CN117926020A - High-homogeneity nickel-based superalloy and preparation method thereof - Google Patents
High-homogeneity nickel-based superalloy and preparation method thereof Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 52
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000003723 Smelting Methods 0.000 claims abstract description 171
- 238000000034 method Methods 0.000 claims abstract description 82
- 239000011261 inert gas Substances 0.000 claims abstract description 47
- 230000008569 process Effects 0.000 claims abstract description 43
- 230000002829 reductive effect Effects 0.000 claims abstract description 37
- 238000007789 sealing Methods 0.000 claims abstract description 36
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims description 74
- 230000008018 melting Effects 0.000 claims description 74
- 230000005540 biological transmission Effects 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 3
- 238000005204 segregation Methods 0.000 abstract description 32
- 230000007547 defect Effects 0.000 abstract description 27
- 206010027146 Melanoderma Diseases 0.000 abstract description 20
- 238000000265 homogenisation Methods 0.000 abstract description 8
- 229910045601 alloy Inorganic materials 0.000 description 31
- 239000000956 alloy Substances 0.000 description 31
- 239000001307 helium Substances 0.000 description 26
- 229910052734 helium Inorganic materials 0.000 description 26
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 19
- 238000007711 solidification Methods 0.000 description 16
- 230000008023 solidification Effects 0.000 description 16
- 230000000694 effects Effects 0.000 description 14
- 238000004321 preservation Methods 0.000 description 11
- 238000010891 electric arc Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 230000006698 induction Effects 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 241001062472 Stokellia anisodon Species 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003031 feeding effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
The invention discloses a high-homogeneity nickel-based superalloy and a preparation method thereof, and belongs to the field of superalloy manufacturing. The preparation method comprises the following steps: preparing a nickel-based superalloy consumable ingot by a vacuum consumable remelting smelting process, wherein the vacuum consumable remelting smelting process comprises the following steps of: in the steady-state smelting stage, inert gas is filled into the consumable furnace, the inert gas is controlled by pressure, the smelting speed is kept stable in the early stage of steady-state smelting, and the smelting speed starts to be reduced in the later stage of steady-state smelting; in the heat-sealing top stage, inert gas adopts flow control; and after the heat capping stage is finished, discharging the nickel-based superalloy from the furnace after vacuum cooling, and obtaining the nickel-based superalloy consumable ingot. The method provided by the invention can relieve the black spot segregation defect of the consumable nickel-base superalloy ingot, and prepare a high-homogenization nickel-base superalloy ingot product.
Description
Technical Field
The invention belongs to the field of high-temperature alloy manufacturing, and particularly relates to a method for preparing a low-segregation and high-homogeneity nickel-based high-temperature alloy by adopting a vacuum consumable remelting smelting process and a product.
Background
The high-temperature alloy is a metal material based on iron, nickel and cobalt, can work for a long time under the action of high temperature above 600 ℃ and certain stress, and has the comprehensive properties of excellent high-temperature strength, good oxidation resistance, hot corrosion resistance, good fatigue property, fracture toughness and the like, and is also called as super alloy.
The high-temperature alloy is a key core material in the fields of electric power, aerospace, national defense science and technology and the like. At present, most high-quality high-temperature alloys are smelted by adopting a duplex or triple smelting process. In the multiple smelting process, vacuum consumable remelting smelting is an important secondary smelting process for producing high-quality high-temperature alloy. However, the high-temperature alloy has high alloying degree and complex components, so that the high-temperature alloy is easy to generate uneven components in the vacuum consumable smelting process, and is easy to generate a typical segregation defect of black spots. The defect can not be eliminated through a homogenization process, the toughness, yield strength and durability of the material are obviously reduced, the material is scrapped, and the product quality and yield are seriously affected. Therefore, the black spot segregation defect of the high-temperature alloy vacuum consumable ingot is alleviated, and the prepared high-temperature alloy ingot with high homogenization plays an important role in manufacturing and developing high-quality high-temperature alloy.
The current research shows that the head and tail of the high-temperature alloy vacuum consumable ingot, especially the head (namely the riser end) is easy to generate black spot segregation, and the main reason is that the local solidification time of the alloy at the head of the ingot is prolonged and the solidification segregation of the alloy is increased along with the weakening of the cooling effect of the bottom plate of the crystallizer when smelting. In the smelting process, the formation of consumable cast ingot black spots is mainly influenced by various factors such as smelting speed, helium pressure and the like. At present, the related technology and the invention develop partial research work on improving the problem of black spot segregation of the vacuum consumable ingot, but the research work and the obtained effect have certain defects.
