CN103805981B - A kind of nickel passivating solution and preparation method thereof and the method for nickel surface passivation - Google Patents
A kind of nickel passivating solution and preparation method thereof and the method for nickel surface passivation Download PDFInfo
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- CN103805981B CN103805981B CN201210450706.9A CN201210450706A CN103805981B CN 103805981 B CN103805981 B CN 103805981B CN 201210450706 A CN201210450706 A CN 201210450706A CN 103805981 B CN103805981 B CN 103805981B
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- dimethylformamide
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Abstract
The invention provides a kind of nickel passivating solution and preparation method thereof, following components is contained in the nickel passivating solution：The 10g/L of chromic anhydride 1, the 100g/L of phosphoric acid 30, the 50g/L of dimethylformamide 20, the 10g/L of MTES 1.Method present invention also offers being passivated to nickel surface using the nickel passivating solution.The nickel passivating solution provided using the present invention, can be formed in metallic nickel layer surface and stablize lasting passivation layer, and salt-fog resistant time is greatly prolonged.Meanwhile, content of 6-valence Cr ions is relatively low in the nickel passivating solution that the present invention is provided, safety and environmental protection.
Description
Technical field
The invention belongs to technical field of surface, and in particular to a kind of nickel passivating solution and preparation method thereof and nickel surface are blunt
The method of change.
Background technology
Nickel plating is widely used in modern electroplating technology, but nickel dam particularly electroless nickel layer surface is due to larger hole
Gap, easily produces potential corrosion and oxidation stain, and salt spray resistance is often poor, therefore generally requires by Passivation Treatment.It is existing
Have technology it is conventional be sexavalence chromium type passivator.But sexavalence chromium type passivator passivation effect is larger with the changes of contents of Cr VI,
Passivation effect also less stable, is 24-48 hours generally with the salt-fog resistant time after sexavalence chromium passivating, it is difficult to resistance to longer simultaneously
The salt spray test time.Simultaneously as hexavalent chromium compound is easily absorbed by the body, its can by digestive system, respiratory tract, skin and
Mucous membrane invades human body, therefore larger to environment and harm.The content of Cr VI is reduced even with not conforming to the blunt of Cr VI
Changing liquid turns into one of direction of passivating solution Future Development.
The content of the invention
The present invention solves that the passivation effect that the sexavalence chromium type passivator that uses in the prior art is present is unstable, salt spray resistance
Time is short and the content of 6-valence Cr ions technical problem for causing to there is larger harm to environment and human body higher.
The invention provides a kind of nickel passivating solution, following components is contained in the nickel passivating solution：Chromic anhydride 1-10g/L, phosphoric acid
30-100g/L, dimethylformamide 20-50g/L, MTES 1-10g/L.
Present invention also offers a kind of preparation method of the nickel passivating solution, including chromic anhydride is first dissolved in phosphoric acid in proportion
In, dimethylformamide is subsequently adding, it is eventually adding MTES.
Finally, the invention provides a kind of method of nickel surface passivation, including the workpiece that surface has metallic nickel is impregnated
In the nickel passivating solution that the present invention is provided.
The nickel passivating solution that the present invention is provided, it contains chromic anhydride, phosphoric acid, dimethylformamide and MTES,
Wherein phosphoric acid is used for activated ni layer surface, and chromic anhydride is used for film forming, and dimethylformamide can improve the resistance to acids and bases of passivation film, first
Ethyl triethoxy silicane alkane improves the hydrophobicity on nickel dam surface, and is suitably allocated by the concrete content to each component so that
The nickel passivation liquid energy provided using the present invention is formed in metallic nickel layer surface stablizes lasting passivation layer, and salt-fog resistant time prolongs significantly
It is long.Meanwhile, content of 6-valence Cr ions is relatively low in the nickel passivating solution that the present invention is provided, safety and environmental protection.
Specific embodiment
The invention provides a kind of nickel passivating solution, following components is contained in the nickel passivating solution：Chromic anhydride 1-10g/L, phosphoric acid
30-100g/L, dimethylformamide 20-50g/L, MTES 1-10g/L.
The nickel passivating solution that the present invention is provided, it contains chromic anhydride, phosphoric acid, dimethylformamide and MTES.
Wherein, phosphoric acid is used for activated ni layer surface；Chromic anhydride can react with nickel dam, and forming layer protecting film on nickel dam surface is used for film forming.
Dimethylformamide can first be adsorbed in metallic nickel layer surface, subsequently hydrolyze, and hydrolysate can be entrained in chromic anhydride formation
In oxide film layer, the hydrolysate is organic matter, its resistance to acids and bases for being favorably improved film layer, during extension salt spray resistance
Between.MTES improves the hydrophobicity on nickel dam surface, and prevent salt fog from being gathered in nickel dam surface carries out etch to it, from
And further extend salt-fog resistant time.
