CN110343929B - Aluminum-molybdenum-vanadium intermediate alloy and preparation method thereof - Google Patents
Aluminum-molybdenum-vanadium intermediate alloy and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
- C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention provides an aluminum-molybdenum-vanadium intermediate alloy and a preparation method thereof, and relates to the technical field of metal materials. The aluminum-molybdenum-vanadium intermediate alloy provided by the invention comprises, by mass, 17.0-22.0% of Al, 40.0-42.0% of Mo and 38.0-41.0% of V. The invention ensures that the aluminum-molybdenum-vanadium intermediate alloy has smaller component segregation by controlling the components and the content, is beneficial to homogenizing the components of the titanium alloy when the titanium alloy is smelted, prevents the component segregation, optimizes the batching procedure when the titanium alloy is smelted, and can realize accurate batching in the production process. The preparation method provided by the invention can improve the uniformity and stability of the components of the aluminum-molybdenum-vanadium intermediate alloy, reduce the content of O, N and other impurities, has a simple process, is easy to control, and is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to an aluminum-molybdenum-vanadium intermediate alloy and a preparation method thereof.
Background
Titanium and its alloy have excellent properties, such as high specific strength, corrosion resistance, high temperature resistance, good comprehensive technological properties and the like, are increasingly attractive materials in the field of modern industrial science and technology, and are widely applied in the fields of space navigation, aviation, petroleum, chemical engineering, light industry, metallurgy, machinery, energy and the like.
Aluminum, molybdenum and vanadium are main alloy components of titanium alloy, are usually added to the titanium alloy in the form of master alloy, and the main application of the titanium alloy is TA11 and TC 16. TA11 is used in the aerospace industry, generally for making aircraft turbine blades; TC16 is a titanium alloy capable of operating above 400 ℃ and is commonly used in the manufacture of fasteners for aircraft. The quality of the intermediate alloy directly influences the performance of the titanium alloy.
At present, most of titanium alloy intermediate alloys are binary alloys, and in order to meet the performance requirements in use, a plurality of binary alloys need to be added, so that the product performance is easy to be unstable, and the difficulty is brought to the intermediate process of producing the titanium alloy. The problem can be effectively solved by using the ternary alloy as the intermediate alloy, and meanwhile, each component of the ternary alloy can be adjusted according to requirements, so that the operation is simple, the preparation of the titanium alloy is convenient, and the development of the project has a long-term significance.
Currently, the preparation method of the aluminum-molybdenum-vanadium ternary alloy is generally prepared by an external aluminothermic method, for example, CN200310119084.2 discloses an aluminum-molybdenum-vanadium intermediate alloy and a preparation method thereof, and the preparation process comprises the following steps: aluminum is used as a reducing agent, vanadium pentoxide and molybdenum trioxide are used as oxidizing agents, calcium fluoride is added as a slagging agent, potassium chlorate is used as a heating agent, and the mixture is ignited and smelted, so that the aluminum-molybdenum-vanadium alloy is prepared. The method has the advantages of simple equipment, convenient operation, low investment and the like, and has the defects of poor alloy uniformity, uncontrollable impurities, particularly oxygen, nitrogen and other gas phase impurities, and increased brittleness of the titanium alloy due to nitrogen elements, and direct influence on the quality of the titanium alloy.
Disclosure of Invention
In view of the above, the present invention provides an aluminum-molybdenum-vanadium intermediate alloy and a preparation method thereof. The aluminum-molybdenum-vanadium intermediate alloy provided by the invention has small component segregation, and is beneficial to homogenization of alloy components when a titanium alloy is smelted. The preparation method provided by the invention can improve the uniform stability of the components of the aluminum-molybdenum-vanadium intermediate alloy, reduce the impurity content, and has the advantages of simple process and easy control.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an aluminum-molybdenum-vanadium intermediate alloy which comprises, by mass, 17.0-22.0% of Al, 40.0-42.0% of Mo and 38.0-41.0% of V.
Preferably, the aluminum-molybdenum-vanadium intermediate alloy comprises, by mass, 18.0-21.0% of Al, 41.0-42.0% of Mo, and 39.0-41.0% of V.
Preferably, the aluminum-molybdenum-vanadium intermediate alloy comprises 19.0% of Al, 41.0% of Mo and 40.0% of V by mass.
The invention provides a preparation method of the aluminum-molybdenum-vanadium intermediate alloy, which comprises the following steps:
(1) mixing aluminum and molybdenum trioxide to carry out aluminothermic reaction, and cooling to obtain an aluminum-molybdenum primary alloy;
(2) mixing aluminum and vanadium pentoxide, carrying out aluminothermic reaction, and cooling to obtain an aluminum-vanadium primary alloy;
(3) carrying out vacuum melting on the aluminum-molybdenum primary alloy, the aluminum-vanadium primary alloy and aluminum, and cooling to obtain the aluminum-molybdenum-vanadium intermediate alloy;
the step (1) and the step (2) have no time sequence limitation.
