CN106191943A - The supercritical electroplating preparation method of a kind of cobalt-nickel alloy light protective coating and preparation system thereof - Google Patents
The supercritical electroplating preparation method of a kind of cobalt-nickel alloy light protective coating and preparation system thereof Download PDFInfo
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- CN106191943A CN106191943A CN201610566035.0A CN201610566035A CN106191943A CN 106191943 A CN106191943 A CN 106191943A CN 201610566035 A CN201610566035 A CN 201610566035A CN 106191943 A CN106191943 A CN 106191943A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/10—Agitating of electrolytes; Moving of racks
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/003—Electroplating using gases, e.g. pressure influence
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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Abstract
The invention discloses supercritical electroplating preparation method and the preparation system thereof of a kind of cobalt-nickel alloy light protective coating, with cobalt, nickel or cobalt-nickel alloy as anode, with workpiece to be plated as negative electrode, ternary system emulsion is electroplated, described ternary system emulsion includes electrolyte, surfactant and supercritical carbon dioxide fluid, and electrolyte is to include cobalt salt 20 100 g/L, nickel salt 50 200 g/L, sodium salt 20 100 g/L, boric acid 10 50 g/L, sodium lauryl sulphate 0.01 0.2 g/L, the mixed solution of saccharin sodium 15 g/L.The alloy layer of preparation is nanocrystalline structure, and crystallite dimension is 10 30 nm, and cobalt content is 70 85%；The nano-alloy plating layer not only surface-brightening of preparation is smooth, hardness is high, has wear-resisting, antifriction and the decay resistance of excellence.It is applicable to requirement high rigidity, high abrasion, low-friction coefficient and corrosion resistant parts.
Description
Technical field
The present invention relates to nanometer functional films technical field of material, be specially a kind of cobalt-nickel alloy light protection plating
The supercritical electroplating preparation method of layer and preparation system thereof.
Background technology
It is known that abrasion, to corrode with fracture be three big main damage forms of component of machine and engineering component, they
The economic loss caused is the hugest.Metal material remains the engineering material that application is most, actually metal material so far
Most unstabilitys start from the surface of material, the process such as fretting wear, corrosion oxidation, fatigue fracture occurs mainly in metal material
Therefore surface, as long as obtaining certain thickness function protecting top layer at material surface, it becomes possible to by surface texture and performance
Optimize overall mechanical property and the environment military service behavior improving metal material.
Electroplate due to low cost, operating condition is simple, efficiency is high and thickness of coating the advantage such as is easily controlled and is extensively used
In in component surface deposition, there is performance and the thin film attractive in appearance such as high rigidity, resisting fatigue abrasion, corrosion-resistant, electrical, magnetic
Material.Cross dechromise (Cr) metal due to possess excellence mechanical strength and corrosion resistance, be often used for surface process.But in system
During Bei, the plating solution containing sexavalence Cr ion need to be used, consider from environmental, sexavalence Cr plating serious environment pollution,
The harm mankind's is healthy, therefore the goods of sexavalence Cr are ordered to disable by European Union and many countries.Therefore, industrial beginning
Finding the protectiveness coating material replaced, wherein nickel (Ni) and cobalt (Co) and alloy firm thereof draw owing to having excellent performance
Play the concern of a lot of scholar.
Relative to monometallic Ni or Co, Co-Ni alloy layer, there is more excellent performance (Electroplating &
Pollution Control, 25 (2005) 14-16), simultaneously because Co-Ni alloy have high rigidity, excellent rub resistance and
Decay resistance is considered to have and is applied to space flight and aviation, automobile and replaces the potentiality of hard Cr coating in general industry
(Applied Surface Science 242 (2005) 326-332).But, owing to traditional plating needs mostly at water
Solution is electrochemically reacted, during plating, the side reaction of water can occur to be electrolysed simultaneously, therefore have on negative electrode
The formation of hydrogen, and then be collected as pin hole or defect, all can adversely affect for the quality of coating, intensity etc..In order to
Solve this problem, have a lot of modification methods to be suggested, such as stirring, pulse plating, the mode such as use of additive, but its effect
Fruit has certain limit, can not tackle the problem at its root.
Summary of the invention
The purpose of patent of the present invention is to solve the defect that prior art exists, and utilizes supercritical electro-deposition techniques, it is provided that
The supercritical electroplating preparation method of a kind of cobalt-nickel alloy light protective coating and preparation system thereof.Cobalt-nickel prepared by the present invention
Nano-alloy plating layer not only surface-brightening is smooth, hardness is high, and has the anti-attrition of excellence, wear-resisting and decay resistance, its system
Preparation Method is simple, has a wide range of applications in space flight and aviation, automobile, machinery and precision manufactureing field.
