CN114433803B - Screening method for cooling rate of amorphous alloy strip - Google Patents
Screening method for cooling rate of amorphous alloy strip Download PDFInfo
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- CN114433803B CN114433803B CN202210125672.XA CN202210125672A CN114433803B CN 114433803 B CN114433803 B CN 114433803B CN 202210125672 A CN202210125672 A CN 202210125672A CN 114433803 B CN114433803 B CN 114433803B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/16—Controlling or regulating processes or operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0637—Accessories therefor
- B22D11/068—Accessories therefor for cooling the cast product during its passage through the mould surfaces
- B22D11/0682—Accessories therefor for cooling the cast product during its passage through the mould surfaces by cooling the casting wheel
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Abstract
The invention relates to a screening method for cooling speed of an amorphous alloy strip, and belongs to the technical field of amorphous alloy preparation. The screening method comprises the following steps of 1) spraying a molten master alloy onto a rotary cooling roller through a nozzle by adopting a single-roller melt rapid quenching method to cool and solidify to form an alloy strip, continuously changing the thickness of the alloy strip by adjusting the surface linear speed of the rotary cooling roller from v 1 to v 2 or from v 2 to v 1 in the process of spraying the molten master alloy, wherein the alloy formed by cooling and solidifying at the linear speed v 1 is in a completely amorphous structure, the alloy formed by cooling and solidifying at the linear speed v 2 is in a crystalline structure, and 2) substituting the thickness value at the position point in an amorphization region or the position point on the boundary line between the crystallization region and the amorphization region on the alloy strip formed during speed change into a linear speed relation of the amorphous alloy strip thickness and the cooling roller surface to obtain the cooling speed. The screening method can complete high-flux screening of the cooling speed through one-time preparation of the alloy strip.
Description
Technical Field
The invention relates to a screening method for cooling speed of an amorphous alloy strip, and belongs to the technical field of amorphous alloy preparation.
Background
Amorphous alloy is a special alloy in which the alloy melt is solidified into a solid state directly under the condition of rapid cooling without the growth of crystals. The atoms in the amorphous alloy retain long-range disordered and short-range ordered arrangements of the distributed states in the liquid state, which makes the amorphous alloy have different physical and chemical performance characteristics from the traditional metal materials. Amorphous alloys have high strength, high plasticity and impact toughness, and higher corrosion resistance than crystalline alloys, and have high magnetic permeability and low loss, and have been widely used in mold materials, corrosion-resistant materials, hydrogen storage materials, sports equipment materials, soft magnetic materials, and the like.
The single-roller melt rapid quenching method is the most important and widely applied rapid solidification technology in the technology for preparing amorphous alloy materials, and is a technological method for spraying the melt on a rotating cooling roller to rapidly quench the melt into amorphous strips. When the melt flows onto the rapidly rotating roll surface, a molten pool is formed on the roll surface, and the thin melt layer contacted with the roll surface is rapidly cooled and continuously pumped out of the molten pool along with the movement of the roll surface to form the amorphous strip. The faster cooling rate can effectively improve the surface quality of the amorphous strip, but the too high rotational speed can cause bubbles to be involved in the melt to affect the stability of the molten pool and thus the surface quality of the strip. However, the cooling rate of the melt on the cooling roll is affected by the thickness of the thin strip, in addition to the material thermal conductivity, density, heat capacity, etc. of the cooling roll. Therefore, when the amorphous alloy strip is prepared by adopting the determined single-roller melt rapid quenching equipment, the amorphous alloy strip with higher quality can be prepared by selecting proper nozzle size and cooling roller rotation speed (namely the cooling speed of the alloy strip). However, the thickness of the alloy strip depends on the correlation between the quantity of the ejected melt (nozzle size and ejection pressure) and the rotation speed of the cooling roller, so far, the screening of the cooling speed of the amorphous alloy and the determination of the critical cooling speed (Rc) in the single-roller melt rapid quenching method are mainly trial-and-error methods, and are time-consuming, laborious and blind exploration processes.
Disclosure of Invention
The invention aims to provide a screening method for the cooling speed of an amorphous alloy strip, which can realize high-flux screening for the cooling speed of the amorphous alloy strip through one-time preparation of the alloy strip.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the method for screening the cooling speed of the amorphous alloy strip comprises the following steps:
1) In the process of spraying the molten master alloy onto the rotary cooling roller, the thickness of the alloy strip is continuously changed by adjusting the surface linear speed of the rotary cooling roller from v 1 to v 2 or from v 2 to v 1, the alloy formed by cooling and solidifying at the linear speed v 1 is in a completely amorphous structure, and the alloy formed by cooling and solidifying at the linear speed v 2 is in a crystalline structure;
2) Substituting the thickness value of the amorphous alloy strip at the position point in the amorphous area or the position point on the boundary line of the crystallization area and the amorphous area in the alloy strip formed in the speed reducing or increasing process into the relation of the amorphous alloy strip thickness and the cooling roller surface linear speed to obtain the alloy strip cooling speed at the corresponding position point.
