CN102277605A - Process for manufacturing smooth surface roughened electrolytic copper foil - Google Patents
Process for manufacturing smooth surface roughened electrolytic copper foil Download PDFInfo
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- CN102277605A CN102277605A CN2011102301940A CN201110230194A CN102277605A CN 102277605 A CN102277605 A CN 102277605A CN 2011102301940 A CN2011102301940 A CN 2011102301940A CN 201110230194 A CN201110230194 A CN 201110230194A CN 102277605 A CN102277605 A CN 102277605A
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Abstract
The invention relates to a process for manufacturing smooth surface roughened electrolytic copper foil, which comprises a step of pickling, a step of primary smooth surface roughening, a step of secondary smooth surface roughening, a step of primary smooth surface curing, a step of secondary smooth surface curing, a step of double-size anti-oxidization treatment, a step of double side passivation and a step of smooth surface coupling agent treatment, which are accomplished continuously on the same production line. Compared with the prior art, the smooth surface roughened electric copper foil manufactured by the process for manufacturing the smooth surface roughened electrolytic copper foil has the advantages of short copper teeth, easy etching, and high impedance controllability. When the copper foil is used in production of downstream products, the needs of blackening micro corrosion and toughening treatment are obviated, so the manufacturing process is shortened, and the short circuit rate and open circuit rate are lowered; meanwhile, the copper foil manufactured by the process has the same quality as the conventional high-precision or double-side toughened electrolytic copper foil, is produced at low cost and is more suitable for manufacturing the inner layers of high-precision multilayer plates and high-density fine line printed circuit boards (PCBs).
Description
Technical field
The present invention relates to a kind of manufacture method of Copper Foil, relate in particular to a kind of manufacturing process of light face alligatoring electrolytic copper foil.
Background technology
Development along with electronic information technology, multilayer complexity or high-density fine rule PCB plate consumption in high precision miniaturization electronics product is increasing, traditional way is used for high-density fine rule PCB plate or multilayer complex PCB internal layer with high-precision electronic Copper Foil or double-sided coarsening electrolytic copper foil usually, adopt traditional high precision electrolytic copper foil then to need to carry out complicated technology such as microetch melanism behind the pressing plate, procedure for producing is long and cost is high; Adopt the double-sided coarsening electrolytic copper foil then to increase the process complexity of Copper Foil own, improved tooling cost; Secondly, these two kinds of Copper Foils are being used for the defective that multi-ply wood internal layer or high-density fine rule PCB plate all exist copper tooth length, the major hidden danger that this very easily brings short circuit, opens circuit to subsequent product.
Summary of the invention
In view of this, be necessary to provide a kind of manufacturing process that can be used in the light face alligatoring electrolytic copper foil of making high-density fine rule PCB plate and high-performance multilayer complex PCB, the Copper Foil of manufacturing of the present invention and conventional Copper Foil can shorten the making process that height becomes more meticulous and requires pcb board, the copper tooth is short, be easy to etching, impedance Control is strong, need not to carry out melanism microetch, roughening treatment, promptly can be used for multi-ply wood lamination and high-density fine rule PCB plate and makes.
The present invention realizes like this, a kind of manufacturing process of light face alligatoring electrolytic copper foil, it is included in, and pickling process, light face alligatoring first operation, light face alligatoring second operation, the light face finished continuously on the production line solidify first operation, the light face solidifies second operation, two-sided anti-oxidation operation, passivation on double surfaces operation, light face coupling agent operation, wherein
The working conditions of described pickling process is a temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L;
The working conditions of described light face alligatoring first operation is current density: 25～40A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L;
The working conditions of described light face alligatoring second operation is current density: 20～30A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L, tungsten ion 0.001～0.005g/L, sodium lauryl sulphate: 0.01～0.03g/L;
The working conditions that described light face solidifies first operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L;
The working conditions that described light face solidifies second operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L;
The working conditions of described two-sided anti-oxidation operation is current density: 5～10A/dm
2, temperature: 40～50 ℃, potassium pyrophosphate: 70～155g/L, zine ion: 4～10g/L, nickel ion: 0.5～1.0g/L, acidity-basicity ph value: 10～12;
The working conditions of described passivation on double surfaces operation is current density: 5～10A/dm
2, temperature: 30～40 ℃, hexavalent chromium: 0.5～2.0g/L, acidity-basicity ph value: 11～13;
The working conditions of described light face coupling agent operation is a temperature: 20～30 ℃, organic membrane coupling agent: 0.5～1.0g/L.
Further, the surface treatment mode of described light face alligatoring electronics Copper Foil adopts the alligatoring of light face, two-sided anti-oxidation, passivation technology.
