CN112779440A - Nickel-molybdenum alloy electrode material and preparation method thereof - Google Patents
Nickel-molybdenum alloy electrode material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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Abstract
The invention discloses a nickel-molybdenum alloy electrode material, which comprises 30-80% of Ni, 10-60% of Mo and 0.1-10% of Fe, Cr, W, Co, Mn and V. The preparation method of the electrode material comprises the following steps: washing and drying the raw materials; putting the dried Ni and Mo into a vacuum induction smelting furnace, and smelting under 10 kW-30 kW; introducing argon into a vacuum induction smelting furnace for smelting Ni and Mo; vacuumizing the vacuum induction smelting furnace after argon is introduced; adding dried Fe, Cr, W, Co, Mn and V into a vacuumized vacuum induction smelting furnace, and heating the vacuum induction smelting furnace under the conditions of 10 kW-30 kW and 30 kW-60 kW in sequence; refining the melted materials; and taking out after vacuum cooling to obtain the nickel-molybdenum alloy electrode material. The invention has simple operation, safety, reliability, short production period and low cost.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and particularly relates to a nickel-molybdenum alloy electrode material and a preparation method thereof.
Background
The hydrogen energy is a clean, high-efficiency, pollution-free and high-combustion-heat-value novel energy source, and is one of the research hotspots of the current novel energy sources. The common hydrogen production methods include hydrogen production by fossil fuel, hydrogen production by using biomass as a raw material and hydrogen production by water decomposition, wherein the hydrogen production by water decomposition can be divided into two types, namely hydrogen production by water electrolysis and hydrogen production by water photolysis, and the method for electrolyzing alkaline aqueous solution is the most mature and economic method and has the advantages of simple and convenient operation, high product purity and the like. The problems of the prior electrolytic hydrogen production technology are that the overpotential of hydrogen evolution of the cathode is high and the energy consumption is large in the electrolytic process, so that the research and development of an electrode material with low overpotential of hydrogen evolution, low energy consumption and high activity becomes a problem to be solved urgently at present.
In recent years, hydrogen evolution electrode materials have been gradually transformed from single metals to multi-element alloys. Researches find that the Ni-based alloy without containing noble metal has better hydrogen evolution catalytic activity. Common nickel alloy materials are Ni-Mo, Ni-Zn, Ni-Co, Ni-W, Ni-Fe and Ni-Cr, and particularly the Ni-Mo alloy is recognized as the most potential hydrogen evolution electrode material. At present, the preparation methods of the hydrogen evolution electrode material comprise electrodeposition, thermal coating decomposition, magnetron sputtering and the like, and the preparation methods have the problems of difficult precise regulation and control of the content of each component, incapability of large-scale production, high preparation cost, complex production process and the like to different degrees.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the nickel-molybdenum alloy electrode material which is simple to operate, safe and reliable, short in production period and low in cost and the preparation method thereof.
The invention adopts the following technical scheme:
the nickel-molybdenum alloy electrode material is characterized by comprising the following components in percentage by mass: ni 30-80%, Mo 10-60%, Fe 0.1-10%, Cr 0.1-10%, W0.1-10%, Co 0.1-10%, Mn 0.1-10%, and V0.1-10%.
A method for preparing the nickel-molybdenum alloy electrode material according to claim 1, wherein the method comprises the following steps:
(1) washing Ni, Mo, Fe, Cr, W, Co, Mn and V with dilute hydrochloric acid, deionized water and absolute ethyl alcohol in sequence, and then drying in a vacuum oven at 50-80 ℃ to obtain dried Ni, Mo, Fe, Cr, W, Co, Mn and V;
(2) putting the dried Ni and Mo into a vacuum induction smelting furnace, and vacuumizing the vacuum induction smelting furnace until the vacuum degree is less than 1 Pa; the mass ratio of Ni to Mo is (3-8): (1-6);
(3) smelting the Ni and the Mo dried in the step (2) for 1 to 5 hours under the condition of 10 to 30 kW;
(4) introducing argon with the flow rate of 10 mL/min-200 mL/min into a vacuum induction melting furnace for melting Ni and Mo, wherein the introduction time of the argon is 10 min-60 min;
(5) vacuumizing the vacuum induction smelting furnace after argon is introduced until the vacuum degree is less than 1 Pa;
(6) adding dried Fe, Cr, W, Co, Mn, V, Ni, Mo, Fe, Cr, W, Co, Mn and V into the vacuum induction smelting furnace vacuumized in the step (5) according to the mass ratio of (3-8): (1-6): (0.01-1): (0.01-1): (0.01-1): (0.01-1): (0.01-1): (0.01 to 1); heating a vacuum induction smelting furnace for 30-180 min under the condition of 10-30 kW, and then heating the vacuum induction smelting furnace for 30-180 min under the condition of 30-60 kW to obtain a melted material;
(7) refining the melted material to obtain a refined material; the refining process conditions are as follows: the refining temperature is 2600-4000 ℃, and the refining time is 10-60 min;
(8) and (4) cooling the refined material in vacuum and taking out to obtain the nickel-molybdenum alloy electrode material.
