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Study on diffusion kinetics of chromium and nickel electrochemical co-deposition in a NaCl–KCl–NaF–Cr2O3–NiO molten salt

  • Shixian Zhang , Kai Hu , Xiaoping Zhao , Jinglong Liang and Yungang Li EMAIL logo
Published/Copyright: May 19, 2023
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High Temperature Materials and Processes
From the journal High Temperature Materials and Processes Volume 42 Issue 1

Abstract

The process of preparing surface composite by molten salt co-deposition is the result of the mass transfer of active particles in molten salt, electrochemical reduction, and solid diffusion. In this study, we prepared Cr–Ni alloy/low-carbon steel surface composites in NaCl, KCl, NaF, Cr2O3, and NiO melt salt system successfully, and analyzed the entire diffusion dynamics process, aiming to find out the limiting links and provide ideas for further improving the preparation efficiency. The results show that chromium and nickel ions are simultaneously reduced on the cathode surface through two and one steps, respectively. And an alloy layer with Fe content of 64.52 wt%, Ni content of 28.96 wt%, and Cr content of 6.52 wt% is formed on the surface of low-carbon steel substrate. The average diffusion coefficients of chromium and nickel atoms in the surface composites are 1.16 × 10−14 and 1.44 × 10−14 m2·s−1. The mass transfer process in molten salt is the limiting link in the whole preparation process.

Keywords: electrochemical co-deposition; diffusion kinetics; Cr–Ni alloy/low-carbon steel surface composite; diffusion mechanism; diffusion coefficients; melt salt

1 Introduction

Electrochemical deposition in molten salt is one of the most important methods to prepare surface composites. This method can not only carry out the reduction of oxides and the purification of rare metals but can also prepare metallurgical bonded surface gradient composites in one step, which are widely used in metallurgical production, energy, environmental protection, material preparation and other industrial technology fields. Sun et al. [1] deposited high-purity tungsten with good adhesion on the graphite cathode. Dubrovskiy et al. [2] electrochemically synthesized Mo2C coatings with different structures on molybdenum substrate. Yasuda et al. [3] studied the effect of temperature and current density on the electrodeposition of Si films in KF–KCl–K2SiF6 molten salt system, and experimentally obtained the diffusion coefficient of Si4+ ions. Zhang [4] studied the co-deposition behavior of Ce(iii) and Mg(ii) on tungsten electrodes in CaCl2–NaCl melt, and calculated the diffusion coefficient of ions. Huang et al. [5] studied the electrochemical reduction process of Y(iii) and the cathodic behavior of Y2O3 in YF3–LiF molten salt system, and calculated the diffusion coefficient of Y(iii). Wang et al. [6] prepared silicide coatings containing MoSi2 and Si–MoSi2 by electrodeposition on molybdenum substrate, and discussed the relevant deposition mechanism. Huang et al. [7,8,9,10], respectively, deposited Ir coatings on graphite, Re, and Mo cathodes. Kuznetsov [11] electrodeposited the niobium coating on M1 copper, MAGT-0.05 copper alloy, and MAGT-0.2 copper alloy, and measured the mutual diffusion coefficient of niobium. The dynamic process of preparing surface composites by molten salt electrochemical method includes three steps: mass transfer of particles in molten salt, reduction of ions, and solid diffusion of atoms in the matrix. The studies on the mass transfer process and electrochemical reduction process of particles in molten salt are more compared to the studies on solid diffusion process of matrix. The solid-state diffusion process of atoms in the matrix should also be considered to comprehensively study the whole dynamic process.

The drawbacks of easy oxidation and corrosion of low-carbon steel severely limit its application in certain special requirement areas. At the same time, the lack of chromium and nickel resources and high prices limit the production and application range of stainless steel. Therefore, preparing a Cr–Ni alloy/low-carbon steel surface composite material can combine the excellent properties of the two materials to make up for the shortcomings, and has important theoretical significance and practical value for saving resources and expanding the range of material use. In this study, the Cr–Ni alloy/low-carbon steel surface composites were successfully prepared by electrochemical deposition method in NaCl–KCl–NaF–Cr2O3–NiO molten salt system. It not only improved the corrosion resistance of low-carbon steel substrate, but also greatly reduced the preparation cost of materials. The diffusion coefficients of chromium and nickel atoms in low-carbon steel were calculated through experiments and dynamic calculations, and the overall diffusion dynamic behavior in the preparation process was discussed. The research results can provide ideas for improving the efficiency of molten salt electrodeposition.

