CN101979709B - Novel chemical copper plating method - Google Patents
Novel chemical copper plating method Download PDFInfo
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- CN101979709B CN101979709B CN2010105429176A CN201010542917A CN101979709B CN 101979709 B CN101979709 B CN 101979709B CN 2010105429176 A CN2010105429176 A CN 2010105429176A CN 201010542917 A CN201010542917 A CN 201010542917A CN 101979709 B CN101979709 B CN 101979709B
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Abstract
The invention discloses a chemical copper plating method. The method comprises steps of degreasing and hole finishing, washing, micro etching, pre-impregnation, activation, washing, dispergation, washing and chemical copper plating. The method is characterized in that: in the degreasing and hole finishing step, a circuit board can be degreased, and more important, high negative electricity is carried in the hole and can adsorb more palladium colloid so that the backlight of a copper layer reaches over level 9; salt-based ammonium sulfate and palladium sulfate solution is adopted in the activation step, and acid mist produced by the traditional palladium colloid is not produced, so the method is environment-friendly and has no any injury to the operating personnel; and in the dispergation step, sulfuric acid and hydrazine sulfate are used for removing ammonium radicals, and the hydrazine can reduce palladium metal into palladium atoms, so copper is better deposited.
Description
Technical field
The present invention relates to a kind of plastic cement, glass, printed wiring (PCB) plate electroless copper plating method, more particularly, relate to the process method of the whole hole of oil removing, preimpregnation, activation, dispergation step in plastic cement, glass, printed wiring (PCB) the plate electroless copper plating method.
Background technology
At present, along with the fast development of the global electronic infotech and the communication technology, printed wiring (PCB) industry becomes the manufacturing maximum pillar of electronic component at world wide.Progressively shift to China and be accompanied by the World PCB industry, the PCB industry of China is also fast-developing since the nineties in 20th century.Prediction along with China's manufacturing powerhouse to production power constantly stride forward and electronics and information industry further develops, will reach 2.45 hundred million square metres to China PCB output in 2012.
In the printed circuit board manufacturing technology, most critical be exactly the electroless copper operation.Its significant feature is exactly to make two-sided and nonmetal hole multilayer printed circuit board, on hole wall, deposits the layer of even conductive layer through redox reaction, through electroplating thickening copper facing, reaches the purpose in loop again.Reaching this purpose just must select stable performance, reliable chemical pretreatment solution and formulate correct, feasible and effective processing sequence.But general printed wiring (PCB) plate electroless copper plating method ionic palladium activation performance is unstable; Acidoid palladium acid mist is excessive; Bigger to environment and operator's influence; Progression backlight is lower in the hole that obtains, and the poor reliability that copper facing has, said existing technological deficiency are the important topics of technician's research in the industry of this area.
Summary of the invention
The objective of the invention is to traditional ionic palladium activation performance unstable; The perhaps excessive shortcoming of acidoid palladium acid mist; A kind of electroless copper plating method is provided, the method for printed wiring (PCB) the plate electroless copper that this a kind of electroless copper plating method is a kind of environmental protection, low cost, be easy to control.
Technical scheme of the present invention is described below: a kind of electroless copper plating method, and this method is made up of the whole hole of oil removing, washing, little erosion, preimpregnation, activation, washing, dispergation, washing, electroless copper step, it is characterized in that,
In the step of the whole hole of oil removing:
(1), get OP emulsifying agent 0.1-10.0g, sodium phosphate 1.0-5.0g, Rhodafac RA-600 tensio-active agent 1.0-5.0g, earlier with getting solution respectively with the less water dissolving, mixed diluting to 1 liter then;
(2), printed circuit board is immersed in the above-mentioned mixing solutions, the time was controlled at 1-10 minute, and pH value remains between the 8-14, and temperature is controlled at 40-70 degree centigrade;
In the preimpregnation step:
(1), get stannous sulfate 1-50g, hydrochloric acid 1-100ml, fluorochemical 0.1-5g, earlier stannous sulfate is dissolved in the hydrochloric acid, add fluoride dissolution again, be diluted with water to 1 liter again;
(2), will be immersed in the above-mentioned mixing solutions through the printed circuit board after the whole hole of oil removing, washing, the little erosion, the time was controlled at 0.1-10 minute, temperature is controlled at 0-50 degree centigrade;
In activation step:
(1), get sulfuric acid 5-50g, palladous sulfate 5-50g, ammonium sulfate 5-200g, urea 10-50g, earlier with Dilution of sulphuric acid to 800ml water, again other three kinds of raw materials are added dissolving, mixed diluting to 1 liter is heated to 60 degrees centigrade then, stirs 1 hour;
(2), the printed circuit board after preimpregnation is immersed in the above-mentioned mixing solutions, the time was controlled at 1-10 minute, and temperature is controlled at 0-80 degree centigrade;
In the dispergation step:
(1), gets sulfuric acid 10-50g and hydrazonium sulfate 0.1-10g, with redilution to 1 after the water dissolution liter;
(2), with activated, the washing after printed circuit board be immersed in the above-mentioned mixing solutions, acidity remains between the 0.3-1.0, the time was controlled at 0.5-10 minute.