The present invention compared with prior art, beneficial effect is: the manufacturing process of light face alligatoring electrolytic copper foil provided by the invention, the light face alligatoring electronics Copper Foil of its manufacturing is compared with existing relative technological products has copper tooth weak point, be easy to etching, the advantage that impedance Control is strong, and be used for derived product production, need not to carry out the melanism microetch, roughening treatment, shortened the making process, reduce short circuit and burn out rate, have the quality of conventional high precision or double-sided coarsening electrolytic copper foil simultaneously, production cost is low, is more suitable for being used for the making of high meticulous multiple-plate internal layer and high-density fine rule pcb board.
Description of drawings
The enforcement synoptic diagram of the manufacturing process of the light face alligatoring electrolytic copper foil that Fig. 1 provides for first embodiment of the invention.
Fig. 2 is the hair side Electronic Speculum figure (1500 magnification) of the Copper Foil made of the manufacturing process of light face alligatoring electrolytic copper foil among Fig. 1.
Fig. 3 is the light face Electronic Speculum figure (2000 magnification) of the Copper Foil made of the manufacturing process of light face alligatoring electrolytic copper foil among Fig. 1.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with drawings and Examples.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
First embodiment
See also Fig. 1, the manufacturing process of the light face alligatoring electrolytic copper foil that first embodiment of the invention provides (being the manufacture method of light face alligatoring electronics Copper Foil) is to change normal copper foil surface processing mode and technology and obtain, it actively carries out roughening treatment to Copper Foil light face, production method will be for will give birth to paper tinsel (not surface-treated electro-deposited copper foil) through surface processing equipment, through pickling process, light face alligatoring first operation, light face alligatoring second operation, the light face solidifies first operation, the light face solidifies second operation, two-sided anti-oxidation operation, the passivation on double surfaces operation, the light face is coated with the coupling agent operation, totally eight operations are finished dealing with continuously, and these operations all concentrate on a surface processing equipment.The manufacture method of light face alligatoring electronics Copper Foil utilizes the living paper tinsel of conventional high precision electrolytic copper foil to be negative electrode, titanium plate in each operation electrolyzer of surface processing equipment is an anode, according to process sequence at the required material of Copper Foil respective surfaces electroplating deposition one deck, its electroplating time is pressed Copper Foil running speed about 2～5 seconds, and it makes parameters such as product roughness, peel strength all by the standard detection of IPC-TM-650.
The following introduction of manufacture method of light face alligatoring electronics Copper Foil.
1, pickling process: the working conditions of described pickling process is a temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L.In this city embodiment, be the living paper tinsel of 18 μ m of 1.82 μ m with light surface roughness Rz, the electrolytic solution with 90～160g/L sulfuric acid, 20～40g/L cupric ion under 35 ℃ of conditions of temperature cleans.The Acidwash solution preparation is consistent with light face alligatoring first operation (as described below) electrolytic solution, direct electrolytic solution from light face alligatoring first operation.
2, light face alligatoring first operation: the working conditions of described light face alligatoring first operation is current density: 25～40A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L.In the present embodiment, with the Copper Foil of pickling at current density 30A/dm
2, 45 ℃ of temperature, sulfuric acid 160g/L, cupric ion 20g/L condition under electroplate.Copper-bath is beaten the electrolytic bath of incidence surface alligatoring first operation by pump, be mixed with the light face alligatoring first operation electrolytic solution, introduce the electrolyzer of alligatoring first operation again by pump according to processing requirement.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
3, light face alligatoring second operation: the working conditions of described light face alligatoring second operation is current density: 20～30A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L, tungsten ion 0.001～0.005g/L, sodium lauryl sulphate: 0.01～0.03g/L.In the present embodiment, the Copper Foil that light face alligatoring first operation is crossed is at current density 25A/dm
2, 40 ℃ of temperature, sulfuric acid 150g/L, cupric ion 20g/L, tungsten ion 0.002g/L, sodium lauryl sulphate 0.01g/L condition under electroplate.Copper-bath is beaten the electrolytic bath of incidence surface alligatoring second operation by pump, mix in right amount according to processing requirement adding sodium lauryl sulphate and sodium wolframate, be mixed with the light face alligatoring second operation electrolytic solution, introduce the electrolyzer of alligatoring second operation again by pump.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
4, the light face solidifies first operation: the working conditions that described light face solidifies first operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L.In the present embodiment, the Copper Foil that light face alligatoring second operation is crossed is at current density 35A/dm
2, 40 ℃ of temperature, sulfuric acid 100g/L, cupric ion 65g/L condition under electroplate.Copper-bath is squeezed into the electrolytic bath that solidifies first operation by pump, be mixed with according to processing requirement and solidify the first operation electrolytic solution, introduce the electrolyzer that solidifies first operation by pump again.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
5, the light face solidifies second operation: the working conditions that described light face solidifies second operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L.In the present embodiment, the light face is solidified Copper Foil that first operation crosses at current density 35A/dm
2, 45 ℃ of temperature, sulfuric acid 100g/L, cupric ion 65g/L condition under electroplate.The electrolytic solution of this operation comes the electrolytic bath of self cure first operation.
