CN112126806B - Preparation method of aluminum molybdenum chromium iron silicon intermediate alloy - Google Patents
Preparation method of aluminum molybdenum chromium iron silicon intermediate alloy Download PDFInfo
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Abstract
The invention belongs to the technical field of metal materials, and particularly relates to a preparation method of an aluminum-molybdenum-chromium-iron-silicon intermediate alloy. The preparation method comprises the following steps: (1) mixing a first aluminum source and a molybdenum source, and carrying out aluminothermic reaction to obtain an aluminum-molybdenum primary alloy; (2) and mixing the aluminum-molybdenum primary alloy with chromium, iron, silicon and a second aluminum source, and carrying out vacuum melting to obtain the aluminum-molybdenum-chromium-iron-silicon intermediate alloy. According to the invention, by selecting a method combining aluminum heating and vacuum melting, and controlling the melting of the medium-frequency vacuum induction furnace, aluminum, molybdenum, chromium, iron and silicon elements are uniformly distributed in the alloy, the content of gas phase impurities such as O, N is reduced, and the homogenization of titanium alloy components is facilitated when the TC6 titanium alloy is melted.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a preparation method of an aluminum-molybdenum-chromium-iron-silicon intermediate alloy.
Background
Titanium and its alloy have excellent properties such as high strength, corrosion resistance, high temperature resistance and good process performance, so it is increasingly an attractive material in the field of modern industrial science and technology, and has been widely used in aerospace, aviation, petroleum, chemical engineering, light industry, metallurgy, machinery and energy.
Aluminum, molybdenum, chromium, iron, silicon are the main alloying components of titanium alloys, and are usually added to titanium alloys in the form of master alloys. The titanium alloy mark of the aluminum molybdenum chromium iron silicon intermediate alloy provided by the invention is TC 6. The TC6 titanium alloy is a good martensite type two-phase titanium alloy, is mainly used for manufacturing parts such as compressor disks, blades and the like of aeroengines, can work for more than 6000 hours at a temperature of below 400 ℃ for a long time and can work for more than 2000 hours at a temperature of 450 ℃, and can also be used as a medium-strength alloy for manufacturing bearing machine members such as bulkheads, joints and the like of airplanes and fasteners for different purposes.
Currently, the preparation method of the aluminum molybdenum chromium iron silicon alloy is generally prepared by an external aluminothermic method, for example, CN1629328A discloses an aluminum molybdenum chromium iron silicon intermediate alloy and a preparation method thereof, wherein the raw materials are chromium trioxide, molybdenum trioxide, iron, silicon, aluminum and calcium fluoride, and an aluminothermic reduction reaction is performed, so as to prepare the aluminum molybdenum chromium iron silicon alloy. The method has the advantages of simple equipment, single process, convenient operation 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.
Therefore, how to provide a preparation method of an aluminum-molybdenum-chromium-iron-silicon intermediate alloy with good component uniformity and low impurity content is a technical problem which needs to be solved in the field.
Disclosure of Invention
The invention aims to provide a preparation method of an aluminum-molybdenum-chromium-iron-silicon intermediate alloy, which is characterized in that the aluminum heating and vacuum smelting are combined to be smelted in a vacuum environment, so that the uniformity of alloy components and extremely low impurity content are ensured.
In order to achieve the above object, the present invention provides the following technical solutions:
a preparation method of an aluminum molybdenum chromium iron silicon intermediate alloy comprises the following steps:
(1) mixing a first aluminum source and a molybdenum source, and carrying out aluminothermic reaction to obtain an aluminum-molybdenum primary alloy;
(2) and mixing the aluminum-molybdenum primary alloy, chromium, iron, silicon and a second aluminum source, and carrying out vacuum melting to obtain the aluminum-molybdenum-chromium-iron-silicon intermediate alloy.
Adopt above-mentioned technical scheme's beneficial effect: in the step (1), the first aluminum source and the molybdenum source are mixed to carry out aluminothermic reaction, so that the density and melting point difference of simple substances of aluminum and molybdenum can be neutralized, and the quinary alloy can be more uniform.
Preferably, before mixing the first aluminum source and the molybdenum source, drying the first aluminum source and the molybdenum source respectively; the drying temperature is 100-120 ℃, and the drying time is more than 6 hours.
Adopt above-mentioned technical scheme's beneficial effect: the drying is to make the material without water, the water can bring impurities, especially H element, which seriously affects the alloy brittleness, and the water can also make the ingot have air holes and other defects.
Preferably, the molybdenum source is molybdenum trioxide or molybdenum dioxide; the first aluminum source is aluminum powder, and the mass ratio of the aluminum powder to the molybdenum trioxide to the molybdenum dioxide is (1.958-2.038): (1.548-1.628): (0.960-1.040).
