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CN112176372B - Method for preparing cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials - Google Patents

Method for preparing cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials Download PDF

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CN112176372B
CN112176372B CN202011031937.7A CN202011031937A CN112176372B CN 112176372 B CN112176372 B CN 112176372B CN 202011031937 A CN202011031937 A CN 202011031937A CN 112176372 B CN112176372 B CN 112176372B
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cobalt
alloy coating
tantalum
electrodeposition
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CN112176372A (en
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刘爱民
郭梦霞
石忠宁
刘风国
王兆文
陶文举
杨酉坚
胡宪伟
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Northeastern University China
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    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
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Abstract

A method for preparing a cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials belongs to the field of low-temperature electrochemical extraction. The method comprises the following steps: (1) adding CoCl under argon atmosphere2Slowly adding into 1, 3-dimethyl-2-imidazolidinone, stirring, and slowly adding TaCl5Stirring to form a uniform solution; (2) building an electrolytic cell system, taking the uniform solution as an electrolyte solution, and performing electrodeposition by adopting a three-electrode system; (3) and taking out the cathode after the electrodeposition is finished, cleaning, and drying to obtain the cobalt-tantalum alloy coating on the surface of the cathode. The method adopts 1, 3-dimethyl-2-imidazolidinone-CoCl2‑TaCl5The cobalt-tantalum alloy coating with uniform particles, compact and smooth surface and excellent adhesion can be obtained by electrodeposition as an electrolyte. The preparation method and the preparation process are all general technologies, and have the advantages of simple equipment, low cost, safety, environmental protection, easy realization and strong practicability.

