CN111876801A - Crack-free Ni-Cr alloy coating and preparation method and application thereof - Google Patents
Crack-free Ni-Cr alloy coating and preparation method and application thereof Download PDFInfo
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- CN111876801A CN111876801A CN202010681788.2A CN202010681788A CN111876801A CN 111876801 A CN111876801 A CN 111876801A CN 202010681788 A CN202010681788 A CN 202010681788A CN 111876801 A CN111876801 A CN 111876801A
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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
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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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
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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Abstract
The invention provides a crack-free Ni-Cr alloy plating layer and a preparation method and application thereof, wherein in the Ni-Cr alloy plating layer, the content of Cr is 15-25% and the balance is Ni in percentage by mass. The preparation method comprises the following steps: putting a titanium platinized plate into the electroplating solution to be used as an anode, and putting a metal workpiece with poor corrosion resistance or poor high-temperature oxidation resistance into the electroplating solution to be used as a cathode; the power supply is switched on, and the current density is controlled to be 8-15A/dm2The temperature of the electroplating solution is 20-30 ℃, the pH value is 2.0-3.0, the mechanical stirring speed is 200-300 r/min, and the electroplating time is 15-35 min. The Ni-Cr alloy coating prepared by the invention can be used as a protective coating of a metal material with poor corrosion resistance or no high-temperature oxidation resistance, and can be used for protecting metal materials of thermal power generation, petrifaction, energy transmission pipelines and offshore oil exploitation platforms.
Description
Technical Field
The invention relates to the technical field of alloy electrodeposition, in particular to a crack-free Ni-Cr alloy plating layer and a preparation method and application thereof.
Background
It is known that Ni-Cr alloys have corrosion resistance in corrosive liquid phase media, which increases with increasing Cr co-precipitation; when the Cr content reaches 20% (mass percent), the alloy can be thermally grown below 1000 DEG CContinuous protective Cr2O3And the oxide film has high temperature oxidation resistance. However, at present, Ni and Cr are not used for preparing a high-quality Ni-Cr alloy plating layer with corrosion resistance and high-temperature oxidation resistance by co-electrodeposition, and the key of the problem is that the plating layer inevitably generates micro cracks and through cracks along with the increase of the Cr content, so that the corrosion resistance and the high-temperature oxidation resistance are poor.
Disclosure of Invention
In order to solve the technical problems, the invention provides a crack-free Ni-Cr alloy plating layer in a first aspect, wherein in the Ni-Cr alloy plating layer, the content of Cr is 15-25% by mass percent, and the balance is Ni.
The second aspect of the invention provides a preparation method of a crack-free Ni-Cr alloy plating layer, wherein a titanium platinum plate is put into electroplating solution to be used as an anode, and a metal workpiece with poor corrosion resistance or no high-temperature oxidation resistance is put into the electroplating solution to be used as a cathode; the power supply is switched on, and the current density is controlled to be 8-15A/dm2The temperature of the electroplating solution is 20-30 ℃, the pH value is 2.0-3.0, the mechanical stirring speed is 200-300 r/min, and the electroplating time is 15-35 min.
Wherein the metal workpiece may be a Ni-based alloy, Fe-based alloy, carbon steel or alloy steel.
Wherein, the components and the concentration of the electroplating solution are as follows: 0.3 to 0.4mol/LCrCl3·6H2O，0.03~0.05mol/LNiCl2·6H2O，0.25~0.35mol/L Na3C6H5O7，0.85~0.9mol/L HCOONa，0.9~1.1mol/L CH4ON2，0.8~0.9mol/L NH4Cl，0.14~0.16mol/L NaB，0.65~0.8 mol/L H3BO30.1-0.2 g/L sodium dodecyl sulfate and 0.75-1.5 g/L saccharin.
Wherein the basic formula of the electroplating solution is a chloride system.
Wherein, in the electroplating solution, the mass percentage concentration of NaCl is 3.0-4.0%.
The metal workpiece is pretreated before electroplating, and the specific process comprises the following steps: mechanical polishing → flow water washing → chemical degreasing → flow water washing → deionized water washing → acid washing → flow water washing → deionized water washing.
Wherein, the metal workpiece is chemically degreased by adopting alkaline solution, and the components and the concentration of the alkaline solution are 15g/L NaOH and 30g/L Na2CO3，10 g/L Na3PO4·12H2O。
Wherein, the metal workpiece is pickled by adopting a pickling solution, and the formula of the pickling solution comprises the following components in percentage by volume: HF: HNO3:H2SO4:H2O =1:1:1:7, and the pickling time is 15 min.