Preferably, the mass ratio of the aluminum to the molybdenum trioxide in the step (1) is (0.0934-1.061): (1.815-2.012); the aluminum and molybdenum trioxide are dried prior to mixing; the drying temperature is 100-120 ℃, and the drying time is more than 6 hours.
Preferably, the temperature of the aluminothermic reaction in the step (1) is 1650-1750 ℃ and the time is 33-42 s.
Preferably, the mass ratio of the aluminum to the vanadium pentoxide in the step (2) is (0.945-1.063): (1.586-1.755); drying the aluminum and the vanadium pentoxide before mixing; the drying temperature is 100-120 ℃, and the drying time is more than 6 hours.
Preferably, the temperature of the aluminothermic reaction in the step (2) is 1750-1850 ℃ and the time is 21-35 s.
Preferably, the vacuum degree of vacuum melting in the step (3) is less than 10 Pa.
Preferably, the vacuum melting in the step (3) comprises melting and refining which are sequentially performed; the temperature of the refining process is 1950-2000 ℃, and the time is 5-10 min.
The invention provides an aluminum-molybdenum-vanadium intermediate alloy which comprises, by mass, 17.0-22.0% of Al, 40.0-42.0% of Mo and 38.0-41.0% of V. The invention ensures that the aluminum-molybdenum-vanadium intermediate alloy has smaller component segregation by controlling the components and the content, is beneficial to homogenizing the components of the titanium alloy when the titanium alloy is smelted, prevents the component segregation, optimizes the batching procedure when the titanium alloy is smelted, and can realize accurate batching in the production process.
The invention provides a preparation method of the aluminum-molybdenum-vanadium intermediate alloy. The preparation method provided by the invention can improve the uniform stability of the components of the aluminum-molybdenum-vanadium intermediate alloy, reduce the content of O, N and other impurities, has a simple process, is easy to control, and is suitable for large-scale industrial production.
Detailed Description
The invention provides an aluminum-molybdenum-vanadium intermediate alloy which comprises, by mass, 17.0-22.0% of Al, 40.0-42.0% of Mo and 38.0-41.0% of V; preferably, the alloy comprises 18.0-21.0% of Al, 41.0-42.0% of Mo and 39.0-41.0% of V; more preferably, it includes 19.0% of Al, 41.0% of Mo, and 40.0% of V.
The invention ensures that the aluminum-molybdenum-vanadium intermediate alloy has smaller component segregation by controlling the components and the content, is beneficial to homogenizing the components of the titanium alloy when the titanium alloy is smelted, prevents the component segregation, optimizes the batching procedure when the titanium alloy is smelted, can realize accurate batching in the production process and is convenient for preparing the titanium alloy.
The invention provides a preparation method of the aluminum-molybdenum-vanadium intermediate alloy, which comprises the following steps:
(1) mixing aluminum and molybdenum trioxide to carry out aluminothermic reaction, and cooling to obtain an aluminum-molybdenum primary alloy;
(2) mixing aluminum and vanadium pentoxide, carrying out aluminothermic reaction, and cooling to obtain an aluminum-vanadium primary alloy;
(3) carrying out vacuum melting on the aluminum-molybdenum primary alloy, the aluminum-vanadium primary alloy and aluminum, and cooling to obtain the aluminum-molybdenum-vanadium intermediate alloy;
the step (1) and the step (2) have no time sequence limitation.
The invention mixes aluminum and molybdenum trioxide to carry out aluminothermic reaction, and obtains the aluminum-molybdenum primary alloy after cooling. In the invention, the mass ratio of the aluminum to the molybdenum trioxide is preferably (0.0934-1.061): 1.815-2.012, more preferably (0.095-1): 1.9-2, and most preferably 1: 1.97. The mass ratio of aluminum to molybdenum in the aluminum-molybdenum primary alloy is controlled by controlling the mass ratio of aluminum to molybdenum trioxide, for example, in the specific embodiment of the invention, the mass ratio of aluminum to molybdenum trioxide is set to be 1:1.97, and the aluminum-molybdenum 80 primary alloy (i.e. the mass percentage of molybdenum is 80%) is obtained after aluminothermic reaction. In the present invention, the aluminum and molybdenum trioxide are preferably in a powdery form. In the present invention, the aluminum and molybdenum trioxide are preferably dried before mixing; the drying temperature is preferably 100-120 ℃, more preferably 110 ℃, and the time is preferably more than 6 hours, more preferably 12 hours. In the invention, the drying can remove water in the aluminum and the molybdenum trioxide, and prevent the hydrogen evolution phenomenon in the smelting process. The method for mixing the aluminum and the molybdenum trioxide does not have special requirements, and the method well known in the field is adopted to ensure that the aluminum and the molybdenum trioxide are uniformly mixed; in a particular embodiment of the invention, the mixing is preferably carried out in a V-blender; the mixing speed of the mixer is preferably 100-140 r/min, more preferably 110-130 r/min, and the mixing time is preferably 4 min. The invention makes aluminum and molybdenum trioxide fully contact by mixing, thereby facilitating the aluminothermic reaction.
