CN113122740A - Method for preparing Zn-Cu-Ti alloy ingot, alloy ingot and alloy plate - Google Patents
Method for preparing Zn-Cu-Ti alloy ingot, alloy ingot and alloy plate Download PDFInfo
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- CN113122740A CN113122740A CN202110373731.0A CN202110373731A CN113122740A CN 113122740 A CN113122740 A CN 113122740A CN 202110373731 A CN202110373731 A CN 202110373731A CN 113122740 A CN113122740 A CN 113122740A
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C18/00—Alloys based on zinc
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- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
- C22C18/02—Alloys based on zinc with copper as the next major constituent
Abstract
The invention provides a method for preparing a Zn-Cu-T i alloy ingot, an alloy ingot and an alloy plate, namely, in the smelting process of a Zn-Cu-T i alloy, rare earth modification and high-energy ultrasonic synergistic treatment are utilized to promote intermediate alloy containing Ti and Cu elements to be efficiently melted/dissolved at low temperature, meanwhile, high-quality Zn-Cu-T i alloy is prepared by the aid of the effects of degassing and impurity removal, melt nucleation rate improvement, grain growth inhibition and the like, and the Zn-Cu-T i alloy plate is produced by multi-pass rolling. Compared with the existing Zn-Cu-T i alloy casting process, the invention not only accelerates the diffusion and dissolution speed of T i and Cu atoms at low temperature, but also reduces the melting temperature, reduces the loss rate of T i and Zn elements, promotes the homogenization of Zn-Cu-T i alloy solute, the purification of melt and the refinement of structure, is beneficial to preparing high-quality plates with high surface quality, high mechanical property and high corrosion resistance which finally reach the European EN988 standard, and has stable process, strong controllability and good application prospect.
Description
Technical Field
The invention relates to the technical field of zinc alloy preparation and smelting, in particular to a material method for efficiently preparing a Zn-Cu-Ti alloy ingot at a low temperature, the alloy ingot prepared by the material method, and an alloy plate prepared from the alloy ingot.
Background
The Zn-Cu-Ti alloy plays an important role in zinc base alloy processing materials. It has excellent comprehensive performance, such as good processing performance, forming performance, welding performance, corrosion resistance and embossing performance, and durable color. The alloy has good creep resistance and can be compared favorably with brass. Because of the excellent performance of Zn-Cu-Ti alloy, it is widely used in construction and decoration industry, such as roof board, wall panel and drainage channel, in the last seventies of the century in foreign countries, especially in developed countries in Western Europe. The performance and the application of the material are researched with great success in China. The Zn-Cu-Ti alloy is reported to be used as a copper substitute material to trial manufacture water tank radiating fins, radiating pipes, automobile brake pipes, oil conveying pipes, medical high-speed dental drills and the like successfully. However, at present, the preparation and application of Zn-Cu-Ti alloy materials are still not mature in China, so that the exploration and optimization of Zn-Cu-Ti alloy and plate preparation technologies thereof can produce high-quality Zn-Cu-Ti alloy plates meeting European standard EN988, and the method has important social and economic benefits.
The melting point of Zn is only 420 ℃, which is far lower than that of Cu and Ti, and the Zn and Ti are burnt at high temperature, if pure Cu and pure Ti are directly used for smelting, the problems of slow melting/dissolving efficiency, incomplete melting/dissolving and even difficult melting/dissolving of Cu and Ti are caused, and Cu and Ti elements are difficult to be uniformly distributed in a melt according to the designed components. At present, Cu and Ti elements are often introduced into a melt in the form of intermediate alloy such as Zn-Cu, Zn-Ti or Zn-Cu-Ti, but the general melting temperature is 650-750 ℃, the melting point of the Zn alloy is far exceeded, long-time heat preservation is needed after the intermediate alloy is added to ensure the complete melting/dissolution of the intermediate alloy, the suction of the melt is serious, excessive oxide inclusions are generated, the quality of the melt is greatly reduced, and meanwhile, the low-quality Zn-Cu-Ti alloy prepared by high-temperature casting has a coarse structure, so that a Zn-Cu-Ti alloy plate meeting the European standard EN988 is difficult to prepare.
The efficient casting of the Zn-Cu-Ti alloy with pure components, low gas content and fine and uniform tissue is the premise for producing high-quality Zn-Cu-Ti alloy plates. In the smelting process of the zinc alloy, gases such as hydrogen, oxygen, nitrogen, water vapor, CO2 and the like are easily dissolved in the melt, rare earth is easy to react with impurity gases such as oxygen, hydrogen and the like in the melt to generate stable compounds, and in addition, the rare earth can react with harmful impurities in the melt, such as metal elements such as lead, cadmium, tin, iron and the like, to generate intermetallic compounds for precipitation and removal, so that the melt purification is realized; in addition, the rare earth is beneficial to the nucleation of a large amount of zinc alloy melt, and plays the role of modification to inhibit the growth of crystal grains, thereby refining the structure.
At present, the large-scale preparation of high-quality and high-quality Zn-Cu-Ti alloy and plates thereof needs to be solved urgently.
