CN107740073A - Reduced form accelerator for soft board electroless copper and its preparation method and application - Google Patents
Reduced form accelerator for soft board electroless copper and its preparation method and application Download PDFInfo
- Publication number
- CN107740073A CN107740073A CN201710737088.9A CN201710737088A CN107740073A CN 107740073 A CN107740073 A CN 107740073A CN 201710737088 A CN201710737088 A CN 201710737088A CN 107740073 A CN107740073 A CN 107740073A
- Authority
- CN
- China
- Prior art keywords
- soft board
- electroless copper
- reduced form
- accelerator
- board electroless
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Classifications
-
- 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
-
- 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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
- C23C18/2053—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment only one step pretreatment
- C23C18/206—Use of metal other than noble metals and tin, e.g. activation, sensitisation with metals
Abstract
The present invention provides a kind of reduced form accelerator for soft board electroless copper.The inorganic reducing agent and excess water that the reduced form accelerator for soft board electroless copper includes the sulfuric acid that content is 8%, content is 100g/L.The present invention also provides a kind of preparation method of the reduced form accelerator for soft board electroless copper, comprises the following steps：Part pure water is added in toward groove；Open stirring and filtration cycle, toward groove in be proportionally added into concentration be 98% sulfuric acid, cool down；It is to be cooled to being proportionally added into inorganic reducing agent, stirring and dissolving after normal temperature；Add surplus water.The present invention also provides a kind of application of the reduced form accelerator for soft board electroless copper.Provided by the present invention for the reduced form accelerator of soft board electroless copper, can effectively former tetravalent tin, avoid the formation of alkali formula stannate, palladium core is set fully to be exposed, the activity of colloid palladium is improved, also significantly improves the bond strength between chemical plating copper layer and base material, elimination is grown dim and copper knurl phenomenon.
Description
Technical field
The present invention relates to a kind of reduced form accelerator for soft board electroless copper and its preparation method and application.
Background technology
During soft board electroless copper, activator is rolled into a ball in the palladium base that substrate surface is adsorbed using palladium particle as core, in palladium
There are a large amount of tin ions and chlorion around core, wherein tin ion is present with bivalent form, in follow-up water-washing process, pole
The oxidizable colloidal compound for being tetravalence tin ion, forming extremely poorly soluble alkali formula stannate, palladium core is wrapped up, influences activation process
Progress, in soft board production process, easily cause to be unable to produce after nog plate, chemical plating and grow dim and copper knurl phenomenon.Traditional adds
Fast agent is all to remove part Bivalent Tin and chlorion with acid or alkaline solution, but is not removed but for tetravalent tin.
Solved the above problems therefore, it is necessary to provide a kind of new accelerator.
The content of the invention
The present invention provides a kind of reduced form accelerator for soft board electroless copper and its preparation method and application.
The reduced form accelerator for soft board electroless copper includes sulfuric acid, inorganic reducing agent and water, wherein sulfuric acid
Content is 8%, and the content of inorganic reducing agent is 100g/L, and surplus is water.
Preferably, one or more of the inorganic reducing agent in nickel salt, ammonium salt, tungstates, chloride.
The preparation method of the reduced form accelerator for soft board electroless copper, comprises the following steps：
(1) toward addition part pure water in groove；
(2) open stirring and filtration cycle, toward groove in be proportionally added into concentration be 98% sulfuric acid, cool down；
(3) it is to be cooled to being proportionally added into inorganic reducing agent, stirring and dissolving after normal temperature；
(4) surplus water is added, obtains the reduced form accelerator for soft board electroless copper.
A kind of accelerated method for soft board electroless copper, accelerated using the reduced form for soft board electroless copper
Agent, at normal temperatures, cylinder 5% is opened, Controlled acidity is 0.1~0.15N, and the acceleration time is 1.5~2.5 minutes.
Preferably, the accelerator is carried out under air-proof condition.
Preferably, 50~80 square meter plates are often produced and adds the reduced form accelerator 1L for being used for soft board electroless copper, often
Rise tank liquor 25 square meter plates of production and change cylinder.
Compared with correlation technique, provided by the present invention for the reduced form accelerator of soft board electroless copper, have has as follows
Beneficial effect：Before electroless copper, can effectively former tetravalent tin, avoid the formation of alkali formula stannate, palladium core is fully exposed,
So that palladium core has very strong and uniform activity.The activity of colloid palladium is not only increased, can be produced in the copper facing in future
Catalytic action, and the bond strength between chemical plating copper layer and base material is significantly improved, elimination is grown dim and copper knurl phenomenon.The opposing party
Face, the reduced form accelerator for soft board electroless copper, simple controllable, the application process facility of its preparation process are easy to raw
Production.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only it is the part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
All other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
The reduced form accelerator for soft board electroless copper includes sulfuric acid, inorganic reducing agent and water, wherein sulfuric acid
Content is 8%, and the content of inorganic reducing agent is 100g/L, and surplus is water.
Preferably, one or more of the inorganic reducing agent in nickel salt, ammonium salt, tungstates, chloride.
The preparation method of the reduced form accelerator for soft board electroless copper, comprises the following steps：
(1) toward addition part pure water in groove；
(2) open stirring and filtration cycle, toward groove in be proportionally added into concentration be 98% sulfuric acid, cool down；
(3) it is to be cooled to being proportionally added into inorganic reducing agent, stirring and dissolving after normal temperature；
(4) surplus water is added, obtains the reduced form accelerator for soft board electroless copper.
