CN101979709A - Novel chemical copper plating method - Google Patents
Novel chemical copper plating method Download PDFInfo
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- CN101979709A CN101979709A CN 201010542917 CN201010542917A CN101979709A CN 101979709 A CN101979709 A CN 101979709A CN 201010542917 CN201010542917 CN 201010542917 CN 201010542917 A CN201010542917 A CN 201010542917A CN 101979709 A CN101979709 A CN 101979709A
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Abstract
The invention discloses a novel 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 processing 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 information technology 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, deposits the layer of even conductive layer by redox reaction on hole wall, 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 instability, acidoid palladium acid mist is excessive, bigger to environment and operator's influence, progression backlight is lower in the hole that obtains, the poor reliability that copper facing has, described 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 at traditional ionic palladium activation performance instability, the perhaps excessive shortcoming of acidoid palladium acid mist, provide a kind of novel electroless copper plating method, the method for printed wiring (PCB) the plate electroless copper that this a kind of new chemical copper electroplating method is a kind of environmental protection, low cost, be easy to control.
Technical scheme of the present invention is as described below: a kind of novel electroless copper plating method, and this method is made up of the whole hole of oil removing, washing, microetch, 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 tensio-active agent 0.1-10.0g/L, sodium phosphate 1.0-5.0g/L, Rhodafac RA-600 tensio-active agent 1.0-5.0g/L, 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/L, hydrochloric acid 1-100ml/L, fluorochemical 0.1-5g/L, earlier sulfate industry tin 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 microetch, 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/L, palladous sulfate 5-50g/L, ammonium sulfate 5-200g/L, urea 10-50g/L, 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 feature also is: described tensio-active agent adopts anionic.
According to above-mentioned the present invention, its feature also is: described tensio-active agent adopts non-ionic type.
According to above-mentioned the present invention, its feature also is: described tensio-active agent adopts anionic and non-ionic type mixed type.
According to above-mentioned the present invention, its feature also is: described tensio-active agent is preferably the 0P emulsifying agent.
According to above-mentioned the present invention, its feature also is: the fluorochemical that adopts in the described preimpregnation step is a Potassium monofluoride, Sodium Fluoride, sodium bifluoride, Neutral ammonium fluoride, any several compositions in the ammonium bifluoride.
According to above-mentioned the present invention, its feature also is: the preferred quality proportioning of each component is in the whole hole step (1) of described oil removing:
Tensio-active agent 0.5g/L sodium phosphate 3.0g/L
Rhodafac RA-600 tensio-active agent 2.0g/L;
The preferred quality proportioning of each component is in the described preimpregnation step (1):
Stannous sulfate 10g/L hydrochloric acid 50ml/L Potassium monofluoride 2g/L;
The preferred quality proportioning of each component is in the described activation step (1):
Sulfuric acid 10g/L palladous sulfate 50ppm
Ammonium sulfate 100g/L urea 25g/L;
The preferred quality proportioning of each component is in the described 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, allow and 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 reliability.
[embodiment]
Below in conjunction with embodiment the present invention is further described:
Embodiment one
A kind of novel 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 oxide film priorly adjusts the electric charge in the hole, makes its surface have negative electricity.
2, washing
To put into water through the pcb board behind the whole hole of oil removing and wash, washing times is twice, washes the unnecessary tensio-active agent of copper face.
3, microetch
To put into 100g/L Sodium Persulfate and 30g/L sulphuric acid soln through the pcb board after the washing, carry out under the condition of room temperature 2 minutes, and take out pcb board again and clean.
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, ammonium bifluoride 2g is dissolved in stannous sulfate in the hydrochloric acid earlier, adds the ammonium bifluoride dissolving again, is diluted with water to 1 liter again;
(2), will put into above-mentioned mixed assemblage solution through the pcb board after the microetch, 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, ammonium bifluoride and dilute hydrochloric acid solution, make and have certain density stannous ion in the hole, palladium ion in can reduction activation, the existence of ammonium bifluoride can be corroded the glass fibre in the PCB hole, makes its surface irregularity, easier absorption palladium ion, 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), will put into above-mentioned mixing solutions through the pcb board after the preimpregnation, 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, and the vitriolic mixed solution, the ammonium root has complexing, can form a group that has positive electricity with palladium ion, 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), will through the washing after pcb board put 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 put into water through the pcb board behind the dispergation washes.
9, electroless copper
To put into the chemical copper plating solution copper layer through the pcb board after the washing, through after the above-mentioned steps, hole wall has had the metallic palladium of one deck, and in chemical copper plating solution, palladium becomes the catalysis heart alive of copper, in the continuous copper layer of hole wall.
The electroless copper operation is finished.
Embodiment two
A kind of novel 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 put into water through the pcb board behind the whole hole of oil removing and wash, washing times is twice, washes the unnecessary tensio-active agent of copper face.
3, microetch
To put into 100g/L Sodium Persulfate and 30g/L sulphuric acid soln through the pcb board after the washing.
