CN112095029A - Ti3Ni intermediate alloy and preparation method thereof - Google Patents

Ti3Ni intermediate alloy and preparation method thereof Download PDF

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Publication number
CN112095029A
CN112095029A CN202010803516.5A CN202010803516A CN112095029A CN 112095029 A CN112095029 A CN 112095029A CN 202010803516 A CN202010803516 A CN 202010803516A CN 112095029 A CN112095029 A CN 112095029A
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electron beam
melting
preparation
intermediate alloy
pumping
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谭毅
郑俊
李鹏廷
王轶农
游小刚
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Dalian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium

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Abstract

The present invention provides a Ti3The Ni intermediate alloy and the preparation method thereof comprise the following steps: weighing Ti3The Ni intermediate alloy comprises the following raw materials: sponge titanium and electrolytic nickel, and then cutting the weighed blocky electrolytic nickel raw material into blocks with proper sizes; polishing the surface of the cut blocky electrolytic nickel raw material, and then respectively soaking the polished electrolytic nickel and the weighed sponge titanium in alcohol, and cleaning the electrolytic nickel and the weighed sponge titanium by using an ultrasonic cleaning machine for later use; putting the cleaned raw materials into a water-cooled copper crucible of an electron beam melting furnace; carrying out vacuum pre-pumping and gas washing on the electron beam smelting furnace, and then carrying out vacuum pre-pumping and high vacuum pumping to reach the high vacuum standard; carrying out electron beam melting on the raw material in the water-cooled copper crucible, and then directly lowering the beam to obtain Ti3A Ni master alloy. The inventionTi prepared by electron beam vacuum melting3The Ni intermediate alloy has lower impurity content, and can effectively avoid the influence of oxygen and nitrogen elements in the raw materials and impurities thereof on the performance of the nickel-based high-temperature alloy.

Description

Ti3Ni intermediate alloy and preparation method thereof
Technical Field
The invention relates to a preparation method of an alloy, in particular to Ti3Ni intermediate alloy and a preparation method thereof.
Background
The nickel-based high-temperature alloy has good high-temperature strength and high-temperature creep property, excellent corrosion resistance and abrasion resistance, and good structure stability and process performance, and is widely applied to the industrial fields of aerospace, chemical metallurgy, energy power stations, transportation and the like. Titanium is added into the nickel-based high-temperature alloy, Ti plays an important role in improving the performance of the nickel-based high-temperature alloy as an important strengthening element, about 10 percent of titanium enters a gamma solid solution to play a role in solid solution strengthening, about 90 percent of titanium enters a gamma 'phase, and under the condition of a certain content of aluminum element, the quantity of the gamma' phase is increased along with the increase of the content of the titanium, so that the room-temperature strength and the high-temperature strength of the alloy are increased. If titanium is directly added into the melt in a simple substance form, the adding temperature needs to be increased, the smelting time needs to be prolonged, or the burning loss in the adding process is increased, the actual yield is difficult to ensure, so that the multiple adjustment of components in front of the furnace is caused, and the production efficiency of the product is influenced. Because the melting point of the pure titanium element is higher, the pure titanium element can not be melted rapidly in the melting temperature range of the nickel-based superalloy, but is slowly dissolved into the nickel-based superalloy melt in an alloying manner. In the process, if a certain amount of gaseous impurity elements such as oxygen and nitrogen exist in the nickel-base superalloy melt, oxide, nitride and other inclusions can be formed rapidly. Moreover, these inclusions have a high melting point and are difficult to decompose once formed, and thus remain in the nickel-base superalloy, affecting its properties. Due to Ti3The Ni intermediate alloy can effectively reduce the nickel-based high temperature and the melting temperature of gold and shorten the mixing time of the nickel-based high temperature and the gold, so that the Ni intermediate alloy is an essential material.
Due to the composition of the intermediate alloyRequired accuracy of classification, Ti3Ni is used as intermediate alloy, a scheme rich in titanium is selected, and the intermediate alloy has high requirement on purity, however, at present, no one has prepared Ti by smelting3The Ni master alloy was studied.
