CN113584353A - Aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy and preparation method thereof - Google Patents
Aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy which comprises the following components in percentage by mass: 25.0-27.0% of molybdenum, 24.0-27.0% of vanadium, 12.0-16.0% of chromium, 6.0-11.0% of titanium, the balance of aluminum and inevitable impurities; the preparation method comprises the following steps: (1) mixing a molybdenum source and a first aluminum source, mixing a vanadium source and a second aluminum source, and respectively carrying out aluminothermic reaction to obtain an aluminum-molybdenum alloy and an aluminum-vanadium alloy; (2) mixing an aluminum-molybdenum alloy, an aluminum-vanadium alloy, metal chromium, a titanium source and a third aluminum source, and carrying out vacuum induction melting to obtain an aluminum-molybdenum-vanadium-chromium-titanium alloy liquid; (3) and cooling the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid to obtain the aluminum-molybdenum-vanadium-chromium-titanium alloy. The invention controls the components and the content to ensure that the aluminum-molybdenum-vanadium-chromium-titanium master alloy has uniform components and small segregation, and is beneficial to the homogenization of the components of the titanium alloy and the prevention of component segregation when the titanium alloy is smelted.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to an aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy and a preparation method thereof.
Background
Titanium and its alloy have excellent performance, such as corrosion resistance, high temperature resistance, low temperature resistance, high strength, non-magnetism, etc., have good comprehensive properties of the process at the same time, become irreplaceable materials gradually in the field of modern industrial science and technology, have extensive application in the fields of aerospace industry, ship manufacturing industry, chemical industry, electric power industry, metallurgy industry, textile industry, food industry, medical industry, vehicle manufacturing industry and sports and leisure industry, etc.
Titanium alloy develops from the last 50 years to the present, from the first 3 elements of Ti-6Al-4V to the present 6-8 elements, the types of alloy elements are gradually increased, and the component proportion of the alloy tends to be reasonable. The alloying of different elements changes the phase transition temperature of heat treatment, and the change of the structure causes the change of the alloy performance; various elements in the alloy interact with each other, so that the comprehensive performance of the titanium alloy is better and better, and the requirement of aerospace development is gradually met. At present, the titanium alloy grades mainly used are TB2, TB9, TB15 and TB16, the titanium alloy is widely used, for example, the TB2 titanium alloy has the nominal component of Ti-5Mo-5V-8Cr-3Al, and is suitable for manufacturing aviation fasteners working below 300 ℃ and aerospace fasteners working at the temperature below 500 ℃ in a short time.
The aluminum is the most widely used stable element in titanium alloy, almost all titanium alloys contain the aluminum element, the aluminum is the most main strengthening element in the titanium alloy, the aluminum has obvious solid solution strengthening effect, the high-temperature mechanical property of the titanium can be obviously improved, the aluminum is the main alloy element which is firstly used for developing the heat-strength titanium alloy, and the aluminum also has lower density and is beneficial to improving the specific strength of the titanium alloy. Molybdenum is an alloy element widely applied to titanium alloy, has a remarkable solid solution strengthening effect, and can maintain good plasticity and improve the thermal stability of the titanium alloy while improving the strength of the alloy. Vanadium is a metal element in the titanium alloy, and the addition of vanadium increases the oxidation resistance of the alloy at high temperature, thereby being beneficial to improving the oxidation resistance of the alloy. Chromium elements impart high strength and good plasticity to the titanium alloy.
When the titanium alloy is smelted, if aluminum elements with low melting points and refractory elements with high melting points, such as molybdenum and vanadium, are added in a pure metal form, great quality hidden troubles exist, segregation and inclusion metallurgical defects of titanium alloy ingots are easily caused, and the aluminum elements and the refractory elements need to be added in an intermediate alloy form. With the continuous development of the titanium alloy industry, more and more metals are added into the titanium alloy in the form of the intermediate alloy, the trouble of respectively adding metal simple substances is avoided, the melting point of the intermediate alloy is lower than the highest melting point of the metal simple substances in the intermediate alloy, the titanium alloy can be ensured to be more stable in the smelting process, and the situation that the smelting process is not easy to control due to the fact that the melting points of the added metal simple substances are inconsistent is better avoided.
