CN111299553B - Multi-mode excited deep supercooling directional solidification device and method - Google Patents
Multi-mode excited deep supercooling directional solidification device and method Download PDFInfo
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- CN111299553B CN111299553B CN202010280826.3A CN202010280826A CN111299553B CN 111299553 B CN111299553 B CN 111299553B CN 202010280826 A CN202010280826 A CN 202010280826A CN 111299553 B CN111299553 B CN 111299553B
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- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
- B22D27/045—Directionally solidified castings
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- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/04—Removing impurities by adding a treating agent
- C21C7/076—Use of slags or fluxes as treating agents
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- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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Abstract
The invention relates to the technical field of directional solidification, in particular to a multi-mode excited deep supercooling directional solidification device and a method, which comprises a reaction furnace, a smelting device, a feeding device, an exciting device, a drawing rod and a drawing device, wherein the feeding device is used for adding a purifying agent into a crucible in the hot melting process; the excitation device comprises an excitation chamber capable of being filled with liquid metal, a water-cooling ring layer and a liquid level controller communicated with the excitation chamber, wherein the liquid level controller is used for controlling the liquid level of the liquid metal in the excitation chamber; the pulling device is capable of pulling at least a portion of the crucible into the excitation chamber through the pulling rod at a predetermined speed range. The device realizes the deep supercooling of the melt by a method combining glass purification and circulating overheating, combines smelting, liquid metal/water dual cooling and a drawing device skillfully, and can select different modes to excite the deep supercooling melt to directionally solidify, thereby obtaining deep supercooling directionally solidified castings with different tissues and performance characteristics to meet more research and application requirements.
Description
Technical Field
The invention relates to the technical field of directional solidification, in particular to a multi-mode excited deep supercooling directional solidification device and method.
Background
The deep supercooling method is an effective way for realizing rapid solidification of three-dimensional large-volume liquid metal by avoiding nucleation of heterogeneous crystal nuclei in metal and alloy liquid as much as possible by various effective purification means, increasing critical nucleation power and inhibiting homogeneous nucleation to ensure that the liquid metal obtains supercooling which is difficult to achieve under conventional solidification conditions. At present, the methods for realizing the deep supercooling of the melt mainly include a droplet emulsification method, a circulation superheating method, a molten glass purification method, and various container-less treatment techniques. The supercooled melt, after solidification, often has its unique structural features such as structure refinement, segregation reduction, appearance of metastable phases, etc.
In recent years, with the development of deep undercooling solidification technology, deep undercooling directional solidification technology has emerged. The method integrates the advantages of deep supercooling and Bridgman directional solidification technology, establishes a micro-scale negative temperature gradient at a solidification interface based on thermodynamic supercooling of the metal melt, releases solidification latent heat to the supercooled melt and stores the same in the supercooled melt, realizes rapid directional solidification or single crystal growth of the melt with a certain size and large volume, and is an ideal means for preparing superfine columnar crystals and single crystals. Compared with the traditional directional solidification, the deep undercooling directional solidification technology can greatly improve the production efficiency, is expected to become a novel manufacturing technology of the single crystal turbine blade of the aero-engine, and has wide application prospect.
The known deep supercooling directional solidification technology is that a crucible containing molten metal is placed on a chilling base, and temperature gradient from bottom to top is established in the molten metal while the molten metal is dynamically supercooled. The bottom with the lowest temperature in the cooling process is firstly nucleated, crystals grow from bottom to top to form a dendritic crystal skeleton which is arranged in an oriented mode, and finally, an oriented solidification structure is obtained. However, the degree of supercooling of the melt achieved by the technology is small, and under the condition of small supercooling, the driving force of crystal growth is still small, and the directional solidification process can be completed by means of an external temperature field, so that a forced cooling device is also needed. The method is a product which is formed by combining self-excited nucleation of supercooled melt and forced crystal growth, so that the heat flow constraint of directional solidification cannot be fundamentally eliminated, and the nucleation process is performed spontaneously in the cooling process of the melt, so that the initial nucleation supercooling degree cannot be accurately controlled, the yield of single crystals is low, and the reliable industrial production technology is difficult to develop. Thereafter, the deep supercooling directional solidification technology is improved to realize directional solidification by manually exciting a supercooled melt, but the purification and solidification processes of the melt need to be carried out in different crucibles, and the process is complicated. Moreover, when the metal melt is excited, only one of point excitation, surface excitation or body excitation can be used, and the controllable parameters in the directional solidification process are few; the smelting volume is small, and a larger sample cannot be prepared. Therefore, it is necessary to design a new apparatus and method for directional solidification of a melt with deep undercooling to meet the demands of more applications.
Disclosure of Invention
Technical problem to be solved
The invention mainly aims to provide a multi-mode excited deep supercooling directional solidification device, and aims to solve the problems that the excitation mode is single, the process is complicated, in-situ melting and directional solidification cannot be carried out and the like in the prior art.
(II) technical scheme
In order to achieve the above object, the multi-mode excited deep supercooling directional solidification apparatus of the present invention includes:
the reaction furnace is internally provided with a sealed chamber;
the melting device comprises a crucible and a heating mechanism, the crucible is arranged in the sealed cavity and used for containing alloy materials, and the heating mechanism is used for carrying out hot melting on the alloy materials in the crucible;
the feeding device is used for adding a purifying agent into the crucible in the hot melting process;
the excitation device is arranged in the sealed cavity and comprises an excitation chamber capable of being filled with liquid metal, a water-cooling ring layer wrapped outside the excitation chamber and a liquid level controller communicated with the excitation chamber, and the liquid level controller is used for controlling the liquid level of the liquid metal in the excitation chamber;
the drawing rod penetrates through the excitation chamber from the outside and can move in the excitation chamber, and the upper end of the drawing rod is connected with the bottom of the crucible;
and the lower end of the pulling rod is connected with the pulling device, and the pulling device can pull at least one part of the crucible into the excitation chamber through the pulling rod in a preset speed range.