Adopt above-mentioned technical scheme's beneficial effect: the reason for using aluminum powder, molybdenum trioxide and molybdenum dioxide is that the aluminum and molybdenum trioxide can splash due to too high reaction heat, the aluminum and molybdenum dioxide have low reaction heat and are not reacted sufficiently, so that two molybdenum sources are selected to be mixed and the reaction is moderate; the aluminum-molybdenum primary alloy produced according to the proportion has a low melting point, the melting point and the density are closer to those of other metal simple substances, and the burning loss and segregation can be reduced during smelting.
Preferably, the thermite reaction is carried out at 1950-2250 ℃ for 35-45 s.
Adopt above-mentioned technical scheme's beneficial effect: if the thermite reaction temperature is too high, splashing can occur; and the reaction is insufficient and the slag iron is not separated due to the excessively low temperature.
Preferably, the second aluminum source is aluminum beans, and the mass ratio of the first aluminum source to the second aluminum source is (0.965-1.035): (1.850-1.920).
Preferably, the vacuum melting is carried out in a medium-frequency vacuum induction furnace; the vacuum degree of the vacuum melting is less than 10 Pa.
Adopt above-mentioned technical scheme's beneficial effect: the vacuum melting avoids introducing impurities, especially gas impurities.
Preferably, the vacuum melting comprises melting and refining which are carried out in sequence;
adopt above-mentioned technical scheme's beneficial effect: the refining is to ensure that the alloy is melted more fully and uniformly and has the functions of purification and impurity removal.
The initial power of melting process is 35 ~ 45kW, and transition power is 50 ~ 65kW, and steady power is 65 ~ 75 kW.
Adopt above-mentioned technical scheme's beneficial effect: the power is gradually increased, the safety and the power saving are better, and the damage to the furnace and various appliances in the furnace is low. By controlling the stable power, the refining temperature is slightly higher than the melting point of the alloy, so as to achieve the refining purpose.
Preferably, the refining temperature is 1750-1850 ℃ and the refining time is 4-7 min.
Preferably, the aluminum-molybdenum-chromium-iron-silicon intermediate alloy comprises the following components in percentage by mass: 22.0-24.0% of Mo, 13.0-15.0% of Cr, 3.0-5.0% of Fe, 2.0-4.0% of Si, and the balance of Al; wherein the impurities C is less than or equal to 0.05 percent, O is less than or equal to 0.03 percent, N is less than or equal to 0.005 percent, H is less than or equal to 0.005 percent, and S is less than or equal to 0.005 percent.
Preferably, the aluminum-molybdenum-chromium-iron-silicon intermediate alloy comprises the following components in percentage by mass: 22.5-23.5% of Mo, 13.5-14.5% of Cr, 3.5-4.5% of Fe, 2.5-3.5% of Si and the balance of Al; wherein the impurities C is less than or equal to 0.05 percent, O is less than or equal to 0.03 percent, N is less than or equal to 0.005 percent, H is less than or equal to 0.005 percent, and S is less than or equal to 0.005 percent.
Compared with the prior art, the invention provides a preparation method of the aluminum-molybdenum-chromium-iron-silicon intermediate alloy, which has the advantages that the aluminum-molybdenum-chromium-iron-silicon intermediate alloy has smaller component segregation by controlling the raw material proportion, and the component segregation of the titanium alloy is prevented when the TC6 titanium alloy is smelted; by controlling the smelting of the medium-frequency vacuum induction furnace, the elements of aluminum, molybdenum, chromium, iron and silicon are uniformly distributed in the alloy, the content of gas-phase impurities such as O, N is reduced, and the homogenization of titanium alloy components is facilitated when the TC6 titanium alloy is smelted. The aluminum molybdenum ferrochrome silicon intermediate alloy prepared by the invention is matched with TC6 titanium alloy components, and the performance of the titanium alloy TC6 is optimal.
The preparation method of the aluminum-molybdenum-chromium-iron-silicon intermediate alloy provided by the invention can optimize the batching process of titanium alloy preparation, realizes accurate batching in the TC6 titanium alloy production process, has a simple preparation process, is easy to control, and is suitable for large-scale industrial production.
Detailed Description
The embodiment of the invention provides a preparation method of an aluminum molybdenum ferrochrome silicon intermediate alloy, which comprises the following steps:
mixing a first aluminum source and a molybdenum source, and carrying out aluminothermic reaction to obtain an aluminum-molybdenum primary alloy;
and mixing the aluminum-molybdenum primary alloy, chromium, iron, silicon and a second aluminum source, and carrying out vacuum melting to obtain the aluminum-molybdenum-chromium-iron-silicon intermediate alloy.
In the embodiment provided by the invention, a first aluminum source and a molybdenum source are mixed and subjected to aluminothermic reaction to obtain the aluminum-molybdenum primary alloy.
