CN104152874B - A kind of printed wiring board electroless copper activating solution - Google Patents
A kind of printed wiring board electroless copper activating solution Download PDFInfo
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- CN104152874B CN104152874B CN201410343987.7A CN201410343987A CN104152874B CN 104152874 B CN104152874 B CN 104152874B CN 201410343987 A CN201410343987 A CN 201410343987A CN 104152874 B CN104152874 B CN 104152874B
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- electroless copper
- sodium chloride
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 32
- 239000010949 copper Substances 0.000 title claims abstract description 32
- 230000003213 activating effect Effects 0.000 title claims abstract description 26
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 60
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000011780 sodium chloride Substances 0.000 claims abstract description 30
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 20
- 239000011734 sodium Substances 0.000 claims abstract description 20
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 20
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 19
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 20
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical group COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 4
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 claims description 4
- 150000001299 aldehydes Chemical class 0.000 claims description 3
- KCDXJAYRVLXPFO-UHFFFAOYSA-N syringaldehyde Chemical compound COC1=CC(C=O)=CC(OC)=C1O KCDXJAYRVLXPFO-UHFFFAOYSA-N 0.000 claims description 3
- COBXDAOIDYGHGK-UHFFFAOYSA-N syringaldehyde Natural products COC1=CC=C(C=O)C(OC)=C1O COBXDAOIDYGHGK-UHFFFAOYSA-N 0.000 claims description 3
- 241000219000 Populus Species 0.000 claims description 2
- 238000001994 activation Methods 0.000 abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 8
- 230000004913 activation Effects 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 239000003381 stabilizer Substances 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000008367 deionised water Substances 0.000 abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 abstract description 4
- 239000000615 nonconductor Substances 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000002525 ultrasonication Methods 0.000 abstract description 3
- -1 stability is high Substances 0.000 abstract 1
- WZUODJNEIXSNEU-UHFFFAOYSA-N 2-Hydroxy-4-methoxybenzaldehyde Chemical compound COC1=CC=C(C=O)C(O)=C1 WZUODJNEIXSNEU-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Chemically Coating (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
The invention discloses a kind of printed wiring board electroless copper activating solution, including following mass parts raw material：Two 100~300 parts of hydrated stannous chlorides, 2~6 parts of palladium bichloride, 150~180 parts of sodium chloride, 4~8 parts of three hydrated stannic acid sodium, 20~30 parts of additive, 0.5~2 part of reducing agent, 500~600 parts of deionized water.Palladium bichloride is made by A liquid using sodium chloride solution, two hydrated stannous chlorides and reducing agent are made B liquid, under ultrasonication, A liquid is scattered in B liquid, it is aided with three hydrated stannic acid sodium, additive, reducing agent as auxiliary stabilizer, it is made electroless copper activating solution, the activation process before electroless copper is carried out for printed wiring board, reach the effect of activation and the interior activation of printed wire plate hole of printed substrate Nonconductor surface, it is low with content of hydrochloric acid, stability is high, raw material are saved, environmental pollution is reduced and is not damaged the advantage of printed substrate substrate.
Description
Technical field
The present invention relates to electroless copper technical field, espespecially a kind of printed wiring board electroless copper activating solution.
Background technology
Electroless copper is widely used in the electronics industry, can be made after the Nonconductor surface conduction that activation is made with electroless copper
The two-sided or multiaspect printed wiring board of through hole is made, printed wiring board is " mother of electronic system product ", on the basis of electroless copper
Plating thicken layers of copper, it can be ensured that its solderability, protectiveness, electric conductivity, wearability, before printed wiring board electroless copper, need by
Matrix carries out activation process.Uniformly activation is the prerequisite for obtaining uniform electroless copper and uniformly-coating, chemistry
Copper facing is a critical process, and the activation process before electroless copper is the key for ensureing chemical plating copper layer quality.Hydrochloric acid-base
Activating solution, it is necessary to a large amount of hydrochloric acid in process for preparation, there is environmental protection problem, and its stability in severe operational environment
It is affected, during hole metallization, because hole wall exposes, denseer hydrochloric acid has certain erosion to hole wall resin, makes
Adhesion into matrix material declines.And the activating solution of alkali is then without disadvantages mentioned above, and easily match somebody with somebody compared with hydrochloric acid-base activating solution activating solution
System, while the consumption of palladium is also suitably reduced, and activity does not subtract.
