CN103806045A - Process of mechanically lapping electroplated nickel-phosphorus alloy plating layer by horizontal vibration - Google Patents
Process of mechanically lapping electroplated nickel-phosphorus alloy plating layer by horizontal vibration Download PDFInfo
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- CN103806045A CN103806045A CN201210450940.1A CN201210450940A CN103806045A CN 103806045 A CN103806045 A CN 103806045A CN 201210450940 A CN201210450940 A CN 201210450940A CN 103806045 A CN103806045 A CN 103806045A
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Abstract
The invention relates to a process of mechanically lapping an electroplated nickel-phosphorus alloy plating layer by horizontal vibration. The process comprises the following steps: placing a glass ball in an electrolytic cell during electroplating; horizontally vibrating a base body at a certain frequency, wherein the glass ball in the electrolytic cell continuously moves on the surface of a test sample; and applying mechanical lapping. According to the process disclosed by the invention, the corrosion resistance and hardness of the electroplated nickel layer can be remarkably improved, and the plating layer is fine in crystalline grain and uniform and compact.
Description
Technical field
The present invention relates to a kind of technique of level concussion mechanical mill nickel-phosphorus alloy plating coating.
Background technology
Corrosion and corrosion protection is related to Economic development and people's life safety, and surface engineering technology is to solve component of machine and material corrosion and the most economical effective measure of protection.Along with modern industry and scientific and technical develop rapidly, more and more higher to the performance requriements of component of machine and material surface, process for treating surface has also had development rapidly thereupon.Surface engineering technology can be processed component or material surface with chemistry, physics or electrochemical method, makes its surface form various protective layers, improves the work-ing life of component or material.Alloy compound surface deposition (galvanic deposit or electroless plating) has higher solidity to corrosion, hardness, compactness, wear resistance, high thermal resistance, weldability and beautiful outward appearance because of it compared with monometallic surface deposition, and is widely used.
In recent years, people have given very big concern to research and development nano-multilayer film.Constantly improving on the basis of galvanic deposit nano-multilayer film, developing nano-multilayer film product and the technique of the better performances such as Cu/Ni, Co/Cu, Co/Pt, but many research as magnetic property, the rarely seen report of research aspect corrosion resistance coating.
Nickel-phosphorus alloy plating, as the protective coating of iron and steel, is widely applied.In order to meet component or material property requirements at the higher level, all strengthen research and the application to zinc base alloy platings such as Zn-Fe, Zn-Ni, Sn-Zn, Zn-Co, Zn-Mn, Zn-Cr, Zn-Ti, Zn-Co-Cr, Zn-Co-Fe, Zn-Ni-P, Zn-Fe-P both at home and abroad, wherein nickel-phosphorus alloy multilayer film, because having good solidity to corrosion, is therefore studied by numerous mechanisms.
But nickel-phosphorus alloy of the prior art plates due to technical defect, the coating of gained still can not meet the demand in some situation aspect hardness, solidity to corrosion.
Summary of the invention
For the deficiencies in the prior art, one of object of the present invention is to provide a kind of technique of level concussion mechanical mill nickel-phosphorus alloy plating coating.Described electroplating technology can obviously improve solidity to corrosion, the hardness of electroless nickel layer, and makes coating crystal grain tiny, even compact.
The technique of level concussion mechanical mill nickel-phosphorus alloy plating coating provided by the present invention is: when plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.
Wherein, the diameter of described glass sphere is 3-7mm;
Wherein, level concussion frequency is 3-5Hz, and amplitude is 5-15mm.
Wherein, nickel-phosphorus alloy plating liquid is in 1 liter of solution, chloride containing nickel 30g, single nickel salt 180～220g, sodium hypophosphite 30～50g, boric acid 20～30g, ammonium bifluoride 15～25g, Ytterbium trichloride 0.20～0.50g or ytterbium nitrate 0.30～0.60g, and all the other are water.
The concocting method of nickel-phosphorus alloy plating liquid, comprises the steps: that (1) is dissolved in water single nickel salt, nickelous chloride, boric acid, ammonium bifluoride, Ytterbium trichloride or ytterbium nitrate mix; (2) sodium hypophosphite is dissolved in water; (3) under the condition stirring, sodium hypophosphite solution is slowly poured in the solution of (1), and stirred; (4) adding distil water or deionized water be to prescribed volume, and stir.
When using, nickel-phosphorus alloy plating liquid regulates pH value to 2.0～4.0 of electroplate liquid with 5%～10% dilute sulphuric acid, best pH value is 2.5～3.5, then electroplate liquid is heated to 50～75 ℃, best constant fixed temperature is 55～65 ℃, put into workpiece, wherein negative electrode is workpiece, and anode is nickel metal, and cathode current density is 1～2A/dm
2.
The present invention adopts nonconducting glass sphere in cathode surface mechanical mill, hinder to a certain extent the electric force lines distribution between anode and cathode, be equivalent under identical electric current, reduce specimen size, current density is increased, cathode overpotential is increased, nucleation rate improves, the refinement gradually of coating crystal grain, thus solidity to corrosion, the hardness of electroless nickel layer obviously improved, and make coating even compact.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
The concocting method of nickel-phosphorus alloy plating liquid, comprises the steps:
(1) single nickel salt, nickelous chloride, boric acid, ammonium bifluoride, Ytterbium trichloride or ytterbium nitrate are dissolved in water and are mixed;
(2) sodium hypophosphite is dissolved in water;
(3) under the condition stirring, sodium hypophosphite solution is slowly poured in the solution of (1), and stirred;
(4) adding distil water or deionized water be to prescribed volume, and stir.