In order to further optimize the technical scheme, the first aluminum source and the molybdenum source are dried before being mixed, wherein the drying temperature is 100-120 ℃, preferably 110 ℃, and the time is more than 6 hours.
Further, the drying method is not particularly limited, and the above temperature and time may be set. Meanwhile, the drying arranged in the embodiment can remove water in the first aluminum source and the molybdenum source, and prevent the hydrogen evolution phenomenon in the smelting process.
In order to further optimize the technical scheme, the first aluminum source is preferably aluminum powder, the molybdenum source is molybdenum trioxide and molybdenum dioxide, and the molybdenum source is a powdery raw material; the mass ratio of the aluminum powder to the molybdenum trioxide to the molybdenum dioxide is (1.958-2.038): (1.548-1.628): (0.960-1.040), preferably 1.998: 1.588: 1.000. the invention controls the mass ratio of the first aluminum source and the molybdenum source, thereby controlling the mass ratio of aluminum to molybdenum in the aluminum-molybdenum primary alloy and further obtaining different aluminum-molybdenum primary alloys, for example, in the specific embodiment of the invention, the mass ratio of aluminum powder to molybdenum trioxide to molybdenum dioxide is set to be 1.998: 1.588: 1.000, the Al-Mo 65 primary alloy is obtained after thermite reaction, the stability of the Al-Mo 65 primary alloy is high, and the Al-Mo 65 primary alloy is also most suitable on a phase diagram.
Further, the mixing method is not particularly limited, and the method well known in the art can ensure that the first aluminum source and the molybdenum source 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 110-130 r/min, preferably 120r/min, and the mixing time is preferably 3-5 min, and more preferably 4 min. The first aluminum source and the molybdenum source are fully contacted through mixing, so that the subsequent aluminothermic reaction is facilitated.
In order to further optimize the above technical solution, after the first aluminum source and the molybdenum source are mixed, the present invention preferably ignites the obtained mixed powder to initiate an aluminothermic reaction; the operation of the ignition in the embodiment of the present invention is not particularly limited, and the ignition method for initiating the thermite reaction, which is well known in the art, may be adopted. In the embodiment of the invention, the thermite reaction temperature is preferably 1950-2250 ℃, preferably 2100 ℃, and the time is preferably 35-45 s, preferably 40 s.
Further, the reaction device for the thermite reaction is not particularly limited, and a thermite reaction device well known in the art can be adopted; 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; the furnace body used in the embodiment of the invention has good heat insulation effect and does not introduce impurities. In the thermite reaction process of the embodiment, aluminum is used as a reducing agent to reduce molybdenum trioxide and molybdenum dioxide into metal simple substance molybdenum, aluminum is oxidized into aluminum oxide, and a large amount of heat energy is released to melt the metal (the 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 aluminum-molybdenum alloy liquid, and is separated from the aluminum-molybdenum alloy liquid and removed. The examples are not particularly limited as to the separation and removal processes, and those known to those skilled in the art may be selected.
In order to further optimize the technical scheme, after the thermite reaction is finished, the obtained aluminum-molybdenum alloy liquid is preferably cooled. In the embodiment of the invention, the cooling mode is preferably furnace cooling; and (5) cooling and discharging to obtain the aluminum-molybdenum primary alloy.
In order to further optimize the technical scheme, after the aluminum-molybdenum primary alloy is obtained, the aluminum-molybdenum primary alloy, chromium, iron, silicon and a second aluminum source are mixed and subjected to vacuum melting to obtain the aluminum-molybdenum-chromium-iron-silicon intermediate alloy. In the embodiment of the invention, the chromium, the iron and the silicon are preferably blocky simple substances with the content of more than 99.5 percent corresponding to each element; the second aluminum source is preferably aluminum beans, and the mass ratio of the first aluminum source to the second aluminum source is preferably (0.965-1.035): (1.850-1.920), preferably 1: 1.885. the mixing process in the embodiment of the present invention is not particularly limited, and the raw materials can be uniformly mixed by selecting a process known to those skilled in the art.
In order to further optimize the technical scheme, before vacuum melting, the embodiment of the invention preferably performs finishing crushing and component analysis on the aluminum-molybdenum primary alloy; the method for the finish crushing and the composition analysis is not particularly limited, and a corresponding method well known in the art may be employed. After finishing the finishing crushing and the component analysis, the obtained alloy is not subjected to any treatment, and the obtained crushed alloy is directly used for vacuum melting. In the embodiment of the invention, the adding amount of the aluminum-molybdenum primary alloy, the chromium, the iron, the silicon and the second aluminum source in the vacuum melting is preferably determined according to the analysis result of the components of the aluminum-molybdenum primary alloy and the mass content of each metal element in the needed aluminum-molybdenum-chromium-iron-silicon intermediate alloy.