The electron beam refining is a process for further refining and purifying materials prepared by the existing method, and the principle of the electron beam refining is that an electron beam with high energy density is utilized to bombard a base metal to generate heat energy to melt the materials, a molten pool is kept at a higher temperature by adjusting power and a melting rate, and the temperature rise speed in the whole process is higher. Vacuum degree of smelting chamber is less than 5X 10-2Pa, the content of air is very low, and the alloy melt fully generates degassing reaction in a high-temperature and high-vacuum environment, so that the removal of impurities and inclusions and the accurate control of components are facilitated; the use of the water-cooled copper crucible can not only avoid the pollution of crucible materials and effectively reduce the cost of refining and purification, but also obtain low segregation high-temperature alloy due to the faster cooling rate.
Disclosure of Invention
According to the above-mentioned requirements for the accuracy of its composition, Ti is proposed3Ni is used as intermediate alloy, a scheme rich in titanium is selected, and the intermediate alloy has high requirement on purity, however, at present, no one has prepared Ti by smelting3The technical problem of research on Ni intermediate alloy is solved, and Ti is provided3Ni intermediate alloy and a preparation method thereof. The invention mainly utilizes electron beam vacuum melting to prepare Ti3The Ni intermediate alloy can effectively reduce oxygen, nitrogen and impurities in the added raw materials, so that the obtained Ti3The Ni intermediate alloy has lower impurity content, thereby avoiding the influence of oxygen and nitrogen elements in the raw materials and the inclusion thereof on the performance of the nickel-based high-temperature alloy. Prepared Ti3The Ni intermediate alloy has low melting point, the melting temperature is 942 ℃, and in the melting temperature range of the nickel-based superalloy, the Ni intermediate alloy can be quickly melted and fully mixed with the nickel-based superalloy melt to inhibit the formation of inclusions such as oxides, nitrides and the like in the nickel-based superalloy, and simultaneously, because the electron beam melting temperature and the vacuum degree are higher, the Ti intermediate alloy can be improved3Purity of the Ni master alloy.
The technical means adopted by the invention are as follows:
ti3The preparation method of the Ni intermediate alloy comprises the following steps:
s1, weighing Ti3The Ni intermediate alloy comprises the following raw materials: sponge titanium and electrolytic nickel, and then cutting the weighed blocky electrolytic nickel raw material into blocks with proper sizes;
s2, polishing the surface of the cut blocky electrolytic nickel raw material, and then respectively soaking the polished electrolytic nickel and the weighed sponge titanium in alcohol, and cleaning the electrolytic nickel and the weighed sponge titanium by using an ultrasonic cleaning machine for later use;
s3, placing the cleaned raw materials in a water-cooled copper crucible of an electron beam melting furnace;
s4, carrying out vacuum pre-pumping and gas washing on the electron beam melting furnace, and then carrying out vacuum pre-pumping and high vacuum pumping to reach the high vacuum standard;
s5, carrying out electron beam melting on the raw material in the water-cooled copper crucible, and then directly lowering the beam to obtain Ti3A Ni master alloy.
Further, in the step S1, Ti3The Ni intermediate alloy is prepared from the following raw materials in parts by mass:
ni: 457 g;
ti: 1207 g;
the purity of the titanium sponge is 99.7%; the electrolytic nickel is cuboid block with purity of 99.98%.
Further, the specific steps of step S3 are as follows:
polishing the water-cooled copper crucible for refining the electron beam smelting furnace and wiping the water-cooled copper crucible with alcohol to ensure that the water-cooled copper crucible is clean and pollution-free, placing all cleaned raw materials into the cleaned water-cooled copper crucible, and placing the blocky electrolytic nickel above the sponge titanium.
Further, the specific steps of step S4 are as follows:
closing the furnace door of the electron beam melting furnace for vacuum pre-pumping, stopping vacuum pumping and introducing argon into the melting chamber when the vacuum degree of the melting chamber of the electron beam melting furnace is less than or equal to 10Pa, performing at least one gas washing on the melting chamber, and then performing vacuum pre-pumping againAfter the vacuum pre-pumping is finished, the electron beam melting furnace is vacuumized to a high degree, so that the vacuum degree of a melting chamber of the electron beam melting furnace is less than 5 multiplied by 10-2Pa, vacuum degree of electron gun body less than 5 × 10-3Pa, reaching the high vacuum standard.
