CN104928659A - Chemical nickel-plating palladium alloy plating solution and technology - Google Patents
Chemical nickel-plating palladium alloy plating solution and technology Download PDFInfo
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- CN104928659A CN104928659A CN201410715328.1A CN201410715328A CN104928659A CN 104928659 A CN104928659 A CN 104928659A CN 201410715328 A CN201410715328 A CN 201410715328A CN 104928659 A CN104928659 A CN 104928659A
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Abstract
The invention discloses a chemical nickel-plating palladium alloy plating solution and technology. The chemical nickel-plating palladium alloy plating solution is characterized by comprising 0.1g/L to 25g/L of nickel salt, 0.1g/L to 5g/L of palladium salt, 5g/L to 30g/L of a reducing agent, 5g/L to 40g/L of a complexing agent, 1mg/L to 50mg/L of a stabilizing agent and 5g/L to 30g/L of a buffer agent. The proportion of the nickel salt and the palladium salt in the plating solution is adjusted, and therefore the composition proportion of nickel and palladium in the alloy can be changed; and alloy coatings with different palladium contents are obtained, and the palladium contents are adjustable within the range of 1wt% to 90wt%.
Description
Technical field
The present invention relates to surperficial plating technique, more specifically a kind of electroless nickel plating palldium alloy plating solution and technique.
Background technology
The feature of Ni-Pd alloy is high corrosion stability, and weldability is good, wear-resisting, hardness is high, conduction resistance is little.Owing to having these characteristics, Ni-Pd alloy layer can be used as the alternative techniques of PCB surface layer gold, or as the substrate of the hard golden membranous layer of micro-electromechanical device, also can be used as the diffusion impervious layer of metallic surface in electronics and electro-optical system.
Patent CN 102098880B provides a kind of technology of electronickelling palldium alloy.For electroplating technology, electroless plating technology equipment is simpler, does not need the anode of specific installation and costliness, more easily realizes the plated nickel palldium alloy on the part of complex contour.
Summary of the invention
Object of the present invention is exactly deficiency in order to solve prior art and a kind of chemical nickel plating palldium alloy plating solution that can adjust the alloy layer of nickel palladium content according to demand provided.
Another object of the present invention is to provide a kind of chemical nickel plating palldium alloy technique.
The present invention adopts following technical solution to realize above-mentioned purpose: a kind of chemical nickel plating palldium alloy plating solution, is characterized in that, plating solution raw materials composition comprises:
Further illustrating as such scheme, described nickel salt is: the one in nickelous chloride, single nickel salt, nickelous nitrate.
Described palladium salt is: the one in Palladous chloride, palladous sulfate, dichloro four ammino palladium.
Described reductive agent is: the one in formate, hypophosphite, hydrazine hydrate, sodium borohydride.
Described complexing agent comprises: the nickel ion complexing agents such as oxysuccinic acid, citric acid, succsinic acid, lactic acid, propionic acid, oxyacetic acid, and the palladium ion complexing agent such as ammonia, trolamine, glycine, EDTA, quadrol.
Described stablizer is: one or more in Bismuth trinitrate, thiocarbamide, Sulfothiorine, UPS, potassiumiodide.
Described pH buffer reagent is: one or more in Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, boric acid, borax, sodium carbonate.
A kind of chemical nickel plating palldium alloy technique, it is characterized in that, in plating process, coating bath temperature controls at 60 ~ 80 DEG C, and pH value controls 4.5 ~ 8.5, and alr mode both also can use pneumatic blending by mechanical stirring; Copper surface chemical nickel plating palldium alloy processing step is: oil removing → microetch → activation → plating, all uses pure water rinsing between every step; This technique is not only applicable to Copper base material, can be used for the material surface such as iron, nickel plating equally.
The beneficial effect that the present invention adopts above-mentioned technical solution to reach is:
The present invention can adjust the alloy layer that nickel salt and the ratio of palladium salt obtain different nickel palladium content according to demand, the coating composition using different reductive agent to obtain is also different, that such as use that hydrazine hydrate obtains is purer Ni-Pd, and that use sodium hypophosphite to obtain as reductive agent is Ni-Pd-P.
Accompanying drawing explanation
Fig. 1 is the coating microscopic appearance figure of embodiment 2;
Fig. 2 is scanning spectrogram sample being carried out to EDS test of embodiment 2;
Fig. 3 is the coating microscopic appearance figure of embodiment 3;
Fig. 4 is scanning spectrogram sample being carried out to EDS test of embodiment 3.
Embodiment
Below in conjunction with specific embodiment, present invention process is described in detail.