6, two-sided anti-oxidation operation: the working conditions of described two-sided anti-oxidation operation is current density: 5～10A/dm
2, temperature: 40～50 ℃, potassium pyrophosphate: 70～155g/L, zine ion: 4～10g/L, nickel ion: 0.5～1.0g/L, acidity-basicity ph value: 10～12.In the present embodiment, the light face is solidified again Copper Foil that second operation crosses at current density 7A/dm
2, 43 ℃ of temperature, potassium pyrophosphate 135g/L, zine ion 5g/L, nickel ion 1.0g/L, acidity-basicity ph value 11 condition under electroplate.Potassium pyrophosphate, zinc sulfate, single nickel salt are dissolved in liquid pool respectively, by pump zinc sulfate, nickel sulfate solution are slowly joined in the potassium pyrophosphate solution tank, be made into the electrolytic solution of above-mentioned ionic concn scope, utilize sodium hydroxide solution to regulate and stablize acidity-basicity ph value, utilize pump to introduce anti-oxidation operation electrolyzer then to the operation scope.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
7, passivation on double surfaces operation: the working conditions of described passivation on double surfaces operation is current density: 5～10A/dm
2, temperature: 30～40 ℃, hexavalent chromium: 0.5～2.0g/L, acidity-basicity ph value: 11～13.In the present embodiment, with the Copper Foil of two-sided anti-oxidation mistake at current density 8A/dm
2, 31 ℃ of temperature, hexavalent chromium 1.5g/L, acidity-basicity ph value 12 condition under electroplate.Chromic trioxide is dissolved in liquid pool, is made into the required chromium ion concentration electrolytic solution of operation, utilize sodium hydroxide solution to regulate and stablize acidity-basicity ph value, utilize pump to introduce the passivation procedure electrolyzer then to the operation scope.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
8, light face coupling agent operation: the working conditions of described light face coupling agent operation is a temperature: 20～30 ℃, organic membrane coupling agent: 0.5～1.0g/L.In the present embodiment, the Copper Foil that passivation on double surfaces is crossed carries out the light face and is coated with the organic membrane coupling agent under the condition of 25 ℃ of temperature, organic membrane coupling agent 1.0g/L.Get silane coupling agent 15～30g and be dissolved in and be equipped with in 25 ℃, the bucket of 30L pure water, pour into after stirring to be coated with and carry out online roller coating in the organic membrane groove, behind its underconsumption in this way preparation add.
After finishing, above-mentioned serial operation dries rolling.Bake out temperature: 200 ℃.Wherein 1. be expressed as the negative electrode conductive rollers among Fig. 1; 2. be expressed as the Copper Foil guide roller, electronics copper foil surface treatment facility no longer is described in detail at this.
See also Fig. 2 and Fig. 3, the hair side of the Copper Foil that its manufacturing process that is respectively light face alligatoring electrolytic copper foil is made and the Electronic Speculum figure of light face, wherein the hair side Electronic Speculum figure of Copper Foil is 1500 magnifications; The light face Electronic Speculum figure of Copper Foil is 2000 magnifications, and the Copper Foil of the manufacture method manufacturing of this light face alligatoring electronics Copper Foil meets processing requirement.
The manufacture method of the light face alligatoring electronics Copper Foil that first embodiment of the invention provides, the light face alligatoring electronics Copper Foil of its manufacturing is compared with existing relative technological products has copper tooth weak point, be easy to etching, the advantage that impedance Control is strong, and be used for derived product production, need not to carry out melanism microetch, roughening treatment, shortened the making process, reduce short circuit and burn out rate, the quality that has conventional high precision or double-sided coarsening electrolytic copper foil simultaneously, production cost is low, is more suitable for being used for the making of high meticulous multiple-plate internal layer and high-density fine rule pcb board.
Second embodiment
Making method with reference to embodiment one is prepared the Copper Foil product, the manufacture method of the light face alligatoring electronics Copper Foil that second embodiment of the invention provides is to change normal copper foil surface processing mode and technology and obtain, it actively carries out roughening treatment to Copper Foil light face, production method will be for will give birth to paper tinsel (not surface-treated electro-deposited copper foil) through surface processing equipment, through pickling process, light face alligatoring first operation, light face alligatoring second operation, the light face solidifies first operation, the light face solidifies second operation, two-sided anti-oxidation operation, the passivation on double surfaces operation, the light face is coated with the coupling agent operation, totally eight operations are finished dealing with continuously, and these operations all concentrate on a surface processing equipment.The manufacture method of light face alligatoring electronics Copper Foil utilizes the living paper tinsel of conventional high precision electrolytic copper foil to be negative electrode, titanium plate in each operation electrolyzer of surface processing equipment is an anode, according to process sequence at the required material of Copper Foil respective surfaces electroplating deposition one deck, its electroplating time is pressed Copper Foil running speed about 2～5 seconds, and it makes parameters such as product roughness, peel strength all by the standard detection of IPC-TM-650.
