CN108118372A - A kind of high dispersive acidic copper plating additive and preparation method and application - Google Patents
A kind of high dispersive acidic copper plating additive and preparation method and application Download PDFInfo
- Publication number
- CN108118372A CN108118372A CN201711406395.5A CN201711406395A CN108118372A CN 108118372 A CN108118372 A CN 108118372A CN 201711406395 A CN201711406395 A CN 201711406395A CN 108118372 A CN108118372 A CN 108118372A
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- Prior art keywords
- copper plating
- high dispersive
- acidic copper
- plating additive
- sulfuric acid
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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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/423—Plated through-holes or plated via connections characterised by electroplating method
- H05K3/424—Plated through-holes or plated via connections characterised by electroplating method by direct electroplating
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The present invention relates to printed wiring board polymolecularity entire bright acid copper-plating fields, refer in particular to a kind of high dispersive acidic copper plating additive and preparation method and application.A kind of high dispersive acidic copper plating additive：At least one divalent main brightener, at least one polyethylene glycol or polypropylene glycol or both block copolymer macromolecule inhibitor, at least one quaternary ammonium alkyl salt form cationic surfactant, the sulfuric acid of 550ml/L, the formaldehyde of 0.14ml/L.Its preparation method is that the concentrated sulfuric acid of specified amount is slowly added in water, after stirring evenly and being cooled to room temperature, the inhibitor, surfactant, main brightener and formaldehyde are added in aqueous sulfuric acid successively, stirring is settled to final volume to after being completely dissolved to get high dispersive acidic copper plating additive of the present invention.The electroplates in hole of the high dispersive acidic copper plating additive of the present invention especially suitable for the high thickness to diameter ratio of printed wiring board can significantly improve the dispersibility of plating solution.
Description
Technical field
The present invention relates to chemical plating fluid field, espespecially a kind of high dispersive acidic copper plating additive and preparation method thereof is with answering
With.
Background technology
Printed circuit manufacturing develops by decades, and manufacturing process is increasingly complicated, the print of high lamination and high thickness to diameter ratio
Circuit board processed increases gradually, also higher and higher to the electrical interconnection technological requirement of layer and interlayer.The acid plating of general business application
Copper additives can meet low radius-thickness ratio (≤6:1) the thick requirement of copper in the hole of the electroplates in hole, when printed circuit board radius-thickness ratio is 8:1
More than when, the electroplating baths physics such as most of acidic copper plating additives need to take reduction current density, and increasing inflates, vibrate aid in
The measures such as machine utilization make up additive in terms of dispersibility the defects of.However, above-mentioned measure will be increased inevitably
Electroplating assembly line energy consumption or the production capacity for reducing plating line increase manufacture cost.Therefore, it is past in order to better adapt to printed circuit board
The superior acidic copper plating additive intermediate of dispersibility and corresponding compounding, user are found in the development in high density direction
Method is of great significance.
The content of the invention
It is plated to solve the above problems, the present invention provides a kind of printed circuit board the electroplates in hole with polymolecularity entire bright is acid
Copper additives and corresponding preparation and application method.The polymolecularity acidic copper plating additive of the present invention has deep plating energy well
Power and covering power are remarkably improved the thick ratios with surface copper thickness of Kong Zhongtong of high thickness to diameter ratio printed circuit board.
To achieve the above object, the present invention, which adopts the following technical scheme that, is：A kind of high dispersive acidic copper plating additive, bag
Component containing following concentration：
Divalent main brightener 0.1-10g/L
Inhibitor 1-100g/L
Quaternary ammonium alkyl salt form cationic surfactant 0.1-5g/L
Sulfuric acid 5-50ml/L
Formaldehyde 0.1-4ml/L
Surplus is deionized water；
Wherein, the divalent main brightener is sodium polydithio-dipropyl sulfonate, phenyl polydithio-dipropyl sulphur
One or more mixtures in sour sodium, thiazolinyl sodium polydithio-dipropyl sulfonate, 2-mercaptobenzimidazole；The inhibition
Agent includes at least one polyethylene glycol or polypropylene glycol or both block copolymer macromolecule；The quaternary ammonium alkyl salt form sun from
Sub- surfactant is methyl triethyl ammonium chloride, benzyltriethylammoinium chloride, dodecyl trimethyl ammonium chloride, cetyl
One or more mixtures in trimethyl ammonium chloride.
Specifically, the inhibitor is Macrogol 4000 or Macrogol 6000 or PEG 8000 or poly- second two
One or more mixtures in alcohol 10000 or poly- (ethylene glycol and 1,2-propylene glycol) monomethyl ether or polyoxyethylene Chinese rose base ether.