A kind of chemical nickel plating palldium alloy of the present invention plating solution, plating solution raw materials composition comprises:
Plating solution forms described nickel salt, palladium salt is water-soluble inorganic salt.In plating solution, the ratio of nickel ion and palladium ion is the most important factor determining that coating forms, the content direct proportionality of nickel ion, palladium ion in the content of nickel, palladium and plating solution in coating.Adjustment nickel salt, palladium salt ratio in the plating solution, can change the proportion of composing of nickel palladium in alloy, obtain the alloy layer of different palladium content, palladium content is adjustable within the scope of 1wt% ~ 90wt%.As in following embodiment 1 ~ 3, the amount ratio of nickel salt and palladium salt reduces gradually, and in gained coating, the ratio of nickel element reduces equally gradually.Nickel salt consumption is at 0.1 ~ 25g/L, and palladium salt consumption is at 0.1 ~ 5g/L.How many consumptions of metal-salt not only can affect coating composition, and also have considerable influence to bath stability and plating speed, consumption is too low simultaneously, and plating speed can not meet Production requirement, and consumption is too high, easily causes plating solution to decompose.
Described reductive agent is the one in formate, hypophosphite, hydrazine hydrate, sodium borohydride.The selection of reductive agent can affect coating composition to a certain extent.As selected sodium hypophosphite as reductive agent in following embodiment 1 ~ 3, then what obtain is Ni-Pd-P coating.If sodium borohydride is selected, B element of easily adulterating in coating same.The reductive agents such as hydrazine hydrate can prepare purer Ni-Pd alloy layer.In preparation plating solution process, generally reductive agent is placed on last interpolation, in order to avoid cause plating solution to decompose.The consumption of reductive agent controls at 5 ~ 30g/L.
Complexing agent and metallic ion coordination complexing, ensure nickel, palladium ion stable existence in the plating solution, so the choosing of complexing agent then needs to comprise nickel ion complexing agent and palladium ion complexing agent.Nickel ion complexing agent comprises: oxysuccinic acid, citric acid, succsinic acid, lactic acid, propionic acid, oxyacetic acid etc., and ionic complexing agent comprises ammonia, trolamine, glycine, EDTA, quadrol etc.Amount of complex and metal ion consumption are adaptive, can meet little over amount than complexing ion needed for the whole metal ion of complexing.The total consumption of complexing agent of the present invention is at 5 ~ 40g/L.
Stablizer is selected to be one or more in Bismuth trinitrate, thiocarbamide, Sulfothiorine, UPS, potassiumiodide.The consumption of stablizer is at 1 ~ 50mg/L.Stabilizing agent dosage is too much unsuitable, and excessive stablizer can have a strong impact on plating solution activity, causes problems such as stopping plating, not plating.
Described pH buffer reagent is one or more in Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, boric acid, borax, sodium carbonate.Concrete chooses according to required pH buffering range, between pH 4.5 ~ 7.0, selects SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic etc. proper, if between pH7.0 ~ 8.5, selects borax, sodium carbonate etc. comparatively suitable.Buffer reagent consumption is at 5 ~ 30g/L.
Plating technology: coating bath temperature controls at 60 ~ 80 DEG C, and pH value controls 4.5 ~ 8.5, alr mode both also can use pneumatic blending by mechanical stirring.The present invention is not only applicable to Copper base material, can be used for the material surface such as iron, nickel plating equally.Copper surface chemical nickel plating palldium alloy processing step is: oil removing → microetch → activation → plating, all uses pure water rinsing between every step.
Embodiment 1
Plating solution forms:
Condition controls:
Temperature 60 C, pH 7.0, alr mode: pneumatic blending.
Operating process:
Copper base material → oil removing → washing → microetch → washing → activation → washing → plating.
Degreasing fluid used is acid deoiling liquid, and activation solution is ionic palladium activation solution.
EDS test is carried out to sample, the nickeliferous 77wt% of prepared coating, containing palladium 10%, phosphorous 13%.
Embodiment 2
Plating solution forms:
Condition controls:
Temperature 70 C, pH 6.0, alr mode: pneumatic blending;
Operating process is with embodiment 1.
Gained coating microscopic appearance as Fig. 1, and carries out EDS test to sample, scans spectrogram as Fig. 2, the nickeliferous 70wt% of coating, containing palladium 18%, and phosphorous 12%.
Embodiment 3
Plating solution forms:
Condition controls:
Temperature 75 DEG C, pH 8.0, alr mode: pneumatic blending;
Operating process is with embodiment 1.
Gained coating microscopic appearance as Fig. 3, and carries out EDS test to sample, and scanning spectrogram, as Fig. 4, prepares the nickeliferous 33wt% of coating, containing palladium 56%, and phosphorous 11%.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (8)
1. a chemical nickel plating palldium alloy plating solution, is characterized in that, plating solution raw materials composition comprises:
2. a kind of chemical nickel plating palldium alloy plating solution according to claim 1, it is characterized in that, described nickel salt is the one in nickelous chloride, single nickel salt, nickelous nitrate.
3. a kind of chemical nickel plating palldium alloy plating solution according to claim 1, is characterized in that, described palladium salt is the one in Palladous chloride, palladous sulfate, dichloro four ammino palladium.