The following introduction of manufacture method of light face alligatoring electronics Copper Foil.
1, pickling process: the working conditions of described pickling process is a temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L.In the present embodiment, be the living paper tinsel of 18 μ m of 1.82 μ m with light surface roughness Rz, the electrolytic solution with 90～160g/L sulfuric acid, 20～40g/L cupric ion under 35 ℃ of conditions of temperature cleans.The Acidwash solution preparation is consistent with light face alligatoring first operation (as described below) electrolytic solution, direct electrolytic solution from light face alligatoring first operation.
2, light face alligatoring first operation: the working conditions of described light face alligatoring first operation is current density: 25～40A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L.In the present embodiment, with the Copper Foil of pickling at current density 35A/dm
2, 46 ℃ of temperature, sulfuric acid 170g/L, cupric ion 25g/L condition under electroplate.Copper-bath is beaten the electrolytic bath of incidence surface alligatoring first operation by pump, be mixed with the light face alligatoring first operation electrolytic solution, introduce the electrolyzer of alligatoring first operation again by pump according to processing requirement.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
3, light face alligatoring second operation: the working conditions of described light face alligatoring second operation is current density: 20～30A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L, tungsten ion 0.001～0.005g/L, sodium lauryl sulphate: 0.01～0.03g/L.In the present embodiment, the Copper Foil that light face alligatoring first operation is crossed is at current density 30A/dm
2, 45 ℃ of temperature, sulfuric acid 155g/L, cupric ion 25g/L, tungsten ion 0.003g/L, sodium lauryl sulphate: 0.02g/L condition under electroplate.Copper-bath is beaten the electrolytic bath of incidence surface alligatoring second operation by pump, mix in right amount according to processing requirement adding sodium lauryl sulphate and sodium wolframate, be mixed with the light face alligatoring second operation electrolytic solution, introduce the electrolyzer of alligatoring second operation again by pump.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
4, the light face solidifies first operation: the working conditions that described light face solidifies first operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L.In the present embodiment, the Copper Foil that light face alligatoring 2 is crossed is at current density 30A/dm
2, 35 ℃ of temperature, sulfuric acid 110g/L, cupric ion 70g/L condition under electroplate.Copper-bath is squeezed into the electrolytic bath that solidifies first operation by pump, be mixed with according to processing requirement and solidify the first operation electrolytic solution, introduce the electrolyzer that solidifies first operation by pump again.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
5, the light face solidifies second operation: the working conditions that described light face solidifies second operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L.In the present embodiment, the light face is solidified Copper Foil that first operation crosses at current density 30A/dm
2, 35 ℃ of temperature, sulfuric acid 110g/L, cupric ion 70g/L condition under electroplate.The electrolytic solution of this operation comes the electrolytic bath of self cure first operation.
6, two-sided anti-oxidation operation: the working conditions of described two-sided anti-oxidation operation is current density: 5～10A/dm
2, temperature: 40～50 ℃, potassium pyrophosphate: 70～155g/L, zine ion: 4～10g/L, nickel ion: 0.5～1.0g/L, acidity-basicity ph value: 10～12.In the present embodiment, the light face is solidified again Copper Foil that second operation crosses at current density 10A/dm
2, 40 ℃ of temperature, potassium pyrophosphate 130g/L, zine ion 3g/L, nickel ion 0.8g/L, acidity-basicity ph value 10.5 condition under electroplate.Potassium pyrophosphate, zinc sulfate, single nickel salt are dissolved in liquid pool respectively, by pump zinc sulfate, nickel sulfate solution are slowly joined in the potassium pyrophosphate solution tank, be made into the electrolytic solution of above-mentioned ionic concn scope, utilize sodium hydroxide solution to regulate and stablize acidity-basicity ph value, utilize pump to introduce anti-oxidation operation electrolyzer then to the operation scope.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
7, passivation on double surfaces operation: the working conditions of described passivation on double surfaces operation is current density: 5～10A/dm
2, temperature: 30～40 ℃, hexavalent chromium: 0.5～2.0g/L, acidity-basicity ph value: 11～13.In the present embodiment, with the Copper Foil of two-sided anti-oxidation mistake at current density 9A/dm
2, 30 ℃ of temperature, hexavalent chromium 1.3g/L, acidity-basicity ph value 12 condition under electroplate.Chromic trioxide is dissolved in liquid pool, is made into the required chromium ion concentration electrolytic solution of operation, utilize sodium hydroxide solution to regulate and stablize acidity-basicity ph value, utilize pump to introduce the passivation procedure electrolyzer then to the operation scope.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
8, light face coupling agent operation: the working conditions of described light face coupling agent operation is a temperature: 20～30 ℃, organic membrane coupling agent: 0.5～1.0g/L.In the present embodiment, the Copper Foil that passivation on double surfaces is crossed carries out the light face and is coated with the organic membrane coupling agent under the condition of 25 ℃ of temperature, organic membrane coupling agent 1.0g/L.Get silane coupling agent 15～30g and be dissolved in and be equipped with in 25 ℃, the bucket of 30L pure water, pour into after stirring to be coated with and carry out online roller coating in the organic membrane groove, behind its underconsumption in this way preparation add.
