CN113913882B - Method for preparing aluminum-titanium alloy by taking titanium oxycarbide as raw material through low-temperature electrodeposition - Google Patents
Method for preparing aluminum-titanium alloy by taking titanium oxycarbide as raw material through low-temperature electrodeposition Download PDFInfo
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- CN113913882B CN113913882B CN202111337225.2A CN202111337225A CN113913882B CN 113913882 B CN113913882 B CN 113913882B CN 202111337225 A CN202111337225 A CN 202111337225A CN 113913882 B CN113913882 B CN 113913882B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/66—Electroplating: Baths therefor from melts
- C25D3/665—Electroplating: Baths therefor from melts from ionic liquids
Abstract
A method for preparing an aluminum-titanium alloy by taking titanium oxycarbide as a raw material through low-temperature electrodeposition comprises the following steps: (1) Anhydrous AlCl is added 3 Dissolved in ethylene carbonate and then TiCl is added 4 Stirring uniformly to prepare carbon solvation ionic liquid; (2) Will solvateThe ionic liquid is used as electrolyte to form an electrolytic cell system, and a three-electrode system is adopted for electrodeposition; wherein the counter electrode, namely the anode, is titanium oxycarbide; (3) And taking out the cathode after the electro-deposition is finished, cleaning to remove the electrolyte adhered to the surface, and drying to obtain the aluminum-titanium alloy on the surface of the cathode. The method has simple process flow, and obviously reduces energy consumption and production cost; the phenomena of grain segregation, oxidation of the aluminum-titanium alloy and the like are effectively reduced, and the quality of the aluminum-titanium alloy coating is improved; the method has the advantages of short flow, low cost, simple operation, energy conservation and environmental protection, and greatly improves the practicability of the method.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for preparing an aluminum-titanium alloy by taking titanium oxycarbide as a raw material through low-temperature electrodeposition.
Background
The aluminum-titanium alloy is an emerging alloy structural material in the world today, and has many excellent properties, such as high strength, and generally, the specific strength of the aluminum-titanium alloy is far greater than that of other metals; the heat strength is high, and the service temperature of the aluminum-titanium alloy is hundreds of degrees centigrade higher than that of the aluminum alloy; the corrosion resistance of the aluminum-titanium alloy is far superior to that of stainless steel, manganese steel and the like; the low-temperature performance is good, and the aluminum-titanium alloy can still maintain excellent mechanical properties under the conditions of low temperature and ultralow temperature; therefore, the aluminum-titanium alloy is widely used in the fields of aerospace, ocean, automobile industry, biomedicine and the like.
The traditional method for preparing the aluminum-titanium alloy mainly comprises the following steps: (1) direct solution and preparation method: the method is a main method for industrially producing the aluminum-titanium alloy, which is to date, by directly dissolving two pure metals of aluminum and titanium in a high-temperature smelting furnace, has the advantages of simple operation, serious energy consumption, high production cost, influence on the quality of the alloy and reduction of the corrosion resistance; (2) sintering method: adding aluminum powder and titanium dioxide into a metallurgical furnace, adding a reducing agent, and sintering by using a powder metallurgy method. The method has complex equipment and higher production cost; (3) reduction method: simple substance aluminum is added into titanium dioxide, and simple substance titanium is prepared by an aluminothermic method, so that alloy is prepared. The method has the advantages of uneven alloy production, no mass production and high production cost; (4) an electrodeposition method: titanium dioxide and alumina are added into an electrolytic bath to be directly electrified to prepare the alloy. The aluminum-titanium alloy obtained by the method has good quality and uniform components, but has the problems of high reaction temperature, high energy consumption, strong corrosivity of molten salt, short service cycle of equipment and high requirement on a matrix.
If the aluminum-titanium alloy can be prepared by electrodeposition at room temperature, the operation is simple and easy to control, the energy consumption is low, and the cost is low. Compared with the traditional method for preparing metal and alloy by using high-temperature molten salt, the ionic liquid is green and pollution-free, has a wider electrochemical window, and has low energy consumption, low cost and very wide application prospect.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing an aluminum-titanium alloy by taking titanium oxycarbide as a raw material through low-temperature electrodeposition.
The method of the invention comprises the following steps:
(1) Anhydrous AlCl is added 3 Dissolved in ethylene carbonate and TiCl is then added 4 Stirring evenly to prepare ethylene carbonate-AlCl 3 -TiCl 4 A solvated ionic liquid;
(2) Forming an electrolytic cell system by using the solvated ionic liquid as an electrolyte, and performing electrodeposition by adopting a three-electrode system; wherein, the working electrode, namely the cathode is a pure aluminum sheet, the counter electrode, namely the anode is titanium oxycarbide, and the reference electrode is an aluminum wire;
(3) And taking out the cathode after the electro-deposition is finished, cleaning to remove the electrolyte adhered to the surface, and drying to obtain the aluminum-titanium alloy on the surface of the cathode.