Optionally, the deep undercooling directional solidification device further comprises:
the water cooling machine is used for cooling the water cooling interlayer, the heating mechanism and the water cooling ring layer in the reaction furnace;
the vacuum pump is used for vacuumizing the sealed chamber;
and the experimental atmosphere source is used for filling protective gas required by the experiment into the sealed chamber.
Optionally, the heating mechanism includes an electric conductor heating sleeve sleeved outside the crucible and a high-frequency induction coil sleeved outside the crucible; the high-frequency induction coil can generate a vortex electromagnetic field to heat the electric conductor heating sleeve; the water cooling machine is used for water cooling the high-frequency induction coil; the high-frequency induction coil is formed by winding a red copper pipe with a hollow channel, and the hollow channel is communicated with the water cooler through a pipeline.
Optionally, the upper end of the pulling rod is connected with the bottom of the crucible through a plurality of support columns;
and/or the bottom of the crucible is provided with at least one blind hole.
Optionally, the drawing device comprises a support frame, a driving mechanism arranged on the support frame, a screw rod driven by the driving mechanism to rotate, and a screw nut sleeved on the screw rod, and the screw nut is fixedly connected with the bottom of the drawing rod;
the top of the excitation chamber is provided with a guide sleeve, and a sealing guide sleeve is arranged between the bottom of the excitation chamber and the pull rod;
the inner wall of the sealing guide sleeve is provided with a convex block, the drawing rod is provided with a groove matched with the convex block, and the groove extends along the axial direction of the drawing rod.
Optionally, the feeding device comprises a screw rod and a feeding scoop, the screw rod penetrates through the furnace wall of the reaction furnace from the outside and extends into the sealed chamber, the screw rod can axially rotate relative to the furnace wall, and the feeding scoop is arranged at one end of the screw rod, which is positioned in the sealed chamber;
and/or the deep supercooling directional solidification device further comprises a temperature measuring instrument, a transparent observation window is arranged on the reaction furnace, and the temperature measuring instrument is arranged corresponding to the transparent observation window.
Further, the invention also provides a multi-mode excited deep undercooling directional solidification method, which comprises the following steps:
s1, preparing an alloy material, putting the alloy material into a crucible, and putting a purifying agent into a feeding spoon;
s2, placing the crucible in a sealed cavity of the reaction furnace, filling protective gas into the sealed cavity after vacuumizing the sealed cavity, and repeating the process from vacuumizing to inflating for many times;
s3, heating the crucible by a heating mechanism to melt the alloy material in the crucible into an alloy melt;
s4, adding a purifying agent into the crucible by using a feeding device;
s5, heating the alloy melt to a preset superheat degree through a heating mechanism, then preserving heat for a preset time, and then cooling the alloy melt to room temperature;
s6, repeating the step S5 for a plurality of times;
s7, after the temperature of the alloy melt is reduced to a preset supercooling degree, drawing at least one part of the crucible into an excitation chamber through a drawing rod at a preset speed range by a drawing device so as to directionally solidify the alloy melt, wherein the excitation device comprises an excitation chamber capable of being filled with liquid metal and a water cooling ring layer wrapped outside the excitation chamber;
and S8, after the directional solidification is finished, pushing the crucible to extend out of the heating mechanism through a drawing rod, opening the reaction furnace, taking out the crucible, and demolding to obtain the directional solidification cast ingot.
Optionally, the predetermined speed range is 1mm/s to 50 mm/s;
and/or the mode of pulling at least a portion of the crucible into the excitation chamber comprises:
point excitation mode: the bottom surface of the crucible enters the excitation chamber, and the blind hole on the bottom surface of the crucible is filled with liquid metal;
surface excitation mode: the bottom surface of the crucible enters the excitation chamber and contacts the liquid metal;
bulk excitation mode: the bottom and a portion of the sides of the crucible enter the excitation chamber and both the bottom and a portion of the sides of the crucible contact the liquid metal.
Optionally, the preset superheat degree is 100K-300K; and/or the preset supercooling degree is 50K-400K.
Optionally, the scavenger comprises B2O3、Na2B4O7、SiO2、CaO、Al2O3、Na2O and K2At least one of O.
(III) advantageous effects
The invention has the beneficial effects that:
(1) the speed and the area of the crucible contacting the liquid metal can be accurately controlled by skillfully combining the drawing device and the excitation device, and the deep undercooling directional solidification casting with different tissues and performance characteristics is obtained by exciting the undercooling melt to nucleate in a plurality of modes of point excitation, surface excitation and body excitation.
(2) According to the invention, liquid metal and water cooling are combined to be used as a nucleation excitation device, so that the temperature of the melt can be rapidly reduced, and a better nucleation excitation effect is achieved.
(3) The smelting and solidification processes of the alloy are carried out in the same crucible, the melting is full, the pouring is not needed, the components of the solidified cast ingot are uniform, the defects of shrinkage cavity and the like are few, the in-situ melting, deep supercooling and directional solidification of the alloy material can be realized by adopting the invention, the production efficiency is improved, and the sample loss is reduced.
(4) Under the condition of large supercooling degree, the growth speed of crystals in the melt is high, so that the size of a substructure in a structure after directional solidification is small, and the segregation degree of microcosmic components is low.
(5) The device has good sealing performance and high vacuum degree, can effectively reduce the oxidation of metal materials, and improves the material utilization rate and the production efficiency.
Therefore, the device realizes the deep supercooling of the melt through glass purification and circulating overheating, combines smelting, liquid metal/water double cooling and a drawing device skillfully, can select different modes to excite the deep supercooling melt to directionally solidify, and can obtain deep supercooling directionally solidified castings with different structures and performance characteristics so as to meet more research and application requirements.
Drawings
FIG. 1 is a schematic structural diagram of a multi-mode excited deep undercooling directional solidification device of the present invention;
FIG. 2 is a schematic view showing the structure of a heating mechanism, a point excitation mode crucible and a pulling rod according to an embodiment of the present invention;
FIG. 3 is a bottom view of the crucible for point excitation of FIG. 2;
FIG. 4 is a schematic view of the structure of a heating mechanism, a surface excitation and body excitation mode crucible and a pulling rod according to another embodiment of the present invention;
FIG. 5 is a schematic diagram of the excitation device of the present invention;
FIG. 6 is a schematic diagram of the embodiment of FIG. 4 in a bulk excitation mode;
FIG. 7 is a schematic view of the construction of the drawer rod and drawer device of the present invention;
figure 8 is a schematic cross-sectional view of the pull rod and seal guide of the present invention;
fig. 9 is a schematic flow diagram of the multi-mode excited deep undercooling directional solidification method of the present invention.