After finishing, above-mentioned serial operation dries rolling.Bake out temperature: 200 ℃.
The manufacture method of the light face alligatoring electronics Copper Foil that second embodiment of the invention provides, the light face alligatoring electronics Copper Foil of its manufacturing is compared with existing relative technological products has copper tooth weak point, be easy to etching, the advantage that impedance Control is strong, and be used for derived product production, need not to carry out melanism microetch, roughening treatment, shortened the making process, reduce short circuit and burn out rate, the quality that has conventional high precision or double-sided coarsening electrolytic copper foil simultaneously, production cost is low, is more suitable for being used for the making of high meticulous multiple-plate internal layer and high-density fine rule pcb board.
The 3rd embodiment
Making method with reference to embodiment one is prepared the Copper Foil product, the manufacture method of the light face alligatoring electronics Copper Foil that third embodiment of the invention provides is to change normal copper foil surface processing mode and technology and obtain, it actively carries out roughening treatment to Copper Foil light face, production method will be for will give birth to paper tinsel (not surface-treated electro-deposited copper foil) through surface processing equipment, through pickling process, light face alligatoring first operation, light face alligatoring second operation, the light face solidifies first operation, the light face solidifies second operation, two-sided anti-oxidation operation, the passivation on double surfaces operation, the light face is coated with the coupling agent operation, totally eight operations are finished dealing with continuously, and these operations all concentrate on a surface processing equipment.The manufacture method of light face alligatoring electronics Copper Foil utilizes the living paper tinsel of conventional high precision electrolytic copper foil to be negative electrode, titanium plate in each operation electrolyzer of surface processing equipment is an anode, according to process sequence at the required material of Copper Foil respective surfaces electroplating deposition one deck, its electroplating time is pressed Copper Foil running speed about 2～5 seconds, and it makes parameters such as product roughness, peel strength all by the standard detection of IPC-TM-650.
The following introduction of manufacture method of light face alligatoring electronics Copper Foil.
1, pickling process: the working conditions of described pickling process is a temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L.In the present embodiment, be the living paper tinsel of 18 μ m of 1.82 μ m with light surface roughness Rz, the electrolytic solution with 90～160g/L sulfuric acid, 20～40g/L cupric ion under 35 ℃ of conditions of temperature cleans.The Acidwash solution preparation is consistent with light face alligatoring first operation (as described below) electrolytic solution, direct electrolytic solution from light face alligatoring first operation.
2, light face alligatoring first operation: the working conditions of described light face alligatoring first operation is current density: 25～40A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L.In the present embodiment, with the Copper Foil of pickling at current density 30A/dm
2, 40 ℃ of temperature, sulfuric acid 180g/L, cupric ion 30g/L condition under electroplate.Copper-bath is beaten the electrolytic bath of incidence surface alligatoring first operation by pump, be mixed with the light face alligatoring first operation electrolytic solution, introduce the electrolyzer of alligatoring first operation again by pump according to processing requirement.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
3, light face alligatoring second operation: the working conditions of described light face alligatoring second operation is current density: 20～30A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L, tungsten ion 0.001～0.005g/L, sodium lauryl sulphate: 0.01～0.03g/L.In the present embodiment, the Copper Foil that light face alligatoring first operation is crossed is at current density 25A/dm
2, 40 ℃ of temperature, sulfuric acid 145g/L, cupric ion 20g/L, tungsten ion 0.003g/L, sodium lauryl sulphate: 0.03g/L condition under electroplate.Copper-bath is beaten the electrolytic bath of incidence surface alligatoring second operation by pump, mix in right amount according to processing requirement adding sodium lauryl sulphate and sodium wolframate, be mixed with the light face alligatoring second operation electrolytic solution, introduce the electrolyzer of alligatoring second operation again by pump.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
4, the light face solidifies first operation: the working conditions that described light face solidifies first operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L.In the present embodiment, the Copper Foil that light face alligatoring second operation is crossed is at current density 35A/dm
2, 30 ℃ of temperature, sulfuric acid 120g/L, cupric ion 75g/L condition under electroplate.Copper-bath is squeezed into the electrolytic bath that solidifies first operation by pump, be mixed with according to processing requirement and solidify the first operation electrolytic solution, introduce the electrolyzer that solidifies first operation by pump again.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
5, the light face solidifies second operation: the working conditions that described light face solidifies second operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L.In the present embodiment, the light face is solidified Copper Foil that first operation crosses at current density 35A/dm
2, 30 ℃ of temperature, sulfuric acid 120g/L, cupric ion 75g/L condition under electroplate.The electrolytic solution of this operation comes the electrolytic bath of self cure first operation.