The screening method of the amorphous alloy strip cooling speed can realize high-throughput screening of the amorphous alloy strip cooling speed through one-time preparation of the compact Jin Daicai, greatly shorten the testing period of the amorphous alloy, effectively reduce the cost of manpower and material resources for developing amorphous alloy components, accurately process parameters for preparing the amorphous alloy, reduce the preparation cost and promote engineering application, and in addition, the critical cooling speed (Rc) required for preparing the amorphous alloy can be rapidly determined through the thickness values of the position points on the boundary between the crystallization area and the amorphous area, and the relation between the cooling speed and the amorphization degree can be rapidly determined through the thickness values of other position points in the crystallization area.
It is understood that the amorphized region in the present invention refers to a region where the alloy melt is rapidly cooled to obtain complete amorphization, and the crystallized region refers to a region where the cooling rate of the alloy melt is lower than the critical cooling rate for amorphous formation, resulting in crystallization.
In the case that the conditions other than the slit size and the cooling roller rotation speed are kept unchanged in the single-roller melt rapid quenching method, the thickness of the amorphous alloy strip is related to the slit size and the cooling roller rotation speed. In order to realize low consumption analysis and efficient screening of the critical cooling speed of the amorphous alloy strip through one-time preparation of the alloy strip, the preparation parameters of the amorphous alloy strip are precisely controlled, the energy consumption is reduced, and furthermore, the slit width of the nozzle continuously increases or decreases in the direction parallel to the rotating shaft of the rotary cooling roller. The slit is in an axisymmetric pattern, and the symmetry axis is parallel to the rotating shaft of the rotary cooling roller.
Further, the slit of the nozzle is isosceles trapezoid. The arrangement of the slit in the isosceles trapezoid can further screen the influence of the slit spacing of the nozzle on the forming capacity of the amorphous strip and the surface quality of the strip, and high-throughput screening of multiple parameters in the amorphous alloy preparation process is realized. The slit width of the isosceles trapezoid slit is not uniform in different positions in the trapezoid height direction, so that the corresponding thickness of the strip is also not uniform. For example, the widest position of the isosceles trapezoid slit is arranged on the left side, the narrowest position of the isosceles trapezoid slit is arranged on the right side, the left side of the prepared strip is prepared at the widest position of the slit, the right side of the prepared strip is prepared at the narrowest position of the slit, and the width of the slit corresponds to the thickness of the strip. The position of the selected position point on the alloy strip in the width direction of the alloy strip can be obtained according to the position of the selected position point on the alloy strip in the length direction of the slit, so that the slit gap size (namely the slit width) corresponding to the selected position point is obtained. And calculating the cooling speed of the alloy strip at the corresponding position point according to the relation between the thickness of the amorphous alloy strip and the linear speed of the surface of the cooling roller based on the thickness of the alloy strip at the selected position point and the corresponding slit gap.
Since the cooling rate is mainly determined by the material of the cooling roll (heat conductivity, density, heat capacity, etc.), the amount of the ejected melt (nozzle size and ejection pressure), and the thickness of the alloy strip, the cooling rate of the alloy melt after the material of the cooling roll and the ejection pressure are determined is determined by the amount of the ejected melt (nozzle size) and the thickness of the alloy strip. In the prior art, the relation formula showing the relation between the thickness of the amorphous alloy strip and the linear speed of the surface of the cooling roller is more, and the relation formula can be used for calculating the cooling speed of the amorphous alloy according to the thickness. Further, spraying argon gas to the molten master alloy, and spraying the molten master alloy onto a rotary cooling roller through a nozzle by utilizing the pressure difference between the pressure of the argon gas and the pressure outside a collision nozzle, wherein the relation formula of the thickness of the amorphous alloy strip and the linear speed of the surface of the cooling roller is as follows:
Wherein d is the thickness of the amorphous alloy strip, m, G is the distance between roller nozzles, m, b is the gap between nozzle slits, m, v is the linear speed of the surface of the rotary cooling roller, m/s, P is the pressure difference between the pressure of spraying argon and the pressure outside the nozzle, pa, and ρ is the density of the master alloy melt, kg/m 3. The method for calculating the cooling speed according to the thickness of the alloy strip by adopting the relational expression has the advantages that parameters are precisely controllable parameters and intrinsic parameters of materials in the amorphous strip preparation process, and the linear speed of a copper roller can be precisely calculated, so that the preparation of the amorphous strip is guided.
