CN113388749A - Aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy and preparation method thereof - Google Patents
Aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides an aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy and a preparation method thereof, and relates to the technical field of metal materials. The aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy comprises, by mass, 23.0-27.0% of molybdenum, 23.0-27.0% of chromium, 6.0-10.0% of zirconium, 0.5-1.5% of silicon and the balance of aluminum. The invention controls the components and the content to ensure that the components of the aluminum-molybdenum-chromium-zirconium-silicon master alloy are uniform and have small segregation, is beneficial to the homogenization of the components of the titanium alloy when the titanium alloy is smelted, and can effectively prevent the metallurgical defects of the components segregation and the like of the titanium alloy. The invention provides a preparation method of the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy, which can improve the uniformity and stability of the components of the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy, reduce the impurity content and better meet the production requirement of titanium alloy.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to an aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy and a preparation method thereof.
Background
Titanium and titanium alloys have been receiving great attention and favor from the aerospace industry because of their superior overall properties of high specific strength and specific stiffness, weldability, high temperature resistance, corrosion resistance, etc. With the continuous development of new generation airplanes and aero-engines, the requirements for the comprehensive performance of titanium alloy materials are higher and higher, and the high use amount, high performance and low cost are the main challenges of the titanium alloy materials for aviation in the 21 st century.
The TC32 titanium alloy is a novel high-performance low-cost titanium alloy with comprehensive performance superior to that of TC4, and the alloy has good matching of comprehensive performance such as high strength, good plasticity, high fracture toughness and fatigue resistance after being subjected to appropriate thermal mechanical treatment.
The intermediate alloy is an additive functional material, which is prepared by adding one or more simple substances into a metal serving as a matrix to solve the problems of easy burning loss, difficult melting of high melting point, high density, easy segregation and the like of the simple substances or improve the performance of the alloy. The application of the intermediate alloy can effectively improve the alloying condition of metal smelting, improve the uniformity of alloy components, overcome segregation and unmelted metal inclusions, and simultaneously effectively reduce the metal burning loss rate. Elements (such as tin, tungsten, molybdenum and the like) which have larger differences between the density and the melting point and a matrix and are easy to generate inclusion and segregation metallurgical defects, elements (such as iron, chromium and the like) which are easy to generate segregation metallurgical defects in the smelting process and trace elements (such as silicon and the like) with low content are usually added in the form of intermediate alloy, and the addition effect of other alloy elements in the form of intermediate alloy is better from the aspects of improving the uniformity of components, improving the metallurgical quality and the like.
In order to meet the requirements of element content and performance in use of TC32 titanium alloy, multiple binary alloys and simple substances are required to be added for smelting the titanium alloy, so that the alloy proportion in the production process of the titanium alloy becomes complex, segregation and inclusion metallurgical defects of a titanium alloy ingot are easily caused, and the existence of the defects can seriously affect the structure and mechanical properties of a product and the reliability of subsequent use.
Disclosure of Invention
In view of the above, the present invention provides an aluminum molybdenum chromium zirconium silicon intermediate alloy and a preparation method thereof. The aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy provided by the invention has uniform and stable components, and is beneficial to the homogenization of alloy components when a titanium alloy is smelted.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy which comprises, by mass, 23.0-27.0% of Mo, 23.0-27.0% of Cr, 6.0-10.0% of Zr, 0.5-1.5% of Si and the balance of Al.
Preferably, the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy comprises, by mass, 24.0-26.0% of Mo, 24.0-26.0% of Cr, 7.0-9.0% of Zr, 0.8-1.2% of Si and the balance of Al.
Preferably, the aluminum-molybdenum-chromium-zirconium-silicon master alloy comprises 25.0% of Mo, 25.0% of Cr, 8.0% of Zr, 1.0% of Si and the balance of Al by mass.
The invention also provides a preparation method of the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy, which comprises the following steps:
mixing molybdenum trioxide, chromium sesquioxide and aluminum for thermite reaction, and cooling to obtain an aluminum-molybdenum-chromium primary alloy;
and carrying out vacuum induction melting on the aluminum-molybdenum-chromium primary alloy, the sponge zirconium and the elemental silicon, and cooling to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy.
Preferably, the mass ratio of the molybdenum trioxide to the chromium oxide to the aluminum is (3.690-4.576): (7.190-8.918): (7.199-7.741).