In the embodiment provided by the invention, the vacuum melting is preferably carried out in a medium-frequency vacuum induction furnace; the degree of vacuum in the vacuum melting is preferably < 10 Pa. Vacuum melting in embodiments of the present invention preferably includes melting and refining in sequence. In the embodiment of the present invention, the melting process is preferably: adjusting the power of the medium-frequency vacuum induction furnace to the initial power to start heating, and increasing the power to the transition power after 20min to heat the metal raw material to start melting; and then the power is increased to the stable power and heated until the metal raw materials are completely melted, so as to obtain the mixed melt. Meanwhile, the initial power is preferably 35-45 kW, and preferably 40 kW; the transition power is preferably 50-65 kW, and preferably 60 kW; the stable power is preferably 65-75 kW, and is preferably 70 kW.
In order to further optimize the above technical solution, after the melting is completed, the embodiment of the present invention preferably refines the obtained mixed melt. In the embodiment of the invention, the refining temperature is preferably 1750-1850 ℃, preferably 1800 ℃, and the time is preferably 4-7 min, preferably 5 min. In the refining process, the power of the medium-frequency vacuum induction furnace is preferably 75-85 kW, and is preferably 80 kW. In the embodiment of the invention, the refining can remove impurities and gases in the mixed melt to obtain pure alloy liquid.
In order to further optimize the technical scheme, after the vacuum melting is completed, the alloy liquid obtained in the embodiment of the invention is preferably cooled. In the embodiment of the invention, the cooling mode is preferably furnace cooling after casting; the embodiment of the invention has no special limitation on the pouring operation, and the pouring method well known in the field can be adopted; the cooling termination temperature is preferably 150 ℃ or lower. And cooling and discharging to obtain the aluminum-molybdenum-chromium-iron-silicon intermediate alloy.
According to the preparation method provided by the embodiment of the invention, the melting point difference and the density difference among elements are neutralized, the problems of element burning loss caused by the melting point difference, uneven components caused by the density difference and the like in the smelting process are solved, the uniform stability of the components of the aluminum-molybdenum-chromium-iron-silicon intermediate alloy can be improved, the content of O, N and other impurities is reduced by refining, the process is simple, the control is easy, and the preparation method is suitable for large-scale industrial production.
The aluminum molybdenum ferrochrome silicon intermediate alloy prepared by the embodiment of the invention comprises the following components in parts by mass:
22.0-24.0% of Mo, 13.0-15.0% of Cr, 3.0-5.0% of Fe, 2.0-4.0% of Si, the balance of Al and inevitable impurities, wherein C is less than or equal to 0.05%, O is less than or equal to 0.03%, N is less than or equal to 0.005%, H is less than or equal to 0.005%, and S is less than or equal to 0.005%.
In the examples of the present invention, the required raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
The aluminum molybdenum ferrochrome silicon intermediate alloy prepared by the embodiment of the invention comprises, by mass, 22.0-24.0% of Mo22.5-23.5%, preferably 23.0%. According to the embodiment of the invention, Mo is added to improve the room temperature and high temperature strength of the titanium alloy, and the hardenability is increased.
The aluminum molybdenum chromium iron silicon intermediate alloy prepared by the embodiment of the invention comprises 13.0-15.0% of Cr13.5-14.5% of Cr0 by mass fraction, preferably 14.0% of Cr0 by mass fraction. According to the embodiment of the invention, the titanium alloy has high strength and good plasticity by adding Cr, and can be strengthened by heat treatment.
The aluminum molybdenum chromium iron silicon intermediate alloy prepared by the embodiment of the invention comprises, by mass, 3.0-5.0% of FeC, preferably 3.5-4.5%, and preferably 4.0%. According to the embodiment of the invention, the stiffness ratio of the titanium alloy can be improved by adding a small amount of Fe.
The aluminum molybdenum chromium iron silicon intermediate alloy prepared by the embodiment of the invention comprises, by mass, 2.0-4.0% of Si, preferably 2.5-3.5%, and preferably 3.0%. According to the embodiment of the invention, the heat resistance of the titanium alloy is improved by adding Si.
The aluminum molybdenum ferrochrome silicon intermediate alloy prepared by the embodiment of the invention comprises Al allowance and inevitable impurities. Wherein, Al element can improve the room temperature and high temperature strength and heat strength of the titanium alloy.
