CN104561961A - Chemical cobalt-nickel plating alloy liquid and process - Google Patents
Chemical cobalt-nickel plating alloy liquid and process Download PDFInfo
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- CN104561961A CN104561961A CN201410835758.7A CN201410835758A CN104561961A CN 104561961 A CN104561961 A CN 104561961A CN 201410835758 A CN201410835758 A CN 201410835758A CN 104561961 A CN104561961 A CN 104561961A
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Abstract
The invention discloses a chemical cobalt-nickel plating alloy liquid and a process. The chemical cobalt-nickel plating alloy liquid is characterized by comprising the following raw materials: 0.1-40g/L of a nickel salt, 0.1-40g/L of a cobalt salt, 5-30g/L of a reducing agent, 10-60g/L of a complexing agent, 1-50mg/L of a stabilizing agent and 5-30g/L of a buffer agent. By adjustment of the proportions of the nickel salt and the cobalt salt in the plating liquid, the composition proportions of cobalt and nickel in an alloy can be changed, alloy plated layers with different cobalt contents can be obtained, and the cobalt content can be adjusted within 1-100wt%.
Description
Technical field
The present invention relates to surperficial plating technique, more specifically a kind of electroless plating cobalt-nickel alloy plating solution and technique.
Background technology
Co-Ni alloy has excellent mechanical property and electromagnetic performance, and along with the difference of Co content in alloy, the performance of alloy also has very large difference.When Co content is below 40%, alloy layer stress is little and even, and tight, has higher solidity to corrosion, hardness and good wear resistance, and its color brightness is good, attractive in appearance.Therefore the Cobalt-Nickel Alloy Electroplating Films of low cobalt content can do decorative coating and functional coating, is widely used in wrist-watch element and part anti-corrosion, wear-resisting in chemical industry, medicine industry; When Co content is greater than 70%, coating has excellent high-temperature behavior and electromagnetic performance, uses under being used to the hot environments such as the interior coating of hot-work die and continuous cast mold.In addition high cobalt alloy also has high magnetic coercive force, is widely used in the fields such as electronics, computer and space industry.
The cobalt-nickel alloy that present market uses is many obtains cobalt-nickel alloy by galvanic deposit or physics forging processing.For electroplating technology, electroless plating technology equipment is simpler, does not need the anode of specific installation and costliness, more easily realizes the plating cobalt-nickel alloy on the part of complex contour.Containing a small amount of phosphorus in cobalt-nickel alloy, its corrosion resisting property can be improved further.And conveniently can obtain Co-Ni-P alloy by the method for electroless plating.Believe that electroless cobalt plating nickelalloy technology one is used widely in multiple industry surely.
Summary of the invention
Object of the present invention is exactly electroless plating formula and the technique of a kind of Cobalt-Nickel Alloy Electroplating Films in order to provide.
Another object of the present invention is to provide the adjustable coating of a kind of cobalt-nickel alloy content.
The present invention adopts following technical solution to realize above-mentioned purpose: a kind of electroless cobalt plating nickelalloy 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, nickel sulfamic acid or other water soluble nickel salt.
Described cobalt salt is: the one in cobalt chloride, rose vitriol, thionamic acid cobalt or other water soluble cobaltous salt.
Described reductive agent is: the one in formaldehyde, formic acid, formate, Hypophosporous Acid, 50, hypophosphite, hydrazine hydrate, sodium borohydride.
Described complexing agent comprises: one or more in oxysuccinic acid, citric acid, succsinic acid, lactic acid, propionic acid, oxyacetic acid, ammonia, trolamine, glycine, tartrate, EDTA, quadrol, hydroxycarboxylate, aminocarboxylate and organic phosphonate.
Described stablizer is: one or more in lead salts, stearate, Bismuth trinitrate, thiocarbamide, diphenyl thiourea, Sulfothiorine, UPS, potassiumiodide and rare-earth oxide or muriate.
Described pH buffer reagent is: one or more in Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, boric acid, borax, sodium carbonate, Padil.
A kind of electroless cobalt plating nickelalloy technique, it is characterized in that, in plating process, coating bath temperature controls at 60 ~ 95 DEG C, pH value controls 6 ~ 10, can the workpiece of direct catalysis to reductive agent, surface chemical plating cobalt-nickel alloy processing step is: oil removing → microetch → plating, all uses pure water rinsing between every step; This technique is not only applicable to ironware and iron containing substrates, can be used for the material surface such as copper, nickel plating equally.Also can plating to not possessing the metal of catalytic activity or other material, only need carry out the process of plating front activating.
