating solution, which enables better uranium foil nickel plating and enables better performance of the plating layer obtained.
In order to achieve the purpose, in a basic embodiment, the invention provides a method for plating nickel on uranium foil by using the electroplating solution, wherein a cathode uranium foil and an anode nickel foil are placed in the electroplating solution for electroplating.
In a preferred embodiment, the invention provides a method for plating uranium foil with nickel by using the electroplating solution, wherein the electroplating temperature is 35-50 ℃.
In a preferred embodiment, the invention provides a method for plating uranium foil with nickel by using the electroplating solution, wherein the electroplating voltage is 10-30V, and the electroplating current density is 10-30A/dm2The electroplating time is 20-40 minutes.
In a preferred embodiment, the invention provides a method for plating uranium foil with nickel by using the electroplating solution, wherein stirring is continuously carried out during electroplating so as to reduce the generation of polymers.
The electroplating solution for uranium foil nickel plating has more ideal performance, and uranium foil nickel plating can be better carried out by utilizing the electroplating solution and the electroplating method thereof, so that the performance of the prepared plating layer is better.
The electroplating solution and the electroplating method thereof can greatly improve the uniform plating capacity and reduce the coating gaps, thereby meeting the target manufacturing requirement of low-concentration uranium foil targets and providing a foundation for completing the preparation of the targets. Meanwhile, the electroplating solution and the electroplating method thereof have less waste liquid generated in the electroplating process, can reduce the pollution to the environment and are beneficial to environmental protection.
Drawings
FIG. 1 shows the results of electron microscopy on the nickel coating obtained by electroplating the plating solution of formulation 1 of example 1.
FIG. 2 shows the results of electron microscopy on the nickel coating obtained by electroplating the plating solution of formulation 2 of example 1.
Detailed Description
The following description will further describe embodiments of the present invention with reference to the accompanying drawings.
Example 1: preparation of nickel coating on uranium foil surface
The plating solutions were prepared after mixing according to the formulations shown in table 1 below.
TABLE 1 electroplating bath formulation composition
Figure BDA0001770544880000041
Note: the average particle size of the silica and sodium vinylsulfonate is 0.1 to 1 μm.
The cathode uranium foil and the anode nickel foil were respectively suspended in the plating solutions of the respective formulations in table 1 by pulling with a copper wire, and the plating was performed under continuous stirring (600rpm), and the specific plating conditions are shown in table 2 below.
TABLE 2 electroplating conditions for the electroplating baths of the respective formulations
Figure BDA0001770544880000051
Example 2: detection of nickel plating
The nickel plating layers obtained by electroplating the plating solutions of the formulation numbers according to example 1 were examined for plating thickness (measured by an X-ray thickness gauge) and plating porosity (measured by the filter paper attachment method defined in GB 5935), and the results are shown in table 3 below. In addition, electron microscope examination results of the nickel plating layers obtained by electroplating the plating solutions of the formulations 1 and 2 are shown in fig. 1 and 2, respectively.
TABLE 3 test results of nickel plating
Figure BDA0001770544880000052
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.

Claims (6)

1. An electroplating solution for uranium foil nickel plating is characterized in that the electroplating solution contains 500 g/L of metal ion salt 400-containing power, 3-8 g/L of conductive salt, 10-50 mg/L of brightening agent and 5-20 g/L of leveling agent, the pH value of the electroplating solution is 3.5-4.5,
the metal ion salt is selected from one or more of nickel sulfamate, nickel methylsulfonate and nickel sulfate;
the conductive salt is selected from nickel chloride and/or nickel bromide;
the brightening agent is selected from silicon dioxide and/or sodium vinyl sulfonate;
the leveling agent is selected from sodium dodecyl sulfate and/or N, N-diethyl propyne amine sulfate.
2. The plating solution as set forth in claim 1, wherein: the average particle size of the brightener is 0.01-1 mu m.
3. A method for plating nickel on uranium foil is characterized by comprising the following steps: the method comprises the step of placing a cathode uranium foil and an anode nickel foil in the electroplating solution according to any one of claims 1-2 for electroplating.
4. The method of claim 3, wherein: the plating temperature is 35-50 ℃.
5. The method of claim 3, wherein: the plating voltage is 10-30V, and the plating current density is 10-30A/dm2The electroplating time is 20-40 minutes.
6. The method of claim 3, wherein: stirring is continuously carried out in the electroplating process so as to reduce the generation of polymers.
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