In order to accurately obtain the mathematical model relationship between the strip thickness and the copper roll surface linear velocity, further, the molten master alloy ejection time is consistent with the deceleration or acceleration time of the rotating chill roll.
The screening method of the invention is applicable to a wide range of amorphous alloy systems, and can be widely applied to the screening of the cooling speed of the amorphous alloy system strips such as Ti-based, fe-based, co-based and the like. Further, the amorphous alloy strip is a Ti-based amorphous alloy strip, a Fe-based amorphous alloy strip, a Zr-based amorphous alloy strip or a Co-based amorphous alloy strip.
Further, the linear velocity v 1 was 50m/s, and the linear velocity v 2 was 5m/s. Setting the linear velocities v 1 and v 2 to 50m/s and 5m/s, respectively, can basically satisfy the screening of the cooling rate of most amorphous alloy strips.
Further, during the speed up or down, the surface linear velocity of the rotating cooling roller varies linearly. Controlling the linear change in the surface linear velocity of the rotating chill roll helps to obtain continuous amorphous alloy strip thickness data to accurately determine the copper roll surface linear velocity required for production.
Drawings
FIG. 1 is a schematic diagram of a single roller copper wheel rapid quenching process in examples 1 and 2;
Fig. 2 is a front view of the quartz tube used in example 1 and example 2;
FIG. 3 is a bottom view of the quartz tube of FIG. 2;
FIG. 4 is a schematic view of the alloy thin strip prepared in example 1;
FIG. 5 is an XRD pattern of the iron-based amorphous alloy strip prepared in example 1;
FIG. 6 is an XRD pattern of the titanium-based amorphous alloy strip prepared in example 2;
The device comprises a 1-induction coil, a 2-argon gas flow, a 3-quartz tube, a 4-master alloy melt, a 5-alloy strip, a 6-cooling copper roller, a 7-rotating shaft, an 8-nozzle and a 9-slit.
Detailed Description
In the prior art, when a single-roller melt rapid quenching method is adopted to prepare an amorphous alloy strip, induction smelting rapid quenching equipment is mainly adopted, the induction frit rapid quenching equipment comprises a quartz tube used for placing a master alloy, an induction coil used for heating and melting the master alloy in the quartz tube and a copper roller used for rapidly cooling the molten master alloy sprayed from a nozzle of the quartz tube, and the screening method can also adopt the induction smelting rapid quenching equipment when the alloy strip is prepared.
The technical scheme of the invention is further described below with reference to the specific embodiments.
Example 1
According to the screening method for the cooling speed of the amorphous alloy strip, the amorphous alloy strip is prepared by adopting a single-roller melt rapid quenching method, as shown in fig. 1, the single-roller melt rapid quenching method is carried out in an induction smelting rapid quenching furnace, the induction fusion cake rapid quenching furnace comprises an induction coil 1, a quartz tube 3 and a cooling copper roller 6, the quartz tube 3 is shown in fig. 2-3, a nozzle 8 is arranged at the bottom of the quartz tube 3, an opening slit 9 of the nozzle 8 is in an isosceles trapezoid shape, the nozzle 8 faces the cooling copper roller 6, and the symmetry axis of the slit 9 is parallel to the rotating shaft of the cooling copper roller 6. When alloy strips are prepared by adopting a single-roller melt rapid quenching method, mother alloy is placed into a quartz tube 3, an induction coil 1 is electrified and then heated and melted to obtain a mother alloy melt 4, argon gas flow 2 is sprayed into the quartz tube 3, and the mother alloy melt 4 is sprayed on the rotating water-cooled copper roller 6 to be rapidly cooled and solidified to obtain alloy strips 5.
