CN111441067A - Method for preparing alloy - Google Patents
Method for preparing alloy Download PDFInfo
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- CN111441067A CN111441067A CN202010456901.7A CN202010456901A CN111441067A CN 111441067 A CN111441067 A CN 111441067A CN 202010456901 A CN202010456901 A CN 202010456901A CN 111441067 A CN111441067 A CN 111441067A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
- C25C7/025—Electrodes; Connections thereof used in cells for the electrolysis of melts
Abstract
The invention discloses a preparation method of an alloy. The preparation method comprises the following steps: arranging a molten salt electrolysis system in an electrolytic cell, wherein the molten salt electrolysis system is a chloride molten salt electrolysis system or a fluoride molten salt electrolysis system containing first metal ions; arranging a cathode, depositing a liquid or solid second metal on the bottom of the electrolytic tank, and communicating a lead with a direct-current power supply cathode; arranging an anode, containing a solid or liquid first metal by using a basket or a crucible, and communicating a direct current power supply anode by adopting a lead; electrolyzing, dissolving the first metal at the anode, depositing and alloying the first metal at the cathode to prepare an alloy; wherein the densities of the liquid or solid first metal and the second metal are both greater than the density of the molten salt electrolysis system. By applying the technical scheme of the invention, the alloy components can be designed and controlled at will between 0.01 and 99 percent, and compared with the process in the prior art, the production efficiency of the alloy is greatly improved.
Description
Technical Field
The invention relates to the technical field of alloy material preparation, in particular to a preparation method of an alloy.
Background
The molten salt electrolysis is a technical means for preparing the alloy, and the production efficiency is high because the molten salt electrolysis is carried out in an ionic reaction system, the ion migration and diffusion speed is high, and the adopted current density is higher; moreover, the molten salt system has higher temperature, can integrate metal preparation and smelting into a whole, and is an efficient alloy preparation means.
At present, the preparation of the molten salt electrolytic alloy is divided into two modes of codeposition and electrolytic diffusion, wherein the codeposition requires that the precipitation potential difference between alloy elements cannot be too large, and has certain limitation; the alloy produced by the electrolytic diffusion method is a process of electrochemically depositing other alloy elements on an alloy cathode by using liquid or solid metal as the alloy cathode, and performing diffusion alloying.
Although the electrolytic system is different, the alloy element raw materials for preparing the alloy by the traditional electrolytic diffusion method generally adopt oxides or chlorides, and the alloy elements in the electrolytic process are supplemented by adding materials containing the alloy elements into a molten salt system, and the elements are deposited on the parent metal in the form of ions to form the alloy. The disadvantages are mainly the following: 1) the raw materials are added into a molten salt system, and volatilization loss can be caused in the process; 2) the dissolution process is slow, and the production efficiency is restricted; 3) certain alloy element chlorides or oxides are difficult to dissolve in a molten salt system; 3) the current efficiency is low and unstable, and the alloy composition is difficult to control.
Disclosure of Invention
The invention aims to provide a preparation method of an alloy so as to improve the production efficiency of the alloy.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method of preparing an alloy. The preparation method comprises the following steps: arranging a molten salt electrolysis system in an electrolytic cell, wherein the molten salt electrolysis system is a chloride molten salt electrolysis system or a fluoride molten salt electrolysis system containing first metal ions; arranging a cathode, depositing a liquid or solid second metal on the bottom of the electrolytic tank, and communicating a lead with a direct-current power supply cathode; arranging an anode, containing a solid or liquid first metal by using a basket or a crucible, and communicating a direct current power supply anode by adopting a lead; electrolyzing, dissolving the first metal at the anode, depositing and alloying the first metal at the cathode to prepare an alloy; wherein the densities of the liquid or solid first metal and the second metal are both greater than the density of the molten salt electrolysis system.
Further, the molten salt electrolysis system is a one-component or multi-component system.
