CN114108042A - Rare earth surface treatment agent for improving electrochemical corrosion resistance of copper foil surface and surface treatment process - Google Patents
Rare earth surface treatment agent for improving electrochemical corrosion resistance of copper foil surface and surface treatment process Download PDFInfo
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- CN114108042A CN114108042A CN202111612894.6A CN202111612894A CN114108042A CN 114108042 A CN114108042 A CN 114108042A CN 202111612894 A CN202111612894 A CN 202111612894A CN 114108042 A CN114108042 A CN 114108042A
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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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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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
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
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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
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention relates to the technical field of electrolytic copper foil, and discloses a rare earth surface treating agent for improving electrochemical corrosion resistance of the surface of copper foil, which comprises the following components: potassium pyrophosphate, zinc sulfate, nickel sulfate, metalloid salt, additive A and rare earth salt, can effectively improve the electrochemical corrosion resistance of the surface of the copper foil. According to the invention, the electrochemical corrosion resistance of the surface of the copper foil is improved by electrolytically depositing the Zn-Ni-metalloid element (Si, As, B) -rare earth element (La, Ce, Pr, Nd) quaternary alloy coating on the surface of the copper foil. The metalloid can make the plating layer present amorphous state, and improve the electrochemical corrosion resistance of the plating layer; the rare earth elements have characteristic adsorption, can effectively improve the compact uniformity of the microstructure of the plating layer, and can also effectively improve the electrochemical corrosion resistance of the plating layer.
Description
Technical Field
The invention belongs to the field of electrolytic copper foil, and particularly relates to a rare earth surface treatment agent for improving electrochemical corrosion resistance of the surface of copper foil and a surface treatment process.
Background
With the rapid development of the electronic information industry, the performance requirements of the electrolytic copper foil are gradually improved, at present, researchers at home and abroad carry out a series of surface strengthening treatment researches on the electrolytic copper foil and obtain corresponding research results, but the electrochemical corrosion resistance of the electrolytic copper foil in China still has obvious difference with the foreign development and needs to be improved.
Relevant researches show that the metalloid can enable the coating to be in an amorphous state, and the electrochemical corrosion resistance of the coating is improved. The method changes the components and the content of the additive while keeping the performance of the original plating solution, can improve the stability of the plating solution, obtains better plating quality, and improves the service performance. The rare earth element has an unfilled 4 f-layer electronic layer structure, so that the chemical property of the rare earth element is more active, and the stability of plating solution and the performance of a plating layer in the traditional electrodeposition process can be obviously improved; and the rare earth ions are easy to be adsorbed on active points of crystal growth, so that the crystal growth speed can be slowed down, the crystal structure of the coating is refined, the microstructure of the coating is compact and uniform, and the effect of improving the electrochemical corrosion resistance is also achieved.
The existing copper foil surface galvanizing technology has the phenomena that the crystallization of an alloy layer is not fine and uniform enough and the electrochemical corrosion resistance is not ideal.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a rare earth surface treatment agent for improving the electrochemical corrosion resistance of the surface of a copper foil and a surface treatment process, wherein a metalloid (Si, As, B) and a rare earth metal (La, Ce, Pr, Nd) are introduced into a zinc alloy coating for research, and in the surface treatment agent, a quaternary alloy coating containing Zn-Ni-metalloid element (Si, As, B) -rare earth element (La, Ce, Pr, Nd) is electrodeposited on the surface of an electrolytic copper foil, so that the electrochemical corrosion resistance of the surface of the copper foil is effectively improved.
The first purpose of the invention is to provide a rare earth surface treating agent for improving the electrochemical corrosion resistance of the surface of copper foil, which comprises the following components: 120 g/L potassium pyrophosphate, 5-25g/L zinc sulfate, 5-30g/L nickel sulfate, 5-35g/L metalloid salt, 3-15mg/L additive A, and rare earth salt.
The beneficial effect who adopts above-mentioned scheme is: the invention provides a surface treating agent containing rare earth elements for electrodeposition on the surface of a copper foil, and particularly provides a surface treating agent for preparing a copper foil with good electrochemical corrosion resistance by electrodeposition of metalloid elements and rare earth elements.
Further, the metalloid element in the metalloid salt is one or a mixture of two or more of Si, As and B.
Preferably, the metalloid salt is sodium borate.
Furthermore, the rare earth elements in the rare earth salt are one or the mixture of more than two of La, Ce, Pr and Nd.
Preferably, the rare earth salt is one or two of cerium sulfate and lanthanum sulfate.
Further, 1-10g/L of cerium sulfate and 1-10g/L of lanthanum sulfate.
Further, the additive A is one or two of sodium polydithio-dipropyl sulfonate (SPS) and polyethylene glycol (PEG), and the solvent of the surface additive is deionized water.
Further, the surface treatment agent comprises the following components: 250g/L potassium pyrophosphate, 5-20g/L zinc sulfate, 5-25g/L nickel sulfate, 5-30g/L sodium borate, 1-8g/L cerium sulfate, 1-8g/L lanthanum sulfate and 3-10mg/L additive A.