Specifically, the method for screening the cooling rate of the amorphous alloy strip according to the embodiment comprises the following steps:
1) The Fe 80Si8B12 master alloy which is evenly smelted is crushed into small blocks, the master alloy is clamped and put into a quartz tube 3, a slit 9 on a nozzle 8 of the quartz tube 2 is isosceles trapezoid (the width (height) is 10mm, the narrowest spacing (bottom) is 0.2mm, and the widest spacing (bottom) is 0.8 mm);
2) Placing a quartz tube 3 into an induction coil 1 in a fast melt quenching furnace cavity, wherein the quartz tube 3 is positioned at a height of 1.0mm right above a cooling copper roller 6;
3) Pumping the induction smelting rapid quenching furnace chamber to a vacuum degree of 6.0X10 -3 Pa, and then filling argon with a purity of 99.999% at 0.05MPa into the chamber;
4) And (3) starting a cooling copper roller 6 through which cooling circulating water is introduced into a cavity of the induction smelting rapid quenching furnace, starting an induction heating power supply and setting a current value, and observing that when the color of the master alloy in the quartz tube 3 is changed from dark red to bright white, determining that the master alloy in the quartz tube 3 is completely melted, blowing argon into the quartz tube 3, spraying the completely melted master alloy melt onto the cooling copper roller 6 which is rotated at a high speed and is introduced with the cooling circulating water by utilizing the pressure difference between the inside and outside of the quartz tube 3, starting the surface linear speed of the rotating cooling copper roller 6 to be 50m/s, and simultaneously starting to reduce the speed, wherein the melt spraying time is consistent with the speed of the reducing surface linear speed of the cooling copper roller 6 by electric control (controlling the surface linear speed to be linearly reduced), so as to prepare the alloy thin strip with gradually increased thickness.
5) Substituting the thickness value at a position point in the amorphized region or a position point on the boundary line between the crystallized region and the amorphized region on the selected alloy strip into a relation of amorphous alloy strip thickness and cooling roller surface linear velocity to obtain the cooling roller surface linear velocity at the corresponding position point:
Wherein d is the thickness of the amorphous alloy strip, m, G is the distance between roller nozzles, m, b is the gap between nozzle slits, m, v is the linear speed of the surface of the rotary cooling roller, m/s, P is the pressure difference between the pressure of spraying argon and the pressure outside the nozzle, pa, and ρ is the density of the master alloy melt, kg/m 3.
When selecting a location point within an amorphized region, XRD testing may be performed on the selected location point, which must be located in the amorphized region if a typical amorphization peak (i.e., amorphous diffuse scattering peak) occurs. The method for selecting the position points on the boundary line between the crystallization area and the amorphization area comprises the steps of carrying out XRD test on two ends (in the length direction) of the prepared strip respectively, carrying out XRD test on the midpoint of the selected two positions by utilizing a dichotomy if crystallization peaks appear on XRD curves of one thicker end of the strip and crystallization peaks do not appear on XRD curves of one thinner end of the strip, and continuing to sample in the direction of the amorphous area by utilizing the dichotomy if crystallization peaks appear at the midpoint of the selected interval, and continuing to sample in the direction of the crystallized area by utilizing the dichotomy if crystallization peaks do not appear at the midpoint. And continuously circulating until the boundary positions of the crystallized region and the amorphized region are found.
The thin alloy strip prepared in this example is shown in fig. 4, where Rc is the critical cooling rate of the amorphous alloy strip. In this embodiment, after the selected position on the prepared alloy strip, the copper roller surface linear velocity corresponding to the selected position is calculated according to the slit width, the strip thickness and the amorphous alloy strip thickness-cooling roller surface linear velocity relation corresponding to the selected position.
According to the relation between the thickness of the amorphous alloy strip and the linear velocity of the surface of the cooling roller, the slit width and the linear velocity corresponding to the middle position of the slit in the length direction are selected to perform XRD detection, as shown in figure 5, when the slit width corresponding to the middle position of the slit in the length direction is selected, the alloy corresponding to the position of the strip is in a completely amorphous structure when the linear velocity of the copper roller is 45m/s, and when the linear velocity of the copper roller is 35m/s and 25m/s, crystallization peaks appear on the XRD curve of the alloy corresponding to the position of the strip, so that the high-throughput screening of the cooling velocity of the amorphous alloy strip can be successfully realized by the screening method of the cooling velocity of the amorphous alloy strip.
Example 2
According to the screening method for the cooling speed of the amorphous alloy strip, the amorphous alloy strip is prepared by adopting a single-roller melt rapid quenching method, as shown in fig. 1, the single-roller melt rapid quenching method is carried out in an induction smelting rapid quenching furnace, the induction fusion cake rapid quenching furnace comprises an induction coil 1, a quartz tube 3 and a cooling copper roller 6, the quartz tube 3 is shown in fig. 2-3, a nozzle 8 is arranged at the bottom of the quartz tube 3, an opening slit 9 of the nozzle 8 is in an isosceles trapezoid shape, the nozzle 8 faces the cooling copper roller 6, and the symmetry axis of the slit 9 is parallel to the rotating shaft of the cooling copper roller 6. When alloy strips are prepared by adopting a single-roller melt rapid quenching method, mother alloy is placed into a quartz tube 3, an induction coil 1 is electrified and then heated and melted to obtain a mother alloy melt 4, argon gas flow 2 is sprayed into the quartz tube 3, and the mother alloy melt 4 is sprayed on the rotating water-cooled copper roller 6 to be rapidly cooled and solidified to obtain alloy strips 5.