Preferably, the molybdenum trioxide, chromium oxide and aluminum are dried separately before mixing; the drying temperature is independently 110-130 ℃, and the drying time is independently more than or equal to 12h
Preferably, the temperature of the thermite reaction is 1750-1850 ℃ and the time is 35-45 s.
Preferably, the vacuum degree of the vacuum induction melting is less than 10 Pa.
Preferably, the vacuum induction melting comprises melting and refining which are carried out in sequence; the refining temperature is 1650-1750 ℃ and the refining time is 5-10 min.
Preferably, the method further comprises the step of casting the alloy liquid obtained by the induction melting in a water-cooled copper crucible for natural cooling after the vacuum induction melting, wherein the time of the natural cooling is more than or equal to 6 hours.
The invention provides an aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy which comprises, by mass, 23.0-27.0% of Mo, 23.0-27.0% of Cr, 6.0-10.0% of Zr, 0.5-1.5% of Si and the balance of Al. The invention controls the element components and the content, so that the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy has uniform components and small segregation, is beneficial to the homogenization of the components of the titanium alloy when the titanium alloy is smelted, and prevents the metallurgical defects of component segregation and inclusion.
The invention provides a preparation method of the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy. The invention adopts a two-step method to prepare the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy, namely the two steps of aluminothermic reduction reaction and vacuum induction smelting are as follows: preparing an aluminum-molybdenum-chromium primary alloy by adopting an aluminothermic method; and then carrying out vacuum induction melting, wherein the aluminum-molybdenum-chromium-primary alloy, the sponge zirconium and the simple substance silicon are used as raw materials to prepare the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy during the vacuum induction melting. The preparation method provided by the invention can improve the uniform stability of the components of the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy, reduce the impurity content and O, N gas impurity content, and can better meet the production requirements of titanium alloy. The data of the embodiment shows that the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy prepared by the invention contains, by mass, less than or equal to 0.30% of Fe, less than or equal to 0.10% of C, less than or equal to 0.10% of O, and less than or equal to 0.10% of N.
Detailed Description
The invention provides an aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy which comprises, by mass, 23.0-27.0% of Mo, 23.0-27.0% of Cr, 6.0-10.0% of Zr, 0.5-1.5% of Si and the balance of Al; preferably comprises 24.0-26.0% of Mo, 24.0-26.0% of Cr, 7.0-9.0% of Zr, 0.8-1.2% of Si and the balance of Al; more preferably, 25.0% Mo, 25.0% Cr, 8.0% Zr, 1.0% Si, and the balance Al.
The invention controls the components and the content to ensure that the aluminum-molybdenum-chromium-zirconium-silicon master alloy has uniform components and small segregation, is beneficial to the homogenization of the components of the titanium alloy when the titanium alloy is smelted, and prevents the metallurgical defects of component segregation and inclusion.
The invention provides a preparation method of the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy, which comprises the following steps:
mixing molybdenum trioxide, chromium sesquioxide and aluminum for thermite reaction, and cooling to obtain an aluminum-molybdenum-chromium primary alloy;
and carrying out vacuum induction melting on the aluminum-molybdenum-chromium primary alloy, the sponge zirconium and the elemental silicon, and cooling to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy.
According to the invention, molybdenum trioxide, chromium sesquioxide and aluminum are mixed for aluminothermic reaction and cooled to obtain the aluminum-molybdenum-chromium primary alloy.
In the invention, the mass ratio of the molybdenum trioxide to the chromium oxide to the aluminum is preferably (3.690-4.576): (7.190-8.918): (7.199-7.741), more preferably (3.905-4.343): (7.609-8.463): (7.610-7.341), most preferably 4.121: 8.030: 7.477.
in the present invention, the molybdenum trioxide, chromium sesquioxide and aluminum are preferably powders. In the present invention, the molybdenum trioxide meets the particle size requirements specified in the color recommendations; the chromic oxide meets the granularity requirement in the chemical recommended standard; the aluminum meets the particle size requirement of air atomized aluminum powder in the national recommended standard.
In the invention, the molybdenum trioxide, the chromium trioxide and the aluminum are preferably dried respectively before mixing, the drying temperature is preferably 110-130 ℃, more preferably 120 ℃, and the time is preferably more than or equal to 12 hours, more preferably 12 hours independently.