The purpose of the present invention is accomplished by:
A kind of supercritical electroplating preparation method of cobalt-nickel alloy light protective coating, with cobalt, nickel or cobalt-nickel alloy as anode, with
Workpiece to be plated is negative electrode, electroplates in ternary system emulsion, and described ternary system emulsion includes living in electrolyte, surface
Property agent and supercritical carbon dioxide fluid, described electrolyte is for including cobalt salt 20-100 g/L, nickel salt 50-200 g/L, sodium salt
20-100 g/L, boric acid 10-50 g/L, sodium lauryl sulphate 0.01-0.2 g/L, the mixed solution of saccharin sodium 1-5 g/L.
By using supercritical carbon dioxide as fluid, make full use of supercritical carbon dioxide and there is low surface tension
With the feature of viscosity, controlled diffusion and the high-solvency to hydrogen, effectively solve the liberation of hydrogen problem occurred in electroplating process.With
Time, use supercritical carbon dioxide as fluid, conventional plating can be avoided to be faced with environmental protection pressure and Cost Problems, such as tradition
Additive can clip to be formed in deposit be mingled with, and causes the pollution of coating；As tradition organic additive exists chemical heat stability
Difference, the shortcomings such as toxicity is stronger, the most easily decompose unfriendly to environment.And supercritical carbon dioxide has nothing
The advantages such as malicious, harmless, low price, super critical condition easily reach, supercritical carbon dioxide fluid technology is generally acknowledged in the world
Green technology.Its preparation process can reduce the consumption of electroplate liquid, and can reclaim profit again for the carbon dioxide in environment
With, not only decrease the generation of heavy metal waste liquid but also reduce processing cost.
Further, one or both during cobalt salt is cobaltous sulfate and cobaltous chloride in described electrolyte, nickel salt is nickel sulfate
Or one or both in Nickel dichloride., sodium salt is one or both in sodium sulfate and sodium chloride.
Further, described surfactant is Dodecyl Polyoxyethylene Ether, PEO-PPO, polyoxyethylene lauryl ether, second
One in base vinyl ethers surfactant.
Further, described surface-active contents is 0.1-2.0 vol%.
Further, described carbon dioxide volume fraction in electroplating reaction still is 10-50 %.
Further, described plating uses direct current or pulsive electroplating, and bath pH value is 3-8, magnetic agitation speed during plating
Degree is for 300-800 rev/min, and electroplating reaction still temperature is 35-80 DEG C, electroplating reaction still pressure is 8-20 MPa, the average electricity of plating
Current density is 1.0-20.0 A/dm2, electroplating time is 0.5-2 h.Use direct current electrode position method, compare traditional plating mode,
The hardness range of the Co-Ni alloy layer that tradition plating mode is prepared in water electrolysis liquid is at 300～500 HV
(Transactions of the IMF 93 (2015) 104-112), and use the preparation method of the present invention, at direct current electrode position
The hardness of the Co-Ni alloy layer of lower preparation also can reach 650 more than HV.
The present invention compared with prior art has the advantages that
1, the preparation method of the present invention can prepare Co-Ni alloy layer at all size and different metal surface, this plating
Not only surface-brightening is smooth, hardness is high for layer, and has wear-resisting, the corrosion proof function of excellence.
2, the present invention solves in tradition water electrolysis liquid electroplating process, owing to forming hydrogen on negative electrode, and then assembles
For pin hole or defect, the problem that the quality of coating, intensity etc. are adversely affected.
3, the preparation method of the present invention is simple, easy to operate；The consumption of electroplate liquid is few, the recyclable recycling of carbon dioxide,
Thus the generation decreasing heavy metal waste liquid reduces again processing cost；Environmental protection, production efficiency is high, it is easy to accomplish industrialization
Produce.
4, the coating prepared by the present invention is applicable to requirement high rigidity, high abrasion, low friction and corrosion resistant parts, at vapour
Car, machinery, precision manufactureing and field of aerospace have a wide range of applications, and can extend the service life of part, reduce power
Consume, save the energy..
Accompanying drawing explanation
Fig. 1 is supercritical fluid electroplanting device schematic diagram.
Detailed description of the invention
In order to make those skilled in the art be more fully understood that technical scheme, below in conjunction with embodiment to this
Bright product is described in further detail.