The content of the invention
A kind of printed wiring board electroless copper activating solution of the present invention, it is characterised in that with sodium chloride as main stabilizer, adopt
Palladium bichloride is made A liquid with sodium chloride solution, two hydrated stannous chlorides and reducing agent are made B liquid, under ultrasonication, by A liquid
It is scattered in B liquid, is aided with three hydrated stannic acid sodium, additive, reducing agent as auxiliary stabilizer, is made electroless copper activating solution,
The activation process before electroless copper is carried out for printed wiring board, activation and the track of printed wiring board Nonconductor surface is realized
The purpose of activation, high with stability in the plate hole of road, reduces environmental pollution and does not damage the advantage of printed wiring board substrate
To achieve these goals, technical solution of the invention is：A kind of printed wiring board electroless copper activating solution
Raw material including following mass parts：Two 100~300 parts of hydrated stannous chlorides, 2~6 parts of palladium bichloride, 150~180 parts of sodium chloride,
Three 4~8 parts of hydrated stannic acid sodium, 20~30 parts of additive, 0.5~2 part of reducing agent, 500~600 parts of deionized water；
Further, described additive is urea or thiocarbamide；
Described reducing agent is 3-methoxy-4-hydroxybenzaldehyde, 3- hydroxyls -4-methoxybenzaldehyde, 4- methoxyl group water
Any one in poplar aldehyde, syringaldehyde.
A kind of preparation method of printed wiring board electroless copper activating solution of the present invention is：Add in the container with agitator
Enter the sodium chloride that mass parts are 150~180 parts and the distilled water that mass parts are 500~600 parts, open stirring, sodium to be chlorinated is complete
After CL, stop stirring, be made sodium chloride solution；The 10% of the sodium chloride solution quality being made is taken, it is 2~6 to add mass parts
The palladium bichloride of part, stirring is completely dissolved to palladium bichloride, is made A liquid；By two hydrated stannous chlorides that mass parts are 100~300 parts
It is added in the remaining sodium chloride solution being made, adds the reducing agent that mass parts are 0.5~2 part, stirring to two hydration chlorine
Change stannous to be completely dissolved, be made B liquid；Under the ul-trasonic irradiation of 550KHz, at a temperature of 27~30 DEG C, A liquid is slowly added to
To in B liquid, after solution to be mixed is changed into brownish black, continues ultrasonic wave and disperse 10 minutes, it is 4~8 parts to be eventually adding mass parts
Three hydrated stannic acid sodium and the additive that mass parts are 20~30 parts, ultrasonic disperse are allowed to be completely dissolved, and are warming up to 45~60 DEG C, ripe
Change 3~5 hours, obtain final product printed wiring board electroless copper activating solution.
Advantages of the present invention and feature are：Using sodium chloride solution by palladium bichloride be made A liquid, by two hydrated stannous chlorides with
Reducing agent is made B liquid, under ultrasonication, A liquid is scattered in B liquid, is aided with three hydrated stannic acid sodium, additive, reducing agent conduct
Auxiliary stabilizer, is made electroless copper activating solution, and the activation process before electroless copper is carried out for printed wiring board, reaches printing
The effect of activation in the activation of wiring board Nonconductor surface and printed wiring plate hole.The activating solution with sodium chloride as main stabilizer,
Sodium chloride base activating solution can be referred to as, activating solution is kept stabilization with the chlorion in sodium chloride, stabilization low with content of hydrochloric acid
Property it is high, save raw material, reduce environmental pollution and do not damage the advantage of printed wiring board substrate.
Specific embodiment
Embodiment 1
A kind of printed wiring board electroless copper activating solution includes the raw material of following mass parts：Two hydrated stannous chlorides 2000
Gram, 40 grams of palladium bichloride, 1600 grams of sodium chloride, 50 grams of three hydrated stannic acid sodium, 250 grams of urea, 3-methoxy-4-hydroxybenzaldehyde 10
Gram, 5500 grams of deionized water；
Its preparation method is：To being added in the container with agitator, mass parts are 1600 grams of sodium chloride and mass parts are
5500 grams of distilled water, opens stirring, after sodium to be chlorinated is completely dissolved, stops stirring, is made sodium chloride solution；Take what is be made
710 grams of sodium chloride solution, adds the palladium bichloride that mass parts are 40 grams, and stirring is completely dissolved to palladium bichloride, is made A liquid；By quality
Part is added in the remaining 6390 grams of sodium chloride solutions being made for 2000 grams of two hydrated stannous chlorides, and adding mass parts is
10 grams of 3-methoxy-4-hydroxybenzaldehyde, stirring is completely dissolved to two hydrated stannous chlorides, is made B liquid；In the super of 550KHz
Under sound wave effect, at a temperature of 28 DEG C, A liquid is slowly added into B liquid, after solution to be mixed is changed into brownish black, continues ultrasound
Wavelength-division dissipates 10 minutes, is eventually adding the three hydrated stannic acid sodium that mass parts are 50 grams and the urea that mass parts are 250 grams, ultrasonic disperse
It is allowed to be completely dissolved, is warming up to 50 DEG C, cure 5 hours, obtains final product printed wiring board electroless copper activating solution.
