CN109967703B - Method for continuously and efficiently preparing wide amorphous thin strip with thickness of 80-1500 mu m at high cooling speed - Google Patents
Method for continuously and efficiently preparing wide amorphous thin strip with thickness of 80-1500 mu m at high cooling speed Download PDFInfo
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- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
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- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
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Abstract
The invention belongs to the field of amorphous alloy preparation, and particularly relates to a method for efficiently preparing a wide amorphous thin strip with the thickness of 80-1500 mu m by using a double-roll method at a continuous high cooling speed. The method comprises the following steps: (1) smelting amorphous alloy according to set components, wherein the components comprise zirconium base, copper base, iron base, nickel base and the like, and the amorphous metal with the ultimate cooling rate of 500-75000 ℃/s is used for designing a method for continuously forming a thin strip of the amorphous alloy, so that a base material is provided for the subsequent processing procedures; (2) forming a wide casting belt with the thickness of 80-1500 mu m after a thin belt continuous casting process; (3) smelting, forming and coiling are carried out under the condition of inert atmosphere. Aiming at the problems that the requirements of amorphous alloy preparation on raw materials and preparation technology are high and mass production of amorphous alloy plate strips is not available, the invention realizes the continuous casting and rolling process of amorphous strips with the length of more than 12m and the thickness of 80-1500 mu m.
Description
Technical Field
The invention belongs to the field of amorphous alloy preparation, and particularly relates to a method for efficiently preparing a wide amorphous thin strip with the thickness of 80-1500 mu m by using a double-roll method at a continuous high cooling speed.
Background
Amorphous Alloy, also called Metallic Glass or Glass Alloy, is a new, special Alloy material with a material state obviously different from the crystalline state, which is prepared by applying modern rapid solidification metallurgy technology. Due to the unique atomic structure arrangement and the metal bond composition of the amorphous alloy, the amorphous alloy has more excellent mechanical property, physical property and chemical property compared with the traditional crystalline metal material. The amorphous alloy has wide application prospect in the aspects of aerospace, weapon industry, precise instruments, biomedical treatment, electric power transmission and the like.
The preparation of early amorphous alloys required very high cooling rates (> 10)6K/s), the amorphous alloy can only exist in the forms of powder, wire, thin strip and the like, the performance potential of the amorphous alloy is greatly weakened, and the application of the amorphous alloy in the industry is limited. Therefore, since the end of the last eighties, how to improve the forming capability of amorphous alloys becomes one of the important research directions in the research field of new materials. In decades from the 20 th century, 80 s to date, a large number of alloy systems having a large glass forming ability, such as Zr-based, Ti-based, Fe-based, Co-based, Ni-based, Cu-based, Pt-based, and the like, have been developed through efforts of a large number of scholars; the preparation technology of various block amorphous alloys such as a water quenching method, a copper mold casting method, a directional solidification method, an amorphous powder extrusion method and the like is developed. The amorphous thin strip with excellent soft magnetic performance produced by the single-roll method is widely applied in China in a large scale, and makes a prominent contribution to energy conservation and emission reduction of electric power systems in China. Moreover, the preparation and application of bulk amorphous alloys have been greatly developed, and due to their excellent mechanical properties, they have been used as structural materials for the production and application of electronic products, sports equipment, automobile parts, etc. At present, the most main production mode of the bulk amorphous alloy products applied to the market is a die casting method, and only small-specification products can be produced due to the limitation of the conditions of the bulk amorphous alloy products. However, there is still no reliable production method for the sheet and strip material widely used as a structural material. Therefore, how to realize continuous, large-scale and stable production of amorphous alloy plates and strips and promote the wide application of bulk amorphous alloys is one of the problems which are urgently needed to be solved by the current amorphous industry.
Currently, the main production methods of amorphous strip include single roll melt quenching, twin roll melt quenching, and cast strip casting. At present, the most widely used method for industrial production is a single-roller melt quenching method, which is called a single-roller method for short. The iron-based amorphous strip produced by the single-roll method has excellent soft magnetic performance, can replace silicon steel and permalloy to manufacture a transformer iron core, further greatly improves the efficiency of the transformer, reduces the iron loss of a distribution transformer, and simultaneously reduces the volume and the weight. However, the single roll process limits the thickness (about 20-50 μm) and width (less than 220mm) of the strip. The twin-roll melt quenching method is abbreviated as twin-roll method. A plurality of continuous casting methods of bulk amorphous alloys are developed based on a double-roller method. U.S. patent (publication No. US2006/0260782A1) discloses a continuous holding device and method for a block amorphous alloy sheet, wherein a plurality of groups of small-diameter cooling rollers are adopted for cooling an alloy strip, the row rollers can only apply small contact pressure, the system cooling speed can only reach less than 10 ℃/s, the thickness of the prepared sheet is 0.1-10 mm, and the sheet is only limited to forming of Zr-based amorphous alloy containing Be with strong forming capacity, and the amorphous life and stability can also Be reduced. The Chinese patent (publication No. CN 107755652A) is close to the technical idea, and uses crawler cooling to continuously cast amorphous, the contact force is small, the cooling speed is limited, and the service life of the amorphous is reduced and the design redundancy of the ingredients for preparing the amorphous is reduced. Chinese patent (publication No. CN1486800A) discloses a continuous casting and rolling technique for bulk amorphous alloy, in which molten metal in a crucible is poured into two water-cooled rollers rotating relatively to each other, and double-roller casting and rolling are used to prepare bulk amorphous plates, bars, etc., but the patent does not have specific process protection nodes and technical implementation schemes, and does not disclose detailed parameters such as melting temperature, heat preservation measures, flow control measures, cooling speed, casting and rolling force, etc. And relatively large rolling force can be applied to the position of the roll gap to realize large cooling speed, the cooling capacity is larger than that of a single-roll method in theory, and the amorphous alloy plate strip with large thickness specification can be prepared. The casting mold drawing casting process is one continuous casting process of smelting mother alloy in a crucible, maintaining temperature, casting the mother alloy into water cooled hole pattern via a nozzle and drawing the amorphous alloy at certain speed to cast amorphous alloy. Chinese patent publication No. CN101543885A discloses a device and method for horizontal continuous casting of bulk amorphous alloy, wherein the cooling of the alloy mainly depends on a water-cooled copper mold, and the solidified casting blank is continuously output by being pulled by a traction rod driven by a motor.
