CN105839099B - A kind of nickel plating surface chromium-free passivating treatment agent and treatment process - Google Patents
A kind of nickel plating surface chromium-free passivating treatment agent and treatment process Download PDFInfo
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- CN105839099B CN105839099B CN201610340390.6A CN201610340390A CN105839099B CN 105839099 B CN105839099 B CN 105839099B CN 201610340390 A CN201610340390 A CN 201610340390A CN 105839099 B CN105839099 B CN 105839099B
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
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Abstract
The invention belongs to passivator field, a kind of nickel plating surface chromium-free passivating treatment agent and treatment process are disclosed.The chromium-free passivating treatment agent is grouped as by the group of following parts by weight：Sodium hydroxide or 3~15 parts of potassium hydroxide, 10~30 parts of water soluble persulfates, 1~10 part of water-soluble silicate, 0~25 part of water-soluble phosphate, water-soluble 0~25 part of tungstates, 1~10 part of sodium carbonate, 20~85 parts of deionized water.The passivation treating agent chromium-free environment-friendly of the present invention is free of volatile acid or organic matter, non-volatile odorlessness in passivating process, to production environment close friend.Through passivator of the present invention treated passivating film while improving to nickel plating surface corrosion resistance and inoxidizability, ensure that nickel coating still has preferable electric conductivity and welding performance.
Description
Technical field
The invention belongs to passivator fields, and in particular to a kind of nickel plating surface chromium-free passivating treatment agent and treatment process.
Background technology
Since chemical nickel plating and electronickelling have excellent hardness, wearability, corrosion resistance, electric conductivity and special magnetics etc.
Comprehensive performance, so being widely used in the key areas such as automobile, oil, space flight, mechanized equipment, computer and electronic communication.But
It is under air or corrosive environment, nickel plating surface is easy to form the oxide of nickel or sulfide, this layer of oxide makes coating surface
Metallic luster is lost, turns to be yellow dimmed or spot occurs, seriously affects the appearance of coating.For the fields PCB, this layer of oxide
The contact resistance for not only increasing nickel plating layer surface also reduces the welding performance of nickel coating, influence wire bonding intensity and
Reliability be easy to cause falling off for weldment.Processing would generally be passivated to nickel plating layer surface, to improve the corrosion resistance of coating
And inoxidizability, it can just put into production use.
Chromating is traditional nickel plating surface passivation treatment technology, by one layer of fine and close chromate of coating surface
Passivating film effectively improves the corrosion resistance and inoxidizability of coating.But Cr VI has greatly health and ecological environment
Harm, cause chromating treatment technology to be gradually restricted.RoHS Directive regulation will be completely forbidden in 2017
Chromyl electronic product enters Europe and is sold within the border, so the substitution chromating processing of chromium-free deactivation treatment technology
Technology has been that the general trend of events is urged.
Invention content
In order to solve the disadvantage that the prior art and shortcoming, the primary purpose of the present invention is that providing a kind of nickel plating surface
Chromium-free passivating treatment agent.The passivation treating agent is not under the premise of influencing coating electric conductivity, weldability and appearance, the plating of realization
It layer corrosion resistance and antioxidative significantly improves.
Nickel plating surface is handled using above-mentioned chromium-free passivating treatment agent another object of the present invention is to provide a kind of
Technique.
The object of the invention is achieved through the following technical solutions：
A kind of nickel plating surface chromium-free passivating treatment agent, the chromium-free passivating treatment agent are grouped as by the group of following parts by weight：
Sodium hydroxide or 3~15 parts of potassium hydroxide, 10~30 parts of water soluble persulfates, 1~10 part of water-soluble silicate, water-soluble phosphorus
0~25 part of hydrochlorate, water-soluble 0~25 part of tungstates, 1~10 part of sodium carbonate, 20~85 parts of deionized water.