Disclosure of Invention
Therefore, the invention aims to solve the problems that the existing Zn-Cu-Ti alloy has high smelting temperature, low efficiency, more impurities, heavy gas absorption, high burning loss rate, uncontrollable alloy components, no high-quality plate can be prepared and the like, and provides the preparation method of the Zn-Cu-Ti alloy ingot. In the process of smelting the Zn-Cu-Ti alloy, by utilizing the synergistic effect of rare earth elements and ultrasonic treatment, the alloy smelting temperature is reduced, the low-temperature melting/dissolving of Ti and Cu elements is accelerated, the gas and impurity removal are carried out, the melt is purified, and the structure is refined, so that the high-quality Zn-Cu-Ti alloy is prepared, and the alloy smelting temperature can be reduced to obtain the high-quality Zn-Cu-Ti alloy.
Furthermore, the invention also provides the Zn-Cu-Ti alloy prepared by the method.
Furthermore, the invention also provides the Zn-Cu-Ti alloy and the alloy plate prepared by the method.
In order to solve the technical problems, the invention adopts the following technical scheme
S1, keeping the temperature of the alloy raw material and the rare earth material at 50-300 ℃ for 2-30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
s2, putting Zn into a melting furnace, heating to 420-500 ℃ to be completely melted, sequentially adding intermediate alloy containing Cu and/or Ti elements and rare earth materials into the Zn melt, heating the melting furnace to 450-650 ℃, and uniformly dispersing a covering agent on the surface of the melt;
s3, applying high-energy ultrasound to the melt to accelerate the diffusion and dissolution speed of Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 20-100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted;
and S4, adding a refining agent, refining for 5-30min, stopping ultrasonic treatment, and slagging off and casting the melt to obtain the Zn-Cu-Ti alloy cast ingot.
In the step S1, the alloy raw material comprises the following elements in percentage by mass: 0.05 to 2.0 percent of Cu, 0.05 to 0.5 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent;
the rare earth material is RE, Zn-REz,RECuxOne or a mixture of more of Cu-Ti-RE;
the rare earth material is calculated by RE, and the mass of RE is 0.01-1% of the total mass of the Zn-Cu-Ti alloy;
the Zn-REzZ in (a) is an integer of 1 to 50, RECuxX in (A) is an integer of 1 to 30.
The RE is one or a mixture of more of La, Ce, Y and Er.
The intermediate alloy containing Ti and/or Cu elements is binary alloy or ternary alloy;
the binary alloy is Zn-TimOr Zn-CunThe ternary alloy is Zn-Cuk-Tit，
M and n are the same or different and are respectively an integer of 1-50;
the k and the t are the same or different and are integers of 1-20 respectively.
The covering agent in the step S2 is one or a mixture of several of charcoal powder, ammonium chloride, sodium chloride and potassium chloride, and the thickness of the covering agent on the surface of the melt is 0.2-10 mm.
The refining agent in the step S4 is a nitrogen and chlorine mixed gas, a chlorine salt or an inert gas.
The ultrasonic power in the step S3 is 100-2000W, and the ultrasonic time is 5-30 min.
A Zn-Cu-Ti alloy ingot prepared by the method.
A Zn-Cu-Ti alloy plate is obtained by rolling the Zn-Cu-Ti alloy cast ingot for multiple times.
The multi-pass rolling process is one of hot rolling, hot rolling → cold rolling, hot rolling → warm rolling → cold rolling.
The hot rolling temperature is 200-350 ℃, the cold rolling temperature is room temperature, the warm rolling temperature is 80-180 ℃, the reduction per pass is 10-30%, the total reduction is controlled to be 65-95%, and the thickness of the finally prepared Zn-Cu-Ti alloy plate is 0.1-10 mm.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the Zn-Cu-Ti alloy ingot, the rare earth element and ultrasonic treatment synergistic effect is utilized, the alloy smelting temperature is reduced, the low-temperature melting/dissolving of Ti and Cu elements is accelerated, the gas and impurity removal are carried out, the melt is purified, and the structure is refined, so that the quality of the Zn-Cu-Ti alloy ingot can be greatly improved.
In the method, the main functions of the ultrasound and the ultrasound matched with the rare earth RE are as follows: the melt can be purified, and the impurity content can be reduced; refining zinc alloy grains to change the zinc alloy grains from coarse dendrites into rose or near-spherulite crystals; RE can also be degassed and used in combination with a refining agent, so that gas in the melt can be removed rapidly and efficiently; improving the performance of the zinc alloy, such as mechanical property, corrosion resistance, creep resistance and the like; RE can refine and homogenize the second phase in the zinc alloy; improving the plasticity of the Zn-Cu-Ti alloy after annealing.
In the step S2, the covering agent with the thickness of 0.2-10mm is uniformly covered on the surface of the melt, so that the burning loss and volatilization of Zn element can be effectively reduced, the oxidation of alloy liquid caused by the damage of the surface layer of the zinc alloy melt due to electromagnetic disturbance can be avoided, and the reduction of the melt quality caused by the air suction of the zinc alloy liquid can be avoided.
