CN102877044A - Method for producing environment-friendly lead-free electroless nickel immersion gold - Google Patents
Method for producing environment-friendly lead-free electroless nickel immersion gold Download PDFInfo
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- CN102877044A CN102877044A CN2012103389417A CN201210338941A CN102877044A CN 102877044 A CN102877044 A CN 102877044A CN 2012103389417 A CN2012103389417 A CN 2012103389417A CN 201210338941 A CN201210338941 A CN 201210338941A CN 102877044 A CN102877044 A CN 102877044A
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Abstract
The invention provides a method for producing environment-friendly lead-free electroless nickel immersion gold. The method comprises the following steps of: etching a line, and treating a circuit board by using solder mask ink; performing pretreatment, namely polishing and brushing or blasting sand; placing the circuit board in an oil removal trough and treating for 5 minutes; washing by using tap water and conveying into a microetching trough for 2 minutes; washing by using deionized water, and feeding into a preimpregnation trough for 1 minute; directly feeding into an activation trough and treating for 1 minute; washing by using the deionized water, and treating in chemical nickel at the temperature of 80 DEG C for 20 minutes; and washing by using the deionized water, and treating in immersion gold which is prepared from 10 percent KOZO 806 and citric acid gold with density of 2g/L. By the method, the technical problem that the conventional production method is not environment-friendly can be solved; lead in the chemical nickel is replaced and is totally environment-friendly; and the condition that tin is not soldered well can be avoided. The toxic potassium aurous cyanide in the immersion gold is replaced, and the immersion gold is totally environment-friendly; and a solution is stable and is prevented from being decomposed.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of production method of environment-friendly type lead-free chemical nickel and gold.
Background technology
The production method of existing nickel gold is a small amount of palladium of copper face displacement at circuit, redox mode deposits the 4 micron thick ni-p alloy coatings (phosphorus is that the eutectoid of chemical nickel byproduct of reaction is in nickel dam) that one deck phosphorus content is about 7-10% as catalytic core utilizes take palladium in the chemical nickel groove to make circuit, replaces the gold layer of 0.07 micron of one deck with the method for displacement at this ni-p alloy coating.Chemical nickel and gold is surface treatment powerful in the wiring board, and it can be used in as in Mobile phone key panel, computer memory bar etc. the electronic product, and it not only can be done soldering part but also can do the current lead-through point of contact simultaneously.But in fact it is a kind of technique of not environmental protection.Referenced patent is as seen: Chinese patent: can obtain the chemical plating nickel-phosphorus alloy solution of high solderability coating, publication number 102011107A, open date 2011-04-13.At first be to contain lead in the chemical nickel plating bath in the chemical nickel and gold, lead effect in chemical nickel is obvious.Chemical nickel belongs to self-catalyzed reaction, and it is to utilize deposition nickle atom catalytic chemistry nickel self well to deposit nickle atom again.The characteristics of this class reaction are that the reaction meeting is more and more violent, until chemical nickel can not use because reacting acutely, because adding a bit the stablizer of inhibited reaction.Lead is one of satisfactory stability agent, and the content in plating bath is generally 0.2-1.5ppm.Plating bath plates more for a long time, and plumbous addition is just more.These plumbous meetings are along with the deposition of nickel in the tank liquor, and eutectoid is in ni-p alloy coating, and content is 300-500ppm approximately.Nickel dam essence is nickel phosphorus lead alloy layer.In the process of wiring board chemical nickel and gold, industry does not change this fact of nickel phosphorus lead alloy layer.Because chemical nickel and gold not only is used for doing the current lead-through point of contact, also to be used for scolding tin.And lead remains best soldering tin material in the prior art.Bad in order to reduce scolding tin, people do not remove to change interior these a small amount of lead of nickel dam in the chemical nickel and gold.And in chemical gold, people's normal operation be to contain the potassium cyanaurite of severe toxicity as the raw material of nickel gold displacement.Prussiate electroless plating have the height stability, so the industry life-time service its as industrial raw material.
Therefore be necessary to provide a kind of method to reach for the lead in the chemical nickel; Adopt a kind of nontoxic and stable golden salt to reach for the potassium cyanaurite in the chemical gold, make chemical nickel and gold become real environmentfriendly products.
