CN105908228A - Nickel alloy composition modulated multilayer alloy (CMMA) coating and preparation method thereof - Google Patents
Nickel alloy composition modulated multilayer alloy (CMMA) coating and preparation method thereof Download PDFInfo
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- CN105908228A CN105908228A CN201610389397.7A CN201610389397A CN105908228A CN 105908228 A CN105908228 A CN 105908228A CN 201610389397 A CN201610389397 A CN 201610389397A CN 105908228 A CN105908228 A CN 105908228A
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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
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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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
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
- C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
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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 provides a nickel alloy composition modulated multilayer alloy (CMMA) coating and a preparation method thereof. The nickel alloy CMMA coating is of a multilayer structure, and the number of layers of the nickel alloy CMMA coating is 50-1000. The coating structure comprises a nanoparticle phase and amorphous embedded nanocrystalline composite structure phase. The preparation method of the nickel alloy CMMA coating comprises the step that during electrodeposition, the nickel alloy CMMA coating with the compositions and structure changing periodically is obtained by changing the current density periodically to control the liquid-phase mass transfer process of an electrolyte in the cathode. According to the nickel alloy CMMA coating, performance design and microstructure adjustment and control can be achieved, the bonding force of the nickel alloy CMMA coating and a base material is good, the corrosion resistance and the abrasion resistance are excellent, and the nickel alloy CMMA coating can be widely applied to surface protection treatment of offshore engineering machines, water engineering metal structures and mechanical parts.
Description
Technical field
The invention belongs to metal protection technical field, be specifically related to a kind of nickel alloy CMMA coating and preparation method thereof.
Background technology
Ni base W, Mo, B alloy is used widely in Aero-Space, electronic device, automotive hub, work mechanical protection field, sea with its good hardness, corrosion-proof wear, mechanical strength.In recent years, composite nano-ceramic granule prepares nano composite ceramic plated layer mutually in the alloy has become study hotspot in recent years, as added TiO in Ni base alloy2、α-Al2O3、SiO2, SiC, TiN etc., not only can improve alloy rigidity, wearability, its corrosion resistance can be strengthened simultaneously.But owing in electrochemical deposition preparation process, cathode hydrogen evolution and residual stress can cause coating to there is pore, through hole or micro-crack defect, these defects are difficult to effectively control, fundamentally limit the raising of its barrier propterty, it has also become the difficult problem that work protection field, sea is urgently to be resolved hurrily.
Regulating microstructure and performance design, as the main path of raising coating ocean barrier propterty further, have taken the important development trend becoming sea work Material Field.Recent study shows, CMMA alloy (Composition modulated multilayer alloy) has the performance more superior than the alloy of same composition thickness, its corrosion resisting property is up to same thickness single layer alloy (Monolayer, Monolithic alloy) 45 times, there is huge performance advantage.CMMA multilamellar multiple solutions structure makes the defect of every layer terminate at adjacent interfaces; do not extend through hole to be formed; corrosive medium has been delayed to arrive the time of base material; owing to the corrosive medium (electrolyte) of surface microdefect, filling forms electric double layer capacitance with adjacent layer interface; process is controlled by charge transfer step; make corrosion tendency in the most progressively carrying out, there is more preferable protected effect.Prior art CN101462819, CN101445946, CN102747389A etc. have studied nickel-base alloy, its performance increases, but not obtaining basic suppression owing to affecting the formation of the key factor-through hole of corrosion resistance of coating, its performance does not has great-leap-forward to promote.For the marine environment that complexity is severe, being regulated and controled by performance design and micro structure, solve through hole problem, the advanced high-performance marine long-lasting protection coating technology of exploitation is to advancing ocean development strategy to have important function.
Summary of the invention
Solve the technical problem that:Instant invention overcomes nickel alloy plating layer in prior art and form the technical problem that the corrosion resistance caused is low due to through hole, it is provided that a kind of nickel alloy CMMA coating and preparation method thereof.