[ description of reference ]
1: a reaction furnace; 2: a smelting device; 3: a temperature measuring instrument; 4: a feeding device; 5: an excitation device; 6: a pull rod; 7: a drawing device; 8: a vacuum pump; 9: an experimental atmosphere source; 10: a water cooling machine; 11: a high-frequency induction coil; 12: an electrical conductor heating jacket; 13: a surface excitation and body excitation mode crucible; 14: an alloy material; 15: a purifying agent; 16: point excitation mode crucible; 17: a support post mounting hole; 18: blind holes; 19: an excitation chamber; 20: a liquid level controller; 21: a water-cooled ring layer; 22: a guide sleeve; 23: sealing the guide sleeve; 24: a feed screw nut; 25: a screw rod; 26: a transmission device; 27: a speed reducer; 28: a servo motor; 29: a support frame.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
It should be noted that all the directional indicators (such as up, down, left, right, front, and rear … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
In addition, the descriptions related to "first", "second", etc. in the present invention are only for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "connected," "secured," and the like are to be construed broadly, and for example, "secured" may be a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
As shown in fig. 1, fig. 2 and fig. 4, the invention provides a multi-mode excited deep supercooling directional solidification device, which comprises a reaction furnace 1, a smelting device 2, a feeding device 4, an excitation device 5, a drawing rod 6 and a drawing device 7. Wherein a sealed chamber is formed in the reaction furnace 1. The melting device 2 comprises a crucible arranged in the sealed chamber and used for accommodating the alloy material 14, and a heating mechanism for hot melting the alloy material 14 in the crucible, wherein the heating mechanism can be fixedly supported inside the reaction furnace 1 through a bracket (not shown) or other supporting structures. The feeding device 4 is used for adding a purifying agent 15 into the crucible in the hot melting process. The excitation device 5 is arranged in the sealed cavity, and can be preferably arranged at the bottom of the reaction furnace 1, the excitation device 5 comprises an excitation chamber 19 capable of being filled with liquid metal, a water-cooling ring layer 21 wrapping the excitation chamber 19, and a liquid level controller 20 communicated with the excitation chamber 19, and the liquid level controller 20 is used for controlling the liquid level of the liquid metal in the excitation chamber 19. The pull rod 6 penetrates through the excitation chamber 19 from the outside and can move in the excitation chamber 19, and the upper end of the pull rod 6 is connected with the bottom of the crucible. The lower end of the drawing rod 6 is connected to a drawing device 7, and the drawing device 7 is able to draw at least a part of the crucible into the excitation chamber 19 through the drawing rod 6 at a predetermined speed range. Wherein, the deep supercooling means that the supercooling degree can reach 50K to 400K, and the crystal growth speed in the melt can be increased in the deep supercooling state.
Wherein, be formed with sealed cavity in the reacting furnace 1, can effectively obstruct ambient air, avoid the oxidation of sample. The liquid metal in the excitation chamber 19 is gallium indium alloy or gallium indium tin alloy, and the melting point of the gallium indium alloy and the melting point of the gallium indium tin alloy are 6-10 ℃. The introduction of the cleaning agent 15 into the molten alloy material 14 in the crucible by means of the charging device 4 mainly works in two ways: one is that the molten glass purifying agent is used to protect the surface of the metal melt from the interface between air and liquid metal and to inhibit the formation of oxide to cause the excited nucleation; the other is to separate the alloy melt from the metal oxide by viscous adsorption or chemical reaction of the molten glass purifying agent to realize physical purification or chemical purification, thereby realizing deep supercooling of the melt to improve the directional solidification effect.
The excitation device 5 is arranged below the crucible, the excitation device 5 is of an annular structure, a plurality of interlayers are separated from the interior of the excitation device through cylindrical partition plates, the outer interlayer is filled with water to form a water-cooling annular layer 21, the inner interlayer forms an excitation chamber 19, and the whole material of the excitation device 5 is stainless steel. The excitation device 5 has double cooling functions of liquid metal and water cooling, and can rapidly excite the nucleation of the deep undercooled melt, thereby realizing directional solidification. In the invention, because the melt is in a deep supercooled state, the temperature gradient direction at the solid-liquid interface during solidification is from a liquid phase to a solid phase, and is a negative temperature gradient (namely the solid phase is high, and the liquid phase is low), and the latent heat of crystallization can be diffused into the liquid phase. Since supercooled melts are metastable, once nucleated by excitation, dendrites grow rapidly from the excitation due to the latent heat of crystallization being released very rapidly through the liquid phase. And the larger the initial supercooling degree of the melt is, the faster the growth rate after excitation is, so that the directional solidification speed is higher.