The present inventor, by further experiment, the concrete content to each component is suitably allocated so that adopted
The nickel passivating solution provided with the present invention（Chromic anhydride 1-10g/L, phosphoric acid 30-100g/L, dimethylformamide 20-50g/L, methyl three
Ethoxysilane 1-10g/L）Can be formed on nickel dam surface and stablize lasting passivation layer, salt-fog resistant time is greatly prolonged.Meanwhile, this
Content of 6-valence Cr ions is relatively low in inventing the nickel passivating solution for providing, safety and environmental protection.
Used as a kind of preferred embodiment of the invention, each component content is in the nickel passivating solution：Chromic anhydride 2-7g/L, phosphorus
Sour 40-80g/L, dimethylformamide 30-40g/L, MTES 2-8g/L.
Present invention also offers a kind of preparation method of the nickel passivating solution, including chromic anhydride is first dissolved in phosphoric acid in proportion
In, dimethylformamide is subsequently adding, it is eventually adding MTES.
To ensure that the nickel passivating solution has optimal passivation effect to metallic nickel, under preferable case, the second of the methyl three
TMOS is added when in use.
Finally, the invention provides a kind of method of nickel surface passivation, including the workpiece that surface has metallic nickel is impregnated
In the nickel passivating solution that the present invention is provided.
Under preferable case, dip time is 5-15min.During dipping, the temperature of the nickel passivating solution is 30-40 DEG C.
In the present invention, the step of also drying including carrying out washing to workpiece surface after the completion of dipping.Washing and the mistake of drying
Cheng Zhong, the dimethylformamide in nickel passivating solution is hydrolyzed, and the hydrolysate of formation is entrained in sull, can be improved
The resistance to acids and bases of passivating film.In the case of more preferably, the time of washing is 1-3min.
In order that technical problem solved by the invention, technical scheme and beneficial effect become more apparent, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention, is not intended to limit the present invention.
Embodiment 1
By formula as below, phosphorus aqueous acid is first prepared, then toward adding chromic anhydride in phosphate aqueous solution, stirring is to completely molten
Solution, is subsequently adding dimethylformamide, and stirring is stood to after dissolving, and MTES is added when to be used, is obtained
The nickel passivating solution S1 of the present embodiment, consisting of：Chromic anhydride 6g/L, phosphoric acid 70g/L, dimethylformamide 40g/L, the ethoxy of methyl three
Base silane 5g/L.
Embodiment 2
Phosphorus aqueous acid is first prepared by formula as below, then toward adding chromic anhydride in phosphate aqueous solution, stirring is to completely molten
Solution, is subsequently adding dimethylformamide, and stirring is stood to after dissolving, and MTES is added when to be used, is obtained
The nickel passivating solution S2 of the present embodiment, consisting of：Chromic anhydride 1g/L, phosphoric acid 30g/L, dimethylformamide 20g/L, the ethoxy of methyl three
Base silane 1g/L.
Embodiment 3
Phosphorus aqueous acid is first prepared by formula as below, then toward adding chromic anhydride in phosphate aqueous solution, stirring is to completely molten
Solution, is subsequently adding dimethylformamide, and stirring is stood to after dissolving, and MTES is added when to be used, is obtained
The nickel passivating solution S3 of the present embodiment, consisting of：Chromic anhydride 10g/L, phosphatase 11 00g/L, dimethylformamide 50g/L, the second of methyl three
TMOS 10g/L.
Comparative example 1
Phosphorus aqueous acid is first prepared by formula as below, then toward adding chromic anhydride in phosphate aqueous solution, stirring is to completely molten
Solution, obtains the nickel passivating solution DS1 of this comparative example, consisting of：Chromic anhydride 6g/L, phosphoric acid 70g/L.
Comparative example 2
Aqueous sulfuric acid is prepared, potassium bichromate and sodium fluoride is added, stirred to being completely dissolved, the nickel for obtaining this comparative example is blunt
Change liquid DS2, consisting of：Potassium bichromate 6g/L, sulfuric acid 50g/L, sodium fluoride 2g/L.
Performance test
The three-dimension mobile phone antenna workpiece after 5PCS laser activations is taken, layer of metal nickel, horse back water are plated after the complete copper of its plated surface
Wash 3 minutes, be then respectively put into nickel the passivating solution S1-S3 and DS1-DS2 of embodiment 1-3 and comparative example 1-2 and impregnate 10min,
Each passivating solution temperature is 35 DEG C.2min is washed after dipping, is dried immediately.Then according to the method for GB/T10125-1997 to each
Workpiece carries out neutral salt spray test, and test result is as shown in table 1.