4. a kind of chemical nickel plating palldium alloy plating solution according to claim 1, it is characterized in that, described reductive agent is the one in formate, hypophosphite, hydrazine hydrate, sodium borohydride.
5. a kind of chemical nickel plating palldium alloy plating solution according to claim 1, it is characterized in that, described complexing agent comprises the nickel ion complexing agents such as oxysuccinic acid, citric acid, succsinic acid, lactic acid, propionic acid, oxyacetic acid, and the palladium ion complexing agent such as ammonia, trolamine, glycine, EDTA, quadrol.
6. a kind of chemical nickel plating palldium alloy plating solution according to claim 1, is characterized in that, described stablizer is one or more in Bismuth trinitrate, thiocarbamide, Sulfothiorine, UPS, potassiumiodide.
7. a kind of chemical nickel plating palldium alloy plating solution according to claim 1, is characterized in that, described pH buffer reagent is one or more in Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, boric acid, borax, sodium carbonate.
8. the chemical nickel plating palldium alloy technique as described in claim 1-7 any one, is characterized in that, coating bath temperature controls at 60 ~ 80 DEG C in plating process, and pH value controls 4.5 ~ 8.5, and alr mode both also can use pneumatic blending by mechanical stirring; Copper surface chemical nickel plating palldium alloy processing step is: oil removing → microetch → activation → plating, all uses pure water rinsing between every step.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106480439A (en) * | 2016-11-29 | 2017-03-08 | 江苏澳光电子有限公司 | A kind of chemical nickel plating palldium alloy crosses liquid and its application |
| CN108336370A (en) * | 2018-02-02 | 2018-07-27 | 浙江金康铜业有限公司 | A kind of multidimensional structure copper alloy electrode |
| CN110643985A (en) * | 2019-08-24 | 2020-01-03 | 东莞市斯坦得电子材料有限公司 | Chemical palladium plating process for chemical nickel-palladium-gold plating production line of printed circuit board |
| 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 |
| CN113005439A (en) * | 2021-02-24 | 2021-06-22 | 深圳市创智成功科技有限公司 | Chemical palladium plating process for electronic packaging carrier plate |
| CN114941135A (en) * | 2022-05-30 | 2022-08-26 | 金川集团镍盐有限公司 | Application of economic and environment-friendly chemical nickel plating stabilizer |
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| DE2014406A1 (en) * | 1970-03-25 | 1971-12-30 | Kleinspor & Co Ind Export Kg | Bath for chemical deposition of palladium alloys - or alloys of other noble metals with nickel and/or cobalt |
| CN101579632A (en) * | 2009-03-24 | 2009-11-18 | 华东师范大学 | Nickel palladium/ silicon microchannel catalyst and application thereof on preparing electrode of integratable direct methanol fuel cell |
| WO2014040662A1 (en) * | 2012-09-11 | 2014-03-20 | Kompoferm Gmbh | Aerobic treatment device for stackable biomass, and method for treating stackable biomass |
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Patent Citations (3)
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| DE2014406A1 (en) * | 1970-03-25 | 1971-12-30 | Kleinspor & Co Ind Export Kg | Bath for chemical deposition of palladium alloys - or alloys of other noble metals with nickel and/or cobalt |
| CN101579632A (en) * | 2009-03-24 | 2009-11-18 | 华东师范大学 | Nickel palladium/ silicon microchannel catalyst and application thereof on preparing electrode of integratable direct methanol fuel cell |
| WO2014040662A1 (en) * | 2012-09-11 | 2014-03-20 | Kompoferm Gmbh | Aerobic treatment device for stackable biomass, and method for treating stackable biomass |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106480439A (en) * | 2016-11-29 | 2017-03-08 | 江苏澳光电子有限公司 | A kind of chemical nickel plating palldium alloy crosses liquid and its application |
| CN108336370A (en) * | 2018-02-02 | 2018-07-27 | 浙江金康铜业有限公司 | A kind of multidimensional structure copper alloy electrode |
| CN108336370B (en) * | 2018-02-02 | 2020-05-05 | 浙江金康铜业有限公司 | Multidimensional structure copper alloy electrode |
| 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 |
| CN110643985A (en) * | 2019-08-24 | 2020-01-03 | 东莞市斯坦得电子材料有限公司 | Chemical palladium plating process for chemical nickel-palladium-gold plating production line of printed circuit board |
| CN113005439A (en) * | 2021-02-24 | 2021-06-22 | 深圳市创智成功科技有限公司 | Chemical palladium plating process for electronic packaging carrier plate |
| CN114941135A (en) * | 2022-05-30 | 2022-08-26 | 金川集团镍盐有限公司 | Application of economic and environment-friendly chemical nickel plating stabilizer |
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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 Applicant after: Guangdong Zhuo Environmental Protection Technology Co., Ltd. Address before: Dali Town, Nanhai District Changhong Ling Industrial Zone 528200 Guangdong city of Foshan Province Applicant before: Guangdong Zhizhuo Precision Metal Technology Co., Ltd. |
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