CN108060443B - A kind of preparation method of the melanism composite layer on extruded metal foil surface - Google Patents

A kind of preparation method of the melanism composite layer on extruded metal foil surface Download PDF

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Publication number
CN108060443B
CN108060443B CN201711390259.1A CN201711390259A CN108060443B CN 108060443 B CN108060443 B CN 108060443B CN 201711390259 A CN201711390259 A CN 201711390259A CN 108060443 B CN108060443 B CN 108060443B
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nickel
melanism
zinc
composite layer
preparation
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CN108060443A (en
Inventor
刘新宽
刘平
陈小红
张宁
李伟
马凤仓
何代华
张柯
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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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
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • 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
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • 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
    • C25D3/22—Electroplating: Baths therefor from solutions of zinc
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

A kind of preparation method of melanism composite layer, for preparing melanism composite layer on extruded metal foil surface, comprising: step 1 carries out degreasing and rust removal pretreatment to extruded metal foil；Step 2, pretreated extruded metal foil surface carries out copper plating treatment in step 1；Step 3, using nickel plating solution to the carry out Nickel Plating Treatment of the extruded metal foil after copper plating treatment in step 2, nickel plating solution contains: Ni2+30~80g/L, 30~60g/L of complexing agent, 10~40g/L of boric acid and nickel-plating additive 0.01-1.2ml/L, the pH value of nickel plating solution are 3-6；Step 4 carries out zinc-plated processing to the extruded metal foil after Nickel Plating Treatment in step 3 using galvanizing solution, and galvanizing solution contains: Zn2+20-60g/L and zinc-plating additive 0.01-2g/L, melanism composite layer includes top-down zinc metal layer, with a thickness of 0.5-1.5 μm of nickel metal layer and copper metal layer, nickel metal layer is nickel coating, nickel crystallite in the nickel coating is column, it is erected in the surface of copper metal layer, the spacing between the nickel crystallite adjacent to each other of same layer is 20-100nm.