2 Experimental method

2.1 Materials and treatment

The raw materials selected for molten salt system include analytically pure NaCl, KCl, NaF, Cr2O3, and NiO. According to XNaCl:XKCl:XNaF = 2:2:1 molar ratio of molten salt components, and 2% molar content of Cr2O3 and NiO, 200 g analytically pure reagents were weighed to ensure sufficient chromium and nickel sources in the process of molten salt electrolytic deposition.

First, grind the used initial reagents into powder, then place the reagents in a vacuum drying oven, dry it at 493 K for 720 min to remove the crystal water in the reagents. Second, put the cooled reagents into a 50 ml high-purity graphite crucible, and cover it for sealing. Finally, put the crucible into a closed well type resistance furnace, and pass 100 ml·min−1 argon for protection. When the temperature reaches 1,073 K, keep the heat for 7 h to saturate the molten salt [12,13].

2.2 Electrochemical detection

The Zahner electrochemical workstation (IM6eX, Germany) and three electrode detection systems were used to measure the parameters of relevant electrochemical reactions in the molten salt system (Figure 1).

Because the common reference electrode cannot work in high temperature molten salt, we chose the platinum electrode with good reversibility, high exchange current density, stable potential, and good reproducibility as the reference electrode. The working electrode, reference electrode, and counter electrode were all made of 99.99% platinum. Keep the distance between the three electrodes at 10 mm during the detection. First, an alumina tube having an inner diameter of 0.6 mm was used as the sleeve to protect the platinum wire with a diameter of 0.5 mm. Two platinum wires of length 1 cm at the upper and lower ends of the corundum tube were used as the reference electrode and working electrode, and the other platinum wire is connected with the platinum sheet as the counter electrode. Second, the platinum sheet was polished slightly with 5,000 mesh sandpaper, washed with 5% dilute hydrochloric acid for 1 min, put into anhydrous ethanol, and shaken with an ultrasonic cleaner for 5 min. Third, the three electrodes were inserted into the molten salt, and connected to the electrochemical workstation to conduct electrochemical measurement in the NaCl–KCl–NaF–Cr2O3–NiO molten salt.

Before the formal measurement, pre-electrolysis was performed for 2 h at a constant voltage of 2 V to remove residual water, oxide anions, and other compounds. And then the chronoamperometry curves of the molten salt were measured in the potential range of −0.33 to −0.98 V.

Figure 1 Schematic diagram of electrochemical detection system.
Figure 1

Schematic diagram of electrochemical detection system.

2.3 Electrodeposition

Two electrode system was used to carry out electrodeposition experiment. The anode material is high-purity graphite plate. The cathode material is Q-195 low-carbon steel plate, and its specific composition is shown in Table 1. Before the experiment, 20 mm × 20 mm × 3 mm low-carbon steel plate was polished with silicon carbide sandpaper (320, 800, 1,000, 1,500, and 2,000 mesh), and then soaked in 5% NaOH hydrothermal solution for 5 min to remove grease. The pickling was soaked in 5% hydrochloric acid solution for 1 min, then rinsed in an ultrasonic cleaner for 5 min with ethanol, and blown dry with a blower to remove surface impurities. The 20 mm × 50 mm × 3 mm high-purity graphite anode was cleaned by ultrasonic cleaner containing 10% hydrochloric acid solution for 5 min, rinsed with deionized water, and blown dry.

Table 1

Composition of low-carbon steel plate

Element C Si Mn P S Fe
Content (wt%) 0.10 0.10 0.3 0.02 0.02 Remaining amount

The processed cathode and anode electrodes were inserted into the molten salt, and the electroplating power (SMD-P, China) was switched on to carry out the molten salt electrodeposition experiment. The specific electrodeposition conditions are shown in Table 2.