In the step (1), ethylene carbonate and anhydrous AlCl 3 And TiCl 4 The molar ratio of (1) to (0.2-0.8) to (0.1-0.5).
In the step (1), the stirring speed is 350-550 r/min, and the stirring time is 15-35 min.
In the step (2), the temperature of the electrolytic cell system is 50-80 ℃ when the electrodeposition is carried out, the applied electromotive force is-1.7 to-3V vs Al, and the electrodeposition time is 0.5-2.5 h.
In the step (2), the inter-electrode distance between the working electrode and the counter electrode is 15mm.
In the step (2), the component of the titanium oxycarbide of the anode is TiC x O y The preparation method comprises the following steps: mixing TiC and TiO 2 Uniformly mixing the components according to a molar ratio of 2:1, and sintering the mixture for 12 hours at the temperature of 900 +/-10 ℃ in vacuum to obtain the soluble anode.
The invention has the beneficial effects that:
1. compared with the traditional process for preparing the aluminum-titanium alloy, the process flow is simple, and the energy consumption and the production cost are obviously reduced;
2. the low-temperature ionic liquid is adopted for electrodeposition, so that a wider electrochemical window is provided, and side reactions are avoided;
3. the titanium content in the aluminum-titanium alloy can be improved by adopting soluble anode titanium oxycarbide;
4. compared with the traditional method, the method effectively reduces the phenomena of grain segregation, oxidation of the aluminum-titanium alloy and the like, and improves the quality of the aluminum-titanium alloy coating;
5. compared with the preparation of metals and alloys by high-temperature molten salt, the method for preparing the aluminum-titanium alloy by using the ionic liquid at the low temperature has the advantages of short flow, low cost, simplicity in operation, energy conservation and environmental friendliness, and greatly improves the practicability of the method.
Detailed Description
In the preparation method of the anode in the embodiment of the invention, reference is made to research on electrochemical behavior of Ti-C-O solid solution synthesized at 900 ℃.
The aluminum-titanium alloy in the embodiment of the invention contains 22-27% of Ti by weight percentage.
The aluminum-titanium alloy in the embodiment of the invention contains less than 0.1% of impurities by mass percent.
In the embodiment of the invention, anhydrous AlCl 3 \ ethylene carbonate and TiCl 4 Reagents were analyzed for commercial availability.
The working electrode and the reference electrode in the embodiment of the invention are commercially available products.
Example 1
Anhydrous AlCl is added 3 Dissolved in carbonic acidTo the vinyl ester, tiCl is then added 4 Stirring evenly to prepare ethylene carbonate-AlCl 3 -TiCl 4 A solvated ionic liquid; ethylene carbonate, anhydrous AlCl 3 And TiCl 4 1; the stirring speed is 350r/min, and the stirring time is 35min;
forming an electrolytic cell system by using the solvated ionic liquid as electrolyte, and performing electrodeposition by adopting a three-electrode system; wherein, the working electrode, namely the cathode is a pure aluminum sheet, the counter electrode, namely the anode is titanium oxycarbide, and the reference electrode is an aluminum wire; when in electrodeposition, the temperature of the electrolytic cell system is 50 ℃, the applied electromotive force is-1.7V vs Al, and the electrodeposition time is 2.5h; the inter-electrode distance between the working electrode and the counter electrode is 15mm;
and taking out the cathode after the electrodeposition is finished, cleaning to remove the electrolyte adhered to the surface, and drying to obtain the aluminum-titanium alloy on the surface of the cathode.
Example 2
The method is the same as example 1 except that;
(1) Ethylene carbonate and anhydrous AlCl 3 And TiCl 4 In a molar ratio of 1; the stirring speed is 550r/min, and the stirring time is 15min;
(2) The temperature of the electrolytic cell system is 80 ℃, the applied electromotive force is-3V vs Al, and the electrodeposition time is 0.5h.
Example 3
The method is the same as example 1, except that;
(1) Ethylene carbonate, anhydrous AlCl 3 And TiCl 4 In a molar ratio of 1; the stirring speed is 450r/min, and the stirring time is 25min;
(2) The temperature of the electrolytic cell system is 60 ℃, the applied electromotive force is-2V vs Al, and the electrodeposition time is 1.5h.
Example 4
The method is the same as example 1, except that;
(1) Ethylene carbonate and anhydrous AlCl 3 And TiCl 4 1; stirring at 400r/min for 20min;
(2) The temperature of the electrolytic cell system is 70 ℃, the applied electromotive force is-2.5V vs Al, and the electrodeposition time is 1h.
Example 5
The method is the same as example 1, except that;
(1) Ethylene carbonate, anhydrous AlCl 3 And TiCl 4 In a molar ratio of 1; stirring at 500r/min for 30min;
(2) The temperature of the electrolytic cell system is 75 ℃, the applied electromotive force is-2V vs Al, and the electrodeposition time is 2h.