When pulling at least a portion of the crucible into the excitation chamber 19, different excitation modes can be selected according to process requirements, for example, a spot excitation mode, a surface excitation mode, and a bulk excitation mode. In the case of the point excitation mode, a point excitation mode crucible 16 can be selected whose bottom is provided with at least one blind hole 18 (see fig. 2 and 3), wherein a plurality of blind holes 18 can be distributed symmetrically about the center in order to achieve a better directional solidification effect. In the point excitation mode, the bottom surface of the crucible is made to enter the excitation chamber 19, the bottom surface of the crucible is made to contact the liquid metal and the blind hole 18 on the bottom surface is filled with the liquid metal, the blind hole 18 is made to be filled with the liquid metal by setting the pull distance in advance (actually, the bottom of the crucible is also made to contact the liquid metal), then the portion of the crucible provided with the blind hole 18 is relatively thin, the cooling is faster, and therefore the point excitation is realized. In the surface excitation mode, the surface excitation and bulk excitation mode crucible 13 (see fig. 4 and 5) may be selected such that the bottom surface of the crucible is not provided with the blind hole 18, and the bottom surface of the crucible is allowed to enter the excitation chamber 19 and contact the liquid metal. In the case of the bulk excitation mode, the surface excitation and bulk excitation mode crucible 13 is also selected such that the bottom surface is not provided with the blind hole 18, the bottom surface and a part of the side surface of the crucible (specifically, the lower half of the side surface of the crucible) enter the excitation chamber 19 and both the bottom surface and a part of the side surface of the crucible contact the liquid metal (see fig. 6). Under these three modes, except letting the crucible move down, can also suitably adjust the liquid level of liquid metal, can specifically adjust the liquid level of liquid metal through liquid level controller 20 to can make pull speed, pull time and liquid level height cooperate mutual compensation jointly, in order to conveniently realize the excitation effect of different modes. Moreover, the liquid level controller 20 is communicated with the liquid metal in the excitation chamber 19, so that the liquid level of the liquid metal can be monitored and kept within a certain range, and the liquid level of the liquid metal is prevented from being greatly changed due to the movement of the drawing rod 6. Wherein, the predetermined speed range can be 1 mm/s-50 mm/s, and the drawing speed can be adjusted according to the required temperature gradient in the actual operation process.
The technical scheme has the following effects:
(1) the pulling device 7 can pull the crucible into the excitation chamber 19 through the pulling rod 6, the speed and the area of the crucible contacting the liquid metal can be accurately controlled through the ingenious combination of the pulling device 7 and the excitation device 5, and the undercooling melt is subjected to nucleation excitation through a plurality of modes of point excitation, surface excitation and body excitation to obtain the deep undercooling directional solidification casting with different tissues and performance characteristics.
(2) According to the invention, liquid metal and water cooling are combined to be used as the nucleation excitation device 5, so that the temperature of the melt can be rapidly reduced, and a better nucleation excitation effect is achieved.
(3) The smelting and solidification processes of the alloy are carried out in the same crucible, the melting is full, the pouring is not needed, the components of the solidified cast ingot are uniform, the defects of shrinkage cavity and the like are few, the in-situ melting, deep supercooling and directional solidification of the alloy material 14 can be realized by adopting the invention, the production efficiency is improved, and the sample loss is reduced.
(4) In a deep undercooled state (or a large undercooling degree), the crystal growth speed in the melt is high, so that the size of a substructure in a structure after directional solidification is small, and the segregation degree of a microcosmic component is low.
(5) The device has good sealing performance and high vacuum degree, can effectively reduce the oxidation of the alloy material 14, and improves the material utilization rate and the production efficiency.
Therefore, the device realizes the deep supercooling of the melt by a method combining glass purification and circulating overheating, and skillfully combines melting, liquid metal/water double cooling and the drawing device 7, and can select different modes to excite the deep supercooling melt to directionally solidify, thereby obtaining the deep supercooling directionally solidified casting with different structures and performance characteristics to meet more research and application requirements.
Further, referring again to fig. 1, in a preferred embodiment, the deep sub-cooling directional solidification apparatus further comprises a water cooler 10, a vacuum pump 8 and a test atmosphere source 9. The water cooler 10 is used for cooling the water-cooling interlayer, the heating mechanism and the water-cooling ring layer 21 in the reaction furnace 1, so that the corresponding components can reach the preset cooling temperature quickly, and the device can be switched to enter the directional solidification process after the smelting process is finished. Furthermore, a vacuum pump 8 is used to evacuate the sealed chamberThe sealed chamber is connected with a vacuum pump 8 (a mechanical pump and a molecular pump) through a stainless steel pipeline, and the vacuum degree of the sealed chamber can reach 1 multiplied by 10-6Pa. The experimental atmosphere source 9 is connected to the sealed chamber through a stainless steel pipe so as to be able to fill the sealed chamber with the protective gas (i.e., inert gas) required for the experiment. The experimental atmosphere source 9 may be a compressed gas tank of helium or argon or a mixture thereof; after the vacuum pump 8 vacuumizes the sealed cavity, the gas is reversely filled into the sealed cavity to 0.5 multiplied by 10 through the experimental atmosphere source 95Pa～1×105Pa. The whole process in the device is carried out under the protection of inert atmosphere, and the processes of vacuumizing, inflating, smelting and solidifying are completed at one time. In addition, the vacuum degree in the sealed cavity is high, the alloy sample is not easy to oxidize, and the casting quality and the material utilization rate are improved.
Furthermore, as shown in fig. 5 and 6, in order to ensure the vertical movement of the crucible, a guide sleeve 22 is provided on the top of the excitation chamber 19, capable of guiding the movement of the crucible. The guide sleeve 22 may be made of stainless steel. In addition, in a more preferred embodiment, a sealing guide sleeve 23 is arranged between the bottom of the excitation chamber 19 and the pull rod 6, and the pull rod 6 and the excitation chamber 19 are sealed and guided through the sealing guide sleeve 23, so that the stability of the pulling process can be ensured, the ambient air can be effectively blocked, and the oxidation of the sample can be avoided. Furthermore, the axis of the sealing guide sleeve 23 extends in the vertical direction to enable the crucible and the pull rod 6 to keep moving vertically, thereby minimizing the interference of the horizontal shaking on the melt solidification process. Wherein, sealed uide bushing 23 can be the softer brass material of material, can wear-resisting, also can guarantee not to damage pull pole 6. In other embodiments, the sealing guide sleeve 23 is additionally provided with a dynamic sealing ring, which may be composed of two rubber rings and a gasket having the same shape as the sealing guide sleeve 23, so as to further improve the sealing performance of the pull rod 6 during the pulling process.
As shown in fig. 2, the heating mechanism includes an electric conductor heating jacket 12 sleeved outside the crucible and a high-frequency induction coil 11 sleeved outside the crucible; the high-frequency induction coil 11 is capable of generating a swirling electromagnetic field to heat the electric conductor heating jacket 12. The water cooler 10 is used for water cooling the high-frequency induction coil 11; the high-frequency induction coil 11 is formed by winding a red copper pipe with a hollow channel, and the hollow channel is communicated with the water cooler 10 through a pipeline. The electric conductor heating jacket 12 can be a graphite heating jacket, and graphite has excellent electric conduction and heat conduction performance and is used as a heating body in a special industrial furnace. The graphite heating jacket may be cylindrical. In the heating process, the graphite heating sleeve is heated in an electromagnetic induction mode after the high-frequency induction coil 11 is electrified, and then heat is transferred to the crucible by the graphite heating sleeve, so that alloy raw materials in the crucible can be melted.