Table 2

Parameter of electrodeposition process in molten salt

Electrode spacing (mm) Bidirectional pulse current Current density (mA·cm−2) Temperature (K) Time (min)
20 1,000 ms, i positive:i reverse = 6:1, t positive:t reverse = 3:1 300 1,073 180

2.4 Analysis and detection

The contents of chromium and nickel in the surface composites of low-carbon steel along the diffusion layer were detected by GDA750 glow discharge spectrometer.

3 Results and discussion

3.1 Analysis of diffusion dynamics results

3.1.1 Kinetic analysis of ion diffusion in molten salt

Figure 2 shows the chronoamperometric curve measured by applying different electrode potentials to the molten salt system. The chronoamperometric curves measured at each electrode potential are typical chronoamperometric curves, which conform to the characteristics that ion diffusion in solution is the control link [14]. The reduction process of chromium and nickel ions on the cathode is shown on the chronoamperometric curve. With the gradual increase in potential, there are three steps in the curve. The first step (−0.39 to −0.41 V) represents the process of Ni2+ being reduced to metal Ni, the second step (−0.60 to −0.63 V) represents the process of Cr3+ being reduced to Cr2+, and the third step (−0.95 to −0.98 V) represents the process of Cr2+ being reduced to metal Cr. At the beginning of the experiment, the circuit is in an open circuit state with the potential of 0. When the constant potential is applied, the double electric layer on the electrode surface charges rapidly, generating current on the cathode, and then decreases rapidly. At the same time, chromium and nickel ions begin to reduce on the cathode surface. With the extension of time, the concentration of chromium and nickel ions near the cathode surface decreases continuously, leading to concentration polarization which reduce the current to a steady state slowly [15].

Figure 2 Chronoamperometric curves of cathodes with different potentials in NaCl–KCl–NaF–Cr2O3–NiO molten salt at 1,073 K.
Figure 2

Chronoamperometric curves of cathodes with different potentials in NaCl–KCl–NaF–Cr2O3–NiO molten salt at 1,073 K.

3.1.2 Diffusion dynamics of reduced atoms on the surface of Cr–Ni alloy/low-carbon steel surface composite

Figure 3 shows the metallographic photo, SEM photo, energy spectrum analysis results, and XRD pattern of the Cr–Ni alloy/low-carbon steel deposited in the NaCl–KCl–NaF–Cr2O3–NiO molten salt for 180 min at 1,073 K. It can be seen from the metallographic photos and scanning electron microscope photos that a deposition diffusion layer is formed on the surface of the substrate. The iron content is 70.09 wt%, chromium content is 6.14 wt%, and nickel content is 23.77 wt%. It can be seen from the XRD pattern that the diffraction peak of the product is consistent with the standard spectrum of Ni–Cr–Fe alloy (35–1,375). It illustrates that the Cr–Ni alloy and low-carbon steel are mutually diffused under the action of high temperature during electrodeposition to form the Cr–Ni alloy/low-carbon steel surface composite.

Figure 3 Cross section metallographic photograph, surface SEM image, EDS test, and XRD pattern of Cr–Ni alloy sample co-electrodeposited in molten salts under different conditions (1,073 K, 300 mA·cm−2, 180 min).
Figure 3

Cross section metallographic photograph, surface SEM image, EDS test, and XRD pattern of Cr–Ni alloy sample co-electrodeposited in molten salts under different conditions (1,073 K, 300 mA·cm−2, 180 min).

Figure 4 shows the relationship between the element content and the depth of the sample. It can be seen that the content of chromium and nickel decreases with the increase in the section depth of the sample, and the content of iron increases with the increase in the section depth of the sample. It shows that chromium, nickel, and iron inter diffused on the surface of low-carbon steel, and a gradient layer with a certain thickness is formed. The Cr–Ni alloy/low-carbon steel surface composite was prepared by means of molten salt electrodeposition and solid-state diffusion.