Further, the chloride molten salt electrolysis system comprises KCl, NaCl and CaCl2L iCl, RbCl, CsCl and MgCl2One or more of the group consisting of; the fluoride molten salt electrolysis system comprises a material selected from KF, NaF and CaF2L iF, RbF, CsF and MgF2One or more of the group consisting of.
Further, the first metal is any metal; preferably, the first metal is titanium, zirconium, tungsten, molybdenum, tantalum or niobium.
Further, the second metal is different from the first metal, and the second metal includes one or more metal elements.
Furthermore, the first metal ions in the molten salt electrolysis system are added in the form of chloride or fluoride, and the concentration of the chloride or fluoride of the first metal ions in the molten salt electrolysis system is 1-15 wt%.
Further, the electrolysis temperature is higher than the melting point of the molten salt electrolysis system.
Further, the cathode current density is 0.1-5A/cm2。
Further, the preparation method also comprises the following steps: and after the electrolysis is finished, taking out the alloy, and smelting and casting the alloy.
Further, when the molten salt electrolysis system is a KCl-NaCl system, the electrolysis temperature is controlled at 700 ℃.
By applying the technical scheme of the invention, various alloys are directly produced by adopting a molten salt electrolysis mode and an electrolysis-electrodeposition method; the cathode is made of liquid or solid metal and is deposited at the bottom of the electrolytic tank, a lead is communicated with a direct current power supply cathode, the anode is made of a basket or crucible type and is filled with the solid or liquid metal, the direct current power supply is connected, then constant current electrolysis-electrodeposition is carried out, the anode metal is continuously dissolved and is deposited and alloyed on the cathode, the passing electric quantity is calculated in advance according to the target alloy components, electrolysis is stopped after a certain time, the alloy is further taken out, then melted and cast to form a target alloy product, and the alloy components can be designed and controlled at will between 0.01 and 99 percent. Compared with the prior art, the production efficiency of the alloy is greatly improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a synthesis system employed in a method of preparing an alloy according to an embodiment of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those described or illustrated herein.
According to an exemplary embodiment of the present invention, a method of making an alloy is provided. The preparation method comprises the following steps: arranging a molten salt electrolysis system in an electrolytic cell, wherein the molten salt electrolysis system is a chloride molten salt electrolysis system or a fluoride molten salt electrolysis system containing first metal (also called as alloy element) ions; arranging a cathode, depositing a liquid or solid second metal (also called a mother metal) at the bottom of the electrolytic bath, and communicating a lead with a direct current power supply cathode; arranging an anode, containing a solid or liquid first metal by using a basket or a crucible, and communicating a direct current power supply anode by adopting a lead; and electrolyzing, dissolving the first metal at the anode, depositing and alloying the first metal at the cathode to prepare the alloy.
By applying the technical scheme of the invention, various alloys are directly produced by adopting a molten salt electrolysis mode and an electrolysis-electrodeposition method; the cathode is made of liquid or solid metal and is deposited at the bottom of the electrolytic tank, a lead is communicated with a direct current power supply cathode, the anode is made of a basket or crucible type and is filled with the solid or liquid metal, the direct current power supply is connected, then constant current electrolysis-electrodeposition is carried out, the anode metal is continuously dissolved and is deposited and alloyed on the cathode, the passing electric quantity is calculated in advance according to the target alloy components, electrolysis is stopped after a certain time, the alloy is further taken out, then melted and cast to form a target alloy product, and the alloy components can be designed and controlled at will between 0.01 and 99 percent. Compared with the prior art, the production efficiency of the alloy is greatly improved.
In the present invention, the molten salt electrolysis system may be a mono-component or multi-component (multi-component includes a binary component and more). Preferably, the chloride molten salt electrolysis system comprises KCl, NaCl and CaCl2L iCl, RbCl, CsCl and MgCl2One or more of the group consisting of; the fluoride molten salt electrolysis system comprises a material selected from KF, NaF and CaF2L iF, RbF, CsF and MgF2One or more of the group consisting of.