The water cooler 10 may also be configured to cool the high-frequency induction coil 11, and the water cooler 10 and the high-frequency induction coil 11 may be communicated with each other through a pipeline. The high-frequency induction coil 11 is formed by winding a copper tube with a hollow channel, namely, the copper tube for winding the coil is a water flow pipeline. The high-frequency induction coil 11 can generate a vortex electromagnetic field to enable the electric conductor heating jacket 12 to generate heat, and meanwhile, the hollow channel in the copper tube is directly communicated with the water cooler 10 through a pipeline, so that the high-frequency induction coil 11 can be prevented from being overheated. The mode of directly introducing cold water into the hollow channel of the copper tube for refrigeration can adapt to a heating mechanism with higher heating requirement.
The water cooler 10 is communicated with the high-frequency induction coil 11 and also forms a water cooling circulation loop with a water cooling ring layer of the excitation device 5 through a group of circulation pipelines, and the water cooler 10 supplies cold to the water cooling ring layer to assist the liquid metal to form a proper temperature gradient in the excitation device 5. In addition, a water cooling interlayer may be formed in the wall of the reaction furnace 1, the water cooling interlayer is connected to the water cooler 10 through a pipe to prevent the temperature of the wall from being too high, and the water cooling interlayer is connected to the water cooler 10 through a set of circulation pipes to form a water cooling circulation loop. Wherein the compressor power of the water cooling machine 10 is 3 kW-6 kW.
Further, the crucible (the point excitation mode crucible 16 or the surface excitation and bulk excitation mode crucible 13) may be a cylindrical quartz crucible. As shown in fig. 2 and fig. 4 to 6, the upper end of the pull rod 6 is connected with the bottom of the crucible through a plurality of support columns, so as to ensure that the pull rod 6 and the crucible can be stably connected in a high-temperature environment. And, be provided with support column mounting hole 17 (see fig. 3) in the bottom surface of crucible, the one end of support column is passed through the screw and is connected with the support column mounting hole 17 of crucible bottom surface, and the other end of support column and the firm joint in upper end of pull pole 6 to can ensure the steady of pull process, reduce because rock the interference to directional solidification process, also can dismantle according to the demand. The support column is a slender strip rod, so that the occupied area of the bottom surface of the crucible can be reduced, and the excitation effect of the bottom surface of the crucible is more uniform.
As shown in fig. 7, the drawing device 7 includes a supporting frame 29, a driving mechanism disposed on the supporting frame 29, a lead screw 25 driven by the driving mechanism to rotate, and a lead screw nut 24 sleeved on the lead screw 25, wherein the lead screw nut 24 is fixedly connected with the bottom of the drawing rod 6. When the driving mechanism drives the screw rod 25 to rotate, the screw rod nut 24 on the screw rod 25 can move along the axial direction of the screw rod 25 and drive the drawing rod 6 to move along the vertical direction to complete drawing action. Wherein, actuating mechanism is including all setting up servo motor 28, speed reducer 27 and transmission 26 on support frame 29, and transmission 26 can include intermeshing's initiative bevel gear and driven bevel gear, and the bottom of lead screw 25 is installed on support frame 29 through the bearing and is provided with the initiative bevel gear on the lead screw 25, is provided with driven bevel gear on the output of speed reducer 27, and the power input of speed reducer 27 and the output of servo motor 28 are connected. The servo motor 28 is connected to the screw rod 25 through the speed reducer 27 and the transmission 26 to transmit torque, that is, the servo motor 28 drives the screw rod 25 to rotate through the speed reducer 27 and the transmission 26. The drawing speed of the drawing rod 6 is determined by the rotation speed of the servo motor 28, the reduction ratio of the reduction gear 27, and the lead of the lead screw 25. In a preferred embodiment, the predetermined speed range of the withdrawal speed of the withdrawal rod 6 is in the range of 1mm/s to 50 mm/s. Moreover, in order to make the feed screw nut 24 move according to the predetermined direction, as shown in fig. 8, a convex block is provided on the inner wall of the sealing guide sleeve 23, a groove adapted to the convex block is provided on the pull rod 6, the groove extends along the axial direction of the pull rod 6, wherein both a rubber ring and a gasket used for the dynamic sealing ring can be shaped to be adapted to the sealing guide sleeve 23 with the convex block, thereby realizing dynamic sealing. When the pull rod 6 moves along the vertical direction, the groove and the lug in the groove move up and down relatively, and the circumferential limit of the pull rod 6 and the sealing guide sleeve 23 is realized through the matching of the lug and the groove.
Further, as shown in fig. 1, the charging device 4 includes a screw rod extending into the sealed chamber from the outside through the furnace wall of the reaction furnace 1, the screw rod being capable of axially rotating with respect to the furnace wall, and a charging spoon provided at one end of the screw rod in the sealed chamber, and adding a material such as a purifying agent during melting. The material to be added is previously placed on the feeding spoon, and the feeding spoon is turned over by rotating the screw from the outside of the reaction furnace 1 at a predetermined temperature or time, so that the cleaning agent 15 can be added to the alloy material 14 to increase the supercooling degree of the melt by glass cleaning.
In addition, referring to fig. 1 again, the deep supercooling directional solidification device further includes a temperature measuring instrument 3, a transparent observation window (which may be a glass observation window) is arranged on the reaction furnace 1, and the temperature measuring instrument 3 is arranged corresponding to the transparent observation window. The temperature detector 3 can be an infrared temperature detector, the temperature measuring range is 400-2000 ℃, and real-time temperature data can be obtained so as to judge the melting, overheating and supercooling states of the sample. The infrared thermometer has the advantages of fast response time, non-contact, safe use, long service life and the like, and can monitor the infrared radiation energy change inside the reaction furnace 1 through the transparent observation window outside the reaction furnace 1, thereby conveniently and quickly obtaining real-time temperature data.
