CN104561943B - Chemical nickel-palladium alloy plating process for circuit boards - Google Patents
Chemical nickel-palladium alloy plating process for circuit boards Download PDFInfo
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- CN104561943B CN104561943B CN201410830802.5A CN201410830802A CN104561943B CN 104561943 B CN104561943 B CN 104561943B CN 201410830802 A CN201410830802 A CN 201410830802A CN 104561943 B CN104561943 B CN 104561943B
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- nickel
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- plating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
Abstract
The invention discloses a chemical nickel-palladium alloy plating process for circuit boards. The chemical nickel-palladium alloy plating process is characterized by comprising the following steps: (1) degreasing: placing a circuit board in an acidic degreasing agent to remove greasy dirt and fingerprints on the surface of the circuit board; (2) microetching: placing the degreased circuit board in microetching liquid to slightly etch the copper surface; (3) activation: placing the micro-etched circuit board in a palladium activating liquid to be activated, so that a layer of activated palladium is deposited on the surface of the circuit board; (4) chemical nickel plating: placing the activated circuit board in nickel plating liquid so as to deposit a layer of nickel on the copper surface; (5) microetching: placing the circuit board plated with nickel in acid liquid so as to slightly etch the nickel surface; (6) activation: placing the micro-etched circuit board in the palladium activating liquid to be activated, so that a layer of activated palladium is deposited on the surface of the circuit board; (7) chemical nickel-palladium plating: placing the activated circuit board in nickel-palladium alloy plating liquid to be plated, and depositing a nickel-palladium alloy plated layer on the nickel surface; (8) washing and drying the circuit board: washing the board surface to remove medicine liquids in former preparation processes, and drying. Through the adoption of the chemical nickel-palladium alloy plating process disclosed by the invention, the production cost can be reduced effectively, and the application of the surface treatment process of circuit boards is facilitated.
Description
Technical field
The present invention relates to PCB surface handling process, is a kind of chemical nickel plating palldium alloy technique for wiring board.
Background technology
At present, the surface treatment being suitable on wiring board mainly has：1st, organic solder protective agent；2nd, replacement ag plating；3、
Immersion tin；4th, chemical nickel/immersion gold plating；5th, chemical NiPdAu (Ni/Pd/Au) technique.Front 4 kinds of surface treatments are all individually present
Certain defect, in recent years popular chemical NiPdAu technique, extensive because coating has good wear resistance and corrosion resistance and solderable row
Using, but using the noble metal Au of high price, and technique slightly complicated.It is therefore desirable to providing a kind of for PCB surface gold
The alternative techniques of layer.
The content of the invention
The purpose of the present invention is exactly that the one kind provided to solve the deficiency of prior art can effectively reduce production cost,
Be conducive to the chemical nickel plating palldium alloy technique for wiring board of the application of PCB surface handling process.
The present invention is to realize above-mentioned purpose using following technical solution：A kind of chemical nickel plating palladium for wiring board
Alloying technology, it is characterised in that it comprises the steps：
(1), oil removing：Product is put in acid deoiling agent, the greasy dirt and fingerprint of plate face is removed；
(2), microetch：Product is put into into micro-corrosion liquid, erosion is slightly stung on copper surface, to obtain fresh surface, improve follow-up
Binding force of cladding material；
(3), activate：Product is put in palladium activating solution and is activated, make product surface deposit one layer of activation palladium, to make follow-upization
Learn the catalysis medium of nickel；
(4), chemical nickel：Product is put in nickel-plating liquid, on copper surface one layer of nickel is deposited；
(5), microetch：Product is placed in acid solution, nickel surface is slightly stung erosion；
(6), activate：Product is put in palladium activating solution, makes product surface deposit one layer of activation palladium, to make subsequent chemistry nickel
The catalysis medium of palldium alloy；
(7), chemical nickel plating palladium：Product is put into into plating in Ni-Pd alloy plating solution, in nickel surface one layer of Ni-Pd alloy is deposited
Coating；
(8), washing drying：The front processing procedure liquid medicine of cleaning plate face residual, drying.
