CN103952687B - Plating penetration prevention method for chemical nickel-plating of printed circuit board - Google Patents
Plating penetration prevention method for chemical nickel-plating of printed circuit board Download PDFInfo
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- CN103952687B CN103952687B CN201410186519.3A CN201410186519A CN103952687B CN 103952687 B CN103952687 B CN 103952687B CN 201410186519 A CN201410186519 A CN 201410186519A CN 103952687 B CN103952687 B CN 103952687B
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Abstract
The invention relates to a plating penetration prevention method for chemical nickel-plating of a printed circuit board. The method is suitable for a chemical nickel-plating process for preparing the printed circuit board. The invention discloses the method comprising the step of adding a trivalent indium compound into a chemical nickel-plating solution, wherein the concentration of indium ions is 0.0005-0.0063g/L. The method disclosed by the invention can be used for preventing the plating penetration phenomenon generated in chemical nickel-plating of the printed circuit board (including a flexible board and a hard board), and ensuring the quality of the chemical nickel-plating process in manufacturing of the printed circuit board.
Description
Technical field
The present invention relates to chemical nickel plating field of surface treatment, specifically it is applied to the chemical plating nickel technology neck of printed wiring board
Domain.
Background technology
Copper is the most frequently used conductive material of current printed wiring board.Because the electric conductivity of copper family elements in all metals all
It is best, wherein silver holds pride of place, copper only takes second place.The base material of wiring board is insulating resin, and surface is thick with tiny copper
Circuit.Under room temperature, copper is stable in the in the air being dried, will be slowly empty but contact with the humid air containing carbon dioxide
Dioxygen oxidation corrosion in gas.Thus, it is ensured that the reliability of circuit, it is necessary for wiring board is surface-treated.Adopt at present
Method has on copper first chemical plating last layer nickel and then immersion plating last layer gold on nickel again, or chemical nickel plating porpezite
Deng because anticorrosion ability is good, being widely used in the manufacturing process of printed circuit board.Therefore, chemical nickel plating is current print
One important production link of circuit board fabrication processed.
Chemical nickel-plating liquid generally using nickel sulfate as nickel source, using the organic acid such as lactic acid or their salt as chelating agent.Also
Generally use sodium hypophosphite for former dose.Chemical nickel plating is carried out under catalytic condition.During chemical nickel plating, metallic nickel separates out
Meanwhile, it is accompanied by the releasing of hydrogen.
Develop towards high density, miniaturization, portable direction with electronic product, the wiring of circuit board is more and more closeer, oozes
Plating is one of problem that chemical nickel plating exists, and particularly in the case that wire spacing is little, between line, the activator of residual cannot be thorough
Bottom cleans up it is easier to this problem.The result of plating exactly can cause short-circuit between conductors, and product can only be scrapped.
In order to prevent the generation of plating, presently mainly by the cleaning repeatedly to plate face after activation：After being cleaned with dilute sulfuric acid,
Deionized water cleaning repeatedly, removes the activating solution of plate face residual again.But, on local plate face is adsorbed under certain apparent condition
Palladium be not easy to be eluted, and can not possibly be cleaned with long-time, substantial amounts of water in production procedure, the effect of cleaning has a fixed limit
System, also cannot guaranteed quality.Solve the rare report of method of this problem.Patent US2011/0051387 A1 be with alkali or wait from
The method of daughter roughening is removed palladium together with resin；Also remove it has been proposed that palladium is dissolved with nitric acid.But the acidity of nitric acid
Too strong, not only operational hazards, and substrate can be corroded, the operability of these methods is all difficult to realize on producing.
Solve the problems, such as chemical nickel plating plating currently without a good method.
Content of the invention
For present situation as described above, the invention aims to provide a kind of printed wiring board chemical nickel plating prevents plating
Method, the method can prevent from, to the chemical nickel plating of wiring board soft board and hardboard, plating occurs it is ensured that printed circuit board manufacture
Product quality.
