A kind of molten salt electrodeposition method of niobium coating

An electrodeposition and molten salt technology, applied in electrolytic components, electrolytic processes, cells, etc., can solve the problems of low stability of complexes, weak reverse polarization, low working temperature, etc., and achieve convenient operation, convenient concentration, fast effect

Active Publication Date: 2022-07-19
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the low-toxicity, environment-friendly NaCl-KCl-CsCl system, the anti-polarization effect of cesium ions is weaker than that of sodium-potassium ions, so the complex containing cesium ions in the second coordination sphere will be more stable in the melt, thus solving the problem of The problem of low complex stability of the perchloride system can be used to prepare continuous and dense coatings. At the same time, the system has a low melting point and low working temperature, which can reduce molten salt volatilization and work energy consumption

Method used

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  • A kind of molten salt electrodeposition method of niobium coating
  • A kind of molten salt electrodeposition method of niobium coating
  • A kind of molten salt electrodeposition method of niobium coating

Examples

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Comparison scheme
Effect test

Embodiment 1

[0054] A molten salt electrodeposition method for niobium coating, comprising the following steps:

[0055] 1. Preparation of molten salt: Weigh NaCl, KCl and CsCl respectively according to the ratio of raw material mass ratio of 1:1.28:3.41, put NaCl, KCl and CsCl in a 200 ℃ oven for drying treatment for 8h to remove crystal water, and then NaCl, KCl and CsCl , KCl and CsCl were ground and mixed in a quartz cup, the device was purged with argon gas three times, and heated to 750°C under an argon gas protective atmosphere to melt. Chlorine was introduced into the molten salt for 10 minutes, then argon was bubbled for 15 minutes, and finally cooled under argon protection. will K 2 NbF 7 After drying for 8 hours in a vacuum drying oven at 120°C and a vacuum degree of 100Pa, it was added to the supporting electrolyte to make the K containing 2 NbF 7 The niobium ion concentration in the molten salt was 2.4 wt.%.

[0056] 2. Pre-treatment of plating parts and crucible plating....

Embodiment 2

[0061] The steps are basically the same as those in Example 1, except that the temperature in Step 3 is adjusted to 800°C.

[0062] Figure 5 It is the SEM picture of the coating surface obtained in Example 2. It can be seen that the coating surface is uniform and undulating, and the crystal grains are in the shape of shells. Image 6 From the SEM picture of the coating section obtained in this example, it can be seen that the coating section has no obvious holes, good compactness, coarse grains, and the thickness of the niobium layer is about 26 μm.

Embodiment 3

[0064] The steps are basically the same as those in Example 1, except that the steady-state current in Step 3 is adjusted to pulse current, and the average current density is 50mA / cm 2 , the duty cycle is 50%, and the frequency is 0.5Hz.

[0065] Figure 7 For the SEM picture of the coating surface obtained in Example 3, it can be seen that the coating surface is uniform and the crystal grains are irregular polygonal. Figure 8 From the SEM picture of the coating section obtained in this example, it can be seen that the coating section has no obvious holes, good compactness, fine columnar crystals, and the thickness of the niobium layer is about 50 μm.

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Abstract

The invention provides a molten salt electrodeposition method of niobium coating, which adopts a NaCl-KCl-CsCl system as a supporting electrolyte, and K 2 NbF 7 It is an active salt, and the supporting electrolyte and active salt are pretreated. Under the protective atmosphere of argon, the pretreated supporting electrolyte is heated to 750 ° C and fully melted, and chlorine gas is introduced for chlorination treatment. The supporting electrolyte and the active salt are mixed evenly in the crucible to obtain the molten salt; the plated parts are pretreated; then the pressure of the electroplating device is lower than 100Pa by vacuuming, and the inert gas is introduced, and the pretreated plated parts are placed in the electroplating device. Put it into the prepared molten salt, control the electroplating temperature between 650℃-850℃, select the corresponding current form and electroplating time according to the thickness of the required coating for electroplating, and obtain a plated part with a niobium coating on the surface. The method is environmentally friendly, efficient and low-cost, and the prepared niobium coating has good uniformity.

Description

technical field [0001] The invention relates to the technical field of molten salt electrochemistry and surface coating, in particular to a molten salt electrodeposition method of niobium coating. Background technique [0002] Niobium (Nb) is a refractory metal with a body-centered cubic structure and has good physical and chemical properties, with a high melting point (2468°C) and a relatively low density (8.57g / cm2). 3 ), high high temperature strength, high thermal conductivity, small thermal neutron capture cross section, high superconducting critical temperature (9.2K), and good corrosion resistance, weldability, ductility and excellent biocompatibility [ Qu Naiqin. Tantalum and Niobium and their alloys and their applications [J]. Rare Metals and Cemented Carbide, 1998(02): 48-54], therefore, niobium and its alloys are often used in the manufacture of superconductors, chemical reaction tanks, biological implants It is a key component that serves in special working cond...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D3/66C25D21/14
CPCC25D3/66C25D21/14
Inventor 朱利安白书欣王震叶益聪胡双鹏王淑祥万红李顺唐宇刘希月
Owner NAT UNIV OF DEFENSE TECH
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