When carrying out this step, solution will carry out pneumatic blending, carries out under the condition of room temperature 2 minutes, takes out the PCB parts and cleans.
4, preimpregnation
(1), get stannous sulfate 10g, hydrochloric acid 30ml, ammonium bifluoride 2g is dissolved in stannous sulfate in the hydrochloric acid earlier, adds the ammonium bifluoride dissolving again, is diluted with water to 1 liter again;
(2), will put into above-mentioned mixed assemblage solution through the pcb board after the microetch, 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), will put into above-mentioned mixing solutions through the pcb board after the preimpregnation, 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), will through the washing after pcb board put into above-mentioned mixing solutions, acidity remains on 0.5, the time was controlled at 5 minutes.
8, washing
To put into water through the PCB parts behind the dispergation washes.
9, electroless copper
To put into the chemical copper plating solution copper layer through the pcb board after the washing.
The electroless copper operation is finished.
Embodiment three
A kind of novel 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 described 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 put into water through the pcb board behind the whole hole of oil removing and wash, washing times is twice, washes the unnecessary tensio-active agent of copper face.
3, microetch
To put into 100g/L Sodium Persulfate and 30g/L sulphuric acid soln through the pcb board after the washing, carry out under the condition of room temperature 1 minute, and take out pcb board and clean.
4, preimpregnation
(1), get hydrochloric acid 100ml, tin protochloride 50g, ammonium bifluoride 5g is dissolved in tin protochloride in the concentrated hydrochloric acid earlier, adds the ammonium bifluoride dissolving again, is diluted with water to 1 liter again;
(2), will put into above-mentioned mixed assemblage solution through the pcb board after the microetch, 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;
(2), will put into above-mentioned mixing solutions through the pcb board after the preimpregnation, 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), will through the washing after pcb board put into above-mentioned mixing solutions, acidity remains on 1.0, the time was controlled at 10 minutes.
8, washing
To put into water through the pcb board behind the dispergation washes.
9, electroless copper
To put into the chemical copper plating solution copper layer through the pcb board after the washing.
The electroless copper operation is finished.
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 illustrate 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 limitation of the invention; as long as in connotation scope of the present invention, all will fall within the protection domain that the present invention requires variation, the distortion of above-described embodiment.
Claims (7)
1. novel electroless copper plating method, this method is made up of the whole hole of oil removing, washing, microetch, 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 tensio-active agent 0.1-10.0g/L, sodium phosphate 1.0-5.0g/L, Rhodafac RA-600 tensio-active agent 1.0-5.0g/L, 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/L, hydrochloric acid 1-100ml/L, fluorochemical 0.1-5g/L, 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 microetch, 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/L, palladous sulfate 5-50g/L, ammonium sulfate 5-200g/L, urea 10-50g/L, 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 novel electroless copper plating method according to claim 1, its feature also is: described tensio-active agent adopts anionic.
3. a kind of novel electroless copper plating method according to claim 1, its feature also is: described tensio-active agent adopts non-ionic type.
4. a kind of novel electroless copper plating method according to claim 1, its feature also is: described tensio-active agent adopts anionic and non-ionic type mixed type.
5. a kind of novel electroless copper plating method according to claim 1, its feature also is: described tensio-active agent is preferably the OP emulsifying agent.
6. a kind of novel electroless copper plating method according to claim 1, its feature also is: the fluorochemical that adopts in the described preimpregnation step is a Potassium monofluoride, Sodium Fluoride, sodium bifluoride, Neutral ammonium fluoride, any several compositions in the ammonium bifluoride.
7. a kind of novel electroless copper plating method according to claim 1, its feature also is: the preferred quality proportioning of each component is in the whole hole step (1) of described oil removing:
Tensio-active agent 0.5g/L sodium phosphate 3.0g/L
Rhodafac RA-600 tensio-active agent 2.0g/L;
The preferred quality proportioning of each component is in the described preimpregnation step (1):
Stannous sulfate 10g/L hydrochloric acid 50ml/L Potassium monofluoride 2g/L;
The preferred quality proportioning of each component is in the described activation step (1):
Sulfuric acid 10g/L palladous sulfate 50ppm
Ammonium sulfate 100g/L urea 25g/L;
The preferred quality proportioning of each component is in the described dispergation step (1):
Sulfuric acid 20g/L hydrazonium sulfate 5g/L.
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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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| CN102899640A (en) * | 2012-10-25 | 2013-01-30 | 南京大地冷冻食品有限公司 | Maintenance method of chemical plating dispergation working fluid |
| CN103205735A (en) * | 2012-01-17 | 2013-07-17 | 江苏华神电子有限公司 | Chemical copper deposition return type process flow for printed wiring board |
| CN103476204A (en) * | 2013-10-08 | 2013-12-25 | 复旦大学 | Addition preparation method for double-side boards |
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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 |
| CN102899640A (en) * | 2012-10-25 | 2013-01-30 | 南京大地冷冻食品有限公司 | Maintenance method of chemical plating dispergation working fluid |
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