The preparation method of the nickel-molybdenum alloy electrode material is characterized in that the mass fraction of the dilute hydrochloric acid in the step (1) is 0.1-30%.
The preparation method of the nickel-molybdenum alloy electrode material is characterized in that in the step (1), Ni, Mo, Fe, Cr, W, Co, Mn and V are sequentially washed for 3-10 times by dilute hydrochloric acid, deionized water and absolute ethyl alcohol and then are dried in a vacuum oven at 50-80 ℃.
The invention has the beneficial technical effects that: the nickel-molybdenum alloy electrode material not only can accurately regulate and control the content of each component, but also can be added with other metals as auxiliary components to regulate other physical and chemical properties of the material, such as mechanical property, corrosivity, conductivity, electrochemistry and the like, and the electrode material can be directly prepared into a working electrode. According to the invention, the raw materials are directly prepared into the working electrode, and the foamed Ni, low-carbon steel and other substrates are not required to be used for supporting the electrode material, so that the preparation process of the working electrode can be simplified, the cost is reduced, the problems of material falling, poor corrosion resistance and the like caused by untight combination of the substrate and the electrode material in the use process can be avoided, the working life of the electrode can be prolonged, and a solid foundation is laid for large-scale and batch production of the electrode; the electrode material does not need to add other auxiliary substances such as adhesive, activated carbon (conductive agent), NMP (solvent) and the like, improves the conductivity of the material, and reduces the resistance in the reaction, thereby achieving the effect of reducing the hydrogen evolution overpotential of the material, ensuring the smooth operation of the material and improving the reaction efficiency. In addition, the electrode material is prepared by a vacuum induction melting method, and has the advantages of simple operation, safety, reliability, short production period, low cost and the like.
Detailed Description
The nickel-molybdenum alloy electrode material comprises the following components in percentage by mass: 30 to 80 percent of Ni, 10 to 60 percent of Mo, 0.1 to 10 percent of Fe, 0.1 to 10 percent of Cr, 0.1 to 10 percent of W, 0.1 to 10 percent of Co, 0.1 to 10 percent of Mn and 0.1 to 10 percent of V. The alloy can be divided into main components and auxiliary components according to different contents of the components, wherein the main components can be metal Ni and Mo, and the auxiliary alloy materials can be metal Fe, Cr, W, Co, Mn and V.
The preparation method of the nickel-molybdenum alloy electrode material comprises the following steps:
(1) washing Ni, Mo, Fe, Cr, W, Co, Mn and V for 3-10 times by using 0.1-30 mass percent of dilute hydrochloric acid, deionized water and absolute ethyl alcohol in sequence, and then drying in a vacuum oven at 50-80 ℃ to obtain dried Ni, Mo, Fe, Cr, W, Co, Mn and V.
(2) Putting the dried Ni and Mo main materials into a crucible, and putting Fe, Cr, W, Co, Mn, V and other alloy materials into a funnel type feeder; putting the crucible into a vacuum induction smelting furnace, and vacuumizing the vacuum induction smelting furnace until the vacuum degree is less than 1 Pa; the mass ratio of Ni to Mo is (3-8): (1-6).
(3) And (3) feeding electricity to heat furnace burden, melting 1-5 h-70-80% of crucible furnace burden after the Ni and the Mo dried in the step (2) under 10-30 kW, and melting layer by layer under low power by utilizing the skin effect of induction current so as to remove gas and nonmetal impurities to the maximum extent.
(4) And after the smelting is finished, introducing argon at the flow rate of 10 mL/min-200 mL/min into a vacuum induction smelting furnace for smelting Ni and Mo, wherein the introduction time of the argon is 10 min-60 min.
(5) And vacuumizing again, and vacuumizing the vacuum induction melting furnace introduced with argon until the vacuum degree is less than 1 Pa.