The invention has no special requirements on the mixing method, and the method well known in the field is adopted to ensure that the molybdenum trioxide, the chromium trioxide and the aluminum are uniformly mixed; in the specific embodiment of the invention, the mixing is preferably performed in a V-shaped mixer, the mixing speed of the V-shaped mixer is preferably 120-160 r/min, more preferably 130-150 r/min, and the mixing time is preferably 2-6 min, more preferably 3-5 min. In the invention, the mixing makes the components fully contacted, so that the thermite reaction is conveniently carried out.
According to the invention, the mixture obtained by mixing is preferably placed in a reaction crucible for aluminothermic reaction.
In the present invention, the aluminothermic reaction crucible is preferably prepared from graphite, magnesia brick or corundum, and more preferably from magnesia brick. The present invention does not require any particular ignition means for initiating the thermite reaction and may be accomplished in a manner well known in the art.
In the invention, the thermite reaction is preferably 1750-1850 ℃, more preferably 1780-1820 ℃ and is preferably carried out for 35-45 s, more preferably 38-42 s. The invention has no special requirement on the reaction device of the aluminothermic reaction, and only needs to adopt the aluminothermic reaction device well known in the field, in the specific embodiment of the invention, the aluminothermic reaction is preferably carried out 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 aluminum oxide or a furnace body built by graphite plates.
In the thermite reaction process, aluminum is used as a reducing agent to reduce molybdenum trioxide and chromium sesquioxide into metal simple substances molybdenum and chromium respectively, aluminum is oxidized into aluminum oxide, a large amount of heat energy is released to melt metal (the metal simple substances molybdenum, chromium and excessive aluminum) to form aluminum-molybdenum-chromium alloy liquid, and the aluminum oxide 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-chromium alloy liquid, the aluminum-molybdenum-chromium alloy liquid is cooled to obtain the aluminum-molybdenum-chromium primary alloy.
In the present invention, the cooling is preferably furnace cooling, and the cooling time is preferably 12 hours.
After cooling, the invention also preferably carries out finishing crushing, component analysis and selection on the cooled alloy ingot 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 selection preferably comprises magnetic separation and manual selection; the invention selects the magnetic impurities, the alloy containing the oxide film and the nitride film, and selects the qualified part as the first-grade alloy of aluminum, molybdenum and chromium. The invention takes aluminum as a reducing agent and molybdenum trioxide and chromium sesquioxide as oxidizing agents, and prepares the aluminum-molybdenum-chromium primary alloy through aluminothermic reaction (namely an external ignition method).
After the aluminum-molybdenum-chromium primary alloy is obtained, the aluminum-molybdenum-chromium primary alloy, the sponge zirconium and the simple substance silicon are subjected to vacuum induction melting and cooled to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy.
In the invention, the mass ratio of the aluminum-molybdenum-chromium primary alloy, the sponge zirconium and the simple substance silicon is preferably (88.50-93.50): (6.00-10.00): (0.50 to 1.50), more preferably (89.80 to 92.20): (7.00-9.00): (0.80 to 1.20), most preferably 91.00: 8.00: 1.00.
in the invention, the vacuum induction melting is preferably carried out in a medium-frequency vacuum induction furnace, and the crucible for vacuum induction melting is preferably a corundum crucible, namely, the aluminum-molybdenum-chromium primary alloy, the sponge zirconium and the simple substance silicon are placed in the corundum crucible, and then the corundum crucible is placed in the medium-frequency vacuum induction furnace for 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 knotting the corundum crucible is preferably prepared by adopting the aluminothermic reaction slag (alumina), so that reaction raw materials are fully utilized, the cost is saved, and the method for preparing the furnace lining for knotting the corundum crucible has no special requirement and can be realized by adopting a method well known in the field.
In the invention, the vacuum degree is preferably less than 10 Pa when the vacuum induction melting is vacuumized; the vacuum induction melting is preferably carried out in a protective atmosphere, preferably argon.
In the present invention, the induction melting preferably includes melting and refining which are performed sequentially. In the present invention, the melting is particularly preferably: and adjusting the power of the medium-frequency vacuum induction furnace to the initial power to start heating, then increasing the power to the transition power to heat until the metal starts to melt, and then increasing the power to the stable power to heat until the metal is completely melted to obtain a mixed melt. In the invention, the initial power is preferably 25-32 kW, and more preferably 28-30 kW; the transition power is preferably 45-65 kW, and more preferably 50-60 kW; the stable power is preferably 65-75 kW, more preferably 68-72 kW, and after the primary aluminum-molybdenum-chromium alloy, the sponge zirconium and the elemental silicon are completely melted, the mixed melt is refined.