Preferably, the surface treatment agent comprises the following components: 230g/L of potassium pyrophosphate 130-.
The second object of the present invention is to provide a method for improving the resistance of the surface of a copper foil to electrochemical corrosion by using the above rare earth surface treating agentThe surface treatment process for etching performance comprises the following steps: placing the pretreated copper foil in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 8-11, temperature 35-45 deg.C, and current density 1-3.5A/dm2The plating time is 5-10 s.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the uniform and fine Zn-Ni-metalloid element (Si, As, B) -rare earth element (La, Ce, Pr and Nd) quaternary alloy coating is formed on the surface of the copper foil by electroplating, so that the electrochemical corrosion resistance of the surface of the copper foil is improved;
(2) the metalloid provided by the invention can enable the plating layer to be in an amorphous state, and improve the electrochemical corrosion resistance of the plating layer;
(3) the rare earth element provided by the invention has characteristic adsorption, can effectively improve the compactness uniformity of the microstructure of the plating layer, and can also effectively improve the electrochemical corrosion resistance of the plating layer.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
A rare earth surface treating agent for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following components: 130g/L potassium pyrophosphate, 10g/L zinc sulfate, 15g/L nickel sulfate, 10g/L sodium borate, 1g/L cerium sulfate and 5mg/L additive A. Wherein, the additive A is SPS, and the solvent of the surface additive is deionized water.
A surface treatment process for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following steps: placing the copper foil with thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 9, temperature 35 deg.C, and current density 1.5A/dm2The plating time was 8 s.
Example 2
A rare earth surface treating agent for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following components: 135g/L of potassium pyrophosphate, 8g/L of zinc sulfate, 15g/L of nickel sulfate, 12g/L of sodium borate, 1g/L of cerium sulfate and 5mg/L of additive A. Wherein, the additive A is PEG, and the solvent of the surface additive is deionized water.
A surface treatment process for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following steps: placing the copper foil with the thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 9.5, temperature 38 deg.C, and current density 2A/dm2The plating time was 6 s.
Example 3
A rare earth surface treating agent for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following components: 140g/L potassium pyrophosphate, 8g/L zinc sulfate, 15g/L nickel sulfate, 10g/L sodium borate, 1g/L lanthanum sulfate and 5mg/L additive A. Wherein, the additive A is SPS, and the solvent of the surface additive is deionized water.
A surface treatment process for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following steps: placing the copper foil with thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 10, temperature 42 deg.C and current density 2.5A/dm2The plating time was 5 s.
Example 4
A rare earth surface treating agent for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following components: 150g/L potassium pyrophosphate, 12g/L zinc sulfate, 20g/L nickel sulfate, 15g/L sodium borate, 1.5g/L lanthanum sulfate and 6mg/L additive A. Wherein, the additive A is PEG, and the solvent of the surface additive is deionized water.
A surface treatment process for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following steps: placing the copper foil with thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 10.5, temperature 41 deg.C, and current density 3A/dm2The plating time was 5 s.
Example 5
A rare earth surface treating agent for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following components: 165g/L potassium pyrophosphate, 15g/L zinc sulfate, 25g/L nickel sulfate, 15g/L sodium borate, 2g/L cerium sulfate and 8mg/L additive A. Wherein, the additive A is formed by mixing SPS and PEG according to the proportion of 1:1, and the solvent of the surface additive is deionized water.
A surface treatment process for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following steps: placing the copper foil with thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 10, temperature 38 deg.C, and current density 3A/dm2The plating time was 4 s.
Example 6
A rare earth surface treating agent for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following components: 170g/L potassium pyrophosphate, 15g/L zinc sulfate, 20g/L nickel sulfate, 20g/L sodium borate, 2.5g/L cerium sulfate and 8mg/L additive A. Wherein, the additive A is formed by mixing SPS and PEG according to the proportion of 1:1, and the solvent of the surface additive is deionized water.
A surface treatment process for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following steps: placing the copper foil with thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 9.5, temperature 41 deg.C, and current density 4A/dm2The plating time was 5 s.
Example 7
A rare earth surface treating agent for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following components: 160g/L potassium pyrophosphate, 12g/L zinc sulfate, 25g/L nickel sulfate, 20g/L sodium borate, 1.5g/L cerium sulfate, 1.5g/L lanthanum sulfate and 8mg/L additive A. Wherein, the additive A is formed by mixing SPS and PEG according to the proportion of 1:1, and the solvent of the surface additive is deionized water.
A surface treatment process for improving electrochemical corrosion resistance of the surface of a copper foil comprises the following steps: placing the copper foil with thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 9.5, temperature 41 deg.C, and current density 3A/dm2The plating time was 5 s.
Comparative example 1
The rare earth surface treating agent for the copper foil comprises the following components: 140g/L of potassium pyrophosphate, 10g/L of zinc sulfate, 20g/L of nickel sulfate, 20g/L of sodium borate and 8mg/L of additive A. Wherein, the additive A is formed by mixing SPS and PEG according to the proportion of 1:1, and the solvent of the surface additive is deionized water.