Aluminum and molybdenum trioxide are mixed and then subjected to aluminothermic reaction. The invention preferably ignites the mixed aluminum and molybdenum trioxide to initiate aluminothermic reaction; the present invention does not require any particular operation for said ignition, as long as the ignition means known in the art for initiating thermite reactions are used. In the invention, the thermite reaction temperature is preferably 1650-1750 ℃, more preferably 1680-1720 ℃, and the time is preferably 33-42 s, more preferably 35-40 s. The invention has no special requirement on the reaction device of the thermite reaction, and can adopt a thermite reaction device well known in the field; in the specific embodiment of the present invention, the aluminothermic reaction is preferably performed in a smelting furnace, and the furnace body of the smelting furnace is preferably a furnace body built by magnesia bricks, a furnace body sintered by alumina, or a furnace body built by graphite plates. In the invention, in the thermite reaction process, aluminum is used as a reducing agent to reduce molybdenum trioxide into metal simple substance molybdenum, aluminum is oxidized into aluminum oxide, and a large amount of heat energy is released to melt metals (metal simple substance molybdenum and excessive aluminum) to form aluminum-molybdenum alloy liquid; the alumina formed by oxidizing the aluminum floats on the surface of the alloy liquid, and is separated from the alloy liquid and removed. After the aluminothermic reaction obtains the aluminum-molybdenum alloy liquid, the invention cools the aluminum-molybdenum alloy liquid. In the present invention, the cooling is preferably furnace cooling; and cooling and discharging to obtain the aluminum-molybdenum primary alloy.
The invention mixes aluminum and vanadium pentoxide to carry out aluminothermic reaction, and obtains the aluminum-vanadium primary alloy after cooling. In the invention, the mass ratio of the aluminum to the vanadium pentoxide is preferably (0.945-1.063): (1.586-1.755), more preferably (0.98-1.05): 1.6-1.7), and most preferably 1: 1.69. The mass ratio of aluminum to vanadium in the aluminum-vanadium primary alloy is controlled by controlling the mass ratio of aluminum to vanadium pentoxide, for example, in the specific embodiment of the invention, the mass ratio of aluminum to vanadium pentoxide is set to 1:1.69, and the aluminum-vanadium 85 primary alloy (i.e., the mass percentage of vanadium is 85%) is obtained by aluminothermic reaction. In the present invention, the aluminum and vanadium pentoxide are preferably in a powdery form. In the present invention, the aluminum and vanadium pentoxide are preferably dried before mixing; the drying temperature is preferably 100-120 ℃, more preferably 110 ℃, and the time is preferably more than 6 hours, more preferably 12 hours. In the invention, the drying can remove water in the aluminum and the molybdenum trioxide, and prevent the hydrogen evolution phenomenon in the smelting process. In the present invention, the method for mixing aluminum and vanadium pentoxide is the same as the above scheme (mixing aluminum and molybdenum trioxide), and is not described herein again. The invention makes the aluminum and the vanadium pentoxide fully contact by mixing, thereby facilitating the aluminothermic reaction.
And mixing aluminum and vanadium pentoxide and then carrying out aluminothermic reaction. In the invention, the temperature of the thermite reaction is preferably 1750-1850 ℃, more preferably 1780-1830 ℃, and the time is preferably 21-35 s, more preferably 25-30 s. In the present invention, the operation and apparatus for aluminothermic reaction of aluminum and vanadium pentoxide are the same as the above scheme (aluminothermic reaction of aluminum and molybdenum trioxide), and are not described herein again. In the invention, in the aluminothermic reaction process, aluminum is used as a reducing agent to reduce vanadium pentoxide into metal simple substance vanadium, aluminum is oxidized into aluminum oxide, and a large amount of heat energy is released to melt metals (metal simple substance vanadium and excessive aluminum) to form an aluminum-vanadium alloy liquid; the alumina formed by oxidizing the aluminum floats on the surface of the alloy liquid, and is separated from the alloy liquid and removed. After the aluminothermic reaction obtains the aluminum-vanadium alloy liquid, the invention cools the alloy liquid. In the present invention, the cooling is preferably furnace cooling; and cooling and discharging to obtain the aluminum-vanadium primary alloy.