In the invention, the refining temperature is preferably 1650-1750 ℃, more preferably 1680-1720 ℃, 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 75-85 kW, more preferably 80kW, and in the refining process, impurities and gases in the mixed melt can be removed to obtain pure alloy liquid.
After the refining is finished, the obtained alloy liquid is cooled. The alloy liquid is preferably cast in a water-cooled copper crucible for cooling, the preferable time of cooling is more than or equal to 6h, the invention has no special requirement on the casting operation and only needs to adopt a casting method well known in the field, and the invention has no special requirement on the water-cooled copper crucible and only needs to adopt a water-cooled copper crucible well known in the field.
In the present invention, the cooling is preferably performed under vacuum conditions.
The invention takes the aluminum-molybdenum-chromium primary alloy, the sponge zirconium and the simple substance silicon as raw materials during vacuum induction smelting, so that the grade of the target alloy is more stable, and the content of gas impurities in the target alloy can be reduced.
The invention provides the preparation method of the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy, which can improve the component uniformity and accuracy of the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy, reduce the impurity content and better meet the production requirement of titanium alloy.
In order to further illustrate the present invention, the aluminum molybdenum chromium zirconium silicon master alloy and the preparation method thereof provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
First, aluminothermic smelting process
(1) Drying aluminum powder, chromium oxide and molybdenum trioxide at 120 deg.C for 12 hr.
(2) The raw material ratio is as follows: 77.71kg of aluminum powder, 71.90kg of chromium oxide and 36.90kg of molybdenum trioxide; the raw materials are put into a V-shaped mixer, the mixing speed is 160r/min, the mixing time is 2min, and the raw materials are uniformly mixed and fully contacted.
(3) And (3) loading the uniformly mixed furnace burden into a sintered corundum crucible, carrying out ignition reaction, cooling for 12 hours along with the furnace after the reaction is finished, dismantling the crucible, taking out an alloy ingot, and weighing.
(4) Removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing, carrying out magnetic separation and manual selection to obtain the aluminum-molybdenum-chromium primary alloy, and carrying out chemical component analysis on the obtained primary alloy.
Second, induction melting process
(1) The raw material ratio is as follows: 93.50kg of aluminum-molybdenum-chromium primary alloy, 6.00kg of sponge zirconium and 0.50kg of simple substance silicon; and (3) putting the primary alloy, the sponge zirconium and the simple substance silicon into a knotted and dried corundum crucible. And vacuumizing the intermediate-frequency vacuum induction smelting furnace to below 10 Pa, and removing gas impurities in the smelting furnace.
(2) And (3) power transmission smelting, wherein the initial power is 30kW, the transition power is adjusted to 60kW within 30 minutes, the stable power is adjusted to 70kW after the alloy starts to melt, after the furnace burden is completely melted, refining is carried out for 10 minutes at 1650 ℃, the smelting furnace is vacuumized to below 10 Pa again, and gas impurities in the melt are removed.
(3) The crucible is inclined, and the melt is slowly and stably cast into the water-cooled crucible. And after the casting is finished, keeping vacuum cooling for more than 6 hours to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy (cylindrical alloy ingot).
One position of the al-mo-cr-zr-si intermediate alloy 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 Al-Mo-Cr-Zr-Si master alloy C, O, N prepared in this example has a low impurity content, and Fe is an inevitable impurity introduced from the raw material.
The aluminum molybdenum chromium zirconium silicon master alloy prepared in the embodiment was sampled at different positions, chemical composition analysis was performed, two points, numbered 1 and 2, were taken from the upper surface of the alloy ingot, two points, numbered 3 and 4, were taken from the lower surface of the alloy ingot, two points, numbered 5 and 6, were taken from the middle portion of the alloy ingot, and composition analysis was performed on the point-taken portions, and the results are shown in table 2. As can be seen from Table 2, the Al-Mo-Cr-Zr-Si master alloy prepared by the embodiment has uniform and stable components and no segregation.
Example 2
First, aluminothermic smelting process
(1) Drying aluminum powder, chromium oxide and molybdenum trioxide at 120 deg.C for 12 hr.
(2) The raw material ratio is as follows: 76.10kg of aluminum powder, 76.09kg of dichromium trioxide and 39.05kg of molybdenum trioxide; the raw materials are loaded into a V-shaped mixer, the mixing speed is 150r/min, the mixing time is 3min, and the raw materials are uniformly mixed and fully contacted.