Summary of the invention
Have the technical problem of not environmental protection in order to solve existing production method, the present invention has adopted a kind of production method of environment-friendly type lead-free chemical nickel and gold.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of production method of environment-friendly type lead-free chemical nickel and gold is characterized in that: the priority of described method is in proper order: pre-treatment, oil removing, microetch, preimpregnation, activation, chemical nickel, chemistry gold; Specifically may further comprise the steps:
1) the good circuit of etching is handled wiring board well through anti-solder ink, passes through the pre-treatments such as polish-brush or sandblast again, forms relatively clean wiring board copper face;
2) this wiring board is placed rinse bath, further remove copper face oxidation and greasy dirt;
3) deliver to the microetch groove with the tap water cleaning, with surperficial little alligatoring of copper;
4) with washed with de-ionized water, enter preimpregnation and activated bath, use the upper a small amount of palladium of copper face displacement;
5) with washed with de-ionized water, enter chemical nickel, the about ni-p alloy coating of 4 micron thick of 7-10% take palladium as catalytic core autocatalysis one deck phosphorus content;
6) with washed with de-ionized water, enter chemical golden groove, replace the approximately gold layer of 0.07 micron thick of one deck with the method for displacement, be used for scolding tin and prevent oxidation.
As further improvement in the technical proposal, the compound method of each reactive tank is as follows in the described step 2:
1) degreasing tank is joined groove processing 5 minutes in 45 ℃ of lower KOZO 801 with 10%;
2) the microetch groove is joined groove processing 2 minutes with the Sodium Persulfate of every liter of 100 gram and 20 milliliters every liter the vitriol oil under 27 ℃;
3) pre-immersion trough is joined groove processing 1 minute with 0.5% vitriol oil under room temperature;
4) activated bath is joined groove processing 1 minute in 27 ℃ of lower KOZO 804 with 8%;
5) chemical nickel groove liquid composite is in 80 ℃ of lower processing 20 minutes;
6) chemical golden groove is joined groove processing 10 minutes in 88 ℃ of lower KOZO 806 and 2 citric acid golds that restrain every liter with 10%.
Implement the present invention: a kind of production method of environment-friendly type lead-free chemical nickel and gold has following beneficial effect:
1, the lead in the substituted chemistry nickel makes the complete environmental protection of chemical nickel, and the bad generation of non-soldering tin.
2, poisonous potassium cyanaurite in the substituted chemistry gold makes the fully environmental protection of chemistry gold, and solution-stabilized, can not decompose.
3, add unleaded stablizer, can play the function of stable inhibited reaction.Added good opening and plated the agent potassium sulfocyanate, without thermal losses, can reduce and drag the cylinder time, increased client's production capacity, reduced consuming; Can reduce simultaneously stablizer determination of total precipitated quantities in the middle of the far super plating piece of plating piece edge determination of total precipitated quantities, and cause the corrosion that the galvanic cell reaction causes.It has stronger corrosion resistance.
4, the wetting angle of scolding tin is little, the scolding tin excellent property.
5, chemical golden cyanide-free, asepsis environment-protecting, and bath stability the phenomenon such as decompose, separate out without gold for a long time under 88 ℃ of high temperature.
Embodiment
The production method of a kind of environment-friendly type lead-free chemical nickel and gold provided by the invention, the method be the good circuit of etching and the wiring board handled well through anti-solder ink at first, passes through and then the pre-treatments such as polish-brush or sandblast; Then this wiring board is placed under 50 ℃ with the degreasing tank of 10% KOZO 801 configurations and processed 5 minutes; Then clean with tap water, deliver under 27 ℃ with the microetch groove of the vitriol oil configuration of the Sodium Persulfate of every liter of 100 gram and 20 milliliters every liter and processed 2 minutes; Then with washed with de-ionized water, enter under the room temperature with the pre-immersion trough of 0.5% vitriol oil configuration and processed 1 minute; Then directly enter under 27 ℃ with the activated bath of 8% KOZO 804 configurations and processed 1 minute.Use at last washed with de-ionized water, the chemical nickel that enters under 80 ℃ was processed 20 minutes.Wherein, chemical nickel groove liquid composite adopts following prescription to realize:
| Single nickel salt | 23-30g/L |
| Inferior sodium phosphate | 23-30g/L |
| Lactic acid | 10-22g/L |
| Succinic Acid | 4-8g/L |
| Potassium sulfocyanate | 1-20ppm |
| Ammoniacal liquor | Regulate the pH value to 4.4-4.7 |
| The preliminary election stablizer | 0.5-15ppm |
Wherein, single nickel salt is for providing the main salt of nickel ion; Inferior sodium phosphate is the reductive agent of self-catalyzed reaction; Lactic acid and Succinic Acid are complexing agent; Potassium sulfocyanate is for opening plating agent (potassium sulfocyanate toxicity is extremely low to be prussiate toxinicide by product); Ammoniacal liquor is pH adjusting agent; The preliminary election stablizer is for replacing other plumbous inorganic stabilizers composition, such as Sb
2O
3, Bi
2O
3, KIO
3And ammonium molybdate in a kind of.At last with washed with de-ionized water, enter under 88 ℃ with the chemical golden groove of the citric acid gold configuration of every liter of 10% KOZO 806 and 2 gram and processed 10 minutes.
