CN108004422B - Preparation method of high-quality aluminum-zirconium alloy rod - Google Patents
Preparation method of high-quality aluminum-zirconium alloy rod Download PDFInfo
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- CN108004422B CN108004422B CN201711219305.1A CN201711219305A CN108004422B CN 108004422 B CN108004422 B CN 108004422B CN 201711219305 A CN201711219305 A CN 201711219305A CN 108004422 B CN108004422 B CN 108004422B
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Abstract
The invention provides a high-qualityA preparation method of an aluminum-zirconium alloy rod belongs to the technical field of preparation of refiners. The invention adopts a variable frequency induction furnace and a medium frequency induction furnace to produce the aluminum zirconium alloy, the aluminum liquid is refined before feeding, and the mixture of villiaumite and diffusant is added as the ZrAl alloy in the alloying process3Nucleating agent of particle, ZrAl formed after alloying3The particles are fine and are distributed more uniformly, and ZrAl is eliminated3The mass point is formed into a rod shape, and the ZrAl is effectively controlled by adding a diffusant into a fluorine salt mixture3The aggregation of mass points and the mechanical stirring in the alloying process effectively prevent ZrAl3The growth of particles and the separation and purification effect of the fluoride salt slag and the alloy are improved, and the ZrAl in the product produced by the method is verified and analyzed3Small mass point, even and dispersed distribution and extremely low slag content, and effectively solves the problem that the waffle-shaped aluminum-zirconium alloy ZrAl on the current market is3Large mass point, serious segregation, unstable deformation structure of the aluminum alloy and poor comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of aluminum zirconium alloy rod preparation, and relates to a preparation method of a high-quality aluminum zirconium alloy rod.
Background
In the fifty years of the 20 th century, the scientists of former Soviet Union, the NEN, Fridelianjiel added zirconium element to Al-Zn-Mg-Cu alloy for the first time, and successfully developed the B96 Ц alloy, and the research on zirconium element started a hot tide in the seventies, and the research on the application of zirconium element in Al-Zn-Mg and Al-Zn-Mg-Cu alloys represented by N.Ryum and E.Nes and the research on the zirconium element in Al-Zn-Mg and Al-Zn-Mg-Cu alloys represented by H.Yoshida, A.K.Mukhopadhay, E.A.Starke and the like.
The zirconium element has a significant effect in each aluminum alloy. In Al-Cu, Al-Li, Al-Cu-Li and Al-Li-Cu-Mg alloys, zirconium is used as a trace element to promote the nucleation of each strengthening phase. In Al-Mn and Al-Cu-Mg alloys, the zirconium element obviously slows down the process of the early stage of aging precipitation. In Al-Zn-Mg and Al-Zn-Mg-Cu alloys, the trace element zirconium has more remarkable effect: inhibit recrystallization, raise the recrystallization temperature of the alloy and improve the strength, fracture toughness and stress corrosion resistance of the alloy. Currently, zirconium is most used in the Al-Zn-Mg-Cu alloy system. In recent years, with the intensive research and wide application of Sc element, Sc and Zr elements are jointly added, so that the Sc-containing alloy not only can maintain all beneficial properties of the Sc-containing alloy, but also has higher thermal stability. This has become a new trend for the currently developed applications of the zirconium element.
Zirconium metal is an important strategic material, and has good plasticity and strong corrosion resistance. Zirconium also has special nuclear properties and good radiation resistance, and zirconium still has good gas absorption at high temperature, so that zirconium becomes an important material for atomic energy, electronics, chemical engineering, metallurgy and national defense departments. However, the waffle aluminum zirconium alloy ZrAl on the market at present3Large mass point, serious segregation, unstable deformation structure of the aluminum alloy and poor comprehensive performance.
Disclosure of Invention
The invention provides a preparation method of a high-quality aluminum-zirconium alloy rod, which solves the problem that the waffle-shaped aluminum-zirconium alloy rod ZrAl on the market in the prior art3Large mass point, serious segregation, unstable deformation structure of the aluminum alloy and poor comprehensive performance.