Description

Method for preparing cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials
Technical Field
The invention belongs to the field of low-temperature electrochemical extraction, and particularly relates to a method for extracting CoCl2And TaCl5A method for preparing a cobalt-tantalum alloy coating at low temperature.
Background
Cobalt is a bright gray steel metal, is relatively hard and brittle, has ferromagnetism, is an important raw material for producing high-temperature alloys, hard alloys, anticorrosion alloys and magnetic alloys, and has attracted more and more attention in recent years. Tantalum is a rare, hard, bluish-grey, shiny, corrosion-resistant transition metal, and is widely used in the fields of chemical engineering, cutting tools, aerospace, electronics, and the like, due to its excellent properties of high density, high melting point, good high-temperature strength, low plasticity, high ductility, good processability, and the like. The high-temperature alloy prepared by adding tantalum into cobalt has better hot corrosion resistance, oxidation resistance, thermal fatigue resistance and weldability, relatively low manufacturing cost and improved lasting strength and stability, and can be used as parts of blades, impellers, pipes, jet engines, rocket engines and missiles of gas turbines, various high-load heat-resistant parts in chemical equipment and important metal materials in atomic energy industry.
At present, the preparation method of the high-temperature cobalt-based alloy mainly comprises a vacuum melting ingot casting method and a powder metallurgy method. The vacuum melting ingot casting method has the problems of uneven distribution of product crystal grain size, complex process, long period, high operating environment temperature, high energy consumption, high cost and the like. The powder metallurgy preparation process is easy to bring impurities, reduces the purity of products, and particularly has difficult control of residual oxygen content and micropores.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing a CoCl2And TaCl5A method for preparing a cobalt-tantalum alloy coating with high purity and uniform grain size distribution by low-temperature electrodeposition of raw materials.
The invention discloses a method for preparing a cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials, which comprises the following steps:
step 1, adding CoCl in an argon atmosphere at 25-100 DEG C2Slowly adding into 1, 3-dimethyl-2-imidazolidinone, stirring, and slowly adding TaCl5Continuously stirring to form a uniform solution;
step 2, building an electrolytic cell system, taking the uniform solution prepared in the step 1 as an electrolyte solution, and performing electrodeposition by adopting a three-electrode system; wherein, the working electrode, namely the cathode, is a tungsten sheet, the counter electrode is a platinum sheet, and the reference electrode is a silver wire; controlling the electrodeposition temperature to be 25-100 ℃, controlling the applied potential to be-1.5-2.4V, and controlling the electrodeposition time to be 0.5-4 h;
and 3, taking out the cathode after the electrodeposition is finished, cleaning, and drying to obtain the cobalt-tantalum alloy coating on the surface of the cathode.
The one is CoCl2And TaCl5The method for preparing the cobalt-tantalum alloy coating at low temperature by using the raw materials comprises the following steps:
in the step 1, the concentration of water and oxygen is ensured to be lower than 1ppm in the preparation process of the uniform solution; control of CoCl in 1, 3-dimethyl-2-imidazolidinone2Has a molar concentration of 0.02-0.2mol/L, TaCl5The molar concentration of (A) is 0.01-0.08 mol/L.
In the step 2, before electrodeposition, the surface of the electrode is sequentially polished by using 800# to 5000# mesh abrasive paper, then the electrode is sequentially ultrasonically cleaned by using absolute ethyl alcohol and deionized water, and finally the electrode is blow-dried by cold air; the interpole distance between the working electrode and the counter electrode was 15 mm.
In the step 3, after the electrodeposition is finished, the cathode electrode is sequentially cleaned by absolute ethyl alcohol and deionized water, and dried by cold air and then placed in a glove box for storage.
Compared with the prior art, the invention has the following advantages:
1. the 1, 3-dimethyl-2-imidazolidinone adopted in the method has low melting point, can reduce energy consumption, has wide electrochemical window, can avoid the generation of hydrogen evolution side reaction, and has low viscosity to CoCl2And TaCl5Has good solubility and coordination capacity and is suitable for electrodepositing a cobalt-tantalum alloy coatingGood solvent.
2. Using 1, 3-dimethyl-2-imidazolidinone-CoCl2-TaCl5The cobalt-tantalum alloy coating with uniform particles, compact and smooth surface and excellent adhesion can be obtained by electrodeposition as an electrolyte. The method has the advantages that no additive is added, the efficiency is high, the controllability is high, and the purpose of controlling the nucleation mechanism and the crystal grain morphology is achieved by controlling the process parameters.
3. The preparation method and the preparation process are all general technologies, and have the advantages of simple equipment, low cost, safety, environmental protection, easy realization and strong practicability.
Drawings
FIG. 1 is a scanning electron microscope image of a cobalt tantalum alloy coating obtained by electrodeposition in example 3 of the present invention.
FIG. 2 is an X-ray energy spectrum of a cobalt-tantalum alloy coating obtained by electrodeposition in example 3 of the present invention.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
Example 1
A method for preparing a cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials comprises the following specific operation steps:
step 1, slowly adding CoCl into 1, 3-dimethyl-2-imidazolidinone in a glove box at room temperature under an argon atmosphere2Stirring to uniform, and slowly adding TaCl5Continuously stirring until a uniform solution is formed; wherein CoCl in 1, 3-dimethyl-2-imidazolidinone is controlled2、TaCl5The molar concentrations of the components are 0.02mol/L and 0.01mol/L respectively;
2, sequentially polishing the surface of the electrode by using 800# to 5000# abrasive paper, then sequentially ultrasonically cleaning by using absolute ethyl alcohol and deionized water, and drying by using a blower with cold air; building an electrolytic cell system, and performing electrodeposition at room temperature by taking the obtained uniform solution as an electrolyte solution; wherein the distance between the working electrode and the counter electrode is 15mm, and the working electrode, namely the cathode is a tungsten sheet (99.99%, the area is 1 cm)2) The counter electrode is a platinum sheet (99.99%, area of 1 cm)2) The reference electrode is silver wire (99.99%, radius ═ 1mm), the applied potential is-1.5V (vs. ag), and the electrodeposition time is 4 h;
and 3, taking out the working electrode after electrodeposition, washing the electrolyte adhered to the surface by using absolute ethyl alcohol and deionized water in sequence, and drying the surface by using cold air to obtain the cobalt-tantalum alloy coating.
And observing by using an SEM (scanning electron microscope) to obtain a compact, uniform and smooth cobalt-tantalum alloy coating. EDS (X-ray spectroscopy) gave 52.10% by weight and 8.44% by weight cobalt and tantalum, respectively.
Example 2
A method for preparing a cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials comprises the following specific operation steps:
step 1, adding CoCl slowly into 1, 3-dimethyl-2-imidazolidinone in a glove box at 50 ℃ in an argon atmosphere2Stirring to uniform, and slowly adding TaCl5Continuously stirring at 50 ℃ until a uniform solution is formed; wherein CoCl in 1, 3-dimethyl-2-imidazolidinone is controlled2、TaCl5The molar concentrations of the components are 0.1mol/L and 0.04mol/L respectively;
2, sequentially polishing the surface of the electrode by using 800# to 5000# abrasive paper, then sequentially ultrasonically cleaning by using absolute ethyl alcohol and deionized water, and drying by using a blower with cold air; building an electrolytic cell system, and performing electrodeposition at 50 ℃ by taking the obtained uniform solution as an electrolyte solution; wherein the distance between the working electrode and the counter electrode is 15mm, and the working electrode, namely the cathode is a tungsten sheet (99.99%, the area is 1 cm)2) The counter electrode is a platinum sheet (99.99%, area of 1 cm)2) The reference electrode is silver wire (99.99%, radius ═ 1mm), the applied potential is-1.8V (vs. ag), and the electrodeposition time is 3 h;
and 3, taking out the working electrode after electrodeposition, washing the electrolyte adhered to the surface by using absolute ethyl alcohol and deionized water in sequence, and drying the surface by using cold air to obtain the cobalt-tantalum alloy coating.
A compact, uniform and smooth cobalt-tantalum alloy coating is obtained through SEM observation, and the weight percentages of cobalt and tantalum obtained through EDS analysis are 41.90% and 17.81% respectively.
Example 3
A method for preparing a cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials comprises the following specific operation steps:
step 1, slowly adding CoCl into 1, 3-dimethyl-2-imidazolidinone in a glove box at 75 ℃ in an argon atmosphere2Stirring to uniform, and slowly adding TaCl5Continuously stirring at 75 ℃ until a uniform solution is formed; wherein CoCl in 1, 3-dimethyl-2-imidazolidinone is controlled2、TaCl5The molar concentrations of the components are 0.2mol/L and 0.08mol/L respectively;
2, sequentially polishing the surface of the electrode by using 800# to 5000# abrasive paper, then sequentially ultrasonically cleaning by using absolute ethyl alcohol and deionized water, and drying by using a blower with cold air; building an electrolytic cell system, and performing electrodeposition at 75 ℃ by taking the obtained uniform solution as an electrolyte solution; wherein the distance between the working electrode and the counter electrode is 15mm, and the working electrode, namely the cathode is a tungsten sheet (99.99%, the area is 1 cm)2) The counter electrode is a platinum sheet (99.99%, area of 1 cm)2) The reference electrode is silver wire (99.99%, radius ═ 1mm), the applied potential is-2.1V (vs. ag), and the electrodeposition time is 2 h;
and 3, taking out the working electrode after electrodeposition, washing the electrolyte adhered to the surface by using absolute ethyl alcohol and deionized water in sequence, and drying the surface by using cold air to obtain the cobalt-tantalum alloy coating.
Scanning electron micrographs and X-ray energy spectrograms of the cobalt-tantalum alloy coating obtained in the example are shown in FIGS. 1 and 2, respectively. A compact, uniform and smooth cobalt-tantalum alloy coating is obtained through SEM observation, and weight percentages of cobalt and tantalum obtained through EDS analysis are 47.31% and 18.61% respectively.
Example 4
A method for preparing a cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials comprises the following specific operation steps:
step 1, slowly adding CoCl into 1, 3-dimethyl-2-imidazolidinone in a glove box at 100 ℃ in an argon atmosphere2Stirring to uniform, and slowly adding TaCl5Continuously stirring at 100 ℃ until a uniform solution is formed; wherein control is performedCoCl in 1, 3-dimethyl-2-imidazolidinone2、TaCl5The molar concentrations of the components are 0.2mol/L and 0.08mol/L respectively;
2, sequentially polishing the surface of the electrode by using 800# to 5000# abrasive paper, then sequentially ultrasonically cleaning by using absolute ethyl alcohol and deionized water, and drying by using a blower with cold air; building an electrolytic cell system, and performing electrodeposition at 100 ℃ by taking the obtained uniform solution as an electrolyte solution; wherein the distance between the working electrode and the counter electrode is 15mm, and the working electrode, namely the cathode is a tungsten sheet (99.99%, the area is 1 cm)2) The counter electrode is a platinum sheet (99.99%, area of 1 cm)2) The reference electrode is silver wire (99.99%, radius ═ 1mm), the applied potential is-2.4V (vs. ag), and the electrodeposition time is 1 h;
and 3, taking out the working electrode after electrodeposition, washing the electrolyte adhered to the surface by using absolute ethyl alcohol and deionized water in sequence, and drying the surface by using cold air to obtain the cobalt-tantalum alloy coating.
A compact, uniform and smooth cobalt-tantalum alloy coating is obtained through SEM observation, and the weight percentages of cobalt and tantalum obtained through EDS analysis are 43.62% and 18.01% respectively.