The refining agent used in step S4 is a mixed gas of nitrogen and chlorine, a chlorine salt or an inert gas, and has the following effects: (1) removing gas inside the zinc alloy melt, wherein the gas is mainly hydrogen; (2) separating impurities in the zinc alloy melt from the melt and floating the impurities; (2) providing nucleation particles and refining zinc alloy grains.
The invention adopts the high-energy ultrasonic with the ultrasonic power of 100-2000W as an effective melt treatment process, the sound flow effect of the high-energy ultrasonic causes melt circulation, the cavitation effect generates a local high-temperature and high-pressure area, the sound flow and cavitation synergistic effect greatly increases the contact area of master alloy particles and the melt, promotes the low-temperature dissolution/melting of the master alloy, and accelerates the absorption process of the zinc alloy melt to Cu and Ti; meanwhile, the ultrasonic treatment also plays a good role in melt purification and tissue refinement for the melt.
The method for efficiently preparing the Zn-Cu-Ti alloy and the plate at low temperature by the rare earth modification and ultrasonic treatment in cooperation enables the finally prepared Zn-Cu-Ti alloy plate to meet EN988 European standard. Through detection, the alloy ingot casting crystal grains are refined, and the size of the crystal grains is less than 300 mu m, even can be less than 100 mu m; the mechanical property of the alloy cast ingot is improved, the tensile strength is 90-100MPa, and the elongation is 3-6%; the corrosion resistance of the alloy is improved, and the corrosion rate is lower than 1.5g.m-2.h-1(ii) a The alloy plate blank has high density, and the porosity is less than 0.1%; the chemical components are uniform and accurate, and the phenomenon of large difference between the chemical components and preparation caused by chemical component segregation or burning loss can not occur; is beneficial to rolling into slabs at lower temperature.
In the process of smelting Zn-Cu-Ti alloy, rare earth modification and high-energy ultrasonic synergistic treatment are utilized to promote intermediate alloy containing Ti and Cu elements to be efficiently melted/dissolved at low temperature, and meanwhile, high-quality Zn-Cu-Ti alloy is prepared by virtue of the effects of degassing and impurity removal, melt nucleation rate improvement, grain growth inhibition and the like, and a Zn-Cu-Ti alloy plate is produced by adopting multi-pass rolling. Compared with the existing Zn-Cu-Ti alloy casting process, the invention not only accelerates the low-temperature diffusion and dissolution speed of Ti and Cu atoms, but also reduces the melting temperature, reduces the burning loss rate of Ti and Zn elements, and simultaneously promotes the homogenization, melt purification and tissue refinement of Zn-Cu-Ti alloy solute, thereby being beneficial to preparing high-quality plates with high surface quality, high mechanical property and high corrosion resistance which finally reach the European EN988 standard.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a microstructure diagram of an ingot of a Zn-Cu-Ti alloy in example 1 of the present invention.
FIG. 2 is a microstructure diagram of an ingot of a Zn-Cu-Ti alloy in comparative example 1 of the present invention.
FIG. 3 is a microstructure diagram of an ingot of a Zn-Cu-Ti alloy in comparative example 2 of the present invention.
FIG. 4 is a microstructure diagram of an ingot of a Zn-Cu-Ti alloy in comparative example 3 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present 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.
The invention provides a preparation method of a Zn-Cu-Ti alloy ingot, which comprises the following steps:
s1, keeping the temperature of the alloy raw material and the rare earth material at 50-300 ℃ for 2-30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
s2, putting Zn into a melting furnace, heating to 420-500 ℃ to be completely melted, sequentially adding intermediate alloy containing Cu and/or Ti elements and rare earth materials into the Zn melt, heating the melting furnace to 450-650 ℃, and uniformly dispersing a covering agent on the surface of the melt;
s3, applying high-energy ultrasound to the melt to accelerate the diffusion and dissolution speed of Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 20-100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted;
and S4, adding a refining agent, refining for 5-30min, stopping ultrasonic treatment, and slagging off and casting the melt to obtain the Zn-Cu-Ti alloy cast ingot.
In the step S1, the alloy raw material comprises the following elements in percentage by mass: 0.05 to 2.0 percent of Cu, 0.05 to 0.5 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent;
the rare earth material is RE, Zn-REz,RECuxOne or a mixture of more of Cu-Ti-RE;
the rare earth material is calculated by RE, and the mass of RE is 0.01-1% of the total mass of the Zn-Cu-Ti alloy;
the Zn-REzZ in (a) is an integer of 1 to 50, RECuxX in (A) is an integer of 1 to 30.
The RE is one or a mixture of more of La, Ce, Y and Er.
The intermediate alloy containing Ti and/or Cu elements is binary alloy or ternary alloy;
the binary alloy is Zn-TimOr Zn-CunThe ternary alloy is Zn-Cuk-Tit，
M and n are the same or different and are respectively an integer of 1-50;
the k and the t are the same or different and are integers of 1-20 respectively.
The covering agent in the step S2 is one or a mixture of several of charcoal powder, ammonium chloride, sodium chloride and potassium chloride, and the thickness of the covering agent on the surface of the melt is 0.2-10 mm.
The refining agent in the step S4 is a nitrogen and chlorine mixed gas, a chlorine salt or an inert gas.