Specifically, the divalent main brightener concentration is 0.5-5g/L.
Specifically, the inhibitor concentration is 2-60g/L.
Specifically, the sulfuric acid concentration is 10-25ml/L sulfuric acid.
Specifically, the concentration of formaldehyde is 0.5-2ml/L.
A kind of preparation method of high dispersive acidic copper plating additive, comprises the following steps：
Step 1：The deionized water of container volume 2/3 is added in a reservoir, is added in the concentrated sulfuric acid of calculation amount, is stirred evenly；
Step 2：After the solution of step 1 is cooled to room temperature, sequentially add calculation amount divalent main brightener,
Inhibitor, quaternary ammonium alkyl salt form cationic surfactant and formaldehyde, stirring is to being completely dissolved；
Step 3：Deionized water is supplemented to container volume to get high dispersive acidic copper plating additive.
A kind of copper plating bath for adding high dispersive acidic copper plating additive, including：
Cupric sulfate pentahydrate 58g/L-78g/L
Sulfuric acid 200g/L-220g/L
Chlorion 40ppm-60ppm
High dispersive acidic copper plating additive 0.5-20ml/L
A kind of high dispersive acidic copper plating additive is applied to the electric plating method of printed wiring board via hole, including following step
Suddenly：
Step 1：Making sheet prepares the printed wiring board of thickness of slab 1.60mm, is needed in printed wiring board by plating region homogeneous phase
Between bore the via hole of a diameter of 0.20mm-0.30mm；
Step 2：With copper plating bath, cupric sulfate pentahydrate, sulfuric acid, chlorion, high dispersive acidic copper plating additive are poured into plating
It is stirred in slot and is hybridly prepared into copper plating bath, copper plating bath is heated and controlled at 25 DEG C；
Step 3：Plating is powered to copper plating bath, and copper plating bath current density is 10-30ASF, will treated through step 1
Printed wiring board, which is inserted in copper plating bath, carries out electroplating processes 60 minutes；
Step 4：The printed wiring board handled through step 3 is put into 150 DEG C of insulating box drying and draws finished product by drying.
The beneficial effects of the present invention are：Present invention employs covering power and the better organic disulfides of covering power
And the quaternary ammonium alkyl salt form cationic surfactant combination compounded therewith, thus have substantially in 10-30ASF current density ranges
The thick effect with surface copper thickness rate value of hole wall copper during printed wiring board the electroplates in hole is improved, obtaining layers of copper, there is satisfaction to produce
The heat resistance and ductility needed can more meet the making demand of high aperture ratio printed circuit board.Add high dispersive acid copper-plating
Sulfuric acid type acid copper plating bath after additive, with ingredient is simple, current efficiency is high, electrical with entire bright, high ductibility, height
The features such as coating of conduction property, makes it have a very wide range of application in printed circuit board manufacturing.High dispersive acid copper-plating adds
Agent is added mainly to include divalent main brightener, inhibitor and quaternary ammonium alkyl salt form cationic surfactant, process specific
Chlorion in three components and the plating solution of ratio allotment acts synergistically, and makes what electro-deposition in printed circuit plate surface or through hole went out
Layers of copper is bright, leveling.
Specific embodiment
The present invention includes the component of following concentration on a kind of high dispersive acidic copper plating additive：
Divalent main brightener 0.1-10g/L
Inhibitor 1-100g/L
Quaternary ammonium alkyl salt form cationic surfactant 0.1-5g/L
Sulfuric acid 5-50ml/L
Formaldehyde 0.1-4ml/L
Surplus is deionized water；
Wherein, the divalent main brightener is sodium polydithio-dipropyl sulfonate, phenyl polydithio-dipropyl sulphur
One or more mixtures in sour sodium, thiazolinyl sodium polydithio-dipropyl sulfonate, 2-mercaptobenzimidazole；The inhibition
Agent includes at least one polyethylene glycol or polypropylene glycol or both block copolymer macromolecule；The quaternary ammonium alkyl salt form sun from
Sub- surfactant is methyl triethyl ammonium chloride, benzyltriethylammoinium chloride, dodecyl trimethyl ammonium chloride, cetyl
One or more mixtures in trimethyl ammonium chloride.
Specifically, the inhibitor is Macrogol 4000 or Macrogol 6000 or PEG 8000 or poly- second two
One or more mixtures in alcohol 10000 or poly- (ethylene glycol and 1,2-propylene glycol) monomethyl ether or polyoxyethylene Chinese rose base ether.