Printed wiring board chemical nickel plating of the present invention prevent plating method, be chemical plating on the basis of chemical nickel-plating liquid
The compound of trivalent indium is added in nickel liquid.
Printed wiring board chemical nickel plating of the present invention prevent plating method, be trivalent indium compound be indium inorganic or
Organic compound and its combination in any.
Printed wiring board chemical nickel plating of the present invention prevent plating method, trivalent indium concentration be 0.0005g/L extremely
0.0063g/L.
Printed wiring board chemical nickel plating of the present invention prevent plating method, add the method for trivalent indium compound to have two kinds：
One kind is once plating occurs, and adds trivalent indium compound immediately toward in plating solution；Another kind is to add trivalent indium compound in advance
Enter in chemical nickel-plating liquid.
Printed wiring board chemical nickel plating of the present invention prevent plating method, its trivalent indium compound be indium sulfate, chlorine
Change indium, indium nitrate, indium acetate or perchloric acid indium.
The above printed wiring board chemical nickel plating prevent plating method, its trivalent indium compound be preferably indium sulfate,
Indium chloride, indium acetate.
The present invention by substantial amounts of experiment, it is found that：Once plating occurs, add the change of trivalent indium immediately toward in plating solution
Compound, can receive the effect got instant result.Its consumption is few, and using method is simple, can promptly make plating solution work become normal.Or
Person is the compound being previously added trivalent indium in the plating solution, allows plating phenomenon not occur.
Nickel chemical plating technology flow process during circuit board fabrication is as follows at present：
Before chemical nickel plating, wiring board is through pre-treatment.Technological process includes：
Oil removing → washing → microetch → washing → pickling twice twice → deionized water washing twice → preimpregnation → activation →
Leaching → deionized water washing twice → chemical nickel plating afterwards.The effect of each operation is described below：
1) oil removing, it is therefore an objective to remove the oxide on copper face, and makes copper face moistening.
2) wash twice.Purpose is to remove the degreasing fluid of residual on copper face.
3) microetch, it is therefore an objective to remove the oxide on copper face further, makes copper face micro-rough, thus increasing simultaneously
The adhesion of nickel coating.
4) wash twice.Purpose is to remove the micro-corrosion liquid of residual on copper face.
5) pickling, removes the micro-corrosion liquid of residual on copper face further, removes nascent oxide on copper face simultaneously.
6) deionized water washing twice.Purpose is to remove the pickle of residual on copper face.
7) preimpregnation, it is therefore an objective to maintain the acidity of activated bath, reduces the pollution to activated bath.
8) activation is it is therefore an objective to displace, in copper face, the catalyst that one layer of palladium reacts as chemical nickel plating.
9) soak afterwards it is therefore an objective to clean the activation liquid medicine of plate face residual.
10) deionized water washing twice is it is therefore an objective to clean the activating solution of plate face residual further.
Implement chemical nickel plating after described 10 pretreatment procedures, consistent with flow process with existing.
The concentration testing used indium compound is 2.000g/L, and compound method is as follows：
(1) preparation of sulphuric acid solution of indium：Weigh 1.0000 grams of anhydrous slufuric acid indium with ten thousand/balance, first burn in 100ml
In cup, deionized water dissolving, transfers to 500ml volumetric flask, last deionized water is diluted to 500ml, is configured to concentration and is
The sulphuric acid solution of indium of 2.000g/L (0.887g/L of indium containing trivalent).
The indiumchloride solution being (2) in the same manner, 2.000g/L (1.038g/L of indium containing trivalent) with same procedure compound concentration,
The indium acetate solution of 2.000g/L (0.787g/L of indium containing trivalent), 2.000g/L (0.720g/L of indium containing trivalent) pin acid indium molten
Liquid, the perchloric acid solution of indium of 2.000g/L (0.556g/L of indium containing trivalent).
In order to further illustrate the present invention, enumerate following examples, but do not limit the scope of the invention.For the ease of seeing
Examine plating phenomenon, this experiment adopts highdensity test board, and specially wire pitch is that 50 μm of plate does test board.