Therefore, how to develop an aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy to improve the comprehensive performance of the titanium alloy is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the present invention provides an aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy and a preparation method thereof, so as to solve the above problems in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
an aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy comprises the following components in percentage by mass: 25.0-27.0% of molybdenum, 24.0-27.0% of vanadium, 12.0-16.0% of chromium, 6.0-11.0% of titanium, the balance of aluminum and inevitable impurities;
preferably: 25.5 to 26.5 percent of molybdenum, 24.5 to 26.5 percent of vanadium, 12.5 to 15.5 percent of chromium, 6.5 to 10.0 percent of titanium, the balance of aluminum and inevitable impurities;
more preferably: 26.0% of molybdenum, 25.0% of vanadium, 14.0% of chromium, 9.0% of titanium, the balance of aluminum and inevitable impurities.
The invention has the beneficial effects that: by adding molybdenum, the room temperature and high temperature strength of the titanium alloy can be improved, the hardenability is increased, and the thermal stability of the alloy containing chromium and iron is improved; by adding vanadium, the oxidation resistance of the titanium alloy at high temperature is increased, and the oxidation resistance of the alloy is favorably improved; by adding chromium, the titanium alloy has high strength and good plasticity; by adding titanium, the melting point difference and the density difference between other elements and the titanium are neutralized, so that the element burning loss is less, the melting is sufficient, and the segregation is less when the titanium alloy is smelted by the intermediate alloy; by adding aluminum, the room temperature and high temperature strength and heat resistance of the titanium alloy can be improved.
The components are prepared into the master alloy by controlling the components and the content, the melting point difference and the density difference among the elements are neutralized, and the density and the melting point of the master alloy are closer to the density and the melting point of titanium; the problems of element burning loss caused by the difference of melting points, uneven components caused by the difference of densities and the like in the titanium alloy smelting process are solved, the components of the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy are uniform and have small segregation, and the titanium alloy smelting process is beneficial to the homogenization of the components of the titanium alloy and the prevention of component segregation.
A preparation method of an aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy specifically comprises the following steps:
(1) mixing a molybdenum source and a first aluminum source, and carrying out a first aluminothermic reaction to obtain an aluminum-molybdenum alloy; mixing a vanadium source and a second aluminum source, and carrying out a second aluminothermic reaction to obtain an aluminum-vanadium alloy;
(2) mixing an aluminum-molybdenum alloy, an aluminum-vanadium alloy, metal chromium, a titanium source and a third aluminum source, and carrying out vacuum induction melting to obtain an aluminum-molybdenum-vanadium-chromium-titanium alloy liquid;
(3) and cooling the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid to obtain the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy.
The invention has the beneficial effects that: in the vacuum induction smelting process, the aluminum-molybdenum alloy and the aluminum-vanadium alloy are used as matrixes, and the chromium metal, the titanium sponge and the third aluminum source are added to adjust the components of the alloy, so that the components of the target alloy are more stable; meanwhile, a good smelting environment is provided for the aluminum-molybdenum alloy and the aluminum-vanadium alloy; and the content of gaseous impurities in the target alloy can be reduced.
Further, in the step (1), before the molybdenum source and the first aluminum source are mixed, the molybdenum source and the first aluminum source are respectively dried; before mixing the vanadium source and the second aluminum source, respectively drying the vanadium source and the second aluminum source; in the step (2), before the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the chromium metal, the titanium source and the third aluminum source are mixed, the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the chromium metal, the titanium source and the third aluminum source are respectively dried. Furthermore, the drying temperature is 118-122 ℃, preferably 120 ℃, and the drying time is more than or equal to 12 hours. The invention has no special requirements on the mixing process, and the process well known in the field can ensure that all the raw materials are uniformly mixed. In the specific embodiment of the present invention, the mixing is preferably carried out in a blender, and there is no particular requirement for other conditions of mixing. In the invention, the mixing can ensure that all components are fully contacted, thereby facilitating the subsequent thermite reaction.
The method has the further beneficial effects that the drying treatment can remove moisture absorbed by the materials and ensure the drying of the materials, so that the impurity gas such as hydrogen, nitrogen, oxygen and the like separated out in the smelting process is reduced; the time is more than or equal to 12 hours to ensure the complete drying of the materials, the materials cannot be completely dried if the time is too short, and resources are wasted if the time is too long.