Wherein, the metal workpiece with the electroplated surface containing the Ni-Cr alloy coating is placed below 1000 ℃, and continuous protective Cr is thermally grown on the surface of the Ni-Cr alloy coating2O3And (5) oxidizing the film.
The third aspect of the invention provides application of a crack-free Ni-Cr alloy coating, wherein the Ni-Cr alloy coating can be used as a protective coating of a metal material with poor corrosion resistance or no high-temperature oxidation resistance, and can be used for protecting metal materials of thermal power generation, petrifaction, energy transmission pipelines and offshore oil exploitation platforms.
The invention has the beneficial effects that:
the invention uses commonly used environment-friendly Cr3+The chloride system is a basic plating solution, and the technical bottleneck of preparing the crack-free Ni-Cr alloy plating layer with the Cr content of up to 25 percent is broken through improving and optimizing the components of the chloride system, and the prepared alloy plating layer not only has excellent corrosion resistance in a corrosive solution, but also can form continuous protective Cr in a high-temperature oxidation atmosphere2O3The oxide film has ideal high-temperature oxidation resistance.
The Ni-Cr alloy coating prepared by the invention has the following advantages:
1. the plating layer has no cracks;
2. the Cr in the plating layer is uniformly distributed, the content is continuously controllable, and the Cr content can reach 25 percent at most;
3. the coating is used as a protective coating of Ni-based alloy, Fe-based alloy, carbon steel, alloy steel and the like, and can greatly improve the corrosion resistance of the Ni-based alloy, the Fe-based alloy, the carbon steel, the alloy steel and the like in a corrosive solution;
4. as Ni-based alloy,High-temperature protective coating of Fe-based alloy, carbon steel, alloy steel and the like, which can be used at high temperature (less than 1000)oC) Ambient thermal growth of Cr2O3Protective oxide films, converting them from non-oxidation to oxidation;
5. the plating layer can be directly used without vacuum diffusion treatment;
6. the coating has bright color and can be used as a corrosion-resistant decorative coating;
7. the coating can be used for protecting metal materials such as thermal power generation, petrifaction, energy transmission pipelines, offshore oil exploitation platforms and the like;
8. the plating layer has simple preparation process, low cost, easy preparation and wide application range.
Detailed Description
The following is a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements are also considered to be within the scope of the present invention.
The invention provides a preparation method of a crack-free Ni-Cr alloy coating, which comprises the following steps:
s1, firstly, preprocessing the nickel sheet of the metal workpiece, wherein the preprocessing comprises the following steps: mechanical polishing → flow washing → chemical degreasing → flow washing → deionized water washing → acid washing → flow washing → deionized water washing;
the mechanical grinding is to grind the nickel sheet to be bright and free of scratches by sequentially adopting 600#, 800#, 1000#, 1200#, 1500# and 2000# sand papers;
the chemical oil removal is to place the nickel sheet in alkaline solution, wherein the components and the concentration of the alkaline solution are 15g/L NaOH and 30g/LNa2CO3，10 g/L Na3PO4·12H2O；
The pickling process is to put the nickel sheet into a pickling solution, wherein the formula of the pickling solution comprises the following components in percentage by volume: HF: HNO3:H2SO4:H2O =1:1:1:7, and the pickling time is 15 min;
s2, putting the titanium platinized plate into the electroplating solution as an anodePutting the nickel sheet pretreated in the step S1 into electroplating solution to be used as a cathode; the power supply is switched on, and the current density is controlled to be 12A/dm2Electroplating at 25 deg.C and pH 2.5 for 20min at a mechanical stirring speed of 250 r/min;
s3, placing the nickel sheet with the Ni-Cr alloy plating layer on the surface after the electroplating in the step S2 below 950 ℃, and thermally growing continuous protective Cr on the surface of the Ni-Cr alloy plating layer2O3And (5) oxidizing the film.
The components and concentrations of the plating solution used in this example were:
0.35mol/LCrCl3·6H2O，0.04mol/L NiCl2·6H2O，0.3mol/L Na3C6H5O7，0.87mol/LHCOONa， 1.0mol/L CH4ON2，0.85mol/L NH4Cl，0.15mol/L NaB，0.7 mol/L H3BO30.15g/L sodium dodecyl sulfate and 1g/L saccharin.
In the coating prepared by adopting the conventional Ni-Cr alloy electroplating solution formula in the prior art, the Cr content is 12% by mass, the coating has more microcracks, and the surface appearance of SEM is shown in figure 1.