Further specify below in conjunction with specific embodiment:
Embodiment 1 nickel groove:
| Single nickel salt | 27g/L |
| Inferior sodium phosphate | 27g/L |
| Lactic acid | 18g/L |
| Succinic Acid | 5g/L |
| Potassium sulfocyanate | 4ppm |
| Ammoniacal liquor | Regulate pH value to 4.5 |
| Sb 2O 3 | 1ppm |
Embodiment 2 nickel grooves:
| Single nickel salt | 27g/L |
| Inferior sodium phosphate | 27g/L |
| Lactic acid | 20g/L |
| Succinic Acid | 5g/L |
| Potassium sulfocyanate | 4ppm |
| Ammoniacal liquor | Regulate pH value to 4.5 |
| Bi2O3 | 6ppm |
Embodiment 3 nickel grooves:
| Single nickel salt | 27g/L |
| Inferior sodium phosphate | 27g/L |
| Lactic acid | 13g/L |
| Succinic Acid | 4g/L |
| Potassium sulfocyanate | 7ppm |
| Ammoniacal liquor | Regulate pH value to 4.5 |
| KIO 3 | 10ppm |
Embodiment 4 nickel grooves:
| Single nickel salt | 27g/L |
| Inferior sodium phosphate | 27g/L |
| Lactic acid | 22g/L |
| Succinic Acid | 8g/L |
[0038]
| Potassium sulfocyanate | 4ppm |
| Ammoniacal liquor | Regulate pH value to 4.45 |
| Ammonium molybdate | 2ppm |
The performance test results is as follows:
Nickel groove stability test:
Method explanation: pipette palladium concentration take 10 milliliters of transfer pipets and record simultaneously the amount of splashing into as the nickel groove working fluid that the palladous sulfate solution of 360ppm gently splashes into 80 ℃ under, extremely decompose fully to the chemical nickel working fluid.The palladous sulfate solution that the splashes into bright stability of more speaking more is stronger.
| The amount of splashing into | |
| Embodiment 1 | 7.5ml |
| Embodiment 2 | 8.3ml |
| Embodiment 3 | 12.2ml |
| Embodiment 4 | 5.6ml |
Illustrate: embodiment 3 and embodiment 2 are best.
Gold groove stability test is as follows:
With 0.5dm
2/ L nickel plate is worked as load.Golden groove temperature is risen to 88 ℃ of lower continuous gold-platings, is that golden groove is when changing groove until the nickel ion semi-invariant of golden groove displacement reaches 700ppm() also find no and separate out generation.Illustrate that selected citric acid gold is fully suitable.
The solderability test is as follows:
Be as the criterion with the wetting angle test.Testing method is, will be with unleaded tin cream with the chemical nickel and gold place of web plate brush on the test line plate; Insert reflow machine (IR machine), utilize high temperature to be the tin of melting tin cream liquefy.Tin cream promptly flattens the wetting gold layer melting surface nickel face that sees through simultaneously at the chemical nickel carat (measure of the purity of gold) and forms the tin-nickel alloy layer as mercury under the effect of high temperature and soldering flux.When circuit card cools off when taking out solid form (this process is exactly scolding tin) of tin liquid on the circuit card again from reflow machine.At this moment there is a wetting angle in the nickel of tin and bottom surface gold face.More the bright scolding tin performance of novel is better for wetting angle.
As seen shown in seeing table.
| Point one | Point two | Point three | Point four |
[0049]
| Embodiment 1 | 8° | 12° | 7° | 14° |
| Embodiment 2 | 4° | 4° | 6° | 3° |
| Embodiment 3 | 6° | 8° | 9° | 8° |
| Embodiment 4 | 20° | 18° | 19° | 20° |
Illustrate: in order to reduce error, each embodiment all gets three points.Upper table shows that embodiment 2 and example 3 are best.
Top combination tabulation is described embodiments of the invention; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment only is schematic; rather than restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not breaking away from the scope situation that aim of the present invention and claim protect, also can make a lot of forms, these all belong within the protection of the present invention.
