CN113463143A - Electrochemical copper plating method based on full addition method - Google Patents
Electrochemical copper plating method based on full addition method Download PDFInfo
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- CN113463143A CN113463143A CN202110709231.XA CN202110709231A CN113463143A CN 113463143 A CN113463143 A CN 113463143A CN 202110709231 A CN202110709231 A CN 202110709231A CN 113463143 A CN113463143 A CN 113463143A
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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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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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
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
- H05K3/182—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating characterised by the patterning method
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Automation & Control Theory (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemically Coating (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention belongs to the technical field of PCBs (printed circuit boards), and provides an electrochemical copper plating method based on a full addition method, which is characterized by comprising the following steps of: drilling, removing glue residues, drying a film, electrochemical copper plating and etching; the electrochemical copper plating process specifically comprises: s1, adopting a catalytic reduction system, adjusting an electrochemical copper plating reaction system, and forming a uniform and compact copper layer on the surface of a base material or a hole in a copper deposition mode; s2, thickening a copper layer by electroplating in the existing plating solution system by taking copper as a soluble anode and titanium as a cathode. The invention can improve the copper plating rate, ensure the copper plating binding force and the copper layer ductility, and realize new connectionBranched polymerization catalytic system for controlling oxidation reduction reaction by-product Cu2The generation of O reduces the generation probability of disproportionation reaction and controls the reaction rate and stability of the electrochemical copper plating system in the electroless plating.
Description
Technical Field
The invention belongs to the technical field of PCBs, and particularly relates to an electrochemical copper plating method based on a full addition method.
Background
The manufacturing process of the Printed Circuit Board (PCB) mainly comprises a subtractive method, a semi-additive method, a full-additive method and the like. Among them, the full-additive method refers to selectively forming a conductive layer on an insulating substrate, and has many advantages such as avoiding lateral etching, reducing the thickness of an HDI (high density interconnect) board, and greatly reducing the waste of copper resources, and thus has received much attention and research. However, the conventional full-addition method adopts an insulating material as a matrix, and a conductive seed layer is manufactured first when a conductive layer is formed, so that the working procedures are increased, the production period is prolonged, and the environmental pollution is aggravated.
In addition, in the prior art, the existing copper deposition-electroplating system has the following defects:
1. the plate surface is easy to oxidize and blacken after chemical copper deposition, the thickness of a copper deposition layer is low, and the copper deposition and electroplating transportation process has a large reliability risk;
2. the interval time between electroplating and copper deposition is long, and a layer of electroplated copper layer needs to be thickened on the surface of the copper deposition layer through electroplating, so that the process is long and the working procedures are complicated;
3. the general full addition method has poor copper surface adhesion, and the standard of heat resistance and reliability has larger difference from the standard of the prior art.
Disclosure of Invention
In view of the above, the present invention provides an electrochemical copper plating method based on full addition.
The technical scheme of the invention is as follows:
an electrochemical copper plating method based on a full addition method is characterized by comprising the following steps: drilling, removing glue residues, drying a film, electrochemical copper plating and etching;
the electrochemical copper plating process specifically comprises:
s1, adopting a catalytic reduction system, adjusting an electrochemical copper plating reaction system, and forming a uniform and compact copper layer on the surface of a base material or a hole in a copper deposition mode;
s2, thickening a copper layer by electroplating in the existing plating solution system by taking copper as a soluble anode and titanium as a cathode.
Further, in the step S1, the electrochemical copper plating reaction system is an acidic system, and the pH value of the acidic system is 1.0 to 2.0.
Further, in step S1, the thickness of the copper layer is 1-4 um.
Further, in the step S1, the copper deposition rate is 0.1-0.5um/min, and the time is controlled to be 3-10 min.
Further, in the step S2, the electroplating uses 8-20ASF dc, and the time is controlled to be 25-45 min.
Further, in step S2, the copper layer is thickened by 3-8 um.
Further, in the step S2, the total thickness of the copper layer is 20-30 um.
Further, the electrochemical copper plating reaction system comprises the following components in concentration:
copper sulfate: 6-13 g/L;
sodium hypophosphite: 8-25 g/L;
HEDTA (hydroxyethylethylenediaminetriacetic acid): 9-28 g/L;
EDTA (ethylenediaminetetraacetic acid): 8-23 g/L;
H2SO4adjusting the pH value to 1.0-2.0.