Description

A kind of preparation method of the melanism composite layer on extruded metal foil surface
Technical field
The present invention relates to a kind of preparation methods of melanism composite layer, and in particular to one kind prepares black on extruded metal foil surface Change the method for composite layer
Background technique
Extruded metal foil especially rolled copper foil has good ductility, shoulders flexibility, low roughness and high folding resistance, The basic material for having become flexible printed-circuit board, is mainly used in flexible electric circuit board and high-frequency circuit board.In order to meet electricity For road plate to the requirement such as copper foil heat resistance and corrosion resistance and solderability, rolled copper foil surface, which generally requires, carries out Darkening process (copper- Cobalt-nickel or copper-nickel coating) and reddening processing (fine copper coating).The processing of reddening (copper facing) processing method, that is, electrolytic copper foil surface Method, but thus flexible printed-circuit board made of kind method treated rolled copper foil, anti-stripping property, etching, solderability It is unable to satisfy the production requirement of flexible print wiring board, therefore forms the surface treatment skill of the rolled copper foil characterized by melanism Art.
Current rolled copper foil surface melanism technology generally carries out complicated processing, rolled copper foil to the surface of rolled copper foil Surface needs to carry out multiple electro-coppering, plating nickel cobalt, zinc-plated or even chromium plating.Plating nickel cobalt processing is wherein most importantly carried out, is passed through Black agent is added in nickel plating solution to obtain black.Common Darkening process has: scheme 1 is added when plating nickel cobalt processing and contains SCN-Black agent such as KSCN, NHSCN, SC (NH2)2Deng acquisition black surface copper foil.Scheme 2, rolled copper foil is by degreasing Reason, primary roughening, secondary roughening, three times roughening, nickel cobalt (alloy) processing, zinc-plated processing, using one layer of antirust treatment and coating Silane coupling agent finally obtains product.Scheme 3, rolled copper foil process flow is electrolytic degreasing, pickling, the first solidification, first thick Change, the second roughening, the second solidification, melanism, plating nickel cobalt, zinc-plated and chromium plating.Rolled copper foil electricity in traditional blackening treatment process Using addition cobalt compound, even rhodanide such as KSCN, NHSCN, SC (NH when plating nickel cobalt2)2It is obtained Deng black agent is used as Preferable black effect, but rhodanide will lead to serious pollution problem, and use agent containing cobalt black merely, often without Method obtains the black met the requirements, more can only obtain grey coating.In addition, since cobalt belongs to strategic materials element, price Height also increases the production cost of copper foil processing.
Therefore, traditional rolled copper foil Darkening process is due to, addition cobalt complicated with technical matters or rhodanide work The problem of will lead to seriously polluted and higher cost for black agent, it would be highly desirable to improve.
Summary of the invention
The present invention is to solve traditional Darkening process and cross, addition cobalt complicated with technical matters or rhodanide conduct Black agent will lead to the problem of seriously polluted and higher cost, and it is an object of the present invention to provide a kind of melanism on extruded metal foil surface is multiple Close the preparation method of layer.
The present invention provides a kind of preparation method of melanism composite layer, for compound in extruded metal foil surface preparation melanism Layer characterized by comprising step 1 carries out degreasing and rust removal pretreatment to extruded metal foil；Step 2, it is pre- in step 1 Treated, and extruded metal foil surface carries out copper plating treatment；Step 3, using nickel plating solution to after copper plating treatment in step 2 Extruded metal foil carry out Nickel Plating Treatment, nickel plating solution contains: Ni2+30~80g/L, 30~60g/L of complexing agent, boric acid 10~ 40g/L and nickel-plating additive 0.01-1.2ml/L, the pH value of nickel plating solution are 3-6；Step 4, using galvanizing solution to through step Extruded metal foil in rapid three after Nickel Plating Treatment carries out zinc-plated processing, and galvanizing solution contains: Zn2+20-60g/L and zinc-plated addition Agent 0.01-2g/L, melanism composite layer include top-down zinc metal layer, with a thickness of 0.5-1.5 μm of nickel metal layer and copper Metal layer, nickel metal layer are nickel coating, and the nickel crystallite in the nickel coating is column, are erected in the surface of copper metal layer, same layer Nickel crystallite adjacent to each other between spacing be 20-100nm.
The preparation method of melanism composite layer provided by the invention, can also have the feature that, it is characterised in that: its In, extruded metal foil is rolled copper foil.
The preparation method of melanism composite layer provided by the invention, can also have the feature that, it is characterised in that: its In, complexing agent is citric acid, sodium citrate, the mixture of one of lactic acid or more.