Figure 4 Relationship between element content and section depth of co-deposition sample in molten salt at 1,073 K.
Figure 4

Relationship between element content and section depth of co-deposition sample in molten salt at 1,073 K.

In the actual diffusion process, the diffusion coefficient of elements in the matrix changes with the concentration of diffusing elements.

In order to obtain the atomic diffusion law of Cr–Ni alloy/low-carbon steel surface composite prepared by molten salt co-deposition process, the diffusion coefficients at different volume concentrations are calculated by Fick’s second law, Arrhenius law [16], and Den Broeder formula [17] (formula (1)) under fixed temperature conditions. And the average diffusion coefficient of the atom is obtained by fitting and averaging the obtained diffusion coefficient curve within the measured volume concentration range to reflect the general law of diffusion coefficient of diffusing atoms at a specific temperature.

(1) D C B ∗ = 1 2 t ∂ C B ∂ x x ∗ ( 1 − y C ∗ ) ∫ − ∞ x ∗ ( C B ⁎ − C B 1 ) d x + y C ∗ ∫ x ∗ + ∞ ( C B 2 − C B ⁎ ) d x .

Taking the surface as zero in the percentage content curves of chromium and nickel, nine groups of percentage contents and corresponding depths were obtained, respectively, in the range of nickel 1–21% (step length 2.5%) and chromium 0.5–6.5% (step length 0.75%). The data of different element volume concentrations and matrix depth were fitted by Boltzmann function, and the fitting equations C Cr = f(x) and C Ni = f(x) of chromium and nickel diffusion were obtained, respectively.

According to Den Broeder formula, Matlab software is used to calculate the mathematical expression of the diffusion fitting equation ∫ x ∗ + ∞ ( C B 2 − C C B ∗ ) d x , ∫ − ∞ x ∗ ( C C B ∗ − C B 1 ) d x , and ( ∂ C B / ∂ x ) x ∗ of chromium and nickel atoms on the surface of low-carbon steel at 1,073 K. Finally, the diffusion coefficients of chromium and nickel atoms at different depths and concentrations are obtained. Figure 5 shows the variation in diffusion coefficient of chromium and nickel atoms with depth and percentage content.

Figure 5 Relationship between Cr and Ni diffusion coefficients and section depth and concentration of samples co-deposited in molten salt (1,073 K, 180 min).
Figure 5

Relationship between Cr and Ni diffusion coefficients and section depth and concentration of samples co-deposited in molten salt (1,073 K, 180 min).

The law in Figure 5 was solved by integral method, and the average diffusion coefficient of chromium and nickel in the surface of low-carbon steel at 1,073 K was obtained, as shown in Table 3.

(2) D ¯ = ∫ C 1 C 2 D ( C ) d C C 2 − C 1 .

Table 3

Average diffusion coefficients of Cr and Ni of samples co-deposited in molten salt (1,073 K, 180 min)

Element Fitting curve D = f(C) R Average diffusion coefficient (m2·s−1)
Cr D = exp(−29.94 – 17.55/(C + 3.53)) 0.99553 1.16 × 10−14
Ni D = exp(−36.20 + 0.28 C − 0.01C 2) 0.99352 1.44 × 10−14

3.2 Discussion on diffusion process

The process of co-deposition of Cr–Ni alloy/low-carbon steel surface composites in molten salt is determined by the combined effect of active particles mass transfer, electrochemical reduction, and solid-state diffusion. The specific process is shown in Figure 6. A large number of active particles in molten salt undergo irregular Brownian motion in molten salt. After the unidirectional current is applied to the system, the active particles move directionally under the action of the electric field, and concentrate near the cathode surface to form an electric double layer [18,19,20]. Chromium and nickel ions close to the cathode get electrons to be reduced to atoms, and are adsorbed on the cathode surface to form another concentration gradient with the cathode material. Chromium, nickel atoms and cathode will mutually diffuse in solid-state at high temperature, and finally Cr–Ni alloy/low-carbon steel surface composite will be obtained.

Figure 6 Dynamic diagram of electrodeposition process in molten salt.
Figure 6

Dynamic diagram of electrodeposition process in molten salt.

