CN112813281B - Method for removing low-density inclusions in high-temperature alloy by combining melt overheating and foamed ceramic filtering - Google Patents
Method for removing low-density inclusions in high-temperature alloy by combining melt overheating and foamed ceramic filtering Download PDFInfo
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Abstract
The invention provides a method for removing low-density inclusions in high-temperature alloy by combining melt overheating and foamed ceramic filtering, which comprises the following steps of: s1, preprocessing a high-temperature alloy raw material; s2, overheating the electron beam melt and filtering the foamed ceramic to remove low-density inclusions in the high-temperature alloy, thereby obtaining the high-purity FGH4096 high-temperature alloy cast ingot. The invention realizes the dissolution and removal of small-size impurities in the high-temperature alloy melt by carrying out overheating treatment on the high-temperature alloy melt, and realizes the filtration of large-size impurities in the alloy by a foamed ceramic filtration method, thereby obtaining a high-purity high-temperature alloy bar by casting; by the method, not only can the low-density inclusions in the alloy be completely removed, but also the situation that an inclusion enrichment area at the top of the ingot needs to be cut off after each refining is finished is avoided, and conditions are created for continuous refining of the high-temperature alloy.
Description
Technical Field
The invention relates to a method for removing low-density inclusions in high-temperature alloy by combining melt overheating and foamed ceramic filtering.
Background
The inclusions in the high-temperature alloy seriously affect the normal-temperature and high-temperature mechanical properties of the alloy, particularly the low-cycle fatigue property, thereby reducing the service stability of the alloy due to long service life. In order to control the inclusions in the high-temperature alloy, China carries out a great deal of research, and currently, the method for filtering and promoting the floating of the inclusions in a molten pool or adsorbing the inclusions floating to the surface by adopting foamed ceramics is a main way for removing the inclusions in the smelting process. According to the Stokes law of the motion of the inclusions, when the sizes of the inclusions are smaller, the floating speed of the inclusions is slower, the inclusions are difficult to remove in a floating mode, and the filtering of the foamed ceramics only has a good effect on the large-size inclusions. The existing method can successfully remove the inclusions with the particle size of more than 10 mu m in the high-temperature alloy, and has very limited effect on removing the inclusions with small particle size (<10 mu m).
The electron beam refining technology is a technological process for bombarding the surface of a material by using an electron beam with high energy density to melt the material and refine the material, and is widely applied to the fields of refining refractory metals and alloys, preparing high-purity special steel and ultra-clean steel, refining and purifying titanium and titanium alloys and the like. The electron beam has extremely high energy density, has the characteristics of controllable beam current, adjustable beam spot and high automation degree, can generate local ultrahigh temperature (>3000K) after the electron beam with high energy density acts on the melt, combines the characteristics of high vacuum (5 multiplied by 10 < -3 > Pa) and large temperature gradient in the melt, can create the condition for removing the impurities in situ, and provides a new way for deeply removing the small-size impurities.
Disclosure of Invention
According to the proposal, the current method of filtering by adopting foamed ceramics and promoting the floating of inclusions in a molten pool or adsorbing the inclusions floating to the surface is a main way for removing the inclusions in the smelting process; according to the Stokes law of the motion of the inclusions, when the sizes of the inclusions are smaller, the floating speed of the inclusions is slower, the inclusions are difficult to remove in a floating mode, and the filtering of the foamed ceramic only has a good effect on the large-size inclusions; the existing means can successfully remove the inclusions with the particle size of more than 10 mu m in the high-temperature alloy, and provides a method for removing low-density inclusions in the high-temperature alloy by combining melt overheating with foamed ceramic filtration for solving the technical problem that the removal effect of the inclusions with the particle size of less than 10 mu m is very limited. The method mainly comprises the steps of carrying out overheating treatment on the high-temperature alloy melt to dissolve and remove small-size impurities in the melt, and filtering large-size impurities in the alloy by a foamed ceramic filtering method, so that a high-purity high-temperature alloy bar is obtained through casting; by the method, not only can the low-density inclusions in the alloy be completely removed, but also the situation that an inclusion enrichment area at the top of the ingot needs to be cut off after each refining is finished is avoided, and conditions are created for continuous refining of the high-temperature alloy.