In above-mentioned inorganic agent, the water soluble persulfates are as strong oxidizer, it is preferable that the water soluble persulfates
Selected from potassium peroxydisulfate or sodium peroxydisulfate.
In above-mentioned inorganic agent, the water-soluble silicate is as film forming agent, it is preferable that the water-soluble silicate refers to silicon
Sour sodium.
In above-mentioned inorganic agent, the water-soluble phosphate and water-soluble tungstates are as auxiliary film former, it is preferable that described
Water-soluble phosphate refers to sodium phosphate, and the water solubility tungstates refers to sodium tungstate.
As a preferred embodiment, the chromium-free passivating treatment agent is grouped as by the group of following parts by weight：Sodium hydroxide 10
Part, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 10 parts of sodium phosphate, 3 parts of sodium carbonate, 52 parts of deionized water.
As a preferred embodiment, the chromium-free passivating treatment agent is grouped as by the group of following parts by weight：Sodium hydroxide 10
Part, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 15 parts of sodium tungstate, 3 parts of sodium carbonate, 47 parts of deionized water.
As a preferred embodiment, the chromium-free passivating treatment agent is grouped as by the group of following parts by weight：Sodium hydroxide 10
Part, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 3 parts of sodium carbonate, 62 parts of deionized water.
A kind of technique handled nickel plating surface using above-mentioned chromium-free passivating treatment agent, is included the following steps：It will be rigid
The complete nickel plating workpiece of plating is immersed in immediately in above-mentioned chromium-free passivating treatment agent, and 15~45min is reacted under the conditions of 30~90 DEG C,
Hot water cleans after taking-up, drying, you can obtain one layer of passivating film in nickel plating surface.
The mechanism of action of chrome-free tanning agent of the present invention is the coating surface in the alkaline solution of the persulfate containing strong oxidizer
W metal be oxidized to form Ni (OH)2And NiOOH, the silicate in solution can be with Ni (OH)2, NiOOH dehydrating condensations, and pass through
Multiple silicic acid polycondensation reaction is crossed, finally forms a strata silicic acid film in nickel plating surface.So chrome-free tanning agent system of the present invention
It is double-layer structure for the passivation film gone out, is conducive to stop attack of the corrosive ions to matrix, there is excellent corrosion resistance and resist
Oxidisability.
The invention has the advantages that and advantageous effect：
(1) passivator ingredient of the invention is simple and environmentally-friendly, without noxious materials such as Cr VIs, is free of volatile acid or organic
Object, the non-volatile odorlessness of passivating solution in passivating process, to production environment close friend；
(2) passivator of the invention can be recycled, repeatedly addition supplement, and waste liquid is easily handled；
(3) after the processing of the passivator of the present invention, the corrosion resistance and inoxidizability of nickel plating surface are all significantly increased, from electricity
From the point of view of chemical attack test data and salt mist experiment result, which is hopeful that traditional chromating agent is replaced to become new
Type ring protects passivator；
(4) passivating film that passivator of the invention generates is the transparent membrane of ten ran thickness, does not influence nickel coating
Original metallic luster；Nickel coating still has preferable electric conductivity and weldability under the protection of the passivating film.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
A kind of nickel plating surface chromium-free passivating treatment agent of the present embodiment, is formulated according to the parts by weight of following components：
10 parts of sodium hydroxide, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 10 parts of sodium phosphate, 3 parts of sodium carbonate, 52 parts of deionized water.
Above-mentioned nickel plating surface chromium-free passivating treatment agent is made according to the following steps：
(1) sodium hydroxide is poured into deionized water, stirring is until be completely dissolved at normal temperatures and pressures；
(2) sodium phosphate, sodium metasilicate and sodium carbonate are poured into the solution that step (1) obtains, at normal temperatures and pressures stirring until
It is completely dissolved；
(3) potassium peroxydisulfate is poured into the solution that step (2) obtains, stirring at normal temperatures and pressures is obtained up to being completely dissolved
The chromium-free passivating treatment agent.