Specifically, the divalent main brightener concentration is 0.5-5g/L.
Specifically, the inhibitor concentration is 2-60g/L.
Specifically, the sulfuric acid concentration is 10-25ml/L sulfuric acid.
Specifically, the concentration of formaldehyde is 0.5-2ml/L.
A kind of preparation method of high dispersive acidic copper plating additive, comprises the following steps：
Step 1：The deionized water of container volume 2/3 is added in a reservoir, is added in the concentrated sulfuric acid of calculation amount, is stirred evenly；
Step 2：After the solution of step 1 is cooled to room temperature, sequentially add calculation amount divalent main brightener,
Inhibitor, quaternary ammonium alkyl salt form cationic surfactant and formaldehyde, stirring is to being completely dissolved；
Step 3：Deionized water is supplemented to container volume to get high dispersive acidic copper plating additive.
A kind of copper plating bath for adding high dispersive acidic copper plating additive, including：
Cupric sulfate pentahydrate 58g/L-78g/L
Sulfuric acid 200g/L-220g/L
Chlorion 40ppm-60ppm
High dispersive acidic copper plating additive 0.5-20ml/L.
Preferably, the concentration of the high dispersive acidic copper plating additive is 2-10ml/L.
A kind of high dispersive acidic copper plating additive is applied to the electric plating method of printed wiring board via hole, including following step
Suddenly：
Step 1：Making sheet prepares the printed wiring board of thickness of slab 1.60mm, is needed in printed wiring board by plating region homogeneous phase
Between bore the via hole of a diameter of 0.20mm-0.30mm；
Step 2：With copper plating bath, cupric sulfate pentahydrate, sulfuric acid, chlorion, high dispersive acidic copper plating additive are poured into plating
It is stirred in slot and is hybridly prepared into copper plating bath, copper plating bath is heated and controlled at 25 DEG C；
Step 3：Plating, to copper plating bath be powered, copper plating bath current density be 10-30ASF (25ASF), will be through step 1 at
Printed wiring board after reason, which is inserted in copper plating bath, carries out electroplating processes 60 minutes；
Step 4：The printed wiring board handled through step 3 is put into 150 DEG C of insulating box drying and draws finished product by drying.
Embodiment：
A kind of high dispersive acidic copper plating additive, component are as follows：
Divalent main brightener 1.5g/L
Polyethylene glycol 10000 15g/L
Poly- (ethylene glycol and 1,2-propylene glycol) monomethyl ether 50g/L
Benzyltriethylammoinium chloride 1g/L
Sulfuric acid 10ml/L
Formaldehyde 1ml/L
Surplus is deionized water；
Wherein, the divalent main brightener is sodium polydithio-dipropyl sulfonate and phenyl polydithio-dipropyl sulfonic acid
Sodium mixture.
A kind of copper plating bath for adding high dispersive acidic copper plating additive, component are as follows：
Cupric sulfate pentahydrate 68g/L
Sulfuric acid 210g/L
Chlorion 50ppm
High dispersive acidic copper plating additive 5ml/L
A kind of high dispersive acidic copper plating additive is applied to the electric plating method of printed wiring board via hole, including following step
Suddenly：
Step 1：Making sheet prepares the printed wiring board of thickness of slab 1.60mm, is needed in printed wiring board by plating region homogeneous phase
Between bore the via hole of a diameter of 0.20mm-0.30mm；
Step 2：With copper plating bath, it is sulfuric acid that cupric sulfate pentahydrate that concentration is 68g/L, concentration are 210g/L, concentration
The chlorion of 50ppm, the high dispersive acidic copper plating additive that concentration is 5ml/L are poured into be stirred in electroplating bath and are hybridly prepared into
Copper plating bath heats copper plating bath and controls at 25 DEG C；
Step 3：Plating is powered to copper plating bath, and copper plating bath current density is 25ASF, will be through
Treated that printed wiring board inserts electroplating processes is carried out in copper plating bath 60 minutes for step 1；
Step 4：The printed wiring board handled through step 3 is put into 150 DEG C of insulating box drying and draws finished product by drying.