The technical means adopted by the invention are as follows:
a method for removing low-density inclusions in a high-temperature alloy by combining melt overheating and foamed ceramic filtering comprises the following steps:
s1, pretreatment of the high-temperature alloy raw material:
s11, the raw material is block-shaped FGH4096 high-temperature alloy;
s12, performing wire cutting processing on the raw materials to a proper size, wherein the raw materials can be placed into a water-cooled copper crucible for refining;
s13, polishing the raw material subjected to wire cutting, and removing a surface oxide layer and a wire cutting trace;
s14, cleaning and drying the polished raw materials for later use;
s2, removing low-density inclusions in the high-temperature alloy by electron beam melt overheating and foamed ceramic filtering:
s21, cleaning the water-cooled copper crucible for electron beam refining: polishing, wiping with alcohol and drying to ensure that the water-cooled copper crucible is clean and pollution-free;
s22, cleaning pollutants on the furnace body and the furnace wall of the electron beam melting furnace, and avoiding the introduction of foreign impurities in the refining process;
s23, placing a proper amount of pretreated raw materials in a water-cooled copper crucible for smelting, and closing a furnace door of the electron beam smelting furnace after the raw materials are determined to be ready and a furnace body is cleaned;
s24, starting electron beam refining equipment, pumping the furnace body and the gun body of the electron gun of the electron beam smelting furnace to a target vacuum state, starting the electron gun on the left side after the target vacuum degree is reached, and preheating;
s25, after preheating, uniformly scanning by using a left-side electron gun to melt the raw materials;
s26, when the alloy is completely melted, carrying out overheating treatment on the melt;
s27, after the melt is subjected to overheating treatment, enabling the overheated high-temperature alloy melt in the water-cooled copper crucible for smelting to flow into the water-cooled copper crucible for solidification through a tilting mechanism;
and S28, turning off the high voltage of the electron gun, increasing the beam current to a certain value, turning off the electron gun after the high voltage is reduced from 30kV to 0kV, and fully cooling the cast ingot in the water-cooled copper crucible for solidification.
And S29, taking out the cast ingot after the electron beam furnace body, the gun body and the alloy ingot are completely cooled, and obtaining the high-purity FGH4096 high-temperature alloy cast ingot.
Further, the specific steps of step S14 are as follows:
and (3) respectively cleaning the polished FGH4096 alloy raw material by using deionized water and alcohol, putting the alloy into a drying box after cleaning, and drying at 30 ℃ for electron beam refining.
Further, the specific steps of step S25 are as follows:
and after preheating, adjusting the beam current of the left electron gun to 0, starting high voltage, increasing the beam current of the left electron gun to 500-600 mA after the high voltage reaches 30kV and is stabilized, and uniformly scanning the FGH4096 high-temperature alloy raw material by using an electron beam spot with the radius of 10mm until the alloy is completely melted.
Further, the specific steps of step S26 are as follows:
after the alloy is completely melted, carrying out overheating treatment on the melt to remove small-size inclusions and ordered atomic groups in the melt, and specifically comprising the following steps: increasing the beam current of the electron beam to 800mA, adjusting the radius of a beam spot of the electron beam to 25mm after reaching the specified beam current, fixing the beam spot at the center of a molten pool, and carrying out melt overheating treatment on the alloy for 20min under the condition so that small-size inclusions in the alloy can be fully dissolved
Further, the specific steps of step S27 are as follows:
after the melt is subjected to overheating treatment, the beam current is rapidly adjusted to 0mA, and the tilting mechanism is started simultaneously, so that the overheated high-temperature alloy melt in the water-cooled copper crucible for smelting flows into the water-cooled copper crucible for solidification through the foamed ceramic filter.