6, two-sided anti-oxidation operation: the working conditions of described two-sided anti-oxidation operation is current density: 5～10A/dm
2, temperature: 40～50 ℃, potassium pyrophosphate: 70～155g/L, zine ion: 4～10g/L, nickel ion: 0.5～1.0g/L, acidity-basicity ph value: 10～12.In the present embodiment, the light face is solidified again Copper Foil that second operation crosses at current density 10A/dm
2, 40 ℃ of temperature, potassium pyrophosphate 130g/L, zine ion 5g/L, nickel ion 1.1g/L, acidity-basicity ph value 11.0 condition under electroplate.Potassium pyrophosphate, zinc sulfate, single nickel salt are dissolved in liquid pool respectively, by pump zinc sulfate, nickel sulfate solution are slowly joined in the potassium pyrophosphate solution tank, be made into the electrolytic solution of above-mentioned ionic concn scope, utilize sodium hydroxide solution to regulate and stablize acidity-basicity ph value, utilize pump to introduce anti-oxidation operation electrolyzer then to the operation scope.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
7, passivation on double surfaces operation: the working conditions of described passivation on double surfaces operation is current density: 5～10A/dm
2, temperature: 30～40 ℃, hexavalent chromium: 0.5～2.0g/L, acidity-basicity ph value: 11～13.In the present embodiment, with the Copper Foil of two-sided anti-oxidation mistake at current density 10A/dm
2, 31 ℃ of temperature, hexavalent chromium 1.4g/L, acidity-basicity ph value 12 condition under electroplate.Chromic trioxide is dissolved in liquid pool, is made into the required chromium ion concentration electrolytic solution of operation, utilize sodium hydroxide solution to regulate and stablize acidity-basicity ph value, utilize pump to introduce the passivation procedure electrolyzer then to the operation scope.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
8, light face coupling agent operation: the working conditions of described light face coupling agent operation is a temperature: 20～30 ℃, organic membrane coupling agent: 0.5～1.0g/L.In the present embodiment, the Copper Foil that passivation on double surfaces is crossed carries out the light face and is coated with the organic membrane coupling agent under the condition of 25 ℃ of temperature, organic membrane coupling agent 1.0g/L.Get silane coupling agent 15～30g and be dissolved in and be equipped with in 25 ℃, the bucket of 30L pure water, pour into after stirring to be coated with and carry out online roller coating in the organic membrane groove, behind its underconsumption in this way preparation add.
After finishing, above-mentioned serial operation dries rolling.Bake out temperature: 200 ℃.
The manufacture method of the light face alligatoring electronics Copper Foil that third embodiment of the invention provides, the light face alligatoring electronics Copper Foil of its manufacturing is compared with existing relative technological products has copper tooth weak point, be easy to etching, the advantage that impedance Control is strong, and be used for derived product production, need not to carry out melanism microetch, roughening treatment, shortened the making process, reduce short circuit and burn out rate, the quality that has conventional high precision or double-sided coarsening electrolytic copper foil simultaneously, production cost is low, is more suitable for being used for the making of high meticulous multiple-plate internal layer and high-density fine rule pcb board.
The 4th embodiment
Making method with reference to embodiment one is prepared the Copper Foil product, the manufacture method of the light face alligatoring electronics Copper Foil that four embodiment of the invention provides is to change normal copper foil surface processing mode and technology and obtain, it actively carries out roughening treatment to Copper Foil light face, production method will be for will give birth to paper tinsel (not surface-treated electro-deposited copper foil) through surface processing equipment, through pickling process, light face alligatoring first operation, light face alligatoring second operation, the light face solidifies first operation, the light face solidifies second operation, two-sided anti-oxidation operation, the passivation on double surfaces operation, the light face is coated with the coupling agent operation, totally eight operations are finished dealing with continuously, and these operations all concentrate on a surface processing equipment.The manufacture method of light face alligatoring electronics Copper Foil utilizes the living paper tinsel of conventional high precision electrolytic copper foil to be negative electrode, titanium plate in each operation electrolyzer of surface processing equipment is an anode, according to process sequence at the required material of Copper Foil respective surfaces electroplating deposition one deck, its electroplating time is pressed Copper Foil running speed about 2～5 seconds, and it makes parameters such as product roughness, peel strength all by the standard detection of IPC-TM-650.