Disclosure of Invention
Aiming at the problems that the requirements of amorphous alloy preparation on raw materials and preparation technology are high and the mass production of amorphous alloy plate strips is not available, the invention aims to provide a method for efficiently preparing a wide amorphous thin strip with the thickness of 80-1500 mu m by using a double-roller method at a continuous high cooling speed, and realize the continuous casting and rolling process of the amorphous strip with the length of more than 12m and the thickness of 80-1500 mu m.
The technical scheme of the invention is as follows:
a method for continuously and efficiently preparing a wide amorphous thin strip with the thickness of 80-1500 mu m at a high cooling speed comprises the following steps:
(1) alloy discharging enters a crucible, a preheating guide pipe and a position control device thereof are cleaned, the inner part of the preheating guide pipe is a quartz lining and is attached with a heating system, the heating temperature is 100-200 ℃ above the solidification temperature of the target alloy, and cooling water is introduced to the outer part of the preheating guide pipe for protection;
(2) the amorphous master alloy is smelted according to set components and comprises the following components: melting metals in a zirconium-based, copper-based, iron-based or nickel-based amorphous alloy component system, uniformly mixing for 5-30 minutes, and controlling the temperature;
(3) controlling the superheat degree of an alloy melt to be 50-300 ℃, protecting by adopting high-purity argon with volume purity of more than 99.999% in the temperature control process, and enabling argon in a smelting cavity to be micro-positive pressure, namely, the pressure is not lower than 0.11 MPa;
(4) in the smelting process, the preparation work of the forming cavity is completed, and the method comprises the following steps: a) all valve bodies on the cavity of the forming cavity are closed, argon is filled after vacuum pumping, the volume purity is more than 99.99 percent, and the micro positive pressure not lower than 0.11MPa is kept; b) preheating a flow distribution nozzle, wherein the flow distribution nozzle adopts slit type flow distribution, and is installed and heated after entering a fixed position, and the heating temperature is 100-200 ℃ above the solidification temperature of a target alloy; c) the temperature of the cooling circulating water of the casting roller is 3-5 ℃, and the total water flow is 70-90 m3H; d) preparing a gas cooling system after casting, wherein the argon pressure is 0.6-0.8 MPa, and the gas temperature is controlled to be 4-6 ℃;
(5) alloy smelting, preheating of a preheating guide pipe and a flow distribution nozzle, and argon filling of a forming cavity, preparing an amorphous thin strip by adopting a vertical thin strip casting and rolling process, and performing a thin strip continuous casting process: opening a gate valve of the smelting cavity, descending the preheating guide pipe to be in butt joint with the flow distribution nozzle, and pouring alloy into the preheating guide pipe by the medium-frequency induction smelting furnace; the flow distribution nozzle is made of transparent quartz, the height of a melt inside the flow distribution nozzle is controlled to be 40-60 mm through the monitoring of an infrared monitoring camera and the tilting speed of a medium-frequency induction smelting furnace, an alloy melt is uniformly distributed and flowed into a roll gap of a casting roll vertically through the flow distribution nozzle by liquid level, the height of the alloy melt at the liquid level of the roll gap is controlled to be 2-10 mm, the cooling speed of the alloy melt is 500-75000 ℃/s, and the alloy is cooled and cast-rolled to form; guiding the formed amorphous thin belt out through a guide roller, further cooling the amorphous thin belt in a cast gas cooling system, and adopting low-temperature argon for blowing and cooling, wherein the gas cooling speed is 50-800 ℃/s;
(6) after the gas is cooled, the thickness range of the amorphous thin strip reaches 80-1500 mu m, and the width range of the amorphous thin strip is 110-550 mm; and coiling the casting strip with the thickness of 80-800 mu m, and directly collecting the casting strip with the thickness of more than 800 mu m in a thin strip form without coiling.
In the method for continuously and efficiently preparing the wide amorphous thin strip with the thickness of 80-1500 mu m at the high cooling speed, in the casting and rolling process, the alloy is rapidly cooled by the heat transfer of a casting roller, the temperature of the alloy thin strip out of the roller is regulated and controlled by controlling the casting and rolling speed, the casting and rolling force and the roll gap, and the temperature of the alloy out of the roller is controlled to be close to or less than the crystallization temperature Tx of the alloy; the casting and rolling speed is 0.20-1.8 m/s, the casting and rolling force is controlled to be 2-15 kN per 1cm width of casting strip, the width of a roll gap opening of a casting roll is set to be 80-1500 mu m, and no side sealing plate is arranged.
The continuous high-cooling-rate efficient preparation method of the wide amorphous thin strip with the thickness of 80-1500 mu m controls the solidification cooling speed to reach 500-75000 ℃/s through the casting and rolling technological parameters of the opening size of the lower end of the flow distribution nozzle, the roll gap value of the casting roll, the casting and rolling speed, the copper casting roll, the steel casting roll and the cooling water amount of the casting roll.
According to the method for continuously and efficiently preparing the wide amorphous ribbon with the thickness of 80-1500 mu m at the high cooling speed, 0.0045-0.020 mass percent of yttrium element is added into a zirconium-based, copper-based, iron-based or nickel-based amorphous alloy for removing O, N pollution brought by the environment.
The method for continuously and efficiently preparing the wide amorphous thin belt with the thickness of 80-1500 mu m at a high cooling speed adopts a quartz slit type flow distribution nozzle for flow distribution, and the opening width of the slit is designed according to the thickness of different products; the flow distribution nozzle is preheated on line, the preheating temperature is 100-200 ℃ above the alloy solidification temperature, the opening end part of the lower end of the flow distribution nozzle conducts heat through a tungsten alloy sheet, the temperature of the end part of the flow distribution nozzle reaches the temperature near the alloy solidification temperature, and a dam punch is arranged inside the flow distribution nozzle to stabilize the flow; the lining of the preheating flow guide pipe is made of quartz glass which can be quickly replaced, the preheating temperature is 100-200 ℃ above the alloy solidification temperature, and cooling water is introduced to the outside of the preheating flow guide pipe for protection.