Embodiment 1
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 3mm.Level concussion frequency is 3Hz, and amplitude is 5mm.When plating, regulating pH value with 5% dilute sulphuric acid is 2.5, heats to 62 ℃.Cathode current density 1A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV700, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 2
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 4mm.Level concussion frequency is 4Hz, and amplitude is 10mm.When plating, regulating pH value with 10% dilute sulphuric acid is 2.8, heats to 60 ℃.Cathode current density 2A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV730, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 3
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 5mm.Level concussion frequency is 5Hz, and amplitude is 15mm.When plating, regulating pH value with 8% dilute sulphuric acid is 3.2, heats to 65 ℃.Cathode current density 1.5A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV750, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 4
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 6mm.Level concussion frequency is 4Hz, and amplitude is 10mm.When plating, regulating pH value with 5% dilute sulphuric acid is 3.5, heats to 60 ℃.Cathode current density 1A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV760, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 5
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 7mm.Level concussion frequency is 4Hz, and amplitude is 10mm.When plating, regulating pH value with 5% dilute sulphuric acid is 3.0, heats to 68 ℃.Cathode current density 2A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV720, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 6
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 3mm.Level concussion frequency is 5Hz, and amplitude is 15mm.When plating, regulating pH value with 5% dilute sulphuric acid is 2.8, heats to 70 ℃.Cathode current density 1.6A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV750, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 7
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 7mm.Level concussion frequency is 3Hz, and amplitude is 5mm.When plating, regulating pH value with 6% dilute sulphuric acid is 2, heats to 75 ℃.Cathode current density 1.5A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV715, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 8
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 3mm.Level concussion frequency is 3Hz, and amplitude is 15mm.When plating, regulating pH value with 5% dilute sulphuric acid is 4.0, heats to 50 ℃.Cathode current density 1A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV725, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 9
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 3.5mm.Level concussion frequency is 4.5Hz, and amplitude is 7mm.When plating, regulating pH value with 5% dilute sulphuric acid is 3.8, heats to 55 ℃.Cathode current density 1A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV700, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 10
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 4.5mm.Level concussion frequency is 3.5Hz, and amplitude is 12mm.When plating, regulating pH value with 10% dilute sulphuric acid is 2.4, heats to 72 ℃.Cathode current density 2A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV705, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Embodiment 11
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill.The diameter of glass sphere is 6mm.Level concussion frequency is 4Hz, and amplitude is 10mm.When plating, regulating pH value with 5% dilute sulphuric acid is 3.6, heats to 66 ℃.Cathode current density 2A/dm
2, anode is nickel metal.Bath stability, gained coating densification, even, the microhardness of coating is HV716, and the organic acid under non-oxidizing acid, high temperature under normal temperature and hot and cold alkali or alkaline medium are had to excellent solidity to corrosion.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the each raw material of product of the present invention and the interpolation of ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (5)
1. the technique of a level concussion mechanical mill nickel-phosphorus alloy plating coating is:
When plating, in electrolyzer, put into glass sphere, make matrix with certain frequency level concussion, thereby the glass sphere in electrolyzer is constantly moved at specimen surface, apply mechanical mill;
Wherein, the diameter of described glass sphere is 3-7mm.
Wherein, level concussion frequency is 3-5Hz.
Wherein, amplitude is 5-15mm.
2. according to the method for claim 1, wherein, nickel-phosphorus alloy plating liquid is in 1 liter of solution, chloride containing nickel 30g, single nickel salt 180～220g, sodium hypophosphite 30～50g, boric acid 20～30g, ammonium bifluoride 15～25g, Ytterbium trichloride 0.20～0.50g or ytterbium nitrate 0.30～0.60g, and all the other are water.
3. according to the process of claim 1 wherein, when plating, dilution heat of sulfuric acid with 5%～10% regulates pH value to 2.0～4.0 of electroplate liquid, then electroplate liquid is heated to 50～75 ℃, puts into workpiece, wherein negative electrode is workpiece, and anode is nickel metal, and cathode current density is 1～2A/dm
2.
4. according to the method for claim 3, wherein, described pH value is 2.5～3.5.
5. according to the method for claim 3, wherein, described electroplating temperature is 55～65 ℃.
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| CN201210450940.1A CN103806045A (en) | 2012-11-12 | 2012-11-12 | Process of mechanically lapping electroplated nickel-phosphorus alloy plating layer by horizontal vibration |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637154A (en) * | 2016-11-14 | 2017-05-10 | 中国石油天然气集团公司 | Device and method for preparing nano Ni-P coating on inner wall of small-size metal pipe through mechanical grinding technology |
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2012
- 2012-11-12 CN CN201210450940.1A patent/CN103806045A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637154A (en) * | 2016-11-14 | 2017-05-10 | 中国石油天然气集团公司 | Device and method for preparing nano Ni-P coating on inner wall of small-size metal pipe through mechanical grinding technology |
| CN106637154B (en) * | 2016-11-14 | 2019-05-07 | 中国石油天然气集团公司 | A kind of device and method preparing Ni nanoparticle-P coating in small sized metallic inside pipe wall using mechanical grinding techniques |
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Application publication date: 20140521 |