Further, the specific steps of step S5 are as follows:
s41, after the high vacuum standard is reached, preheating a filament of the electron beam melting furnace, and then starting to carry out electron beam melting;
s42, adjusting the beam current of the electron gun to 0 after the filament is preheated, starting high voltage, slowly increasing the beam current of the electron gun to initial beam current parameters of a determined melting process at 2-3 mA/S after the high voltage is stabilized, then sequentially carrying out the melting process and the refining process, and directly reducing the beam current after the melting preparation is finished;
s43, closing the high voltage of the electron gun, increasing the beam current to 60mA to enable the high voltage value to be 0, and then closing the electron gun;
s44, cooling the furnace body of the electron beam melting furnace and the gun body of the electron gun for 3 hours, and taking out Ti prepared by electron beam melting3Ni intermediate alloy to obtain Ti3A Ni master alloy.
Further, in step S42, the process parameters of the electron gun beam in the melting process are 150mA, 200mA, and 300 mA.
Further, the electron beam spot size of the melting process is 10 × 10.
Further, in the step S42, the process parameters of the electron gun beam in the refining process are 350mA and 400 mA.
Further, the electron beam spot size of the refining process was 10 × 10 and 5 × 5.
The invention also provides a Ti as defined above3Ti prepared by Ni intermediate alloy preparation method3Ni master alloy, said Ti3The Ni intermediate alloy consists of the following elements in percentage by mass:
26.6% Ni and 73.3% Ti;
the Ti3The melting temperature of the Ni master alloy is 942 ℃.
Compared with the prior art, the invention has the following advantages:
1. ti provided by the invention3Ni intermediate alloy and preparation method thereof, and Ti prepared by electron beam vacuum melting3The Ni intermediate alloy can effectively reduce oxygen, nitrogen and impurities in the added raw materials, so that the obtained intermediate alloy has lower impurity content, and the influence of the oxygen, nitrogen and impurities in the raw materials on the performance of the nickel-based high-temperature alloy is avoided.
2. Ti provided by the invention3The Ni intermediate alloy and the preparation method thereof are characterized in that the prepared raw materials are blocky electrolytic nickel and sponge titanium, and the blocky electrolytic nickel is placed on the sponge titanium in a crucible material placing mode; prepared Ti3The Ni intermediate alloy has low melting point, the melting temperature is 942 ℃, and in the melting temperature range of the nickel-based superalloy, the Ni intermediate alloy can be quickly melted and fully mixed with the nickel-based superalloy melt to inhibit the formation of inclusions such as oxides, nitrides and the like in the nickel-based superalloy, and simultaneously, because the electron beam melting temperature and the vacuum degree are higher, the Ti intermediate alloy can be improved3Purity of the Ni master alloy.
In conclusion, the technical scheme of the invention can solve the problem that Ti has requirements on the component accuracy of the intermediate alloy3Ni is used as intermediate alloy, a scheme rich in titanium is selected, and the intermediate alloy has high requirement on purity, however, at present, no one has prepared Ti by smelting3The research of Ni intermediate alloy is carried out.
Based on the reasons, the invention can be widely popularized in the fields of alloy preparation 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 illustration of electron beam melting (start of melting) in an embodiment of the present invention.
FIG. 2 is a schematic representation of electron beam melting (start of refining) in an embodiment of the present invention.
FIG. 3 is a schematic view of an ingot produced by melting in an embodiment of the present invention.
In the figure: 1. an electron gun; 2. electron beam scanning range; 3. electrolyzing nickel; 4. a furnace shell; 5. water-cooling the copper crucible; 6. circulating cooling water; 7. a crucible support; 8. titanium sponge; 9. a molten bath.
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.
The invention provides a Ti3The preparation method of the Ni intermediate alloy comprises the following steps:
firstly, preparing raw materials
1. Cutting of
Sponge titanium with the purity of 99.7 percent and electrolytic nickel with the purity of 99.98 percent are prepared as raw materials, 457g of Ni and 1207g of Ti are weighed, and the weighed blocky electrolytic nickel raw materials are cut into blocks with proper sizes, wherein the electrolytic nickel is cuboid blocks.
2. Raw material treatment
Before smelting, the surface of the cut blocky electrolytic nickel raw material is polished to remove linear cutting marks, oil stains, impurities and defects on the surface of the raw material. And then, soaking the polished electrolytic nickel and the weighed sponge titanium in alcohol respectively, and cleaning the raw materials by using an ultrasonic cleaning machine.