According to the embodiment provided by the invention, the aluminum-molybdenum-chromium-iron-silicon intermediate alloy has smaller component segregation by controlling the raw material proportion, the aluminum, molybdenum, chromium, iron and silicon elements are uniformly distributed in the alloy by controlling the smelting of the medium-frequency vacuum induction furnace, the content of gas-phase impurities such as O, N and the like is reduced, the melting point difference and the density difference among the elements are neutralized, the problems of element burning loss caused by the melting point difference, component unevenness caused by the density difference and the like in the smelting process are avoided, the aluminum-molybdenum-chromium-iron-silicon intermediate alloy has smaller component segregation, the titanium alloy component homogenization is facilitated when the TC6 titanium alloy is smelted, the component segregation is prevented, the batching process in the smelting of the TC6 titanium alloy is optimized, the accurate batching in the production process can be realized, and the preparation of the titanium alloy is facilitated.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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
One, aluminothermic reaction smelting process
(1) Drying aluminum powder, molybdenum trioxide and molybdenum dioxide at the temperature of 110 ℃ for 12 h;
(2) calculating the mass ratio of the alloy in the aluminothermic smelting process according to the mass fractions of molybdenum in molybdenum trioxide and molybdenum dioxide and the aluminum consumption of the molybdenum trioxide and the molybdenum dioxide in the chemical reaction: the mass ratio of aluminum powder to molybdenum trioxide to molybdenum dioxide is 1.998: 1.588: 1.000;
(3) aluminum powder, molybdenum trioxide and molybdenum dioxide are filled into a mixer to be mixed for 4min at the speed of 120 r/min;
(4) preheating the mixed aluminum powder, molybdenum trioxide and molybdenum dioxide to the charging temperature of 43 ℃, igniting and smelting, wherein the reaction temperature is 1950-2250 ℃, the reaction time is 35-45 seconds, and discharging after 24 hours to obtain the aluminum-molybdenum 65 primary alloy.
Proportioning in vacuum smelting process
After the first-grade aluminum-molybdenum 65 alloy is obtained, the first-grade aluminum-molybdenum alloy is finished and crushed, and the smelting process proportion is calculated according to the component requirements of the required intermediate alloy after the components are analyzed: 24.1kg of aluminum beans, 16.9kg of aluminum-molybdenum 65 primary alloy, 6.5kg of metal chromium, 1.5kg of high-purity iron and 1.0kg of metal silicon; according to the mass percentage, the first-grade aluminum-molybdenum alloy contains 65.00 percent of Mo, 0.004 percent of C, 0.001 percent of H, 0.015 percent of O, 0.004 percent of N, 0.003 percent of S and the balance of Al.
Third, preparation before power transmission
(1) Starting a circulating water pump, checking whether the pipelines have leakage or not, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper;
(2) checking whether the power system is normal or not, and if the power system is abnormal, maintaining in time;
(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, and when the pressure is pumped to 30Pa, transmitting power for smelting;
(2) power is transmitted, and the initial power is 40 kW;
(3) after 20min, adjusting the power to 60 kW;
(4) after the alloy is melted by naked eyes, the power is adjusted to 70 kW;
(5) after the alloy is melted, the power is increased to 80kW, refining is carried out for 7min at 1750 ℃, and pouring is carried out.
And fourthly, cooling and discharging to obtain the aluminum-molybdenum-chromium-iron-silicon 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-Cr-Fe-Si intermediate alloy ingot (cylinder) prepared in this example was sampled at different positions and analyzed for chemical composition, two points, numbered 1 and 2 respectively, were taken from the upper surface of the ingot and 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 and analyzed for composition, and the results are shown in Table 1. As can be seen from Table 1, the Al-Mo-Cr-Fe-Si master alloy C, O, N prepared by the embodiment has low impurity content, uniform and stable components and no segregation.
TABLE 1 EXAMPLE 1 chemical composition of different sites of Al-Mo-Cr-Fe-Si master alloy
Example 2
One, aluminothermic reaction smelting process
(1) Drying aluminum powder, molybdenum trioxide and molybdenum dioxide at the temperature of 110 ℃ for 12 h;
(2) calculating the mass ratio of the alloy in the aluminothermic smelting process according to the mass fractions of molybdenum in molybdenum trioxide and molybdenum dioxide and the aluminum consumption of the molybdenum trioxide and the molybdenum dioxide in the chemical reaction: the mass ratio of aluminum powder to molybdenum trioxide to molybdenum dioxide is 1.998: 1.588: 1.000;
(3) aluminum powder, molybdenum trioxide and molybdenum dioxide are filled into a mixer to be mixed for 4min at the speed of 120 r/min;
(4) preheating the mixed aluminum powder, molybdenum trioxide and molybdenum dioxide to the charging temperature of 43 ℃, igniting and smelting, wherein the reaction temperature is 1950-2250 ℃, the reaction time is 35-45 seconds, and discharging after 24 hours to obtain the aluminum-molybdenum 65 primary alloy.