According to above-mentioned the present invention, its characteristic also is: the fluorochemical that adopts in the said preimpregnation step is a Potassium monofluoride, Sodium Fluoride, sodium bifluoride, Neutral ammonium fluoride, any several kinds of compsns in the matt salt.
According to above-mentioned the present invention, its characteristic also is: each constituent mass proportioning is in the whole hole step (1) of said oil removing:
Tensio-active agent 0.5g/L sodium phosphate 3.0g/L
Rhodafac RA-600 tensio-active agent 2.0g/L;
Each constituent mass proportioning is in the said preimpregnation step (1):
Stannous sulfate 10g/L hydrochloric acid 50ml/L Potassium monofluoride 2g/L;
Each constituent mass proportioning is in the said activation step (1):
Sulfuric acid 10g/L palladous sulfate 50g/L
Ammonium sulfate 100g/L urea 25g/L;
Each constituent mass proportioning is in the said dispergation step (1):
Sulfuric acid 20g/L hydrazonium sulfate 5g/L.
According to above-mentioned the present invention; Its beneficial effect is: the present invention utilizes aniorfic surfactant; Let have electronegativity in the hole of PCB parts, make its surface can adsorb the palladium of capacity, colloidal palladium is the palladous sulfate system; The acid mist puzzlement of no hydrochloric acid palladium has no effect to environment and operator.Progression backlight is higher in the hole that obtains, and copper facing has very high safety.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment one
A kind of electroless copper plating method may further comprise the steps:
1, the whole hole of oil removing
(1), get op emulsifying agent 0.1g, sodium phosphate 1.0g, Rhodafac RA-600 tensio-active agent 1.5g, earlier with getting solution respectively with the less water dissolving, mixed diluting to 1 liter then;
(2), pcb board is immersed in the above-mentioned mixing solutions, the time was controlled at 6 minutes, and pH value is 8, and temperature is controlled at 55 degrees centigrade;
During the whole hole of oil removing, workpiece is waved, make the combination solution in the hole have certain circulation.
This step mainly is to remove the greasy dirt of copper face, and sull priorly adjusts the electric charge in the hole, makes its surface have negative electricity.
2, washing
To pass through pcb board behind the whole hole of oil removing and put into water and wash, washing times is twice, washes the unnecessary tensio-active agent of copper face.
3, little erosion
The pcb board that will pass through after the washing is put into 100g/L Sodium Persulfate and 30g/L sulphuric acid soln, carries out under the condition of room temperature 2 minutes, takes out pcb board again and cleans.
This step is so long as for to make copper face have certain roughness, can strengthen electroless copper, the bonding force of electro-coppering.
4, preimpregnation
(1), get stannous sulfate 5g, hydrochloric acid 10ml, matt salt 2g is dissolved in stannous sulfate in the hydrochloric acid earlier, adds the matt salt dissolving again, is diluted with water to 1 liter again;
(2), the pcb board that will pass through after little erosion puts into above-mentioned mixed assemblage solution, the time is 2 minutes, temperature is 23 degrees centigrade.
This step is forbidden pneumatic blending, but pcb board is waved, and liquid medicine is better circulation in the hole, makes to have competent stannous ion in the hole.
In this step, use stannous sulfate, matt salt and dilute hydrochloric acid solution; Make and have certain density stannous ion in the hole; Palladium ion in can reduction activation, the existence of matt salt can be corroded the spun glass in the PCB hole, makes its surface irregularity; Adsorb palladium ion more easily, and improve copper layer bonding force.