Further, in the step (1), the molybdenum source is a mixture of molybdenum dioxide and molybdenum trioxide, and the purity is preferably more than or equal to 99.8%; the vanadium source is vanadium pentoxide, and the purity is preferably more than or equal to 99.8%; the first aluminum source and the second aluminum source are both aluminum powder, and the purity is preferably more than or equal to 99.7%; and the molybdenum source, the vanadium source, the first aluminum source and the second aluminum source are preferably powders. Further, the mass ratio of the molybdenum dioxide, the molybdenum trioxide and the first aluminum source is (0.99-1.01): (1.89-1.92): (1.50-1.53), preferably 1: 1.9: 1.52; the mass ratio of the vanadium pentoxide to the second aluminum source is (1.67-1.69): (0.99-1.01), preferably 1.68: 1.
the method has the further beneficial effects that the mass ratio of molybdenum to vanadium in the aluminum-molybdenum alloy and the aluminum-vanadium alloy is controlled by controlling the mass ratio of the molybdenum source to the vanadium source to the first aluminum source to the second aluminum source. In the present invention, the reason why the molybdenum source is selected from a mixture of molybdenum dioxide and molybdenum trioxide is: the reaction between aluminum and molybdenum dioxide is too mild, which is not beneficial to the generation of first-grade alloy; since aluminum reacts with molybdenum trioxide too vigorously and is produced in a large amount with a high loss and danger, molybdenum dioxide and molybdenum trioxide are used in combination.
Further, in the step (1), the temperature of the first aluminothermic reaction is 1600-; the temperature of the second aluminothermic reaction is 1550-. In the present invention, the reaction crucible is preferably prepared from graphite, magnesia brick or corundum, and more preferably from corundum, so that the introduction of other elements is avoided and the reaction crucible can be recycled. The ignition mode for initiating the thermite reaction is not particularly limited in the present invention, and may be any mode known in the art. The reaction apparatus for the thermite reaction of the present invention is not particularly limited, and a known thermite reaction apparatus may be used. After the thermite reaction is finished, the obtained aluminum-molybdenum alloy liquid and aluminum-vanadium alloy liquid are preferably cooled in a furnace, and the cooling time is preferably 12 hours. After cooling, the invention also preferably carries out finishing crushing and selection on the cooled alloy ingot in sequence; the method of finish-crushing is not particularly limited in the present invention, and the cooled alloy ingot is finish-crushed into 5 to 50mm pieces by a method well known in the art. In the invention, the selection preferably comprises magnetic separation and manual selection, magnetic impurities, an oxide film, a nitride film alloy and other impurities are selected, and qualified parts are selected as the aluminum-molybdenum alloy and the aluminum-vanadium alloy.
The aluminum is used as a reducing agent in the thermite reaction process, molybdenum dioxide and molybdenum trioxide are reduced into metal simple substance molybdenum, vanadium pentoxide is reduced into simple substance vanadium, aluminum is oxidized into aluminum oxide, and a large amount of heat energy is released to melt the metal to form aluminum-molybdenum alloy liquid or aluminum-vanadium alloy liquid; the alumina formed by oxidizing the aluminum floats on the surface of the aluminum-molybdenum alloy liquid or the aluminum-vanadium alloy liquid, and is separated and removed from the aluminum-molybdenum alloy liquid or the aluminum-vanadium alloy liquid. The separation and removal process of the present invention is not particularly limited, and a process known to those skilled in the art may be selected.
Furthermore, in the step (2), the shape of the metal chromium is preferably blocky, and the purity is preferably more than or equal to 99.5%; the titanium source is sponge titanium, preferably blocky, and the purity is preferably more than or equal to 99.5%; the third aluminum source is aluminum beans which are used for adjusting the alloy grade and increasing the magnetic conductivity during smelting, and are beneficial to alloy melting; furthermore, the mass ratio of the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the metal chromium, the sponge titanium and the third aluminum source is (5.20-5.65): (4.70-5.65): (1.99-2.68): (0.98-1.84): (0.91-3.76), preferably (5.30-5.50): (4.80-5.10): (2.10-2.20): (1.20-1.60): (1.30-3.00), more preferably 5.4: 4.9: 2.3: 1.5: 2.5. in the invention, the adding amount of the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the chromium and the third aluminum source in vacuum melting is preferably determined according to the analysis result of the components of the aluminum-molybdenum alloy and the aluminum-vanadium alloy and the mass content of each metal element in the needed aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy. The mixing process is not particularly limited in the present invention, and the raw materials can be uniformly mixed by selecting a process known to those skilled in the art.