The technical scheme of the invention is realized as follows:
a preparation method of a high-quality aluminum-zirconium alloy rod comprises the following steps:
(1) burdening and mixing: weighing potassium fluorozirconate and a dispersing agent according to the weight parts, adding the potassium fluorozirconate and the dispersing agent into a mixer, and mixing for 30min to prepare a villiaumite mixture;
(2) alloying in the first step: weighing aluminum ingots according to the weight parts, putting the aluminum ingots into a variable frequency induction furnace, heating to 800-850 ℃, adding a refining agent into molten aluminum to refine the molten aluminum, starting a mechanical stirrer and a feeder for the variable frequency induction furnace to uniformly add 46-55% of a fluorine salt mixture into the molten aluminum of the variable frequency induction furnace, and stirring for 60-90 min to obtain an aluminum-zirconium alloy liquid;
(3) alloying in the second step: starting the variable frequency induction furnace and enabling the variable frequency induction furnace to be in a stirring frequency range, adjusting the power of the variable frequency induction furnace for stirring, starting the environment-friendly equipment and the stirring device, uniformly adding a 45-54% fluorine salt mixture into molten aluminum of the variable frequency induction furnace through a feeder, wherein the feeding time is 10-30 min, the reaction temperature of the molten aluminum is 800-950 ℃ by adjusting the power and the feeding speed of the variable frequency induction furnace, and after the feeding is finished for 20-40 min; adjusting the power of a variable frequency induction furnace, keeping the temperature of the aluminum liquid at 800-950 ℃, continuing stirring for 10-20 min, switching the variable frequency induction furnace to a heating frequency band, keeping the temperature for 5-10 min, stopping the furnace, pouring a fluoride salt slag water layer on the upper layer in the furnace, adding a proper amount of slag cleaning agent into the aluminum zirconium alloy liquid, and removing scum on the surface of the alloy liquid after stirring uniformly;
(4) degassing and refining: transferring the metal liquid after slag removal into a refining casting furnace, starting a variable frequency induction furnace to reach the maximum power, heating to 800-1000 ℃, shoveling the furnace wall, performing rotary degassing by using a rotary degassing machine, adjusting the medium frequency induction furnace to be in a heat preservation state, degassing for 30-60 min, stopping degassing, closing the furnace, and removing dross on the surface of the alloy liquid;
(5) casting: and after cleaning, starting the medium-frequency induction furnace, stirring for 5-10 min with high current, heating to 800-900 ℃, adjusting the power of the furnace to keep the furnace in a heat preservation state, preparing for casting, adjusting the casting temperature to 800-900 ℃, the casting speed to 2-3 t/h, adjusting a cooling system to control the rolling temperature, and rolling to obtain the aluminum-zirconium alloy rod, wherein the rolling temperature is 450-550 ℃.
As a further technical scheme, the weight ratio of the potassium fluozirconate to the refining agent to the slag remover to the aluminum ingot is 140-180: 8-12: 8-12: 800 to 1000 parts of a first material, a second material,
the slag remover comprises the following raw materials in parts by weight: 3.2-4.8 parts of sodium chloride, 2.4-3.6 parts of potassium chloride, 2-3 parts of sodium fluosilicate and 0.4-0.6 part of calcium fluoride.
As a further technical scheme, the weight ratio of the diffusant to the aluminum ingot is 8-13: 800 to 1000.
As a further technical scheme, the dispersing agent comprises the following raw materials in parts by weight:
1.5-2.2 parts of sodium chloride, 1-1.6 parts of potassium chloride, 1-1.8 parts of magnesium chloride, 0.4-0.8 part of aluminum fluoride, 0.2-0.6 part of barium chloride, 0.5-1 part of cerium chloride, 3-4 parts of sodium fluoroaluminate and 0.4-1 part of calcium fluoride.
As a further technical scheme, the stirring speed of the mechanical stirrer in the step (3) is 200-500 r/min.
As a further technical scheme, the rotating speed of the rotary degasser in the step (4) is 250-350 r/min, the used gas is argon, and the gas flow is 1-1.5 m3/min。
The invention has the following using principle and beneficial effects:
the invention changes the traditional preparation method of the aluminum zirconium alloy rod, adopts a variable frequency induction furnace and a medium frequency induction furnace to produce the aluminum zirconium alloy rod, refines the aluminum liquid before feeding and adds the mixture of potassium fluozirconate and a diffusant as ZrAl in the alloying process3Nucleating agent of ZrAl formed after alloying3Are all in block or rod shape and are evenly distributed. The diffusant is added into the potassium fluozirconate to effectively control TiAl3The aggregation of mass points and the mechanical stirring in the alloying process effectively prevent ZrAl3The growth of particles and the separation and purification effect of the fluoride salt slag and the alloy are improved. By inspection and analysis, ZrAl in the product produced by the invention3Small mass point, even and dispersed distribution and extremely low slag content, and effectively solves the problem that the waffle-shaped aluminum-zirconium alloy ZrAl on the current market is3Large mass point, serious segregation, unstable deformation structure of aluminum alloy and poor comprehensive performance.
In order to select the optimal mixture ratio, the performances of the embodiments 1 to 6 are compared, and the grain refinement degree of the embodiment 6 without the addition of the dispersing agent is the worst, the grain refinement degree of the embodiments 4 to 5 is lower than that of the embodiments 1 to 3, and the grain refinement degree of the embodiment 3 in the embodiments 1 to 3 is relatively better than that of the other two. To further verify the performance and the stability of repeated production of the Al-Zr alloy rods prepared by the method of the present invention, 100 furnaces were produced according to the process of example 3, and 9 furnaces were randomly selected for chemical composition testing (see Table 1) and ZrAl was added3Metallographic structure picture (magnified 100 times, detailed)See FIGS. 1-9).
TABLE 1 chemical composition determination
Through comparative analysis, the chemical components of the 9-furnace product meet the national standard GB/T27677-2011, and the error of the Zr content measured by the 9-furnace product is less than 2%, so that the batch production capacity of the high-quality aluminum-zirconium alloy rod preparation method provided by the invention is fully determined, and the stability of the repeatedly produced product is high.