After the aluminum-molybdenum primary alloy and the aluminum-vanadium primary alloy are obtained, the aluminum-molybdenum primary alloy, the aluminum-vanadium primary alloy and aluminum are subjected to vacuum melting, and the aluminum-molybdenum-vanadium intermediate alloy is obtained after cooling. Before vacuum smelting, the invention preferably carries out finishing crushing and component analysis on the aluminum-molybdenum primary alloy and the aluminum-vanadium primary alloy in sequence; the method of the present invention for the size reduction and the composition analysis is not particularly required, and the corresponding method well known in the art may be employed. In the invention, the adding amount of the aluminum, the aluminum-molybdenum primary alloy and the aluminum-vanadium primary alloy in the vacuum melting is determined according to the analysis result of the components of the aluminum-molybdenum primary alloy and the aluminum-vanadium primary alloy and the mass content of each metal element in the needed aluminum-molybdenum-vanadium intermediate alloy; in a particular embodiment of the invention, the aluminum is preferably added in the form of aluminum beans. In the present invention, the vacuum melting is preferably performed in a medium frequency vacuum induction furnace; the vacuum degree of the vacuum melting is preferably less than 10 Pa; the vacuum melting is preferably carried out under a protective atmosphere, which is preferably argon. In the present invention, the vacuum melting preferably includes melting and refining which are performed sequentially. In the present invention, the melting is particularly preferably: adjusting the power of the medium-frequency vacuum induction furnace to the initial power to start heating, and then increasing the power to the transition power to heat until metal starts to melt; and then the power is increased to the stable power and heated until the metal is completely melted, and a mixed melt is obtained. In the invention, the initial power is preferably 20-25 kW, and more preferably 20-22 kW; the transition power is preferably 50-70 kW, and more preferably 58-70 kW; the stable power is preferably 88-100 kW, and more preferably 92-100 kW. After the aluminum-molybdenum primary alloy, the aluminum-vanadium primary alloy and the aluminum are melted, the mixed melt is refined. In the invention, the refining temperature is preferably 1950-2000 ℃, more preferably 1960-1980 ℃, and the time is preferably 5-10 min, more preferably 6-8 min. In the refining process, the power of the medium-frequency vacuum induction furnace is preferably 92-100 kW, and more preferably 100 kW. In the invention, the refining can remove impurities and gases in the mixed melt to obtain pure alloy liquid.
After vacuum melting, the alloy liquid obtained is cooled. In the present invention, the cooling is preferably furnace cooling after casting; the invention has no special requirements on the casting operation, and the casting method well known in the field can be adopted; the cooling termination temperature is preferably 150 ℃ or lower. And discharging after cooling to obtain the aluminum-molybdenum-vanadium intermediate alloy.
The invention provides a preparation method of the aluminum-molybdenum-vanadium intermediate alloy. The preparation method provided by the invention can improve the uniform stability of the components of the aluminum-molybdenum-vanadium intermediate alloy, reduce the content of O, N and other impurities, has a simple process, is easy to control, and is suitable for large-scale industrial production.
The aluminum-molybdenum-vanadium master alloy and the preparation method thereof provided by the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
First, aluminothermic smelting process
(1) And drying the aluminum powder, the molybdenum trioxide and the vanadium pentoxide at the drying temperature of 110 ℃ for 12 hours.
(2) Calculating the mass ratio of the alloy in the aluminothermic smelting process: the ratio of aluminum powder to molybdenum trioxide is 1: 1.97; the ratio of aluminum powder to vanadium pentoxide is 1: 1.69.
(3) respectively loading aluminum powder and molybdenum trioxide, and aluminum powder and vanadium pentoxide into a mixer to mix for 4min at a speed of 120r/min, wherein the mixing requirement is as follows: all raw materials must be fully and uniformly mixed to ensure the full contact between the raw materials.
(4) Respectively preheating the mixed aluminum powder and molybdenum trioxide, aluminum powder and vanadium pentoxide to a charging temperature of 43 ℃, igniting and smelting, and discharging after 24 hours to obtain the aluminum-molybdenum 80 primary alloy and the aluminum-vanadium 85 primary alloy.
Proportioning in vacuum smelting process
After obtaining the aluminum-molybdenum 80 primary alloy and the aluminum-vanadium 85 primary alloy, finishing and crushing the alloys, and calculating the proportion in the smelting process after analyzing the components: 2.30kg of aluminum beans, 29.46kg of aluminum-molybdenum 80 primary alloy and 28.24kg of aluminum-vanadium 85 primary alloy.
Preparation before power transmission of medium-frequency vacuum induction furnace
(1) And (4) starting a circulating water pump, checking whether the pipeline has leakage, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper.
(2) And (5) checking whether the power system is normal or not, and if the power system is abnormal, timely maintaining.
(3) And if the transparent condition of the glass of the observation hole is determined to be poor, the cover needs to be opened for wiping or is polished by sand paper, and after the observation hole is installed back, the position-adjusting hand button is twisted, the position adjustment needs to be flexible, and the gland is sealed well.