The typical chronoamperometric curves conform to the characteristics that ion diffusion in solution is the control link. This shows that the mass transfer rate of active particles is the limiting link in the whole preparation process, which affects the preparation rate of materials. Under the action of the directional electric field, the chromium and nickel active particles are concentrated on the cathode surface. The high concentration of active particles is helpful to improve the electrochemical reduction reaction speed. However, due to the high electrochemical reduction speed, the active ion concentration in the electric double layer cannot be rapidly supplemented, which reduces the speed of the whole preparation process.

4 Conclusion

The Cr–Ni alloy/low-carbon steel surface composites were prepared by molten salt co-deposition in NaCl, KCl, NaF, Cr2O3, and NiO melt salt system, and the kinetics of the preparation process was systematically studied. The results show that a certain thickness of alloy gradient layer is prepared on the surface of low-carbon steel under the combined action of the mass transfer of chromium and nickel active particles in molten salt, electrochemical reduction, and high-temperature solid diffusion. The chromium and nickel ions are simultaneously reduced on the cathode surface through two and one steps, respectively. According to the detection data of the deposition layer, the average diffusion coefficients of chromium and nickel atoms in the surface composite are calculated to be 1.16 × 10−14 and 1.44 × 10−14 m2·s−1. Affected by the mass transfer rate, the concentration of ions in the electric double layer near the cathode cannot be rapidly supplemented, thus reducing the speed of the entire preparation process.

  1. Funding information: The study is financially supported by the National Natural Science Foundation of China (Project No. 51974129), and the Hebei Province “three three three talent project” Funding (Project No. A202101030).

  2. Author contributions: Shixian Zhang: conceptualization, writing – review and editing, methodology, and formal analysis; Kai Hu: original draft and methodology; Xiaoping Zhao: original draft, software, and methodology; Jinglong Liang: methodology, formal analysis, and validation; Yungang Li: conceptualization, validation, and funding acquisition. All authors have read and agreed to the published version of the manuscript.

  3. Conflict of interest: Authors state no conflict of interest.

  4. Data availability statement: Data sharing is not applicable for this article.

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Received: 2022-11-16
Revised: 2023-04-27
Accepted: 2023-05-02
Published Online: 2023-05-19