Comparing the metallographic pictures (FIG. 1 to FIG. 9), ZrAl in FIG. 13The maximum size is 35.21 μm, the minimum size is 4.32 μm; ZrAl in FIG. 23The maximum size is 29.51 μm, the minimum size is 6.11 μm; ZrAl in FIG. 33The maximum size is 39.21 μm, and the minimum size is 5.57 μm; ZrAl in FIG. 43The maximum size is 34.83 μm, the minimum size is 6.11 μm; ZrAl in FIG. 53The maximum size is 37.12 μm, the minimum size is 4.68 μm; ZrAl in FIG. 63The maximum size is 41.46 μm, the minimum size is 7.12 μm; ZrAl in FIG. 73The maximum size is 57.12 μm, and the minimum size is 5.38 μm; ZrAl in FIG. 83The maximum size is 31.01 μm, and the minimum size is 3.23 μm; ZrAl in FIG. 93The maximum size is 12.01 μm, and the minimum size is 7.12 μm;
the aluminum-zirconium alloy rod prepared by the preparation method of the high-quality aluminum-zirconium alloy rod provided by the invention is 1cm at will2ZrAl in longitudinal section3The particles are in block or rod shape and are distributed approximately uniformly, the average size of particles is less than 30 mu m, and the maximum size of single particle is less than 60 mu m, which is far superior to the existing products in the market.
As can be seen from the analysis of a plurality of aluminum zirconium alloy rods produced by the company, the aluminum zirconium alloy rods prepared by the method provided by the invention have uniform tissue distribution without cluster aggregation, the appearance, the size and the distribution of internal particles of the aluminum zirconium alloy rods uniformly reach the advanced level of similar products at home and abroad, the aluminum zirconium alloy rods have a remarkable stabilizing effect on the deformed tissues of the aluminum alloy, and the comprehensive performance of the alloy is improved in detail.
The particles β' (Al3Zr) of elemental zirconium are fine in size (< 30nm), have a good coherent relationship with the matrix, do not have a tendency to become preferential nucleation sites for the η phase particles, and are therefore much less sensitive to quenching.
The most remarkable effect of the zirconium element is the inhibition of the recrystallization behavior of the alloy, thereby providing possibility for obtaining various semi-finished products with completely non-recrystallized structures and keeping high-density dislocation and fiber structures generated in the deformation process. And the existence of the non-recrystallization structure enables the alloy semi-finished product to have better performance. This effect of the zirconium element is due to the presence of metastable Al3Zr(L12) Phase-by-phase. High density metastable Al3The Zr is dispersed finely, the mismatch rate with the mother phase is only 0.8 percent, and the Zr is an extremely effective strengthening dispersoid and recrystallization inhibitor.
Zirconium has certain influence on the aging behavior of the aluminum alloy, the zirconium has close interaction with vacancies at the initial stage of aging, and the binding energy between the zirconium and the vacancies is 0.32 ev. The vacancy controls the migration and diffusion rate of elements, and simultaneously can act with impurities, so that the vacancy is very key to the nucleation and growth of a GP zone at the early stage of time efficiency. The effect of the zirconium element and the vacancy changes the forming rate and the quantity of GP zones, so that the nucleation of the GP zones on the precipitation phase is influenced, and the subsequent aging behavior is directly influenced.
The fracture toughness of the zirconium-containing aluminum alloy is good. The interface strength between the particles and the matrix is high, the particle size is small, the particle spacing is large, and the improvement of the fracture toughness of the alloy is facilitated. Al (Al)3The Zr particles and the matrix are in a semi-coherent relationship, and the interface strength is greater than that of the unqualified Mn and Cr-containing particles and the matrix. Al (Al)3The Zr particle size is much smaller than that of the Mn and Cr containing particle phase, the Mn and Cr containing particles are about 70nm, and the Al3Zr is less than 30 nm. Al (Al)3The Zr particles are spherical, and the Mn-containing and Cr-containing particle phases are irregular in shape. Obviously, Al3The interface strength, the particle size and the shape of the Zr particles are beneficial to improving the fracture toughness of the alloy.
The zirconium-containing aluminum alloy has stress corrosion resistance, and the small-angle crystal boundary is more favorable for improving the stress corrosion resistance than the large-angle crystal boundary. Zirconium is added into the alloy, a completely non-recrystallized fiber structure is obtained after deformation, and the stress corrosion resistance of the alloy is improved by the small-angle grain boundary of the fiber structure. Thus, it can be said that the contribution of the zirconium element to the stress corrosion resistance is indirect, and it is achieved by obtaining a fibrous structure by suppressing recrystallization.
Strength of zirconium-containing aluminum alloys, in zirconium-containing aluminum alloys, on the one hand, due to the strengthening phase Al3Zr is dispersed and precipitated during alloy homogenization treatment and hot working, and has high microhardness of>5000MPa), once precipitated, is difficult to redissolve or aggregate, and has a large dispersion strengthening effect. On the other hand, the alloy is still a non-recrystallization structure after hot processing and final heat treatment, a large amount of dislocation and fiber structures generated in the deformation process are preserved, and the alloy has a great deformation strengthening effect. Under the action of the two aspects, the strength of the alloy is obviously improved.