In the present invention, the first metal may be any metal, especially for metals that are less soluble and difficult to alloy, such as titanium, zirconium, tungsten, molybdenum, tantalum, niobium, and the like. The metals which are difficult to dissolve and alloy are difficult to prepare by the method in the prior art, or the production efficiency is extremely low, but the technical scheme of the invention can be used for producing the metals with high efficiency. The second metal, i.e., the mother metal in the alloy, is any metal or any alloy, and may be in a liquid state or a solid state.
Preferably, the first metal ions in the molten salt electrolysis system are added in the form of chloride or fluoride, and the concentration of the chloride or fluoride of the first metal ions in the molten salt electrolysis system is 1-15 wt%. The electrolysis temperature is determined according to the melting point of a molten salt electrolysis system, generally is above 50 ℃, such as the electrolysis temperature of a KCl-NaCl system, and is controlled at 700 ℃.
The electrolysis temperature is higher than the melting point of a molten salt electrolysis system.
In a typical embodiment of the present invention, the cathode current density is generally controlled to be 0.1 to 5A/cm2The crucible is used to carry the formed liquid alloy. The anode may be in the form of a basket if it is solid metal or in the form of a crucible if it is liquid metal. As shown in fig. 1, the left drawing is a solid anode, a basket is used for containing anode material, a cathode is liquid, and a crucible is used for containing cathode material; in the right drawing, the anode and the cathode are both liquid, and both adopt crucibles to contain electrode materials. The electrolysis time is controlled according to the Faraday electric quantity of the alloy components, and after the electrolysis is finished, the alloy is taken out from the crucible and is smelted and cast to form the target alloy.
The following examples are provided to further illustrate the advantageous effects of the present invention.
Example 1
Adopting a KCl-NaCl system at 750 ℃, adding 8 wt% TiCl2The aluminum-magnesium-titanium alloy is prepared by carrying titanium solid by a graphite basket and electrolytically depositing titanium on a liquid cathode aluminum-magnesium alloy, and the current density of the cathode is controlled to be 0.8A/cm2And electrolyzing for 10 hours to finally obtain the alloy with 5wt percent of Al-Mg-Ti.
Example 2
Adopting a KCl-NaCl system at 750 ℃, adding 8 wt% TiCl2Carrying titanium solid by a graphite basket, preparing an aluminum-titanium alloy by electrolytically depositing titanium on liquid cathode aluminum, and controlling the current density of the cathode at 0.5A/cm2And electrolyzing for 5 hours to finally obtain the Al-Ti alloy with the weight percent of 2.
Example 3
Adopting a KCl-NaCl system at 750 ℃, adding 5 wt% YCl3Carrying yttrium solid by a graphite basket, preparing an aluminum-yttrium alloy by electrolyzing yttrium through a liquid cathode aluminum, and controlling the cathode current density to be 1A/cm2And electrolyzing for 10 hours to finally obtain the Al-Y30wt percent alloy.
Example 4
Adopting a KCl-NaCl system at 750 ℃, adding 5 wt% YCl3Carrying yttrium solid by a graphite basket, preparing an aluminum-yttrium alloy by electrolyzing yttrium through a liquid cathode aluminum, and controlling the cathode current density to be 1A/cm2And electrolyzing for 5 hours to obtain the alloy with 10wt percent of Al-Y.
Taking the obtained alloy as a cathode, adopting a KCl-NaCl system at 750 ℃, and adding 8 wt% TiCl2Carrying titanium solid by a graphite basket, preparing the Al-Y-Ti alloy by electrolytically depositing titanium on the liquid Al-Y10 wt% alloy, and controlling the cathode current density to be 0.5A/cm2And electrolyzing for 5 hours to finally obtain the alloy of Al-Y10 wt-Ti 2 wt%.
