CN114507886A - Hole-filling electroplating method - Google Patents
Hole-filling electroplating method Download PDFInfo
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- CN114507886A CN114507886A CN202210323395.3A CN202210323395A CN114507886A CN 114507886 A CN114507886 A CN 114507886A CN 202210323395 A CN202210323395 A CN 202210323395A CN 114507886 A CN114507886 A CN 114507886A
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- electroplating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
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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
Abstract
The invention discloses a hole-filling electroplating method, which comprises the following steps: adding an accelerator to the first plating solution to form a pre-dip; wherein the content of the accelerator in the pre-immersion liquid is 100-120 mg/L; immersing the production plate with the metallized blind holes into pre-immersion liquid so as to enable the metallized blind holes to be fully immersed by the pre-immersion liquid; then, carrying out hole filling electroplating on the production board by adopting a second electroplating solution containing an accelerator and an inhibitor so as to electroplate and fill up the metallized blind holes; wherein, the content of the accelerator in the second electroplating solution is 6-12mg/L, and the content of the inhibitor is 300-1600 mg/L. According to the invention, through optimizing the process flow, a mode of presoaking the high-concentration accelerator is adopted, so that a leveling agent is not required to be added into the electroplating solution, the mutual influence of multiple addition components is reduced by adopting two additives, the presoaking accelerator is firstly distributed in the blind hole as required, the control difficulty is reduced, the quality of hole filling is improved, and the cost is reduced.
Description
Technical Field
The invention relates to the technical field of printed circuit board manufacturing, in particular to a hole filling electroplating method.
Background
The micro blind hole filling electroplating technology can realize one-time completion of copper plating filling and electrical interconnection, and because the conductivity and the heat dissipation of the copper material are superior to those of conductive adhesive and resin material, the electrical performance can be improved, and the connection reliability is improved, so the micro blind hole filling electroplating technology becomes an important method for realizing interconnection of printed circuit boards at present. In order to ensure the reliability of circuit connection, the blind holes need to be completely filled with electroplated copper, and the hole filling rate of the blind holes and the thickness of copper after electroplating in the process are important indexes for measuring the performance of the acid copper sulfate plating solution.
Generally, when blind vias are filled with copper by electroplating in an acid copper plating solution without additives, the blind vias cannot be filled because the current density at the bottom of the vias is relatively low and the copper deposition speed is relatively slow. When the plating solution contains chloride ions, an accelerator, an inhibitor and a leveling agent, the perfect filling of the blind hole, also called Superfilling, can be finally realized only by changing the distribution difference of the current density at the bottom of the blind hole and the surface of the panel through the interaction among the additives.
The organic additives used in the blind micro-hole filling electroplating process mainly comprise three types: accelerators, suppressors and levelers.
Accelerators (also called brightening agents), usually small molecular sulfur-containing compounds, are used to accelerate the reduction of copper ions in the blind via holes and simultaneously form new copper plating nuclei to make the copper layer structure finer, mainly including SPS (sodium polydithio dipropyl sulfonate) and MPS (sodium 3-thiopropane sulfonate).
The inhibitor (also called carrier) is mostly polyether compound, which is easy to be adsorbed on the active point of crystal grain growth, and can increase electrochemical reaction resistance and enhance electrochemical polarization, thereby achieving the effects of refining crystal grain and inhibiting plate surface coating growth, and commonly used are polyethylene glycol, aromatic polyoxyethylene ether, nonyl phenol and ethylene oxide reactant, etc.
The leveling agent is generally a nitrogen-containing heterocyclic compound which is easily adsorbed in a raised area of the plate surface, namely a high current density area, so that the electroplating speed at the position is slowed down, the deposition of copper in the high current density area is inhibited, and the adsorption in a sunken position of the plate surface and a micro blind hole is less, so that the copper deposition at the position is not influenced, and the effect of leveling the plate surface is achieved.
The three additives play different roles in electroplating and are matched with each other, and the micro blind hole can be well filled only when the additives reach a proper proportion.