Embodiment 1
The supercritical electroplating preparation method of a kind of cobalt-nickel alloy light protective coating, specifically comprises the following steps that
Preparing the electrolyte of cobalt-nickel nano-alloy plating layer, its component is: cobaltous sulfate 30 g/L, Nickel dichloride. 80 g/L, sodium sulfate 50
G/L, boric acid 30 g/L, sodium lauryl sulphate 0.1 g/L, saccharin sodium 3 g/L, Dodecyl Polyoxyethylene Ether 0.5 vol%.Will
Above-mentioned plating solution joins reactor, is passed through carbon dioxide until reactor pressure is 8 MPa, and it is 40 that heating makes reactor temperature
DEG C, make carbon dioxide reach supercriticality, and to account for reactor volume be 40 %.Electroplating cathode is to live through oil removing-cleaning-acid
Change-clean-be dried brass substrate, anode is nickel sheet, use pulse plating method, average current density is 1.5 A/dm2, plating
Liquid pH is 4, and magnetic agitation speed is 400 revs/min, and electroplating time is 1 h, prepares cobalt-nickel nano-alloy plating layer, and performance is such as
Shown in table 1.
Embodiment 2
The supercritical electroplating preparation method of a kind of cobalt-nickel alloy light protective coating, specifically comprises the following steps that
Preparing the electrolyte of cobalt-nickel nano-alloy plating layer, its component is: cobaltous chloride 30 g/L, nickel sulfate 100 g/L, sodium chloride
30 g/L, boric acid 30 g/L, sodium lauryl sulphate 0.1 g/L, saccharin sodium 1 g/L, polyoxyethylene lauryl ether 1 vol%.Will
Above-mentioned plating solution joins reactor, is passed through carbon dioxide until reactor pressure is 10 MPa, and heating makes the reactor temperature be
50 DEG C, make carbon dioxide reach supercriticality, and to account for reactor volume be 30 %.Electroplating cathode be through oil removing-cleaning-
Acid activation-cleaning-be dried brass substrate, anode is cobalt sheet, use direct current electrode position method, average current density is 2.5 A/
dm2, plating solution pH is 5, and magnetic agitation speed is 500 revs/min, and electroplating time is 1 h, prepares cobalt-nickel nano-alloy plating layer,
Performance is as shown in table 1.
Embodiment 3
The supercritical electroplating preparation method of a kind of cobalt-nickel alloy light protective coating, specifically comprises the following steps that
Preparing the electrolyte of cobalt-nickel nano-alloy plating layer, its component is: cobaltous chloride 50 g/L, nickel sulfate 150 g/L, sodium chloride
40 g/L, boric acid 50 g/L, sodium lauryl sulphate 0.2 g/L, saccharin sodium 2 g/L, Dodecyl Polyoxyethylene Ether 2 vol%.Will
Above-mentioned plating solution joins reactor, is passed through carbon dioxide until reactor pressure is 15 MPa, and heating makes the reactor temperature be
60 DEG C, make carbon dioxide reach supercriticality, and to account for reactor volume be 30 %.Electroplating cathode be through oil removing-cleaning-
Acid activation-cleaning-be dried brass substrate, anode is nickel sheet, use pulse plating method, average current density is 5.0A/
dm2, plating solution pH is 6, and magnetic agitation speed is 450 revs/min, and electroplating time is 1 h, prepares cobalt-nickel nano-alloy plating layer,
Performance is as shown in table 1.
Embodiment 4
The supercritical electroplating preparation method of a kind of cobalt-nickel alloy light protective coating, specifically comprises the following steps that
Preparing the electrolyte of cobalt-nickel nano-alloy plating layer, its component is: cobaltous sulfate 100 g/L, nickel sulfate 200 g/L, sodium sulfate
50 g/L, boric acid 40 g/L, sodium lauryl sulphate 0.1 g/L, saccharin sodium 1 g/L, ethyl vinyl ether 1 vol%.By above-mentioned
Plating solution joins reactor, is passed through carbon dioxide until reactor pressure is 12 MPa, and it is 70 that heating makes reactor temperature
DEG C, make carbon dioxide reach supercriticality, and to account for reactor volume be 40 %.Electroplating cathode is to live through oil removing-cleaning-acid
Change-clean-be dried brass substrate, anode is cobalt sheet, use direct current electrode position method, average current density is 10.0A/dm2, plating
Liquid pH is 5, and magnetic agitation speed is 600 revs/min, and electroplating time is 0.5 h, prepares cobalt-nickel nano-alloy plating layer, performance
As shown in table 1.