In addition, as shown in fig. 9, the present invention also provides a multi-mode excited deep undercooling directional solidification method, which comprises the following steps.
S1, preparing the alloy material 14 and putting the alloy material into a crucible. The alloy material 14 is prepared according to the proportion of alloy elements, the total mass of the alloy material 14 is 0.01 kg-5 kg, the alloy material 14 is placed into a crucible after the preparation is finished, and then a purifying agent is placed into a feeding spoon.
S2, placing the crucible in a sealed cavity of the reaction furnace 1, and filling protective gas into the sealed cavity after vacuumizing the sealed cavity. Specifically, the sealed chamber was evacuated to 1 × 10-6Pa or so, then refilling the experimental atmosphere to0.5×105Pa～1×105Pa, and repeating the process from vacuumizing to inflating for multiple times;
and S3, heating the crucible by using a heating mechanism so as to melt the alloy material 14 in the crucible into an alloy melt. Specifically, the melting device 2 is started (i.e., the power supply of the heating mechanism is turned on), the temperature of the alloy material 14 is monitored through the temperature measuring instrument 3, and the temperature is kept for 10-30 minutes after the alloy material 14 is completely melted, so that the alloy material 14 is uniformly melted.
S4, adding the purifying agent 15 into the crucible by using the feeding device 4. Specifically, the purifying agent in the feeding spoon can enter the crucible by rotating the screw.
S5, heating the alloy melt to a preset superheat degree (which can be 100-300K) through a heating mechanism, preserving heat for a preset time (which can be 5-20 min), and then cooling the alloy melt to room temperature (20-25 ℃).
S6, repeating the step S5 for multiple times, performing circulating overheating and supercooling on the alloy melt by changing the heating power of the smelting device 2, and realizing deep supercooling of the melt by a method combining glass purification and circulating overheating.
S7, after the temperature of the alloy melt is reduced to a preset supercooling degree (which can be 50K-400K), the drawing device 7 draws at least one part of the crucible into the excitation chamber 19 through the drawing rod 6 at a preset speed range so as to directionally solidify the alloy material 14. Specifically, when the temperature of the alloy melt is reduced to a certain supercooling degree, the drawing device 7 is started, the crucible is drawn into the liquid metal in the excitation chamber 19 through the drawing speed and the drawing distance which are designed in advance, the supercooled melt is excited to nucleate, and the deep supercooling directional solidification is realized. Wherein, the excitation device 5 comprises an excitation chamber 19 which can be filled with liquid metal and a water cooling ring layer 21 which is wrapped outside the excitation chamber 19.
And S8, after the directional solidification is finished, pushing the crucible to extend out of the heating mechanism through the drawing rod 6, opening the reaction furnace 1, taking out the crucible, and demolding to obtain the directional solidification cast ingot. Specifically, after finishing the directional solidification, the power supply of the heating mechanism and the drawing device 7 is closed, the reaction furnace 1 is opened after cooling for 5-30 min, and the crucible is taken out and demoulded to obtain the directional solidification ingot.
The method realizes the deep supercooling of the melt by combining the glass purification and the circulating superheat, skillfully combines the melting, the liquid metal/water double cooling and the drawing device 7, and can select different modes to excite the deep supercooling melt to directionally solidify, thereby obtaining the deep supercooling directionally solidified casting with different structures and performance characteristics to meet more research and application requirements.
Wherein, when at least a part of the crucible is pulled into the excitation chamber 19, different excitation modes can be selected according to the process requirements, and the modes for pulling at least a part of the crucible into the excitation chamber 19 include: 1. point excitation mode: the bottom surface of the crucible enters an excitation chamber 19 and a blind hole 18 on the bottom surface of the crucible is filled with liquid metal; 2. surface excitation mode: the bottom of the crucible enters the excitation chamber 19 and contacts the liquid metal; 3. bulk excitation mode: the bottom and part of the side of the crucible enter the excitation chamber 19 and both the bottom and part of the side of the crucible contact the liquid metal. By skillfully combining the drawing device 7 and the excitation device 5, the speed and the area of the crucible contacting the liquid metal can be accurately controlled, and the supercooled melt is nucleated by a plurality of modes of point excitation, surface excitation and body excitation to obtain the deep supercooled directional solidification casting with different tissues and performance characteristics.
When the temperature of the alloy melt drops to a certain supercooling degree, the pulling device 7 is started to pull the crucible into the liquid metal in the excitation chamber 19 at a pulling rate and a pulling distance which are designed in advance. Wherein, the drawing distance means that 0-100% of the side surface of the metal melt in the crucible can be correspondingly arranged under the liquid level of the liquid metal after the crucible moves for a preset distance, so as to realize different excitation modes (0% is a point excitation mode or a surface excitation mode contacted with the bottom of the crucible, and more than 0% is a body excitation mode). For example, in the bulk-excited mode, 80% of the side of the molten metal is exposed to the liquid metal (i.e., 80% of the molten metal in the crucible near the bottom of the crucible is below the level of the liquid metal). In addition, the drawing rate is in the range from 1mm/s to 50 mm/s. According to the invention, the drawing device 7 and the excitation device 5 are skillfully combined, the supercooled melt nucleation can be excited in multiple modes of point excitation, surface excitation and body excitation in different degrees, and the speed of the crucible contacting liquid metal can be adjusted, so that the deep supercooled directional solidification casting with more tissues and performance characteristics can be obtained.
It is noted that the purifying agent may be a glass purifying agent, specifically including B2O3(boron oxide), Na2B4O7(sodium tetraborate), SiO2(silicon dioxide), CaO (calcium oxide), Al2O3(alumina), Na2O (sodium oxide) and K2At least one of O (potassium oxide). Aiming at different alloy systems, a proper glass purifying agent and a proper proportion are selected, and the purifying agent selection principle mainly comprises the following steps: 1. does not react with the alloy per se; 2. the softening temperature is lower than the melting point of the alloy, and the alloy has good fluidity in the softening temperature range; 3. it should have a suitable viscosity (too high a viscosity would result in insufficient wetting of the scavenger with the metal melt, while too low a viscosity would be detrimental to adsorbing heterogeneous nuclei in the melt); 4. can react with high-melting point oxides and other heterogeneous cores in the alloy to generate low-melting point compounds. The purifying agent selected according to the principle can improve the directional solidification effect and ensure the quality of the directional solidification casting.