Further illustrating as such scheme, micro-corrosion liquid sodium peroxydisulfate containing 50-200g/L in described step (2),
The 20-100ml/L concentrated sulfuric acids.
Acid solution in described step (5) is one kind of sulfuric acid, nitric acid, hydrochloric acid.
Described palladium activating solution 1-50ml/L containing the concentrated sulfuric acid, ionic palladium 10-100ppm, the temperature of activating solution is room temperature.
Described nickel-plating liquid active principle content be 0.1-3mol/L hypophosphorous acid roots, 15-100g/L nickel salts, nickel plating liquid temp
70-90 DEG C, pH value is 4.5-6.8.
The component of described Ni-Pd alloy plating solution include 0.1-5g/L palladium salts, 2-60g/L nickel salts, 10-65g/L reducing agents,
20-100g/L complexing agents, 1-10mg/L stabilizers, 10-60g/L buffers, 10-300mg/L brighteners, wherein palladium salt are acetic acid
Palladium, palladium sulfate, palladium bichloride, one kind of palladium nitrate, nickel salt is one kind of nickel sulfate, nickel chloride, nickel acetate, nickel nitrate, reducing agent
It is one kind of borine, hydrazine, hypophosphite, sodium borohydride, complexing agent is mainly citric acid, lactic acid, ammoniacal liquor, triethanolamine, sweet
Propylhomoserin, EDTA, ethylenediamine, the combination that one or more of 8-hydroxyquinoline plasma complexing agent, stabilizer selects thiocarbamide, thio sulphur
One or more in sour sodium, KI, buffer has sodium acetate, ammoniacal liquor-ammonium chloride, Glycine-NaOH, sodium carbonate,
Brightener is one or more combination of benzoic sulfimide sodium, sodium vinyl sulfonate, OP-10, ALS etc.；Nickel
The temperature of palldium alloy plating solution is 50-85 DEG C, and pH range is 7.1-11.
The present invention is using the above-mentioned technical solution beneficial effect to be reached：
, using Ni-Pd alloy coating as a kind of cash equivalent coating, solderability is good, wear-and corrosion-resistant, hardness high, and hole for the present invention
Gap rate is low, while performance is ensured, reduces manufacturing cost.
Description of the drawings
Fig. 1 is the sample test surface of position microscopic appearance SEM figures of the present invention；
Fig. 2 is EDS1 EDAX results in Fig. 1；
Fig. 3 is EDS2 EDAX results in Fig. 1；
Fig. 4 is the sample test surface of position microscopic appearance SEM figures of the present invention；
Fig. 5 is EDS1 EDAX results in Fig. 4；
Fig. 6 is EDS2 EDAX results in Fig. 4.
Specific embodiment
Specific embodiments of the present invention are described in further detail below in conjunction with specific embodiment.
The present invention is a kind of chemical nickel plating palldium alloy technique for wiring board, and it comprises the steps：
Step 1：Oil removing：During product to be put into the acid deoiling agent for being furnished with 80-150ml/L, with 30-40 DEG C of Temperature Treatment
4-6min, to remove the plate face such as the greasy dirt and fingerprint pollution of plate face；
Step 2：Microetch：Product is put into and is furnished with 50-200g/L sodium peroxydisulfates, the mixed solution of the 20-100ml/L concentrated sulfuric acids
Middle process 1-2min, by copper surface erosion is slightly stung, and to obtain fresh surface, improves subsequent plating layer adhesion；
Step 3：Activation：Product is put into and is furnished with concentrated sulfuric acid 1-50ml/L, the mixed solution of ionic palladium 10-100ppm living
Change 3-5min, make product surface deposit one layer of activation palladium, to make the catalysis medium of subsequent chemistry nickel；
Step 4：Chemical nickel：Product is put into into plating in nickel plating solution, PH=4.5-6.8 is controlled, in 70-90 DEG C of temperature
Lower process 15-30min, on copper surface one layer of nickel is deposited；
Step 5：Microetch：Product is put in 10% hydrochloric acid, nickel surface is slightly stung erosion；
Step 6：Palladium is activated：Product is put into and is furnished with the mixed solution of concentrated sulfuric acid 1-50ml/L, palladium salt 10-100ppm living
Change 3-5min, make product surface deposit one layer of activation palladium, to make the catalysis medium of subsequent chemistry Ni-Pd alloy；
Step 7：Chemical nickel palladium：Product is put into into plating in alloy electroplating bath, PH=7.1-11 is controlled, in 50-85 DEG C of temperature
Degree is lower to process 15-30min, and in nickel surface one layer of Ni-Pd alloy coating is deposited；
Step 8：Washing drying：The front processing procedure liquid medicine of thoroughly cleaning plate face residual, then dries.
