CN113430598B - Circuit board blind hole filling electro-coppering solution and application thereof - Google Patents
Circuit board blind hole filling electro-coppering solution and application thereof Download PDFInfo
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- CN113430598B CN113430598B CN202110992097.9A CN202110992097A CN113430598B CN 113430598 B CN113430598 B CN 113430598B CN 202110992097 A CN202110992097 A CN 202110992097A CN 113430598 B CN113430598 B CN 113430598B
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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
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- 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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- Microelectronics & Electronic Packaging (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention provides a circuit board blind hole filling electro-coppering solution which is composed of the following components in concentration: 40-120g/L of sulfuric acid, 240g/L of copper sulfate pentahydrate, 40-80ppm of chloride ions, 1-10ppm of accelerator, 1000ppm of inhibitor and 10-100ppm of leveling agent; the leveling agent is 2-mercaptobenzothiazole amine derivatives containing imidazole groups. Leveling agent molecules of the imidazole group-containing 2-mercaptobenzothiazole amine derivatives in the copper electroplating solution have strong competitive adsorption capacity on the surface of copper, and when the leveling agent molecules are applied, imidazole functional groups, thiazole functional groups and amine functional groups in the leveling agent and other components in the copper electroplating solution are cooperated with each other, so that blind hole filling can be realized, and copper after electroplating is finished is thinner. The thickness of the surface copper plating can be less than 15 microns after the blind hole with the aperture of 100 microns and the hole depth of 75 microns is filled.
Description
Technical Field
The invention relates to the technical field of circuit board electroplating, in particular to a circuit board blind hole filling electro-coppering solution and application thereof.
Background
The printed wiring board is an important electronic component, is a support of an electronic component, is a carrier for electrical connection of the electronic component, and is applied to almost all electronic products.
In recent years, the electronic industry technology has been rapidly developed, and many electronic products have strong functions and good portability, so that the electronic products have smaller and smaller volumes and more concentrated functions, which promotes the development of a printed circuit Board as a carrier thereof toward High Density Interconnection (HDI) printed circuit boards. The HDI board is a multilayer, thin, stable and high-density printed circuit board which cannot be realized by a conventional multilayer circuit board and is manufactured by introducing a micro via hole and a fine circuit technology into the printed circuit board and superposing a circuit layer and an insulating layer by layer. The combination of the tiny via holes and the fine circuit technology is a premise for realizing the high density of the printed circuit board.
And the micro via holes (including through holes, blind holes and buried holes) realize the electrical interconnection between the HDI board layers.
In the aspect of fine circuits, the HDI adopts a semi-additive manufacturing process, firstly, hole metallization, through hole electroplating and hole filling electroplating are carried out on a copper-carrying substrate, then, film pressing and pattern electroplating are carried out, and after film stripping, bottom copper is etched away in a differential etching mode to form the precise circuits. In the etching process, the etching rates in all directions are different, so that the upper bottom width and the lower bottom width of the circuit inevitably have certain difference, and the phenomenon is lateral erosion. The less obvious the side etching phenomenon, the closer the cross section of the line is to a rectangle, the more serious the side etching phenomenon is, the worse the line quality is, and the like a trapezoid.
At present, when the minimum line width/line distance of HDI is 40/50 micrometers or less, the cost for manufacturing fine lines by simply relying on the promotion of etching technology is high. The difficulty of reducing the thickness of the surface copper and the etching of the circuit is greatly facilitated to the manufacture of the circuit by reducing the thickness of the surface copper as much as possible, and the thickness of the surface copper after hole filling is reduced to the pursuit direction of hole filling electroplating of the circuit board. In the existing electroplating additive for filling the traditional HDI blind hole, the copper thickness of the back surface of the filled HDI common blind hole is generally 16-20 micrometers, sometimes more than 20 micrometers, and a more uniform and thinner surface copper plating layer is needed for the existing higher-precision circuit.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: and the thickness of the surface copper after filling the blind hole is reduced, so that the thickness of the surface copper plating is lower than 15 microns after the blind hole is filled to be qualified.
In order to solve the technical problems, the invention adopts the technical scheme that:
the circuit board blind hole filling electro-coppering solution consists of the following components in concentration: 40-120g/L of sulfuric acid, 240g/L of copper sulfate pentahydrate, 40-80ppm of chloride ions, 1-10ppm of accelerator, 1000ppm of inhibitor and 10-100ppm of leveling agent; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group.
Further, said imidazole group-containingThe structural formula of the 2-mercaptobenzothiazole amine derivative is as follows:
wherein R is
Or
Or
。
Further, the accelerator is an alcoholic thiopropane sulfonate or a polydithio-dipropane sulfonate.
Further, the thiolpropane sulfonate is sodium thiolpropane sulfonate, and the polydithio-dipropyl sulfonate is sodium polydithio-dipropyl sulfonate.