The ultrasonic power in the step S3 is 100-2000W, and the ultrasonic time is 5-30 min.
A Zn-Cu-Ti alloy ingot prepared by the method.
A Zn-Cu-Ti alloy plate is obtained by rolling the Zn-Cu-Ti alloy cast ingot for multiple times.
The multi-pass rolling process is one of hot rolling, hot rolling → cold rolling, hot rolling → warm rolling → cold rolling.
The hot rolling temperature is 200-350 ℃, the cold rolling temperature is room temperature, the warm rolling temperature is 80-180 ℃, the reduction per pass is 10-30%, the total reduction is controlled to be 65-95%, and the thickness of the finally prepared Zn-Cu-Ti alloy plate is 0.1-10 mm.
To further illustrate the above technical solutions, the present invention provides the following embodiments
Example 1
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the temperature of the alloy raw material and the rare earth material at 150 ℃ for 10min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 0.1 percent of Cu, 0.1 percent of Ti and the balance of Zn, wherein pure Zn (the purity is more than or equal to 99.995 percent), Zn-5Cu and Zn-5Ti intermediate alloy are adopted for proportioning, the total weight is 120kg, the selected rare earth is Zn-10Y intermediate alloy, and the mass fraction of rare earth Y is 0.15 percent of the total mass of the Zn-Cu-Ti alloy;
s2, putting Zn into a melting furnace, heating to 450 ℃ until the Zn is completely melted, sequentially adding dried Zn-5Ti, Zn-5Cu and Zn-10Y intermediate alloys into a Zn melt, heating the melting furnace to 550 ℃, and covering the surface of the melt with a mixture of sodium chloride (50 wt.%) and potassium chloride (50 wt.%), wherein the thickness of the covering agent on the surface of the melt is 5 mm;
s3, applying high-energy ultrasonic with ultrasonic power of 400W to the melt to accelerate the diffusion and dissolution speed of Ti, Cu and RE elements while performing the step S2, performing ultrasonic treatment for 30min to completely dissolve/melt the intermediate alloy, and reducing the temperature of the melting furnace to 460 ℃ after completely dissolving/melting;
and S4, filling mixed gas of nitrogen and chlorine (the volume ratio of nitrogen to chlorine is 4: 1) into the melt for refining, stopping ultrasonic treatment after refining for 10min, skimming the melt, and then casting the melt into a metal mold to obtain the high-quality Zn-Cu-Ti alloy cast ingot, wherein the microstructure of the high-quality Zn-Cu-Ti alloy cast ingot is shown in figure 1.
Heating the prepared Zn-Cu-Ti alloy cast ingot and a roller to 270 ℃, then carrying out multi-pass rolling, wherein the rolling reduction of each pass is 15%, the total rolling reduction is 92%, finally rolling out a Zn-Cu-Ti alloy plate with the thickness of 0.8mm, and trimming and straightening the plate.
Example 2
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the temperature of the alloy raw material and the rare earth material at 200 ℃ for 5min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 0.8 percent of Cu, 0.1 percent of Ti and the balance of Zn, wherein pure Zn (the purity is more than or equal to 99.995 percent) and a Zn-16Cu-2Ti intermediate alloy are adopted for proportioning, the total weight is 200kg, the selected rare earth types are Zn-5Er and Zn-5Ce mixed intermediate alloy, and the mass fractions of the rare earth Er and the rare earth Ce are respectively 0.1 percent and 0.05 percent;
s2, putting Zn into a melting furnace, heating to 420 ℃ until the Zn is completely melted, sequentially adding dried Zn-16Cu-2Ti, Zn-5Er and Zn-5Ce intermediate alloys into the Zn melt, heating the melting furnace to 580 ℃, and covering charcoal powder on the surface of the melt; simultaneously, applying high-energy ultrasound to the melt, wherein the ultrasound power is 500W, completely dissolving/melting the intermediate alloy after performing ultrasound for 10min, and then reducing the temperature of the smelting furnace to 450 ℃; covering ammonium chloride on the surface of the melt, wherein the thickness of the covering agent on the surface of the melt is 10 mm;
s3, applying high-energy ultrasonic with ultrasonic power of 1000W to the melt to accelerate the diffusion and dissolution speed of Ti, Cu and RE elements while performing the step S2, performing ultrasonic treatment for 15min to completely dissolve/melt the intermediate alloy, and reducing the temperature of the melting furnace to 460 ℃ after completely dissolving/melting;
and S4, filling ammonium chloride into the melt for refining, stopping ultrasonic treatment after refining for 10min, slagging off the melt, and casting the melt into a metal mold to obtain the high-quality Zn-Cu-Ti alloy cast ingot.
Heating the prepared Zn-Cu-Ti alloy cast ingot and a roller to 300 ℃, then starting rolling, firstly, roughly rolling the alloy with the thickness of 20mm to 5mm, then, finish rolling the alloy to the thickness of 0.6mm with the rolling reduction of 15% per pass, and then, trimming and straightening the plate to obtain the high-quality plate with accurate chemical components, no deformation, no crack, uniform thickness and excellent comprehensive performance.