Further, the electrochemical copper plating reaction system comprises the following components in concentration:
copper sulfate: 8-10 g/L;
sodium hypophosphite: 10-20 g/L;
HEDTA (hydroxyethylethylenediaminetriacetic acid): 10-20 g/L;
EDTA (ethylenediaminetetraacetic acid): 10-20 g/L;
H2SO4adjusting the pH value to 1.0-2.0.
Furthermore, the electrochemical copper plating reaction system also comprises a plurality of auxiliary additives, and the auxiliary additives can be added by the prior art according to the concentration ratio by a person skilled in the art.
The electrochemical copper plating technology is adopted, and the production flow of the product integrates the original copper deposition, plate electricity and pattern electricity procedures; meanwhile, the existing production equipment does not need to be updated and upgraded, and the production efficiency can be greatly improved; meanwhile, the process and time are saved in the project, and the defects of scratching, crushing, scratching and the like caused by transfer of each process can be greatly reduced.
The invention combines the chemical copper plating and the electro-coppering together, and can reduce two major procedures of copper deposition and plate electricity; the flow is changed into: drilling, removing glue residues, drying a film, electrochemical copper plating, etching, eliminating a plate electric process, reducing the etching amount per unit area, and saving 10.8% of copper balls by calculating the total copper thickness of 24um, the plate electric thickness of 6um and the plated area of a pattern of 40% compared with the positive film process in the prior art. The etching treatment capacity is improved by more than 40%, the manufacturing capacity of fine lines is improved, and the probability of no copper in holes is reduced.
The invention provides an electrochemical copper plating process which can effectively improve the copper plating rate, ensure the copper plating binding force and the copper layer ductility, and control the oxidation-reduction reaction byproduct Cu by using a new graft polymerization catalytic system2The generation of O reduces the generation probability of disproportionation reaction and controls the reaction rate and stability of the electrochemical copper plating system in the electroless plating.
In the invention, the electrochemical copper plating is carried out in two steps in a plating solution system, wherein the first step is as follows: a catalytic reduction system is adopted to adjust an electrochemical copper plating reaction system, an alkaline system is changed into an acidic system, and the acidity is adjusted to 1.0-1.5; forming a uniform and compact copper layer on the surface of the substrate or the hole; and controlling the copper deposition rate, wherein the actual control time of the reaction process is 5-8min based on that the acid reduction plating early-stage rate is slightly faster than the later-stage rate. The second step is that: in the existing plating solution system, copper is used as a soluble anode, and titanium is used as a cathode; applying direct current, and processing for 25-45min to realize the thickening of the copper layer, wherein the total thickness can reach 20-30 um.
Compared with the prior art, the method changes the acidity of the plating solution and the operation system, the acid electroplating system is easier to control than the alkaline electroplating system in actual operation, and the glossiness and compactness of the product are greatly improved compared with the alkaline system. Meanwhile, the current efficiency in the direct electroplating process is increased by more than 30% by adopting a high-copper low-acid ratio, and currently, copper sulfate is still adopted as a main copper ion source, so that the actual cost is not obviously improved, and the raw materials are easy to obtain.
Under the condition of providing a certain amount of additional current, the rapid and effective copper layer deposition is realized, the defects of accelerated deposition speed, rough copper layer and poor adhesive force of an alkaline electroless copper plating system and an acidic electroless copper plating system are effectively overcome by adjusting the components of a plating solution system and using copper as an additional current auxiliary deposition system of a soluble anode material, and the deposition of the chemical plating layer with the thickness of 3-8um is completed within 25-45min of immersion plating.
The invention can effectively improve the copper plating rate, ensure the copper plating binding force and the copper layer ductility, and control the by-product Cu of the oxidation-reduction reaction by a new graft polymerization catalytic system2The generation of O reduces the generation probability of disproportionation reaction and controls the reaction rate and stability of the electrochemical copper plating system in the electroless plating.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
An electrochemical copper plating method based on a full addition method is characterized by comprising the following steps: drilling, removing glue residues, drying a film, electrochemical copper plating and etching;
the electrochemical copper plating process specifically comprises:
s1, adopting a catalytic reduction system, adjusting an electrochemical copper plating reaction system, and forming a uniform and compact copper layer on the surface of a base material or a hole in a copper deposition mode;
s2, thickening a copper layer by electroplating in the existing plating solution system by taking copper as a soluble anode and titanium as a cathode.
Further, in the step S1, the electrochemical copper plating reaction system is an acidic system, and the pH of the acidic system is 1.5.
Further, in step S1, the thickness of the copper layer is 3 um.
Further, in the step S1, the copper deposition rate is 0.3um/min, and the time is controlled to be 6 min.