Further, the inhibitor is one of polyethylene glycol, polypropylene glycol-polyethylene glycol-polypropylene glycol triblock copolymer and ethylene oxide-propylene oxide block copolymer.
Further, the molecular weight of the inhibitor is 4000-10000.
The application of the circuit board blind hole filling electro-coppering solution is applied to filling the blind holes of the printed circuit board.
Further, the electroplating process conditions for filling the blind holes are as follows: the electroplating temperature is 10-40 ℃, and the current density is 0.5-5A/dm2。
The invention has the beneficial effects that: leveling agent molecules of the imidazole group-containing 2-mercaptobenzothiazole amine derivatives in the copper electroplating solution have strong competitive adsorption capacity on the surface of copper, and when the leveling agent molecules are applied, imidazole functional groups, thiazole functional groups and amine functional groups in the leveling agent and other components in the copper electroplating solution are cooperated with each other, so that blind hole filling can be realized, and copper after electroplating is finished is thinner. The thickness of the surface copper plating can be less than 15 microns after the blind hole with the aperture of 100 microns and the hole depth of 75 microns is filled.
Drawings
The following detailed description of the invention will be made with reference to the accompanying drawings
FIG. 1 is a diagram showing the plating result of test example 1 in which a blind via of a circuit board of the present invention is filled with an electrolytic copper plating solution;
FIG. 2 is a diagram showing the plating result of test example 2 in which a blind via of a circuit board of the present invention was filled with an electrolytic copper plating solution;
FIG. 3 is a diagram showing the plating result of test example 3 in which a blind via of a circuit board of the present invention was filled with an electrolytic copper plating solution;
FIG. 4 is a diagram showing the plating result of test example 4 in which a blind via of a circuit board of the present invention was filled with an electrolytic copper plating solution;
FIG. 5 is a diagram showing the plating result of test example 5 in which a blind via of a circuit board of the present invention was filled with an electrolytic copper plating solution;
FIG. 6 is a graph showing the plating result of comparative example 1 in which a blind via of a wiring board of the present invention is filled with an electrolytic copper plating solution;
FIG. 7 is a graph showing the plating result of comparative example 2 in which blind holes of a wiring board of the present invention are filled with an electrolytic copper plating solution;
FIG. 8 is a graph showing the plating result of comparative example 3 in which blind holes of a wiring board of the present invention are filled with an electrolytic copper plating solution;
FIG. 9 is a graph showing the plating result of comparative example 4 in which blind holes of a wiring board of the present invention are filled with an electrolytic copper plating solution;
FIG. 10 is a graph showing the plating result of comparative example 5 in which blind holes of a wiring board of the present invention are filled with an electrolytic copper plating solution.
Detailed Description
Example 1
The circuit board blind hole filling electro-coppering solution consists of the following components in concentration: 40-120g/L of sulfuric acid, 240g/L of copper sulfate pentahydrate, 40-80ppm of chloride ions, 1-10ppm of accelerator, 1000ppm of inhibitor and 10-100ppm of leveling agent. The accelerator is sodium thiolpropane sulfonate or sodium polydithio-dipropanesulfonate. The inhibitor is one of polyethylene glycol, polypropylene glycol-polyethylene glycol-polypropylene glycol triblock copolymer and ethylene oxide-propylene oxide block copolymer; the molecular weight of the inhibitor is 4000-10000. The leveling agent isThe imidazole group-containing 2-mercaptobenzothiazole amine derivative has the structural formula:
wherein R is
Or
Or
。
Is- (CH)2）3-NH2；
Is- (CH)2）3-NH-（CH2）2-NH2；
Is- (CH)2）3-NH-（CH2）2-NH-（CH2）2-NH2。
Example 2
The application of the circuit board blind hole filling electro-coppering solution in the embodiment 1 is applied to blind hole filling. The electroplating process conditions for filling the blind holes are as follows: the current density is 0.5-5A/dm2The temperature is 10-40 ℃.
In order to further explain the feasibility of the present invention, the technical contents, construction features, and concrete examples of the achieved objects and effects according to the present invention will be described in detail with reference to the accompanying drawings.