Example 3
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the heat of the alloy raw material and the rare earth material at 50 ℃ for 30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 0.05 percent of Cu, 0.5 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent; 100kg of intermediate alloy Zn-5Ti, 100kg of Zn-5Cu and 100kg of Zn-5Cu-5T, wherein the selected rare earth is a Zn-3Er and Zn-3Ce mixed intermediate alloy, and the mass fractions of the rare earth Er and the rare earth Ce are respectively 0.01 percent of the total mass of the Zn-Cu-Ti alloy;
s2, putting Zn into a melting furnace, heating to 500 ℃ to be completely melted, sequentially adding an intermediate alloy containing Cu and/or Ti elements and a rare earth material into a Zn melt, heating the melting furnace to 650 ℃, and uniformly dispersing a covering agent on the surface of the melt; the covering agent is charcoal powder, and the thickness of the covering agent on the surface of the melt is 0.2 mm.
S3, applying 2000W high-energy ultrasonic wave to the melt to accelerate the diffusion and dissolution speed of the Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted; ultrasonic treatment for 5 min;
s4, adding refining agents of chloride salt and inert gas, refining for 5min, stopping ultrasonic treatment, slagging off and casting the melt to obtain a Zn-Cu-Ti alloy ingot, wherein the chloride salt KCl and MgCl are adopted2The mass ratio of the two is 2: 1; the inert gas is a mixed gas of nitrogen and chlorine, and the volume ratio of the nitrogen to the chlorine is 10: 1.
heating the prepared Zn-Cu-Ti alloy ingot and a roller to 250 ℃, then starting rolling, firstly, roughly rolling the alloy with the thickness of 10mm to 3mm, then, cold-rolling the alloy to the thickness of 1mm with the rolling reduction of 25% per pass, and then, trimming and straightening the plate to obtain the high-quality plate with accurate chemical components, no deformation, no crack, uniform thickness and excellent comprehensive performance.
Example 4
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the temperature of the alloy raw material and the rare earth material at 300 ℃ for 2min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 2 percent of Cu, 0.05 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent; the intermediate alloy is a Zn-10Cu-10Ti ternary alloy, the weight of the intermediate alloy is 500kg, the selected rare earth is a Zn-5Er and Zn-3Ce mixed intermediate alloy, and the mass fractions of the rare earth Er and the rare earth Ce are respectively 1% of the total mass of the Zn-Cu-Ti alloy;
s2, putting Zn into a melting furnace, heating to 480 ℃ to be completely melted, sequentially adding an intermediate alloy containing Cu and/or Ti elements and a rare earth material into a Zn melt, heating the melting furnace to 450 ℃, and uniformly dispersing a covering agent on the surface of the melt; the covering agent is charcoal powder, and the thickness of the covering agent on the surface of the melt is 5 mm.
S3, applying 100W high-energy ultrasonic waves with ultrasonic power to the melt to accelerate the diffusion and dissolution speed of the Ti, Cu and RE elements while performing the step S2, and reducing the temperature of the smelting furnace to 60 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted; ultrasonic treatment time is 30 min;
s4, adding a refining agent of chlorine salt and inert gas, refining for 20min, stopping ultrasonic treatment, and slagging off and casting the melt to obtain a Zn-Cu-Ti alloy cast ingot;
the chloride salts KCl and MgCl2The mass ratio of the two is 2: 1; the inert gas is argon.
Heating the prepared Zn-Cu-Ti alloy cast ingot and a roller to 300 ℃, then starting rolling, firstly, roughly rolling the alloy with the thickness of 12mm to 6mm, then rolling to the thickness of 3mm at the temperature of 120 ℃ with the rolling reduction of 25% per pass, and then cold rolling to the thickness of 0.8mm with the rolling reduction of 20% per pass; and then, trimming and straightening the plate to obtain the high-quality plate with accurate chemical components, no deformation, no crack, uniform thickness and excellent comprehensive performance.
Example 5
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the heat of the alloy raw material and the rare earth material at 50 ℃ for 30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 0.5 percent of Cu, 0.1 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent; 20kg of intermediate alloy Zn-20Ti, 100kg of Zn-20Cu or 100kg of Zn-20Cu-4Ti, wherein the selected rare earth is a Zn-20Er and Zn-20Ce mixed intermediate alloy, and the mass fractions of the rare earth Er and the rare earth Ce are respectively 0.02 percent of the total mass of the Zn-Cu-Ti alloy;
s2, putting Zn into a melting furnace, heating to 500 ℃ to be completely melted, sequentially adding an intermediate alloy containing Cu and/or Ti elements and a rare earth material into a Zn melt, heating the melting furnace to 650 ℃, and uniformly dispersing a covering agent on the surface of the melt; the covering agent is charcoal powder, and the thickness of the covering agent on the surface of the melt is 0.2 mm.