5, activation
(1), get sulfuric acid 5g, palladous sulfate 5g, ammonium sulfate 150g, urea 10g, earlier with Dilution of sulphuric acid to 800ml water, again other three kinds of raw materials are added dissolving, mixed diluting to 1 liter is heated to 60 degrees centigrade then, stirs 1 hour;
(2), the pcb board that will pass through after the preimpregnation puts into above-mentioned mixing solutions, the time was controlled at 6 minutes, 45 degrees centigrade of temperature.
Preferably wave in this step, but forbid pneumatic blending, this step makes the hole internal adsorption have the palladium ion of positive electricity, and tin protoxide becomes tetravalent tin, and the part palladium ion is reduced to the metallic palladium that copper is had catalytic activity by Bivalent Tin.
This activation solution adopts palladous sulfate, ammonium sulfate, the vitriolic mixed solution, the ammonium root has complexing, can with palladium ion form one have positive electricity group, inhale mutually with hole wall that has negative electricity and Ya Xi, and the tin protoxide ion.
6, washing
Will the pcb board behind overactivation putting into water washes.
7, dispergation
(1), get sulfuric acid 10g, hydrazonium sulfate 2g is with redilution to 1 after the water dissolution liter.
(2), the pcb board that will pass through after the washing puts into above-mentioned mixing solutions, acidity remains on 0.3, the time was controlled at 0.5 minute.
In this step, ammonium root and tin ion are dissolved, and part makes palladium ion be reduced to metallic palladium fully and is adsorbed on hole wall not by inferior tin reductive palladium ion oxidation hydrazonium sulfate.
8, washing
To pass through pcb board behind the dispergation puts into water and washes.
9, electroless copper
The pcb board that will pass through after the washing is put into the chemical copper plating solution copper layer, and through after the above-mentioned steps, hole wall has had the metallic palladium of one deck, and in chemical copper plating solution, the catalysis that palladium the becomes copper heart of living is in the continuous copper layer of hole wall.
The electroless copper operation is accomplished.
Embodiment two
A kind of electroless copper plating method may further comprise the steps:
1, the whole hole of oil removing
(1), get op emulsifying agent 0.5g, sodium phosphate 2.5g, Rhodafac RA-600 tensio-active agent 1.5g, earlier with getting solution respectively with the less water dissolving, mixed diluting to 1 liter then;
(2), pcb board is immersed in the above-mentioned mixing solutions, temperature is 50 degrees centigrade, and the time is 6 minutes, and pH value is 10.
2, washing
To pass through pcb board behind the whole hole of oil removing and put into water and wash, washing times is twice, washes the unnecessary tensio-active agent of copper face.
3, little erosion
The pcb board that will pass through after the washing is put into 100g/L Sodium Persulfate and 30g/L sulphuric acid soln.
When carrying out this step, solution will carry out pneumatic blending, under the condition of room temperature, carries out 2 minutes, takes out the PCB parts and cleans.
4, preimpregnation
(1), get stannous sulfate 10g, hydrochloric acid 30ml, matt salt 2g is dissolved in stannous sulfate in the hydrochloric acid earlier, adds the matt salt dissolving again, is diluted with water to 1 liter again;
(2), the pcb board that will pass through after little erosion puts into above-mentioned mixed assemblage solution, the time was controlled at 2 minutes, temperature is 25 degrees centigrade.
5, activation
(1), get sulfuric acid 20g, palladous sulfate 10g, ammonium sulfate 150g, urea 50g, earlier with Dilution of sulphuric acid to 800ml water, again other three kinds of raw materials are added dissolving, mixed diluting to 1 liter is heated to 60 degrees centigrade then, stirs 1 hour;
(2), the pcb board that will pass through after the preimpregnation puts into above-mentioned mixing solutions, the time was controlled at 8 minutes, temperature 40 degree.
6, washing
Will the pcb board behind overactivation putting into water washes.
7, dispergation
(1), sulfuric acid 20g, hydrazonium sulfate 2g is with redilution to 1 after the water dissolution liter.
(2), the pcb board that will pass through after the washing puts into above-mentioned mixing solutions, acidity remains on 0.5, the time was controlled at 5 minutes.
8, washing
To pass through PCB parts behind the dispergation puts into water and washes.
9, electroless copper
The pcb board that will pass through after the washing is put into the chemical copper plating solution copper layer.
The electroless copper operation is accomplished.
Embodiment three
A kind of electroless copper plating method may further comprise the steps:
1, the whole hole of oil removing
(1), get op emulsifying agent 10g, sodium phosphate 5.0g, Rhodafac RA-600 tensio-active agent 5.0g, earlier with said combination solution respectively with the less water dissolving, mixed diluting to 1 liter then;
(2), pcb board is immersed in the above-mentioned mixing solutions, temperature is 45 degrees centigrade, and the time is 2 minutes, and pH value is 14.