The preparation method of melanism composite layer provided by the invention, can also have the feature that, it is characterised in that: its In, the mixture of nickel-plating additive BN-91, one or both of BN-92.
The preparation method of melanism composite layer provided by the invention, can also have the feature that, it is characterised in that: its In, the temperature of Nickel Plating Treatment is 20-40 DEG C, current density 16-48A/dm2, electroplating time 2-20s.
The preparation method of melanism composite layer provided by the invention, can also have the feature that, it is characterised in that: its In, zinc-plating additive is the mixture of one or both of o-benzoic sulfimide and Isosorbide-5-Nitrae-butynediols.
The preparation method of melanism composite layer provided by the invention, can also have the feature that, it is characterised in that: its In, the temperature of zinc-plated processing is 20-40 DEG C, current density 13-39A/dm2, electroplating time 2-20s.
The action and effect of invention
The preparation method of the melanism composite layer on the extruded metal foil surface in the present invention only needs to carry out oil removing before plating to remove Rust does not use any black agent containing SCN- such as KSCN, NH in entire electroplating process4SCN、SC(NH2)2Equal Toxics Matter, also eliminates the cobalt of higher cost, has both met the requirement that rolled copper foil surface is in black, has in turn avoided in process Pollution problem.The preparation method of melanism composite layer of the invention, simple process is pollution-free, low in cost.
The melanism composite layer prepared using the preparation method in the present invention includes the electro-coppering of bottoming, guarantees that melanism is multiple That closes layer and substrate has good combination；Nanometer column is presented in nickel coating above copper coating, the crystal grain in layer, it is seen that light enters When penetrating, light wave reflects repeatedly between column and column, can largely be predominantly absorbed, therefore coating can show black；Nickel coating The zinc coating of top, the crystal grain in layer are similarly a nanometer column, it is contemplated that the second layer is not fine and close smooth structure, third layer plating The column of layer president on second layer column is askew, dendritic structure occurs；By two layers of column structure, forms in coating and much receive Meter level micropore since the double-deck gap has lower refraction coefficient, thus increases the uptake to light, so that coating be made to present Deeper black out.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of melanism composite layer；And
Fig. 2 is the photo of melanism composite layer.
Specific embodiment
It is real below in order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention Apply composition of the example combination attached drawing to the preparation method of the melanism composite layer on extruded metal foil provided by the invention surface, working principle And beneficial effect is specifically addressed.
BN-91 in the present invention, BN-92 are the additive of commercially available nickel plating.
The preparation method of the melanism composite layer on the extruded metal foil surface in the present invention is as follows:
Step 1 carries out degreasing and rust removal pretreatment to rolled copper foil.That is, using the sodium hydroxide water of 30-50g/L under room temperature Solution carries out oil removal treatment to the surface of rolled copper foil；It is the sulfuric acid of 30-50% to calendering copper that mass percent is used under room temperature The surface of foil carries out pickling processes.
Step 2, pretreated rolled copper foil surface carries out copper plating treatment in step 1.
Step 3, using nickel plating solution to the carry out Nickel Plating Treatment of the rolled copper foil after copper plating treatment in step 2, plating Nickel solution contains:
Ni2+30~80g/L, 30~60g/L of complexing agent, 10~40g/L of boric acid and nickel-plating additive 0.01-1.2ml/L, The pH value of nickel plating solution is 3-6.Complexing agent is citric acid, sodium citrate, the mixture of one of lactic acid or more, nickel plating Additive is BN-91, the mixture of one or both of BN-92,
The temperature of Nickel Plating Treatment is 20-40 DEG C, current density 16-48A/dm2, electroplating time 2-20s.
Step 4 carries out zinc-plated processing to the rolled copper foil after Nickel Plating Treatment in step 3 using galvanizing solution, zinc-plated Solution contains:
Zn2+20-60g/L and zinc-plating additive 0.01-2g/L, zinc-plating additive are o-benzoic sulfimide and Isosorbide-5-Nitrae- The mixture of one or both of butynediols,
The temperature of zinc-plated processing is 20-40 DEG C, current density 13-39A/dm2, electroplating time 2-20s.
Fig. 1 is the structural schematic diagram of melanism composite layer.
Fig. 2 is the photo of melanism composite layer.
As depicted in figs. 1 and 2, the melanism composite layer prepared on the rolled copper foil surface in the present invention includes copper coating 2, nickel Coating 3 and zinc coating 4.