Embodiment 1.
Test piece is lamellar soft board, before entering chemical nickel plating groove, sequentially through normal pre-treating technology flow process as follows：
Oil removing → washing → microetch → washing → pickling twice twice → deionized water washing twice → preimpregnation → activation →
Leaching → deionized water washing twice afterwards
Chemical nickel-plating liquid is commodity soft board chemical nickel-plating liquid, pH=5.4.Plating solution volume is 1 liter, and beaker contains, and is placed in perseverance
In warm groove.
Plating temperature is 83 DEG C.
During plating, bubble amount is big, after 5 minutes, test piece is taken out and finds, plating is serious, is deposited on substrate
Metallic nickel part circuit connect.
With suction pipe, sulphuric acid solution of indium noted earlier for 0.6ml (trivalent indium concentration is 0.887g/L) is added dropwise to chemical plating at once
In nickel tank liquor, in plating solution, trivalent indium ion concentration is 0.0005g/L, stirs.Continue by above-mentioned normal pre-treating technology
Flow processing tests piece, lower groove plating, and going out hydrogen amount becomes normal.Plating was taken out after 5 minutes, and circuit silvery white is clear, does not have plating
Phenomenon, coating is completely covered.Continue plating to take out for 20 minutes, also do not find plating phenomenon.Often take out test piece twice to use
1:3 ammonia recall to 5.4 pH value, repeatable operation, and still silvery white is clear for circuit, no plating phenomenon.
Embodiment 2
Test piece is lamellar soft board, enters the pretreatment procedure being passed through before chemical nickel plating groove identical with embodiment 1.Change
Nickel-plating liquid is commodity soft board chemical nickel-plating liquid, pH=5.4.Plating solution volume is 1 liter, and beaker contains, and is placed in temperature chamber.
Plating temperature is 83 DEG C.
In implementing nickel process, bubble amount is big, after 5 minutes, test piece is taken out and finds, plating is serious, deposition
Metallic nickel on substrate connects part circuit.
With suction pipe, 7.1ml sulphuric acid solution of indium (trivalent indium concentration is 0.887g/L) is added dropwise to chemical nickel plating tank liquor at once
In, in plating solution, trivalent indium ion concentration is 0.0063g/L, stirs.Continue the pre-treating technology flow process as described in embodiment 1
Process test piece, lower groove plating, going out hydrogen amount becomes normal.Plating is taken out for 5 minutes, and circuit silvery white is clear, does not have the phenomenon of plating, plating
Layer is completely covered.Continue plating to take out for 20 minutes, also do not find plating phenomenon.Often take out test piece twice and use 1:3 ammonia handles
PH value recalls to 5.4, repeatable operation, and still silvery white is clear for circuit, no plating phenomenon.
Embodiment 3
Test piece is lamellar hardboard, enters the identical of the pretreatment procedure such as embodiment 1 passed through before chemical nickel plating groove.Change
Nickel-plating liquid is commodity hardboard chemical nickel-plating liquid, pH=4.8.Plating solution volume is 1 liter, and beaker contains, and is placed in temperature chamber.
Plating temperature is 83 DEG C.
In implementing nickel process, liberation of hydrogen is violent.After 5 minutes, test piece is taken out and find, plating is serious, is deposited on base
Metallic nickel on plate connects part circuit.
Immediately with suction pipe, indiumchloride solution noted earlier for 0.5ml (trivalent indium concentration is 1.038g/L) is added dropwise to chemical plating
In nickel tank liquor, in plating solution, trivalent indium ion concentration is 0.0005g/L, stirs.Continue the pre-treatment work as described in embodiment 1
Skill flow processing tests piece, lower groove plating, and going out hydrogen amount becomes normal.Plating is taken out for 5 minutes, and circuit silvery white is clear, does not have plating
Phenomenon, coating is completely covered.Take out after continuing plating 20 minutes, circuit silvery white is clear, does not have the phenomenon of plating, also will not leak
Plating.Often take out test piece twice and use 1:3 ammonia recall to 4.8 pH value, repeatable operation, and still silvery white is clear for circuit, no plating phenomenon.