Technical scheme:A kind of nickel alloy CMMA coating, this coating is multiple structure, and the number of plies is 50～1000；Containing nano-particle phase and amorphous embedding nano crystalline substance composite construction phase in coating structure.
Further, the one during described nickel alloy is Ni-W, Ni-B or Ni-Zn alloy.
The preparation method of described nickel alloy CMMA coating, when electro-deposition by periodically-varied electric current density to control the electrolyte mass transfer in liquid phase process at negative electrode, thus obtains the nickel alloy CMMA coating of composition and structural periodicity change.
Further, described periodic current density is particularly as follows: electric current existsi 1- i 2Between circulation change, the low value of electric current densityi 1It is 0.10～2.00A/dm2, the high level of electric current densityi 2It is 2.50～10A/dm2, each deposition cycle T is 0.2～10s, and total periodicity N is 50～1000.
Further, described electrolyte includes in terms of mass concentration: nickel salt 150～350g/L, the second main salt 1～6 g/L, nanoparticle 0.01～20g/L, buffer agent 20～50g/L, dispersant 0～1g/L, wetting agent 0～1g/L, auxiliary agent 0.1～2g/L, solvent is water.
Further, at least one in nickel sulfate, Nickel dichloride. or basic nickel carbonate of described nickel salt, and nickel sulfate must be contained.
Further, described second main salt is the one in sodium tungstate, potassium tungstate, ammonium tungstate, trimethylamine borane, sodium borohydride, zinc sulfate, zinc chloride, zinc nitrate.
Further, described nanoparticle is TiO2、α-Al2O3、SiO2, one in SiC or TiN, particle diameter is 0.005～2 μm.
Further, described buffer agent is boric acid.
Further, the one during described dispersant is sodium citrate, citric acid, sodium tartrate, tartaric acid, boric acid, sodium borate or sulfamic acid.
Further, the one during described wetting agent is sodium lauryl sulphate, dodecyl sodium sulfate, polyoxyethylenated alcohol sodium sulfate (AES), polyoxyethylated alkyl phenol sodium sulfate salt (DRO), fatty alcohol-polyoxyethylene ether (JFC), NPE (NP-10) or OPEO (OP-10).
Further, described auxiliary agent can be saccharin, brightener, smoothing agent.
Further, the pH value of described electrolyte is 3～9.
Further, during electro-deposition, the temperature of electrolyte is 35～75 DEG C.
Beneficial effect:
1, a kind of nickel alloy CMMA coating CMMA structure design disclosed by the invention regulates and controls method with performance, the Ni base alloy of preparation has CMMA multiple structure (50-1000 layer), compare traditional multiple structure (generally less than five layers), greatly suppressing the formation of coating through hole, corrosion resistance significantly improves.Simultaneously because the addition of nano-ceramic particle, the wearability of coating, hardness have also been obtained and significantly improves, and improves its protection life-span under the complexity various factors coupling environment of ocean.
2, the preparation method of the Ni base alloy CMMA overcoat that the present invention provides can be according to actual needs, the number of plies to coating, Rotating fields, layer thickness, layer composition, and the content distribution of nano-ceramic particle phase, nanometer crystalline phase is designed, improve the operability of coating micro structure regulation and control, the performance design research to advanced coating from now on has reference value.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of electric current density straight line in time change in embodiment 1；
Fig. 2 is the schematic diagram of electric current density nonlinear change in time in embodiment 2；
Fig. 3 is the Ni-B/SiC of embodiment 11.0/4.0/500The structural representation of coating.
Detailed description of the invention
Following example further illustrate present disclosure, but should not be construed as limitation of the present invention.Without departing from the spirit and substance of the case in the present invention, the amendment that the inventive method, step or condition are made and replacement, belong to the scope of the present invention.If not specializing, the conventional means that technological means used in embodiment is well known to those skilled in the art.