S3, applying 1500W high-energy ultrasonic to the melt to accelerate the diffusion and dissolution speed of the Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted; ultrasonic treatment for 5 min;
s4, adding refining agents of chloride salt and inert gas, refining for 5min, stopping ultrasonic treatment, slagging off and casting the melt to obtain a Zn-Cu-Ti alloy ingot, wherein the chloride salt KCl and MgCl are adopted2The mass ratio of the two is 2: 1; the inert gas is a mixed gas of nitrogen and chlorine, and the volume ratio of the nitrogen to the chlorine is 10: 1.
heating the prepared Zn-Cu-Ti alloy ingot and a roller to 250 ℃, then starting rolling, firstly, roughly rolling the alloy with the thickness of 10mm to 3mm, then, cold-rolling the alloy to the thickness of 1mm with the rolling reduction of 25% per pass, and then, trimming and straightening the plate to obtain the high-quality plate with accurate chemical components, no deformation, no crack, uniform thickness and excellent comprehensive performance.
Example 6
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the heat of the alloy raw material and the rare earth material at 50 ℃ for 30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 1% of Cu, 0.1% of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2%; 10kg of intermediate alloy Zn-20Ti, 50kg of Zn-40Cu or 100kg of Zn-20Cu-2Ti, wherein the selected rare earth is Zn-40Y intermediate alloy, and the mass fraction of the rare earth Y is 0.03 percent of the total mass of the Zn-Cu-Ti alloy;
s2, putting Zn into a melting furnace, heating to 550 ℃ to be completely melted, sequentially adding an intermediate alloy containing Cu and/or Ti elements and a rare earth material into a Zn melt, heating the melting furnace to 680 ℃, and uniformly dispersing a covering agent on the surface of the melt; the covering agent is charcoal powder, and the thickness of the covering agent on the surface of the melt is 0.2 mm.
S3, applying high-energy ultrasonic with the ultrasonic power of 1200W to the melt to accelerate the diffusion and dissolution speed of the Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted; ultrasonic treatment for 5 min;
s4, adding refining agents of chloride salt and inert gas, refining for 5min, stopping ultrasonic treatment, slagging off and casting the melt to obtain a Zn-Cu-Ti alloy ingot, wherein the chloride salt KCl and MgCl are adopted2The mass ratio of the two is 2: 1; the inert gas is a mixed gas of nitrogen and chlorine, and the volume ratio of the nitrogen to the chlorine is 10: 1.
heating the prepared Zn-Cu-Ti alloy ingot and a roller to 250 ℃, then starting rolling, firstly, roughly rolling the alloy with the thickness of 15mm to 5mm, then, cold-rolling the alloy to the thickness of 1mm by the rolling reduction of 20% per pass, and then, trimming and straightening the plate to obtain the high-quality plate with accurate chemical components, no deformation, no crack, uniform thickness and excellent comprehensive performance.
Example 7
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the heat of the alloy raw material and the rare earth material at 50 ℃ for 30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 0.05 percent of Cu, 0.5 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent; 10kg of intermediate alloy Zn-50Ti, 1kg of Zn-50Cu or 25kg of Zn-2Cu-20Ti, wherein the selected rare earth is Zn-50Er intermediate alloy, and the mass fraction of the rare earth Er is 0.02 percent of the total mass of the Zn-Cu-Ti alloy;
s2, putting Zn into a melting furnace, heating to 520 ℃ to be completely melted, sequentially adding an intermediate alloy containing Cu and/or Ti elements and a rare earth material into a Zn melt, heating the melting furnace to 650 ℃, and uniformly dispersing a covering agent on the surface of the melt; the covering agent is charcoal powder, and the thickness of the covering agent on the surface of the melt is 0.2 mm.
S3, applying 1500W high-energy ultrasonic to the melt to accelerate the diffusion and dissolution speed of the Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted; ultrasonic treatment for 5 min;
s4, adding refining agents of chloride salt and inert gas, refining for 5min, stopping ultrasonic treatment, slagging off and casting the melt to obtain a Zn-Cu-Ti alloy ingot, wherein the chloride salt KCl and MgCl are adopted2The mass ratio of the two is 2: 1; the inert gas is a mixed gas of nitrogen and chlorine, and the volume ratio of the nitrogen to the chlorine is 10: 1.
heating the prepared Zn-Cu-Ti alloy ingot and a roller to 250 ℃, then starting rolling, firstly, roughly rolling the alloy with the thickness of 12mm to 4mm, then, cold-rolling the alloy to the thickness of 0.8mm by the rolling reduction of 25% per pass, and then, trimming and straightening the plate to obtain the high-quality plate with accurate chemical components, no deformation, no crack, uniform thickness and excellent comprehensive performance.
Example 8
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the heat of the alloy raw material and the rare earth material at 50 ℃ for 30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 2 percent of Cu, 0.5 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent; 10kg of intermediate alloy Zn-10Ti, 10kg of Zn-40Cu or 20kg of Zn-20Cu-5Ti, wherein the selected rare earth is Zn-10Ce intermediate alloy, and the mass fraction of the rare earth Ce is 0.02 percent of the total mass of the Zn-Cu-Ti alloy;
s2, putting Zn into a melting furnace, heating to 500 ℃ to be completely melted, sequentially adding an intermediate alloy containing Cu and/or Ti elements and a rare earth material into a Zn melt, heating the melting furnace to 650 ℃, and uniformly dispersing a covering agent on the surface of the melt; the covering agent is charcoal powder, and the thickness of the covering agent on the surface of the melt is 0.2 mm.