However, the above electroplating process has the following problems:
1. three or more types of additives are adopted, and the control of the components of each additive is strict and the control difficulty is very high.
2. Leveling agent is expensive, accelerator is consumed more, and hole-filling electroplating cost is higher.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a hole filling electroplating method, which adopts a mode of presoaking a high-concentration accelerator, so that a leveling agent is not required to be added into electroplating liquid, two additives are adopted to reduce the mutual influence of various addition components, the presoaking accelerator is firstly distributed in a blind hole, the control difficulty is reduced, the hole filling quality is improved, and the cost is reduced.
In a first aspect, to solve the above technical problem, the present invention provides a method for via filling electroplating, comprising the following steps:
s1, adding an accelerator to the first plating liquid to form a pre-dip; wherein the content of the accelerator in the pre-immersion liquid is 100-120 mg/L;
s2, immersing the production board with the metallized blind holes into a pre-immersion liquid so that the metallized blind holes are fully immersed by the pre-immersion liquid;
s3, performing hole filling electroplating on the production board by using a second electroplating solution containing an accelerator and an inhibitor to electroplate and fill up the metallized blind holes; wherein, the content of the accelerator in the second electroplating solution is 6-12mg/L, and the content of the inhibitor is 300-1600 mg/L.
Further, the first electroplating solution and the second electroplating solution both comprise sulfuric acid, copper sulfate pentahydrate and chloride ions; wherein the content of the sulfuric acid is 60-80g/L, the content of the blue copperas is 200-250g/L, and the content of the chloride ion is 50-80 ppm.
Further, in step S2, after the production board is immersed in the pre-dip, ultrasonic vibration is applied to the pre-dip to remove air bubbles in the metallized blind holes.
Further, in step S2, the time of ultrasonic vibration is 10-40S.
Further, in step S2, the current density during the hole-filling electroplating is 0.8-1.5ASD, and the electroplating time is 1.5-2 h.
In a second aspect, the present invention also provides a method of via-filling electroplating, comprising the steps of:
s1, adding an accelerator into the pure water to form a pre-immersion liquid; wherein the content of the accelerator in the pre-immersion liquid is 30-100 mg/L;
s2, immersing the production board with the metallized blind holes into a pre-immersion liquid so that the metallized blind holes are fully immersed by the pre-immersion liquid;
s3, drying the production board;
s4, performing hole filling electroplating on the production board by using electroplating solution containing an accelerator and an inhibitor to fill and level up the metallized blind holes by electroplating; wherein, the content of the accelerator in the electroplating solution is 6-12mg/L, and the content of the inhibitor is 300-1600 mg/L.
Further, in step S2, after the production board is immersed in the pre-dip, ultrasonic vibration is applied to the pre-dip to remove air bubbles in the metallized blind holes.
Further, in step S2, the time of ultrasonic vibration is 10-40S.
Further, in step S4, the current density during the hole-filling electroplating is 0.8-1.5ASD, and the electroplating time is 1.5-2 h.
Further, in step S4, the electroplating solution includes sulfuric acid, copper sulfate pentahydrate, and chloride ions; wherein the content of the sulfuric acid is 60-80g/L, the content of the blue copperas is 200-250g/L, and the content of the chloride ion is 50-80 ppm.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, through optimizing the process flow, the pre-immersion liquid containing the high-concentration accelerator is used for pre-immersing the blind hole before electroplating, so that the high-concentration accelerator is fully adsorbed in the blind hole, the electroplating copper in the blind hole can be rapidly grown by adding a small amount of accelerator in the electroplating solution because the high-concentration accelerator exists in the blind hole, and the high-concentration inhibitor is added in the electroplating solution during hole-filling electroplating to inhibit the growth of the electroplating copper on the surface; in addition, when the hole filling electroplating is carried out, the accelerator on the surface of the production board can be washed away by liquid flow, so that the accelerator generates concentration difference between the board surface and the blind hole and is matched with a high-concentration inhibitor, and a leveling agent is not required to be added to be matched with the accelerator and the inhibitor during the electroplating, so that the effect of quickly filling the hole can be realized, the hole filling quality is improved, and the growth of surface electroplated copper is effectively inhibited; in the method, only two additives are adopted in the electroplating solution, so that the mutual influence of various addition components is reduced compared with a mode of adding three additives in the prior art, the pre-dipping accelerator is firstly distributed in the blind hole to form the required distribution, the control difficulty is also reduced, the hole filling quality is improved, and the cost is reduced.