Claims (2)
1. the production method of an environment-friendly type lead-free chemical nickel and gold, it is characterized in that: the priority of described method is in proper order: pre-treatment, oil removing, microetch, preimpregnation, activation, chemical nickel, chemistry gold; Specifically may further comprise the steps:
1) the good circuit of etching is handled wiring board well through anti-solder ink, after pre-treatments such as polish-brush or sandblasts, forms relatively clean wiring board copper face;
2) this wiring board is placed degreasing tank, further remove copper face oxidation and greasy dirt;
3) clean with tap water, deliver to the microetch groove, with surperficial little alligatoring of copper;
4) with washed with de-ionized water, enter preimpregnation and activated bath, make the upper a small amount of palladium of copper face displacement;
5) with washed with de-ionized water, enter chemical nickel, the about ni-p alloy coating of 4 micron thick of 7-10% take palladium as catalytic core autocatalysis one deck phosphorus content;
6) with washed with de-ionized water, enter chemical golden groove, replace the approximately gold layer of 0.07 micron thick of one deck with the method for displacement, be used for scolding tin and prevent oxidation.
2. the production method of environment-friendly type lead-free chemical nickel and gold according to claim 1, it is characterized in that: the method for the preparation of each reactive tank and processing is as follows in the described step 2:
1) degreasing tank KOZO 801 with 10% under 45 ℃ joins groove processing 5 minutes;
2) the microetch groove is joined groove processing 2 minutes with the Sodium Persulfate of every liter of 100 gram and 20 milliliters every liter the vitriol oil under 27 ℃;
3) pre-immersion trough is joined groove processing 1 minute with 0.5% the vitriol oil under room temperature;
4) activated bath KOZO 804 with 8% under 27 ℃ joins groove processing 1 minute;
5) the chemical nickel groove was processed 20 minutes in 80 ℃ of lower chemical nickel groove liquid composites that use;
6) chemical golden groove KOZO 806 and 2 citric acid golds that restrain every liter with 10% under 88 ℃ are joined groove processing 10 minutes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103389417A CN102877044A (en) | 2012-09-13 | 2012-09-13 | Method for producing environment-friendly lead-free electroless nickel immersion gold |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103389417A CN102877044A (en) | 2012-09-13 | 2012-09-13 | Method for producing environment-friendly lead-free electroless nickel immersion gold |
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|---|---|---|---|
| CN2012103389417A Pending CN102877044A (en) | 2012-09-13 | 2012-09-13 | Method for producing environment-friendly lead-free electroless nickel immersion gold |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104540322A (en) * | 2014-12-22 | 2015-04-22 | 泰州市博泰电子有限公司 | Semi-plugged silver melting module substrate pretreatment method |
| CN104768330A (en) * | 2014-07-30 | 2015-07-08 | 昆山圆裕电子科技有限公司 | Method for processing nickel-gold residue on high-density line flexible circuit board |
| CN111349917A (en) * | 2018-12-24 | 2020-06-30 | 天津环鑫科技发展有限公司 | Gold plating solution for semiconductor chip, gold plating method and nickel and gold plating method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525744A (en) * | 2009-04-27 | 2009-09-09 | 深圳市成功化工有限公司 | Superficial treatment method of printed wiring board |
| CN101760731A (en) * | 2008-12-23 | 2010-06-30 | 三星电机株式会社 | Electroless nickel plating solution composition, flexible printed circuit board and manufacturing method thereof |
| CN102011107B (en) * | 2010-12-24 | 2012-07-11 | 杭州东方表面技术有限公司 | Chemical nickel-phosphorus alloy plating solution capable of obtaining high-solderability plating layer |
-
2012
- 2012-09-13 CN CN2012103389417A patent/CN102877044A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760731A (en) * | 2008-12-23 | 2010-06-30 | 三星电机株式会社 | Electroless nickel plating solution composition, flexible printed circuit board and manufacturing method thereof |
| CN101525744A (en) * | 2009-04-27 | 2009-09-09 | 深圳市成功化工有限公司 | Superficial treatment method of printed wiring board |
| CN102011107B (en) * | 2010-12-24 | 2012-07-11 | 杭州东方表面技术有限公司 | Chemical nickel-phosphorus alloy plating solution capable of obtaining high-solderability plating layer |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104768330A (en) * | 2014-07-30 | 2015-07-08 | 昆山圆裕电子科技有限公司 | Method for processing nickel-gold residue on high-density line flexible circuit board |
| CN104768330B (en) * | 2014-07-30 | 2018-05-01 | 昆山圆裕电子科技有限公司 | High-density line flexible PCB nickel gold residual substance treating method |
| CN104540322A (en) * | 2014-12-22 | 2015-04-22 | 泰州市博泰电子有限公司 | Semi-plugged silver melting module substrate pretreatment method |
| CN111349917A (en) * | 2018-12-24 | 2020-06-30 | 天津环鑫科技发展有限公司 | Gold plating solution for semiconductor chip, gold plating method and nickel and gold plating method |
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Application publication date: 20130116 |