The nickel alloy CMMA coating of the present invention, for CMMA multiple structure, the number of plies is 50～1000；Coating structure has heterogeneous Analysis On Multi-scale Features: include the nano-particle phase of nanoscale, nanometer crystalline phase and the amorphous phase of micro-meter scale, the amorphous embedding nano crystalline substance composite construction phase of micro-meter scale, the most also layer structure of micro-meter scale.
CMMA alloy (Composition modulated multilayer alloy) has the performance more superior than the alloy of same composition thickness, its corrosion resisting property up to same thickness single layer alloy (Monolayer,
Monolithic alloy) 45 times, there is huge performance advantage.In the present invention, the CMMA multilamellar multiple solutions structure of nickel alloy CMMA coating makes the defect of every layer terminate at adjacent interfaces, does not extends through hole and is formed, and has delayed corrosive medium to arrive the time of base material.Owing to the corrosive medium (electrolyte) of surface microdefect, filling forms electric double layer capacitance with adjacent layer interface, process is controlled by charge transfer step, makes corrosion tendency in the most progressively carrying out, has more preferable protected effect.
This nickel alloy CMMA coating uses electro-deposition method to prepare, anode is graphite, nickel plate or DSA, negative electrode is workpiece, changes the electrolyte mass transfer in liquid phase process at negative electrode by periodic current density domination, thus obtains the nickel alloy CMMA coating of composition and structural periodicity change.Computer or automatic control unit is used to automatically control cathode-current density and existi 1- i 2Between circulation change, the low value of electric current densityi 1It is 0.10～2.00A/dm2, the high level of electric current densityi 2Span is 2.50～10.00A/dm2, each deposition cycle T is 0.2～10s, and electrodeposition time total periodicity N in terms of the electric current density cycle is 50～1000, and the total number of plies therefore obtaining coating is also 50～1000 with number of deposition cycles.
In the present invention, electric current density existsi 1- i 2Between consecutive variations, can be linear change, it is also possible to be nonlinear change, Fig. 1 represents that cathode current existsi 1- i 2Between continuous print nonlinear change, in like manner,i 1- i 2Between consecutive variations can be straight line, but can not interrupt, the interrupting of electric current can produce certain adverse effect to the regulation and control of CMMA micro structure.
The present invention makees electrolyte with the mixed liquor containing nickel salt, the second main salt, nanoparticle, buffer agent, dispersant, wetting agent and auxiliary agent, by control design case and control circulate cathode-current density (cycle
Cathode current censities, is designated as CCCD ' s), makes CCCD ' s existi 1- i 2Between consecutive variations circulation, each current cycle cycle is designated as T, and the time is 0.2～10s, electro-deposition 50～1000 periodicity (being designated as N), it is thus achieved that have CMMA(composition
Modulated multilayer alloy, is designated as CMMA) coating of structure, it is designated as Ni-B/SiC1/2/n, wherein 1,2 representing the low of CCCD ' s and high current density value respectively, cyclomorphosis is to obtain the layer of different composition between 1,2 for deposition current, and n represents total number of plies of coating.CMMA multilamellar multiple solutions structure makes the defect of every layer terminate at adjacent interfaces, does not extends through hole and is formed, and has delayed corrosive medium to arrive the time of base material.Owing to the corrosive medium (electrolyte) of surface microdefect, filling forms electric double layer capacitance with adjacent layer interface, process is controlled by charge transfer step, makes corrosion tendency in the most progressively carrying out, has more preferable protected effect.
Embodiment 1
Take nickel sulfate 250g, trimethylamine borane 2g, boric acid 60g, the SiC 4g of 1 μm particle diameter, saccharin 1g and sodium lauryl sulphate 0.01g, the electrolyte of 1 liter it is configured to deionized water, using sodium hydroxide solution to adjust its pH value is 3.5, using water-bath to control temperature is 45 DEG C, mechanical agitation 1 hour, ultrasound wave disperses 30 minutes.