Further, in the step (2), the vacuum induction melting comprises melting and refining which are sequentially carried out; furthermore, the vacuum degree of vacuum induction melting is less than or equal to 10 Pa; the refining power is 100kW, the temperature is 1850-1900 ℃, preferably 1850 ℃, and the time is 5-10min, preferably 6-8 min. In the present invention, the vacuum induction melting is preferably performed in a medium frequency vacuum induction furnace, and the crucible for vacuum induction melting is preferably a corundum crucible, that is: and placing the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the metal chromium, the sponge titanium and a third aluminum source in a corundum crucible, and then placing the corundum crucible in a medium-frequency vacuum induction furnace for vacuum induction melting. In the invention, in order to control the content of impurity elements in the alloy, the purity of the corundum crucible is preferably more than or equal to 99 percent; the furnace lining for the corundum crucible knotting is preferably prepared by adopting the aluminothermic slag (alumina), so that reaction raw materials are fully utilized, and the cost is saved; the preparation method of the furnace lining for knotting the corundum crucible has no special requirement, and the method well known in the field can be adopted. According to the invention, the heating power of the vacuum induction melting is preferably slowly increased to melt the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the metal chromium, the sponge titanium and the third aluminum source, and refining is carried out after all the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the metal chromium, the sponge titanium and the third aluminum source are melted. The invention preferably adjusts the smelting power according to the alloy melting degree. In the present invention, the vacuum induction melting process is preferably: adjusting the initial power to 20kW, adjusting the power to 30kW after 10min, adjusting the power to 80kW after 20min, and keeping the power until the alloy is completely melted; finally, the power is adjusted to 100kW for refining, the power is reduced to 80kW, and pouring is started. In the present invention, the refining process is preferably carried out under electromagnetic stirring conditions, and the frequency of the electromagnetic stirring is preferably 2 Hz. The raw materials are melted firstly, and the alloy can be fully mixed under the action of electromagnetic stirring, so that the final alloy components are more uniform; and smelting is carried out under the vacuum condition, so that gas-phase impurities in the alloy can further escape, and the content of the gas-phase impurities in the final alloy is reduced.
The medium-frequency vacuum induction melting furnace has the further beneficial effects of high thermal efficiency, quick melting, difficult introduction of impurities due to vacuum operation and small environmental pollution. The refining can ensure that the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy is more fully and uniformly melted, plays a role in purifying and removing impurities, and can ensure that the refining temperature is slightly higher than the melting point of the alloy by controlling the temperature so as to achieve the aim of refining. By controlling the degree of vacuum, the content of O, N gas phase impurities in the finally prepared master alloy can be reduced.
Further, in the step (3), after the refining is completed, the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid obtained by vacuum induction melting is preferably poured into a water-cooled copper crucible for cooling, so as to obtain the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy. The cooling is preferably carried out under vacuum condition, the cooling mode is preferably furnace cooling after casting, and the cooling time is more than or equal to 12 h. The casting operation is not particularly limited in the present invention, and a casting method well known in the art may be used. The water-cooled copper crucible of the present invention is not particularly limited, and a water-cooled copper crucible known in the art may be used.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
the melting points of molybdenum (the melting point is 2610 ℃) and vanadium (the melting point is 1890 ℃) are very high, if metal molybdenum and metal vanadium are directly adopted for vacuum melting, the melting difficulty is high, the melting time is long, alloy elements with low melting points can be burnt, and the melting cost is increased. In order to solve the problems, the molybdenum source and the vanadium source are respectively prepared into the aluminum-molybdenum alloy and the aluminum-vanadium alloy, the melting points of the two alloys are close to the melting point of metal titanium, the melting is simpler during vacuum melting, the melting time is shorter, and the cost of oxides is lower compared with that of metal molybdenum and metal vanadium.