According to the method for continuously preparing the wide amorphous thin strip with the thickness of 80-1500 mu m at high cooling speed and high efficiency, the infrared monitoring camera is arranged on the width side surface of the flow distribution nozzle and is fed back to a tipping control system to achieve the purpose of flow distribution control; wherein, the height control range of the opening at the lower end of the flow distribution nozzle from the Kiss line of the casting roll is 10-50 mm, and the liquid level height in the flow distribution nozzle is 40-60 mm.
According to the method for continuously and efficiently preparing the wide amorphous thin strip with the thickness of 80-1500 mu m at the large cooling speed, two horizontally opposite rollers are used as casting rollers, supporting rollers are additionally arranged on two sides of each roller, the diameter of each casting roller is 280-420 mm, and the diameter of each group of supporting rollers is 100mm larger than that of each casting roller.
the method for continuously and efficiently preparing the wide amorphous thin strip with the thickness of 80-1500 mu m at high cooling speed adopts a graded vacuum design for a smelting cavity and a forming cavity, wherein the working vacuum degree of the smelting cavity reaches 1 × 10-2The vacuum degree of the forming cavity reaches below 1 Pa; and in the pouring state, the environment is in an argon protection state, the smelting cavity and the forming cavity are separated by a gate valve, and the gate valve is opened after the argon is filled before the casting and rolling are started.
The method for continuously and efficiently preparing the wide amorphous ribbon with the thickness of 80-1500 mu m at high cooling speed adopts a medium-frequency induction smelting furnace and a high-purity graphite (the carbon content is more than or equal to 99.99 wt%) crucible to carry out amorphous alloy smelting, the heating temperature is not more than 400 ℃ above the melting temperature of metal, and oxidation and burning loss of metal elements are prevented.
According to the method for continuously and efficiently preparing the wide amorphous thin strip with the thickness of 80-1500 mu m at a high cooling speed, the cast strip trimming waste material which is not more than 20wt% is added into the amorphous master alloy incoming material.
The invention has the advantages and beneficial effects that:
1. for the continuous forming process of bulk amorphous alloys, a large cooling rate and good stability are essential. And the casting mode of the common casting and rolling equipment is simple, and the alloy molten pool is wide, so that the cooling speed of the alloy in a shallow supercooled liquid region is low, and the amorphous alloy is difficult to form. According to the characteristics of bulk amorphous solidification, a double-roller casting and rolling technology is combined, a deep roll gap casting method is adopted, and the alloy molten pool is narrow, the cooling speed is high, and the deformation is small. The principle, structure and method are not reported in public.
2. The solidification cooling speed can be controlled to reach 500-75000 ℃/s through casting and rolling technological parameters such as slit width of a flow distribution nozzle, roll gap value of a casting roll, casting speed, copper casting roll, steel casting roll, cooling water quantity of the casting roll and the like. The method for continuously forming the thin strip of the amorphous metal is designed aiming at the amorphous metal with the series forming limit cooling rate of 500-75000 ℃/s, and a base material is provided for the subsequent processing procedures.
3. The invention adopts a quartz slit type flow distribution nozzle for flow distribution, and the opening width of the slit is designed to be 0.15-0.8 mm according to the thickness of different products. The flow distribution nozzle can be preheated on line at a working position, the preheating temperature is 100-200 ℃ above the alloy solidification temperature, the end part of the flow distribution nozzle conducts heat through the tungsten alloy sheet, and the temperature of the end part reaches the vicinity of the alloy solidification temperature. A dam is arranged in the flow distribution nozzle for flow stabilization.
4. According to the invention, the infrared monitoring camera is arranged on the width side surface of the flow distribution nozzle and feeds back to the tipping control system to achieve the aim of flow distribution control. Wherein the height control range of the opening at the lower end of the flow distribution nozzle from a Kiss line (Kiss line refers to the line closest to the double working rolls) of the casting roll gap is 10-50 mm, and the liquid level height in the flow distribution nozzle is 40-60 mm. The casting and rolling system adopts a flow-casting speed matching strategy to control the roll gap of the alloy melt to freely flow along the vertical direction, and a side sealing plate in the casting and rolling process is eliminated.
5. The casting and rolling system adopts a mode of additionally installing the supporting roll of the casting roll to improve the transverse stable control and reduce the thickness deviation of the transmission side and the operation side of the casting machine. The diameter of the casting roll is 280-420 mm, the diameter of each group of supporting rolls is larger than the diameter of the working roll (casting roll) by 100mm, and the roughness Ra of the roll surface is less than or equal to 10 mu m.
6. The invention adopts a flow guide design with preheating, the lining of the preheating flow guide pipe is made of quartz glass which can be quickly replaced, the preheating temperature is 100-200 ℃ above the alloy solidification temperature, and the preheating flow guide pipe can be protected by introducing cooling water to the outside.
7. the invention relates to a graded vacuum design of a smelting cavity and a forming cavity, wherein the working vacuum degree of the smelting cavity reaches 1 × 10-2And (4) below Pa, ensuring that the vacuum degree of the forming cavity reaches below 1Pa, and quickly filling argon. And in the pouring state, the environment is in an argon protection state, the smelting cavity and the forming cavity are separated by a gate valve, and the gate valve is opened after the argon is filled before the casting and rolling are started.
8. The cast gas cooling system adopts low-temperature argon purging cooling, and the cooling speed is 50-800 ℃/s.
Drawings
FIG. 1 is a schematic structural diagram of a casting and rolling device for continuously and efficiently preparing a wide amorphous thin strip at a high cooling speed. In the figure, 1 a medium frequency induction melting furnace; 2, a high vacuum smelting cavity; 3, the guide pipe can be preheated; 4, a gate valve; 5, a flow distribution nozzle and an infrared camera monitoring device; 51 a flow distribution nozzle; 52 infrared monitoring camera; 6 forming a cavity; 7, supporting the roller; 8, casting rolls; 9, a post-casting gas cooling system; 10, a coiling device; 11 tip-over control system.