2, washing
To pass through pcb board behind the whole hole of oil removing and put into water and wash, washing times is twice, washes the unnecessary tensio-active agent of copper face.
3, little erosion
The pcb board that will pass through after the washing is put into 100g/L Sodium Persulfate and 30g/L sulphuric acid soln, carries out under the condition of room temperature 1 minute, takes out pcb board and cleans.
4, preimpregnation
(1), get hydrochloric acid 100ml, tin protochloride 50g, matt salt 5g is dissolved in tin protochloride in the concentrated hydrochloric acid earlier, adds the matt salt dissolving again, is diluted with water to 1 liter again;
(2), the pcb board that will pass through after little erosion puts into above-mentioned mixed assemblage solution, the time is 10 minutes, temperature is 50 degrees centigrade.
5, activation
(1), get ammonium sulfate 200g, palladous sulfate 50g, sulfuric acid 50g, urea 10g, earlier with Dilution of sulphuric acid to 800ml water, again other three kinds of raw materials are added dissolving, mixed diluting to 1 liter is heated to 60 degrees centigrade then, stirs 1 hour;
The pcb board that (2), will pass through after the preimpregnation is put into above-mentioned mixing solutions, this activity time control 10 minutes, 20 degrees centigrade of temperature.
6, washing
Will the pcb board behind overactivation putting into water washes.
7, dispergation
(1), get sulfuric acid 50g, hydrazonium sulfate 10g is with redilution to 1 after the water dissolution liter.
(2), the pcb board that will pass through after the washing puts into above-mentioned mixing solutions, acidity remains on 1.0, the time was controlled at 10 minutes.
8, washing
To pass through pcb board behind the dispergation puts into water and washes.
9, electroless copper
The pcb board that will pass through after the washing is put into the chemical copper plating solution copper layer.
The electroless copper operation is accomplished.
Though the present invention describes with reference to the above embodiments; But those of ordinary skill in the art can recognize very clearly that fully above embodiment is used to explain the present invention; Wherein can make variations and modifications and not break away from the present invention in a broad sense; So be not as to qualification of the present invention,, all will fall within the protection domain that the present invention requires variation, the distortion of above-described embodiment as long as in connotation scope of the present invention.
Claims (3)
1. electroless copper plating method, this method is made up of the whole hole of oil removing, washing, little erosion, preimpregnation, activation, washing, dispergation, washing, electroless copper step, it is characterized in that,
In the step of the whole hole of oil removing:
(1), get OP emulsifying agent 0.1-10.0g, sodium phosphate 1.0-5.0g, Rhodafac RA-600 tensio-active agent 1.0-5.0g, earlier with getting solution respectively with the less water dissolving, mixed diluting to 1 liter then;
(2), printed circuit board is immersed in the above-mentioned mixing solutions, the time was controlled at 1-10 minute, and pH value remains between the 8-14, and temperature is controlled at 40-70 degree centigrade;
In the preimpregnation step:
(1), get stannous sulfate 1-50g, hydrochloric acid 1-100ml, fluorochemical 0.1-5g, earlier stannous sulfate is dissolved in the hydrochloric acid, add fluoride dissolution again, be diluted with water to 1 liter again;
(2), will be immersed in the above-mentioned mixing solutions through the printed circuit board after the whole hole of oil removing, washing, the little erosion, the time was controlled at 0.1-10 minute, temperature is controlled at 0-50 degree centigrade;
In activation step:
(1), get sulfuric acid 5-50g, palladous sulfate 5-50g, ammonium sulfate 5-200g, urea 10-50g, earlier with Dilution of sulphuric acid to 800ml water, again other three kinds of raw materials are added dissolving, mixed diluting to 1 liter is heated to 60 degrees centigrade then, stirs 1 hour;
(2), the printed circuit board after preimpregnation is immersed in the above-mentioned mixing solutions, the time was controlled at 1-10 minute, and temperature is controlled at 0-80 degree centigrade;
In the dispergation step:
(1), gets sulfuric acid 10-50g and hydrazonium sulfate 0.1-10g, with redilution to 1 after the water dissolution liter;
(2), with activated, the washing after printed circuit board be immersed in the above-mentioned mixing solutions, acidity remains between the 0.3-1.0, the time was controlled at 0.5-10 minute.