(6) Opening a funnel type feeder, adding dried Fe, Cr, W, Co, Mn and V auxiliary alloy materials into the vacuum induction smelting furnace vacuumized in the step (5), wherein the mass ratio of Ni, Mo, Fe, Cr, W, Co, Mn and V is (3-8): (1-6): (0.01-1): (0.01-1): (0.01-1): (0.01-1): (0.01-1): (0.01 to 1); and (3) heating the vacuum induction melting furnace again for 30-180 min under the condition of low power of 10-30 kW to avoid splashing after cold materials are added, and heating the vacuum induction melting furnace for 30-180 min under the condition of 30-60 kW after the auxiliary alloy materials begin to redden to obtain the melted materials.
(7) When the materials are completely melted and no bubbles escape from the surface of the molten pool, the molten pool enters a refining period, and the melted materials are refined to obtain refined materials; the refining process conditions are as follows: the refining temperature is 2600-4000 ℃, and the refining time is 10-60 min; and after the components are qualified, casting the alloy melt into a prepared die.
(8) And taking out after vacuum cooling to obtain the nickel-molybdenum alloy electrode material.
Example 1
And washing Ni, Mo, Fe, Cr, W, Co, Mn and V for 5 times by using dilute hydrochloric acid, deionized water and absolute ethyl alcohol with the mass fraction of 5% in sequence, and then placing the washed materials in a vacuum oven at 60 ℃ for drying to obtain the dried Ni, Mo, Fe, Cr, W, Co, Mn and V. The dried Ni and Mo main materials are loaded into a crucible, and Fe, Cr, W, Co, Mn and V alloy materials are placed into a funnel type feeder, wherein the content of each component is shown in Table 1. Putting the crucible into a vacuum induction smelting furnace, and vacuumizing the vacuum induction smelting furnace until the vacuum degree is less than 1 Pa; the mass ratio of Ni to Mo is 5.0: 1.8. and (3) feeding electricity to heat the furnace charge, and smelting the dried Ni and Mo under 30kW for 1h to 70-80% of crucible furnace charge to melt. And after the smelting is finished, introducing argon at the flow rate of 100mL/min into a vacuum induction smelting furnace for smelting Ni and Mo, wherein the introduction time of the argon is 30 min. And vacuumizing again, and vacuumizing the vacuum induction melting furnace introduced with argon until the vacuum degree is less than 1 Pa. Opening a funnel type feeder, adding dried Fe, Cr, W, Co, Mn and V auxiliary alloy materials into the vacuum induction smelting furnace after vacuumizing again, wherein the mass ratio of Ni, Mo, Fe, Cr, W, Co, Mn and V is 5.0: 1.8: 0.8: 0.8: 0.4: 0.4: 0.4: 0.4; and heating the vacuum induction melting furnace for 30min at low power of 30kW to avoid splashing after cold materials are added, and heating the vacuum induction melting furnace for 30min at 45kW after the auxiliary alloy materials begin to glow red to obtain melted materials. When the materials are completely melted and no bubbles escape from the surface of the molten pool, entering a refining period, and refining the melted materials at 2800 ℃ for 60 min; and after the components are qualified, casting the alloy melt into a prepared die. And taking out after vacuum cooling to obtain the nickel-molybdenum alloy electrode material.
Table 1 the electrode material in example 1 contains the components and their mass percentages
| Element(s) | Ni | Mo | Fe | Cr | W | Co | Mn | V |
| Content (%) | 50 | 18 | 8 | 8 | 4 | 4 | 4 | 4 |
Example 2
And washing Ni, Mo, Fe, Cr, W, Co, Mn and V for 5 times by using dilute hydrochloric acid, deionized water and absolute ethyl alcohol with the mass fraction of 5% in sequence, and then placing the washed materials in a vacuum oven at 60 ℃ for drying to obtain the dried Ni, Mo, Fe, Cr, W, Co, Mn and V. The dried Ni and Mo main materials are loaded into a crucible, and Fe, Cr, W, Co, Mn and V alloy materials are placed into a funnel type feeder, wherein the content of each component is shown in Table 2. Putting the crucible into a vacuum induction smelting furnace, and vacuumizing the vacuum induction smelting furnace until the vacuum degree is less than 1 Pa; the mass ratio of Ni to Mo is 5.0: 2.4. and (3) feeding electricity to heat the furnace charge, and smelting the dried Ni and Mo for 3h to 70-80% of crucible furnace charge under 30kW to melt. And after the smelting is finished, introducing argon at the flow rate of 100mL/min into a vacuum induction smelting furnace for smelting Ni and Mo, wherein the introduction time of the argon is 30 min. And vacuumizing again, and vacuumizing the vacuum induction melting furnace introduced with argon until the vacuum degree is less than 1 Pa. Opening a funnel type feeder, adding dried Fe, Cr, W, Co, Mn and V auxiliary alloy materials into the vacuum induction smelting furnace after vacuumizing again, wherein the mass ratio of Ni, Mo, Fe, Cr, W, Co, Mn and V is 5.0: 2.4: 0.7: 0.7: 0.3: 0.3: 0.3: 0.3; and heating the vacuum induction melting furnace for 60min at low power of 30kW to avoid splashing after cold materials are added, and heating the vacuum induction melting furnace for 180min at 45kW after the auxiliary alloy materials begin to glow red to obtain melted materials. When the materials are completely melted and no bubbles escape from the surface of the molten pool, entering a refining period, and refining the melted materials at 2800 ℃ for 60 min; and after the components are qualified, casting the alloy melt into a prepared die. And taking out after vacuum cooling to obtain the nickel-molybdenum alloy electrode material.