FIG. 2 is a schematic illustration of a 0.55mm thick amorphous ribbon.
Fig. 3 is a photograph (a) of the microstructure and an XRD chart (b). In the figure, the abscissa 2 θ represents the diffraction angle (drge) and the ordinate intensity represents the relative intensity (a.u.).
Fig. 4 shows a microstructure photograph (a) and an XRD chart (b). In the figure, the abscissa 2 θ represents the diffraction angle (drge) and the ordinate intensity represents the relative intensity (a.u.).
Detailed Description
As shown in FIG. 1, the casting and rolling device for continuously preparing the wide amorphous thin strip at high cooling speed and high efficiency mainly comprises: the medium-frequency induction smelting furnace 1, the high vacuum smelting chamber 2 (the chamber pressure is less than 0.1Pa), can preheat honeycomb duct 3, slide valve 4, flow distribution nozzle and infrared camera monitoring device 5, forming chamber 6, backing roll 7, casting roll 8, after-casting gas cooling system 9, coiling equipment 10, tipping control system 11 etc. and the concrete structure is as follows:
the bottom opening of the high vacuum melting cavity 2 corresponds to the top opening of the forming cavity 6, and the bottom opening of the high vacuum melting cavity 2 is communicated with the top opening of the forming cavity 6 through a gate valve 4; a medium-frequency induction smelting furnace 1, a preheating guide pipe 3 and a tipping control system 11 are arranged in the high-vacuum smelting chamber 2, the preheating guide pipe 3 is positioned at one side of the medium-frequency induction smelting furnace 1, the preheating guide pipe 3 is vertically arranged, and the lower end port of the preheating guide pipe corresponds to the upper end port of a flow distribution nozzle 51 at the top in the forming chamber 6; the intermediate frequency induction smelting furnace 1 is installed on the tilting control system 11, and the intermediate frequency induction smelting furnace 1 rotates around the tilting control system 11 through a rotating shaft, so that the upper opening of the intermediate frequency induction smelting furnace 1 corresponds to the upper opening of the preheating guide pipe 3.
The flow distribution nozzle and infrared camera monitoring device 5 comprises a flow distribution nozzle 51 and an infrared monitoring camera 52, a dam is arranged in the flow distribution nozzle 51 for steady flow, the infrared monitoring camera 52 is arranged on one wide side face of the flow distribution nozzle 51, and the purpose of flow distribution control is achieved by feeding back to the tipping control system 11 through the infrared monitoring camera 52. When the amorphous master alloy melt is obtained by smelting in the medium-frequency induction smelting furnace 1, the amorphous master alloy melt is poured into the preheating guide pipe 3, the preheating guide pipe 3 moves downwards to penetrate through the bottom opening of the medium-frequency induction smelting furnace 1 and the gate valve 4, and the amorphous master alloy melt enters the flow distribution nozzle 51 through the preheating guide pipe 3.
The lower port of the distribution nozzle 51 corresponds to the roll gap between the two casting rolls 8, the outer sides of the two casting rolls 8 are respectively provided with the supporting rolls 7, alloy melt in the preheating guide pipe 3 is uniformly distributed to the roll gap between the two casting rolls 8 through the distribution nozzle 51, the alloy melt continuously passes through the cast gas cooling system 9 below the casting rolls 8 to form a casting strip, and the casting strip is coiled through the coiling device 10.
In the specific implementation process, the method for continuously and efficiently preparing the wide amorphous ribbon at the high cooling speed comprises the following steps: (1) smelting amorphous alloy according to set components, wherein the components comprise zirconium base, copper base, iron base, nickel base and the like, and the amorphous metal with the ultimate cooling rate of 500-75000 ℃/s is used for designing a method for continuously forming a thin strip of the amorphous alloy, so that a base material is provided for the subsequent processing procedures; (2) forming a wide casting belt with the thickness of 80-1500 mu m after a thin belt continuous casting process; (3) smelting, forming and coiling are carried out under the condition of inert atmosphere.
The invention will be further described with reference to the accompanying drawings and specific embodiments.
Example one
Alloy components: (Zr)53.5Hf1.5Cu30Al10Ni5)99.9O0.1(atomic percent at.%, the same below);
a flow distribution mode: deeply entering a roller seam for distributing;
the preparation process comprises the following steps:
a. 20kg of raw materials are mixed according to atomic percentage, put into a medium-frequency induction smelting furnace, and a smelting cavity is vacuumized to 6 × 10-2Pa, heating the alloy raw materials until the alloy raw materials are completely melted, and continuously smelting at 1500 ℃ for 10 min.
b. In the smelting process, the preparation work of the forming cavity is completed, and the method comprises the following steps: 1) all valve bodies on the cavity of the forming cavity are closed, the vacuum pumping is carried out until the pressure is 0.5Pa, then argon is filled, the volume purity is more than 99.99 percent, and the micro-positive pressure of 0.12MPa is kept; 2) preheating a flow distribution nozzle, wherein the flow distribution nozzle adopts slit type flow distribution, and is installed into a fixed position and then heated, and the heating temperature is 1150 ℃; 3) the temperature of the cooling circulating water of the casting roller is 5 ℃, and the total water flow is 80m3H; 4) preparing a gas cooling system after casting, wherein the argon pressure is 0.7MPa, and the gas temperature is controlled to be 5 ℃; 5) the nip opening width was set to 0.55 mm.
c. And (3) closing the vacuum pump, filling high-purity argon with the volume purity of 99.999 percent into the intermediate frequency induction smelting furnace to the micro-positive pressure of 0.12MPa, opening the gate valve, putting down the preheating flow guide pipe, and uniformly distributing and flowing the alloy melt into the roll gap of the casting roll through the preheating flow guide pipe (the preheating temperature of the flow guide pipe is 1150 ℃) and the flow distribution nozzle.
The parameters are shown in table 1 below.