Fourthly, smelting
(1) Vacuumizing, starting the mechanical pump and the Roots pump, and keeping for 15 minutes. When the reading of the vacuum display is less than 10Pa, stopping vacuumizing and starting power transmission heating smelting;
(2) power is transmitted, and the initial power is 20 kW;
(3) after 20 minutes, the power is adjusted to 60 kW;
(4) after the alloy is melted, the power is adjusted to 90 kW;
(5) after the alloy is melted down, the power is properly increased to 100kW, refining is carried out for 8 minutes at the temperature of 1980 ℃, the smelting furnace is vacuumized to 10Pa again, gas impurities in the melt are removed, and casting is carried out.
Fifthly, cooling for 150 minutes and discharging to obtain the aluminum-molybdenum-vanadium intermediate alloy
During the smelting process it was observed that: the alloy becomes dark red and slowly melts, and the alloy liquid brightens and becomes clear.
One position of the Al-Mo-V intermediate alloy ingot (cylinder) prepared in this example was sampled for chemical composition analysis, and the results are shown in Table 1. As can be seen from table 1, the content of the aluminum molybdenum vanadium master alloy C, O, N impurity prepared in this example is low, and Fe and Si are inevitable impurities introduced by the raw materials.
The Al-Mo-V intermediate alloy ingot (cylinder) prepared in this example was sampled at different positions and analyzed for chemical components, two points, numbered 1 and 2 respectively, were taken from the upper surface of the ingot, two points, numbered 3 and 4 respectively, were taken from the lower surface of the ingot, and two points, numbered 5 and 6 respectively, were taken from the middle of the ingot to analyze the components, and the results are shown in Table 2. As can be seen from Table 2, the Al-Mo-V master alloy prepared in this example has uniform and stable components and no segregation.
Example 2
First, aluminothermic smelting process
(1) And drying the aluminum powder, the molybdenum trioxide and the vanadium pentoxide at the drying temperature of 110 ℃ for 12 hours.
(2) Calculating the mass ratio of the alloy in the aluminothermic smelting process: the ratio of aluminum powder to molybdenum trioxide is 1: 1.97; the ratio of aluminum powder to vanadium pentoxide is 1: 1.69.
(3) respectively loading aluminum powder and molybdenum trioxide, and aluminum powder and vanadium pentoxide into a mixer to mix for 4min at a speed of 120r/min, wherein the mixing requirement is as follows: all raw materials must be fully and uniformly mixed to ensure the full contact between the raw materials.
(4) Respectively preheating the mixed aluminum powder and molybdenum trioxide, aluminum powder and vanadium pentoxide to a charging temperature of 43 ℃, igniting and smelting, and discharging after 24 hours to obtain the aluminum-molybdenum 80 primary alloy and the aluminum-vanadium 85 primary alloy.
Proportioning in vacuum smelting process
After the aluminum-molybdenum 80 primary alloy and the aluminum-vanadium 85 primary alloy are obtained, the alloys are finished and crushed, and the proportion in the smelting process is calculated after the components are analyzed: 0.52kg of aluminum beans, 30.54kg of aluminum molybdenum 80 primary alloy and 28.94kg of aluminum vanadium 85 primary alloy.
Preparation before power transmission of medium-frequency vacuum induction furnace
(1) And (4) starting a circulating water pump, checking whether the pipeline has leakage, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper.
(2) And (5) checking whether the power system is normal or not, and if the power system is abnormal, timely maintaining.
(3) And if the transparent condition of the glass of the observation hole is determined to be poor, the cover needs to be opened for wiping or is polished by sand paper, and after the observation hole is installed back, the position-adjusting hand button is twisted, the position adjustment needs to be flexible, and the gland is sealed well.
Fourthly, smelting
(1) Vacuumizing, starting the mechanical pump and the Roots pump, and keeping for 15 minutes. When the reading of the vacuum display is less than 10Pa, stopping vacuumizing and starting power transmission heating smelting;
(2) power is transmitted, and the initial power is 20 kW;
(3) after 20 minutes, the power is adjusted to 60 kW;
(4) after the alloy is melted, the power is adjusted to 90 kW;
(5) after the alloy is melted down, the power is properly increased to 100kW, refining is carried out for 10 minutes at 1950 ℃, the smelting furnace is vacuumized again to 10Pa, gas impurities in the melt are removed, and casting is carried out.
Fifthly, cooling for 150 minutes and discharging to obtain the aluminum-molybdenum-vanadium intermediate alloy
During the smelting process it was observed that: the alloy becomes dark red and slowly melts, and the alloy liquid brightens and becomes clear.
The Al-Mo-V master alloy ingot (cylinder) prepared in this example was sampled at one position (same as the sampling position in example 1) for chemical composition analysis, and the results are shown in Table 1.