The following introduction of manufacture method of light face alligatoring electronics Copper Foil.
1, pickling process: the working conditions of described pickling process is a temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L.In the present embodiment, be the living paper tinsel of 18 μ m of 1.82 μ m with light surface roughness Rz, the electrolytic solution with 90～160g/L sulfuric acid, 20～40g/L cupric ion under 35 ℃ of conditions of temperature cleans.The Acidwash solution preparation is consistent with light face alligatoring first operation (as described below) electrolytic solution, direct electrolytic solution from light face alligatoring first operation.
2, light face alligatoring first operation: the working conditions of described light face alligatoring first operation is current density: 25～40A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L, in the present embodiment, with the Copper Foil of pickling at current density 30A/dm
2, 45 ℃ of temperature, sulfuric acid 180g/L, cupric ion 35g/L condition under electroplate.Copper-bath is beaten the electrolytic bath of incidence surface alligatoring first operation by pump, be mixed with the light face alligatoring first operation electrolytic solution, introduce the electrolyzer of alligatoring first operation again by pump according to processing requirement.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
3, light face alligatoring second operation: the working conditions of described light face alligatoring second operation is current density: 20～30A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L, tungsten ion 0.001～0.005g/L, sodium lauryl sulphate: 0.01～0.03g/L.In the present embodiment, the Copper Foil that light face alligatoring first operation is crossed is at current density 30A/dm
2, 40 ℃ of temperature, sulfuric acid 150g/L, cupric ion 25g/L, tungsten ion 0.005g/L, sodium lauryl sulphate: 0.02g/L condition under electroplate.Copper-bath is beaten the electrolytic bath of incidence surface alligatoring second operation by pump, mix in right amount according to processing requirement adding sodium lauryl sulphate and sodium wolframate, be mixed with the light face alligatoring second operation electrolytic solution, introduce the electrolyzer of alligatoring second operation again by pump.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
4, the light face solidifies first operation: the working conditions that described light face solidifies first operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L.In the present embodiment, the Copper Foil that light face alligatoring second operation is crossed is at current density 30A/dm
2, 35 ℃ of temperature, sulfuric acid 120g/L, cupric ion 70g/L condition under electroplate.Copper-bath is squeezed into the electrolytic bath that solidifies first operation by pump, be mixed with according to processing requirement and solidify the first operation electrolytic solution, introduce the electrolyzer that solidifies first operation by pump again.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
5, the light face solidifies second operation: the working conditions that described light face solidifies second operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L.In the present embodiment, the light face is solidified Copper Foil that first operation crosses at current density 30A/dm
2, 35 ℃ of temperature, sulfuric acid 120g/L, cupric ion 70g/L condition under electroplate.The electrolytic solution of this operation comes the electrolytic bath of self cure first operation.
6, two-sided anti-oxidation operation: the working conditions of described two-sided anti-oxidation operation is current density: 5～10A/dm
2, temperature: 40～50 ℃, potassium pyrophosphate: 70～155g/L, zine ion: 4～10g/L, nickel ion: 0.5～1.0g/L, acidity-basicity ph value: 10～12.In the present embodiment, light face roughened layer is solidified again Copper Foil that second operation crosses at current density 9A/dm
2, 40 ℃ of temperature, potassium pyrophosphate 130g/L, zine ion 5g/L, nickel ion 1.0g/L, acidity-basicity ph value 11.0 condition under electroplate.Potassium pyrophosphate, zinc sulfate, single nickel salt are dissolved in liquid pool respectively, by pump zinc sulfate, nickel sulfate solution are slowly joined in the potassium pyrophosphate solution tank, be made into the electrolytic solution of above-mentioned ionic concn scope, utilize sodium hydroxide solution to regulate and stablize acidity-basicity ph value, utilize pump to introduce anti-oxidation operation electrolyzer then to the operation scope.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
7, passivation on double surfaces operation: the working conditions of described passivation on double surfaces operation is current density: 5～10A/dm
2, temperature: 30～40 ℃, hexavalent chromium: 0.5～2.0g/L, acidity-basicity ph value: 11～13.In the present embodiment, with the Copper Foil of two-sided anti-oxidation mistake at current density 9A/dm
2, 30 ℃ of temperature, hexavalent chromium 1.5g/L, acidity-basicity ph value 12 condition under electroplate.Chromic trioxide is dissolved in liquid pool, is made into the required chromium ion concentration electrolytic solution of operation, utilize sodium hydroxide solution to regulate and stablize acidity-basicity ph value, utilize pump to introduce the passivation procedure electrolyzer then to the operation scope.The sampling in per 1 hour of bath composition concentration detects once, and carries out concentration according to detected result and adjust to processing range.