Arrangei 1=1A/dm2,i 2=4A/dm2, T=2s, N=500, with graphite as anode, Q235 steel is negative electrode, and electric current density existsi 1、i 2Between continuous linear change, as it is shown in figure 1, deposition obtain Ni-B/SiC1.0/4.0/500, wherein subscript 1.0 representsi 1=1A/dm2, subscript 4.0 representsi 2=4A/dm2, it is 500 that subscript 500 represents the total number of plies of coating.
Through the Ni-B/SiC that said method obtains1.0/4.0/500Coating, the total number of plies of coating is 500, gross thickness about 66 μm, and microstructure display coating contains nanometer crystalline phase, and SiC nanometer is evenly distributed mutually, without through hole.Coating is good with the adhesion of base material, and corrosion resistance wearability significantly improves.As it is shown on figure 3, gained coating is CMMA multiple structure, there is CMMA multilamellar multiple solutions Analysis On Multi-scale Features.
Embodiment 2
Take nickel sulfate 150g, Nickel dichloride. 120g, trimethylamine borane 6g, the SiC 5g of boric acid 30,1 μm particle diameter, saccharin 2g, AES 0.4g, the electrolyte of 1 liter it is configured to deionized water, using sodium hydroxide solution to adjust its pH value is 4.0, using water-bath to control temperature is 60 DEG C, mechanical agitation 1 hour, ultrasound wave disperses 15 minutes.
Arrangei 1=1.0A/dm2,i 2=5A/dm2, T=4s, N=250, with nickel plate as anode, Q235 steel is negative electrode, and electric current density existsi 1、i 2Between Continuous Nonlinear change, as in figure 2 it is shown, deposition obtain Ni-B/SiC1.0/5.0/250, wherein subscript 1.0 representsi 1=1.0A/dm2, subscript 5.0 representsi 2=5.0A/dm2, it is 250 that subscript 250 represents total number of plies of coating.
Through the Ni-B/SiC that said method obtains1.0/5.0/250Coating, the total number of plies of coating is 250, gross thickness about 95 μm, and microstructure display coating contains nanometer crystalline phase, and SiC nanometer is evenly distributed mutually, without through hole.Coating is good with the adhesion of base material, and corrosion resistance wearability significantly improves.
Embodiment 3
Take nickel sulfate 150g, Nickel dichloride. 50g, sodium tungstate 120g, sulfamic acid 12g, the TiO of 1 μm particle diameter215g, ammonium chloride 65g, AES 0.4g, be configured to the electrolyte of 1 liter with deionized water, and using sodium hydroxide solution to adjust its pH value is 7.0, and using water-bath to control temperature is 70 DEG C, mechanical agitation 1 hour, and ultrasound wave disperses 15 minutes.
Arrangei 1=1.0A/dm2 , i 2=5A/dm2, T=4s, N=250, with nickel plate as anode, Q235 steel is negative electrode, and electric current density is at i1、i2Between continuous linear change, deposition obtain Ni-W/
TiO21.0/5.0/250, wherein subscript 1.0 representsi 1=1.0A/dm2, subscript 5.0 representsi 2=5.0A/dm2, it is 250 that subscript 250 represents total number of plies of coating.
Through the Ni-W/ TiO that said method obtains21.0/5.0/250Coating, the total number of plies of coating is 250, gross thickness about 94 μm, and microstructure display coating contains nanometer crystalline phase, TiO2Nanometer is evenly distributed mutually, without through hole.Coating is good with the adhesion of base material, and corrosion resistance wearability significantly improves.
Embodiment 4
Take nickel sulfate 350g, sodium tungstate 100g, boric acid 20g, the α-Al of 2 μm particle diameters2O3
2g, ammonium chloride 70g, DRO
1g, is configured to the electrolyte of 1 liter with deionized water, and using sodium hydroxide solution to adjust its pH value is 7.0, and using water-bath to control temperature is 75 DEG C, mechanical agitation 1 hour, and ultrasound wave disperses 30 minutes.