Copper coating 2 with a thickness of 0.1-1 μm, compact structure is directly plated on copper foil matrix 1.
Nickel coating 3 is plated on the surface of copper coating 2, with a thickness of 0.5-1.5 μm.Nickel crystallite in nickel coating 3 is array It is uniformly distributed in the column on 2 surface of copper coating, is erected in the surface of copper coating 2.The width of nickel crystallite cross section is 50-500nm, Spacing between the nickel crystallite adjacent to each other of same layer is 20-100nm.
Zinc coating 4 is plated on the surface of nickel coating 3, with a thickness of 0.5-1.5 μm.Zinc crystal grain in zinc coating 4 is column, is erected The surface of nickel coating 3 is stood on, corresponding growth has at least one zinc crystal grain above a nickel crystallite.The width of the cross section of zinc crystal grain For 50-500nm.
Specific experiment process is as described below:
Step 1 is carried out at oil removing using surface of the sodium hydrate aqueous solution of 30-50g/L to rolled copper foil under room temperature Reason；Mass percent is used to carry out pickling processes for surface of the sulfuric acid of 30-50% to rolled copper foil under room temperature.
Step 2, pretreated rolled copper foil surface carries out copper plating treatment in step 1.
Step 3, using different nickel plating solutions and different electroplating technologies to the calendering after copper plating treatment in step 2 The carry out Nickel Plating Treatment of copper foil.Different nickel plating solutions be include Ni2+30~80g/L, 30~60g/L of complexing agent, boric acid 10 ~40g/L and nickel-plating additive 0.01-1.2ml/L, the pH value of nickel plating solution are 3-6.Wherein, complexing agent is citric acid, lemon Lemon acid sodium, the mixture of one of lactic acid or more, nickel-plating additive BN-91's, one or both of BN-92 is mixed Close object.Different electroplating technologies include: the pH value of nickel plating solution, the temperature of Nickel Plating Treatment, the current density of Nickel Plating Treatment and The electroplating time of Nickel Plating Treatment.
Step 4 is adopted using different galvanizing solutions and different electroplating technologies to the pressure after Nickel Plating Treatment in step 3 Prolong copper foil and carries out zinc-plated processing.Different galvanizing solutions be include Zn2+20-60g/L and zinc-plating additive 0.01-2g/L. Wherein, zinc-plating additive is the mixture of one or both of o-benzoic sulfimide and Isosorbide-5-Nitrae-butynediols.Different Electroplating technology includes: the electroplating time of the temperature of zinc-plated processing, the current density of zinc-plated processing and zinc-plated processing.
Under in conjunction with the embodiments 1-6 come the effect of the rolled copper foil for the surface melanism being described in detail in the present embodiment.
The technological parameter of melanism composite layer is prepared in 1 embodiment 1-6 of table
The surface color of the rolled copper foil of surface melanism carries out colorimetric card pair using the world RAL-K7 colour atla in embodiment 1-6 According to test, surface color value meets the color requirement of melanism copper foil between RAL-7016 to RAL-7022.According to GB/T 29847-2013 " printing board-use copper-clad test method " tests its surface roughness, surface roughness Ra≤2.0 μm, Rz≤1.77μm.The test of peel strength, removing are carried out according to GB/T 29847-2013 " printing board-use copper-clad test method " Intensity reaches 1.4N/mm or more；With good acid resistance, alkali resistance, soldering resistance and etching.
The action and effect of embodiment
The preparation method of the melanism composite layer on the extruded metal foil surface in the present invention only needs to carry out oil removing before plating to remove Rust contains SCN without using any in entire electroplating process-Black agent such as KSCN, NH4SCN、SC(NH2)2Equal Toxics Matter, also eliminates the cobalt of higher cost, has both met the requirement that rolled copper foil surface is in black, has in turn avoided in process Pollution problem.The preparation method of melanism composite layer of the invention, simple process is pollution-free, low in cost.
The melanism composite layer prepared using the preparation method in the present invention includes the electro-coppering of bottoming, guarantees that melanism is multiple That closes layer and substrate has good combination；Nanometer column is presented in nickel coating above copper coating, the crystal grain in layer, it is seen that light enters When penetrating, light wave reflects repeatedly between column and column, can largely be predominantly absorbed, therefore coating can show black；Nickel coating The zinc coating of top, the crystal grain in layer are similarly a nanometer column, it is contemplated that the second layer is not fine and close smooth structure, third layer plating The column of layer president on second layer column is askew, dendritic structure occurs；By two layers of column structure, forms in coating and much receive Meter level micropore since the double-deck gap has lower refraction coefficient, thus increases the uptake to light, so that coating be made to present Deeper black out.
The embodiment is preferred case of the invention, the protection scope being not intended to limit the invention.