Chinese patent CN 115896471A proposes: in the consumable smelting process, when 1000 kg-1600 kg of consumable electrode weight is remained, 200 Pa-800 Pa of argon gas is filled from the upper part of the crucible to increase heat conduction in a furnace chamber at the later stage of smelting, so that segregation defects of the head of the TC17 cast ingot are relieved. It should be noted that the argon gas pressure charged into the upper part of the cast ingot is high, which can obviously influence the vacuum degree of consumable smelting and the stability of electric arc, further influence the stability of a molten pool and a solidification structure, and increase the risk that splash inclusions around the wall of a crystallizer are swept into the molten pool by the electric arc to pollute the molten pool.
Chinese patent CN 116287744A proposes: the compressed low-temperature liquid helium with the purity of more than 99.999 percent is adopted to replace the common bottled helium, and the high-flow helium is adopted to properly break the liquid seal of the liquid molten pool to enhance the cooling effect of the molten pool, and meanwhile, the heat input is reduced by adopting a mode of gradually reducing the smelting melting speed in a steady-state stage to lighten the black spots of the consumable ingot. The method has the following problems: the use of high flow helium breaks the liquid seal of the liquid bath and reduces the vacuum degree and the stability of the electric arc and the bath in the smelting process. The instability of the arc and bath increases the probability of black spots, and also increases the risk of the formation of splashes of the walls of the ingot or of the crown being swept by the arc, which falls into the metal bath, increasing the risk of contamination of the bath. Meanwhile, the smelting speed of the patent is gradually reduced in the whole steady-state smelting stage, so that the production efficiency is affected, and the smelting period is prolonged. After the melting speed is gradually reduced in the whole steady-state stage, the surface quality of the cast ingot in the whole steady-state stage can be obviously reduced, the peeling amount of the cast ingot is increased, and the yield is reduced.
Likewise, none of other published technical documents effectively solves the segregation problem of the vacuum consumable ingot and does not affect the stability of the smelting process and the quality of the solidified ingot.
Disclosure of Invention
In order to overcome the defects in the prior art and solve the problem of black spot segregation of a high-temperature alloy vacuum consumable ingot, a high-homogenization high-temperature alloy ingot is prepared, and the technical scheme of the invention is as follows:
in one aspect, the invention provides a method for preparing a high-homogeneity nickel-base superalloy, comprising: preparing a nickel-based superalloy consumable ingot by a vacuum consumable remelting smelting process, wherein the vacuum consumable remelting smelting process comprises an arcing stage, a steady-state smelting stage and a heat-sealing top stage, and the vacuum consumable remelting smelting process comprises the following steps of:
In the arcing stage, the current is controlled to be 4.0-8.0 kA, and the voltage is controlled to be 22.0-24.0V;
In the steady-state smelting stage, inert gas is filled into the consumable furnace, the inert gas is controlled by pressure, the smelting speed is kept stable in the early stage of steady-state smelting, the smelting speed starts to be reduced in the later stage of steady-state smelting, the smelting speed is controlled to be 3.0-4.5 kg/min, and the number of molten drops is controlled to be 3-10 1/s;
In the heat-sealing top stage, inert gas adopts flow control, the melting speed is controlled to be 1.5-4.0 kg/min, and the number of molten drops is controlled to be 10-18 1/s;
And after the heat capping stage is finished, discharging the nickel-based superalloy from the furnace after vacuum cooling, and obtaining the nickel-based superalloy consumable ingot.
According to one embodiment of the invention, the vacuum consumable remelting process comprises: and (3) placing the consumable electrode into a consumable furnace, closing a furnace door, starting vacuumizing, starting power transmission smelting when the vacuum degree is less than 0.10Pa and the leak rate is less than 0.10Pa/min, and entering an arcing stage.
According to one embodiment of the invention, in the steady-state smelting stage, the maximum pressure range of the inert gas is 400-800 Pa.
According to one embodiment of the invention, the number of droplets is controlled to be 6.5-8.5/s during the steady state smelting stage.
According to one embodiment of the invention, the melting rate begins to decrease at a position 1/4 to 1/3 height from the top of the ingot during the later stages of steady state melting.
According to one embodiment of the invention, the melting rate drop ranges from 0.3 to 0.7kg/min in the later stages of steady state smelting.