Arrangei 1=1.0A/dm2,i 2=2A/dm2, T=2 s, N=800, with graphite as anode, Q235 steel is negative electrode, and electric current density is at i1、i2Between continuous linear change, deposition obtain Ni-W/Al2O31.0/2.0/800, wherein subscript 1.0 representsi 1=1.0A/dm2, subscript 2.0 representsi 2=2.0A/dm2, it is 800 that subscript 800 represents total number of plies of coating.
Through the Ni-W/Al that said method obtains2O31.0/2.0/800Coating, the total number of plies of coating is 800, gross thickness about 112 μm, and microstructure display coating contains nanometer crystalline phase, Al2O3Nanometer is evenly distributed mutually, without through hole.Coating is good with the adhesion of base material, and corrosion resistance wearability significantly improves.
Embodiment 5
Take nickel sulfate 300g, zinc phosphate 100g, trimethylamine borane 4g, boric acid 35g, the TiN 9g of 1 μm particle diameter, saccharin 1g, JFC 0.3g, the electrolyte of 1 liter it is configured to deionized water, using sodium hydroxide solution to adjust its pH value is 3.8, using water-bath to control temperature is 40 DEG C, mechanical agitation 6 hours, ultrasound wave disperses 25 minutes.
Arrangei 1=2.0A/dm2,i 2=8A/dm2, T=2s, N=100, with nickel plate as anode, Q235 steel is negative electrode, and electric current density is at i1、i2Between continuous linear change, deposition obtain Ni-B/TiN
2.0/8.0/100, wherein subscript 2.0 representsi 1=2.0 A/dm2, subscript 8.0 representsi 2=8A/dm2, it is 100 that subscript 100 represents total number of plies of coating.
Through the Ni-Zn/TiN that said method obtains2.0/8.0/100Coating, the total number of plies of coating is 100, gross thickness about 153 μm, and microstructure display coating contains nanometer crystalline phase, and TiN nanometer is evenly distributed mutually, without through hole.Coating is good with the adhesion of base material, and corrosion resistance wearability significantly improves.
Claims (10)
1. a nickel alloy CMMA coating, it is characterised in that: this coating is multiple structure, and the number of plies is 50～1000；Containing nano-particle phase and amorphous embedding nano crystalline substance composite construction phase in coating structure.
Nickel alloy CMMA coating the most according to claim 1, it is characterised in that: described nickel alloy is the one in Ni-W, Ni-B or Ni-Zn alloy.
3. the preparation method of the nickel alloy CMMA coating described in claim 1, it is characterized in that: when electro-deposition by periodically-varied electric current density to control the electrolyte mass transfer in liquid phase process at negative electrode, thus obtain the nickel alloy CMMA coating of composition and structural periodicity change.
The preparation method of nickel alloy CMMA coating the most according to claim 3, it is characterised in that: described periodic current density is particularly as follows: electric current existsi 1- i 2Between circulation change, the low value of electric current densityi 1It is 0.10～2.00A/dm2, the high level of electric current densityi 2It is 2.50～10A/dm2, each deposition cycle T is 0.2～10s, and total periodicity N is 50～1000.
The preparation method of nickel alloy CMMA coating the most according to claim 3, it is characterized in that: described electrolyte includes in terms of mass concentration: nickel salt 150～350g/L, second main salt 1～6 g/L, nanoparticle 0.01～20g/L, buffer agent 20～50g/L, dispersant 0～1g/L, wetting agent 0～1g/L, auxiliary agent 0.1～2g/L, solvent is water.
The preparation method of nickel alloy CMMA coating the most according to claim 5, it is characterised in that: at least one in nickel sulfate, Nickel dichloride. or basic nickel carbonate of described nickel salt, and nickel sulfate must be contained.
The preparation method of nickel alloy CMMA coating the most according to claim 5, it is characterised in that: described second main salt is the one in sodium tungstate, potassium tungstate, ammonium tungstate, trimethylamine borane, sodium borohydride, zinc sulfate, zinc chloride, zinc nitrate.