S3, applying 1500W high-energy ultrasonic to the melt to accelerate the diffusion and dissolution speed of the Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted; ultrasonic treatment for 5 min;
s4, adding refining agents of chloride salt and inert gas, refining for 5min, stopping ultrasonic treatment, slagging off and casting the melt to obtain a Zn-Cu-Ti alloy ingot, wherein the chloride salt KCl and MgCl are adopted2The mass ratio of the two is 2: 1; the inert gas is a mixed gas of nitrogen and chlorine, and the volume ratio of the nitrogen to the chlorine is 10: 1.
heating the prepared Zn-Cu-Ti alloy ingot and a roller to 250 ℃, then starting rolling, firstly, roughly rolling the alloy with the thickness of 10mm to 3mm, then, cold-rolling the alloy to the thickness of 0.75mm by the rolling reduction of 20% per pass, and then, trimming and straightening the plate to obtain the high-quality plate with accurate chemical components, no deformation, no crack, uniform thickness and excellent comprehensive performance.
Example 9
The embodiment provides a method for preparing a Zn-Cu-Ti alloy ingot at a low temperature efficiently by rare earth modification and ultrasonic treatment, which comprises the following steps:
s1, preserving the heat of the alloy raw material and the rare earth material at 50 ℃ for 30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
the alloy raw materials comprise pure Zn and intermediate alloy containing Ti and/or Cu elements, and the mass percentage of each element is as follows: 0.05 percent of Cu, 0.05 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent; 100kg of intermediate alloy Zn-Ti, 100kg of Zn-Cu or 100kg of Zn-Cu-Ti, wherein the selected rare earth is Zn-10Y intermediate alloy, and the mass fraction of the rare earth Y is 0.01 percent of the total mass of the Zn-Cu-Ti alloy;
s2, putting Zn into a melting furnace, heating to 520 ℃ to be completely melted, sequentially adding an intermediate alloy containing Cu and/or Ti elements and a rare earth material into a Zn melt, heating the melting furnace to 600 ℃, and uniformly dispersing a covering agent on the surface of the melt; the covering agent is charcoal powder, and the thickness of the covering agent on the surface of the melt is 0.2 mm.
S3, applying 2000W high-energy ultrasonic wave to the melt to accelerate the diffusion and dissolution speed of the Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted; ultrasonic treatment for 5 min;
s4, adding refining agents of chloride salt and inert gas, refining for 5min, stopping ultrasonic treatment, slagging off and casting the melt to obtain a Zn-Cu-Ti alloy ingot, wherein the chloride salt KCl and MgCl are adopted2The mass ratio of the two is 2: 1; the inert gas is a mixed gas of nitrogen and chlorine, and the volume ratio of the nitrogen to the chlorine is 10: 1.
heating the prepared Zn-Cu-Ti alloy ingot and a roller to 230 ℃, then starting rolling, firstly, roughly rolling the alloy with the thickness of 12mm to 3mm, then, cold-rolling the alloy to the thickness of 0.8mm by the rolling reduction of 25% per pass, and then, trimming and straightening the plate to obtain the high-quality plate with accurate chemical components, no deformation, no crack, uniform thickness and excellent comprehensive performance.
Comparative example 1
This comparative example provides a Zn-Cu-Ti alloy and a method for manufacturing a plate thereof, which are different from those of example 1 in that a Zn-10Y rare earth intermediate alloy is not added, and the rest is the same as that of example 1, and the microstructure of the alloy is shown in FIG. 2.
Comparative example 2
This comparative example provides a Zn-Cu-Ti alloy and a method for manufacturing a plate thereof, which are different from those of example 1 in that a Zn-Cu-Ti alloy melt was not subjected to ultrasonic treatment, and the rest were the same as those of example 1, and the microstructure of the alloy thereof is shown in FIG. 3.
Comparative example 3
The present comparative example provides a Zn-Cu-Ti alloy and a method for manufacturing a plate thereof, which are different from example 1 in that a Zn-10Y rare earth intermediate alloy is not introduced into a Zn-Cu-Ti alloy melt and is not subjected to ultrasonic treatment, and the rest is the same as example 1, and the alloy microstructure thereof is shown in fig. 4.
Comparative example 4
The comparative example provides a Zn-Cu-Ti alloy and a preparation method of a plate thereof, which are different from those of the example 2 in that Zn-5Er and Zn-5Ce mischmetal intermediate alloy are not added, and the rest is the same as that of the example 2.
Comparative example 5
This comparative example provides a Zn-Cu-Ti alloy and a method for manufacturing a plate thereof, which are different from example 2 in that the melt of the Zn-Cu-Ti alloy is not subjected to ultrasonic treatment, and the others are the same as example 2.
Comparative example 6
The comparative example provides a Zn-Cu-Ti alloy and a preparation method of a plate thereof, which are different from those of the example 2 in that a Zn-Cu-Ti alloy melt is not introduced with a Zn-5Er and Zn-5Ce mischmetal intermediate alloy and is not subjected to ultrasonic treatment, and the rest is the same as that of the example 2.