The mode of presoaking the high-concentration accelerator is adopted, so that leveling agent is not required to be added into electroplating solution, the mutual influence of multiple added components is reduced by adopting two additives, the presoaking accelerator is firstly distributed in the blind hole, the control difficulty is reduced, the hole filling quality is improved, and the cost is reduced
Firstly, electroplating is carried out by adopting an electroplating solution of a matt agent, copper ion deposition can continue epitaxial growth along the crystallization of a copper substrate to form a pure copper crystallization, so that a first copper plating layer without impurities is formed on the copper substrate by electroplating, and then a second copper plating layer which is smooth and bright is formed on the first copper plating layer by adopting the electroplating solution containing the gloss agent by electroplating, so that the problems of electroplating burrs and pinholes are avoided; in addition, the plating efficiency of the plating solution of the matt agent is much higher than that of the plating solution of the lustrous agent, so that the method can effectively improve the plating efficiency and the production efficiency.
Drawings
FIG. 1 is a partial SEM image of a production board after filling a plurality of blind holes by electroplating in example 1;
FIG. 2 is a partial SEM image of a plated single blind hole in a production board of example 1;
FIG. 3 is a partial SEM image of a production board plated with a plurality of blind vias as in example 2.
Detailed Description
In order to more fully understand the technical contents of the present invention, the technical solutions of the present invention will be further described and illustrated with reference to specific embodiments.
Example 1
The method for hole-filling electroplating in this embodiment sequentially includes the following steps:
a. adding an accelerator to the first plating solution to form a pre-dip; wherein the content of the accelerator in the pre-immersion liquid is 100mg/L, and the accelerator is preferably sodium polydithio dipropyl sulfonate.
Specifically, the first electroplating solution comprises sulfuric acid, copper sulfate pentahydrate and chloride ions; wherein the content of sulfuric acid is 75g/L, the content of blue vitriol is 200g/L, and the content of chloride ion is 55 ppm.
b. And (3) immersing the production board with the metallized blind holes into the pre-immersion liquid so that the metallized blind holes are fully immersed by the pre-immersion liquid, and thus, high-concentration accelerators are adsorbed in the board surface and the metallized blind holes, and the blind holes are conveniently plated and filled in the later period.
After the production plate is immersed in the pre-immersion liquid, ultrasonic vibration is applied to the pre-immersion liquid to remove air bubbles in the metallized blind hole in a vibration mode, so that the metallized blind hole is fully immersed by the pre-immersion liquid; the time of ultrasonic vibration is controlled to be 10-40 s.
c. Because the pre-immersion liquid also adopts the electroplating liquid as the main liquid, the hole filling electroplating treatment can be directly carried out without drying the board after the board is pre-immersed; then, a second electroplating solution containing an accelerator and an inhibitor is used for hole filling electroplating on the production board to fill and level up the metallized blind holes (as shown in figures 1 and 2), the current density during electroplating is 1.0ASD, and the electroplating time is 2 h; wherein, the content of the accelerator in the second electroplating solution is 6mg/L, the content of the inhibitor in the second electroplating solution is 450mg/L, the accelerator is preferably sodium polydithio dipropyl sulfonate, and the inhibitor is preferably polyethylene glycol.
Wherein the second electroplating solution comprises sulfuric acid, copper sulfate pentahydrate and chloride ions; wherein the content of sulfuric acid is 75g/L, the content of blue vitriol is 200g/L, and the content of chloride ion is 55 ppm.