Compared with the prior art, the invention has the following advantages:
1. the method for removing the low-density inclusions in the high-temperature alloy by combining melt overheating and foamed ceramic filtering creatively provides that the electron beam special metallurgy is adopted to realize the in-situ dissolution and removal of the small-size inclusions in the high-temperature alloy, the filtering action of the foamed ceramic is utilized to realize the filtration and removal of the large-size inclusions in the alloy, and the basic principle of removing the inclusions by the electron beam overheating dissolution is that the small-size inclusions in the melt can generate diffusion dissolution reaction under the environment of local ultrahigh temperature and large overheating in the melt; the principle of the foamed ceramic filtration is that when alloy melt flows through the pore channels of the foamed ceramic, large-size impurities can be adsorbed by the pore channels and further retained in the ceramic filter. By the method, low-density inclusions in the high-temperature alloy can be completely removed, an inclusion enrichment area at the top of the ingot needing to be cut off after each refining is finished is avoided, and conditions are created for continuous preparation of high-purity and large-size ingots.
2. According to the method for removing the low-density inclusions in the high-temperature alloy by combining melt overheating and foamed ceramic filtering, on the basis of fully removing volatile impurities in the process of refining the high-temperature alloy by using an electron beam, the diffusion and dissolution reaction of small-size inclusions in the melt is strengthened by using the local overheating of the melt, and the filtering of large-size inclusions in the alloy is realized by using the foamed ceramic filtering method, so that the aim of comprehensively reducing the low-density inclusions in the high-temperature alloy is fulfilled, and the high-purity high-temperature alloy bar is obtained by casting.
In conclusion, the technical scheme of the invention can solve the problem that the current method for removing the impurities in the smelting process is mainly to adopt the foamed ceramic for filtering and promoting the impurities in the molten pool to float upwards or adsorb the impurities floating to the surface; according to the Stokes law of the motion of the inclusions, when the sizes of the inclusions are smaller, the floating speed of the inclusions is slower, the inclusions are difficult to remove in a floating mode, and the filtering of the foamed ceramic only has a good effect on the large-size inclusions; the existing method can successfully remove the inclusions with the particle size of more than 10 mu m in the high-temperature alloy, and has very limited removal effect on the inclusions with small particle size (<10 mu m).
Based on the reasons, the method can be widely popularized in the fields of removing low-density inclusions in the high-temperature alloy and the like.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic view of the superheating treatment of a superalloy melt according to the present invention.
FIG. 2 is a schematic diagram of the inclusion filtering of the high temperature alloy melt ceramic foam of the present invention.
In the figure: 1. an oil diffusion pump; 2. a valve; 3. a mechanical pump; 4. local overheating areas of the melt; 5. an alloy melt; 6. water-cooling the copper crucible; 7. a tilting mechanism; 8. cooling water; 9. an electron gun; 10. an electron beam; 11. a ceramic foam filter; 12. a roots pump.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. Any specific values in all examples shown and discussed herein are to be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
As shown in the figure, the invention provides a method for removing low-density inclusions in a high-temperature alloy by combining melt overheating with foamed ceramic filtering, which comprises the following steps:
pretreatment of high-temperature alloy raw materials
1. The block-shaped FGH4096 high-temperature alloy is used as a raw material, and the FGH4096 alloy is subjected to wire cutting processing to an appropriate size so as to be placed in a water-cooled copper crucible for refining. And polishing the block raw material subjected to wire cutting, and removing a surface oxidation layer and a wire cutting trace.
2. And (3) respectively cleaning the polished FGH4096 alloy raw material by using deionized water and alcohol, putting the alloy into a drying box after cleaning, and drying at 30 ℃ for electron beam refining.
Secondly, removing low-density inclusions in the high-temperature alloy by electron beam melt overheating and foamed ceramic filtering
1. And cleaning (polishing, alcohol wiping and drying) the water-cooled copper crucible for electron beam refining to ensure that the water-cooled copper crucible is clean and pollution-free.
2. Cleaning the furnace body and the furnace wall of the electron beam melting furnace, and avoiding the introduction of foreign impurities in the refining process.
3. Placing a proper amount of pretreated FGH4096 alloy raw materials in a water-cooled copper crucible for smelting (namely a water-cooled copper crucible for refining), closing a furnace door of the electron beam smelting furnace after the readiness is determined and a furnace body is cleaned.
4. And starting electron beam refining equipment, pumping the furnace body of the electron beam smelting furnace and the gun body of the electron gun to a target vacuum state, starting the electron gun on the left side after the target vacuum degree is reached, and preheating.