TABLE 1 Experimental Main parameters
d. The flow distribution nozzle used in the experiment is made of transparent quartz. In the experimental process, the melt liquid level height inside the distributing nozzle is monitored and controlled to be 60mm through the infrared monitoring camera and the crucible tilting speed. Uniformly distributing and flowing the alloy melt into a roll gap of a casting roll through a flow distribution nozzle by depending on the pressure of the alloy liquid, controlling the liquid level height of the alloy melt in the roll gap to be 5-10 mm, and cooling the alloy for cast-rolling forming without a side sealing plate, wherein the cooling speed of the alloy melt is 10000 ℃/s; in the casting and rolling process, the alloy is rapidly cooled through heat transfer of a casting roller, the temperature of the thin alloy strip out of the roller is regulated and controlled by controlling the casting and rolling speed, the casting and rolling force and the roll gap, and the temperature of the alloy out of the roller is controlled to be about 400 ℃; and the formed amorphous thin strip is led out of the casting and rolling device through the guide roll and enters a gas cooling system after casting to be further cooled to be below 100 ℃, and the cooling speed of the gas cooling system is 100 ℃/s.
The experiment yielded amorphous ribbon of 0.55mm thickness as shown in figure 2. The microstructure photograph and XRD curve are shown in FIG. 3. As can be seen from fig. 2-3, the cast strip matrix is amorphous with only few crystalline impurities.
Example two
Alloy components: (Zr)53.5Hf1.5Cu30Al10Ni5)99.9O0.1；
A flow distribution mode: deeply entering a roller seam for distributing;
the preparation process comprises the following steps:
a. 50kg of raw materials are prepared according to atomic percentage, put into a medium-frequency induction smelting furnace, and a smelting cavity is vacuumized to 6 × 10-2Pa, heating the alloy raw materials until the alloy raw materials are completely melted, and continuously smelting at 1400 ℃ for 20 min.
b. In the smelting process, the preparation work of the forming cavity is completed, and the method comprises the following steps: 1) all valve bodies on the cavity of the forming cavity are closed, the vacuum pumping is carried out until the pressure is 0.5Pa, then argon is filled, the volume purity is more than 99.99 percent, and the micro-positive pressure of 0.11MPa is kept; 2) preheating a flow distribution nozzle, wherein the flow distribution nozzle adopts slit type flow distribution, and is installed into a fixed position and then heated, and the heating temperature is 1000 ℃; 3) the temperature of the cooling circulating water of the casting roller is 5 ℃, and the total water flow is 80m3H; 4) preparing a gas cooling system after casting, wherein the argon pressure is 0.7MPa, and the gas temperature is controlled to be 5 ℃; 5) the roll gap opening width was set to 0.5 mm.
c. And (3) closing the vacuum pump, filling high-purity argon with the volume purity of 99.999 percent into the intermediate frequency induction smelting furnace to the micro-positive pressure of 0.11MPa, opening the gate valve, putting down the preheating flow guide pipe, and uniformly distributing and flowing the alloy melt into the roll gap of the casting roll through the preheating flow guide pipe (the preheating temperature of the flow guide pipe is 1150 ℃) and the flow distribution nozzle.
The parameters are shown in table 2 below.
TABLE 2 Experimental Main parameters
d. The flow distribution nozzle used in the experiment is made of transparent quartz. In the experimental process, the melt liquid level height inside the distributing nozzle is monitored and controlled to be 60mm through the infrared monitoring camera and the crucible tilting speed. Uniformly distributing and flowing the alloy melt into a roll gap of a casting roll through a flow distribution nozzle by depending on the pressure of the alloy liquid, controlling the liquid level height of the alloy melt in the roll gap to be 5-10 mm, and cooling the alloy for cast-rolling forming without a side sealing plate, wherein the cooling speed of the alloy melt is 6000 ℃/s; in the casting and rolling process, the alloy is rapidly cooled through heat transfer of a casting roller, the temperature of the thin alloy strip out of the roller is regulated and controlled by controlling the casting and rolling speed, the casting and rolling force and the roll gap, and the temperature of the alloy out of the roller is controlled to be about 400 ℃; and the formed amorphous thin strip is led out of the casting and rolling device through the guide roll and enters a gas cooling system after casting to be further cooled to be below 100 ℃, and the cooling speed of the gas cooling system is 80 ℃/s.
The test results in amorphous strips of 0.5mm thickness. The microstructure photograph and XRD curve are shown in FIG. 4. As can be seen from FIG. 4, the cast strip has a completely amorphous structure.
EXAMPLE III
Alloy components: (Cu)60Zr20Hf10Ti10)99.9O0.1；
A flow distribution mode: deeply entering a roller seam for distributing;
the preparation process comprises the following steps:
a. mixing 30kg of raw materials according to atomic percentage, putting the raw materials into a medium-frequency induction smelting furnace, and vacuumizing a smelting cavity to 7 × 10-2Pa, heating the alloy raw materials until the alloy raw materials are completely melted, and continuously smelting at 1500 ℃ for 10 min.
b. In the smelting process, the preparation work of the forming cavity is completed, and the method comprises the following steps: 1) all valve bodies on the cavity of the forming cavity are closed, the vacuum pumping is carried out until the pressure is 0.5Pa, then argon is filled, the volume purity is more than 99.99 percent, and the micro-positive pressure of 0.11MPa is kept; 2) preheating a flow distribution nozzle, wherein the flow distribution nozzle adopts slit type flow distribution, and is installed into a fixed position and then heated, and the heating temperature is 1150 ℃; 3) the temperature of the cooling circulating water of the casting roller is 5 ℃, and the total water flow is 80m3H; 4) preparing a gas cooling system after casting, wherein the argon pressure is 0.7MPa, and the gas temperature is controlled to be 5 ℃; 5) the roll gap opening width was set to 0.5 mm.
c. And (3) closing the vacuum pump, filling high-purity argon with the volume purity of 99.999 percent into the intermediate frequency induction smelting furnace to the micro-positive pressure of 0.11MPa, opening the gate valve, putting down the preheating flow guide pipe, and uniformly distributing and flowing the alloy melt into the roll gap of the casting roll through the preheating flow guide pipe (the preheating temperature of the flow guide pipe is 1150 ℃) and the flow distribution nozzle.
The parameters are shown in table 3 below.