The aluminum-zirconium alloy rod produced by the preparation method provided by the invention can improve the stress corrosion resistance and the spalling (or layered) corrosion resistance of the alloy, simultaneously the quenching sensitivity of the alloy is not obviously increased, the corrosion resistance is obviously improved, however, the zirconium element has an obvious stabilizing effect on the deformation structure of the alloy, and the comprehensive performance of the alloy is improved.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a metallographic structure diagram corresponding to a product produced by a 2017A171973 furnace number;
FIG. 2 is a metallographic structure diagram corresponding to a product produced by the 2017A171974 furnace number;
FIG. 3 is a metallographic structure diagram corresponding to a product produced by 2017A 171975;
FIG. 4 is a metallographic structure diagram corresponding to a product produced with a 2017A171976 furnace number;
FIG. 5 is a metallographic structure diagram corresponding to a product produced with a 2017A171977 furnace number;
FIG. 6 is a metallographic structure diagram corresponding to a product produced by 2017A 171978;
FIG. 7 is a metallographic structure diagram corresponding to a product produced with a 2017A171979 furnace number;
FIG. 8 is a metallographic structure diagram corresponding to a product produced in accordance with run number 2017A 171980;
FIG. 9 is a metallographic structure diagram corresponding to a product produced by the 2017A171981 furnace number.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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
(1) Burdening and mixing: weighing 140 parts of potassium fluorozirconate and 8 parts of dispersing agent according to the parts by weight, and adding the two into a mixer to mix for 30min to prepare a fluorine salt mixture;
(2) alloying in the first step: weighing 800 parts of aluminum ingots according to the weight parts, putting the aluminum ingots into a variable frequency induction furnace, heating to 800 ℃, adding 8 parts of refining agent into the aluminum liquid to refine the aluminum liquid, starting a mechanical stirrer and a feeder for the variable frequency induction furnace to uniformly add 46% of fluorine salt mixture into the aluminum liquid of the variable frequency induction furnace, and stirring for 60min to obtain aluminum-zirconium alloy liquid;
(3) alloying in the second step: starting the variable frequency induction furnace and enabling the variable frequency induction furnace to be in a stirring frequency range, adjusting the power of the variable frequency induction furnace for stirring, starting the environment-friendly equipment and the stirring device, uniformly adding a 54% fluorine salt mixture into molten aluminum of the variable frequency induction furnace through a feeder, wherein the feeding time is 10min, the reaction temperature of the molten aluminum is 800 ℃ by adjusting the power and the feeding speed of the variable frequency induction furnace, and after the feeding is finished for 20 min; adjusting the power of a variable frequency induction furnace, keeping the temperature of the aluminum liquid at 800 ℃, continuing stirring for 10min, switching the variable frequency induction furnace to a heating frequency band, keeping the temperature for 5min, stopping the furnace, pouring out a fluoride salt slag water layer on the upper layer in the furnace, adding a proper amount of 8 parts of slag removing agent into the aluminum zirconium alloy liquid, and removing scum on the surface of the alloy liquid after stirring uniformly;
(4) degassing and refining: transferring the metal liquid after slag removal into a refining casting furnace, starting a variable frequency induction furnace to reach the maximum power, heating to 800 ℃, shoveling the furnace wall, performing rotary degassing by using a rotary degassing machine, adjusting the medium frequency induction furnace to be in a heat preservation state, stopping degassing after 30min, shutting down the furnace, and removing dross on the surface of the alloy liquid;
(5) casting: and after cleaning, starting the medium-frequency induction furnace, stirring for 5min at a high current, heating to 800 ℃, adjusting the power of the furnace to keep the furnace in a heat-preservation state, preparing for casting, wherein the casting temperature is 800 ℃, the casting speed is 2t/h, adjusting a cooling system to control the rolling temperature, and the rolling temperature is 450 ℃ to roll the aluminum-zirconium alloy rod.
