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Method of preparing transition metal and alloy thereof through low temperature molten salt electro-deposition

A technology of transition group metals and low-temperature molten salts, which is applied in the field of preparation of transition group metals and their alloys by electrodeposition of low-temperature molten salts, and the preparation of transition group metals and their alloys, which can solve the problems of poor electroplating layer quality, low current efficiency, and hydrogen evolution reaction and other problems, to achieve the effect of light equipment corrosion, low energy consumption, and low electrolysis temperature

Inactive Publication Date: 2015-11-11
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the above-mentioned problems in the prior art, aiming at the problems and deficiencies in the electrodeposition of transition metals in the existing aqueous solution, such as the electroplating process accompanied by hydrogen evolution reaction, low current efficiency and hydrogen embrittlement during the electrodeposition process. In order to solve the problems of poor layer quality and other problems, a method for preparing transition metals and their alloys by low-temperature molten salt electrodeposition is proposed.

Method used

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  • Method of preparing transition metal and alloy thereof through low temperature molten salt electro-deposition
  • Method of preparing transition metal and alloy thereof through low temperature molten salt electro-deposition
  • Method of preparing transition metal and alloy thereof through low temperature molten salt electro-deposition

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Embodiment 1

[0038] The method for preparing metal cobalt by low-temperature molten salt electrodeposition is characterized by comprising the following steps.

[0039] 1) Fully mix the anhydrous urea, acetamide and anhydrous LiBr that have been vacuum-dried, and heat and stir to form a colorless uniform liquid molten salt. The mass ratio of urea to acetamide and LiBr is: 35.2:50:14.8.

[0040] 2) the transition metal chloride CoCl 2 Dissolve in the low-temperature liquid molten salt prepared in the above steps, and stir and mix uniformly to form a low-temperature molten salt electrolyte; wherein the molten salt and CoCl 2 The mass ratio is: 100:1.

[0041] 3) With the treated copper sheet as the cathode and graphite as the anode, the electrolysis temperature is 70°C, the constant potential method is used, and the control potential is -0.7V (vs.Ag) and the low-temperature melt prepared in step 2) Electrodeposition in salt electrolyte for 1h.

[0042] 4) after the electrolysis, take out the...

Embodiment 2

[0044] The method for preparing metallic nickel by low-temperature molten salt electrodeposition is characterized by comprising the following steps.

[0045] 1) Fully mix the anhydrous urea, acetamide and anhydrous LiBr that have been vacuum-dried, and heat and stir to form a colorless uniform liquid molten salt. The mass ratio of urea to acetamide and LiBr is: 35.2:50:14.8.

[0046] 2) the transition metal chloride NiCl 2 Dissolve in the low-temperature liquid molten salt prepared in the above steps, and stir and mix uniformly to form a low-temperature molten salt electrolyte; wherein the molten salt and NiCl 2 The mass ratio is: 100:2.

[0047] 3) With the treated copper sheet as the cathode and graphite as the anode, the electrolysis temperature is 80°C, the constant potential method is used, and the control potential is -0.8V (vs. Electrodeposition in salt electrolyte for 2h.

[0048] 4) Take out the copper sheet after the electrolysis and clean it with ethanol first, t...

Embodiment 3

[0050] The method for preparing metallic iron by low-temperature molten salt electrodeposition is characterized by comprising the following steps.

[0051] 1) Fully mix the anhydrous urea, acetamide and anhydrous LiCl that have been vacuum-dried, and heat and stir to form a colorless uniform liquid molten salt. The mass ratio of urea to acetamide and LiCl is: 40.45:50:9.55.

[0052] 2) the transition metal chloride FeCl 2 Dissolve in the low-temperature liquid molten salt prepared in the above steps, and stir and mix uniformly to form a low-temperature molten salt electrolyte; wherein the molten salt and FeCl 2 The mass ratio is: 100:3.

[0053] 3) With the treated copper sheet as the cathode and graphite as the anode, the electrolysis temperature is 90°C, the constant potential method is used, the control potential is -0.9V (vs.Ag) and the low-temperature melt prepared in step 2) Electrodeposition in salt electrolyte for 3h.

[0054] 4) After the electrolysis, take out the...

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Abstract

A method of preparing transition metal and alloy thereof through low temperature molten salt electro-deposition is characterized by comprising the steps of (1) mixing anhydrous urea, acetamide and anhydrous LiX uniformly and heating and stirring the mixture to form a colorless uniform liquid molten salt; (2) dissolving a transition metal chloride TMCl2 in low temperature molten salt and stirring and mixing the mixture uniformly to form a low temperature molten salt electrolyte; (3) with a copper sheet or stainless steel as a cathode and graphite as an anode, performing electro-deposition in the low temperature molten salt electrolyte at the electrolyzing temperature of 70-90 DEG C in a manner of constant potential and constant current to control the potential or cathode current density; and (4) when the electrolysis is finished, taking the copper sheet or stainless steel out and cleaning and drying it to obtain the transition metal and alloy thereof deposited on the surface of the cathode. The molten salt is low in price and is low in eutectic temperature so that the method is low in cost, is low in electrolysis temperature, is energy-saving, is less in pollution and is slight in corrosion on equipment.

Description

technical field [0001] The invention relates to a method for preparing transition group metals and alloys thereof, in particular to a method for preparing transition group metals and alloys thereof by low-temperature molten salt electrodeposition, and belongs to the technical field of inorganic chemistry. Background technique [0002] Transition metals and their alloys are widely used in the preparation of functional materials such as corrosion resistance, magnetism, electrocatalysis, and magnetic recording due to their special properties. At present, the research on electrodeposition of transition metals and their alloys is mainly concentrated in aqueous solution. Aqueous solution electrolysis has the advantages of low price, low electrolysis temperature and low energy consumption. However, due to the narrow electrochemical window of water, hydrogen evolution reaction usually occurs during the electrodeposition process, resulting in reduced current efficiency and poor coati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25C3/34C25C3/32C25C3/36
Inventor 王兆文李敏高炳亮石忠宁胡宪伟李亮星
Owner NORTHEASTERN UNIV LIAONING
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