According to one embodiment of the invention, in the heat-sealing stage, the flow rate of the inert gas is controlled to be 0.05-0.12L/min.
According to one embodiment of the invention, the flow rate of the inert gas is controlled to be 0.08-0.12L/min in the early stage of heat sealing, and 0.05-0.08L/min in the later stage of heat sealing.
According to one embodiment of the invention, the smelting time is 40-60 min in the later stage of heat capping.
In another aspect, the present invention provides a high homogenized nickel-base superalloy prepared by the method described above.
By adopting the technical scheme, the invention has the following beneficial effects:
The method controls heat input and heat loss of the head of the ingot by systematically optimizing the vacuum consumable remelting process of the nickel-based superalloy, effectively reduces the black spot defect of the head of the ingot, and realizes the stable production of the consumable ingot of the nickel-based superalloy easy to segregate. The method can alleviate the black spot segregation defect of the consumable nickel-base superalloy ingot, prepare a high-homogenization superalloy ingot product, and improve the quality and yield of the nickel-base superalloy product.
Compared with the method for gradually reducing the smelting melting speed in the whole steady-state smelting stage, the method provided by the invention considers that the probability of black spots appearing on the head of the consumable ingot is maximum, and according to the situation of the black spots appearing on site, the method only starts to reduce the smelting speed in the later stage of steady-state smelting, reduces the heat input of the head of the ingot and the local solidification time of the alloy, and effectively reduces the segregation defect of the head of the ingot. Compared with the method in the prior art, the method provided by the invention does not obviously influence the smelting period and the cost, and does not influence the surface quality, the skinning amount and the yield of the cast ingot.
Compared with the method for increasing the cooling of the molten pool by increasing the gas flow and the helium pressure, the invention provides a method for ensuring the cooling effect of inert gas on the cast ingot by adopting proper inert gas flow control in the heat-sealing stage, and simultaneously reducing the phenomenon that the molten pool is obviously broken by the inert gas. This is because the melt rate is lowered during heat-sealing, the molten bath liquid sealing state may be changed, and if pressure control is employed, the pressure of the inert gas charged may be significantly affected by the molten bath liquid sealing state, resulting in difficulty in ensuring the accuracy of control of the inert gas pressure during heat-sealing. The inert gas flow control is adopted to avoid the problem, so the invention adopts the inert gas flow control in the heat sealing stage, and reduces the phenomenon that the molten pool is obviously broken through by the inert gas flow control, thereby ensuring the cooling effect of the filled inert gas. Compared with the method in the prior art, the method provided by the invention reduces the phenomenon that the molten pool is obviously broken by inert gas during heat sealing, the phenomenon can cause the problems of unstable vacuum degree and electric arc, the inclusion, segregation and the like of the cast ingot, and meanwhile, the method can ensure that the filled inert gas has a good cooling effect and lightens the segregation tendency of the head part of the cast ingot.
Drawings
FIG. 1 is a flow chart of a method for preparing a high-homogeneity nickel-base superalloy provided by the invention.
FIG. 2 is a low power optical view of a forged bar according to an embodiment of the present invention and a comparative example.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
As required, detailed embodiments of the present invention are disclosed in the present specification; however, it is to be understood that the embodiments disclosed herein are merely exemplary of the invention that may be embodied in various and alternative forms. In the following description, a number of operating parameters and components are described in terms of various embodiments contemplated. These specific parameters and components are presented as examples and are not meant to be limiting.
As mentioned in the background section, the high temperature alloy is prone to form a typical segregation defect of black spots during the vacuum consumable smelting process, which cannot be eliminated by the homogenization process, and the toughness, yield strength and durability of the material are significantly reduced, so that the material is scrapped, and the product quality and yield are seriously affected. Therefore, the invention provides a method for preparing a high-homogenization superalloy ingot casting product by alleviating the black spot segregation defect of a superalloy vacuum consumable ingot casting.
In particular, the invention provides a preparation method of a high-homogeneity nickel-base superalloy. The preparation method comprises the step of smelting the high-homogeneity nickel-base superalloy cast ingot by adopting a duplex or triple smelting process. For example, the nickel-based superalloy is obtained by vacuum induction smelting and vacuum consumable remelting smelting, or the nickel-based superalloy ingot is obtained by vacuum induction smelting, electroslag remelting smelting and vacuum consumable remelting smelting. Wherein, the vacuum induction smelting process and the electroslag remelting smelting process adopt conventional processes in the field, the invention does not improve the vacuum induction smelting process and the electroslag remelting smelting process, and the invention mainly improves the vacuum consumable remelting smelting process.