The Al-Mo-V master alloy ingot (cylinder) prepared in this example was sampled at different positions for chemical composition analysis by the method of example 1, and the results are shown in FIG. 3. As can be seen from Table 3, the Al-Mo-V master alloy prepared by the present embodiment has uniform and stable components and no segregation.
Example 3
First, aluminothermic smelting process
(1) And drying the aluminum powder, the molybdenum trioxide and the vanadium pentoxide at the drying temperature of 110 ℃ for 12 hours.
(2) Calculating the mass ratio of the alloy in the aluminothermic smelting process: the ratio of aluminum powder to molybdenum trioxide is 1: 1.97; the ratio of aluminum powder to vanadium pentoxide is 1: 1.69.
(3) respectively loading aluminum powder and molybdenum trioxide, and aluminum powder and vanadium pentoxide into a mixer to mix for 4min at a speed of 120r/min, wherein the mixing requirement is as follows: all raw materials must be fully and uniformly mixed to ensure the full contact between the raw materials.
(4) Respectively preheating the mixed aluminum powder and molybdenum trioxide, aluminum powder and vanadium pentoxide to a charging temperature of 43 ℃, igniting and smelting, and discharging after 24 hours to obtain the aluminum-molybdenum 80 primary alloy and the aluminum-vanadium 85 primary alloy.
Proportioning in vacuum smelting process
After obtaining the aluminum-molybdenum 80 primary alloy and the aluminum-vanadium 85 primary alloy, finishing and crushing the alloys, and calculating the proportion in the smelting process after analyzing the components: 4.43kg of aluminum beans, 28.74kg of aluminum molybdenum 80 primary alloy and 26.82kg of aluminum vanadium 85 primary alloy.
Preparation before power transmission of medium-frequency vacuum induction furnace
(1) And (4) starting a circulating water pump, checking whether the pipeline has leakage, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper.
(2) And (5) checking whether the power system is normal or not, and if the power system is abnormal, timely maintaining.
(3) And if the transparent condition of the glass of the observation hole is determined to be poor, the cover needs to be opened for wiping or is polished by sand paper, and after the observation hole is installed back, the position-adjusting hand button is twisted, the position adjustment needs to be flexible, and the gland is sealed well.
Fourthly, smelting
(1) Vacuumizing, starting the mechanical pump and the Roots pump, and keeping for 15 minutes. When the reading of the vacuum display is less than 10Pa, stopping vacuumizing and starting power transmission heating smelting;
(2) power is transmitted, and the initial power is 20 kW;
(3) after 20 minutes, the power is adjusted to 60 kW;
(4) after the alloy is melted, the power is adjusted to 90 kW;
(5) after the alloy is melted down, the power is properly increased to 100kW, the refining is carried out for 5 minutes at 2000 ℃, the smelting furnace is vacuumized to 10Pa again, the gas impurities in the melt are removed, and the casting is carried out.
Fifthly, cooling for 150 minutes and discharging to obtain the aluminum-molybdenum-vanadium intermediate alloy
During the smelting process it was observed that: the alloy becomes dark red and slowly melts, and the alloy liquid brightens and becomes clear.
The Al-Mo-V master alloy ingot (cylinder) prepared in this example was sampled at one position (same as the sampling position in example 1) for chemical composition analysis, and the results are shown in Table 1.
The Al-Mo-V master alloy ingot (cylinder) prepared in this example was sampled at different positions for chemical composition analysis by the method of example 1, and the results are shown in FIG. 4. As can be seen from Table 4, the Al-Mo-V master alloy prepared by the present embodiment has uniform and stable components and no segregation.
Example 4
First, aluminothermic smelting process
(1) And drying the aluminum powder, the molybdenum trioxide and the vanadium pentoxide at the drying temperature of 110 ℃ for 12 hours.
(2) Calculating the mass ratio of the alloy in the aluminothermic smelting process: the ratio of aluminum powder to molybdenum trioxide is 1: 1.97; the ratio of aluminum powder to vanadium pentoxide is 1: 1.69.
(3) respectively loading aluminum powder and molybdenum trioxide, and aluminum powder and vanadium pentoxide into a mixer to mix for 4min at a speed of 120r/min, wherein the mixing requirement is as follows: all raw materials must be fully and uniformly mixed to ensure the full contact between the raw materials.
(4) And respectively preheating the mixed aluminum powder and molybdenum trioxide, aluminum powder and vanadium pentoxide to a charging temperature of 43 ℃, igniting and smelting, and discharging after 24 hours to obtain the primary alloy of aluminum and molybdenum 80 and the primary alloy of aluminum and vanadium 85.
Proportioning in vacuum smelting process
After an alloy of 80 grade of aluminum and molybdenum and 85 grade of aluminum and vanadium is obtained, the alloy is finely finished and crushed, and the proportion in the smelting process is calculated after the components are analyzed: 6.41kg of aluminum beans, 29.46kg of aluminum-molybdenum 80 primary alloy and 28.94kg of aluminum-vanadium 85 primary alloy.