Specifically, the invention adopts a two-step method to prepare the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy, namely the aluminothermic reaction and the vacuum induction melting: preparing an aluminum-molybdenum alloy and an aluminum-vanadium alloy by adopting an aluminothermic method; and then carrying out vacuum induction melting, taking the aluminum-molybdenum alloy and the aluminum-vanadium alloy as matrixes, adding metal chromium, sponge titanium and a third aluminum source to adjust the alloy components, improving the uniformity, stability and accuracy of the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy components, and reducing the content of O, N and other impurities. The aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy prepared by the method has more uniform components, less element segregation and lower gas phase impurity content, and can better meet the production requirements of titanium alloys.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy specifically comprises the following steps:
(1) firstly, respectively drying molybdenum dioxide, molybdenum trioxide and aluminum powder at 118 ℃ for 12 hours, then weighing 84.40kg of molybdenum dioxide, 160.00kg of molybdenum trioxide and 128.32kg of aluminum powder, loading the weighed materials into a V-shaped mixer, fully and uniformly mixing, then respectively loading the uniformly mixed furnace materials into a sintered corundum crucible, carrying out ignition reaction, carrying out a first aluminothermic reaction at 1600 ℃ for 45s, cooling for 12 hours, then removing the crucible, taking out an alloy ingot, removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-molybdenum alloy;
firstly, respectively drying vanadium pentoxide and aluminum powder at 118 ℃ for 12h, then weighing 160.00kg of vanadium pentoxide and 95.40kg of aluminum powder, loading the weighed materials into a V-shaped mixer, fully mixing the materials uniformly, respectively loading the uniformly mixed furnace materials into sintered corundum crucibles, carrying out ignition reaction for a second aluminothermic reaction at 1550 ℃ for 40s, cooling for 12h, removing the crucibles, taking out alloy ingots, removing slag layers and oxide films on the surfaces of the alloy ingots, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-vanadium alloy;
(2) firstly, respectively drying an aluminum-molybdenum alloy, an aluminum-vanadium alloy, metal chromium, sponge titanium and aluminum beans at the temperature of 120 ℃ for 12 hours, then weighing 31.25kg of the aluminum-molybdenum alloy, 28.24kg of the aluminum-vanadium alloy, 12.00kg of the metal chromium, 6.00kg of the sponge titanium and 22.51kg of the aluminum beans, uniformly mixing, putting into a knotted and dried corundum crucible, vacuumizing a medium-frequency vacuum induction smelting furnace to below 10Pa, removing gas impurities in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, adjusting the power to be 80kW after 20min, and keeping the power until the alloy is melted down; adjusting the power to 100kW after melting down, refining for 5min at the power and 1900 ℃, vacuumizing the smelting furnace to below 10Pa again, and removing gas impurities in the melt to obtain an aluminum-molybdenum-vanadium-chromium-titanium alloy solution;
(3) adjusting the power to 80kW, inclining the crucible, slowly and stably pouring the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid into the water-cooled crucible, and after the pouring is finished, keeping vacuum cooling for 12 hours to obtain the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy.
Example 2
The preparation method of the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy specifically comprises the following steps:
(1) firstly, respectively drying molybdenum dioxide, molybdenum trioxide and aluminum powder at the temperature of 119 ℃ for 12 hours, then weighing 84.40kg of molybdenum dioxide, 160.00kg of molybdenum trioxide and 128.32kg of aluminum powder, putting the molybdenum dioxide, the 160.00kg of molybdenum trioxide and the aluminum powder into a V-shaped mixer, fully and uniformly mixing, then respectively putting the uniformly mixed furnace burden into a sintered corundum crucible, carrying out ignition reaction, carrying out a first aluminothermic reaction at the temperature of 1620 ℃ for 42s, cooling for 12 hours, then removing the crucible, taking out an alloy ingot, removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-molybdenum alloy;
firstly, respectively drying vanadium pentoxide and aluminum powder at the temperature of 119 ℃ for 12 hours, then weighing 160.00kg of vanadium pentoxide and 95.40kg of aluminum powder, loading the weighed materials into a V-shaped mixer, fully mixing the materials uniformly, respectively loading the uniformly mixed furnace materials into sintered corundum crucibles, carrying out ignition reaction, carrying out a second aluminothermic reaction at the temperature of 1580 ℃ for 38 seconds, cooling the materials for 12 hours, removing the crucibles, taking out alloy ingots, removing slag layers and oxidation films on the surfaces of the alloy ingots, crushing and finishing the materials to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-vanadium alloy;
(2) firstly, respectively drying an aluminum-molybdenum alloy, an aluminum-vanadium alloy, metal chromium, sponge titanium and aluminum beans at the temperature of 120 ℃ for 12 hours, then weighing 33.75kg of the aluminum-molybdenum alloy, 33.75kg of the aluminum-vanadium alloy, 16.00kg of the metal chromium, 11.00kg of the sponge titanium and 5.50kg of the aluminum beans, uniformly mixing, putting into a knotted and dried corundum crucible, vacuumizing a medium-frequency vacuum induction smelting furnace to below 10Pa, removing gas impurities in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, adjusting the power to be 80kW after 20min, and keeping the power until the alloy is melted down; adjusting the power to 100kW after melting down, refining for 10min at 1850 ℃ under the power, vacuumizing the smelting furnace to below 10Pa again, and removing gas impurities in the melt to obtain aluminum-molybdenum-vanadium-chromium-titanium alloy liquid;
(3) adjusting the power to 80kW, inclining the crucible, slowly and stably pouring the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid into the water-cooled crucible, and after the pouring is finished, keeping vacuum cooling for 12 hours to obtain the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy.