In soft board chemical-copper-plating process, needed before carrying out accelerator by following partial routine：
(1) presoak：The copper coated foil plate sample for having carried out roughening treatment early stage is taken, is containing Sn respectively2+Acid solution in
1~2min of pre-preg is carried out, is directly immersed in after taking-up in colloidal pd activation solution and carries out activation process；
(2) activate：3~5min is handled at ambient temperature, and copper coated foil plate should be constantly moved in processing procedure, makes activation
Liquid flows in hole, to form uniform Catalytic Layer on hole wall.Active cylinder uses Salt-Based Colloid Palladium：
PdCl2：1g/L、NaCl：250g/L、SnCl2：8g/l、HCl：40ml/L、Na2SnO3：2g/L, urea element：50g/L.
After the completion of activation process accelerator is carried out using the soft board electroless copper accelerated method：Using the reduced form
Accelerator, at normal temperatures, cylinder 5% is opened, Controlled acidity is 0.1~0.15N, and the acceleration time is 1.5~2.5 minutes.Need to illustrate
Be the accelerator processing when answer strict controlled concentration, temperature, time.Concentration is low, the time is short, the low then alkali formula stannic acid of temperature
Salt can not be completely dissolved, and palladium core can not expose, and heavy copper reaction can not be carried out；Excessive concentration, temperature is too high, time length, then not
Only alkali formula stannate dissolves, and also results in coming off for palladium core, equally causes heavy copper reaction to be smoothed out.
Preferably, the accelerator is carried out under air-proof condition, can use filtration cycle, often produces 50~80 square meters
Plate adds the reduced form accelerator 1L, and every liter of tank liquor produces 25 square meter plates and changes cylinder.
Detection accelerates tetravalence tin concentration in cylinder after the completion of reaction, it can be found that tetravalent tin has been completely removed in tank liquor, changes
Learn in the obtained finished product wiring board of copper facing, occur growing dim, the defect ware rate of copper knurl is greatly decreased.
, can by above-mentioned analysis it is known that reduced form accelerator provided by the present invention for soft board electroless copper
Tetravalent tin is reduced, avoids the formation of alkali formula stannate, chemical plating is effectively eliminated and grows dim and copper knurl scene；On the other hand, the use
In the reduced form accelerator of soft board electroless copper, simple controllable, the application process facility of its preparation process is readily produced.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (6)
- A kind of 1. reduced form accelerator for soft board electroless copper, it is characterised in that including sulfuric acid, inorganic reducing agent and water, Wherein the content of sulfuric acid is 8%, and the content of inorganic reducing agent is 100g/L, and surplus is water.
- 2. the reduced form accelerator according to claim 1 for soft board electroless copper, it is characterised in that it is described it is inorganic also One or more of the former agent in nickel salt, ammonium salt, tungstates, chloride.
- 3. a kind of preparation method of the reduced form accelerator for soft board electroless copper described in claim 1 or 2, its feature exist In comprising the following steps：(1) toward addition part pure water in groove；(2) open stirring and filtration cycle, toward groove in be proportionally added into concentration be 98% sulfuric acid, cool down；(3) it is to be cooled to being proportionally added into inorganic reducing agent, stirring and dissolving after normal temperature；(4) surplus water is added, obtains the reduced form accelerator for soft board electroless copper.
- A kind of 4. accelerated method for soft board electroless copper, it is characterised in that using described in claim 1 or 2 be used for it is soft The reduced form accelerator of plate chemical copper, at normal temperatures, open cylinder 5%, Controlled acidity is 0.1~0.15N, the acceleration time is 1.5~ 2.5 minute.
- 5. the accelerated method according to claim 4 for soft board electroless copper, it is characterised in that the accelerator exists Carried out under air-proof condition.
- 6. the accelerated method according to claim 4 for soft board electroless copper, it is characterised in that it is flat often to produce 50~80 Rice plate adds the reduced form accelerator 1L for soft board electroless copper, and every liter of tank liquor produces 25 square meter plates and changes cylinder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710737088.9A CN107740073A (en) | 2017-08-24 | 2017-08-24 | Reduced form accelerator for soft board electroless copper and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710737088.9A CN107740073A (en) | 2017-08-24 | 2017-08-24 | Reduced form accelerator for soft board electroless copper and its preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107740073A true CN107740073A (en) | 2018-02-27 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710737088.9A Pending CN107740073A (en) | 2017-08-24 | 2017-08-24 | Reduced form accelerator for soft board electroless copper and its preparation method and application |
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|---|---|
| CN (1) | CN107740073A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979709A (en) * | 2010-11-15 | 2011-02-23 | 深圳市成功科技有限公司 | Novel chemical copper plating method |
| CN102776494A (en) * | 2012-08-10 | 2012-11-14 | 杭州东方表面技术有限公司 | Peptizing solution for metalized modification on surface of macromolecule material |
| CN103556135A (en) * | 2013-11-07 | 2014-02-05 | 杭州东方表面技术有限公司 | Peptization solution for metalizing modification of plastic surface |
| CN105887053A (en) * | 2016-05-06 | 2016-08-24 | 广东利尔化学有限公司 | Chemical copper plating pretreatment process for printed wiring board |
-
2017
- 2017-08-24 CN CN201710737088.9A patent/CN107740073A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979709A (en) * | 2010-11-15 | 2011-02-23 | 深圳市成功科技有限公司 | Novel chemical copper plating method |
| CN102776494A (en) * | 2012-08-10 | 2012-11-14 | 杭州东方表面技术有限公司 | Peptizing solution for metalized modification on surface of macromolecule material |
| CN103556135A (en) * | 2013-11-07 | 2014-02-05 | 杭州东方表面技术有限公司 | Peptization solution for metalizing modification of plastic surface |
| CN105887053A (en) * | 2016-05-06 | 2016-08-24 | 广东利尔化学有限公司 | Chemical copper plating pretreatment process for printed wiring board |
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Application publication date: 20180227 |