The technique handled nickel plating surface using above-mentioned chromium-free passivating treatment agent, is included the following steps：
Passivation treating agent is heated to 70 DEG C, and is kept the temperature at this temperature.The complete nickel plating workpiece of rigid plating is soaked completely
Enter in passivating solution, 30min is reacted at 70 DEG C, with 70 DEG C of hot water cleaning workpiece surfaces after taking-up, is then dried in 100 DEG C of baking ovens
Dry-cure 20min, you can obtain one layer of passivating film in nickel plating surface.
Embodiment 2
A kind of nickel plating surface chromium-free passivating treatment agent of the present embodiment, is formulated according to the parts by weight of following components：
10 parts of sodium hydroxide, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 15 parts of sodium tungstate, 3 parts of sodium carbonate, 47 parts of deionized water.
Above-mentioned nickel plating surface chromium-free passivating treatment agent is made according to the following steps：
(1) sodium hydroxide is poured into deionized water, stirring is until be completely dissolved at normal temperatures and pressures；
(2) sodium tungstate, sodium metasilicate and sodium carbonate are poured into the solution that step (1) obtains, at normal temperatures and pressures stirring until
It is completely dissolved；
(3) potassium peroxydisulfate is poured into the solution that step (2) obtains, stirring at normal temperatures and pressures is obtained up to being completely dissolved
The chromium-free passivating treatment agent.
The technique handled nickel plating surface using above-mentioned chromium-free passivating treatment agent, is included the following steps：
Passivation treating agent is heated to 70 DEG C, and is kept the temperature at this temperature.The complete nickel plating workpiece of rigid plating is soaked completely
Enter in passivating solution, 30min is reacted at 70 DEG C, with 70 DEG C of hot water cleaning workpiece surfaces after taking-up, is then dried in 100 DEG C of baking ovens
Dry-cure 20min, you can obtain one layer of passivating film in nickel plating surface.
Embodiment 3
A kind of nickel plating surface chromium-free passivating treatment agent of the present embodiment, is formulated according to the parts by weight of following components：
10 parts of sodium hydroxide, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 3 parts of sodium carbonate, 62 parts of deionized water.
Above-mentioned nickel plating surface chromium-free passivating treatment agent is made according to the following steps：
(1) sodium hydroxide is poured into deionized water, stirring is until be completely dissolved at normal temperatures and pressures；
(2) sodium metasilicate and sodium carbonate are poured into the solution that step (1) obtains, stirring at normal temperatures and pressures is until completely molten
Solution；
(3) potassium peroxydisulfate is poured into the solution that step (2) obtains, stirring at normal temperatures and pressures is obtained up to being completely dissolved
The chromium-free passivating treatment agent.
The technique handled nickel plating surface using above-mentioned chromium-free passivating treatment agent, is included the following steps：
Passivation treating agent is heated to 70 DEG C, and is kept the temperature at this temperature.The complete nickel plating workpiece of rigid plating is soaked completely
Enter in passivating solution, 30min is reacted at 70 DEG C, with 70 DEG C of hot water cleaning workpiece surfaces after taking-up, is then dried in 100 DEG C of baking ovens
Dry-cure 20min, you can obtain one layer of passivating film in nickel plating surface.