5. And after preheating, adjusting the beam current of the left electron gun to 0, starting high voltage, increasing the beam current of the left electron gun to 500-600 mA after the high voltage reaches 30kV and is stabilized, and uniformly scanning the FGH4096 high-temperature alloy raw material by using an electron beam spot with the radius of 10mm until the alloy is completely melted.
6. After the alloy is completely melted, carrying out overheating treatment on the melt to remove small-size inclusions and ordered atomic groups in the melt, and specifically comprising the following steps: increasing the beam current of the electron beam to 800mA, adjusting the radius of a beam spot of the electron beam to 25mm after reaching the specified beam current, fixing the beam spot at the center of a molten pool, and carrying out melt overheating treatment on the alloy for 20min under the condition so as to fully dissolve small-size inclusions (figure 1).
7. After the melt is subjected to overheating treatment, the beam current is rapidly adjusted to 0mA, and the tilting mechanism is started simultaneously, so that the overheated high-temperature alloy melt in the water-cooled copper crucible for smelting flows into the water-cooled copper crucible for solidification through the foamed ceramic filter.
8. And (3) closing the high voltage of the electron gun, increasing the beam current to a certain value, closing the electron gun after the high voltage is reduced from 30kV to 0kV, and fully cooling the cast ingot in a water-cooled copper crucible for solidification.
9. And taking out the cast ingot after the electron beam furnace body, the gun body and the alloy ingot are completely cooled, thereby obtaining the high-purity FGH4096 high-temperature alloy cast ingot.
FIG. 1 is a schematic diagram showing the overheating treatment of the superalloy melt according to the present invention, and FIG. 2 is a schematic diagram showing the inclusion filtering of the superalloy melt ceramic foam according to the present invention. The invention adopts the equipment shown in figures 1 and 2 to remove low-density inclusions in the high-temperature alloy. The electron gun 9 is fixed at two side angles at the top of the electron beam melting furnace, the water-cooled copper crucible for melting 6 is placed in the electron beam melting furnace through the tilting mechanism 7, the water-cooled copper crucible for solidification 6 is placed at the bottom of the electron beam melting furnace, cooling water 8 is introduced, the water-cooled copper crucible for melting 6 is tilted through the tilting mechanism 7, and the overheated high-temperature alloy melt refined in the water-cooled copper crucible for melting 6 flows into the water-cooled copper crucible for solidification 6 through the foamed ceramic filter 11. The DD406 alloy raw material is placed in a water-cooled copper crucible 6 for melting and is in the scanning range of an electron beam 10. The oil diffusion pump 1 is adjacent to the mechanical pump 3, and the communication relationship between the oil diffusion pump 1 and the mechanical pump is controlled by a valve 2; the roots pump 12 is adjacent to the furnace body mechanical pump 3, and the two are connected together. The alloy melt 5 is a molten metal raw material in a water-cooled copper crucible 6 and forms a local overheating zone 4 of the melt after melting.
On the basis of fully removing volatile impurities in the process of refining the high-temperature alloy by using the electron beams, the method of the invention utilizes local overheating of the melt to strengthen the diffusion and dissolution reaction of small-size impurities in the melt, and utilizes a method of filtering foamed ceramics to filter large-size impurities in the alloy, thereby achieving the purpose of comprehensively reducing low-density impurities in the high-temperature alloy. The in-situ removal method avoids the need of cutting off the impurity enrichment area at the top of the ingot after each refining is finished, and creates conditions for continuous preparation of high-purity and large-size ingots.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. A method for removing low-density inclusions in high-temperature alloy by combining melt overheating and foamed ceramic filtering is characterized in that electron beam overheating treatment is carried out on high-temperature alloy melt to dissolve and remove small-size inclusions in the melt, filtering of large-size inclusions in the alloy is achieved by the foamed ceramic filtering method, high-purity high-temperature alloy bars are obtained through casting, comprehensive removal of the low-density inclusions in the alloy is achieved, the situation that an inclusion enrichment area at the top of an ingot is cut off after each refining is avoided, and conditions are created for continuous refining of the high-temperature alloy; the basic principle of removing inclusions by electron beam overheating dissolution is that small-size inclusions in a melt can generate diffusion dissolution reaction in the local ultrahigh temperature and large overheating environment in the melt; the principle of the foamed ceramic filtration is that when alloy melt flows through the pore channels of the foamed ceramic, large-size impurities can be adsorbed by the pore channels and further retained in the ceramic filter;