Example 5
Adopts 900 ℃ NaF-L iF system, and adds 5 wt% MgF2The magnesium oxide crucible is adopted to bear liquid magnesium, the liquid cathode is adopted to electrolyze and deposit magnesium to prepare the aluminum-magnesium alloy, and the cathode current density is controlled to be 0.4A/cm2And electrolyzing for 10 hours to finally obtain the Al-Mg40wt percent alloy.
Example 6
Adopting a KCl-NaCl system at 750 ℃, adding 15 wt% YCl3Carrying yttrium solid by a graphite basket, preparing an aluminum-yttrium alloy by electrolyzing yttrium through a liquid cathode aluminum, and controlling the cathode current density to be 1A/cm2And electrolyzing for 5 hours to obtain the alloy with 10wt percent of Al-Y.
Example 7
Adopting a KCl-NaCl-L iCl system at 750 ℃, adding 15 wt% YCl3Carrying yttrium solid by a graphite basket, preparing an aluminum-yttrium alloy by electrolyzing yttrium through a liquid cathode aluminum, and controlling the cathode current density to be 1A/cm2Electrolyzing for 5h to obtain Al-Y10 wt% alloy。
Example 8
Adopting a KCl-NaCl-CsCl system at 750 ℃, adding 15wt percent YCl3Carrying yttrium solid by a graphite basket, preparing an aluminum-yttrium alloy by electrolyzing yttrium through a liquid cathode aluminum, and controlling the cathode current density to be 1A/cm2And electrolyzing for 5 hours to obtain the Al-Y10wt percent alloy.
Example 9
Adopts a NaCl-CsCl system at 750 ℃, and 15wt percent of YCl is added3Carrying yttrium solid by a graphite basket, preparing an aluminum-yttrium alloy by electrolyzing yttrium through a liquid cathode aluminum, and controlling the cathode current density to be 1A/cm2And electrolyzing for 5 hours to obtain the alloy with 10wt percent of Al-Y.
Example 10
Adopts a NaF-L iF-KF system at 900 ℃, and adds 5wt percent of MgF2The magnesium oxide crucible is adopted to bear liquid magnesium, the liquid cathode is adopted to electrolyze and deposit magnesium to prepare the aluminum-magnesium alloy, and the cathode current density is controlled to be 0.4A/cm2And electrolyzing for 10 hours to finally obtain the Al-Mg40wt percent alloy.
Example 11
Adopts a 900 ℃ L iF-KF system and adds 5wt percent of MgF2The magnesium oxide crucible is adopted to bear liquid magnesium, the liquid cathode is adopted to electrolyze and deposit magnesium to prepare the aluminum-magnesium alloy, and the cathode current density is controlled to be 0.4A/cm2And electrolyzing for 10 hours to finally obtain the Al-Mg40wt percent alloy.
Example 12
Adopting a KCl-NaCl system at 750 ℃, adding 8 wt% TiCl2The aluminum-magnesium-titanium alloy is prepared by carrying titanium solid by a graphite basket and electrolytically depositing titanium on a liquid cathode aluminum-magnesium alloy, and the current density of the cathode is controlled to be 4A/cm2And electrolyzing for 10 hours to finally obtain the alloy with 5wt percent of Al-Mg-Ti.
Example 13
Adopting a KCl-NaCl system at 750 ℃, adding 8 wt% TiCl2The aluminum-magnesium-titanium alloy is prepared by carrying titanium solid by a graphite basket and electrolytically depositing titanium on a liquid cathode aluminum-magnesium alloy, and the current density of the cathode is controlled to be 5A/cm2And electrolyzing for 10 hours to finally obtain the alloy with 5wt percent of Al-Mg-Ti.
Example 14
Adopting a KCl-NaCl-L iCl system at 750 ℃, adding 15 wt% YCl3Carrying solid yttrium by graphite basketry, preparing aluminum-yttrium alloy by liquid cathode aluminum electrolytic deposition yttrium, controlling cathode current density at 5A/cm2And electrolyzing for 5 hours to obtain the Al-Y10wt percent alloy.