(3) And (3) loading the uniformly mixed furnace burden into a sintered corundum crucible, carrying out ignition reaction, cooling for 12 hours along with the furnace after the reaction is finished, dismantling the crucible, taking out an alloy ingot, and weighing.
(4) Removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing, carrying out magnetic separation and manual selection to obtain the aluminum-molybdenum-chromium primary alloy, and carrying out chemical component analysis on the obtained primary alloy.
Second, induction melting process
(1) The raw material ratio is as follows: 92.20kg of aluminum-molybdenum-chromium primary alloy, 7.00kg of sponge zirconium and 0.80kg of simple substance silicon; and (3) putting the primary alloy, the sponge zirconium and the simple substance silicon into a knotted and dried corundum crucible. And vacuumizing the intermediate-frequency vacuum induction smelting furnace to below 10 Pa, and removing gas impurities in the smelting furnace.
(2) And (3) power transmission smelting, wherein the initial power is 30kW, the transition power is adjusted to 60kW within 30 minutes, the stable power is adjusted to 70kW after the alloy starts to melt, after the furnace burden is completely melted, refining is carried out for 8 minutes at 1680 ℃, the smelting furnace is vacuumized to below 10 Pa again, and gas impurities in the melt are removed.
(3) The crucible is inclined, and the melt is slowly and stably cast into the water-cooled crucible. And after the casting is finished, keeping vacuum cooling for more than 6 hours to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy (cylindrical alloy ingot).
One position of the Al-Mo-Cr-Zr-Si master alloy prepared in this example (the same position as the sampling position of example 1) was sampled and analyzed for chemical composition, and the results are shown in Table 1.
The method of example 1 is adopted to sample different parts of the aluminum molybdenum chromium zirconium silicon intermediate alloy prepared in this example for chemical composition analysis, and the results are shown in table 3, which shows that the aluminum molybdenum chromium zirconium silicon intermediate alloy prepared in this example has uniform and stable composition and no segregation.
Example 3
First, aluminothermic smelting process
(1) Drying aluminum powder, chromium oxide and molybdenum trioxide at 120 deg.C for 12 hr.
(2) The raw material ratio is as follows: 74.77kg of aluminum powder, 80.30kg of chromium oxide and 41.21kg of molybdenum trioxide; the raw materials are put into a V-shaped mixer, the mixing speed is 140r/min, the mixing time is 4min, and the raw materials are uniformly mixed and fully contacted.
(3) And (3) loading the uniformly mixed furnace burden into a sintered corundum crucible, carrying out ignition reaction, cooling for 12 hours along with the furnace after the reaction is finished, dismantling the crucible, taking out an alloy ingot, and weighing.
(4) Removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing, carrying out magnetic separation and manual selection to obtain the aluminum-molybdenum-chromium primary alloy, and carrying out chemical component analysis on the obtained primary alloy.
Second, induction melting process
(1) The raw material ratio is as follows: 91.00kg of aluminum-molybdenum-chromium primary alloy, 8.00kg of sponge zirconium and 1.00kg of simple substance silicon; and (3) putting the primary alloy, the sponge zirconium and the simple substance silicon into a knotted and dried corundum crucible. And vacuumizing the intermediate-frequency vacuum induction smelting furnace to below 10 Pa, and removing gas impurities in the smelting furnace.
(2) And (3) power transmission smelting, wherein the initial power is 30kW, the transition power is adjusted to 60kW within 30 minutes, the stable power is adjusted to 70kW after the alloy starts to melt, refining is carried out for 7 minutes at 1700 ℃ after the furnace burden is completely melted, the smelting furnace is vacuumized to below 10 Pa again, and gas impurities in the melt are removed.
(3) The crucible is inclined, and the melt is slowly and stably cast into the water-cooled crucible. And after the casting is finished, keeping vacuum cooling for more than 6 hours to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy (cylindrical alloy ingot).
One position of the Al-Mo-Cr-Zr-Si master alloy prepared in this example (the same position as the sampling position of example 1) was sampled and analyzed for chemical composition, and the results are shown in Table 1.
The method of example 1 is adopted to sample different parts of the aluminum molybdenum chromium zirconium silicon master alloy prepared in this example for chemical composition analysis, and the results are shown in table 4, which shows that the aluminum molybdenum chromium zirconium silicon master alloy prepared in this example has uniform and stable composition and no segregation.