2. a kind of electroless copper plating method according to claim 1, its characteristic also is: the fluorochemical that adopts in the said preimpregnation step is a Potassium monofluoride, Sodium Fluoride, sodium bifluoride, Neutral ammonium fluoride, any several kinds of compsns in the matt salt.
3. a kind of electroless copper plating method according to claim 1, its characteristic also is: each constituent mass proportioning is in the whole hole step (1) of said oil removing:
Tensio-active agent 0.5g/L sodium phosphate 3.0g/L
Rhodafac RA-600 tensio-active agent 2.0g/L;
Each constituent mass proportioning is in the said preimpregnation step (1):
Stannous sulfate 10g/L hydrochloric acid 50ml/L Potassium monofluoride 2g/L;
Each constituent mass proportioning is in the said activation step (1):
Sulfuric acid 10g/L palladous sulfate 50g/L
Ammonium sulfate 100g/L urea 25g/L;
Each constituent mass proportioning is in the said dispergation step (1):
Sulfuric acid 20g/L hydrazonium sulfate 5g/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105429176A CN101979709B (en) | 2010-11-15 | 2010-11-15 | Novel chemical copper plating method |
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|---|---|---|---|
| CN2010105429176A CN101979709B (en) | 2010-11-15 | 2010-11-15 | Novel chemical copper plating method |
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| CN101979709A CN101979709A (en) | 2011-02-23 |
| CN101979709B true CN101979709B (en) | 2012-11-21 |
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| CN103205735B (en) * | 2012-01-17 | 2015-01-28 | 江苏华神电子有限公司 | Chemical copper deposition return type process flow for printed wiring board |
| CN102899640B (en) * | 2012-10-25 | 2014-06-25 | 南京大地冷冻食品有限公司 | Maintenance method of chemical plating dispergation working fluid |
| CN103108501B (en) * | 2013-01-18 | 2016-12-28 | 金悦通电子（翁源）有限公司 | A kind of microwell plate chemical copper activation back scrubbing technique and system thereof |
| CN104113989B (en) * | 2013-04-17 | 2017-11-07 | 深南电路股份有限公司 | The method of heavy copper on pcb board |
| CN103476204B (en) * | 2013-10-08 | 2016-06-08 | 复旦大学 | A kind of addition preparation method of dual platen |
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| CN104066267A (en) * | 2014-06-03 | 2014-09-24 | 深圳市创智成功科技有限公司 | Chemical plating structure of copper base material and technique thereof |
| US9563233B2 (en) * | 2014-08-14 | 2017-02-07 | Microsoft Technology Licensing, Llc | Electronic device with plated electrical contact |
| CN105112893A (en) * | 2015-08-04 | 2015-12-02 | 永利电子铜陵有限公司 | Highly-stable electroless copper plating process of PCB (Printed circuit board) |
| CN105112896A (en) * | 2015-08-04 | 2015-12-02 | 永利电子铜陵有限公司 | Chemical silver plating technology of PCBs |
| CN107278057A (en) * | 2016-04-08 | 2017-10-20 | 东莞市斯坦得电子材料有限公司 | A kind of technique being roughened for conducting hole of printed circuit board hole wall glass |
| CN106521592A (en) * | 2016-11-29 | 2017-03-22 | 延康汽车零部件如皋有限公司 | Electroplating dispergation solution |
| CN106944044B (en) * | 2017-03-27 | 2020-02-04 | 中国科学院深圳先进技术研究院 | Palladium-based catalyst and preparation method and application thereof |
| CN107740073A (en) * | 2017-08-24 | 2018-02-27 | 深圳市新日东升电子材料有限公司 | Reduced form accelerator for soft board electroless copper and its preparation method and application |
| CN108265282B (en) * | 2018-02-27 | 2019-03-22 | 深圳市祥盛兴科技有限公司 | Apply the printed wiring board clamping device in printed wiring board electroless copper plating technique |
| CN109825375B (en) * | 2019-02-26 | 2021-01-01 | 湖南互连微电子材料有限公司 | Cleaning and pore-finishing agent and using method thereof |
| CN112030148A (en) * | 2020-09-03 | 2020-12-04 | 深圳市生利科技有限公司 | Chromium plating process with high wear resistance of plating layer |
| CN114449759A (en) * | 2020-11-04 | 2022-05-06 | 竞华电子(深圳)有限公司 | PTH process |
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