Embodiment 1,2,3 and the chemical nickel plating finished product of unpassivated processing are subjected to performance contrast test.Electrochemical corrosion
It is 3.5wt.%NaCl aqueous solutions that test, which uses three-electrode system, corrosive liquid, and test temperature is room temperature (25 DEG C), and reference electrode is
Ag/AgCl/sat.KCl.Salt mist experiment carries out neutral salt spray test according to GB/T 10125-1997.The results are shown in Table 1：
Table 1
The corrosion resistance of passivator it can be seen from 1 result of table through the invention treated nickel plating surface and anti-oxidant
Property is all significantly increased, and from the point of view of electrochemical corrosion test data and salt mist experiment result, passivator of the invention does not influence to plate
The original metallic luster of nickel layer.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (5)
1. a kind of nickel plating surface chromium-free passivating treatment agent, it is characterised in that the chromium-free passivating treatment agent by following parts by weight group
It is grouped as：3~15 parts of sodium hydroxide or potassium hydroxide, 10~30 parts of water soluble persulfates, 1~10 part of water-soluble silicate,
0~25 part of water-soluble phosphate, water-soluble 0~25 part of tungstates, 1~10 part of sodium carbonate, 20~85 parts of deionized water；
The water soluble persulfates are selected from potassium peroxydisulfate or sodium peroxydisulfate；
The water-soluble silicate refers to sodium metasilicate；
The water-soluble phosphate refers to sodium phosphate, and the water solubility tungstates refers to sodium tungstate.
2. a kind of nickel plating surface chromium-free passivating treatment agent according to claim 1, it is characterised in that：At the chromium-free deactivation
Reason agent is grouped as by the group of following parts by weight：10 parts of sodium hydroxide, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 10 parts of sodium phosphate, carbon
3 parts of sour sodium, 52 parts of deionized water.
3. a kind of nickel plating surface chromium-free passivating treatment agent according to claim 1, it is characterised in that：At the chromium-free deactivation
Reason agent is grouped as by the group of following parts by weight：10 parts of sodium hydroxide, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 15 parts of sodium tungstate, carbon
3 parts of sour sodium, 47 parts of deionized water.
4. a kind of nickel plating surface chromium-free passivating treatment agent according to claim 1, it is characterised in that：At the chromium-free deactivation
Reason agent is grouped as by the group of following parts by weight：10 parts of sodium hydroxide, 20 parts of potassium peroxydisulfate, 5 parts of sodium metasilicate, 3 parts of sodium carbonate, go from
62 parts of sub- water.
5. a kind of technique that nickel plating surface is handled using Claims 1 to 4 any one of them chromium-free passivating treatment agent,
It is characterized by comprising following steps：The complete nickel plating workpiece of rigid plating is immersed in immediately in above-mentioned chromium-free passivating treatment agent,
15~45min is reacted under the conditions of 30~90 DEG C, hot water cleans after taking-up, drying, you can obtain one layer of passivating film in nickel plating surface.
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| CN201610340390.6A CN105839099B (en) | 2016-05-19 | 2016-05-19 | A kind of nickel plating surface chromium-free passivating treatment agent and treatment process |
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| CN107313101B (en) * | 2017-06-08 | 2019-06-18 | 华南理工大学 | A kind of preparation method of environmentally friendly nickel envelope-chromium-free deactivation layer |
| CN107841740A (en) * | 2017-11-06 | 2018-03-27 | 常熟市梅李合金材料有限公司 | A kind of nickel filament |
| CN108179410A (en) * | 2017-11-22 | 2018-06-19 | 无锡伊佩克科技有限公司 | A kind of electronickelling chrome-free tanning agent and preparation method thereof |
| CN114231962B (en) * | 2021-12-16 | 2024-05-24 | 厦门华弘昌科技有限公司 | Chromium-free passivating agent, preparation method thereof and passivating method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5873953A (en) * | 1996-12-26 | 1999-02-23 | The Boeing Company | Non-chromated oxide coating for aluminum substrates |
| US6432224B1 (en) * | 2000-02-08 | 2002-08-13 | Lynntech, Inc. | Isomolybdate conversion coatings |
| CN101709466B (en) * | 2009-12-08 | 2011-07-20 | 广东工业大学 | Alkaline passivation method of chemical nickel coating |
| CN102234800A (en) * | 2011-07-27 | 2011-11-09 | 华南理工大学 | Aluminum alloy rare earth passivating liquid taking chlorine salt as accelerator and use method thereof |
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