Wherein the slag remover is formed by mixing 3.2 parts of sodium chloride, 2.4 parts of potassium chloride, 2 parts of sodium fluosilicate and 0.4 part of calcium fluoride. The dispersing agent consists of the following components in parts by weight: 1.5 parts of sodium chloride, 1 part of potassium chloride, 1 part of magnesium chloride, 0.4 part of aluminum fluoride, 0.2 part of barium chloride, 0.5 part of cerium chloride, 3 parts of sodium fluoroaluminate and 0.4 part of calcium fluoride. And (4) stirring speed of the mechanical stirrer in the step (3) is 200 r/min. The rotating speed of the rotary degasser in the step (4) is 250r/min, the used gas is argon, and the gas flow is 1m3/min。
Example 2
(1) Burdening and mixing: weighing 180 parts of potassium fluorozirconate and 13 parts of dispersing agent according to the parts by weight, and adding the two into a mixer to mix for 30min to prepare a villiaumite mixture;
(2) alloying in the first step: weighing 1000 parts of aluminum ingots according to the weight parts, putting the aluminum ingots into a variable frequency induction furnace, heating to 850 ℃, adding 12 parts of refining agent into the aluminum liquid to refine the aluminum liquid, starting a mechanical stirrer and a feeder for the variable frequency induction furnace to uniformly add 55% of fluorine salt mixture into the aluminum liquid of the variable frequency induction furnace, and stirring for 90min to obtain aluminum-zirconium alloy liquid;
(3) alloying in the second step: starting the variable frequency induction furnace and enabling the variable frequency induction furnace to be in a stirring frequency range, adjusting the power of the variable frequency induction furnace for stirring, starting the environment-friendly equipment and the stirring device, uniformly adding a 45% fluorine salt mixture into molten aluminum of the variable frequency induction furnace through a feeder, wherein the feeding time is 30min, the reaction temperature of the molten aluminum is 950 ℃ by adjusting the power and the feeding speed of the variable frequency induction furnace, and finishing the feeding for 40 min; adjusting the power of a variable frequency induction furnace, keeping the temperature of the aluminum liquid at 950 ℃, continuing stirring for 20min, switching the variable frequency induction furnace to a heating frequency band, keeping the temperature for 10min, stopping the furnace, pouring out a fluoride salt slag water layer on the upper layer in the furnace, adding a proper amount of 12 parts of slag removal agent into the aluminum zirconium alloy liquid, and removing scum on the surface of the alloy liquid after stirring uniformly;
(4) degassing and refining: transferring the metal liquid after slag removal into a refining casting furnace, starting a variable frequency induction furnace to reach the maximum power, heating to 1000 ℃, shoveling the furnace wall, performing rotary degassing by using a rotary degassing machine, adjusting the medium frequency induction furnace to be in a heat preservation state, stopping degassing after 60min, shutting down the furnace, and removing dross on the surface of the alloy liquid;
(5) casting: and after cleaning, starting the medium-frequency induction furnace, stirring for 10min at a high current, heating to 900 ℃, adjusting the power of the furnace to keep the furnace in a heat-preservation state, preparing for casting, wherein the casting temperature is 900 ℃, the casting speed is 3t/h, adjusting a cooling system to control the rolling temperature, and the rolling temperature is 500 ℃ to roll the aluminum-zirconium alloy rod.
Wherein the slag remover is prepared by mixing 4.8 parts of sodium chloride, 3.6 parts of potassium chloride, 3 parts of sodium fluosilicate and 0.6 part of calcium fluoride. The dispersing agent consists of the following components in parts by weight: 2.2 parts of sodium chloride, 1.6 parts of potassium chloride, 1.8 parts of magnesium chloride, 0.8 part of aluminum fluoride, 0.6 part of barium chloride, 1 part of cerium chloride, 4 parts of sodium fluoroaluminate and 1 part of calcium fluoride. And (3) stirring speed of the mechanical stirrer in the step (3) is 500 r/min. In the step (4), the rotating speed of the rotary degasser is 350r/min, the used gas is argon, and the gas flow is 1.5m3/min。
Example 3
(1) Burdening and mixing: weighing 160 parts of potassium fluorozirconate and 10 parts of a dispersing agent according to the parts by weight, and adding the two into a mixer to mix for 30min to prepare a villiaumite mixture;
(2) alloying in the first step: weighing 900 parts of aluminum ingots according to the weight parts, putting the aluminum ingots into a variable frequency induction furnace, heating to 825 ℃, adding 10 parts of refining agent into the aluminum liquid to refine the aluminum liquid, starting a mechanical stirrer and a feeder for the variable frequency induction furnace to uniformly add 50% of fluorine salt mixture into the aluminum liquid of the variable frequency induction furnace, and stirring for 75min to obtain aluminum-zirconium alloy liquid;
(3) alloying in the second step: starting the variable frequency induction furnace and enabling the variable frequency induction furnace to be in a stirring frequency range, adjusting the power of the variable frequency induction furnace for stirring, starting the environment-friendly equipment and the stirring device, uniformly adding a 50% fluorine salt mixture into molten aluminum of the variable frequency induction furnace through a feeder, wherein the feeding time is 20min, the reaction temperature of the molten aluminum is 900 ℃ by adjusting the power and the feeding speed of the variable frequency induction furnace, and finishing feeding for 30 min; adjusting the power of a variable frequency induction furnace, keeping the temperature of the aluminum liquid at 900 ℃, continuing stirring for 15min, switching the variable frequency induction furnace to a heating frequency band, keeping the temperature for 7min, stopping the furnace, pouring out a fluoride salt slag water layer on the upper layer in the furnace, adding a proper amount of 10 parts of slag removal agent into the aluminum zirconium alloy liquid, and removing scum on the surface of the alloy liquid after stirring uniformly;
(4) degassing and refining: transferring the metal liquid after slag removal into a refining casting furnace, starting a variable frequency induction furnace to reach the maximum power, heating to 900 ℃, shoveling the furnace wall, performing rotary degassing by using a rotary degassing machine, adjusting the medium frequency induction furnace to be in a heat preservation state, stopping degassing after 45min, shutting down the furnace, and removing dross on the surface of the alloy liquid;
(5) casting: and after cleaning, starting the medium-frequency induction furnace, stirring for 7min at a high current, heating to 850 ℃, adjusting the power of the furnace to keep the furnace in a heat-preservation state, preparing for casting, wherein the casting temperature is 850 ℃, the casting speed is 2.5t/h, adjusting the rolling temperature of a cooling system, and the rolling temperature is 480 ℃ to roll the aluminum-zirconium alloy rod.