In this embodiment, the production board is a multi-layer board obtained by laminating copper foils on the outer layers of inner core boards through prepregs, and before step a, the multi-layer board is subjected to drilling, copper deposition and full-board electroplating in sequence, and the steps are as follows:
(1) cutting: and cutting a core board, a prepreg and a copper base material according to the size of the jointed board of 520mm multiplied by 620mm, wherein the thickness of the core board is 0.5mm, and the thickness of copper layers on two surfaces of the core board is 0.5 oz.
(2) Inner layer circuit manufacturing (negative film process): transferring the inner layer pattern, coating a photosensitive film with a vertical coating machine, controlling the film thickness of the photosensitive film to be 8 μm, completing the exposure of the inner layer circuit by using a full-automatic exposure machine and 5-6 exposure rulers (21 exposure rulers), and forming the inner layer circuit pattern after development; etching the inner layer, etching the exposed and developed core board to form an inner layer circuit, wherein the line width of the inner layer is measured to be 3 mil; and (4) inner layer AOI, and then, detecting defects of an inner layer circuit, such as open short circuit, circuit notch, circuit pinhole and the like, and performing defect scrapping treatment, wherein a defect-free product is discharged to the next flow.
(3) And (3) laminating: and (3) brown-oxidizing at the brown-oxidizing speed according to the thickness of the copper of the bottom copper, sequentially laminating the core plate, the prepreg and the copper foil according to the requirement, and then pressing the laminated plate by selecting proper lamination conditions according to the Tg of the plate to form the production plate.
(4) Drilling: according to the existing drilling technology, drilling machining is carried out on a production plate according to design requirements so as to drill blind holes needing electroplating filling.
(5) Copper deposition: and (3) depositing a layer of thin copper on the plate surface and the hole wall by using a chemical copper plating method so as to form a metalized blind hole in the blind hole, wherein the thickness of the deposited copper in the hole is 0.5 mu m in a backlight test level of 10.
(6) Electroplating the whole plate: the hole copper and the plate surface copper layer are thickened through the whole plate electroplating process,
in other embodiments, the sulfuric acid content in the first and second electroplating solutions may be 60-80g/L, the copper sulfate pentahydrate content may be 200-250g/L, and the chloride ion content may be 50-80 ppm.
In other embodiments, the content of the accelerator in the pre-immersion liquid can also be 100-120 mg/L.
In other embodiments, the accelerator is present in the second plating solution in an amount of 6-12mg/L and the suppressor is present in an amount of 300-1600 mg/L.
Example 2
The method for hole-filling electroplating in this embodiment sequentially includes the following steps:
a. adding an accelerator into pure water to form a pre-immersion liquid; wherein, the content of the accelerator in the pre-immersion liquid is 33mg/L, and the accelerator is preferably sodium polydithio dipropyl sulfonate.
b. And (3) immersing the production board with the metallized blind holes into the pre-immersion liquid so that the metallized blind holes are fully immersed by the pre-immersion liquid, and thus, high-concentration accelerators are adsorbed in the board surface and the metallized blind holes, and the blind holes are conveniently plated and filled in the later period.
After the production plate is immersed in the pre-immersion liquid, ultrasonic vibration is applied to the pre-immersion liquid to remove air bubbles in the metallized blind hole in a vibration mode, so that the metallized blind hole is fully immersed by the pre-immersion liquid; the time of ultrasonic vibration is controlled to be 10-40 s.
c. Because the pre-immersion liquid adopts the pure water as main liquid, for avoiding the pure water to exert an influence to the plating solution when the back spot is electroplated, need dry the production board earlier to get rid of the pure water on the board, and the accelerator can be attached to in face of the board and the metallization blind hole.
d. Then, the production board is subjected to hole filling electroplating by using electroplating solution containing an accelerator and an inhibitor so as to fill and level up the metallized blind holes (as shown in figure 3) in an electroplating way, the current density during electroplating is 1.0ASD, and the electroplating time is 2 h; wherein, the content of the accelerator in the electroplating solution is 6mg/L, the content of the inhibitor in the electroplating solution is 450mg/L, the accelerator is preferably sodium polydithio dipropyl sulfonate, and the inhibitor is preferably polyethylene glycol.