Preparation before power transmission of medium-frequency vacuum induction furnace
(1) And (4) starting a circulating water pump, checking whether the pipeline has leakage, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper.
(2) And (5) checking whether the power system is normal or not, and if the power system is abnormal, timely maintaining.
(3) And if the transparent condition of the glass of the observation hole is determined to be poor, the cover needs to be opened for wiping or is polished by sand paper, and after the observation hole is installed back, the position-adjusting hand button is twisted, the position adjustment needs to be flexible, and the gland is sealed well.
Fourthly, smelting
(1) Vacuumizing, starting the mechanical pump and the Roots pump, and keeping for 15 minutes. When the reading of the vacuum display is less than 10Pa, stopping vacuumizing and starting power transmission heating smelting;
(2) power is transmitted, and the initial power is 20 kW;
(3) after 20 minutes, the power is adjusted to 60 kW;
(4) after the alloy is melted, the power is adjusted to 90 kW;
(5) after the alloy is melted down, the power is properly increased to 100kW, the refining is carried out for 9 minutes at the temperature of 1960 ℃, the smelting furnace is vacuumized to 10Pa again, the gas impurities in the melt are removed, and the casting is carried out.
Fifthly, cooling for 150 minutes and discharging to obtain the aluminum-molybdenum-vanadium intermediate alloy
During the smelting process it was observed that: the alloy becomes dark red and slowly melts, and the alloy liquid brightens and becomes clear.
The chemical composition analysis of the aluminum molybdenum vanadium master alloy prepared in this example was performed, and the results are shown in table 1.
The Al-Mo-V master alloy ingot (cylinder) prepared in this example was sampled at different positions for chemical composition analysis by the method of example 1, and the results are shown in FIG. 5. As can be seen from Table 5, the Al-Mo-V master alloy prepared in this example has uniform and stable components and no segregation.
Example 5
First, aluminothermic smelting process
(1) And drying the aluminum powder, the molybdenum trioxide and the vanadium pentoxide at the drying temperature of 110 ℃ for 12 hours.
(2) Calculating the mass ratio of the alloy in the aluminothermic smelting process: the ratio of aluminum powder to molybdenum trioxide is 1: 1.97; the ratio of aluminum powder to vanadium pentoxide is 1: 1.69.
(3) respectively loading aluminum powder and molybdenum trioxide, and aluminum powder and vanadium pentoxide into a mixer to mix for 4min at a speed of 120r/min, wherein the mixing requirement is as follows: all raw materials must be fully and uniformly mixed to ensure the full contact between the raw materials.
(4) Respectively preheating the mixed aluminum powder and molybdenum trioxide, aluminum powder and vanadium pentoxide to a charging temperature of 43 ℃, igniting and smelting, and discharging after 24 hours to obtain the aluminum-molybdenum 80 primary alloy and the aluminum-vanadium 85 primary alloy.
Proportioning in vacuum smelting process
After obtaining the aluminum-molybdenum 80 primary alloy and the aluminum-vanadium 85 primary alloy, finishing and crushing the alloys, and calculating the proportion in the smelting process after analyzing the components: 3.72kg of aluminum beans, 29.46kg of aluminum molybdenum 80 primary alloy and 26.82kg of aluminum vanadium 85 primary alloy.
Preparation before power transmission of medium-frequency vacuum induction furnace
(1) And (4) starting a circulating water pump, checking whether the pipeline has leakage, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper.
(2) And (5) checking whether the power system is normal or not, and if the power system is abnormal, timely maintaining.
(3) And if the transparent condition of the glass of the observation hole is determined to be poor, the cover needs to be opened for wiping or is polished by sand paper, and after the observation hole is installed back, the position-adjusting hand button is twisted, the position adjustment needs to be flexible, and the gland is sealed well.
Fourthly, smelting
(1) Vacuumizing, starting the mechanical pump and the Roots pump, and keeping for 15 minutes. When the reading of the vacuum display is less than 10Pa, stopping vacuumizing and starting power transmission heating smelting;
(2) power is transmitted, and the initial power is 20 kW;
(3) after 20 minutes, the power is adjusted to 60 kW;
(4) after the alloy is melted, the power is adjusted to 90 kW;
(5) after the alloy is melted down, the power is properly increased to 100kW, the refining is carried out for 7 minutes at 1990 ℃, the smelting furnace is vacuumized to 10Pa again, the gas impurities in the melt are removed, and the casting is carried out.
Fifthly, cooling for 150 minutes and discharging to obtain the aluminum-molybdenum-vanadium intermediate alloy
During the smelting process it was observed that: the alloy becomes dark red and slowly melts, and the alloy liquid brightens and becomes clear.
The Al-Mo-V master alloy ingot (cylinder) prepared in this example was sampled at one position (same as the sampling position in example 1) for chemical composition analysis, and the results are shown in Table 1.