Embodiment 5
The supercritical electroplating preparation method of a kind of cobalt-nickel alloy light protective coating, specifically comprises the following steps that
Preparing the electrolyte of cobalt-nickel nano-alloy plating layer, its component is: cobaltous sulfate 100 g/L, nickel sulfate 200 g/L, sodium sulfate
50 g/L, boric acid 40 g/L, sodium lauryl sulphate 0.1 g/L, saccharin sodium 1 g/L, ethyl vinyl ether 1 vol%.By above-mentioned
Plating solution joins reactor, is passed through carbon dioxide until reactor pressure is 12 MPa, and it is 70 that heating makes reactor temperature
DEG C, make carbon dioxide reach supercriticality, and to account for reactor volume be 40 %.Electroplating cathode is to live through oil removing-cleaning-acid
Change-clean-be dried brass substrate, anode is cobalt sheet, use direct current electrode position method, average current density is 10.0A/dm2, plating
Liquid pH is 5, and magnetic agitation speed is 600 revs/min, and electroplating time is 0.5 h, prepares cobalt-nickel nano-alloy plating layer, performance
As shown in table 1.
Embodiment 6
As it is shown in figure 1, the supercritical plating preparation system of a kind of cobalt-nickel alloy light protective coating, including reactor 1, dioxy
Changing carbon gas bomb 2 and anolyte storage tank 3, described supercritical carbon dioxide fluid passes through cold from carbon dioxide steel cylinder 2
But using delivery pump 5 to be delivered in reactor 1 after device 4 cooling, described electrolyte is after anolyte storage tank 3 is by condenser 6
Being delivered in reactor 1, the electrolyte in described reactor 1 is dissolved with surfactant, is provided with magnetic agitation inside reactor
Device 7, with cobalt, nickel or cobalt-nickel alloy as anode in reactor 1, with workpiece to be plated as negative electrode, anode, negative electrode and electroplating power supply 8
Both positive and negative polarity electrical connection.In order to ensure the cooling effect of supercritical carbon dioxide fluid, arrange between delivery pump and reactor
There is heat exchanger 9.In order to ensure the stability of insurance system, at conveying supercritical carbon dioxide fluid and the conveyance conduit of electrolyte
Be additionally provided with Pressure gauge 10, thermometer 11 on reactor, conveniently carry out running monitoring.Meanwhile, at anolyte storage tank 3
Middle bottom is provided with enterprise's separator 12.
The performance of cobalt-nickel alloy coating prepared by the various example of table 1
| Numbering | Crystallite dimension/nm | Hardness/HV | Wear rate/10-5 mm3·(N·m)-1 | Rate of corrosion/mm y-1 |
| Embodiment 1 | 22 | 680~710 | 3.4 | 2.80×10-2 |
| Embodiment 2 | 12 | 730~750 | 2.0 | 1.10×10-2 |
| Embodiment 3 | 15 | 715~735 | 2.3 | 1.75×10-2 |
| Embodiment 4 | 20 | 690~725 | 2.7 | 2.30×10-2 |
| Embodiment 5 | 18 | 690~730 | 3.1 | 2.50×10-2 |
As it can be seen from table 1 the cobalt-nickel alloy coating hardness prepared of the present invention program is high, and there is the anti-attrition of excellence, wear-resisting
And decay resistance.And, from contrasting in appearance, cobalt-nickel alloy coating surface light prepared by the present invention program；Preparation
Process is simple, and prepared coating is applicable to requirement high rigidity, high abrasion, low friction and corrosion resistant parts, at automobile, machine
Tool, precision manufactureing and field of aerospace have a wide range of applications, and can extend the service life of part, reduce power consumption,
Save the energy, beneficially environmental conservation.
, being found by test, cobalt-nickel alloy coating prepared by the method for the invention is nanocrystalline structure, crystal grain meanwhile
A size of 10-30 nm；In nano-alloy plating layer, cobalt content is 70-85 %.Coating microhardness is 650-760 HV.Dry friction
Wear test shows (MS-T3000 clipping the ball dish friction wear testing machine, antithesis Φ 4.0 mm GCr15 steel ball, grinding defect diameter Φ
12 mm, load 2.0 N, rotating speed 0.188 m/s, rub 10 min, and friction environment is room temperature), coating wear rate is 1.8～3.5
×10-5 mm3•(N•m)-1；Electrochemical corrosion test uses electrochemical workstation, and measuring samples is at the NaCl aqueous solution of 3.5 wt%
In rate of corrosion, result shows that the rate of corrosion of coating is 0.8～3.2 × 10-2 mm∙y-1。
The above, only presently preferred embodiments of the present invention, not the present invention is made any pro forma restriction；All
The those of ordinary skill of the industry all can shown in by specification and the above and implement the present invention swimmingly；But, all familiar
Professional and technical personnel, in the range of without departing from technical solution of the present invention, may utilize disclosed above technology contents and makes
A little change, the equivalent variations modifying and develop, be the Equivalent embodiments of the present invention；Meanwhile, all realities according to the present invention
The change of any equivalent variations that above example is made by matter technology, modify and differentiation etc., all still fall within the technology of the present invention
Within the protection domain of scheme.