The vacuum consumable remelting smelting process mainly comprises the stages of consumable electrode preparation, vacuum consumable smelting and the like, and the black spot defect formation of a vacuum consumable ingot is mainly in the stage of vacuum consumable smelting. Therefore, the preparation process steps and relevant parameters of the consumable electrode are all those commonly used in the art, and the present invention will not be described in detail. The vacuum consumable smelting process performed after the consumable electrode preparation process is the key analysis process of the invention.
The vacuum consumable smelting process sequentially comprises an arcing stage, a steady-state smelting stage and a heat-sealing top stage. And after the consumable electrode is placed into the consumable furnace and the furnace door is closed, vacuumizing is started, and when the vacuum degree and the leakage rate reach the requirements, power transmission can be started to smelt and enter an arcing stage. The arcing stage creates a molten pool and then enters a steady-state smelting stage. And after the steady-state smelting stage is finished, entering a heat-sealing top stage, and cooling and discharging after the heat-sealing top smelting is finished, so that the high-temperature alloy consumable ingot can be obtained. The following describes the specific case of a vacuum consumable remelting process used in the production method of the present invention with reference to fig. 1.
As shown in FIG. 1, the vacuum consumable remelting smelting process provided by the invention comprises the following specific steps: s1: placing the nickel-based superalloy consumable electrode into a consumable furnace, closing a furnace door, starting vacuumizing, transmitting power when the vacuum degree and the leak rate meet the requirements, starting smelting, and entering an arcing stage; s2: in the arcing stage, current and voltage control are adopted, the current is controlled to be 4.0-8.0 kA, the voltage is controlled to be 22.0-24.0V, and the pressure of inert gas is controlled to be 0Pa; s3: in the steady-state smelting stage, adopting molten drop and melting speed control, keeping the melting speed stable in the early stage of steady-state smelting, starting to reduce the melting speed in the later stage of steady-state smelting, controlling the melting speed to be 3.0-4.5 kg/min, controlling the number of molten drops to be 3-10/s, starting to charge inert gas in the early stage of steady-state smelting to strengthen the cooling of the cast ingot, adopting pressure control for the inert gas, keeping the inert gas pressure to be 0Pa in the early stage of steady-state smelting, and keeping the inert gas pressure stable after continuously increasing from 0Pa to the maximum value along with the continuous growth of the cast ingot so that the charged inert gas plays a role in cooling the cast ingot; s4: in the heat-sealing top stage, the melting speed is controlled to be stable after gradually decreasing from the steady-state melting stage value, the melting speed is controlled to be 1.5-4.0 kg/min, the melting drop number is controlled to be 10-18 1/s, and the inert gas is controlled by flow rate; s5: and after the heat capping stage is finished, discharging the nickel-based superalloy from the furnace after vacuum cooling, and obtaining the nickel-based superalloy consumable ingot.
The nickel-based superalloy consumable electrode used in step S1 contains a segregation-prone element such as W, mo, al, ti, nb. Here, the above-mentioned segregation-prone elements are not necessarily all contained in one type of nickel-base superalloy consumable electrode, and there is a case where one type of nickel-base superalloy consumable electrode contains only a part of segregation-prone elements.
Preferably, in step S1, when the vacuum degree is less than 0.10Pa and the leak rate is less than 0.10Pa/min, power transmission can be started to smelt, and the arcing stage is entered.
Preferably, in step S3, the number of droplets is controlled to be 6.5-8.5/S in the steady-state smelting stage. Namely smelting is carried out by adopting a relatively short arc length. This is because the stability of the arc generally decreases as the arc length increases.
Preferably, in step S3, the maximum pressure range of the inert gas is 400 to 800pa.
Preferably, in the later stage of steady-state smelting, namely at a height position which is 1/4-1/3 of the height position from the top of the ingot, the smelting speed starts to be reduced so as to reduce the heat input of the head position of the ingot, reduce the local solidification time of the alloy and reduce the segregation of the head of the ingot. If the melting speed reducing position is far away from the top of the ingot, the whole smelting period is longer, and the smelting cost is increased. If the melting speed reduction position is closer to the top of the ingot, the improvement effect of the black spots on the head of the ingot may be insignificant.