Wherein the slag remover is prepared by mixing 4 parts of sodium chloride, 3 parts of potassium chloride, 2.5 parts of sodium fluosilicate and 0.5 part of calcium fluoride. The dispersing agent consists of the following components in parts by weight: 2 parts of sodium chloride, 1.3 parts of potassium chloride, 1.4 parts of magnesium chloride, 0.6 part of aluminum fluoride, 0.4 part of barium chloride, 0.7 part of cerium chloride, 3.5 parts of sodium fluoroaluminate and 0.7 part of calcium fluoride. And (3) stirring speed of the mechanical stirrer in the step (3) is 350 r/min. In the step (4), the rotating speed of the rotary degasser is 300r/min, the used gas is argon, and the gas flow is 1.3m3/min。
Example 4
(1) Burdening and mixing: weighing 160 parts of potassium fluorozirconate and 6 parts of a dispersing agent according to the parts by weight, and adding the two into a mixer to mix for 30min to prepare a villiaumite mixture;
(2) alloying in the first step: weighing 900 parts of aluminum ingots according to the weight parts, putting the aluminum ingots into a variable frequency induction furnace, heating to 825 ℃, adding 10 parts of refining agent into the aluminum liquid to refine the aluminum liquid, starting a mechanical stirrer and a feeder for the variable frequency induction furnace to uniformly add 50% of fluorine salt mixture into the aluminum liquid of the variable frequency induction furnace, and stirring for 75min to obtain aluminum-zirconium alloy liquid;
(3) alloying in the second step: starting the variable frequency induction furnace and enabling the variable frequency induction furnace to be in a stirring frequency range, adjusting the power of the variable frequency induction furnace for stirring, starting the environment-friendly equipment and the stirring device, uniformly adding a 50% fluorine salt mixture into molten aluminum of the variable frequency induction furnace through a feeder, wherein the feeding time is 20min, the reaction temperature of the molten aluminum is 900 ℃ by adjusting the power and the feeding speed of the variable frequency induction furnace, and finishing feeding for 30 min; adjusting the power of a variable frequency induction furnace, keeping the temperature of the aluminum liquid at 900 ℃, continuing stirring for 15min, switching the variable frequency induction furnace to a heating frequency band, keeping the temperature for 7min, stopping the furnace, pouring out a fluoride salt slag water layer on the upper layer in the furnace, adding a proper amount of 10 parts of slag removal agent into the aluminum zirconium alloy liquid, and removing scum on the surface of the alloy liquid after stirring uniformly;
(4) degassing and refining: transferring the metal liquid after slag removal into a refining casting furnace, starting a variable frequency induction furnace to reach the maximum power, heating to 900 ℃, shoveling the furnace wall, performing rotary degassing by using a rotary degassing machine, adjusting the medium frequency induction furnace to be in a heat preservation state, stopping degassing after 45min, shutting down the furnace, and removing dross on the surface of the alloy liquid;
(5) casting: and after cleaning, starting the medium-frequency induction furnace, stirring for 7min at a high current, heating to 850 ℃, adjusting the power of the furnace to keep the furnace in a heat-preservation state, preparing for casting, wherein the casting temperature is 850 ℃, the casting speed is 2.5t/h, adjusting the rolling temperature of a cooling system, and the rolling temperature is 500 ℃ to roll the aluminum-zirconium alloy rod.