Wherein the electroplating solution comprises sulfuric acid, blue vitriol and chloride ions; wherein the content of sulfuric acid is 75g/L, the content of blue vitriol is 200g/L, and the content of chloride ion is 55 ppm.
In this embodiment, the production board is a multi-layer board obtained by laminating copper foils on the outer layers of inner core boards through prepregs, and before step a, the multi-layer board is subjected to drilling, copper deposition and full-board electroplating in sequence, and the steps are as follows:
(1) cutting: and cutting a core board, a prepreg and a copper base material according to the size of the jointed board of 520mm multiplied by 620mm, wherein the thickness of the core board is 0.5mm, and the thickness of copper layers on two surfaces of the core board is 0.5 oz.
(2) Inner layer circuit manufacturing (negative film process): transferring the inner layer pattern, coating a photosensitive film with a vertical coating machine, controlling the film thickness of the photosensitive film to be 8 μm, completing the exposure of the inner layer circuit by using a full-automatic exposure machine and 5-6 exposure rulers (21 exposure rulers), and forming the inner layer circuit pattern after development; etching the inner layer, etching the exposed and developed core board to form an inner layer circuit, wherein the line width of the inner layer is measured to be 3 mil; and (4) inner layer AOI, and then, detecting defects of an inner layer circuit, such as open short circuit, circuit notch, circuit pinhole and the like, and performing defect scrapping treatment, wherein a defect-free product is discharged to the next flow.
(3) And (3) laminating: and (3) brown-oxidizing at the brown-oxidizing speed according to the thickness of the copper of the bottom copper, sequentially laminating the core plate, the prepreg and the copper foil according to the requirement, and then pressing the laminated plate by selecting proper lamination conditions according to the Tg of the plate to form the production plate.
(4) Drilling: according to the existing drilling technology, drilling machining is carried out on a production plate according to design requirements so as to drill blind holes needing electroplating filling.
(5) Copper deposition: and (3) depositing a layer of thin copper on the plate surface and the hole wall by using a chemical copper plating method so as to form a metalized blind hole in the blind hole, wherein the thickness of the deposited copper in the hole is 0.5 mu m in a backlight test level of 10.
(6) Electroplating the whole plate: the hole copper and the plate surface copper layer are thickened through the whole plate electroplating process,
in other embodiments, the content of sulfuric acid in the electroplating solution can be 60-80g/L, the content of copper sulfate pentahydrate can be 200-250g/L, and the content of chloride ion can be 50-80 ppm.
In other embodiments, the accelerator may be present in the pre-dip in an amount of 30-100 mg/L.
In other embodiments, the accelerator is present in the plating solution at 6-12mg/L and the suppressor is present at 300-1600 mg/L.
The technical solutions provided by the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained herein by using specific examples, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, for a person skilled in the art, according to the embodiments of the present invention, there may be variations in the specific implementation manners and application ranges, and in summary, the content of the present description should not be construed as a limitation to the present invention.
Claims (10)
1. A method of via-filling electroplating, comprising the steps of:
s1, adding an accelerator to the first plating liquid to form a pre-dip; wherein the content of the accelerator in the pre-immersion liquid is 100-120 mg/L;
s2, immersing the production board with the metallized blind holes into a pre-immersion liquid so that the metallized blind holes are fully immersed by the pre-immersion liquid;
s3, performing hole filling electroplating on the production board by using a second electroplating solution containing an accelerator and an inhibitor to electroplate and fill up the metallized blind holes; wherein, the content of the accelerator in the second electroplating solution is 6-12mg/L, and the content of the inhibitor is 300-1600 mg/L.