Test example 1
Preparing an electrolytic copper plating solution according to the following components: sulfuric acid: 60g/L of copper sulfate pentahydrate, 200g/L of copper sulfate pentahydrate, 60ppm of chloride ions and 1p of acceleratorpm, inhibitor 100ppm, leveler 10 ppm. Wherein the accelerator is sodium polydithio-dipropyl sulfonate; the inhibitor is polyethylene glycol with molecular weight of 10000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
wherein R is
。
Test example 2
Preparing an electrolytic copper plating solution according to the following components: 60g/L of sulfuric acid, 200g/L of copper sulfate pentahydrate, 60ppm of chloride ions, 10ppm of an accelerator, 1000ppm of an inhibitor and 100ppm of a leveling agent. Wherein the accelerator is sodium polydithio-dipropyl sulfonate; the inhibitor is polyethylene glycol, and the molecular weight of the polyethylene glycol is 4000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
wherein R is
。
Test example 3
Preparing an electrolytic copper plating solution according to the following components: 60g/L of sulfuric acid, 200g/L of copper sulfate pentahydrate, 60ppm of chloride ions, 5ppm of an accelerator, 600ppm of an inhibitor and 30ppm of a leveling agent. Wherein the accelerator is sodium thiolpropanate; the inhibitor is polypropylene glycol-polyethylene glycol-polypropylene glycol triblock copolymer, and the molecular weight of the polypropylene glycol-polyethylene glycol-polypropylene glycol triblock copolymer is 8000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
wherein R is
。
Test example 4
Preparing an electrolytic copper plating solution according to the following components: 40g/L of sulfuric acid, 240g/L of copper sulfate pentahydrate, 80ppm of chloride ions, 5ppm of an accelerator, 600ppm of an inhibitor and 30ppm of a leveling agent. Wherein the accelerator is sodium polydithio-dipropyl sulfonate; the inhibitor is polyethylene glycol, and the molecular weight of the polyethylene glycol is 6000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
，
wherein R is
。
Test example 5
Preparing an electrolytic copper plating solution according to the following components: 120g/L of sulfuric acid, 120g/L of copper sulfate pentahydrate, 40ppm of chloride ions, 5ppm of an accelerator, 600ppm of an inhibitor and 50ppm of a leveling agent. Wherein the accelerator is sodium thiolpropanate; the inhibitor is polypropylene glycol-polyethylene glycol-polypropylene glycol triblock copolymer, and the molecular weight of the polypropylene glycol-polyethylene glycol-polypropylene glycol triblock copolymer is 6000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
wherein R is
。
Comparative example 1
Preparing an electrolytic copper plating solution according to the following components: 60g/L of sulfuric acid, 200g/L of copper sulfate pentahydrate, 60ppm of chloride ions, 5ppm of an accelerator, 600ppm of an inhibitor and 5ppm of a leveling agent. Wherein the accelerator is sodium polydithio-dipropyl sulfonate; the inhibitor is polyethylene glycol with molecular weight of 10000; the leveling agent is Kennelv.
Comparative example 2
Preparing an electrolytic copper plating solution according to the following components: 60g/L of sulfuric acid, 200g/L of copper sulfate pentahydrate, 60ppm of chloride ions, 10ppm of an accelerator, 1000ppm of an inhibitor and 5ppm of a leveling agent. Wherein the accelerator is sodium polydithio-dipropyl sulfonate; the inhibitor is polyethylene glycol, and the molecular weight of the polyethylene glycol is 4000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
wherein R is
。
Comparative example 3
Preparing an electrolytic copper plating solution according to the following components: 60g/L of sulfuric acid, 200g/L of copper sulfate pentahydrate, 60ppm of chloride ions, 10ppm of an accelerator, 1000ppm of an inhibitor and 110ppm of a leveling agent. Wherein the accelerator is sodium polydithio-dipropyl sulfonate; the inhibitor is polyethylene glycol, and the molecular weight of the polyethylene glycol is 4000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
wherein R is
。
Comparative example 4
Preparing an electrolytic copper plating solution according to the following components: sulfuric acid: 60g/L, 200g/L of copper sulfate pentahydrate, 60ppm of chloride ions, 15ppm of accelerator, 100ppm of inhibitor and 20ppm of leveling agent. Wherein the accelerator is poly-diSodium thiodipropanesulfonate; the inhibitor is polyethylene glycol with molecular weight of 10000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
wherein R is
。
Comparative example 5
Preparing an electrolytic copper plating solution according to the following components: sulfuric acid: 60g/L, 200g/L of copper sulfate pentahydrate, 60ppm of chloride ions, 1ppm of accelerator, 80ppm of inhibitor and 20ppm of leveling agent. Wherein the accelerator is sodium polydithio-dipropyl sulfonate; the inhibitor is polyethylene glycol with molecular weight of 10000; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group, and the structural formula of the 2-mercaptobenzothiazole amine derivative containing the imidazole group is as follows:
wherein R is
。
The electrolytic copper plating solutions prepared in the test examples 1 to 5 and the comparative examples 1 to 5 were respectively added into 1500mL of a Harlin bath, clean phosphor-copper plates with a phosphor content of 0.04 to 0.065% were placed at both ends of the Harlin bath as anodes, and stirred by pumping up gas in the middle of the bath at an air stirring speed of 2 to 3L/min.