Wherein the slag remover is prepared by mixing 4 parts of sodium chloride, 3 parts of potassium chloride, 2.5 parts of sodium fluosilicate and 0.5 part of calcium fluoride. The dispersing agent consists of the following components in parts by weight: 2 parts of sodium chloride, 1.3 parts of potassium chloride, 1.4 parts of magnesium chloride, 0.6 part of aluminum fluoride, 0.4 part of barium chloride, 0.7 part of cerium chloride, 3.5 parts of sodium fluoroaluminate and 0.7 part of calcium fluoride. And (3) stirring speed of the mechanical stirrer in the step (3) is 350 r/min. Step (ii) of(4) The rotating speed of the medium-rotation degassing machine is 300r/min, the used gas is argon, and the gas flow is 1.3m3/min。
Example 5
(1) Burdening and mixing: weighing 160 parts of potassium fluorozirconate and 15 parts of a dispersing agent according to the parts by weight, and adding the two into a mixer to mix for 30min to prepare a villiaumite mixture;
(2) alloying in the first step: weighing 900 parts of aluminum ingots according to the weight parts, putting the aluminum ingots into a variable frequency induction furnace, heating to 825 ℃, adding 10 parts of refining agent into the aluminum liquid to refine the aluminum liquid, starting a mechanical stirrer and a feeder for the variable frequency induction furnace to uniformly add 50% of fluorine salt mixture into the aluminum liquid of the variable frequency induction furnace, and stirring for 75min to obtain aluminum-zirconium alloy liquid;
(3) alloying in the second step: starting the variable frequency induction furnace and enabling the variable frequency induction furnace to be in a stirring frequency range, adjusting the power of the variable frequency induction furnace for stirring, starting the environment-friendly equipment and the stirring device, uniformly adding a 50% fluorine salt mixture into molten aluminum of the variable frequency induction furnace through a feeder, wherein the feeding time is 20min, the reaction temperature of the molten aluminum is 900 ℃ by adjusting the power and the feeding speed of the variable frequency induction furnace, and finishing feeding for 30 min; adjusting the power of a variable frequency induction furnace, keeping the temperature of the aluminum liquid at 900 ℃, continuing stirring for 15min, switching the variable frequency induction furnace to a heating frequency band, keeping the temperature for 7min, stopping the furnace, pouring out a fluoride salt slag water layer on the upper layer in the furnace, adding a proper amount of 10 parts of slag removal agent into the aluminum zirconium alloy liquid, and removing scum on the surface of the alloy liquid after stirring uniformly;
(4) degassing and refining: transferring the metal liquid after slag removal into a refining casting furnace, starting a variable frequency induction furnace to reach the maximum power, heating to 900 ℃, shoveling the furnace wall, performing rotary degassing by using a rotary degassing machine, adjusting the medium frequency induction furnace to be in a heat preservation state, stopping degassing after 45min, shutting down the furnace, and removing dross on the surface of the alloy liquid;
(5) casting: and after cleaning, starting the medium-frequency induction furnace, stirring for 7min at a high current, heating to 850 ℃, adjusting the power of the furnace to keep the furnace in a heat-preservation state, preparing for casting, wherein the casting temperature is 850 ℃, the casting speed is 2.5t/h, adjusting the rolling temperature of a cooling system, and the rolling temperature is 500 ℃ to roll the aluminum-zirconium alloy rod.
Wherein the slag remover is prepared by mixing 4 parts of sodium chloride, 3 parts of potassium chloride, 2.5 parts of sodium fluosilicate and 0.5 part of calcium fluoride. The dispersing agent consists of the following components in parts by weight: 2 parts of sodium chloride, 1.3 parts of potassium chloride, 1.4 parts of magnesium chloride, 0.6 part of aluminum fluoride, 0.4 part of barium chloride, 0.7 part of cerium chloride, 3.5 parts of sodium fluoroaluminate and 0.7 part of calcium fluoride. And (3) stirring speed of the mechanical stirrer in the step (3) is 350 r/min. In the step (4), the rotating speed of the rotary degasser is 300r/min, the used gas is argon, and the gas flow is 1.3m3/min。
Example 6
(1) Burdening and mixing: weighing 160 parts of potassium fluozirconate for later use;
(2) alloying in the first step: weighing 900 parts of aluminum ingots according to the weight parts, putting the aluminum ingots into a variable frequency induction furnace, heating to 825 ℃, adding 10 parts of refining agent into the aluminum liquid to refine the aluminum liquid, starting a mechanical stirrer and a feeder for the variable frequency induction furnace to uniformly add 50% of potassium fluozirconate into the aluminum liquid of the variable frequency induction furnace, and stirring for 75min to obtain aluminum-zirconium alloy liquid;
(3) alloying in the second step: starting the variable frequency induction furnace and enabling the variable frequency induction furnace to be in a stirring frequency range, adjusting the power of the variable frequency induction furnace for stirring, starting the environment-friendly equipment and the stirring device, uniformly adding 50% of potassium fluozirconate into molten aluminum of the variable frequency induction furnace through a feeder, wherein the feeding time is 20min, the reaction temperature of the molten aluminum is 900 ℃ by adjusting the power and the feeding speed of the variable frequency induction furnace, and finishing the feeding for 30 min; adjusting the power of a variable frequency induction furnace, keeping the temperature of the aluminum liquid at 900 ℃, continuing stirring for 15min, switching the variable frequency induction furnace to a heating frequency band, keeping the temperature for 7min, stopping the furnace, pouring out a fluoride salt slag water layer on the upper layer in the furnace, adding a proper amount of 10 parts of slag removal agent into the aluminum zirconium alloy liquid, and removing scum on the surface of the alloy liquid after stirring uniformly;
(4) degassing and refining: transferring the metal liquid after slag removal into a refining casting furnace, starting a variable frequency induction furnace to reach the maximum power, heating to 900 ℃, shoveling the furnace wall, performing rotary degassing by using a rotary degassing machine, adjusting the medium frequency induction furnace to be in a heat preservation state, stopping degassing after 45min, shutting down the furnace, and removing dross on the surface of the alloy liquid;
(5) casting: and after cleaning, starting the medium-frequency induction furnace, stirring for 7min at a high current, heating to 850 ℃, adjusting the power of the furnace to keep the furnace in a heat-preservation state, preparing for casting, wherein the casting temperature is 850 ℃, the casting speed is 2.5t/h, adjusting the rolling temperature of a cooling system, and the rolling temperature is 500 ℃ to roll the aluminum-zirconium alloy rod.