Example 3
The preparation method of the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy specifically comprises the following steps:
(1) firstly, respectively drying molybdenum dioxide, molybdenum trioxide and aluminum powder at the temperature of 120 ℃ for 12 hours, then weighing 84.40kg of molybdenum dioxide, 160.00kg of molybdenum trioxide and 128.32kg of aluminum powder, putting the molybdenum dioxide, the 160.00kg of molybdenum trioxide and the aluminum powder into a V-shaped mixer, fully and uniformly mixing, then respectively putting the uniformly mixed furnace materials into sintered corundum crucibles, carrying out ignition reaction, carrying out primary aluminothermic reaction at the temperature of 1650 ℃ for 40s, cooling for 12 hours, then removing the crucibles, taking out alloy ingots, removing slag layers and oxidation films on the surfaces of the alloy ingots, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-molybdenum alloy;
firstly, respectively drying vanadium pentoxide and aluminum powder at the temperature of 120 ℃ for 12 hours, then weighing 160.00kg of vanadium pentoxide and 95.40kg of aluminum powder, loading the materials into a V-shaped mixer, fully mixing the materials uniformly, respectively loading the uniformly mixed furnace materials into sintered corundum crucibles, carrying out ignition reaction, carrying out a second aluminothermic reaction at the temperature of 1600 ℃ for 40s, cooling the materials for 12 hours, removing the crucibles, taking out alloy ingots, removing slag layers and oxide films on the surfaces of the alloy ingots, crushing and finishing the materials to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-vanadium alloy;
(2) firstly, respectively drying an aluminum-molybdenum alloy, an aluminum-vanadium alloy, metal chromium, sponge titanium and aluminum beans at the temperature of 120 ℃ for 12 hours, then weighing 31.88kg of the aluminum-molybdenum alloy, 28.82kg of the aluminum-vanadium alloy, 13.00kg of the metal chromium, 8.00kg of the sponge titanium and 18.30kg of the aluminum beans, uniformly mixing, putting into a knotted and dried corundum crucible, vacuumizing a medium-frequency vacuum induction melting furnace to below 10Pa, removing gas impurities in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, adjusting the power to be 80kW after 20min, and keeping the power until the alloy is melted down; adjusting the power to 100kW after melting down, refining for 8min at 1860 ℃ under the power, vacuumizing the smelting furnace to below 10Pa again, and removing gas impurities in the melt to obtain aluminum-molybdenum-vanadium-chromium-titanium alloy liquid;
(3) adjusting the power to 80kW, inclining the crucible, slowly and stably pouring the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid into the water-cooled crucible, and after the pouring is finished, keeping vacuum cooling for 12 hours to obtain the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy.
Example 4
The preparation method of the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy specifically comprises the following steps:
(1) firstly, respectively drying molybdenum dioxide, molybdenum trioxide and aluminum powder at the temperature of 121 ℃ for 12 hours, then weighing 84.40kg of molybdenum dioxide, 160.00kg of molybdenum trioxide and 128.32kg of aluminum powder, putting the molybdenum dioxide, the 160.00kg of molybdenum trioxide and the aluminum powder into a V-shaped mixer, fully and uniformly mixing, then respectively putting the uniformly mixed furnace burden into a sintered corundum crucible, carrying out ignition reaction, carrying out primary aluminothermic reaction at the temperature of 1680 ℃ for 39s, cooling for 12 hours, then removing the crucible, taking out an alloy ingot, removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-molybdenum alloy;
firstly, respectively drying vanadium pentoxide and aluminum powder at the temperature of 121 ℃ for 12 hours, then weighing 160.00kg of vanadium pentoxide and 95.40kg of aluminum powder, loading the weighed materials into a V-shaped mixer, fully and uniformly mixing, respectively loading the uniformly mixed furnace materials into sintered corundum crucibles, carrying out ignition reaction, carrying out a second aluminothermic reaction at the temperature of 1620 ℃ for 36s, cooling for 12 hours, removing the crucibles, taking out alloy ingots, removing slag layers and oxidation films on the surfaces of the alloy ingots, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-vanadium alloy;
(2) firstly, respectively drying an aluminum-molybdenum alloy, an aluminum-vanadium alloy, metal chromium, sponge titanium and aluminum beans at the temperature of 120 ℃ for 12 hours, then weighing 32.50kg of the aluminum-molybdenum alloy, 29.41kg of the aluminum-vanadium alloy, 14.00 kg of the metal chromium, 9.00kg of the sponge titanium and 15.90kg of the aluminum beans, uniformly mixing, putting into a knotted and dried corundum crucible, vacuumizing a medium-frequency vacuum induction smelting furnace to below 10Pa, removing gas impurities in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, adjusting the power to be 80kW after 20min, and keeping the power until the alloy is melted down; adjusting the power to 100kW after melting down, refining for 7min at 1870 ℃ under the power, vacuumizing the smelting furnace to below 10Pa again, and removing gas impurities in the melt to obtain an aluminum-molybdenum-vanadium-chromium-titanium alloy liquid;
(3) adjusting the power to 80kW, inclining the crucible, slowly and stably pouring the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid into the water-cooled crucible, and after the pouring is finished, keeping vacuum cooling for 12 hours to obtain the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy.