Further, in the step S2, the electroplating uses a 16ASF dc current, and the time is controlled to be 35 min.
Further, in step S2, the copper layer is thickened by 5 um.
Further, in step S2, the total thickness of the copper layer is 25 um.
Further, the electrochemical copper plating reaction system comprises the following components in concentration:
copper sulfate: 9 g/L;
sodium hypophosphite: 15 g/L;
HEDTA (hydroxyethylethylenediaminetriacetic acid): 15 g/L;
EDTA (ethylenediaminetetraacetic acid): 16 g/L;
H2SO4the pH was adjusted to 1.5.
Furthermore, the electrochemical copper plating reaction system also comprises a plurality of auxiliary additives, and the auxiliary additives can be added by the prior art according to the concentration ratio by a person skilled in the art.
Example 2
This example provides an electrochemical copper plating method by a full addition process similar to that of example 1, except that in step S1, the electrochemical copper plating reaction system is an acidic system having a pH of 1.0.
Further, in step S1, the thickness of the copper layer is 2 um.
Further, in the step S1, the copper deposition rate is 0.2um/min, and the time is controlled to be 4 min.
Further, in the step S2, 10ASF dc is used for electroplating, and the time is controlled to be 25 min.
Further, in step S2, the copper layer is thickened by 4 um.
Further, in step S2, the total thickness of the copper layer is 20 um.
Example 3
This example provides an electrochemical copper plating method by a full addition process similar to that of example 1, except that in step S1, the electrochemical copper plating reaction system is an acidic system having a pH of 2.0.
Further, in step S1, the thickness of the copper layer is 4 um.
Further, in the step S1, the copper deposition rate is 0.5um/min, and the time is controlled to be 10 min.
Further, in the step S2, 20ASF dc is used for electroplating, and the time is controlled to be 45 min.
Further, in step S2, the copper layer is thickened by 8 um.
Further, in step S2, the total thickness of the copper layer is 30 um.
Example 4
This example provides an electrochemical copper plating method based on the full addition method the same as that of example 1, except that, further, the electrochemical copper plating reaction system includes the following components in the concentrations:
copper sulfate: 6/L;
sodium hypophosphite: 8 g/L;
HEDTA (hydroxyethylethylenediaminetriacetic acid): 9 g/L;
EDTA (ethylenediaminetetraacetic acid): 8 g/L;
H2SO4the pH was adjusted to 2.0.
Furthermore, the electrochemical copper plating reaction system also comprises a plurality of auxiliary additives, and the auxiliary additives can be added by the prior art according to the concentration ratio by a person skilled in the art.
Example 5
Further, the electrochemical copper plating reaction system comprises the following components in concentration:
copper sulfate: 13 g/L;
sodium hypophosphite: 25 g/L;
HEDTA (hydroxyethylethylenediaminetriacetic acid): 28 g/L;
EDTA (ethylenediaminetetraacetic acid): 23 g/L;
H2SO4the pH was adjusted to 1.0.
Furthermore, the electrochemical copper plating reaction system also comprises a plurality of auxiliary additives, and the auxiliary additives can be added by the prior art according to the concentration ratio by a person skilled in the art.
Example 6
Further, the electrochemical copper plating reaction system comprises the following components in concentration:
copper sulfate: 8 g/L;
sodium hypophosphite: 11 g/L;
HEDTA (hydroxyethylethylenediaminetriacetic acid): 12 g/L;
EDTA (ethylenediaminetetraacetic acid): 10 g/L;
H2SO4the pH was adjusted to 1.8.
Furthermore, the electrochemical copper plating reaction system also comprises a plurality of auxiliary additives, and the auxiliary additives can be added by the prior art according to the concentration ratio by a person skilled in the art.
Example 7
Further, the electrochemical copper plating reaction system comprises the following components in concentration:
copper sulfate: 10 g/L;
sodium hypophosphite: 18 g/L;
HEDTA (hydroxyethylethylenediaminetriacetic acid): 19 g/L;
EDTA (ethylenediaminetetraacetic acid): 17 g/L;
H2SO4the pH was adjusted to 1.2.
Furthermore, the electrochemical copper plating reaction system also comprises a plurality of auxiliary additives, and the auxiliary additives can be added by the prior art according to the concentration ratio by a person skilled in the art.