The preparation method of nickel alloy CMMA coating the most according to claim 5, it is characterised in that: described nanoparticle is TiO2、α-Al2O3、SiO2, one in SiC or TiN, particle diameter is 0.005～2 μm.
The preparation method of nickel alloy CMMA coating the most according to claim 5, it is characterised in that: described buffer agent is boric acid；Described dispersant is the one in sodium citrate, citric acid, sodium tartrate, tartaric acid, boric acid, sodium borate or sulfamic acid；Described wetting agent is the one in sodium lauryl sulphate, dodecyl sodium sulfate, polyoxyethylenated alcohol sodium sulfate, polyoxyethylated alkyl phenol sodium sulfate salt, fatty alcohol-polyoxyethylene ether, NPE or OPEO.
The preparation method of nickel alloy CMMA coating the most according to claim 3, it is characterised in that: during electro-deposition, the temperature of electrolyte is 35～75 DEG C.
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Cited By (7)
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| CN107034496A (en) * | 2017-06-26 | 2017-08-11 | 河海大学 | A kind of method for preparing Ni Co nano composite multiple layer alloys |
| CN107268046A (en) * | 2017-06-14 | 2017-10-20 | 河海大学 | A kind of preparation method of Ni W P graded alloy |
| CN107268045A (en) * | 2017-06-08 | 2017-10-20 | 河海大学 | A kind of Ni B CMMA multilayer alloy preparation methods based on cyclic voltammetry |
| CN107326410A (en) * | 2017-06-23 | 2017-11-07 | 河海大学 | A kind of method that many current potential cycle step methods prepare CMMA multilayer Ni W alloys |
| CN111607816A (en) * | 2020-06-03 | 2020-09-01 | 暨南大学 | Method for pulse electrodeposition of Ni-SiC composite coating on surface of aluminum alloy |
| WO2022013354A1 (en) * | 2020-07-17 | 2022-01-20 | Parker Hannifin Emea S.À.R.L. | Method and system for forming a multilayered zinc alloy coating and metallic article |
| CN115928162A (en) * | 2022-12-13 | 2023-04-07 | 国网辽宁省电力有限公司锦州供电公司 | Alloy electroplating solution for overhead transmission line tower and electroplating method thereof |
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| CN107268045A (en) * | 2017-06-08 | 2017-10-20 | 河海大学 | A kind of Ni B CMMA multilayer alloy preparation methods based on cyclic voltammetry |
| CN107268045B (en) * | 2017-06-08 | 2019-06-07 | 河海大学 | A kind of Ni-B CMMA multilayer alloy preparation method based on cyclic voltammetry |
| CN107268046A (en) * | 2017-06-14 | 2017-10-20 | 河海大学 | A kind of preparation method of Ni W P graded alloy |
| CN107268046B (en) * | 2017-06-14 | 2019-03-01 | 河海大学 | A kind of preparation method of Ni-W-P graded alloy |
| CN107326410A (en) * | 2017-06-23 | 2017-11-07 | 河海大学 | A kind of method that many current potential cycle step methods prepare CMMA multilayer Ni W alloys |
| CN107034496A (en) * | 2017-06-26 | 2017-08-11 | 河海大学 | A kind of method for preparing Ni Co nano composite multiple layer alloys |
| CN107034496B (en) * | 2017-06-26 | 2019-04-26 | 河海大学 | A method of preparing Ni-Co nano composite multiple layer alloy |
| CN111607816A (en) * | 2020-06-03 | 2020-09-01 | 暨南大学 | Method for pulse electrodeposition of Ni-SiC composite coating on surface of aluminum alloy |
| WO2022013354A1 (en) * | 2020-07-17 | 2022-01-20 | Parker Hannifin Emea S.À.R.L. | Method and system for forming a multilayered zinc alloy coating and metallic article |
| CN115928162A (en) * | 2022-12-13 | 2023-04-07 | 国网辽宁省电力有限公司锦州供电公司 | Alloy electroplating solution for overhead transmission line tower and electroplating method thereof |
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