Proportioning in vacuum smelting process
After the first-grade aluminum-molybdenum 65 alloy is obtained, the first-grade aluminum-molybdenum alloy is finished and crushed, and the smelting process proportion is calculated according to the component requirements of the required intermediate alloy after the components are analyzed: 22.9kg of aluminum beans, 17.3kg of aluminum-molybdenum 65 primary alloy, 6.75kg of metal chromium, 1.75kg of high-purity iron and 1.25kg of metal silicon; according to the mass percentage, the first-grade aluminum-molybdenum alloy contains 65.00 percent of Mo, 0.004 percent of C, 0.001 percent of H, 0.015 percent of O, 0.004 percent of N, 0.003 percent of S and the balance of Al.
Third, preparation before power transmission
(1) Starting a circulating water pump, checking whether the pipelines have leakage or not, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper;
(2) checking whether the power system is normal or not, and if the power system is abnormal, maintaining in time;
(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, and when the pressure is pumped to 30Pa, transmitting power for smelting;
(2) power is transmitted, and the initial power is 40 kW;
(3) after 20min, adjusting the power to 60 kW;
(4) after the alloy is melted by naked eyes, the power is adjusted to 70 kW;
(5) after the alloy is melted, the power is increased to 80kW, refining is carried out for 6min at 1750 ℃, and pouring is carried out.
And fourthly, cooling and discharging to obtain the aluminum-molybdenum-chromium-iron-silicon 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-Cr-Fe-Si 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 and 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 and analyzed for components, and the results are shown in Table 2. As can be seen from Table 2, the Al-Mo-Cr-Fe-Si master alloy C, O, N prepared by the embodiment has low impurity content, uniform and stable components and no segregation.
TABLE 2 EXAMPLE 2 chemical composition of different sites of Al-Mo-Cr-Fe-Si master alloy
Example 3
One, aluminothermic reaction smelting process
(1) Drying aluminum powder, molybdenum trioxide and molybdenum dioxide at the temperature of 110 ℃ for 12 h;
(2) calculating the mass ratio of the alloy in the aluminothermic smelting process according to the mass fractions of molybdenum in molybdenum trioxide and molybdenum dioxide and the aluminum consumption of the molybdenum trioxide and the molybdenum dioxide in the chemical reaction: the mass ratio of aluminum powder to molybdenum trioxide to molybdenum dioxide is 1.998: 1.588: 1.000;
(3) aluminum powder, molybdenum trioxide and molybdenum dioxide are filled into a mixer to be mixed for 4min at the speed of 120 r/min;
(4) preheating the mixed aluminum powder, molybdenum trioxide and molybdenum dioxide to the charging temperature of 43 ℃, igniting and smelting, wherein the reaction temperature is 1950-2250 ℃, the reaction time is 35-45 seconds, and discharging after 24 hours to obtain the aluminum-molybdenum 65 primary alloy.
Proportioning in vacuum smelting process
After the first-grade aluminum-molybdenum 65 alloy is obtained, the first-grade aluminum-molybdenum alloy is finished and crushed, and the smelting process proportion is calculated according to the component requirements of the required intermediate alloy after the components are analyzed: 21.8kg of aluminum beans, 17.7kg of aluminum-molybdenum 65 primary alloy, 7.0kg of metal chromium, 2.0kg of high-purity iron and 1.5kg of metal silicon; according to the mass percentage, the first-grade aluminum-molybdenum alloy contains 65.00 percent of Mo, 0.004 percent of C, 0.001 percent of H, 0.015 percent of O, 0.004 percent of N, 0.003 percent of S and the balance of Al.
Third, preparation before power transmission
(1) Starting a circulating water pump, checking whether the pipelines have leakage or not, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper;
(2) checking whether the power system is normal or not, and if the power system is abnormal, maintaining in time;
(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, and when the pressure is pumped to 30Pa, transmitting power for smelting;
(2) power is transmitted, and the initial power is 40 kW;
(3) after 20min, adjusting the power to 60 kW;
(4) after the alloy is melted by naked eyes, the power is adjusted to 70 kW;
(5) after the alloy is melted, the power is increased to 80kW, and the alloy is refined for 5min at 1800 ℃ and poured.
And fourthly, cooling and discharging to obtain the aluminum-molybdenum-chromium-iron-silicon 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-Cr-Fe-Si 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 and 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 and analyzed for components, and the results are shown in Table 3. As can be seen from Table 3, the Al-Mo-Cr-Fe-Si master alloy C, O, N prepared by the embodiment has low impurity content, uniform and stable components and no segregation.
TABLE 3 EXAMPLE 3 chemical composition of different sites of Al-Mo-Cr-Fe-Si master alloy
Example 4
One, aluminothermic reaction smelting process
(1) Drying aluminum powder, molybdenum trioxide and molybdenum dioxide at the temperature of 110 ℃ for 12 h;
(2) calculating the mass ratio of the alloy in the aluminothermic smelting process according to the mass fractions of molybdenum in molybdenum trioxide and molybdenum dioxide and the aluminum consumption of the molybdenum trioxide and the molybdenum dioxide in the chemical reaction: the mass ratio of aluminum powder to molybdenum trioxide to molybdenum dioxide is 1.998: 1.588: 1.000;
(3) aluminum powder, molybdenum trioxide and molybdenum dioxide are filled into a mixer to be mixed for 4min at the speed of 120 r/min;
(4) preheating the mixed aluminum powder, molybdenum trioxide and molybdenum dioxide to the charging temperature of 43 ℃, igniting and smelting, wherein the reaction temperature is 1950-2250 ℃, the reaction time is 35-45 seconds, and discharging after 24 hours to obtain the aluminum-molybdenum 65 primary alloy.