Table 2 components contained in the electrode material in example 2 and their mass percentages
| Element(s) | Ni | Mo | Fe | Cr | W | Co | Mn | V |
| Content (%) | 50 | 24 | 7 | 7 | 3 | 3 | 3 | 3 |
Example 3
And washing Ni, Mo, Fe, Cr, W, Co, Mn and V for 5 times by using dilute hydrochloric acid, deionized water and absolute ethyl alcohol with the mass fraction of 5% in sequence, and then placing the washed materials in a vacuum oven at 60 ℃ for drying to obtain the dried Ni, Mo, Fe, Cr, W, Co, Mn and V. The dried Ni and Mo main materials are loaded into a crucible, and Fe, Cr, W, Co, Mn and V alloy materials are placed into a funnel type feeder, wherein the content of each component is shown in Table 3. Putting the crucible into a vacuum induction smelting furnace, and vacuumizing the vacuum induction smelting furnace until the vacuum degree is less than 1 Pa; the mass ratio of Ni to Mo is 5: 3. and (3) feeding electricity to heat the furnace charge, and smelting the dried Ni and Mo for 4h to 70-80% of crucible furnace charge under 30kW to melt. And after the smelting is finished, introducing argon at the flow rate of 100mL/min into a vacuum induction smelting furnace for smelting Ni and Mo, wherein the introduction time of the argon is 30 min. And vacuumizing again, and vacuumizing the vacuum induction melting furnace introduced with argon until the vacuum degree is less than 1 Pa. Opening a funnel type feeder, adding dried Fe, Cr, W, Co, Mn and V auxiliary alloy materials into the vacuum induction smelting furnace after vacuumizing again, wherein the mass ratio of Ni, Mo, Fe, Cr, W, Co, Mn and V is 5: 3: 0.6: 0.6: 0.2: 0.2: 0.2: 0.2; and heating the vacuum induction melting furnace for 120min at low power of 30kW to avoid splashing after cold materials are added, and heating the vacuum induction melting furnace for 120min at 45kW after the auxiliary alloy materials begin to glow red to obtain melted materials.
When the materials are completely melted and no bubbles escape from the surface of the molten pool, entering a refining period, and refining the melted materials at 2800 ℃ for 60 min; and after the components are qualified, casting the alloy melt into a prepared die. And taking out after vacuum cooling to obtain the nickel-molybdenum alloy electrode material.
Table 3 components contained in electrode material in example 3 and their mass percentages
| Element(s) | Ni | Mo | Fe | Cr | W | Co | Mn | V |
| Content (%) | 50 | 30 | 6 | 6 | 2 | 2 | 2 | 2 |
Example 4
And washing Ni, Mo, Fe, Cr, W, Co, Mn and V for 5 times by using dilute hydrochloric acid, deionized water and absolute ethyl alcohol with the mass fraction of 5% in sequence, and then placing the washed materials in a vacuum oven at 60 ℃ for drying to obtain the dried Ni, Mo, Fe, Cr, W, Co, Mn and V. The dried Ni and Mo main materials are loaded into a crucible, and Fe, Cr, W, Co, Mn and V alloy materials are placed into a funnel type feeder, wherein the content of each component is shown in Table 4. Putting the crucible into a vacuum induction smelting furnace, and vacuumizing the vacuum induction smelting furnace until the vacuum degree is less than 1 Pa; the mass ratio of Ni to Mo is 5.0: 3.6. and (3) feeding electricity to heat the furnace charge, and smelting the dried Ni and Mo under 30kW for 5h to 70-80% of crucible furnace charge to melt. And after the smelting is finished, introducing argon at the flow rate of 100mL/min into a vacuum induction smelting furnace for smelting Ni and Mo, wherein the introduction time of the argon is 30 min. And vacuumizing again, and vacuumizing the vacuum induction melting furnace introduced with argon until the vacuum degree is less than 1 Pa. Opening a funnel type feeder, adding dried Fe, Cr, W, Co, Mn and V auxiliary alloy materials into the vacuum induction smelting furnace after vacuumizing again, wherein the mass ratio of Ni, Mo, Fe, Cr, W, Co, Mn and V is 5.0: 3.6: 0.5: 0.5: 0.1: 0.1: 0.1: 0.1; and heating the vacuum induction melting furnace for 180min at low power of 30kW to avoid splashing after cold materials are added, and heating the vacuum induction melting furnace for 60min at 45kW after the auxiliary alloy materials begin to glow red to obtain melted materials. When the materials are completely melted and no bubbles escape from the surface of the molten pool, entering a refining period, and refining the melted materials at 2800 ℃ for 60 min; and after the components are qualified, casting the alloy melt into a prepared die. And taking out after vacuum cooling to obtain the nickel-molybdenum alloy electrode material.