A plurality of blind hole plates (the specification is 50mm multiplied by 100mm, the diameter of a blind hole is 100 mu m, the hole depth is 75 mu m) to be filled are pretreated by oil removal, microetching, activation in dilute sulfuric acid solution and the like, and then the blind hole plates are respectively put into the liquid of the Harlin groove for electroplating (vertically put in the middle position). In the case of plating, the plating conditions of the test examples 1 to 5 and the comparative examples 1 to 5 were: the temperature is 25 ℃, and the current density is 1.5A/dm2The plating time was 45 minutes.
And respectively sectioning the electroplated samples, respectively observing the sections of the sectioned samples by using a metallographic microscope, and evaluating the filling effect of the blind holes and the thickness of the surface copper, wherein the results are detailed in table 1 and figures 1 to 10.
TABLE 1 electroplated blind via fill Effect and surface copper thickness results
In summary, the leveling agent molecules of the imidazole group-containing 2-mercaptobenzothiazole amine derivatives in the copper electroplating solution have strong competitive adsorption capacity on the copper surface, and when the leveling agent molecules are applied, the imidazole functional groups, the thiazole functional groups and the amine functional groups in the leveling agent and other components in the copper electroplating solution are cooperated with each other, so that blind hole filling can be realized, and copper after electroplating is finished is thinner. The thickness of the surface copper plating can be less than 15 microns after the blind hole with the aperture of 100 microns and the hole depth of 75 microns is filled.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent flow transformations made by using the contents of the specification and drawings, or applied directly or indirectly to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. The copper electroplating solution for filling the blind holes of the circuit board is characterized by comprising the following components in concentration: 40-120g/L of sulfuric acid, 240g/L of copper sulfate pentahydrate, 40-80ppm of chloride ions, 1-10ppm of accelerator, 1000ppm of inhibitor and 10-100ppm of leveling agent; the leveling agent is a 2-mercaptobenzothiazole amine derivative containing an imidazole group;
the structural formula of the imidazole group-containing 2-mercaptobenzothiazole amine derivative is as follows:
wherein R is
Or
Or
；
The accelerator is thiolane sulfonate or polydithio-dipropyl sulfonate; the inhibitor is one of polyethylene glycol, polypropylene glycol-polyethylene glycol-polypropylene glycol triblock copolymer and ethylene oxide-propylene oxide block copolymer.
2. The circuit board blind hole filling electrolytic copper plating solution according to claim 1, wherein the thiolpropane sulfonate is sodium thiolpropane sulfonate and the polydithio-dipropyl sulfonate is sodium polydithio-dipropyl sulfonate.
3. The circuit board blind hole filling electrolytic copper plating solution as claimed in claim 1, wherein the molecular weight of the inhibitor is 4000-10000.
4. Use of the electro-coppering solution for filling blind holes in circuit boards according to any one of claims 1 to 3, characterized in that it is used for filling blind holes in printed circuit boards.
5. The application of the circuit board blind hole filling electro-coppering solution as claimed in claim 4, wherein the electroplating process conditions of the blind hole filling are as follows: the electroplating temperature is 10-40 ℃, and the current density is 0.5-5A/dm2。
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| CN202110992097.9A CN113430598B (en) | 2021-08-27 | 2021-08-27 | Circuit board blind hole filling electro-coppering solution and application thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1069211A2 (en) * | 1999-07-15 | 2001-01-17 | The Boc Group, Inc. | Electroplating solutions |
| CN102277567A (en) * | 2011-07-26 | 2011-12-14 | 陕西师范大学 | Chemical copper plating solution for micropore filling |
| CN103103586A (en) * | 2013-02-22 | 2013-05-15 | 陕西师范大学 | Thiazole compound-containing copper electroplating solution |
| CN104177353A (en) * | 2014-07-23 | 2014-12-03 | 华东交通大学 | Mercaptobenzothiazolyl imidazoline derivative, and preparation method and application thereof |
| CN111593375A (en) * | 2020-05-15 | 2020-08-28 | 电子科技大学 | Leveling agent for electronic circuit copper electroplating pore filling and copper electroplating bath |
-
2021
- 2021-08-27 CN CN202110992097.9A patent/CN113430598B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1069211A2 (en) * | 1999-07-15 | 2001-01-17 | The Boc Group, Inc. | Electroplating solutions |
| CN102277567A (en) * | 2011-07-26 | 2011-12-14 | 陕西师范大学 | Chemical copper plating solution for micropore filling |
| CN103103586A (en) * | 2013-02-22 | 2013-05-15 | 陕西师范大学 | Thiazole compound-containing copper electroplating solution |
| CN104177353A (en) * | 2014-07-23 | 2014-12-03 | 华东交通大学 | Mercaptobenzothiazolyl imidazoline derivative, and preparation method and application thereof |
| CN111593375A (en) * | 2020-05-15 | 2020-08-28 | 电子科技大学 | Leveling agent for electronic circuit copper electroplating pore filling and copper electroplating bath |
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