Example 5
The preparation method of the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy specifically comprises the following steps:
(1) firstly, respectively drying molybdenum dioxide, molybdenum trioxide and aluminum powder at the temperature of 122 ℃ for 12 hours, then weighing 84.40kg of molybdenum dioxide, 160.00kg of molybdenum trioxide and 128.32kg of aluminum powder, putting the molybdenum dioxide, the 160.00kg of molybdenum trioxide and the aluminum powder into a V-shaped mixer, fully and uniformly mixing, then respectively putting the uniformly mixed furnace burden into a sintered corundum crucible, carrying out ignition reaction, carrying out a first aluminothermic reaction at the temperature of 1700 ℃ for 35s, cooling for 12 hours, then removing the crucible, taking out an alloy ingot, removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-molybdenum alloy;
firstly, respectively drying vanadium pentoxide and aluminum powder at 122 ℃ for 12h, then weighing 160.00kg of vanadium pentoxide and 95.40kg of aluminum powder, loading the materials into a V-shaped mixer, fully mixing the materials uniformly, respectively loading the uniformly mixed furnace materials into sintered corundum crucibles, carrying out ignition reaction for a second aluminothermic reaction at 1650 ℃ for 32s, cooling the materials for 12h, removing the crucibles, taking out alloy ingots, removing slag layers and oxidation films on the surfaces of the alloy ingots, crushing and finishing the materials to 5-50mm, and carrying out magnetic separation and manual selection to obtain an aluminum-vanadium alloy;
(2) firstly, respectively drying an aluminum-molybdenum alloy, an aluminum-vanadium alloy, metal chromium, sponge titanium and aluminum beans at the temperature of 120 ℃ for 12 hours, then weighing 33.13kg of the aluminum-molybdenum alloy, 30.59kg of the aluminum-vanadium alloy, 15.00kg of the metal chromium, 10.00kg of the sponge titanium and 11.29kg of the aluminum beans, uniformly mixing, putting into a knotted and dried corundum crucible, vacuumizing a medium-frequency vacuum induction smelting furnace to below 10Pa, removing gas impurities in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, adjusting the power to be 80kW after 20min, and keeping the power until the alloy is melted down; adjusting the power to 100kW after melting down, refining for 7min at the power and the temperature of 1880 ℃, vacuumizing the smelting furnace to below 10Pa again, and removing gas impurities in the melt to obtain aluminum-molybdenum-vanadium-chromium-titanium alloy liquid;
(3) adjusting the power to 80kW, inclining the crucible, slowly and stably pouring the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid into the water-cooled crucible, and after the pouring is finished, keeping vacuum cooling for 12 hours to obtain the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy.
Performance detection
1. The Al-Mo-V-Cr-Ti intermediate alloy ingots (cylinders) prepared in examples 1 to 5 were sampled, and chemical composition analysis was carried out on two points (1, 2) from the upper surface of the ingot, two points (3, 4) from the lower surface of the ingot, and two points (5, 6) from the middle portion of the ingot, as shown in tables 1 to 5.
Table 1 example 1 analysis results of chemical composition of al-mo-v-cr-ti master alloy ingot
Table 2 example 2 analysis results of chemical composition of al-mo-v-cr-ti master alloy ingot
Table 3 example 3 analysis results of chemical composition of al-mo-v-cr-ti master alloy ingot
Table 4 example 4 analysis results of chemical composition of al-mo-v-cr-ti master alloy ingot
TABLE 5 example 5 chemical composition analysis results of Al-Mo-V-Cr-Ti master alloy ingot
As can be seen from tables 1-5, the Al-Mo-V-Cr-Ti intermediate alloy prepared in the embodiments 1-5 of the present invention has high purity, uniform and stable components, less segregation and lower gas phase impurity content, and can better satisfy the production requirements of titanium alloy.
2. Samples of the Al-Mo-V-Cr-Ti master alloy ingots (cylinders) prepared in examples 1-5 were taken for chemical composition analysis, and the optimum results are shown in Table 6.