the method comprises the following steps:
s1, pretreatment of the high-temperature alloy raw material:
s11, the raw material is block-shaped FGH4096 high-temperature alloy;
s12, performing wire cutting processing on the raw materials to a proper size, wherein the raw materials can be placed into a water-cooled copper crucible for refining;
s13, polishing the raw material subjected to wire cutting, and removing a surface oxide layer and a wire cutting trace;
s14, cleaning and drying the polished raw materials for later use;
s2, removing low-density inclusions in the high-temperature alloy by electron beam melt overheating and foamed ceramic filtering:
s21, cleaning the water-cooled copper crucible for electron beam refining: polishing, wiping with alcohol and drying to ensure that the water-cooled copper crucible is clean and pollution-free;
s22, cleaning pollutants on the furnace body and the furnace wall of the electron beam melting furnace, and avoiding the introduction of foreign impurities in the refining process;
s23, placing a proper amount of pretreated raw materials in a water-cooled copper crucible for smelting, and closing a furnace door of the electron beam smelting furnace after the raw materials are determined to be ready and a furnace body is cleaned;
s24, starting electron beam refining equipment, pumping the furnace body and the gun body of the electron gun of the electron beam smelting furnace to a target vacuum state, starting the electron gun on the left side after the target vacuum degree is reached, and preheating;
s25, after preheating, uniformly scanning by using a left-side electron gun to melt the raw materials;
s26, when the alloy is completely melted, carrying out overheating treatment on the melt;
s27, after the melt is subjected to overheating treatment, enabling the overheated high-temperature alloy melt in the water-cooled copper crucible for smelting to flow into the water-cooled copper crucible for solidification through a tilting mechanism;
s28, turning off the high voltage of the electron gun, increasing the beam current to a certain value, turning off the electron gun after the high voltage is reduced from 30kV to 0kV, and fully cooling the cast ingot in a water-cooled copper crucible for solidification;
and S29, taking out the cast ingot after the electron beam furnace body, the gun body and the alloy ingot are completely cooled, and obtaining the high-purity FGH4096 high-temperature alloy cast ingot.
2. The method for removing low-density inclusions in a superalloy by combining melt superheating and ceramic foam filtering according to claim 1, wherein the specific steps of the step S14 are as follows:
and (3) respectively cleaning the polished FGH4096 alloy raw material by using deionized water and alcohol, putting the alloy into a drying box after cleaning, and drying at 30 ℃ for electron beam refining.
3. The method for removing low-density inclusions in a superalloy by combining melt superheating and ceramic foam filtering according to claim 1, wherein the specific steps of the step S25 are as follows:
and after preheating, adjusting the beam current of the left electron gun to 0, starting high voltage, increasing the beam current of the left electron gun to 500-600 mA after the high voltage reaches 30kV and is stabilized, and uniformly scanning the FGH4096 high-temperature alloy raw material by using an electron beam spot with the radius of 10mm until the alloy is completely melted.
4. The method for removing low-density inclusions in a superalloy by combining melt superheating and ceramic foam filtering according to claim 1, wherein the specific steps of the step S26 are as follows:
after the alloy is completely melted, carrying out overheating treatment on the melt to remove small-size inclusions and ordered atomic groups in the melt, and specifically comprising the following steps: increasing the beam current of the electron beam to 800mA, adjusting the radius of a beam spot of the electron beam to 25mm after reaching the specified beam current, fixing the beam spot at the center of a molten pool, and carrying out melt overheating treatment on the alloy for 20min under the condition so as to fully dissolve small-size inclusions in the alloy.
5. The method for removing low-density inclusions in a superalloy by combining melt superheating and ceramic foam filtering according to claim 1, wherein the specific steps of the step S27 are as follows:
after the melt is subjected to overheating treatment, the beam current is rapidly adjusted to 0mA, and the tilting mechanism is started simultaneously, so that the overheated high-temperature alloy melt in the water-cooled copper crucible for smelting flows into the water-cooled copper crucible for solidification through the foamed ceramic filter.
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