Claims (10)
1. the supercritical electroplating preparation method of a cobalt-nickel alloy light protective coating, it is characterised in that with cobalt, nickel or cobalt-nickel
Alloy is anode, with workpiece to be plated as negative electrode, electroplates in ternary system emulsion, and described ternary system emulsion includes
Electrolyte, surfactant and supercritical carbon dioxide fluid, described electrolyte is for including cobalt salt 20-100 g/L, nickel salt
50-200 g/L, sodium salt 20-100 g/L, boric acid 10-50 g/L, sodium lauryl sulphate 0.01-0.2 g/L, saccharin sodium 1-5
The mixed solution of g/L.
The supercritical electroplating preparation method of cobalt-nickel alloy light protective coating the most according to claim 1, its feature exists
In: one or both during cobalt salt is cobaltous sulfate and cobaltous chloride in described electrolyte, nickel salt is in nickel sulfate or Nickel dichloride.
Planting or two kinds, sodium salt is one or both in sodium sulfate and sodium chloride.
The supercritical electroplating preparation method of cobalt-nickel alloy light protective coating the most according to claim 2, its feature exists
In: described surfactant is Dodecyl Polyoxyethylene Ether, PEO-PPO, polyoxyethylene lauryl ether, ethyl vinyl ether surface
One in activating agent.
The supercritical electroplating preparation method of cobalt-nickel alloy light protective coating the most according to claim 3, its feature exists
In: described surface-active contents is 0.1-2.0 vol%.
The supercritical electroplating preparation method of cobalt-nickel alloy light protective coating the most according to claim 3, its feature exists
In: described carbon dioxide volume fraction in electroplating reaction still is 10-50 %.
The supercritical electroplating preparation method of cobalt-nickel alloy light protective coating the most according to claim 4, its feature exists
In: described electrolyte ph is 3-8, and during plating, magnetic agitation speed is 300-800 rev/min, and electroplating time is 0.5-2 h, electricity
Plating reactor pressure is 8-20 MPa, and reactor temperature is 35-80 DEG C.
The supercritical electroplating preparation method of cobalt-nickel alloy light protective coating the most according to claim 6, its feature exists
In: described plating uses unidirectional current or pulsive electroplating.
The supercritical electroplating preparation method of cobalt-nickel alloy light protective coating the most according to claim 7, its feature exists
In: described average current density is 1.0-20.0 A/dm2。
The supercritical electroplating preparation method of cobalt-nickel alloy light protective coating the most according to claim 8, its feature exists
In: described workpiece to be plated is copper, iron and steel, titanium or its alloy.
10. a cobalt-nickel alloy light protective coating supercritical plating preparation system, it is characterised in that include reactor, two
Carbon oxide gas steel cylinder and anolyte storage tank, described supercritical carbon dioxide fluid passes through cooling from carbon dioxide steel cylinder
Using delivery pump to be delivered in reactor after device cooling, described anolyte storage tank is defeated after anolyte storage tank is by condenser
Delivering in reactor, the electrolyte in described reactor is dissolved with surfactant, is provided with magnetic stirring apparatus inside reactor,
With cobalt, nickel or cobalt-nickel alloy as anode in reactor, with workpiece to be plated as negative electrode, anode, negative electrode and the both positive and negative polarity of electroplating power supply
Electrical connection.
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Cited By (2)
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| CN108130587A (en) * | 2018-02-05 | 2018-06-08 | 西南石油大学 | A kind of supercritical CO2Under the conditions of visualization electroplanting device and method |
| CN113618177A (en) * | 2021-08-17 | 2021-11-09 | 青岛理工大学 | Method for improving surface quality of alloy micro-area by salt film method and application |
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| CN108130587A (en) * | 2018-02-05 | 2018-06-08 | 西南石油大学 | A kind of supercritical CO2Under the conditions of visualization electroplanting device and method |
| CN113618177A (en) * | 2021-08-17 | 2021-11-09 | 青岛理工大学 | Method for improving surface quality of alloy micro-area by salt film method and application |
| CN113618177B (en) * | 2021-08-17 | 2022-06-28 | 青岛理工大学 | Method for improving surface quality of alloy micro-area by salt film method and application |
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Application publication date: 20161207 |
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