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 cobalt salt obtain different content of cobalt and nickel according to demand, and the coating using different reductive agent to obtain composition also has difference.
Embodiment
Below in conjunction with specific embodiment, present invention process is described in detail.
A kind of electroless cobalt plating nickelalloy of the present invention plating solution, plating solution raw materials composition comprises:
Plating solution forms described nickel salt, cobalt salt is water-soluble salt.Described nickel salt is the one in nickelous chloride, single nickel salt, nickelous nitrate, nickel sulfamic acid or other water soluble nickel salt.Described cobalt salt is the one in cobalt chloride, rose vitriol, thionamic acid cobalt or other water soluble cobaltous salt.
In plating solution, the ratio of nickel ion and cobalt ion is the most important factor determining that coating forms, the content direct proportionality of nickel ion, cobalt ion in the content of nickel, cobalt and plating solution in coating.Adjustment nickel salt, cobalt salt ratio in the plating solution, can change the proportion of composing of cobalt nickel element in alloy, obtain the alloy layer of different cobalt contents, cobalt contents is adjustable within the scope of 1wt% ~ 100wt%.As in embodiment 1 ~ 3, the consumption of cobalt salt raises gradually, and nickel salt usage ratio reduces, and in gained coating, the ratio of cobalt element improves gradually.Nickel salt consumption is at 0.1 ~ 40g/L, and cobalt salt consumption is at 0.1 ~ 40g/L.
Described reductive agent is the one in formaldehyde, formic acid, formate, Hypophosporous Acid, 50, 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 Co-Ni-P coating.Reductive agent used in amounts will strictly control, and it is slow that reaction at least crossed by reductive agent, and the process time is longer; The excessive then plating solution of reductive agent is unstable.The consumption of reductive agent controls at 5 ~ 30g/L.
Complexing agent and metallic ion coordination complexing, ensure nickel and cobalt ions stable existence in the plating solution, so the choosing of complexing agent then needs to comprise nickel ion complexing agent and cobalt ion complexing agent.Described complexing agent comprise in oxysuccinic acid, citric acid, succsinic acid, lactic acid, propionic acid, oxyacetic acid, ammonia, trolamine, glycine, tartrate, EDTA, quadrol, hydroxycarboxylate, aminocarboxylate and organic phosphonate one or more.Amount of complex is at 10 ~ 60g/L
Described stablizer is one or more in lead salts, stearate, Bismuth trinitrate, thiocarbamide, diphenyl thiourea, Sulfothiorine, UPS, potassiumiodide and rare-earth oxide or muriate.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 the problem of stopping plating, not plating.Add in addition metal or rare earth class stablizer in plating process may doped with rare-earth elements in coating, change is to a certain extent risen to coating performance.
Described pH buffer reagent is one or more in Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, boric acid, borax, sodium carbonate, Padil.Concrete chooses according to required pH buffering range, between pH 6 ~ 8, selects potassium primary phosphate proper, if between pH 8 ~ 10, selects boric acid, Padil etc. comparatively suitable.Buffer reagent consumption is at 5 ~ 30g/L.
Plating technology: coating bath temperature controls at 60 ~ 95 DEG C, and pH value controls 6 ~ 10, ironware or steel part etc. can the workpiece of direct catalysis to reductive agent, and surface chemical plating cobalt-nickel alloy processing step is: oil removing → microetch → plating, all uses pure water rinsing between every step; This technique is not only applicable to ironware and iron containing substrates, can be used for the material surface such as copper, nickel plating equally.The process of plating front activating need be carried out to the metal or other material that do not possess catalytic activity.
Embodiment 1
Plating solution forms:
Condition controls:
Temperature 80 DEG C, pH 8.5, alr mode: pneumatic blending.
EDS test is carried out to sample, the nickeliferous 70wt% of prepared coating, containing cobalt 23%, phosphorous 7%.
Embodiment 2
Plating solution forms:
Condition controls:
Temperature 85 DEG C, pH 9.0, alr mode: pneumatic blending;
EDS test is carried out to sample, the nickeliferous 48wt% of coating, containing cobalt 46%, phosphorous 6%.
Embodiment 3
Plating solution forms:
Condition controls:
Temperature 90 DEG C, pH 8.5, alr mode: pneumatic blending;
EDS test is carried out to sample, prepares the nickeliferous 5wt% of coating, containing cobalt 91%, phosphorous 4%.
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 (9)
1. an electroless cobalt plating nickelalloy plating solution, is characterized in that, plating solution raw materials composition comprises:
2. a kind of electroless cobalt plating nickelalloy plating solution according to claim 1, is characterized in that, described nickel salt is the one in nickelous chloride, single nickel salt, nickelous nitrate, nickel sulfamic acid or other water soluble nickel salt.