3. Discharging
And (3) putting the cleaned raw materials of the electrolytic nickel and the sponge titanium into a water-cooled copper crucible of an electron beam melting furnace (the electrolytic nickel block is put above the sponge titanium), and polishing the water-cooled copper crucible for refining the electron beam melting furnace and wiping the water-cooled copper crucible with alcohol before discharging so as to ensure that the water-cooled copper crucible is clean and pollution-free.
Second, electron beam melting and refining
1. And after the feeding is finished, closing the furnace door for vacuum pre-pumping. When the vacuum degree of the smelting chamber is less than or equal to 10Pa, stopping vacuumizing, introducing argon into the smelting chamber, and performing gas washing (which can be performed for multiple times) on the smelting chamber. After thatAnd performing vacuum pre-pumping again, and performing high vacuum pumping on the equipment after the vacuum pre-pumping is finished. Before the smelting operation is carried out, the requirements of equipment vacuum conditions are met: vacuum degree of smelting chamber is less than 5X 10-2Pa, vacuum degree of electron gun body less than 5 × 10-3Pa。
2. After the high vacuum standard is reached, a filament of the electron beam melting furnace is preheated, after the preheating is finished, the beam current of an electron gun is adjusted to 0, high pressure is started, after the high pressure is stabilized, the beam current of the electron gun is slowly increased to the initial beam current parameter of a determined melting process at the rate of 2-3 mA/s, then the melting process and the refining process are sequentially carried out, and the process parameters of the melting preparation process are shown in Table 1. And after the smelting preparation is finished, directly reducing the beam.
The schematic diagram of the melting process is shown in figure 1, and the schematic diagram of the refining process is shown in figure 2. At the beginning of melting, the electron gun 1 is fixed at two side angles at the top of a smelting furnace shell 4 of the electron beam smelting furnace, the water-cooled copper crucible 5 is placed in the smelting furnace shell 4 through a crucible support 7, circulating cooling water 6 is introduced into the water-cooled copper crucible 5, and raw materials of electrolytic nickel 3 and sponge titanium 8 are added into the water-cooled copper crucible 5 and are within an electron beam scanning range 2. When the refining process is carried out, the electron beam bombards the base metal to generate heat energy to melt the electrolytic nickel 3 and the sponge titanium 8 raw materials to form a molten pool 9.
TABLE 1 Process parameters of the smelting preparation
Figure BDA0002628263960000071
3. And closing the high voltage of the electron gun, reducing the beam current to 60mA to enable the high voltage value to be 0, and then closing the electron gun.
4. Taking out Ti prepared by electron beam melting after the furnace body and the gun body are cooled for 3 hours3Ni intermediate alloy to obtain Ti3A Ni master alloy.
Ti obtained by the method of the present invention3The Ni intermediate alloy ingot can effectively control the macrosegregation of the Ni intermediate alloy ingot while reducing the contents of oxygen, nitrogen and impurities thereof in the nickel-based high-temperature alloy. Obtained Ti3The Ni intermediate alloy has low melting point, the melting temperature is 942 ℃, and the Ni intermediate alloy can be quickly melted and fused within the melting temperature range of the nickel-based superalloyFully mixed with the nickel-based high-temperature alloy melt, the formation of inclusions such as oxides, nitrides and the like in the nickel-based high-temperature alloy is inhibited, and meanwhile, the Ti can be improved due to higher temperature and vacuum degree of electron beam melting3Purity of the Ni master alloy. In the preparation of Ti3After sampling at different positions on the Ni intermediate alloy, XRF detection is carried out, and the contents of titanium and nickel are 73.3 percent and 26.6 percent respectively. Fig. 3 shows an ingot obtained by melting.
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 (10)

1. Ti3The preparation method of the Ni intermediate alloy is characterized by comprising the following steps of:
s1, weighing Ti3The Ni intermediate alloy comprises the following raw materials: sponge titanium and electrolytic nickel, and then cutting the weighed blocky electrolytic nickel raw material into blocks with proper sizes;
s2, polishing the surface of the cut blocky electrolytic nickel raw material, and then respectively soaking the polished electrolytic nickel and the weighed sponge titanium in alcohol, and cleaning the electrolytic nickel and the weighed sponge titanium by using an ultrasonic cleaning machine for later use;
s3, placing the cleaned raw materials in a water-cooled copper crucible of an electron beam melting furnace;
s4, carrying out vacuum pre-pumping and gas washing on the electron beam melting furnace, and then carrying out vacuum pre-pumping and high vacuum pumping to reach the high vacuum standard;
s5, carrying out electron beam melting on the raw material in the water-cooled copper crucible, and then directly lowering the beam to obtain Ti3A Ni master alloy.