Example 6
The method is the same as example 1, except that;
(1) Ethylene carbonate, anhydrous AlCl 3 And TiCl 4 In a molar ratio of 1; the stirring speed is 450r/min, and the stirring time is 30min;
(2) The temperature of the electrolytic cell system is 65 ℃, the applied electromotive force is-2V vs Al, and the electrodeposition time is 1.5h.
Claims (9)
1. A method for preparing an aluminum-titanium alloy by taking titanium oxycarbide as a raw material through low-temperature electrodeposition is characterized by comprising the following steps:
(1) Anhydrous AlCl is added 3 Dissolved in ethylene carbonate and then TiCl is added 4 Stirring evenly to prepare ethylene carbonate-AlCl 3 -TiCl 4 A solvated ionic liquid;
(2) Forming an electrolytic cell system by using the solvated ionic liquid as an electrolyte, and performing electrodeposition by adopting a three-electrode system; wherein, the working electrode, namely the cathode is a pure aluminum sheet, the counter electrode, namely the anode is titanium oxycarbide, and the reference electrode is an aluminum wire;
(3) And taking out the cathode after the electrodeposition is finished, cleaning to remove the electrolyte adhered to the surface, and drying to obtain the aluminum-titanium alloy on the surface of the cathode.
2. The method for preparing the aluminum-titanium alloy by using the titanium oxycarbide as the raw material through the low-temperature electrodeposition as claimed in claim 1, wherein in the step (1), ethylene carbonate and anhydrous AlCl are adopted 3 And TiCl 4 The molar ratio of (1) to (0.2-0.8) to (0.1-0.5)。
3. The method for preparing the aluminum-titanium alloy by using the titanium oxycarbide as the raw material through the low-temperature electrodeposition as claimed in claim 1, wherein the stirring speed in the step (1) is 350 to 550r/min.
4. The method for preparing the aluminum-titanium alloy by using the titanium oxycarbide as the raw material through the low-temperature electrodeposition as claimed in claim 1, wherein the stirring time in the step (1) is 15-35 min.
5. The method for preparing the aluminum-titanium alloy by using the titanium oxycarbide as the raw material through the low-temperature electrodeposition as claimed in claim 1, wherein in the step (2), the temperature of an electrolytic cell system during the electrodeposition is 50-80 ℃.
6. The method for preparing Al-Ti alloy by low-temperature electrodeposition of titanium oxycarbide as raw material according to claim 1, wherein in the step (2), the electrodeposition is carried out with an electromotive force of-1.7 to-3V vs Al.
7. The method for preparing the aluminum-titanium alloy by using the titanium oxycarbide as the raw material through the low-temperature electrodeposition as claimed in claim 1, wherein in the step (2), the electrodeposition time is 0.5-2.5 h.
8. The method for preparing the aluminum-titanium alloy by using the titanium oxycarbide as the raw material through the low-temperature electrodeposition as claimed in claim 1, wherein in the step (2), the polar distance between the working electrode and the counter electrode is 15mm.
9. The method for preparing Al-Ti alloy from Ti oxycarbide by low-temperature electrodeposition as claimed in claim 1, wherein in step (2), the composition of Ti oxycarbide in anode is TiC x O y The preparation method comprises the following steps: mixing TiC and TiO 2 Uniformly mixing according to a molar ratio of 2:1, and sintering for 12 hours at the temperature of 900 +/-10 ℃ in vacuum to obtain the soluble anode.
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| CN101949038B (en) * | 2010-09-21 | 2011-12-14 | 攀钢集团钢铁钒钛股份有限公司 | Method for preparing TiCxOy composite anode with electrolysis method |
| CN101994128A (en) * | 2010-11-26 | 2011-03-30 | 昆明理工大学 | Method for preparing Al-Ti alloy or plated Al-Ti alloy by low-temperature electrolytic deposition of ionic liquid |
| US10208391B2 (en) * | 2014-10-17 | 2019-02-19 | Ut-Battelle, Llc | Aluminum trihalide-neutral ligand ionic liquids and their use in aluminum deposition |
| CN107190282B (en) * | 2017-05-19 | 2019-07-30 | 东北大学 | A kind of room temperature molten salt and its preparation method and application |
| CN107130264B (en) * | 2017-05-19 | 2018-12-18 | 东北大学 | A kind of method of nearly room temperature electrolytic preparation aluminium-based rare-earth alloy |
| CN106967998B (en) * | 2017-05-19 | 2018-10-02 | 东北大学 | The method for preparing Al-Li master alloys as the nearly room temperature electro-deposition of raw material using lithia |
| CN109023431B (en) * | 2018-09-30 | 2020-05-12 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing titanium-aluminum alloy |
| CN110983378B (en) * | 2019-11-15 | 2020-12-18 | 北京理工大学 | Device and method for preparing metal aluminum and titanium tetrachloride in molten salt by soluble anode |
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