Wherein the slag remover is prepared by mixing 4 parts of sodium chloride, 3 parts of potassium chloride, 2.5 parts of sodium fluosilicate and 0.5 part of calcium fluoride. And (3) stirring speed of the mechanical stirrer in the step (3) is 350 r/min. In the step (4), the rotating speed of the rotary degasser is 300r/min, the used gas is argon, and the gas flow is 1.3m3/min。
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (3)
1. A preparation method of a high-quality aluminum zirconium alloy rod is characterized by comprising the following steps:
(1) burdening and mixing: weighing potassium fluorozirconate and a dispersing agent according to the weight parts, adding the potassium fluorozirconate and the dispersing agent into a mixer, and mixing for 30min to prepare a villiaumite mixture;
(2) alloying in the first step: weighing aluminum ingots according to the weight parts, putting the aluminum ingots into a variable frequency induction furnace, heating to 800-850 ℃, adding a refining agent into molten aluminum to refine the molten aluminum, starting a mechanical stirrer and a feeder for the variable frequency induction furnace to uniformly add 46-55% of a fluorine salt mixture into the molten aluminum of the variable frequency induction furnace, and stirring for 60-90 min to obtain an aluminum-zirconium alloy liquid;
(3) alloying in the second step: starting the variable frequency induction furnace and enabling the variable frequency induction furnace to be in a stirring frequency range, adjusting the power of the variable frequency induction furnace for stirring, starting the environment-friendly equipment and the stirring device, uniformly adding a 45-54% fluorine salt mixture into molten aluminum of the variable frequency induction furnace through a feeder, wherein the feeding time is 10-30 min, the reaction temperature of the molten aluminum is 800-950 ℃ by adjusting the power and the feeding speed of the variable frequency induction furnace, and after the feeding is finished for 20-40 min; adjusting the power of a variable frequency induction furnace, keeping the temperature of the aluminum liquid at 800-950 ℃, continuing stirring for 10-20 min, switching the variable frequency induction furnace to a heating frequency band, keeping the temperature for 5-10 min, stopping the furnace, pouring a fluoride salt slag water layer on the upper layer in the furnace, adding a proper amount of slag cleaning agent into the aluminum zirconium alloy liquid, and removing scum on the surface of the alloy liquid after stirring uniformly;
(4) degassing and refining: transferring the metal liquid after slag removal into a refining casting furnace, starting a variable frequency induction furnace to reach the maximum power, heating to 800-1000 ℃, shoveling the furnace wall, performing rotary degassing by using a rotary degassing machine, adjusting the medium frequency induction furnace to be in a heat preservation state, degassing for 30-60 min, stopping degassing, closing the furnace, and removing dross on the surface of the alloy liquid;
(5) casting: after cleaning, starting a medium-frequency induction furnace, stirring for 5-10 min with high current, heating to 800-900 ℃, adjusting the power of the furnace to keep the furnace in a heat-preservation state, preparing for casting, adjusting the casting temperature to 800-900 ℃, the casting speed to 2-3 t/h, adjusting a cooling system to control the rolling temperature, and rolling to obtain an aluminum-zirconium alloy rod, wherein the rolling temperature is 450-550 ℃;
the weight ratio of the potassium fluozirconate to the refining agent to the slag remover to the aluminum ingot is 140-180: 8-12: 8-12: 800 to 1000 parts of a first material, a second material,
the slag remover comprises the following raw materials in parts by weight: 3.2-4.8 parts of sodium chloride, 2.4-3.6 parts of potassium chloride, 2-3 parts of sodium fluosilicate and 0.4-0.6 part of calcium fluoride;
the weight ratio of the diffusant to the aluminum ingot is 8-13: 800-1000 parts;
the dispersing agent comprises the following raw materials in parts by weight:
1.5-2.2 parts of sodium chloride, 1-1.6 parts of potassium chloride, 1-1.8 parts of magnesium chloride, 0.4-0.8 part of aluminum fluoride, 0.2-0.6 part of barium chloride, 0.5-1 part of cerium chloride, 3-4 parts of sodium fluoroaluminate and 0.4-1 part of calcium fluoride.
2. The method for preparing a high-quality Al-Zr alloy rod according to claim 1, wherein the stirring speed of the mechanical stirrer in the step (3) is 200-500 r/min.
3. A high quality as claimed in claim 2The preparation method of the aluminum-zirconium alloy rod is characterized in that the rotating speed of the rotary degasser in the step (4) is 250-350 r/min, the used gas is argon, and the gas flow is 1-1.5 m3/min。
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