Claims (2)

1. A method for preparing a cobalt-tantalum alloy coating at low temperature by taking cobalt dichloride and tantalum pentachloride as raw materials is characterized by comprising the following steps:
step 1, adding CoCl in an argon atmosphere at 25-100 DEG C2Slowly adding into 1, 3-dimethyl-2-imidazolidinone, stirring, and slowly adding TaCl5Continuously stirring to form a uniform solution;
step 2, building an electrolytic cell system, taking the uniform solution prepared in the step 1 as an electrolyte solution, and performing electrodeposition by adopting a three-electrode system; wherein, the working electrode, namely the cathode, is a tungsten sheet, the counter electrode is a platinum sheet, and the reference electrode is a silver wire; controlling the electrodeposition temperature to be 25-100 ℃, controlling the applied potential to be-1.5 to-2.4V, and controlling the electrodeposition time to be 1-4 h;
and 3, taking out the cathode after the electrodeposition is finished, cleaning, and drying to obtain the cobalt-tantalum alloy coating on the surface of the cathode.
2. The method for preparing the cobalt-tantalum alloy coating according to claim 1, wherein in the step 1, the water and oxygen concentration is ensured to be lower than 1ppm in the preparation process of the uniform solution; control of CoCl in 1, 3-dimethyl-2-imidazolidinone2Has a molar concentration of 0.02-0.2mol/L, TaCl5The molar concentration of (A) is 0.01-0.08 mol/L.
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