Embodiment 2
A kind of printed wiring board electroless copper activating solution includes the raw material of following mass parts：Two hydrated stannous chlorides 1000
Gram, 20 grams of palladium bichloride, 1500 grams of sodium chloride, 40 grams of three hydrated stannic acid sodium, 300 grams of thiocarbamide, 5 grams of 4-methoxysalicylaldehyde, go from
5000 grams of sub- water；
Its preparation method is：To being added in the container with agitator, mass parts are 1500 grams of sodium chloride and mass parts are
5000 grams of distilled water, opens stirring, after sodium to be chlorinated is completely dissolved, stops stirring, is made sodium chloride solution；Take the chlorine being made
Change 650 grams of sodium solution, add the palladium bichloride that mass parts are 20 grams, stirring is completely dissolved to palladium bichloride, is made A liquid；By mass parts
For 1000 grams of two hydrated stannous chlorides are added in the remaining 5850 grams of sodium chloride solutions being made, it is 5 to add mass parts
Gram 4-methoxysalicylaldehyde, stirring be completely dissolved to two hydrated stannous chlorides, be made B liquid；In the ul-trasonic irradiation of 550KHz
Under, at a temperature of 27 DEG C, A liquid is slowly added into B liquid, after solution to be mixed is changed into brownish black, continue ultrasonic wave dispersion 10
Minute, the three hydrated stannic acid sodium that mass parts are 40 grams and the thiocarbamide that mass parts are 300 grams are eventually adding, ultrasonic disperse is allowed to complete
Dissolving, is warming up to 60 DEG C, cures 3 hours, obtains final product printed wiring board electroless copper activating solution.
Embodiment 3
A kind of printed wiring board electroless copper activating solution includes the raw material of following mass parts：Two hydrated stannous chlorides 3000
Gram, 60 grams of palladium bichloride, 1800 grams of sodium chloride, 80 grams of three hydrated stannic acid sodium, 200 grams of urea, 3,5- dimethoxy-4 's-hydroxy benzenes first
20 grams of aldehyde, 6000 grams of deionized water；
Its preparation method is：To being added in the container with agitator, mass parts are 1800 grams of sodium chloride and mass parts are
6000 grams of distilled water, opens stirring, after sodium to be chlorinated is completely dissolved, stops stirring, is made sodium chloride solution；Take the chlorine being made
Change the 10% of sodium solution quality, add the palladium bichloride that mass parts are 60 grams, stirring is completely dissolved to palladium bichloride, is made A liquid；By matter
Amount part is that 3000 grams of two hydrated stannous chlorides are added in the remaining sodium chloride solution being made, and adds mass parts for 20 grams
Syringaldehyde, stirring be completely dissolved to two hydrated stannous chlorides, be made B liquid；In the super of 550KHz
Under sound wave effect, at a temperature of 30 DEG C, A liquid is slowly added into B liquid, after solution to be mixed is changed into brownish black, continues ultrasound
Wavelength-division dissipates 10 minutes, is eventually adding the three hydrated stannic acid sodium that mass parts are 80 grams and the urea that mass parts are 200 grams, ultrasonic disperse
It is allowed to be completely dissolved, is warming up to 45 DEG C, cure 4 hours, obtains final product printed wiring board electroless copper activating solution.
The above, implementation method is only that the preferred embodiment of the present invention is described, not to of the invention
Scope is defined, and on the premise of the spirit for not departing from the technology of the present invention, this area engineers and technicians are to skill of the invention
Various modifications and improvement that art scheme is made, all should fall into the protection domain of claims of the present invention determination.