Embodiment 4
Test piece is lamellar hardboard, enters the pretreatment procedure being passed through before chemical nickel plating groove also identical with embodiment 1.
Chemical nickel-plating liquid is commodity hardboard chemical nickel-plating liquid, pH=4.8.Plating solution volume is 1 liter, and beaker contains, and is placed in perseverance
In warm groove.
Plating temperature is 83 DEG C.
In implementing nickel process, liberation of hydrogen is violent.After 5 minutes, test piece is taken out and find, plating is serious, is deposited on base
Metallic nickel on plate connects part circuit.
Immediately with suction pipe, indium acetate solution noted earlier for 8.0ml (trivalent indium concentration is 0.787g/L) is added dropwise to chemical plating
In nickel tank liquor, in plating solution, trivalent indium ion concentration is 0.0063g/L, stirs.Continue the pre-treatment work as described in embodiment 1
Skill flow processing tests piece, lower groove plating, and gas output becomes normal.Plating is taken out for 25 minutes, and circuit silvery white is clear, do not have plating and
The situation of plating leakage.Often take out test piece twice and use 1:3 ammonia recall to 4.8 pH value, repeatable operation, and still silvery white is clear, no for circuit
Plating phenomenon.
Embodiment 5
Test piece is lamellar hardboard, enter before chemical nickel plating groove the pre-treating technology flow process passed through also with embodiment 1
Identical.
Chemical nickel-plating liquid is commodity hardboard chemical nickel-plating liquid, pH=4.8.Plating solution volume is 1 liter, and beaker contains, and is placed in perseverance
In warm groove.
Plating temperature is 83 DEG C.
In implementing nickel process, liberation of hydrogen is violent.After 5 minutes, test piece is taken out and find, plating is serious, is deposited on base
Metallic nickel on plate connects part circuit.
Immediately with suction pipe, indium acetate solution noted earlier for 3.0ml (trivalent indium concentration is 0.787g/L) is added dropwise to chemical plating
In nickel tank liquor, then, then with another suction pipe sulphuric acid solution of indium noted earlier for 3.0ml (trivalent indium concentration is 0.887g/L) Deca
Enter in chemical nickel plating tank liquor, in plating solution, trivalent indium ion concentration is 0.0050g/L, stirs.Continue to press aforesaid pre-treatment
Method process test piece, lower groove plating, gas output becomes normal.Plating is taken out for 25 minutes, and circuit silvery white is clear, does not have plating and leakage
The situation of plating.Often take out test piece twice and use 1:3 ammonia recall to 4.8 pH value, repeatable operation, and still silvery white is clear for circuit, no oozes
Plating phenomenon.
Embodiment 6
Test piece is lamellar hardboard, enter before chemical nickel plating groove the pre-treating technology flow process passed through also with embodiment 1
Identical.
1 liter of autogamy chemical nickel-plating liquid, composition and pH value are as follows：
With this nickel-plating liquid plating, in plating solution, trivalent indium ion concentration is 0.0044g/L, and plating temperature brings up to 90 DEG C.?
Implement liberation of hydrogen in nickel process normal.Plating was taken out after 20 minutes, and circuit silvery white is clear, does not have the phenomenon of plating, also will not
Plating leakage.Often take out test piece twice and use 1:3 ammonia recall to 5.3 pH value, repeatable operation, and still silvery white is clear for circuit, and no plating is existing
As.
Comparative example 1
Test piece is lamellar soft board, sequentially through normal pre-treating technology flow process as follows before entering chemical nickel plating groove：Oil removing →
The deionized water of washing → microetch → washing → pickling twice twice → twice washing → preimpregnation → activation → soak → go twice afterwards from
Sub- water washing.
Chemical nickel-plating liquid is commodity soft board chemical nickel-plating liquid, pH=5.4.Plating solution volume is 1 liter, and beaker contains, and is placed in perseverance
In warm groove.
Plating temperature is 83 DEG C.