Specifically, the method for screening the cooling rate of the amorphous alloy strip according to the embodiment comprises the following steps:
1) Crushing the uniformly melted Ti 37.5Zr37.5Cu15Ni10 master alloy into small blocks, clamping the master alloy, putting the small blocks into a quartz tube 3, and arranging a slit 9 on a nozzle 8 of the quartz tube 2 into an isosceles trapezoid (with the width (height) of 10mm, the narrowest spacing (bottom) of 0.2mm and the widest spacing (bottom) of 0.8 mm;
2) Placing a quartz tube 3 into an induction coil 1 in a fast melt quenching furnace cavity, wherein the quartz tube 3 is positioned at a height of 1.0mm right above a cooling copper roller 6;
3) Pumping the induction smelting rapid quenching furnace chamber to a vacuum degree of 6.0X10 -3 Pa, and then filling argon with a purity of 99.999% at 0.05MPa into the chamber;
4) And (3) starting a cooling copper roller 6 through which cooling circulating water is introduced into a cavity of the induction smelting rapid quenching furnace, starting an induction heating power supply and setting a current value, and observing that when the color of the master alloy in the quartz tube 3 is changed from dark red to bright white, determining that the master alloy in the quartz tube 3 is completely melted, blowing argon into the quartz tube 3, spraying the completely melted master alloy melt onto the cooling copper roller 6 which is rotated at a high speed and is introduced with the cooling circulating water by utilizing the pressure difference between the inside and outside of the quartz tube 3, starting the surface linear speed of the rotating cooling copper roller 6 to be 40m/s, and simultaneously starting to reduce the speed, wherein the melt spraying time is consistent with the speed of the reducing surface linear speed of the cooling copper roller 6 by electric control (controlling the surface linear speed to be linearly reduced), so as to prepare the alloy thin strip with gradually increased thickness.
5) Substituting the thickness value at a position point in the amorphized region or a position point on the boundary line between the crystallized region and the amorphized region on the selected alloy strip into a relation of amorphous alloy strip thickness and cooling roller surface linear velocity to obtain the cooling roller surface linear velocity at the corresponding position point:
Wherein d is the thickness of the amorphous alloy strip, m, G is the distance between roller nozzles, m, b is the gap between nozzle slits, m, v is the linear speed of the surface of the rotary cooling roller, m/s, P is the pressure difference between the pressure of spraying argon and the pressure outside the nozzle, pa, and ρ is the density of the master alloy melt, kg/m 3.
When selecting a location point within an amorphized region, XRD testing may be performed on the selected location point, which must be located in the amorphized region if a typical amorphization peak (i.e., amorphous diffuse scattering peak) occurs. The method for selecting the position points on the boundary line between the crystallization area and the amorphization area comprises the steps of carrying out XRD test on two ends (in the length direction) of the prepared strip respectively, carrying out XRD test on the midpoint of the selected two positions by utilizing a dichotomy if crystallization peaks appear on XRD curves of one thicker end of the strip and crystallization peaks do not appear on XRD curves of one thinner end of the strip, and continuing to sample in the direction of the amorphous area by utilizing the dichotomy if crystallization peaks appear at the midpoint of the selected interval, and continuing to sample in the direction of the crystallized area by utilizing the dichotomy if crystallization peaks do not appear at the midpoint. And continuously circulating until the boundary positions of the crystallized region and the amorphized region are found.
The thin alloy strip prepared in this example is shown in fig. 4, where Rc is the critical cooling rate of the amorphous alloy strip. In this embodiment, after the selected position on the prepared alloy strip, the copper roller surface linear velocity corresponding to the selected position is calculated according to the slit width, the strip thickness and the amorphous alloy strip thickness-cooling roller surface linear velocity relation corresponding to the selected position.
According to the relation between the thickness of the amorphous alloy strip and the linear velocity of the surface of the cooling roller, the slit width and the linear velocity corresponding to the middle position of the slit in the length direction are selected to perform XRD detection, as shown in figure 6, when the slit width corresponding to the middle position of the slit in the length direction is selected, the alloy corresponding to the position of the strip is in a completely amorphous structure when the linear velocity of the copper roller is 30m/s, and when the linear velocity of the copper roller is 20m/s and 10m/s, crystallization peaks appear on the XRD curve of the alloy corresponding to the position of the strip, so that the high-throughput screening of the cooling velocity of the amorphous alloy strip can be successfully realized by the screening method of the cooling velocity of the amorphous alloy strip.
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