In the plating layer prepared by adopting the electroplating solution formula and the electroplating method provided by the embodiment of the invention, the mass percentage of the Cr content is 20%, the crystallization of the plating layer is fine, the micro-cracks of the plating layer are eliminated, and the surface appearance of SEM is shown in figure 2.
In order to verify the effect of current density on the Cr content of the Ni-Cr alloy coating, the current density was set to 6A/dm in sequence with reference to the above examples, while keeping other process parameters unchanged2，8A/dm2，10A/dm2，12A/dm2，14A/dm2，16A/dm2And testing the content of Cr in the coating. FIG. 3 is a graph showing the Cr content of the plated layer as a function of current density, and it can be seen from FIG. 3 that the Cr content of the plated layer increases as the current density increases when the current density is small, and at a current density of 12A/dm2The maximum value is reached, but then the Cr content in the coating is reduced with the increase of the current density. This is because Cr3+The deposition potential of (a) is relatively negative,at lower current densities, the cathode deposits mainly Ni2+，Cr3+Is difficult to be deposited, and as the current density is increased, the cathode polarization is increased, so that Cr is generated3+The reduction reaction at the cathode is smoothly performed; however, when the cathode current density is too high, a large amount of hydrogen is evolved on the cathode surface and competes with the cathode metal reduction deposition, which is not favorable for Cr3+The surface of the coating is scorched and blackened, the edge of the coating is loose and skinned, and the binding force of the coating is poor, so that the cathode current density is preferably 10-14A/dm to obtain the qualified coating with high Cr content2。
Fig. 4 is a comparison graph of polarization curves of the Ni substrate and the Ni-20Cr (Cr content 20%) alloy plating layer in the NaCl solution with a mass concentration of 3.5%, and it can be seen from fig. 4 that the self-corrosion current of the Ni-Cr alloy plating layer is significantly smaller than that of the Ni substrate, and therefore the corrosion resistance of the Ni-Cr alloy plating layer in the NaCl solution with a mass concentration of 3.5% is significantly improved.
In order to verify the influence of the Cr content in the Ni-Cr alloy coating on the oxidation rate of the Ni-Cr alloy coating, the temperature is controlled at 900 DEGoGrowth of Cr during oxidation of Ni-20Cr alloy coating2O3The oxidation characteristics and properties of the film were compared with the oxidation characteristics of a Ni substrate containing no Cr and a Ni-15Cr (Cr content 15%) alloy coating.
FIG. 5 is a graph showing the oxidation kinetics of a Ni substrate, a Ni-15Cr alloy plating layer, and a Ni-20Cr alloy plating layer at 900 ℃ for 20h, and it can be seen from FIG. 5 that the oxidation rate of the Ni-20Cr alloy plating layer is sharply reduced, and the plating layer is hardly increased in weight from the 15 th h, indicating that a dense protective film is formed on the surface of the plating layer, and the inner layer metal is protected from further oxidation, and the oxidation rate of the Ni-15Cr alloy plating layer is lower than that of the Ni substrate but higher than that of the Ni-20Cr alloy plating layer, indicating that a part of the oxide layer protective film is formed on the surface of the plating layer.
FIG. 6 is an SEM surface morphology of an oxide layer of a Ni substrate, and it can be seen from FIG. 6 that NiO grains grown on the Ni substrate are coarse; the grains of the oxide growing on the Ni-15Cr alloy plating layer and the Ni-20Cr alloy plating layer are fine, FIG. 7 is an SEM surface topography of the oxide layer of the Ni-20Cr alloy plating layer, and as can be seen from FIG. 7, the oxidation on the Ni-20Cr alloy plating layerThe crystal grains are more obvious. From this, it is understood that the reduction of the crystal grains is associated with the reduction of the oxidation growth rate due to the formation of Cr-rich2O3Due to the oxide layer(s).
The above results were also confirmed from the corresponding XRD analysis, and FIG. 8 is a graph showing the results of XRD analysis of Ni-20Cr alloy plating, and it can be seen from FIG. 8 that NiO and NiCr are contained in the oxide layer of Ni-20Cr alloy plating2O4Very little, mainly Cr2O3Description of the continuous protective Cr2O3The film can be formed quickly. The corresponding cross-sectional shapes of the Ni substrate, the Ni-15Cr alloy plating layer and the Ni-20Cr alloy plating layer after being oxidized for 20 hours at 900 ℃ are respectively shown in fig. 9, fig. 10 and fig. 11, and the thick non-compact NiO oxide layer can be grown on the Ni substrate, while the Ni-15Cr alloy plating layer can grow Cr2O3But becomes significantly thinner due to the growth of Cr in different places2O3The uneven speed of the Ni-20Cr alloy coating results in uneven thickness of the oxide layer, and continuous Cr2O3The film can be formed quickly, so that the oxide film is very thin, and the Ni-20Cr alloy coating has ideal high-temperature oxidation resistance.