TABLE 3 Experimental Main parameters
d. The flow distribution nozzle used in the experiment is made of transparent quartz. In the experimental process, the melt liquid level height inside the distributing nozzle is monitored and controlled to be 60mm through the infrared monitoring camera and the crucible tilting speed. Uniformly distributing and flowing the alloy melt into a roll gap of a casting roll through a flow distribution nozzle by depending on the pressure of the alloy liquid, controlling the liquid level height of the alloy melt in the roll gap to be 5-10 mm, and cooling the alloy for cast-rolling forming without a side sealing plate, wherein the cooling speed of the alloy melt is 8000 ℃/s; in the casting and rolling process, the alloy is rapidly cooled through heat transfer of a casting roller, the temperature of the thin alloy strip out of the roller is regulated and controlled by controlling the casting and rolling speed, the casting and rolling force and the roll gap, and the temperature of the alloy out of the roller is controlled to be about 400 ℃; and the formed amorphous thin strip is led out of the casting and rolling device through the guide roll and enters a gas cooling system after casting to be further cooled to be below 100 ℃, and the cooling speed of the gas cooling system is 60 ℃/s.
The test yielded amorphous ribbon of 0.5mm thickness.
Example four
Alloy components: fe69C5Si3B5P8Cr3Al2Mo5；
A flow distribution mode: deeply entering a roller seam for distributing;
the preparation process comprises the following steps:
a. 20kg of raw materials are prepared according to atomic percentage, put into a medium-frequency induction smelting furnace, and a smelting cavity is vacuumized to 8 × 10-2Pa, heating the alloy raw materials until the alloy raw materials are completely melted, and continuously smelting at 1500 ℃ for 10 min.
b. In the smelting process, the preparation work of the forming cavity is completed, and the method comprises the following steps: 1) all valve bodies on the cavity of the forming cavity are closed, the vacuum pumping is carried out until the pressure is 0.5Pa, then argon is filled, the volume purity is more than 99.99 percent, and the micro-positive pressure of 0.11MPa is kept; 2) preheating a flow distribution nozzle, wherein the flow distribution nozzle adopts slit type flow distribution, and is installed into a fixed position and then heated, and the heating temperature is 1200 ℃; 3) the temperature of the cooling circulating water of the casting roller is 5 ℃, and the total water flow is 80m3H; 4) preparing a gas cooling system after casting, wherein the argon pressure is 0.7MPa, and the gas temperature is controlled to be 5 ℃; 5) the roll gap opening width was set to 0.5 mm.
c. And (3) closing the vacuum pump, filling high-purity argon with the volume purity of 99.999 percent into the intermediate frequency induction smelting furnace to the micro-positive pressure of 0.11MPa, opening the gate valve, putting down the preheating flow guide pipe, and uniformly distributing and flowing the alloy melt into the roll gap of the casting roll through the preheating flow guide pipe (the preheating temperature of the flow guide pipe is 1150 ℃) and the flow distribution nozzle.
The parameters are shown in table 4 below.
TABLE 4 Experimental Main parameters
d. The flow distribution nozzle used in the experiment is made of transparent quartz. In the experimental process, the melt liquid level height inside the distributing nozzle is monitored and controlled to be 60mm through the infrared monitoring camera and the crucible tilting speed. Uniformly distributing and flowing the alloy melt into a roll gap of a casting roll through a flow distribution nozzle by depending on the pressure of the alloy liquid, controlling the liquid level height of the alloy melt in the roll gap to be 5-10 mm, and cooling the alloy for cast-rolling forming without a side sealing plate, wherein the cooling speed of the alloy melt is 5000 ℃/s; in the casting and rolling process, the alloy is rapidly cooled through heat transfer of a casting roller, the temperature of the thin alloy strip out of the roller is regulated and controlled by controlling the casting and rolling speed, the casting and rolling force and the roll gap, and the temperature of the alloy out of the roller is controlled to be about 520 ℃; and the formed amorphous thin strip is led out of the casting and rolling device through the guide roll and enters a gas cooling system after casting to be further cooled to be below 100 ℃, and the cooling speed of the gas cooling system is 50 ℃/s.
The test yielded amorphous ribbon of 0.25 mm thickness.
EXAMPLE five
Alloy components: ni40Cu5Ti16Zr28Hf1Al10；
A flow distribution mode: deeply entering a roller seam for distributing;
the preparation process comprises the following steps:
a. 20kg of raw materials are mixed according to atomic percentage, put into a medium-frequency induction smelting furnace, and a smelting cavity is vacuumized to 6 × 10-2Pa, heating the alloy raw materials until the alloy raw materials are completely melted, and continuously smelting at 1500 ℃ for 10 min.
b. In the smelting process, the preparation work of the forming cavity is completed, and the method comprises the following steps: 1) all valve bodies on the cavity of the forming cavity are closed, the vacuum pumping is carried out until the pressure is 0.5Pa, then argon is filled, the volume purity is more than 99.99 percent, and the micro-positive pressure of 0.11MPa is kept; 2) preheating a flow distribution nozzle, wherein the flow distribution nozzle adopts slit type flow distribution, and is installed into a fixed position and then heated, and the heating temperature is 1200 ℃; 3) the temperature of the cooling circulating water of the casting roller is 5 ℃, and the total water flow is 80m3H; 4) preparing a gas cooling system after casting, wherein the argon pressure is 0.7MPa, and the gas temperature is controlled to be 5 ℃; 5) the roll gap opening width was set to 0.5 mm.
c. And (3) closing the vacuum pump, filling high-purity argon with the volume purity of 99.999 percent into the intermediate frequency induction smelting furnace to the micro-positive pressure of 0.11MPa, opening the gate valve, putting down the preheating flow guide pipe, and uniformly distributing and flowing the alloy melt into the roll gap of the casting roll through the preheating flow guide pipe (the preheating temperature of the flow guide pipe is 1150 ℃) and the flow distribution nozzle.
The parameters are shown in table 5 below.