Embodiment 1
The present embodiment is, with copper sheet as base material, to be tested by the step；Wherein, the Ni-Pd alloy that step 7 is adopted
The composition of plating solution includes：
SEM tests are carried out to sample, gained coating microscopic appearance such as Fig. 1, EDS test gained coating and scanning spectra are as schemed
2 and Fig. 3.
Embodiment 3
The present embodiment is, with copper sheet as base material, to be tested by above-mentioned steps；Wherein, the Ni-Pd alloy that step 7 is adopted
The composition of plating solution includes：
SEM tests are carried out to sample, gained coating microscopic appearance such as Fig. 4, EDS test gained coating and scanning spectra are as schemed
5 and Fig. 6.
Above-described is only the preferred embodiment of the present invention, it is noted that for one of ordinary skill in the art
For, without departing from the concept of the premise of the invention, some deformations and improvement can also be made, these belong to the present invention
Protection domain.
Claims (5)
1. a kind of chemical nickel plating palldium alloy technique for wiring board, it is characterised in that it comprises the steps：
(1), oil removing：Product is put in acid deoiling agent, the greasy dirt and fingerprint of plate face is removed；
(2), microetch：Product is put into into micro-corrosion liquid, erosion is slightly stung on copper surface；
(3), activate：Product is put in palladium activating solution and is activated, make product surface deposit one layer of activation palladium, to make subsequent chemistry nickel
Catalysis medium；
(4), chemical nickel：Product is put in nickel-plating liquid, on copper surface one layer of nickel is deposited；
(5), microetch：Product is placed in acid solution, nickel surface is slightly stung erosion；
(6), activate：Product is put in palladium activating solution, makes product surface deposit one layer of activation palladium, to make the conjunction of subsequent chemistry nickel palladium
The catalysis medium of gold；
(7), chemical nickel plating palladium：Product is put into into plating in Ni-Pd alloy plating solution, in nickel surface one layer of Ni-Pd alloy coating is deposited；
(8), washing drying：The front processing procedure liquid medicine of cleaning plate face residual, drying；
The component of described Ni-Pd alloy plating solution includes 0.1-5g/L palladium salts, 2-60g/L nickel salts, 10-65g/L reducing agents, 20-
100g/L complexing agents, 1-10mg/L stabilizers, 10-60g/L buffers, 10-300mg/L brighteners, wherein palladium salt be palladium,
Palladium sulfate, palladium bichloride, one kind of palladium nitrate, nickel salt is one kind of nickel sulfate, nickel chloride, nickel acetate, nickel nitrate, and reducing agent is boron
Alkane, hydrazine, hypophosphite, one kind of sodium borohydride, complexing agent be citric acid, lactic acid, ammoniacal liquor, triethanolamine, glycine,
EDTA, ethylenediamine, one or more of 8-hydroxyquinoline of combination, stabilizer is from thiocarbamide, sodium thiosulfate, KI
One or more, buffer has sodium acetate, ammoniacal liquor-ammonium chloride, Glycine-NaOH, sodium carbonate, and brightener is adjacent sulphonyl benzene
Acid imide sodium, sodium vinyl sulfonate, OP-10, one or more combination of ALS；The temperature of Ni-Pd alloy plating solution is
50-85 DEG C, pH range is 7.1-11.
2. the chemical nickel plating palldium alloy technique for wiring board according to claim 1, it is characterised in that described step
(2) the micro-corrosion liquid sodium peroxydisulfate containing 50-200g/L, the 20-100ml/L concentrated sulfuric acids in.