3. a kind of electroless cobalt plating nickelalloy plating solution according to claim 1, is characterized in that, described cobalt salt is the one in cobalt chloride, rose vitriol, thionamic acid cobalt or other water soluble cobaltous salt.
4. a kind of electroless cobalt plating nickelalloy plating solution according to claim 1, it is characterized in that, described reductive agent is the one in formaldehyde, formic acid, formate, Hypophosporous Acid, 50, hypophosphite, hydrazine hydrate, sodium borohydride.
5. a kind of electroless cobalt plating nickelalloy plating solution according to claim 1, it is characterized in that, described complexing agent comprise in oxysuccinic acid, citric acid, succsinic acid, lactic acid, propionic acid, oxyacetic acid, ammonia, trolamine, glycine, tartrate, EDTA, quadrol, hydroxycarboxylate, aminocarboxylate and organic phosphonate one or more.
6. a kind of electroless cobalt plating nickelalloy plating solution according to claim 1, it is characterized in that, described stablizer is: one or more in lead salts, stearate, Bismuth trinitrate, thiocarbamide, diphenyl thiourea, Sulfothiorine, UPS, potassiumiodide and rare-earth oxide or muriate.
7. a kind of electroless cobalt plating nickelalloy plating solution according to claim 1, it 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, Padil.
8. the electroless cobalt plating nickelalloy technique as described in claim 1-7 any one, is characterized in that, its processing step is: oil removing → microetch → plating, all uses pure water rinsing between every step; In plating process, coating bath temperature controls at 60 ~ 95 DEG C, and pH value controls 6 ~ 10.
9. electroless cobalt plating nickelalloy technique according to claim 8, is characterized in that, in described processing step, need carry out the process of plating front activating to the metal or other material not possessing catalytic activity.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105002481A (en) * | 2015-07-07 | 2015-10-28 | 苏州华日金菱机械有限公司 | Electroplating solution |
| CN105349973A (en) * | 2015-11-24 | 2016-02-24 | 安徽天思朴超精密模具股份有限公司 | Material combination of high-temperature-resistance electroplating liquid and preparation method and application of high-temperature-resistance electroplating liquid |
| CN107460454A (en) * | 2017-09-20 | 2017-12-12 | 吴国明 | A kind of method of phase-inversion technologies deposition Nanoalloy film layer |
| CN107641801A (en) * | 2017-09-20 | 2018-01-30 | 吴国明 | A kind of inversion of phases smithcraft |
| CN108611626A (en) * | 2018-05-10 | 2018-10-02 | 中山市美仑化工有限公司 | A kind of no ammonia nitrogen chemical nickel treatment process |
| CN109576686A (en) * | 2019-01-11 | 2019-04-05 | 江门市德商科佐科技实业有限公司 | A kind of additive enhancing chemical nickel-plating solution stability |
| CN110158129A (en) * | 2019-05-27 | 2019-08-23 | 广州三孚新材料科技股份有限公司 | Pre- bleeding agent composition, pre- bleeding agent, copper facing preprocess method and cyanide-free copper electroplating method |
| CN110484902A (en) * | 2019-09-23 | 2019-11-22 | 常德力元新材料有限责任公司 | Electroless Ni-Co-P Alloy Plating plating solution |
| CN110565078A (en) * | 2019-07-11 | 2019-12-13 | 中国科学院兰州化学物理研究所 | Method for preparing cobalt-sulfur film on copper surface based on reverse replacement |
| CN110629249A (en) * | 2019-09-29 | 2019-12-31 | 济南大学 | Method for preparing high-activity hydrogen evolution electrode by surface chemical plating-pore forming of flocked steel plate |
| CN111074250A (en) * | 2020-02-13 | 2020-04-28 | 西安交通大学 | High-corrosion-resistance stable chemical nickel plating solution for aluminum alloy surface, and preparation method and application thereof |
| CN111575686A (en) * | 2020-06-11 | 2020-08-25 | 青田永拓金属表面技术处理有限公司 | Wear-resistant corrosion-resistant high-phosphorus plating solution for surface of stainless steel ball valve and wear-resistant corrosion-resistant preparation method |
| CN111962052A (en) * | 2020-08-07 | 2020-11-20 | 浙江集工阀门有限公司 | Composite plating process for nickel-based alloy |