In embodiments 1 to 7 of the present invention, the plate electrode process is eliminated, the etching amount per unit area is reduced, and compared with the positive process in the prior art, the total copper thickness is 24um, the plate electrode thickness is 6um, and the pattern electroplating area is 40%, and the copper ball is saved by 10.8%. The etching treatment capacity is improved by more than 40%, the manufacturing capacity of fine lines is improved, and the probability of no copper in holes is reduced. The glossiness and compactness of the electroplating product are greatly improved compared with an alkaline system. Meanwhile, the current efficiency in the direct electroplating process is increased by more than 30% by adopting a high-copper low-acid ratio, and currently, copper sulfate is still adopted as a main copper ion source, so that the actual cost is not obviously improved, and the raw materials are easy to obtain.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art. It should be noted that the technical features not described in detail in the present invention can be implemented by any prior art in the field.
Claims (10)
1. The electrochemical copper plating method based on the full addition method is characterized by comprising the following steps: drilling, removing glue residues, drying a film, electrochemical copper plating and etching;
the electrochemical copper plating process specifically comprises:
s1, adopting a catalytic reduction system, adjusting an electrochemical copper plating reaction system, and forming a uniform and compact copper layer on the surface of a base material or a hole in a copper deposition mode;
s2, thickening a copper layer by electroplating in the existing plating solution system by taking copper as a soluble anode and titanium as a cathode.
2. The full addition based electrochemical copper plating method according to claim 1, characterized in that in step S1, the electrochemical copper plating reaction system is an acidic system, and the pH value of the acidic system is 1.0-2.0.
3. The full addition based electrochemical copper plating method according to claim 2, characterized in that in the step S1, the copper layer has a thickness of 1-4 um.
4. The full addition based electrochemical copper plating method according to claim 3, characterized in that in the step S1, the copper deposition rate is 0.1-0.5um/min, and the time is controlled at 3-10 min.
5. The full-addition based electrochemical copper plating method according to claim 1, characterized in that in step S2, 8-20ASF dc is used for electroplating and the time is controlled to be 25-45 min.
6. The full addition based electrochemical copper plating method according to claim 5, characterized in that in the step S2, the copper layer is thickened by 3-8 um.
7. The full addition based electrochemical copper plating method according to claim 6, characterized in that in step S2, the total thickness of the copper layer is 20-30 um.
8. The full addition process-based electrochemical copper plating method according to claim 1, characterized in that the electrochemical copper plating reaction system comprises the following components in the following concentrations:
copper sulfate: 6-13 g/L;
sodium hypophosphite: 8-25 g/L;
HEDTA：9-28g/L；
EDTA：8-23g/L；
H2SO4adjusting the pH value to 1.0-2.0.
9. The full addition process-based electrochemical copper plating method according to claim 8, characterized in that the electrochemical copper plating reaction system comprises the following components in the following concentrations:
copper sulfate: 8-10 g/L;
sodium hypophosphite: 10-20 g/L;
HEDTA：10-20g/L；
EDTA：10-20g/L；
H2SO4adjusting the pH value to 1.0-2.0.
10. The full addition based electrochemical copper plating process according to claim 8 or 9, characterized by further comprising a plurality of auxiliary additives.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114457392A (en) * | 2022-02-28 | 2022-05-10 | 广东骏亚电子科技股份有限公司 | Novel electroplating method |
| CN114554702A (en) * | 2022-02-28 | 2022-05-27 | 广东骏亚电子科技股份有限公司 | Manufacturing method of ultrathin copper-thick printed circuit board |
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| CN107675218A (en) * | 2017-09-30 | 2018-02-09 | 广东骏亚电子科技股份有限公司 | A kind of acid electrochemical copper-plating technique |
| CN108601244A (en) * | 2018-04-19 | 2018-09-28 | 中国电子科技集团公司第十五研究所印制板与装联中心 | A kind of flex-rigid multiple-layer printed board hole metallization technology |
| US20210130970A1 (en) * | 2019-11-05 | 2021-05-06 | Macdermid Enthone Inc. | Single Step Electrolytic Method of Filling Through Holes in Printed Circuit Boards and Other Substrates |
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2021
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| CN102127781A (en) * | 2011-02-25 | 2011-07-20 | 湖南大学 | Electrochemical copper plating applicable to hole metallization of printed board |
| CN107675218A (en) * | 2017-09-30 | 2018-02-09 | 广东骏亚电子科技股份有限公司 | A kind of acid electrochemical copper-plating technique |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114457392A (en) * | 2022-02-28 | 2022-05-10 | 广东骏亚电子科技股份有限公司 | Novel electroplating method |
| CN114554702A (en) * | 2022-02-28 | 2022-05-27 | 广东骏亚电子科技股份有限公司 | Manufacturing method of ultrathin copper-thick printed circuit board |
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Application publication date: 20211001 |