To in printed wiring board electroplating process, divalent main brightener can generate under chlorion collaboration and " go to pole
Change " effect, copper ion is accelerated in addition, divalent main brightener also participates in the crystallization process of copper, to make crystalline substance in the deposition of cathode
Grain refinement, high molecular polymer inhibitor generally comprises one or more combinations, under the collaboration of chlorion, can sink to the electricity of copper
Product generates inhibitory action, is inhibiting copper while high potential goes deposition, is assisting divalent main brightener in low potential area
Area deposition layers of copper.In addition, inhibitor sheet can effectively reduce the surface tension of acid copper plating bath, promote high as surfactant
Each component movement in the plating solution and scattered in scattered acidic copper plating additive.Quaternary ammonium alkyl salt form cationic surfactant band
There is very strong electropositive, competed in high current density region and copper ion, reduce the deposition of areas of high potential copper ion.
By the printed wiring board after the completion of plating, according to IPC-TM6502.6.8, (test common in the art refers to
Mark) in method carry out thermal shock test, through hole fine heat-resisting performance, at 288 DEG C, 0.20mm or 0.30mm through holes through 3 times, 5
Copper fracture in hole is not found after secondary or 8 thermal shocks.
By the printed wiring board after the completion of plating, polyester resin microsection is done in different zones sampling, uses metallographic microscope
6 copper thickness in 4 points of the plate face and hole of single hole are measured, then calculate copper thickness and plate face copper in hole according to 6 methods and 10 methods
Thickness rate value (TP values) evaluates solution dispersibility according to its actual measured results.
Experiment is drawn, printed wiring board via hole is carried out by using the copper plating bath of addition high dispersive acidic copper plating additive
It electroplates, copper is thick in gained via hole and plate face copper thickness mean ratio is than copper is thick thick with plate face copper in via hole obtained by existing copper plating bath
The high 5-10% of mean ratio.The result shows that the copper plating bath of addition high dispersive acidic copper plating additive has good dispersibility,
Adding high dispersive acidic copper plating additive has the performance for the dispersibility for improving high thickness to diameter ratio printed wiring board the electroplates in hole.
Embodiment of above be only the preferred embodiment of the present invention is described, not to the scope of the present invention into
Row limits, and on the premise of design spirit of the present invention is not departed from, this field ordinary skill technical staff is to the technical side of the present invention
The various modifications and improvement that case is made should all be fallen into the protection domain that claims of the present invention determines.
Claims (9)
1. a kind of high dispersive acidic copper plating additive, it is characterised in that：Include：
Divalent main brightener 0.1-10g/L
Inhibitor 1-100g/L
Quaternary ammonium alkyl salt form cationic surfactant 0.1-5g/L
Sulfuric acid 5-50ml/L
Formaldehyde 0.1-4ml/L
Surplus is deionized water；
Wherein, the divalent main brightener for sodium polydithio-dipropyl sulfonate, phenyl sodium polydithio-dipropyl sulfonate,
One or more mixtures in thiazolinyl sodium polydithio-dipropyl sulfonate, 2-mercaptobenzimidazole；The inhibitor bag
Include at least one polyethylene glycol or polypropylene glycol or both block copolymer macromolecule；The quaternary ammonium alkyl salt form cation form
Face activating agent is methyl triethyl ammonium chloride, benzyltriethylammoinium chloride, dodecyl trimethyl ammonium chloride, cetyl front three
One or more mixtures in ammonium chloride.
2. a kind of high dispersive acidic copper plating additive according to claim 1, it is characterised in that：The inhibitor is poly-
Ethylene glycol 4000 or Macrogol 6000 or PEG 8000 or polyethylene glycol 10000 or poly- (ethylene glycol and 1,2-propylene glycol) single first
One or more mixtures in ether or polyoxyethylene Chinese rose base ether.
3. a kind of high dispersive acidic copper plating additive according to claim 1, it is characterised in that：The divalent
Main brightener concentration is 0.5-5g/L.
4. a kind of high dispersive acidic copper plating additive according to claim 1, it is characterised in that：The inhibitor concentration
For 2-60g/L.
5. a kind of high dispersive acidic copper plating additive according to claim 1, it is characterised in that：The sulfuric acid concentration is
10-25ml/L sulfuric acid.
6. a kind of high dispersive acidic copper plating additive according to claim 1, it is characterised in that：The concentration of formaldehyde is
0.5-2ml/L。
7. a kind of preparation method of high dispersive acidic copper plating additive according to claim 1, it is characterised in that：Including such as
Lower step：
Step 1：The deionized water of container volume 2/3 is added in a reservoir, is added in the concentrated sulfuric acid of calculation amount, is stirred evenly；
Step 2：After the solution of step 1 is cooled to room temperature, sequentially adds the divalent main brightener of calculation amount, inhibit
Agent, quaternary ammonium alkyl salt form cationic surfactant and formaldehyde, stirring is to being completely dissolved；
Step 3：Deionized water is supplemented to container volume to get high dispersive acidic copper plating additive.