Comparative example 1
Adopting a KCl-NaCl system at 750 ℃, adding 8 wt% TiCl2The aluminum-magnesium-titanium alloy is prepared by carrying titanium solid by a graphite basket and electrolytically depositing titanium on a liquid cathode aluminum-magnesium alloy, and the current density of the cathode is controlled to be 6A/cm2And electrolyzing for 10 hours to finally obtain the alloy with 5 wt% of Al-Mg-Ti, wherein the content of the alkali metal Na is too high.
Comparative example 2
Adopting a KCl-NaCl system at 750 ℃, adding 0.1wt percent TiCl2The aluminum-magnesium-titanium alloy is prepared by carrying titanium solid by a graphite basket and electrolytically depositing titanium on a liquid cathode aluminum-magnesium alloy, and the current density of the cathode is controlled to be 3A/cm2And electrolyzing for 10 hours to finally obtain the alloy with 5 wt% of Al-Mg-Ti, wherein the content of the alkali metal Na is too high.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: the invention combines the soluble anode electrolysis and the cathode electrolysis diffusion method to form a brand new method for preparing the alloy, and has the characteristics of simplicity, high efficiency and accurate control of alloy components.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method of making an alloy, comprising:
arranging a molten salt electrolysis system in an electrolytic cell, wherein the molten salt electrolysis system is a chloride molten salt electrolysis system or a fluoride molten salt electrolysis system containing first metal ions;
arranging a cathode, depositing a liquid or solid second metal on the bottom of the electrolytic tank, and communicating a lead with a direct-current power supply cathode;
arranging an anode, containing a solid or liquid first metal by using a basket or a crucible, and communicating a direct current power supply anode by adopting a lead; and
electrolyzing, dissolving the first metal at the anode, depositing and alloying the first metal on the second metal at the cathode, and preparing to obtain the alloy;
wherein the density of both the first metal and the second metal in liquid or solid state is greater than the density of the molten salt electrolysis system.
2. The method of claim 1 wherein the molten salt electrolysis system is a one-component or multi-component system.
3. The method of claim 2, wherein the chloride molten salt electrolysis system comprises a material selected from KCl, NaCl, CaCl2L iCl, RbCl, CsCl and MgCl2One or more of the group consisting of; the fluoride molten salt electrolysis system comprises KF, NaF and CaF2L iF, RbF, CsF and MgF2One or more of the group consisting of.
4. The production method according to claim 1, wherein the first metal is any metal; preferably, the first metal is titanium, zirconium, tungsten, molybdenum, tantalum or niobium.
5. The method according to claim 1, wherein the second metal is different from the first metal, and the second metal includes one or more metal elements.
6. The preparation method of claim 1, wherein the first metal ions in the molten salt electrolysis system are added in the form of chloride or fluoride, and the concentration of the chloride or fluoride of the first metal ions in the molten salt electrolysis system is 1-15 wt%.
7. The method of claim 1 wherein the electrolysis temperature is above the melting point of the molten salt electrolysis system.
8. The production method according to claim 1, characterized in that the cathodic current density is 0.1 to 5A/cm2。
9. The method of manufacturing according to claim 1, further comprising: and after the electrolysis is finished, taking out the alloy, and smelting and casting the alloy.
10. The preparation method according to claim 7, wherein when the molten salt electrolysis system is a KCl-NaCl system, the electrolysis temperature is controlled at 700 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103243385A (en) * | 2013-05-13 | 2013-08-14 | 北京科技大学 | Method for preparing high-purity monocrystalline silicon through electrolytic refining-liquid cathode in-situ directional solidification |
| CN104099643A (en) * | 2014-07-29 | 2014-10-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method for titanium-aluminium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103243385A (en) * | 2013-05-13 | 2013-08-14 | 北京科技大学 | Method for preparing high-purity monocrystalline silicon through electrolytic refining-liquid cathode in-situ directional solidification |
| CN104099643A (en) * | 2014-07-29 | 2014-10-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method for titanium-aluminium alloy |
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