3. the chemical nickel plating palldium alloy technique for wiring board according to claim 1, it is characterised in that described step
(5) acid solution in is one kind of sulfuric acid, nitric acid, hydrochloric acid.
4. the chemical nickel plating palldium alloy technique for wiring board according to claim 1, it is characterised in that described palladium is lived
Change liquid 1-50ml/L containing the concentrated sulfuric acid, ionic palladium 10-100ppm, the temperature of activating solution is room temperature.
5. the chemical nickel plating palldium alloy technique for wiring board according to claim 1, it is characterised in that described nickel plating
Liquid active principle content is 0.1-3mol/L hypophosphorous acid roots, 15-100g/L nickel salts, and 70-90 DEG C of nickel plating liquid temp, pH value is 4.5-
6.8。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410830802.5A CN104561943B (en) | 2014-12-27 | 2014-12-27 | Chemical nickel-palladium alloy plating process for circuit boards |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410830802.5A CN104561943B (en) | 2014-12-27 | 2014-12-27 | Chemical nickel-palladium alloy plating process for circuit boards |
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| CN104561943A CN104561943A (en) | 2015-04-29 |
| CN104561943B true CN104561943B (en) | 2017-05-10 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104928658B (en) * | 2015-05-13 | 2017-10-17 | 电子科技大学 | A kind of method that activation PCB circuit surfaces realize chemical nickel plating |
| CN106540282B (en) * | 2015-09-16 | 2019-09-24 | 天津赛德生物制药有限公司 | A kind of preparation method of -103 sealed seed source source core of palladium |
| CN109112506B (en) * | 2018-09-18 | 2020-09-04 | 宏维科技（深圳）有限公司 | Activation inhibitor for production of fine line products and preparation method thereof |
| CN109468617A (en) * | 2018-11-30 | 2019-03-15 | 浙江长兴电子厂有限公司 | A kind of local electroplating nickel gold process |
| WO2020129095A1 (en) * | 2018-12-20 | 2020-06-25 | Top Finish 2002 S.R.L. | Galvanic bath for making a corrosion- and oxidation-resistant palladium and nickel alloy-based plating, preparation and use thereof |
| CN110484900A (en) * | 2019-09-27 | 2019-11-22 | 广州皓悦新材料科技有限公司 | A kind of Novel horizontal electroless copper plating ionic palladium activating solution |
| CN110629249B (en) * | 2019-09-29 | 2021-07-13 | 济南大学 | Method for preparing high-activity hydrogen evolution electrode by surface chemical plating-pore forming of flocked steel plate |
| CN110724940A (en) * | 2019-10-24 | 2020-01-24 | 中电国基南方集团有限公司 | Chemical nickel-palladium-gold plating process method for low-temperature co-fired ceramic substrate |
| CN112609173A (en) * | 2020-12-10 | 2021-04-06 | 安徽环瑞电热器材有限公司 | Corrosion-resistant material and manufacturing method thereof |
| CN114100536A (en) * | 2021-11-26 | 2022-03-01 | 珠海市钯金电子科技有限公司 | Composite microsphere particles and method for depositing nickel, palladium and gold on circuit board by using same |
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| CN101525744B (en) * | 2009-04-27 | 2011-12-21 | 深圳市创智成功科技有限公司 | Superficial treatment method of printed wiring board |
| CN102817056B (en) * | 2012-08-15 | 2015-03-25 | 中山品高电子材料有限公司 | Electroplating process for lead wire frame palladium-nickel alloy plating layer |
| CN102912329A (en) * | 2012-11-15 | 2013-02-06 | 苏州正信电子科技有限公司 | Chemical nickel and palladium plating process used for circuit boards |
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Effective date of registration: 20170616 Address after: 528225, Foshan District, Guangdong City, Nanhai District, lion Town, Changhong Ridge Industrial Park, West Changxin Road, 3 (office building) two floor, B District Patentee after: Guangdong Zhuo Environmental Protection Technology Co., Ltd. Address before: Dali Town, Nanhai District Changhong Ling Industrial Zone 528200 Guangdong city of Foshan Province Patentee before: Guangdong Zhizhuo Precision Metal Technology Co., Ltd. |