TABLE 6 examples 1-5 optimum results for aluminum molybdenum vanadium chromium titanium master alloy ingots
As can be seen from Table 6, the Al-Mo-V-Cr-Ti master alloy C, O, N prepared in examples 1-5 of the present invention has low impurity content, wherein Fe and Si are inevitable impurities introduced from raw materials.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy is characterized by comprising the following components in percentage by mass: 25.0 to 27.0 percent of molybdenum, 24.0 to 27.0 percent of vanadium, 12.0 to 16.0 percent of chromium, 6.0 to 11.0 percent of titanium, the balance being aluminum and inevitable impurities.
2. The Al-Mo-V-Cr-Ti intermediate alloy as claimed in claim 1, wherein the Al-Mo-V-Cr-Ti intermediate alloy comprises the following components by mass percent: 25.5 to 26.5 percent of molybdenum, 24.5 to 26.5 percent of vanadium, 12.5 to 15.5 percent of chromium, 6.5 to 10.0 percent of titanium, the balance of aluminum and inevitable impurities.
3. The Al-Mo-V-Cr-Ti intermediate alloy as claimed in claim 2, wherein the Al-Mo-V-Cr-Ti intermediate alloy comprises the following components by mass percent: 26.0% of molybdenum, 25.0% of vanadium, 14.0% of chromium, 9.0% of titanium, the balance of aluminum and inevitable impurities.
4. A method for preparing an aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy as claimed in any one of claims 1 to 3, which comprises the following steps:
(1) mixing a molybdenum source and a first aluminum source, and carrying out a first aluminothermic reaction to obtain an aluminum-molybdenum alloy; mixing a vanadium source and a second aluminum source, and carrying out a second aluminothermic reaction to obtain an aluminum-vanadium alloy;
(2) mixing an aluminum-molybdenum alloy, an aluminum-vanadium alloy, metal chromium, a titanium source and a third aluminum source, and carrying out vacuum induction melting to obtain an aluminum-molybdenum-vanadium-chromium-titanium alloy liquid;
(3) and cooling the aluminum-molybdenum-vanadium-chromium-titanium alloy liquid to obtain the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy.
5. The method for preparing the Al-Mo-V-Cr-Ti intermediate alloy as claimed in claim 4, wherein in step (1), the Mo source and the first Al source are dried respectively before mixing them; before mixing the vanadium source and the second aluminum source, respectively drying the vanadium source and the second aluminum source; in the step (2), before the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the chromium metal, the titanium source and the third aluminum source are mixed, the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the chromium metal, the titanium source and the third aluminum source are respectively dried;
the drying temperature is 118-122 ℃, and the drying time is more than or equal to 12 h.
6. The method for preparing the aluminum-molybdenum-vanadium-chromium-titanium intermediate alloy as claimed in claim 4, wherein in the step (1), the molybdenum source is a mixture of molybdenum dioxide and molybdenum trioxide, the vanadium source is vanadium pentoxide, and the first aluminum source and the second aluminum source are both aluminum powder;
the mass ratio of the molybdenum dioxide to the molybdenum trioxide to the first aluminum source is (0.99-1.01): (1.89-1.92): (1.50-1.53); the mass ratio of the vanadium pentoxide to the second aluminum source is (1.67-1.69): (0.99-1.01).
7. The method as claimed in claim 4, wherein in the step (1), the first aluminothermic reaction is carried out at 1600-1700 ℃ for 35-45 s; the temperature of the second aluminothermic reaction is 1550-.
8. The method for preparing the Al-Mo-V-Cr-Ti intermediate alloy as claimed in claim 4, wherein in step (2), the Ti source is sponge Ti, and the third Al source is Al-bean;
the mass ratio of the aluminum-molybdenum alloy, the aluminum-vanadium alloy, the metal chromium, the sponge titanium and the third aluminum source is (5.20-5.65): (4.70-5.65): (1.99-2.68): (0.98-1.84): (0.91-3.76).
9. The method for preparing the Al-Mo-V-Cr-Ti intermediate alloy as claimed in claim 4, wherein in the step (2), the vacuum induction melting comprises melting and refining which are carried out sequentially;
the vacuum degree of the vacuum induction melting is less than or equal to 10 Pa; the power of the refining is 100kW, the temperature is 1850-1900 ℃, and the time is 5-10 min.
10. The method for preparing the Al-Mo-V-Cr-Ti intermediate alloy as claimed in claim 4, wherein in step (3), the cooling time is not less than 12 h.
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