In step S6, step S5 may be repeated 2 to 6 times. The principle of the cyclic overheating method is to remove or passivate heterogeneous cores in the alloy material by melting, decomposition or evaporation to lose the substrate effect, so as to realize deep undercooling of the liquid alloy material.
The multi-mode excited deep undercooling directional solidification method of the present invention is further described with reference to the following specific examples.
Example 1:
1. preparing 1kg of 302 stainless steel (1Cr18Ni9) alloy raw material, and putting the alloy raw material into a crucible; according to B2O3、Na2B4O7Preparing a glass purifying agent in a ratio of 1:1 and putting the glass purifying agent into a feeding spoon.
2. The vacuum pump 8 is turned on to pump the sealed chamber to 1X 10-6Pa, then filling high-purity argon into the sealed chamber to 0.8 multiplied by 105Pa, this procedure was repeated five times. Starting the smelting unit 2 and increasing the heating powerAnd (3) observing the melting condition of the alloy through a thermodetector 3, and preserving the temperature for 30 minutes after the alloy is completely melted.
3. The glass purifying agent is added into the crucible through the feeding device 4, the sample is heated to be overheated to 250K and then is kept warm for 10 minutes, then the power supply of the smelting device 2 is turned off, and the steps are repeated five times after the sample is cooled to the room temperature.
4. When the alloy temperature is reduced to 50K supercooling degree, starting a power supply of the drawing device 7, drawing down the crucible at the speed of 10mm/s, just filling the blind hole 18 at the bottom of the crucible with liquid metal, and exciting the deep supercooling melt to directionally solidify in a point excitation mode.
5. And after solidification, closing the power supplies of the smelting device 2 and the drawing device 7, cooling for 30 minutes, opening the reaction furnace 1, taking out the crucible, and demolding to obtain the deep super-cooling directional solidification 302 stainless steel.
Example 2:
1. 5kg of Monel K500 nickel-based alloy raw material is prepared and put into a crucible; b is to be2O3And (4) putting the glass purifying agent into the feeding spoon.
2. The vacuum pump 8 is turned on to pump the sealed chamber to 1X 10-6Pa, filling high-purity helium gas into the sealed chamber to 1 × 105Pa, this procedure was repeated three times. Starting the smelting device 2, increasing the heating power, observing the melting condition of the metal through the temperature measuring instrument 3, and preserving the temperature for 30 minutes after the metal is completely melted.
3. Adding a glass purifying agent into the crucible through the feeding device 4, heating the sample to be overheated for 300K, then preserving the heat for 20 minutes, then turning off the power supply of the smelting device 2, cooling the sample to room temperature, and repeating the steps for six times.
4. When the alloy temperature is reduced to 230K supercooling degree, starting a power supply of the drawing device 7, drawing down the crucible at the speed of 1mm/s and just enabling the bottom of the crucible to contact with liquid metal, and exciting the deep supercooling melt to directionally solidify in a surface excitation mode.
5. And after solidification, closing the power supplies of the smelting device 2 and the drawing device 7, cooling for 30 minutes, opening the reaction furnace 1, taking out the crucible, and demolding to obtain the deep super-cooling directional solidification Monel K500 nickel-based alloy.
Example 3:
1. preparing 0.01kg of metal raw materials according to the atomic ratio of Ti, Ni, Al and Cr of 14:3:2:1, and putting the metal raw materials into a crucible; according to SiO2、B2O3、CaO、Al2O3、Na2O、K2And (4) preparing a glass purifying agent according to the ratio of 5:2:2:1:1:1, and putting the glass purifying agent into the feeding spoon.
2. The vacuum pump 8 is turned on to pump the sealed chamber to 1X 10-6Pa, then filling the mixed gas of high-purity helium and argon into the sealed chamber in a ratio of 1:3 to 0.5 × 105Pa, this procedure was repeated three times. Starting the smelting device 2, increasing the heating power, observing the melting condition of the metal through the temperature measuring instrument 3, and preserving the temperature for 10 minutes after the metal is completely melted.
3. Adding a glass purifying agent into the crucible through a feeding device 4, heating the sample to be overheated for 100K, then preserving the heat for 5 minutes, then turning off the power supply of the smelting device 2, and repeating the steps twice after cooling the sample to the room temperature.
4. When the alloy temperature is reduced to 400K supercooling degree, the power supply of the drawing device 7 is started, the crucible is drawn downwards at the speed of 50mm/s, 100% of the side surface of the metal melt is contacted with the liquid metal (namely, the metal melt in the crucible is totally below the liquid level of the liquid metal), and the directional solidification of the deeply supercooled melt is excited in a body excitation mode.
5. After solidification, the power supplies of the smelting device 2 and the drawing device 7 are closed, the reaction furnace 1 is opened after cooling for 5 minutes, and the crucible is taken out and demoulded to obtain the deep super-cooling directional solidification Ti70Ni15Al10Cr5And (3) alloying.
It should be understood that the above description of specific embodiments of the present invention is only for the purpose of illustrating the technical lines and features of the present invention, and is intended to enable those skilled in the art to understand the contents of the present invention and to implement the present invention, but the present invention is not limited to the above specific embodiments. It is intended that all such changes and modifications as fall within the scope of the appended claims be embraced therein.