A surface treatment process of copper foil comprises the following steps: placing the copper foil with thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 10, temperature 40 deg.C, and current density 2A/dm2The plating time was 8 s.
Comparative example 2
The rare earth surface treating agent for the copper foil comprises the following components: 140g/L of potassium pyrophosphate, 10g/L of zinc sulfate, 20g/L of nickel sulfate and 8mg/L of additive A. Wherein, the additive A is formed by mixing SPS and PEG according to the proportion of 1:1, and the solvent of the surface additive is deionized water.
A surface treatment process of copper foil comprises the following steps: placing the copper foil with thickness of 12 μm after acid cleaning, roughening and curing treatment in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 10, temperature 40 deg.C, and current density 2A/dm2The plating time was 8 s.
And (3) performance testing:
the copper foils provided in the examples and comparative examples were subjected to a performance test by the following method:
and fitting a Tafel curve tested by an electrochemical workstation to obtain the self-corrosion current density and the self-corrosion potential so as to evaluate the electrochemical corrosion resistance of the coating. The self-corrosion potential reflects the difficulty of alloy corrosion, and the self-corrosion current density reflects the corrosion rate of the alloy. The closer the self-corrosion potential is to 0, the smaller the self-corrosion current density is, the better the electrochemical corrosion resistance of the alloy is.
The electrochemical test adopts a three-electrode system, the prepared copper foil is used as a working electrode, a lead plate is used as a counter electrode, and a saturated calomel electrode is used as a reference electrode; the corrosion medium is NaCl solution with the mass fraction of 3.5%, the three-electrode system is soaked in the corrosion medium, the polarization curve is measured by connecting equipment to obtain the self-corrosion current density and self-corrosion potential data, and the intuitive electrochemical corrosion resistance of the surface layer of the copper foil is obtained according to the self-corrosion current density and self-corrosion potential data.
The experimental data of the performance test of each example and comparative example are shown in table 1.
TABLE 1 data of performance test experiment for each example and comparative example
It can be seen by comparing the test data in table 1 that the self-corrosion current density of examples 1 to 7 is one order of magnitude lower than that of comparative examples 1 to 2, the self-corrosion potential is also significantly higher than that of comparative examples 1 to 2 to which no metalloid element B and no rare earth metals La and Ce are added, the self-corrosion potential of examples 1 to 7 is closer to 0, and it can be judged that the electrochemical corrosion resistance of the surface of the copper foil can be significantly improved by adding the metalloid element and the rare earth metals.
Comparing examples 1 to 7, the self-etching current density of example 7 with the simultaneous addition of cerium sulfate and lanthanum sulfate was lower than that of examples 1 to 6, and the self-etching potential thereof was higher than that of examples 1 to 6, and the self-etching potential of example 7 was closer to 0, so that it was determined that the simultaneous addition of cerium sulfate and lanthanum sulfate could more effectively improve the electrochemical corrosion resistance of the copper foil surface.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The rare earth surface treating agent for improving the electrochemical corrosion resistance of the surface of the copper foil is characterized by comprising the following components: 120 g/L potassium pyrophosphate, 5-25g/L zinc sulfate, 5-30g/L nickel sulfate, 5-35g/L metalloid salt, 3-15mg/L additive A, and rare earth salt.
2. The surface treating agent according to claim 1, wherein the metalloid element in the metalloid salt is one or a mixture of two or more of Si, As and B.
3. The surface treating agent according to claim 2, wherein the metalloid salt is sodium borate.
4. The surface treating agent according to claim 1, wherein the rare earth element in the rare earth salt is one or a mixture of two or more of La, Ce, Pr and Nd.
5. The surface treating agent according to claim 4, wherein the rare earth salt is one or both of cerium sulfate and lanthanum sulfate.
6. The surface treating agent according to claim 5, wherein the cerium sulfate is 1 to 10g/L and the lanthanum sulfate is 1 to 10 g/L.
7. The surface treating agent according to claim 1, wherein the additive A is one or two of sodium polydithio-dipropyl sulfonate and polyethylene glycol, and the solvent of the surface additive is deionized water.
8. The surface treating agent according to claim 1, characterized by comprising the following components: 250g/L potassium pyrophosphate, 5-20g/L zinc sulfate, 5-25g/L nickel sulfate, 5-30g/L sodium borate, 1-8g/L cerium sulfate, 1-8g/L lanthanum sulfate and 3-10mg/L additive A.
9. The surface treating agent according to claim 8, characterized by comprising the following components: 230g/L of potassium pyrophosphate 130-.
10. Improvement by using the rare earth surface treatment agent according to any one of claims 1 to 9The surface treatment process for the electrochemical corrosion resistance of the surface of the copper foil is characterized by comprising the following steps of: placing the pretreated copper foil in an electrolytic bath containing the surface treating agent, controlling the process conditions of pH 8-11, temperature 35-45 deg.C, and current density 1-3.5A/dm2The plating time is 5-10 s.
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2021
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