Table 1
。
The nickel passivating solution provided using the present invention is can be seen that from the test result of upper table 1 to be passivated metal nickel dam
After treatment, the time of nickel coating salt spray resistance test can be greatly prolonged, hence it is evident that better than the passivating solution sample of comparative example.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of nickel passivating solution, it is characterised in that contain following components in the nickel passivating solution：Chromic anhydride 1-6g/L, phosphoric acid 30-
100g/L, dimethylformamide 20-50g/L, MTES 1-10g/L.
2. nickel passivating solution according to claim 1, it is characterised in that each component content is in the nickel passivating solution：Chromic anhydride
2-7g/L, phosphatase 24 0-80g/L, dimethylformamide 30-40g/L, MTES 2-8g/L.
3. the preparation method of the nickel passivating solution described in claim 1 or 2, it is characterised in that including first dissolving chromic anhydride in proportion
In phosphoric acid, dimethylformamide is subsequently adding, is eventually adding MTES.
4. a kind of method that nickel surface is passivated, it is characterised in that the workpiece including surface to be had metallic nickel impregnated in right will
In seeking the nickel passivating solution described in 1 or 2.
5. method according to claim 4, it is characterised in that dip time is 5-15min, the temperature of the nickel passivating solution
It is 30-40 DEG C.
6. method according to claim 4, it is characterised in that also including carrying out washing baking to workpiece surface after the completion of dipping
Dry step.
7. method according to claim 6, it is characterised in that the time of washing is 1-3min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210450706.9A CN103805981B (en) | 2012-11-13 | 2012-11-13 | A kind of nickel passivating solution and preparation method thereof and the method for nickel surface passivation |
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| CN201210450706.9A CN103805981B (en) | 2012-11-13 | 2012-11-13 | A kind of nickel passivating solution and preparation method thereof and the method for nickel surface passivation |
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| CN105331959B (en) * | 2015-11-02 | 2018-02-16 | 麦垲门电子科技(上海)有限公司 | Lug nickel strap Surface treatment passivation solution |
| CN108796479B (en) * | 2017-04-28 | 2020-02-07 | 比亚迪股份有限公司 | Nickel protective agent and preparation method and use method thereof |
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| CN101583739A (en) * | 2006-09-29 | 2009-11-18 | 莫门蒂夫性能材料股份有限公司 | Storage stable composition of partial and/or complete condensate of hydrolyzable organofunctional silane |
| CN101688309A (en) * | 2007-06-29 | 2010-03-31 | 日本帕卡濑精株式会社 | Aqueous fluid for surface treatment of zinc-plated steel sheets and zinc-plated steel sheets |
| CN101891998A (en) * | 2009-05-18 | 2010-11-24 | 攀钢集团钢铁钒钛股份有限公司 | Paint composition and galvanized passivated material |
| CN102312234A (en) * | 2011-10-20 | 2012-01-11 | 无锡伊佩克科技有限公司 | Passivating solution for plated metal |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1021063C (en) * | 1988-12-30 | 1993-06-02 | 杨延松 | Passivating liquid for steel and iron surface treatment |
| JPH0696778B2 (en) * | 1990-10-05 | 1994-11-30 | 新日本製鐵株式会社 | Chromate treatment method for galvanized steel sheet |
| JP2628782B2 (en) * | 1990-10-08 | 1997-07-09 | 日本パーカライジング株式会社 | Chromate treatment method for galvanized steel sheet |
| CN1021705C (en) * | 1992-03-07 | 1993-07-28 | 冶金工业部钢铁研究总院 | Passivating liquid for surface of galvanized steel plate |
| CN1267749A (en) * | 2000-04-07 | 2000-09-27 | 清华大学 | Lead-tin anode scavenger for chromium plating process |
| CN101899658B (en) * | 2009-05-27 | 2012-10-03 | 潍坊学院 | Galvanized greenblack passivation solution and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101583739A (en) * | 2006-09-29 | 2009-11-18 | 莫门蒂夫性能材料股份有限公司 | Storage stable composition of partial and/or complete condensate of hydrolyzable organofunctional silane |
| CN101688309A (en) * | 2007-06-29 | 2010-03-31 | 日本帕卡濑精株式会社 | Aqueous fluid for surface treatment of zinc-plated steel sheets and zinc-plated steel sheets |
| CN101891998A (en) * | 2009-05-18 | 2010-11-24 | 攀钢集团钢铁钒钛股份有限公司 | Paint composition and galvanized passivated material |
| CN102312234A (en) * | 2011-10-20 | 2012-01-11 | 无锡伊佩克科技有限公司 | Passivating solution for plated metal |
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