8, light face coupling agent operation: the working conditions of described light face coupling agent operation is a temperature: 20～30 ℃, organic membrane coupling agent: 0.5～1.0g/L.In the present embodiment, the Copper Foil that passivation on double surfaces is crossed carries out the light face and is coated with the organic membrane coupling agent under the condition of 25 ℃ of temperature, organic membrane coupling agent 1.0g/L.Get silane coupling agent 15～30g and be dissolved in and be equipped with in 25 ℃, the bucket of 30L pure water, pour into after stirring to be coated with and carry out online roller coating in the organic membrane groove, behind its underconsumption in this way preparation add.
After finishing, above-mentioned serial operation dries rolling.Bake out temperature: 200 ℃.
The manufacture method of the light face alligatoring electronics Copper Foil that four embodiment of the invention provides, the light face alligatoring electronics Copper Foil of its manufacturing is compared with existing relative technological products has copper tooth weak point, be easy to etching, the advantage that impedance Control is strong, and be used for derived product production, need not to carry out melanism microetch, roughening treatment, shortened the making process, reduce short circuit and burn out rate, the quality that has conventional high precision or double-sided coarsening electrolytic copper foil simultaneously, production cost is low, is more suitable for being used for the making of high meticulous multiple-plate internal layer and high-density fine rule pcb board.
The light face alligatoring electrolytic copper foil that example 1～4 is made is 18 μ m specifications, and its key parameter index is: light surface roughness Rz is that 3～4 μ m, light face peel strength are greater than 1.2kgf/cm.Concrete leading indicator is as shown in table 1 below:
Table 1
Be appreciated that in other true mode when light face alligatoring electrolytic copper foil was 35 μ m specifications, its key parameter index was: light surface roughness R is that 4～5 μ m, light face peel strength are greater than 1.3kgf/cm.
The Copper Foil that example 1～4 is made is being heated under 200 ℃ of conditions the equal nondiscoloration of 60min.
The above only is preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of being done within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. the manufacturing process of a light face alligatoring electrolytic copper foil, it is included in, and pickling process, light face alligatoring first operation, light face alligatoring second operation, the light face finished continuously on the production line solidify first operation, the light face solidifies second operation, two-sided anti-oxidation operation, passivation on double surfaces operation, light face coupling agent operation, it is characterized in that
The working conditions of described pickling process is a temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L;
The working conditions of described light face alligatoring first operation is current density: 25～40A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L;
The working conditions of described light face alligatoring second operation is current density: 20～30A/dm
2, temperature: 30～60 ℃, sulfuric acid: 90～160g/L, cupric ion: 20～40g/L, tungsten ion 0.001～0.005g/L, sodium lauryl sulphate: 0.01～0.03g/L;
The working conditions that described light face solidifies first operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L;
The working conditions that described light face solidifies second operation is current density: 20～40A/dm
2, temperature: 40～60 ℃, sulfuric acid: 70～150g/L, cupric ion: 40～75g/L;
The working conditions of described two-sided anti-oxidation operation is current density: 5～10A/dm
2, temperature: 40～50 ℃, potassium pyrophosphate: 70～155g/L, zine ion: 4～10g/L, nickel ion: 0.5～1.0g/L, acidity-basicity ph value: 10～12;
The working conditions of described passivation on double surfaces operation is current density: 5～10A/dm
2, temperature: 30～40 ℃, hexavalent chromium: 0.5～2.0g/L, acidity-basicity ph value: 11～13;
The working conditions of described light face coupling agent operation is a temperature: 20～30 ℃, organic membrane coupling agent: 0.5～1.0g/L.
2. the manufacturing process of light face alligatoring electrolytic copper foil according to claim 1 is characterized in that, the surface treatment mode of described light face alligatoring electronics Copper Foil adopts the alligatoring of light face, two-sided anti-oxidation, passivation technology.
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| CN114481245B (en) * | 2022-02-24 | 2022-09-16 | 广东盈华电子科技有限公司 | Surface treatment process of reverse electrolytic copper foil for flexible copper clad laminate |
| CN114990654A (en) * | 2022-06-02 | 2022-09-02 | 山东金宝电子股份有限公司 | Electrolytic copper foil surface treatment process, HVLP copper foil product and application thereof |
| CN114990654B (en) * | 2022-06-02 | 2024-04-26 | 山东金宝电子有限公司 | Electrolytic copper foil surface treatment process, HVLP copper foil product and application thereof |
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| CN102277605B (en) | 2013-11-13 |
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Address after: 230001 Anhui city of Hefei Province Economic and Technological Development Zone No. 11 Zi Peng Lu Patentee after: Hefei Tongguan electronic copper foil Co., Ltd Address before: 230001 Anhui city of Hefei Province Economic and Technological Development Zone No. 11 Zi Peng Lu Patentee before: HEFEI TONGGUAN GUOXUAN COPPER PRODUCTS Co.,Ltd. |