2. The method of via-filling electroplating according to claim 1, wherein the first and second electroplating solutions each comprise sulfuric acid, copper sulfate pentahydrate, and chloride ions; wherein the content of the sulfuric acid is 60-80g/L, the content of the blue copperas is 200-250g/L, and the content of the chloride ion is 50-80 ppm.
3. The method of via-filling electroplating according to claim 1, wherein in step S2, after the production board is immersed in the pre-dip solution, ultrasonic vibration is applied to the pre-dip solution to remove air bubbles in the metallized blind via.
4. The method of hole-filling electroplating according to claim 3, wherein in step S2, the time of ultrasonic vibration is 10-40S.
5. The method of via-filling electroplating according to claim 1, wherein in step S2, the current density during via-filling electroplating is 0.8-1.5ASD, and the electroplating time is 1.5-2 h.
6. A method of via-filling electroplating, comprising the steps of:
s1, adding an accelerator into pure water to form a pre-immersion liquid; wherein the content of the accelerator in the pre-immersion liquid is 30-100 mg/L;
s2, immersing the production board with the metallized blind holes into a pre-immersion liquid so that the metallized blind holes are fully immersed by the pre-immersion liquid;
s3, drying the production board;
s4, performing hole filling electroplating on the production board by using electroplating solution containing an accelerator and an inhibitor to fill and level up the metallized blind holes by electroplating; wherein, the content of the accelerator in the electroplating solution is 6-12mg/L, and the content of the inhibitor is 300-1600 mg/L.
7. The method of via-filling electroplating according to claim 6, wherein in step S2, after the production board is immersed in the pre-dip solution, ultrasonic vibration is applied to the pre-dip solution to remove air bubbles in the metallized blind holes.
8. The method of via-filling electroplating according to claim 7, wherein the ultrasonic vibration is performed for 10 to 40 seconds in step S2.
9. The method of via-filling electroplating according to claim 6, wherein in step S4, the current density during via-filling electroplating is 0.8-1.5ASD, and the electroplating time is 1.5-2 h.
10. The method of hole-filling electroplating according to claim 6, wherein in step S4, the electroplating solution comprises sulfuric acid, copper sulfate pentahydrate and chloride ions; wherein the content of the sulfuric acid is 60-80g/L, the content of the blue copperas is 200-250g/L, and the content of the chloride ion is 50-80 ppm.
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| JP2003129273A (en) * | 2001-10-29 | 2003-05-08 | Applied Materials Inc | Electroplating process |
| US20120175264A1 (en) * | 2009-09-28 | 2012-07-12 | Basf Se | Wafer pretreatment for copper electroplating |
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| JP2013044007A (en) * | 2011-08-23 | 2013-03-04 | Ishihara Chem Co Ltd | Method of filling copper, and electronic component using the same |
| CN108601245A (en) * | 2018-05-30 | 2018-09-28 | 江门崇达电路技术有限公司 | A kind of electro-plating method of HDI plates high thickness to diameter ratio blind hole |
| CN112437558A (en) * | 2020-11-16 | 2021-03-02 | 淮安特创科技有限公司 | Blind hole electroplating hole filling method and circuit board |
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2022
- 2022-03-29 CN CN202210323395.3A patent/CN114507886A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003129273A (en) * | 2001-10-29 | 2003-05-08 | Applied Materials Inc | Electroplating process |
| US20120175264A1 (en) * | 2009-09-28 | 2012-07-12 | Basf Se | Wafer pretreatment for copper electroplating |
| JP2013044007A (en) * | 2011-08-23 | 2013-03-04 | Ishihara Chem Co Ltd | Method of filling copper, and electronic component using the same |
| CN102912395A (en) * | 2012-11-15 | 2013-02-06 | 苏州正信电子科技有限公司 | Method for filling blind-buried holes through electro-coppering |
| CN108601245A (en) * | 2018-05-30 | 2018-09-28 | 江门崇达电路技术有限公司 | A kind of electro-plating method of HDI plates high thickness to diameter ratio blind hole |
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