Proportioning in vacuum smelting process
After the first-grade aluminum-molybdenum 65 alloy is obtained, the first-grade aluminum-molybdenum alloy is finished and crushed, and the smelting process proportion is calculated according to the component requirements of the required intermediate alloy after the components are analyzed: 20.7kg of aluminum beans, 18.1kg of aluminum-molybdenum 65 primary alloy, 7.25kg of metal chromium, 2.25kg of high-purity iron and 1.75kg of metal silicon; according to the mass percentage, the first-grade aluminum-molybdenum alloy contains 65.00 percent of Mo, 0.004 percent of C, 0.001 percent of H, 0.015 percent of O, 0.004 percent of N, 0.003 percent of S and the balance of Al.
Third, preparation before power transmission
(1) Starting a circulating water pump, checking whether the pipelines have leakage or not, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper;
(2) checking whether the power system is normal or not, and if the power system is abnormal, maintaining in time;
(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, and when the pressure is pumped to 30Pa, transmitting power for smelting;
(2) power is transmitted, and the initial power is 40 kW;
(3) after 20min, adjusting the power to 60 kW;
(4) after the alloy is melted by naked eyes, the power is adjusted to 70 kW;
(5) after the alloy is melted, the power is increased to 80kW, and the alloy is refined for 5min at 1850 ℃ and cast.
And fourthly, cooling and discharging to obtain the aluminum-molybdenum-chromium-iron-silicon 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-Cr-Fe-Si intermediate alloy ingot (cylinder) prepared in this example was sampled at different positions and analyzed for chemical composition, two points, numbered 1 and 2 respectively, were taken from the upper surface of the ingot and 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 and analyzed for composition, and the results are shown in Table 4. As can be seen from Table 4, the Al-Mo-Cr-Fe-Si master alloy C, O, N prepared by the embodiment has low impurity content, uniform and stable components and no segregation.
TABLE 4 EXAMPLE 4 chemical composition of different sites of Al-Mo-Cr-Fe-Si master alloy
Example 5
One, aluminothermic reaction smelting process
(1) Drying aluminum powder, molybdenum trioxide and molybdenum dioxide at the temperature of 110 ℃ for 12 h;
(2) calculating the mass ratio of the alloy in the aluminothermic smelting process according to the mass fractions of molybdenum in molybdenum trioxide and molybdenum dioxide and the aluminum consumption of the molybdenum trioxide and the molybdenum dioxide in the chemical reaction: the mass ratio of aluminum powder to molybdenum trioxide to molybdenum dioxide is 1.998: 1.588: 1.000;
(3) aluminum powder, molybdenum trioxide and molybdenum dioxide are filled into a mixer to be mixed for 4min at the speed of 120 r/min;
(4) preheating the mixed aluminum powder, molybdenum trioxide and molybdenum dioxide to the charging temperature of 43 ℃, igniting and smelting, wherein the reaction temperature is 1950-2250 ℃, the reaction time is 35-45 seconds, and discharging after 24 hours to obtain the aluminum-molybdenum 65 primary alloy.
Proportioning in vacuum smelting process
After the first-grade aluminum-molybdenum 65 alloy is obtained, the first-grade aluminum-molybdenum alloy is finished and crushed, and the smelting process proportion is calculated according to the component requirements of the required intermediate alloy after the components are analyzed: 19.5kg of aluminum beans, 18.5kg of aluminum-molybdenum 65 primary alloy, 7.5kg of metal chromium, 2.5kg of high-purity iron and 2.0kg of metal silicon; according to the mass percentage, the first-grade aluminum-molybdenum alloy contains 65.00 percent of Mo, 0.004 percent of C, 0.001 percent of H, 0.015 percent of O, 0.004 percent of N, 0.003 percent of S and the balance of Al.
Third, preparation before power transmission
(1) Starting a circulating water pump, checking whether the pipelines have leakage or not, and adjusting the water quantity distribution of each pipeline to be proper and the pressure to be proper;
(2) checking whether the power system is normal or not, and if the power system is abnormal, maintaining in time;
(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, and when the pressure is pumped to 30Pa, transmitting power for smelting;
(2) power is transmitted, and the initial power is 40 kW;
(3) after 20min, adjusting the power to 60 kW;
(4) after the alloy is melted by naked eyes, the power is adjusted to 70 kW;
(5) after the alloy is melted, the power is increased to 80kW, refining is carried out for 4min at 1850 ℃, and casting is carried out.