During plating, bubbles volume is big.Test piece is taken out and finds, plating is serious, be deposited on metallic nickel on substrate portion
Separated time road connects.
Comparative example 2
Test piece is lamellar hardboard, enters the phase of the pre-treating technology flow process passed through before chemical nickel plating groove and comparative example 1
With.
Chemical nickel-plating liquid is commodity hardboard chemical nickel-plating liquid, pH=4.8.Plating solution volume is 1 liter, and beaker contains, and is placed in perseverance
In warm groove.
Plating temperature is 83 DEG C.
In implementing nickel process, bubbles volume is big.Test piece is taken out and finds, plating is serious, is deposited on the gold on substrate
Belong to nickel part circuit is connected.
Comparative example 3
Test piece is lamellar soft board, enter before chemical nickel plating groove the pre-treating technology flow process passed through also with comparative example 1
Identical.
1 liter of autogamy chemical nickel-plating liquid, is added without indium, and composition and pH value are as follows：
With this nickel-plating liquid plating.Plating temperature is 90 DEG C.
During plating, bubbles volume is big.Test piece is taken out and finds, plating is serious, be deposited on metallic nickel on substrate portion
Separated time road connects.
Claims (5)
1. printed wiring board chemical nickel plating prevent plating method, including chemical nickel-plating liquid, it is characterized in that in chemical nickel-plating liquid plus
Enter the compound of trivalent indium, trivalent indium concentration is 0.0005g/L to 0.0063g/L.
2. according to claim 1 printed wiring board chemical nickel plating prevent plating method, it is characterized in that trivalent indium compound
For the inorganic of indium or organic compound and its combination in any.
3. according to claim 1 printed wiring board chemical nickel plating prevent plating method, it is characterized in that into trivalent indium chemical combination
The method of thing has two kinds：One kind is once plating occurs, and adds trivalent indium compound immediately toward in plating solution；Another kind is by trivalent
Indium compound is pre-added in chemical nickel-plating liquid.
4. according to claim 2 printed wiring board chemical nickel plating prevent plating method, it is characterized in that trivalent indium compound
For indium sulfate, indium chloride, indium nitrate, indium acetate or perchloric acid indium.
5. according to claim 4 printed wiring board chemical nickel plating prevent plating method, it is characterized in that trivalent indium compound
It is preferably indium sulfate, indium chloride, indium acetate.
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| CN201410186519.3A CN103952687B (en) | 2014-05-05 | 2014-05-05 | Plating penetration prevention method for chemical nickel-plating of printed circuit board |
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| CN201410186519.3A CN103952687B (en) | 2014-05-05 | 2014-05-05 | Plating penetration prevention method for chemical nickel-plating of printed circuit board |
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| EP3026143A1 (en) * | 2014-11-26 | 2016-06-01 | ATOTECH Deutschland GmbH | Plating bath and method for electroless deposition of nickel layers |
| CN109852951A (en) * | 2019-04-04 | 2019-06-07 | 深圳市互连微电子材料有限公司 | A kind of chemistry NiPdAu production line and production technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013182489A2 (en) * | 2012-06-04 | 2013-12-12 | Atotech Deutschland Gmbh | Plating bath for electroless deposition of nickel layers |
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| US4816070A (en) * | 1985-08-29 | 1989-03-28 | Techo Instruments Investments Ltd. | Use of immersion tin and alloys as a bonding medium for multilayer circuits |
| JP2005350728A (en) * | 2004-06-10 | 2005-12-22 | Toyo Kohan Co Ltd | Electroless nickel plating bath, substrate for magnetic disk and magnetic disk |
| JP4998704B2 (en) * | 2007-01-22 | 2012-08-15 | 上村工業株式会社 | Method for forming substituted tin alloy plating film, substituted tin alloy plating bath, and method for maintaining plating performance |
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| WO2013182489A2 (en) * | 2012-06-04 | 2013-12-12 | Atotech Deutschland Gmbh | Plating bath for electroless deposition of nickel layers |
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