The Al-Mo-V master alloy ingot (cylinder) prepared in this example was sampled at different positions for chemical composition analysis by the method of example 1, and the results are shown in FIG. 6. As can be seen from Table 6, the Al-Mo-V master alloy prepared in this example has uniform and stable components and no segregation.
TABLE 1 examples 1-5 chemical compositions of Al-Mo-V master alloys
TABLE 2 EXAMPLE 1 chemical composition of different sites of Al-Mo-V master alloy
TABLE 3 EXAMPLE 2 chemical composition of different sites of Al-Mo-V master alloy
Table 4 example 3 chemical composition of different sites of aluminum molybdenum vanadium master alloy
TABLE 5 EXAMPLE 4 chemical composition of different sites of Al-Mo-V master alloy
TABLE 6 EXAMPLE 5 chemical composition of different sites of Al-Mo-V master alloy
The embodiment shows that the aluminum-molybdenum-vanadium intermediate alloy provided by the invention has uniform and stable components and low impurity content, so that the aluminum-molybdenum-vanadium intermediate alloy is beneficial to the homogenization of titanium alloy components, prevents component segregation, optimizes the batching process during titanium alloy smelting and can realize accurate batching in the production process when being used as a raw material for producing titanium alloy. In addition, the preparation method provided by the invention is simple, easy to operate, free of special equipment, low in cost, stable in smelting process and good in alloy forming state, and aluminum and various oxides are used as raw materials.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. An Al-Mo-V intermediate alloy is characterized by comprising 18.0-21.0% of Al, 41.0-42.0% of Mo and 39.0-41.0% of V by mass;
the preparation method of the aluminum-molybdenum-vanadium intermediate alloy comprises the following steps:
(1) mixing aluminum and molybdenum trioxide to carry out aluminothermic reaction, and cooling to obtain an aluminum-molybdenum primary alloy;
(2) mixing aluminum and vanadium pentoxide, carrying out aluminothermic reaction, and cooling to obtain an aluminum-vanadium primary alloy;
(3) carrying out vacuum melting on the aluminum-molybdenum primary alloy, the aluminum-vanadium primary alloy and aluminum, and cooling to obtain the aluminum-molybdenum-vanadium intermediate alloy;
the step (1) and the step (2) have no time sequence limitation;
the mass ratio of the aluminum to the molybdenum trioxide in the step (1) is (0.0934-1.061): 1.815-2.012; the aluminum and molybdenum trioxide are dried prior to mixing; the drying temperature is 100-120 ℃, and the drying time is more than 6 hours;
the mass ratio of the aluminum to the vanadium pentoxide in the step (2) is (0.945-1.063): 1.586-1.755); drying the aluminum and the vanadium pentoxide before mixing; the drying temperature is 100-120 ℃, and the drying time is more than 6 hours.
2. The Al-Mo-V master alloy according to claim 1, which comprises, by mass, 19.0% Al, 41.0% Mo, 40.0% V.
3. The method for preparing the aluminum-molybdenum-vanadium intermediate alloy as claimed in any one of claims 1 to 2, which is characterized by comprising the following steps:
(1) mixing aluminum and molybdenum trioxide to carry out aluminothermic reaction, and cooling to obtain an aluminum-molybdenum primary alloy;
(2) mixing aluminum and vanadium pentoxide, carrying out aluminothermic reaction, and cooling to obtain an aluminum-vanadium primary alloy;
(3) carrying out vacuum melting on the aluminum-molybdenum primary alloy, the aluminum-vanadium primary alloy and aluminum, and cooling to obtain the aluminum-molybdenum-vanadium intermediate alloy;
the step (1) and the step (2) have no time sequence limitation;
the mass ratio of the aluminum to the molybdenum trioxide in the step (1) is (0.0934-1.061): 1.815-2.012; the aluminum and molybdenum trioxide are dried prior to mixing; the drying temperature is 100-120 ℃, and the drying time is more than 6 hours;
the mass ratio of the aluminum to the vanadium pentoxide in the step (2) is (0.945-1.063): 1.586-1.755); drying the aluminum and the vanadium pentoxide before mixing; the drying temperature is 100-120 ℃, and the drying time is more than 6 hours.
4. The preparation method according to claim 3, wherein the aluminothermic reaction in the step (1) is carried out at 1650-1750 ℃ for 33-42 s.
5. The preparation method according to claim 3, wherein the temperature of the aluminothermic reaction in the step (2) is 1750-1850 ℃ for 21-35 s.
6. The production method according to claim 3, wherein the vacuum degree of the vacuum melting in the step (3) is less than 10 Pa.
7. The production method according to claim 3 or 6, wherein the vacuum melting in the step (3) includes melting and refining which are performed sequentially; the refining temperature is 1950-2000 ℃, and the refining time is 5-10 min.
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