TABLE 5 Experimental Main parameters
d. The flow distribution nozzle used in the experiment is made of transparent quartz. In the experimental process, the melt liquid level height inside the distributing nozzle is monitored and controlled to be 60mm through the infrared monitoring camera and the crucible tilting speed. Uniformly distributing and flowing the alloy melt into a roll gap of a casting roll through a flow distribution nozzle by depending on the pressure of the alloy liquid, controlling the liquid level height of the alloy melt in the roll gap to be 5-10 mm, and cooling the alloy melt to be cast and rolled to form without a side sealing plate, wherein the cooling speed of the alloy melt is 7000 ℃/s; in the casting and rolling process, the alloy is rapidly cooled through heat transfer of a casting roller, the temperature of the thin alloy strip out of the roller is regulated and controlled by controlling the casting and rolling speed, the casting and rolling force and the roll gap, and the temperature of the alloy out of the roller is controlled to be about 520 ℃; and the formed amorphous thin strip is led out of the casting and rolling device through the guide roll and enters a gas cooling system after casting to be further cooled to be below 100 ℃, and the cooling speed of the gas cooling system is 80 ℃/s.
The test yielded amorphous ribbon of 0.25 mm thickness.
The above-mentioned embodiments are only for illustrating the technical features of the present invention, and are not to be construed as limiting the scope of the present invention, which is intended to be detailed description of the present invention. It is within the scope of the present invention to cover all equivalent alternatives falling within the spirit of the invention without departing from the technical spirit of the invention.
Claims (10)
1. A method for continuously and efficiently preparing a wide amorphous thin strip with the thickness of 80-1500 mu m at a high cooling speed is characterized by comprising the following steps of:
(1) feeding the amorphous master alloy into a crucible, cleaning a preheating guide pipe and a position control device thereof, wherein the preheating guide pipe is internally provided with a quartz lining and is attached with a heating system, the heating temperature is 100-200 ℃ above the solidification temperature of the amorphous master alloy, and cooling water is introduced to the outside of the preheating guide pipe for protection;
(2) the amorphous master alloy is smelted according to set components and comprises the following components: melting metals in a zirconium-based, copper-based, iron-based or nickel-based amorphous alloy component system, uniformly mixing for 5-30 minutes, and controlling the temperature;
(3) controlling the superheat degree of an alloy melt to be 50-300 ℃, protecting by adopting high-purity argon with volume purity of more than 99.999% in the temperature control process, and enabling argon in a smelting cavity to be micro-positive pressure, namely, the pressure is not lower than 0.11 MPa;
(4) in the smelting process, the preparation work of the forming cavity is completed, and the method comprises the following steps: a) all valve bodies on the cavity of the forming cavity are closed, argon is filled after vacuum pumping, the volume purity is more than 99.99 percent, and the micro positive pressure not lower than 0.11MPa is kept; b) preheating a flow distribution nozzle, wherein the flow distribution nozzle adopts slit type flow distribution, and is installed and heated after entering a fixed position, and the heating temperature is 100-200 ℃ above the solidification temperature of a target alloy; c) the temperature of the cooling circulating water of the casting roller is 3-5 ℃, and the total water flow is 70-90 m3H; d) preparing a gas cooling system after casting, wherein the argon pressure is 0.6-0.8 MPa, and the gas temperature is controlled at 4-6 ℃;
(5) alloy smelting, preheating of a preheating guide pipe and a flow distribution nozzle, and argon filling of a forming cavity, preparing an amorphous thin strip by adopting a vertical thin strip casting and rolling process, and performing a thin strip continuous casting process: opening a gate valve of the smelting cavity, descending the preheating guide pipe to be in butt joint with the flow distribution nozzle, and pouring alloy into the preheating guide pipe by the medium-frequency induction smelting furnace; the flow distribution nozzle is made of transparent quartz, the height of a melt inside the flow distribution nozzle is controlled to be 40-60 mm through the monitoring of an infrared monitoring camera and the tilting speed of a medium-frequency induction smelting furnace, an alloy melt is uniformly distributed and flowed into a roll gap of a casting roll vertically through the flow distribution nozzle by liquid level, the height of the alloy melt at the roll gap is controlled to be 2-10 mm, the cooling speed of the alloy melt is 500-75000 ℃/s, and the alloy is cooled, cast and rolled to form; guiding the formed amorphous thin belt out through a guide roller, further cooling the amorphous thin belt in a cast gas cooling system, and adopting low-temperature argon for blowing and cooling, wherein the gas cooling speed is 50-800 ℃/s;
(6) after the gas is cooled, the thickness range of the amorphous thin strip reaches 80-1500 mu m, and the width range of the amorphous thin strip is 110-550 mm; and coiling the casting strip with the thickness of 80-800 mu m, and directly collecting the casting strip with the thickness of more than 800 mu m in a thin strip form without coiling.
2. The method for continuously and efficiently preparing the wide amorphous thin strip with the thickness of 80-1500 microns at the high cooling speed according to the claim 1, characterized in that in the casting process, an alloy melt is rapidly cooled through heat transfer of a casting roller, the temperature of the alloy thin strip outlet roller is regulated and controlled by controlling the casting speed, the casting force and the roll gap, and the temperature of the alloy outlet roller is controlled to be lower than the crystallization temperature Tx of the alloy; the casting and rolling speed is 0.20-1.8 m/s, the casting and rolling force is controlled to be 2-15 kN per 1cm width of casting strip, the width of a roll gap opening of a casting roll is set to be 80-1500 mu m, and no side sealing plate is arranged.
3. The method for continuously and efficiently preparing the wide amorphous thin strip with the thickness of 80-1500 μm at the high cooling speed according to claim 1, characterized in that the solidification cooling speed is controlled to reach 500-75000 ℃/s through the opening size at the lower end of the flow distribution nozzle, the opening width of a roll gap of a casting roll, the casting-rolling speed, the casting-rolling process parameters of copper casting rolls, steel casting rolls and the cooling water amount of the casting rolls.
4. The method for continuously and efficiently preparing the wide amorphous ribbon with the thickness of 80-1500 mu m at the high cooling speed according to claim 1, which is characterized in that yttrium element with the mass percent of 0.0045-0.020 is added into a zirconium-based, copper-based, iron-based or nickel-based amorphous alloy for removing O, N pollution brought by the environment.