Example 4
First, aluminothermic smelting process
(1) Drying aluminum powder, chromium oxide and molybdenum trioxide at 120 deg.C for 12 hr.
(2) The raw material ratio is as follows: 73.41kg of aluminum powder, 84.63kg of chromium oxide and 43.43kg of molybdenum trioxide; the raw materials are put into a V-shaped mixer, the mixing speed is 130r/min, the mixing time is 5min, and the raw materials are uniformly mixed and fully contacted.
(3) And (3) loading the uniformly mixed furnace burden into a sintered corundum crucible, carrying out ignition reaction, cooling for 12 hours along with the furnace after the reaction is finished, dismantling the crucible, taking out an alloy ingot, and weighing.
(4) Removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing, carrying out magnetic separation and manual selection to obtain the aluminum-molybdenum-chromium primary alloy, and carrying out chemical component analysis on the obtained primary alloy.
Second, induction melting process
(1) The raw material ratio is as follows: 89.80kg of aluminum-molybdenum-chromium primary alloy, 9.00kg of sponge zirconium and 1.20kg of simple substance silicon; and (3) putting the primary alloy, the sponge zirconium and the simple substance silicon into a knotted and dried corundum crucible. And vacuumizing the intermediate-frequency vacuum induction smelting furnace to below 10 Pa, and removing gas impurities in the smelting furnace.
(2) And (3) power transmission smelting, wherein the initial power is 30kW, the transition power is adjusted to 60kW within 30 minutes, the stable power is adjusted to 70kW after the alloy starts to be molten, after the furnace burden is completely molten, refining is carried out for 6 minutes at 1720 ℃, the smelting furnace is vacuumized to below 10 Pa again, and gas impurities in the melt are removed.
(3) The crucible is inclined, and the melt is slowly and stably cast into the water-cooled crucible. And after the casting is finished, keeping vacuum cooling for more than 6 hours to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy (cylindrical alloy ingot).
One position of the Al-Mo-Cr-Zr-Si master alloy prepared in this example (the same position as the sampling position of example 1) was sampled and analyzed for chemical composition, and the results are shown in Table 1.
The method of example 1 is adopted to sample different parts of the aluminum molybdenum chromium zirconium silicon master alloy prepared in this example for chemical composition analysis, and the results are shown in table 5, which shows that the aluminum molybdenum chromium zirconium silicon master alloy prepared in this example has uniform and stable composition and no segregation.
Example 5
First, aluminothermic smelting process
(1) Drying aluminum powder, chromium oxide and molybdenum trioxide at 120 deg.C for 12 hr.
(2) The raw material ratio is as follows: 71.99kg of aluminum powder, 89.18kg of chromium oxide and 45.76kg of molybdenum trioxide; the raw materials are put into a V-shaped mixer, the mixing speed is 120r/min, the mixing time is 6min, and the raw materials are uniformly mixed and fully contacted.
(3) And (3) loading the uniformly mixed furnace burden into a sintered corundum crucible, carrying out ignition reaction, cooling for 12 hours along with the furnace after the reaction is finished, dismantling the crucible, taking out an alloy ingot, and weighing.
(4) Removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing, carrying out magnetic separation and manual selection to obtain the aluminum-molybdenum-chromium primary alloy, and carrying out chemical component analysis on the obtained primary alloy.
Second, induction melting process
(1) The raw material ratio is as follows: 88.50kg of aluminum-molybdenum-chromium primary alloy, 10.00kg of sponge zirconium and 1.50kg of simple substance silicon; and (3) putting the primary alloy, the sponge zirconium and the simple substance silicon into a knotted and dried corundum crucible. And vacuumizing the intermediate-frequency vacuum induction smelting furnace to below 10 Pa, and removing gas impurities in the smelting furnace.
(2) And (3) power transmission smelting, wherein the initial power is 30kW, the transition power is adjusted to 60kW within 30 minutes, the stable power is adjusted to 70kW after the alloy starts to melt, after the furnace burden is completely melted, refining is carried out for 5 minutes at 1750 ℃, the smelting furnace is vacuumized to below 10 Pa again, and gas impurities in the melt are removed.
(3) The crucible is inclined, and the melt is slowly and stably cast into the water-cooled crucible. And after the casting is finished, keeping vacuum cooling for more than 6 hours to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy (cylindrical alloy ingot).