And fourthly, cooling and discharging to obtain the aluminum-molybdenum-chromium-iron-silicon 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-Cr-Fe-Si 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 and 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 and analyzed for components, and the results are shown in Table 5. As can be seen from Table 5, the Al-Mo-Cr-Fe-Si master alloy C, O, N prepared by the present embodiment has low impurity content, uniform and stable composition, and no segregation.
TABLE 5 EXAMPLE 5 chemical composition of different sites of Al-Mo-Cr-Fe-Si master alloy
One position of the al-mo-cr-fe-si intermediate alloy ingot (cylinder) prepared in examples 1 to 5 was sampled by a conventional analysis method for chemical component analysis, and the results are shown in table 6. As can be seen from Table 6, the Al-Mo-Cr-Fe-Si master alloys C, O, N prepared in examples 1-5 have low impurity levels.
TABLE 6 examples 1-5 chemical compositions of Al-Mo-Cr-Fe-Si master alloys
The embodiment shows that the aluminum molybdenum ferrochrome silicon intermediate alloy prepared by the method provided by the invention has uniform and stable components and low impurity content, so that the method is beneficial to the homogenization of titanium alloy components, prevents component segregation, optimizes the batching process in titanium alloy smelting and can realize accurate batching in the production process when being used as a raw material for producing titanium alloy. Moreover, the preparation method provided by the invention is simple and easy to operate, the preparation process is stable and controllable, and the alloy forming state is good.
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 (9)
1. A preparation method of an aluminum molybdenum chromium iron silicon intermediate alloy is characterized by comprising the following steps:
(1) mixing a first aluminum source and a molybdenum source, and carrying out aluminothermic reaction to obtain an aluminum-molybdenum primary alloy;
(2) mixing the aluminum-molybdenum primary alloy with chromium, iron, silicon and a second aluminum source, and carrying out vacuum melting to obtain an aluminum-molybdenum-chromium-iron-silicon intermediate alloy;
the aluminum-molybdenum-chromium-iron-silicon intermediate alloy comprises the following components in percentage by mass:
22.0-24.0% of Mo, 13.0-15.0% of Cr, 3.0-5.0% of Fe, 2.0-4.0% of Si, and the balance of Al; wherein, the impurities C is less than or equal to 0.05 percent, O is less than or equal to 0.03 percent, N is less than or equal to 0.005 percent, H is less than or equal to 0.005 percent, and S is less than or equal to 0.005 percent.
2. The production method according to claim 1, characterized in that the first aluminum source and the molybdenum source are separately dried before being mixed; the drying temperature is 100-120 ℃, and the drying time is more than 6 hours.
3. The production method according to claim 1, wherein the molybdenum source is molybdenum trioxide and molybdenum dioxide; the first aluminum source is aluminum powder, and the mass ratio of the aluminum powder to the molybdenum trioxide to the molybdenum dioxide is (1.958-2.038): (1.548-1.628): (0.960-1.040).
4. The method of claim 1, wherein the thermite reaction is performed at 1950-2250 ℃ for 35-45 s.
5. The preparation method according to claim 3, wherein the second aluminum source is aluminum beans, and the mass ratio of the first aluminum source to the second aluminum source is (0.965-1.035): (1.850-1.920).
6. The method of manufacturing according to claim 1, wherein the vacuum melting is performed in a medium frequency vacuum induction furnace; the vacuum degree of the vacuum melting is less than 10 Pa.
7. The production method according to claim 6, wherein the vacuum melting comprises melting and refining in this order;
the initial power of melting process is 35 ~ 45kW, and transition power is 50 ~ 65kW, and steady power is 65 ~ 75 kW.
8. The method of claim 7, wherein the refining is carried out at 1750-1850 ℃ for 4-7 min.
9. The method according to any one of claims 1 to 8, wherein the Al-Mo-Cr-Fe-Si master alloy comprises the following components in parts by mass: 22.5-23.5% of Mo, 13.5-14.5% of Cr, 3.5-4.5% of Fe, 2.5-3.5% of Si and the balance of Al; wherein the impurities C is less than or equal to 0.05 percent, O is less than or equal to 0.03 percent, N is less than or equal to 0.005 percent, H is less than or equal to 0.005 percent, and S is less than or equal to 0.005 percent.
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Denomination of invention: A preparation method of Al Mo CR Fe Si master alloy Effective date of registration: 20220620 Granted publication date: 20210709 Pledgee: China Construction Bank Corporation Chengde high tech Zone sub branch Pledgor: CHENGDE TIANDA VANADIUM INDUSTRY Co.,Ltd. Registration number: Y2022130000037 |