2. According to claimThe Ti as set forth in claim 13The method for preparing the Ni master alloy is characterized in that in the step S1, Ti3The Ni intermediate alloy is prepared from the following raw materials in parts by mass:
ni: 457 g;
ti: 1207 g;
the purity of the titanium sponge is 99.7%; the electrolytic nickel is cuboid block with purity of 99.98%.
3. The Ti of claim 13The preparation method of the Ni master alloy is characterized in that the specific steps of the step S3 are as follows:
polishing the water-cooled copper crucible for refining the electron beam smelting furnace and wiping the water-cooled copper crucible with alcohol to ensure that the water-cooled copper crucible is clean and pollution-free, placing all cleaned raw materials into the cleaned water-cooled copper crucible, and placing the blocky electrolytic nickel above the sponge titanium.
4. The Ti of claim 13The preparation method of the Ni master alloy is characterized in that the specific steps of the step S4 are as follows:
closing the furnace door of the electron beam melting furnace for vacuum pre-pumping, stopping vacuum pumping and introducing argon into the melting chamber when the vacuum degree of the melting chamber of the electron beam melting furnace is less than or equal to 10Pa, performing at least one gas washing on the melting chamber, then performing vacuum pre-pumping again, and performing high vacuum pumping on the electron beam melting furnace after the vacuum pre-pumping is finished so that the vacuum degree of the melting chamber of the electron beam melting furnace is less than 5 multiplied by 10-2Pa, vacuum degree of electron gun body less than 5 × 10-3Pa, reaching the high vacuum standard.
5. The Ti of claim 13The preparation method of the Ni master alloy is characterized in that the specific steps of the step S5 are as follows:
s41, after the high vacuum standard is reached, preheating a filament of the electron beam melting furnace, and then starting to carry out electron beam melting;
s42, adjusting the beam current of the electron gun to 0 after the filament is preheated, starting high voltage, slowly increasing the beam current of the electron gun to initial beam current parameters of a determined melting process at 2-3 mA/S after the high voltage is stabilized, then sequentially carrying out the melting process and the refining process, and directly reducing the beam current after the melting preparation is finished;
s43, closing the high voltage of the electron gun, increasing the beam current to 60mA to enable the high voltage value to be 0, and then closing the electron gun;
s44, cooling the furnace body of the electron beam melting furnace and the gun body of the electron gun for 3 hours, and taking out Ti prepared by electron beam melting3Ni intermediate alloy to obtain Ti3A Ni master alloy.
6. The Ti of claim 53The preparation method of the Ni master alloy is characterized in that in the step S42, the process parameters of electron gun beam current in the melting process are 150mA, 200mA and 300 mA.
7. The Ti of claim 63The preparation method of the Ni intermediate alloy is characterized in that the electron beam spot size of the melting process is 10 multiplied by 10.
8. The Ti of claim 53The preparation method of the Ni master alloy is characterized in that in the step S42, the process parameters of electron gun beam current in the refining process are 350mA and 400 mA.
9. The Ti of claim 83The preparation method of the Ni master alloy is characterized in that the electron beam spot size of the refining process is 10 x 10 and 5 x 5.
10. A Ti according to any of claims 1-93Ti prepared by Ni intermediate alloy preparation method3Ni master alloy, characterized in that, the Ti3The Ni intermediate alloy consists of the following elements in percentage by mass:
26.6% Ni and 73.3% Ti;
the Ti3The melting temperature of the Ni master alloy is 942 ℃.
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CN116790924A (en) * 2023-08-25 2023-09-22 北京理工大学 Method for preparing refractory high-entropy alloy by remelting return materials through electron beam melting
CN116790924B (en) * 2023-08-25 2023-11-17 北京理工大学 Method for preparing refractory high-entropy alloy by remelting return materials through electron beam melting

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