5. The method for continuously preparing the wide amorphous thin strip with the thickness of 80-1500 μm at high cooling speed and high efficiency according to claim 1, is characterized in that a quartz slit type flow distribution nozzle is adopted for flow distribution, and the opening width of the slit is designed according to different product thicknesses; the flow distribution nozzle is preheated on line, the preheating temperature is 100-200 ℃ above the alloy solidification temperature, the opening end part of the lower end of the flow distribution nozzle conducts heat through a tungsten alloy sheet, the temperature of the end part of the flow distribution nozzle reaches the temperature near the alloy solidification temperature, and a dam punch is arranged inside the flow distribution nozzle to stabilize the flow; the lining of the preheating guide pipe is made of quartz glass which can be quickly replaced, the preheating temperature is 100-200 ℃ above the alloy solidification temperature, and cooling water is introduced to the outside of the preheating guide pipe for protection.
6. The method for continuously preparing the wide amorphous thin strip with the thickness of 80-1500 mu m at high cooling speed and high efficiency according to claim 1, characterized in that an infrared monitoring camera is arranged on the width side surface of a flow distribution nozzle and is fed back to a tipping control system to achieve the purpose of flow distribution control; wherein, the height control range of the opening at the lower end of the flow distribution nozzle from the Kiss line of the casting roll is 10-50 mm, and the liquid level height in the flow distribution nozzle is 40-60 mm.
7. The method for continuously and efficiently preparing the wide amorphous thin strip with the thickness of 80-1500 microns at the large cooling speed according to claim 1, wherein two horizontally opposite rollers are used as casting rollers, supporting rollers are additionally arranged on two sides of the two rollers, the diameter of the casting rollers is 280-420 mm, and the diameter of each group of supporting rollers is 100mm larger than that of the casting rollers.
8. the method for continuously and efficiently preparing the wide amorphous ribbon with the thickness of 80-1500 mu m at the high cooling speed according to claim 1, which is characterized in that a smelting cavity and a forming cavity adopt a graded vacuum design, wherein the working vacuum degree of the smelting cavity reaches 1 × 10- 2The vacuum degree of the forming cavity reaches below 1 Pa; and in the pouring state, the environment is in an argon protection state, the smelting cavity and the forming cavity are separated by a gate valve, and the gate valve is opened after the argon is filled before the casting and rolling are started.
9. The method for continuously preparing the wide amorphous ribbon with the thickness of 80-1500 mu m at high cooling speed and high efficiency according to claim 1, characterized in that a medium frequency induction smelting furnace and a high-purity graphite crucible are adopted for amorphous alloy smelting, the heating temperature is not more than 400 ℃ above the melting temperature of metal, and oxidation and burning loss of metal elements are prevented.
10. The method for continuously and efficiently preparing the wide amorphous thin strip with the thickness of 80-1500 mu m at the high cooling speed according to claim 1, characterized in that the scrap of cast strip trimming is added into the amorphous master alloy incoming material by not more than 20 wt%.
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| PCT/CN2019/081935 WO2020206611A1 (en) | 2019-04-08 | 2019-04-09 | METHOD FOR CONTINUOUS AND HIGH-EFFICIENT PREPARATION OF WIDE AMORPHOUS THIN STRIP HAVING THICKNESS OF 80-1,500 μM AT HIGH COOLING SPEED |
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| CN115283629B (en) * | 2022-08-02 | 2024-04-12 | 太原科技大学 | Method for preparing nickel-based superalloy by using double-roller casting and rolling process |
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| US4380262A (en) * | 1980-10-27 | 1983-04-19 | Gte Laboratories Incorporated | Apparatus for double roller chill casting of continuous metal foil |
| JPS5858962A (en) * | 1981-09-30 | 1983-04-07 | Sanyo Electric Co Ltd | Producing device for ribbon-like amorphous alloy |
| JPS59137162A (en) * | 1983-01-26 | 1984-08-07 | Ishikawajima Harima Heavy Ind Co Ltd | Device for producing quenched strip |
| JPS6068139A (en) * | 1983-09-21 | 1985-04-18 | Kawasaki Steel Corp | Production of quickly cooled light-gauge strip |
| BG60092B2 (en) * | 1990-04-13 | 1993-10-29 | Markov | Method and device for the production of microcrystalline and amorphous metal strips from smelt |
| JPH06297109A (en) * | 1993-04-15 | 1994-10-25 | Nippon Steel Corp | Production of cr-ni series stainless steel cast strip excellent in surface characteristic |
| US6416879B1 (en) * | 2000-11-27 | 2002-07-09 | Nippon Steel Corporation | Fe-based amorphous alloy thin strip and core produced using the same |
| CN1327990C (en) * | 2002-09-27 | 2007-07-25 | 学校法人浦项工科大学校 | Method and apparatus for producing amorphous alloy sheet, and amorphous alloy sheet produced using the same |
| CN1486800A (en) * | 2003-05-09 | 2004-04-07 | 燕山大学 | Continuous casting and rolling technology of massive non-crystal alloy |
| CN201669392U (en) * | 2010-05-18 | 2010-12-15 | 南昌市南方连铸工程有限责任公司 | Semi-solid casting-rolling double-roll type thin strip bloom conticaster |
| EP2759614B1 (en) * | 2013-01-25 | 2019-01-02 | ThyssenKrupp Steel Europe AG | Method for generating a flat steel product with an amorphous, semi-amorphous or fine crystalline structure and flat steel product with such structures |
| CN103752785B (en) * | 2014-01-21 | 2015-09-02 | 罗冉 | A kind of rapid solidification metal strip production device and method thereof |
| CN205110716U (en) * | 2015-11-25 | 2016-03-30 | 滕州高科康纳合金材料有限公司 | Banding structure in metallic glass area |
| CN206083799U (en) * | 2016-11-01 | 2017-04-12 | 东莞市逸昊金属材料科技有限公司 | Novel amorphous foundry alloy spindle continuous casting system |
| CN107245672B (en) * | 2017-06-15 | 2018-10-02 | 天津中晟泰新能源科技有限公司 | A kind of iron-based amorphous nanometer crystalline thin strip magnet and its methods for making and using same |
| CN207723444U (en) * | 2018-01-10 | 2018-08-14 | 江苏知行科技有限公司 | A kind of amorphous band cooling device |
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