The Zn-Cu-Ti alloy sheets prepared in examples 1 and 2 above and the Zn-Cu-Ti alloy sheets prepared in comparative examples 1 to 6 were compared in microstructure and mechanical properties, and the results are shown in FIGS. 1 to 4 and Table 1.
TABLE 1
As can be seen from Table 1 and FIGS. 1 to 4, compared with the Zn-Cu-Ti alloy sheets prepared in comparative examples 1 to 6, the Zn-Cu-Ti alloy sheet obtained in the present invention has a finer microstructure, and the prepared Zn-Cu-Ti alloy sheet has more excellent toughness, so that the Zn-Cu-Ti alloy sheet developed in the present invention has a wide application range and good economic benefits.
The method for efficiently preparing the Zn-Cu-Ti alloy and the plate at low temperature by the rare earth modification synergistic ultrasonic treatment provided by the embodiment of the application patent is described in detail. The above description of the embodiments is only for the purpose of helping to understand the method of the present application and its core ideas;
it should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (12)
1. A preparation method of a Zn-Cu-Ti alloy ingot is characterized by comprising the following steps:
s1, keeping the temperature of the alloy raw material and the rare earth material at 50-300 ℃ for 2-30min, and preheating and drying; the alloy raw material comprises Zn and intermediate alloy containing Ti and/or Cu elements;
s2, putting Zn into a melting furnace, heating to 420-500 ℃ to be completely melted, sequentially adding intermediate alloy containing Cu and/or Ti elements and rare earth materials into the Zn melt, heating the melting furnace to 450-650 ℃, and uniformly dispersing a covering agent on the surface of the melt;
s3, applying high-energy ultrasound to the melt to accelerate the diffusion and dissolution speed of Ti, Cu and RE elements while the step S2 is carried out, and reducing the temperature of the smelting furnace to be 20-100 ℃ above the liquidus temperature of the Zn-Cu-Ti alloy after the Ti, Cu and RE elements are completely dissolved/melted;
and S4, adding a refining agent, refining for 5-30min, stopping ultrasonic treatment, and slagging off and casting the melt to obtain the Zn-Cu-Ti alloy cast ingot.
2. The method of producing a Zn-Cu-Ti alloy ingot according to claim 1, wherein,
in the step S1, the alloy raw material comprises the following elements in percentage by mass: 0.05 to 2.0 percent of Cu, 0.05 to 0.5 percent of Ti and the balance of Zn, wherein the mass fraction of impurities is less than or equal to 0.2 percent;
the rare earth material is RE, Zn-REz,RECuxOne or a mixture of more of Cu-Ti-RE;
the rare earth material is calculated by RE, and the mass of RE is 0.01-1% of the total mass of the Zn-Cu-Ti alloy;
the Zn-REzZ in (a) is an integer of 1 to 50, RECuxX in (A) is an integer of 1 to 30.
3. The method of producing a Zn-Cu-Ti alloy ingot according to claim 2, wherein,
the RE is one or a mixture of more of La, Ce, Y and Er.
4. The method of producing a Zn-Cu-Ti alloy ingot according to claim 2, wherein,
the intermediate alloy containing Ti and/or Cu elements is binary alloy or ternary alloy;
the binary alloy is Zn-TimOr Zn-CunThe ternary alloy is Zn-Cuk-Tit，
M and n are the same or different and are respectively an integer of 1-50;
the k and the t are the same or different and are integers of 1-20 respectively.
5. The method of producing a Zn-Cu-Ti alloy ingot according to claim 1, wherein,
the covering agent in the step S2 is one or a mixture of several of charcoal powder, ammonium chloride, sodium chloride and potassium chloride, and the thickness of the covering agent on the surface of the melt is 0.2-10 mm.
6. The method of producing a Zn-Cu-Ti alloy ingot according to claim 1, wherein,
the refining agent in the step S4 is a nitrogen and chlorine mixed gas, a chlorine salt or an inert gas.
7. The method for producing an ingot of Zn-Cu-Ti alloy as set forth in claim 1, wherein the ultrasonic power in the step S3 is 100-2000W and the ultrasonic time is 5-30 min.
8. The method of producing an ingot of Zn-Cu-Ti alloy as set forth in claim 7, wherein the volume ratio of the nitrogen gas to the chlorine gas in the mixed gas is (20: 1) - (5: 1).
9. An ingot of a Zn-Cu-Ti alloy produced by the method according to any one of claims 1 to 8.
10. A Zn-Cu-Ti alloy plate, characterized in that the plate is obtained by rolling the Zn-Cu-Ti alloy ingot of claim 7 in multiple passes.
11. The Zn-Cu-Ti alloy sheet according to claim 10, wherein the multi-pass rolling process is one of a hot rolling, a hot rolling → a cold rolling, a hot rolling → a warm rolling → a cold rolling.
12. The Zn-Cu-Ti alloy sheet as claimed in claim 11, wherein the hot rolling temperature is 200-350 ℃, the cold rolling temperature is room temperature, the warm rolling temperature is 80-180 ℃, the reduction per pass is 10-30%, the total reduction is controlled at 65-95%, and the thickness of the finally prepared Zn-Cu-Ti alloy sheet is 0.1-10 mm.
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