One position of the Al-Mo-Cr-Zr-Si master alloy prepared in this example (the same position as the sampling position of example 1) was sampled and analyzed for chemical composition, and the results are shown in Table 1.
The method of example 1 is adopted to sample different parts of the aluminum molybdenum chromium zirconium silicon master alloy prepared in this example for chemical composition analysis, and the results are shown in table 6, which shows that the aluminum molybdenum chromium zirconium silicon master alloy prepared in this example has uniform and stable composition and no segregation.
TABLE 1 chemical composition of Al-Mo-Cr-Zr-Si master alloy in examples 1-5
Table 2 example 1 al-mo-cr-zr-si master alloy with different site chemistries
Table 3 example 2 al-mo-cr-zr-si master alloy different site chemistries
Table 4 example 3 al-mo-cr-zr-si master alloy with different site chemistries
TABLE 5 EXAMPLE 4 Al-Mo-Cr-Zr-Si master alloy different site chemistries
TABLE 6 EXAMPLE 5 Al-Mo-Cr-Zr-Si master alloy different site chemistries
The embodiment shows that the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy provided by the invention has the advantages of high purity, uniform and stable components, less segregation and lower content of gas phase impurities, and can better meet the production requirements of titanium alloys.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. An aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy is characterized by comprising 23.0-27.0% of Mo, 23.0-27.0% of Cr, 6.0-10.0% of Zr, 0.5-1.5% of Si and the balance of Al by mass.
2. The Al-Mo-Cr-Zr-Si master alloy according to claim 1, comprising, by mass, 24.0-26.0% of Mo, 24.0-26.0% of Cr, 7.0-9.0% of Zr, 0.8-1.2% of Si, and the balance of Al.
3. The Al-Mo-Cr-Zr-Si master alloy according to claim 1, characterized by comprising, by mass, 25.0% Mo, 25.0% Cr, 8.0% Zr, 1.0% Si and balance Al.
4. The method for preparing the Al-Mo-Cr-Zr-Si master alloy as claimed in any one of claims 1 to 3, comprising the following steps:
mixing molybdenum trioxide, chromium sesquioxide and aluminum for thermite reaction, and cooling to obtain an aluminum-molybdenum-chromium primary alloy;
and carrying out vacuum induction melting on the aluminum-molybdenum-chromium primary alloy, the sponge zirconium and the elemental silicon, and cooling to obtain the aluminum-molybdenum-chromium-zirconium-silicon intermediate alloy.
5. The preparation method according to claim 4, wherein the mass ratio of the molybdenum trioxide to the chromium oxide to the aluminum is (3.690-4.576): (7.190-8.918): (7.199-7.741).
6. The method according to claim 4 or 5, wherein the molybdenum trioxide, chromium oxide and aluminum are dried separately before mixing; the drying temperature is independently 110-130 ℃, and the time is independently more than or equal to 12 h.
7. The preparation method according to claim 4 or 5, wherein the thermite reaction is carried out at 1750-1850 ℃ for 35-45 s.
8. The method as claimed in claim 4, wherein the vacuum degree of the vacuum induction melting is less than 10 Pa.
9. The production method according to claim 4 or 8, wherein the vacuum induction melting comprises melting and refining which are performed in sequence; the refining temperature is 1650-1750 ℃ and the refining time is 5-10 min.
10. The preparation method of claim 4, further comprising the step of casting the alloy liquid obtained by the induction melting in a water-cooled copper crucible for natural cooling after the vacuum induction melting, wherein the time of the natural cooling is more than or equal to 6 hours.
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| CN115181872A (en) * | 2022-07-15 | 2022-10-14 | 承德天大钒业有限责任公司 | Aluminum tin zirconium molybdenum silicon intermediate alloy and preparation method thereof |
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| CN115094272A (en) * | 2022-07-11 | 2022-09-23 | 承德天大钒业有限责任公司 | Zirconium-nickel-copper-aluminum-tantalum intermediate alloy and preparation method thereof |
| CN115094272B (en) * | 2022-07-11 | 2023-09-12 | 承德天大钒业有限责任公司 | Zirconium-nickel-copper-aluminum-tantalum intermediate alloy and preparation method thereof |
| CN115181872A (en) * | 2022-07-15 | 2022-10-14 | 承德天大钒业有限责任公司 | Aluminum tin zirconium molybdenum silicon intermediate alloy and preparation method thereof |
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