Claims (10)
1. A multi-mode excited deep supercooling directional solidification device, characterized by comprising:
the reaction furnace is internally provided with a sealed chamber;
the melting device comprises a crucible and a heating mechanism, the crucible is arranged in the sealed cavity and used for containing alloy materials, and the heating mechanism is used for carrying out hot melting on the alloy materials in the crucible;
the feeding device is used for adding a purifying agent into the crucible in the hot melting process;
the excitation device is arranged in the sealed cavity and comprises an excitation chamber capable of being filled with liquid metal, a water-cooling ring layer wrapped outside the excitation chamber and a liquid level controller communicated with the excitation chamber, and the liquid level controller is used for controlling the liquid level of the liquid metal in the excitation chamber;
the drawing rod penetrates through the excitation chamber from the outside and can move in the excitation chamber, and the upper end of the drawing rod is connected with the bottom of the crucible;
a drawing device, the lower end of the drawing rod is connected with the drawing device, and the drawing device can draw at least one part of the crucible into the excitation chamber through the drawing rod in a preset speed range;
the mode of pulling at least a portion of the crucible into the excitation chamber comprises:
point excitation mode: the bottom surface of the crucible enters the excitation chamber, and the blind hole on the bottom surface of the crucible is filled with liquid metal;
surface excitation mode: the bottom surface of the crucible enters the excitation chamber and contacts the liquid metal;
bulk excitation mode: the bottom and a portion of the sides of the crucible enter the excitation chamber and both the bottom and a portion of the sides of the crucible contact the liquid metal.
2. The multi-mode excited deep subcooling directional solidification device as defined in claim 1, wherein: the deep undercooling directional solidification device further comprises:
the water cooling machine is used for cooling the water cooling interlayer, the heating mechanism and the water cooling ring layer in the reaction furnace;
the vacuum pump is used for vacuumizing the sealed chamber;
and the experimental atmosphere source is used for filling protective gas required by the experiment into the sealed chamber.
3. The multi-mode excited deep subcooling directional solidification device as defined in claim 2, wherein: the heating mechanism comprises an electric conductor heating sleeve sleeved outside the crucible and a high-frequency induction coil sleeved outside the crucible; the high-frequency induction coil can generate a vortex electromagnetic field to heat the electric conductor heating sleeve; the water cooling machine is used for water cooling the high-frequency induction coil; the high-frequency induction coil is formed by winding a red copper pipe with a hollow channel, and the hollow channel is communicated with the water cooler through a pipeline.
4. The multi-mode excited deep subcooling directional solidification device as defined in any one of claims 1 to 3 wherein: the upper end of the pulling rod is connected with the bottom of the crucible through a plurality of support columns;
and/or the bottom of the crucible is provided with at least one blind hole.
5. The multi-mode excited deep subcooling directional solidification device as defined in any one of claims 1 to 3 wherein: the drawing device comprises a support frame, a driving mechanism arranged on the support frame, a screw rod driven by the driving mechanism to rotate and a screw rod nut sleeved on the screw rod, and the screw rod nut is fixedly connected with the bottom of the drawing rod;
the top of the excitation chamber is provided with a guide sleeve, and a sealing guide sleeve is arranged between the bottom of the excitation chamber and the pull rod;
the inner wall of the sealing guide sleeve is provided with a convex block, the drawing rod is provided with a groove matched with the convex block, and the groove extends along the axial direction of the drawing rod.
6. The multi-mode excited deep subcooling directional solidification device as defined in any one of claims 1 to 3 wherein: the feeding device comprises a screw and a feeding spoon, the screw penetrates through the furnace wall of the reaction furnace from the outside and extends into the sealed cavity, the screw can axially rotate relative to the furnace wall, and the feeding spoon is arranged at one end of the screw, which is positioned in the sealed cavity;
and/or the deep supercooling directional solidification device further comprises a temperature measuring instrument, a transparent observation window is arranged on the reaction furnace, and the temperature measuring instrument is arranged corresponding to the transparent observation window.
7. A multi-mode excited deep supercooling directional solidification method, wherein the deep supercooling directional solidification method is implemented based on the multi-mode excited deep supercooling directional solidification device of any one of claims 1 to 6, and the deep supercooling directional solidification method comprises:
s1, preparing an alloy material, putting the alloy material into a crucible, and putting a purifying agent into a feeding spoon;
s2, placing the crucible in a sealed cavity of the reaction furnace, filling protective gas into the sealed cavity after vacuumizing the sealed cavity, and repeating the process from vacuumizing to inflating for many times;
s3, heating the crucible by a heating mechanism to melt the alloy material in the crucible into an alloy melt;
s4, adding a purifying agent into the crucible by using a feeding device;
s5, heating the alloy melt to a preset superheat degree through a heating mechanism, then preserving heat for a preset time, and then cooling the alloy melt to room temperature;
s6, repeating the step S5 for a plurality of times;
s7, after the temperature of the alloy melt is reduced to a preset supercooling degree, drawing at least one part of the crucible into an excitation chamber through a drawing rod at a preset speed range by a drawing device so as to directionally solidify the alloy melt, wherein the excitation device comprises an excitation chamber capable of being filled with liquid metal and a water cooling ring layer wrapped outside the excitation chamber;
and S8, after the directional solidification is finished, pushing the crucible to extend out of the heating mechanism through a drawing rod, opening the reaction furnace, taking out the crucible, and demolding to obtain the directional solidification cast ingot.
8. The multi-mode excited deep undercooling directional solidification method of claim 7, wherein: the predetermined speed range is 1 mm/s-50 mm/s.
9. The multi-mode excited deep undercooling directional solidification method of claim 7, wherein: presetting the degree of superheat to be 100K-300K; and/or the preset supercooling degree is 50K-400K.
10. The multi-mode excited deep undercooling directional solidification method of claim 7, wherein: the purifying agent comprises B2O3、Na2B4O7、SiO2、CaO、Al2O3、Na2O and K2At least one of O.
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| CN113957276B (en) * | 2021-10-26 | 2022-07-26 | 西北工业大学 | Liquid deep undercooling and solid phase change duplex coordination control method and device for metal material |
| CN113957369B (en) * | 2021-10-28 | 2022-07-12 | 西北工业大学 | Method for regulating and controlling high-entropy alloy structure and performance by using magnetic field |
| CN114381668B (en) * | 2022-01-18 | 2022-12-13 | 浙江大学 | Supersaturated solid solution soft magnetic material and preparation method thereof |
| CN115418588B (en) * | 2022-09-15 | 2023-04-14 | 西北工业大学 | Magnetic field deep supercooling treatment method for improving toughness of cobalt-based high-temperature alloy |
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