Table 4 components contained in the electrode material in example 4 and their mass percentages
| Element(s) | Ni | Mo | Fe | Cr | W | Co | Mn | V |
| Content (%) | 50 | 36 | 5 | 5 | 1 | 1 | 1 | 1 |
Claims (4)
1. The nickel-molybdenum alloy electrode material is characterized by comprising the following components in percentage by mass: ni 30-80%, Mo 10-60%, Fe 0.1-10%, Cr 0.1-10%, W0.1-10%, Co 0.1-10%, Mn 0.1-10%, and V0.1-10%.
2. A method for preparing the nickel-molybdenum alloy electrode material according to claim 1, wherein the method comprises the following steps:
(1) washing Ni, Mo, Fe, Cr, W, Co, Mn and V with dilute hydrochloric acid, deionized water and absolute ethyl alcohol in sequence, and drying in a vacuum oven at 50-80 ℃;
(2) putting the dried Ni and Mo into a vacuum induction smelting furnace, and vacuumizing the vacuum induction smelting furnace until the vacuum degree is less than 1 Pa; the mass ratio of Ni to Mo is (3-8) to (1-6);
(3) smelting the Ni and the Mo dried in the step (2) for 1 to 5 hours under the condition of 10 to 30 kW;
(4) introducing argon with the flow rate of 10 mL/min-200 mL/min into a vacuum induction melting furnace for melting Ni and Mo, wherein the introduction time of the argon is 10 min-60 min;
(5) vacuumizing the vacuum induction smelting furnace after argon is introduced until the vacuum degree is less than 1 Pa;
(6) adding the dried Fe, Cr, W, Co, Mn, V, Ni, Mo, Fe, Cr, W, Co, Mn and V into the vacuum induction smelting furnace vacuumized in the step (5) in a mass ratio of (3-8) to (1-6) to (0.01-1); heating a vacuum induction smelting furnace for 30-180 min under the condition of 10-30 kW, and then heating the vacuum induction smelting furnace for 30-180 min under the condition of 30-60 kW to obtain a melted material;
(7) refining the melted material to obtain a refined material; the refining process conditions are as follows: the refining temperature is 2600-4000 ℃, and the refining time is 10-60 min;
(8) and (4) cooling the refined material in vacuum and taking out to obtain the nickel-molybdenum alloy electrode material.
3. The method for preparing the nickel-molybdenum alloy electrode material as claimed in claim 2, wherein the mass fraction of the dilute hydrochloric acid in the step (1) is 0.1-30%.
4. The method for preparing the nickel-molybdenum alloy electrode material as claimed in claim 3, wherein in the step (1), Ni, Mo, Fe, Cr, W, Co, Mn and V are sequentially washed with dilute hydrochloric acid, deionized water and absolute ethyl alcohol for 3-10 times and then dried in a vacuum oven at 50-80 ℃.
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| CN113957292A (en) * | 2021-10-29 | 2022-01-21 | 江苏新航合金科技有限公司 | High-purity nickel-based alloy material for hydrogenation reactor equipment |
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|---|---|---|---|---|
| CN113430557A (en) * | 2021-06-09 | 2021-09-24 | 有研工程技术研究院有限公司 | Multifunctional power layer electrode material and preparation method thereof |
| CN113430557B (en) * | 2021-06-09 | 2023-01-13 | 有研工程技术研究院有限公司 | Multifunctional power layer electrode material and preparation method thereof |
| CN113957292A (en) * | 2021-10-29 | 2022-01-21 | 江苏新航合金科技有限公司 | High-purity nickel-based alloy material for hydrogenation reactor equipment |
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Application publication date: 20210511 |