© 2023 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/htmp-2022-0276
Keywords for this article
electrochemical co-deposition; diffusion kinetics; Cr–Ni alloy/low-carbon steel surface composite; diffusion mechanism; diffusion coefficients; melt salt
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  10. Simultaneous extraction of uranium and niobium from a low-grade natural betafite ore
  11. Transfer and transformation mechanism of chromium in stainless steel slag in pedosphere
  12. Effect of tool traverse speed on joint line remnant and mechanical properties of friction stir welded 2195-T8 Al–Li alloy joints
  13. Technology and analysis of 08Cr9W3Co3VNbCuBN steel large diameter thick wall pipe welding process
  14. Influence of shielding gas on machining and wear aspects of AISI 310–AISI 2205 dissimilar stainless steel joints
  15. Effect of post-weld heat treatment on 6156 aluminum alloy joint formed by electron beam welding
  16. Ash melting behavior and mechanism of high-calcium bituminous coal in the process of blast furnace pulverized coal injection
  17. Effect of high temperature tempering on the phase composition and structure of steelmaking slag
  18. Numerical simulation of shrinkage porosity defect in billet continuous casting
  19. Influence of submerged entry nozzle on funnel mold surface velocity
  20. Effect of cold-rolling deformation and rare earth yttrium on microstructure and texture of oriented silicon steel
  21. Investigation of microstructure, machinability, and mechanical properties of new-generation hybrid lead-free brass alloys
  22. Soft sensor method of multimode BOF steelmaking endpoint carbon content and temperature based on vMF-WSAE dynamic deep learning
  23. Mechanical properties and nugget evolution in resistance spot welding of Zn–Al–Mg galvanized DC51D steel
  24. Research on the behaviour and mechanism of void welding based on multiple scales
  25. Preparation of CaO–SiO2–Al2O3 inorganic fibers from melting-separated red mud
  26. Study on diffusion kinetics of chromium and nickel electrochemical co-deposition in a NaCl–KCl–NaF–Cr2O3–NiO molten salt
  27. Enhancing the efficiency of polytetrafluoroethylene-modified silica hydrosols coated solar panels by using artificial neural network and response surface methodology
  28. High-temperature corrosion behaviours of nickel–iron-based alloys with different molybdenum and tungsten contents in a coal ash/flue gas environment
  29. Characteristics and purification of Himalayan salt by high temperature melting
  30. Temperature uniformity optimization with power-frequency coordinated variation in multi-source microwave based on sequential quadratic programming
  31. A novel method for CO2 injection direct smelting vanadium steel: Dephosphorization and vanadium retention
  32. A study of the void surface healing mechanism in 316LN steel
  33. Effect of chemical composition and heat treatment on intergranular corrosion and strength of AlMgSiCu alloys
  34. Soft sensor method for endpoint carbon content and temperature of BOF based on multi-cluster dynamic adaptive selection ensemble learning
  35. Evaluating thermal properties and activation energy of phthalonitrile using sulfur-containing curing agents
  36. Investigation of the liquidus temperature calculation method for medium manganese steel
  37. High-temperature corrosion model of Incoloy 800H alloy connected with Ni-201 in MgCl2–KCl heat transfer fluid
  38. Investigation of the microstructure and mechanical properties of Mg–Al–Zn alloy joints formed by different laser welding processes
  39. Effect of refining slag compositions on its melting property and desulphurization
  40. Effect of P and Ti on the agglomeration behavior of Al2O3 inclusions in Fe–P–Ti alloys
  41. Cation-doping effects on the conductivities of the mayenite Ca12Al14O33
  42. Modification of Al2O3 inclusions in SWRH82B steel by La/Y rare-earth element treatment
  43. Possibility of metallic cobalt formation in the oxide scale during high-temperature oxidation of Co-27Cr-6Mo alloy in air
  44. Multi-source microwave heating temperature uniformity study based on adaptive dynamic programming
  45. Round-robin measurement of surface tension of high-temperature liquid platinum free of oxygen adsorption by oscillating droplet method using levitation techniques
  46. High-temperature production of AlN in Mg alloys with ammonia gas
  47. Review Article
  48. Advances in ultrasonic welding of lightweight alloys: A review
  49. Topical Issue on High-temperature Phase Change Materials for Energy Storage
  50. Compositional and thermophysical study of Al–Si- and Zn–Al–Mg-based eutectic alloys for latent heat storage
  51. Corrosion behavior of a Co−Cr−Mo−Si alloy in pure Al and Al−Si melt
  52. Al–Si–Fe alloy-based phase change material for high-temperature thermal energy storage
  53. Density and surface tension measurements of molten Al–Si based alloys
  54. Graphite crucible interaction with Fe–Si–B phase change material in pilot-scale experiments
  55. Topical Issue on Nuclear Energy Application Materials
  56. Dry synthesis of brannerite (UTi2O6) by mechanochemical treatment
  57. Special Issue on Polymer and Composite Materials (PCM) and Graphene and Novel Nanomaterials - Part I
  58. Heat management of LED-based Cu2O deposits on the optimal structure of heat sink
  59. Special Issue on Recent Developments in 3D Printed Carbon Materials - Part I
  60. Porous metal foam flow field and heat evaluation in PEMFC: A review
  61. Special Issue on Advancements in Solar Energy Technologies and Systems
  62. Research on electric energy measurement system based on intelligent sensor data in artificial intelligence environment
  63. Study of photovoltaic integrated prefabricated components for assembled buildings based on sensing technology supported by solar energy
  64. Topical Issue on Focus of Hot Deformation of Metaland High Entropy Alloys - Part I
  65. Performance optimization and investigation of metal-cored filler wires for high-strength steel during gas metal arc welding
  66. Three-dimensional transient heat transfer analysis of micro-plasma arc welding process using volumetric heat source models
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