| CN112853415A (en) * | 2020-12-31 | 2021-05-28 | 江门市瑞期精细化学工程有限公司 | Nickel-phosphorus alloy electroplating solution and application thereof |
| CN113463140A (en) * | 2021-06-23 | 2021-10-01 | 灵宝金源朝辉铜业有限公司 | Nickel plating solution and high-corrosion-resistance double-sided thick nickel plating rolled copper foil process |
| CN113774369A (en) * | 2021-08-20 | 2021-12-10 | 张家口原轼新型材料有限公司 | Plating solution and plating process for plating nickel-cobalt-phosphorus alloy on surface of emery and obtained emery and golden steel wire |
| CN114657544A (en) * | 2022-03-24 | 2022-06-24 | 彭州航大新材料有限公司 | Aluminizing cobalt process for inner cavity surface of nickel-based superalloy and cobalt-aluminum infiltration layer |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105002481A (en) * | 2015-07-07 | 2015-10-28 | 苏州华日金菱机械有限公司 | Electroplating solution |
| CN105349973A (en) * | 2015-11-24 | 2016-02-24 | 安徽天思朴超精密模具股份有限公司 | Material combination of high-temperature-resistance electroplating liquid and preparation method and application of high-temperature-resistance electroplating liquid |
| CN105349973B (en) * | 2015-11-24 | 2018-01-30 | 安徽天思朴超精密模具股份有限公司 | The preparation method and application of high temperature resistant electroplate liquid material compositions and high temperature resistant electroplate liquid |
| CN107460454A (en) * | 2017-09-20 | 2017-12-12 | 吴国明 | A kind of method of phase-inversion technologies deposition Nanoalloy film layer |
| CN107641801A (en) * | 2017-09-20 | 2018-01-30 | 吴国明 | A kind of inversion of phases smithcraft |
| CN108611626A (en) * | 2018-05-10 | 2018-10-02 | 中山市美仑化工有限公司 | A kind of no ammonia nitrogen chemical nickel treatment process |
| CN109576686A (en) * | 2019-01-11 | 2019-04-05 | 江门市德商科佐科技实业有限公司 | A kind of additive enhancing chemical nickel-plating solution stability |
| CN110158129A (en) * | 2019-05-27 | 2019-08-23 | 广州三孚新材料科技股份有限公司 | Pre- bleeding agent composition, pre- bleeding agent, copper facing preprocess method and cyanide-free copper electroplating method |
| CN110565078A (en) * | 2019-07-11 | 2019-12-13 | 中国科学院兰州化学物理研究所 | Method for preparing cobalt-sulfur film on copper surface based on reverse replacement |
| CN110484902A (en) * | 2019-09-23 | 2019-11-22 | 常德力元新材料有限责任公司 | Electroless Ni-Co-P Alloy Plating plating solution |
| CN110629249A (en) * | 2019-09-29 | 2019-12-31 | 济南大学 | Method for preparing high-activity hydrogen evolution electrode by surface chemical plating-pore forming of flocked steel plate |
| CN111074250A (en) * | 2020-02-13 | 2020-04-28 | 西安交通大学 | High-corrosion-resistance stable chemical nickel plating solution for aluminum alloy surface, and preparation method and application thereof |
| CN111575686A (en) * | 2020-06-11 | 2020-08-25 | 青田永拓金属表面技术处理有限公司 | Wear-resistant corrosion-resistant high-phosphorus plating solution for surface of stainless steel ball valve and wear-resistant corrosion-resistant preparation method |
| CN111962052A (en) * | 2020-08-07 | 2020-11-20 | 浙江集工阀门有限公司 | Composite plating process for nickel-based alloy |
| CN112853415A (en) * | 2020-12-31 | 2021-05-28 | 江门市瑞期精细化学工程有限公司 | Nickel-phosphorus alloy electroplating solution and application thereof |
| CN113463140A (en) * | 2021-06-23 | 2021-10-01 | 灵宝金源朝辉铜业有限公司 | Nickel plating solution and high-corrosion-resistance double-sided thick nickel plating rolled copper foil process |
| CN113774369A (en) * | 2021-08-20 | 2021-12-10 | 张家口原轼新型材料有限公司 | Plating solution and plating process for plating nickel-cobalt-phosphorus alloy on surface of emery and obtained emery and golden steel wire |
| CN114657544A (en) * | 2022-03-24 | 2022-06-24 | 彭州航大新材料有限公司 | Aluminizing cobalt process for inner cavity surface of nickel-based superalloy and cobalt-aluminum infiltration layer |
| CN114657544B (en) * | 2022-03-24 | 2023-10-27 | 彭州航大新材料有限公司 | Cobalt aluminizing process and cobalt aluminizing layer for inner cavity surface of nickel-based superalloy |
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