8. a kind of high dispersive acidic copper plating additive application according to claim 1, it is characterised in that：Applied to track
The electric plating method of road plate via hole, comprises the following steps：
Step 1：Making sheet prepares the printed wiring board of thickness of slab 1.60mm, is needed in printed wiring board by the uniform alternate brill in plating region
The via hole of a diameter of 0.20mm-0.30mm；
Step 2：With copper plating bath, cupric sulfate pentahydrate, sulfuric acid, chlorion, high dispersive acidic copper plating additive are poured into electroplating bath
It is stirred and is hybridly prepared into copper plating bath, copper plating bath is heated and control at 25 DEG C；
Step 3：Plating, to copper plating bath be powered, copper plating bath current density be 10-30ASF, will through step 1 treated printing
Wiring board, which is inserted in copper plating bath, carries out electroplating processes 60 minutes；
Step 4：The printed wiring board handled through step 3 is put into 150 DEG C of insulating box drying and draws finished product by drying.
9. a kind of high dispersive acidic copper plating additive application according to claim 8, it is characterised in that：The copper plating bath is each
Component ratio is as follows：
Cupric sulfate pentahydrate 58g/L-78g/L
Sulfuric acid 200g/L-220g/L
Chlorion 40ppm-60ppm
High dispersive acidic copper plating additive 0.5-20ml/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711406395.5A CN108118372A (en) | 2017-12-22 | 2017-12-22 | A kind of high dispersive acidic copper plating additive and preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711406395.5A CN108118372A (en) | 2017-12-22 | 2017-12-22 | A kind of high dispersive acidic copper plating additive and preparation method and application |
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| CN201711406395.5A Pending CN108118372A (en) | 2017-12-22 | 2017-12-22 | A kind of high dispersive acidic copper plating additive and preparation method and application |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110373687A (en) * | 2019-08-30 | 2019-10-25 | 广州皓悦新材料科技有限公司 | A kind of pulse plating photo etching and preparation method thereof plating high aspect ratio through-hole and blind hole |
| CN110453254A (en) * | 2019-08-30 | 2019-11-15 | 广州皓悦新材料科技有限公司 | A kind of pulse plating brightener and preparation method thereof |
| CN110453255A (en) * | 2019-08-30 | 2019-11-15 | 广州皓悦新材料科技有限公司 | A kind of VCP copper brightener and preparation method thereof with high covering power |
| CN110644021A (en) * | 2019-09-16 | 2020-01-03 | 铜陵市华创新材料有限公司 | 4.5-micron electrolytic copper foil for lithium ion battery, preparation method and additive |
| CN111778545A (en) * | 2020-07-31 | 2020-10-16 | 中南大学 | Micropore filling method based on small-size quaternary ammonium salt single additive |
| CN111892706A (en) * | 2020-07-23 | 2020-11-06 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | PEG (polyethylene glycol) coupled heterocyclic compound and application thereof in acid bright copper plating |
| CN112877739A (en) * | 2021-01-13 | 2021-06-01 | 苏州天承化工有限公司 | Electroplating solution and electroplating method and application thereof |
-
2017
- 2017-12-22 CN CN201711406395.5A patent/CN108118372A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110373687A (en) * | 2019-08-30 | 2019-10-25 | 广州皓悦新材料科技有限公司 | A kind of pulse plating photo etching and preparation method thereof plating high aspect ratio through-hole and blind hole |
| CN110453254A (en) * | 2019-08-30 | 2019-11-15 | 广州皓悦新材料科技有限公司 | A kind of pulse plating brightener and preparation method thereof |
| CN110453255A (en) * | 2019-08-30 | 2019-11-15 | 广州皓悦新材料科技有限公司 | A kind of VCP copper brightener and preparation method thereof with high covering power |
| CN110644021A (en) * | 2019-09-16 | 2020-01-03 | 铜陵市华创新材料有限公司 | 4.5-micron electrolytic copper foil for lithium ion battery, preparation method and additive |
| CN111892706A (en) * | 2020-07-23 | 2020-11-06 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | PEG (polyethylene glycol) coupled heterocyclic compound and application thereof in acid bright copper plating |
| CN111778545A (en) * | 2020-07-31 | 2020-10-16 | 中南大学 | Micropore filling method based on small-size quaternary ammonium salt single additive |
| CN112877739A (en) * | 2021-01-13 | 2021-06-01 | 苏州天承化工有限公司 | Electroplating solution and electroplating method and application thereof |
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Application publication date: 20180605 |