Claims (7)

1. a kind of preparation method of melanism composite layer, for preparing the melanism composite layer, feature on extruded metal foil surface It is, comprising:
Step 1 carries out degreasing and rust removal pretreatment to the extruded metal foil；
Step 2, pretreated extruded metal foil surface carries out copper plating treatment in step 1；
Step 3, using nickel plating solution to the carry out Nickel Plating Treatment of the extruded metal foil after copper plating treatment in step 2, The nickel plating solution contains:
Ni2+30~80g/L, 30~60g/L of complexing agent, 10~40g/L of boric acid and nickel-plating additive 0.01-1.2ml/L,
The pH value of the nickel plating solution is 3-6；
Step 4 carries out zinc-plated processing, institute to the extruded metal foil after Nickel Plating Treatment in step 3 using galvanizing solution Galvanizing solution is stated to contain:
Zn2+20-60g/L and zinc-plating additive 0.01-2g/L,
The current density of the zinc-plated processing is 13-39A/dm2,
The melanism composite layer includes the top-down zinc metal layer with a thickness of 0.5-1.5 μm, with a thickness of 0.5-1.5 μm of nickel Metal layer and copper metal layer,
The nickel metal layer is nickel coating, and the nickel crystallite in the nickel coating is column, is erected in the surface of the copper metal layer, together Spacing between one layer of the nickel crystallite adjacent to each other is 20-100nm,
The zinc metal layer is zinc coating, and the zinc crystal grain in the zinc coating is column, is erected in the surface of the nickel coating,
At least one described zinc crystal grain is correspondingly arranged on above each described nickel crystallite.
2. the preparation method of melanism composite layer according to claim 1, it is characterised in that:
Wherein, the extruded metal foil is rolled copper foil.
3. the preparation method of melanism composite layer according to claim 1, it is characterised in that:
Wherein, the complexing agent is citric acid, sodium citrate, the mixture of one of lactic acid or more.
4. the preparation method of melanism composite layer according to claim 1, it is characterised in that:
Wherein, the nickel-plating additive is BN-91, the mixture of one or both of BN-92.
5. the preparation method of melanism composite layer according to claim 1, it is characterised in that:
Wherein, the temperature of the Nickel Plating Treatment is 20-40 DEG C, current density 16-48A/dm2, electroplating time 2-20s.
6. the preparation method of melanism composite layer according to claim 1, it is characterised in that:
Wherein, the zinc-plating additive is the mixing of one or both of o-benzoic sulfimide and Isosorbide-5-Nitrae-butynediols Object.
7. the preparation method of melanism composite layer according to claim 1, it is characterised in that:
Wherein, the temperature of the zinc-plated processing is 20-40 DEG C, electroplating time 2-20s.
CN201711390259.1A 2017-12-21 2017-12-21 A kind of preparation method of the melanism composite layer on extruded metal foil surface Expired - Fee Related CN108060443B (en)

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CN112501659B (en) * 2020-11-11 2022-01-18 中铜华中铜业有限公司 Blackening plating solution of rolled copper foil and cyanide-free electroplated nickel blackening process
CN113463140B (en) * 2021-06-23 2022-08-05 灵宝金源朝辉铜业有限公司 Nickel plating solution and high-corrosion-resistance double-sided thick nickel plating rolled copper foil process

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CN1995473A (en) * 2006-11-28 2007-07-11 招远金宝电子有限公司 Enivironment-friendly type surface treatment process for electrolytic copper foil
CN101906630B (en) * 2010-08-03 2011-08-10 山东金宝电子股份有限公司 Black surface treatment process of electrolytic copper foil
TW201621096A (en) * 2014-12-05 2016-06-16 財團法人金屬工業研究發展中心 Black titanium-containing oxide layer and method for preparing the same, and implant
CN105603480B (en) * 2016-03-02 2019-01-01 山东天和压延铜箔有限公司 The black surface processing method of rolled copper foil
CN106086973A (en) * 2016-06-03 2016-11-09 安徽铜冠铜箔有限公司 A kind of process of surface treatment of black electronic Copper Foil
CN106191980A (en) * 2016-07-27 2016-12-07 中铝上海铜业有限公司 The surface Darkening process method of rolled copper foil
CN106319585A (en) * 2016-10-31 2017-01-11 中色奥博特铜铝业有限公司 Surface treatment method of high-precision blackened rolled copper foil

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