The Ni-Cr alloy coating prepared by the method provided by the invention can form Cr-rich alloy in corrosive solution2O3And thermally growing protective Cr in a high temperature environment2O3The film can be used as a protective coating of metal materials with poor normal-temperature corrosion resistance or high-temperature oxidation resistance, such as Ni-based alloy, Fe-based alloy, carbon steel, alloy steel and the like, has simple process and low preparation cost, and is easy to popularize and apply to normal-temperature/high-temperature corrosion protection of metal structural materials of thermal power generation, petrifaction, energy transmission pipelines, offshore oil exploitation platforms and the like.
The above examples only express the specific embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the spirit of the present invention, and these changes and modifications are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A crack-free Ni-Cr alloy coating is characterized in that: in the Ni-Cr alloy plating layer, the content of Cr is 15-25% by mass percent, and the balance is Ni.
2. A preparation method of a crack-free Ni-Cr alloy coating is characterized by comprising the following steps: putting a titanium platinized plate into the electroplating solution to be used as an anode, and putting a metal workpiece with poor corrosion resistance or poor high-temperature oxidation resistance into the electroplating solution to be used as a cathode; the power supply is switched on, and the current density is controlled to be 8-15A/dm2The temperature of the electroplating solution is 20-30 ℃, the pH value is 2.0-3.0, the mechanical stirring speed is 200-300 r/min, and the electroplating time is 15-35 min.
3. The method of claim 2, wherein the plating solution comprises the following components in concentration: 0.3 to 0.4mol/LCrCl3·6H2O，0.03~0.05mol/L NiCl2·6H2O，0.25~0.35mol/L Na3C6H5O7，0.85~0.9mol/L HCOONa，0.9~1.1mol/L CH4ON2，0.8~0.9mol/LNH4Cl，0.14~0.16mol/L NaB，0.65~0.8 mol/L H3BO30.1-0.2 g/L sodium dodecyl sulfate and 0.75-1.5 g/L saccharin.
4. The method for producing a crack-free Ni — Cr alloy plating layer according to claim 3, wherein: the basic formula of the electroplating solution is a chloride system.
5. The method for producing a crack-free Ni — Cr alloy plating layer according to claim 4, wherein: in the electroplating solution, the mass percentage concentration of NaCl is 3.0-4.0%.
6. The method of claim 2, wherein the Ni-Cr alloy plating layer is formed by: the metal workpiece is pretreated before electroplating, and the specific process comprises the following steps: mechanical polishing → flow water washing → chemical degreasing → flow water washing → deionized water washing → acid washing → flow water washing → deionized water washing.
7. The method of claim 6, wherein the Ni-Cr alloy plating layer is formed by: and chemically removing oil from the metal workpiece by using alkaline wash, wherein the alkaline wash comprises the following components in concentration: 15g/L NaOH, 30g/LNa2CO3，10 g/L Na3PO4·12H2O。
8. The method of claim 6, wherein the Ni-Cr alloy plating layer is formed by: adopting a pickling solution to pickle the metal workpiece, wherein the formula of the pickling solution comprises the following components in percentage by volume: HF: HNO3:H2SO4:H2O =1:1:1:7, and the pickling time is 15 min.
9. The method for producing a crack-free Ni — Cr alloy plating layer according to any one of claims 2 to 8, wherein: placing the metal workpiece with the electroplated Ni-Cr alloy coating on the surface below 1000 ℃, and thermally growing continuous protective Cr on the surface of the Ni-Cr alloy coating2O3And (5) oxidizing the film.
10. The application of the crack-free Ni-Cr alloy coating is characterized in that: the Ni-Cr alloy coating can be used as a protective coating of a metal material with poor corrosion resistance or no high-temperature oxidation resistance, and can be used for protecting metal materials of thermal power generation, petrifaction, energy transmission pipelines and offshore oil exploitation platforms.
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Cited By (1)
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| CN116970896A (en) * | 2023-09-22 | 2023-10-31 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving pre-oxidation effect of Ni-Cr electrothermal alloy product |
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