Claims (1)
1. a kind of preparation method of printed wiring board electroless copper activating solution, it is characterized in that：
(1) is 150~180 parts of sodium chloride to addition mass parts in the container with agitator and mass parts are 500~600
The distilled water of part, opens stirring, after sodium to be chlorinated is completely dissolved, stops stirring, is made sodium chloride solution；Take the sodium chloride being made
The 10% of solution quality, adds the palladium bichloride that mass parts are 2~6 parts, and stirring is completely dissolved to palladium bichloride, is made A liquid；
(2) be added to two hydrated stannous chlorides that mass parts are 100~300 parts in the remaining sodium chloride solution being made by, then
The reducing agent that mass parts are 0.5~2 part is added, stirring is completely dissolved to two hydrated stannous chlorides, is made B liquid；
(3) at a temperature of 27~30 DEG C, A liquid is slowly added into B liquid under the ul-trasonic irradiation of 550KHz, to be mixed molten
After liquid is changed into brownish black, continues ultrasonic wave and disperse 10 minutes, be eventually adding three hydrated stannic acid sodium and matter that mass parts are 4~8 parts
Amount part is 20~30 parts of additive, and ultrasonic disperse is allowed to be completely dissolved, and is warming up to 45~60 DEG C, cures 3~5 hours, obtains final product
Printed wiring board electroless copper activating solution；
Wherein, described reducing agent is 3-methoxy-4-hydroxybenzaldehyde, 3- hydroxyls -4-methoxybenzaldehyde, 4- methoxyl group water
Any one in poplar aldehyde, syringaldehyde；Described additive is urea or thiocarbamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410343987.7A CN104152874B (en) | 2014-07-20 | 2014-07-20 | A kind of printed wiring board electroless copper activating solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410343987.7A CN104152874B (en) | 2014-07-20 | 2014-07-20 | A kind of printed wiring board electroless copper activating solution |
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| CN104152874A CN104152874A (en) | 2014-11-19 |
| CN104152874B true CN104152874B (en) | 2017-06-09 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106149018A (en) * | 2016-08-09 | 2016-11-23 | 安徽广德威正光电科技有限公司 | A kind of process for pcb board electro-coppering |
| CN106591809A (en) * | 2016-12-26 | 2017-04-26 | 长沙理工大学 | Low-concentration colloid palladium activation solution for printed circuit board electroless copper |
| CN109023316A (en) * | 2018-07-31 | 2018-12-18 | 广东利尔化学有限公司 | A kind of circuit board activation solution and activation method thereof |
| CN113151812B (en) * | 2021-04-20 | 2022-10-11 | 广东工业大学 | A kind of tin activation solution and its preparation method and chemical nickel plating method |
| CN117385345A (en) * | 2023-10-17 | 2024-01-12 | 江苏贺鸿电子有限公司 | Preparation method and application of electroless nickel gold activator |
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|---|---|---|---|---|
| US4933010A (en) * | 1988-01-12 | 1990-06-12 | Eric F. Harnden | Sensitizing activator composition for chemical plating |
| CN101928937A (en) * | 2009-06-22 | 2010-12-29 | 比亚迪股份有限公司 | Colloid palladium activation solution, preparation method thereof and non-metal surface activation method |
| CN102321878A (en) * | 2011-08-29 | 2012-01-18 | 深圳市化讯应用材料有限公司 | Surface activation method for nonmetal material |
| CN102677026A (en) * | 2012-05-25 | 2012-09-19 | 长沙理工大学 | Preparation method of colloidal palladium |
| CN102912324A (en) * | 2012-10-25 | 2013-02-06 | 南京大地冷冻食品有限公司 | High-stability palladium catalyst concentrated solution and preparation method thereof |
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2014
- 2014-07-20 CN CN201410343987.7A patent/CN104152874B/en active Active
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|---|---|---|---|---|
| US4933010A (en) * | 1988-01-12 | 1990-06-12 | Eric F. Harnden | Sensitizing activator composition for chemical plating |
| CN101928937A (en) * | 2009-06-22 | 2010-12-29 | 比亚迪股份有限公司 | Colloid palladium activation solution, preparation method thereof and non-metal surface activation method |
| CN102321878A (en) * | 2011-08-29 | 2012-01-18 | 深圳市化讯应用材料有限公司 | Surface activation method for nonmetal material |
| CN102677026A (en) * | 2012-05-25 | 2012-09-19 | 长沙理工大学 | Preparation method of colloidal palladium |
| CN102912324A (en) * | 2012-10-25 | 2013-02-06 | 南京大地冷冻食品有限公司 | High-stability palladium catalyst concentrated solution and preparation method thereof |
Non-Patent Citations (1)
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Denomination of invention: An activation solution for electroless copper plating on printed circuit boards Granted publication date: 20170609 Pledgee: Postal Savings Bank of China Limited Zhuhai Gongbei Branch Pledgor: Zhuhai Weizhihua New Materials Co.,Ltd. Registration number: Y2024980011865 |