Preferably, the melting speed is reduced in the range of 0.3-0.7 kg/min in the later stage of steady-state smelting. If the melting speed is reduced to a larger extent, the depth of the molten pool is reduced to a larger extent, the consistency of the solidification structure is difficult to ensure, and the formation probability of white spot defects is increased. If the melting speed reduction range is smaller, the local solidification time of the alloy cannot be obviously reduced, and the black spot defect cannot be effectively reduced.
In the invention, the inert gas in the heat-sealing top stage adopts flow control, which is beneficial to obviously reducing the local solidification time of the alloy at the head of the ingot, improving the solidification structure and effectively reducing the black spot segregation defect at the head of the ingot. Preferably, in the heat-sealing top stage, the flow rate of the inert gas is in the range of 0.05-0.12L/min. The flow range adopted correspondingly from the steady-state melting speed to the low smelting speed (namely the early stage of heat capping) in the heat capping stage is 0.08-0.12L/min, and the flow range adopted in the later stage of heat capping (namely the low-melting-speed heat preservation smelting stage) is 0.05-0.08L/min. The adoption of the flow control in a proper range at different stages of the heat sealing roof can effectively avoid the problems of remarkable bursting of a molten pool, unstable vacuum degree and unstable electric arc during the heat sealing roof, and can lead the filled inert gas to have an effective cooling effect. If a large flow value of inert gas is used, the metal bath may also be at risk of being significantly broken by the inert gas; if the flow value of the inert gas is smaller, the amount of the inert gas filled is smaller, and the cooling effect of the inert gas on the cast ingot is weakened.
Preferably, in the step S4, in the later stage of heat capping (i.e., the low melting rate heat preservation smelting stage), the smelting time is 40-60 min. Compared with the smelting time in the prior art, the smelting time in the later period of heat capping is shortened by 10-20 min. If the low melting speed heat preservation smelting time is shortened for a long time, the feeding effect of the alloy can be obviously reduced, and the shrinkage cavity depth of the head part of the ingot is increased. If the low melting speed heat preservation smelting time is shortened to be shorter, the heat input of the head part of the cast ingot is not obviously reduced, and the local solidification time and segregation tendency of the head alloy are reduced. Compared with the condition that the feeding time of the heat seal top is not concerned at present and influences the segregation of the cast ingot, the invention provides the method for properly shortening the smelting time in the later smelting stage of the heat seal top (namely the low melting speed heat preservation smelting stage) and reducing the heat input and segregation tendency of the head part of the cast ingot on the premise of not obviously influencing the feeding effect.
The inert gas mentioned in the present invention may be helium.
The number of droplets referred to in the present invention, in 1/s, means the number of droplets per second.
The method controls the heat input and heat loss of the head of the ingot through systematically optimizing the smelting process, effectively reduces the black spot defect of the head of the ingot, and realizes the stable production of the consumable ingot of the easy segregation nickel-based superalloy. The method can alleviate the black spot segregation defect of the cast ingot, prepare the high-homogenization nickel-based superalloy product, and improve the product quality and the yield.
Compared with the method for gradually reducing the smelting melting speed in the whole steady-state smelting stage, the method provided by the invention considers that the probability of black spots appearing on the head of the consumable ingot is maximum, and according to the situation of the black spots appearing on site, the method only starts to reduce the smelting speed in the later stage of steady-state smelting, reduces the heat input of the head of the ingot and the local solidification time of the alloy, and effectively reduces the segregation defect of the head of the ingot. Compared with the method in the prior art, the method provided by the invention does not obviously influence the smelting period and the cost, and does not influence the surface quality, the skinning amount and the yield of the cast ingot.
Compared with the method for increasing the cooling of the molten pool by increasing the gas flow and the helium pressure, which are proposed in the prior art, the method of the invention proposes to adopt proper inert gas flow control in the heat-seal top stage to ensure the cooling effect of inert gas on the cast ingot. Compared with the method in the prior art, the method provided by the invention can reduce the phenomenon that a molten pool is obviously broken by inert gas, the phenomenon can cause the problems of unstable vacuum degree and electric arc, increase of cast ingot inclusion, segregation and the like, and meanwhile, the method can ensure that the filled inert gas has a good cooling effect and lightens the segregation tendency of the cast ingot head.
The invention is further illustrated below in connection with specific examples, but is not limited in any way. For the avoidance of doubt, all methods are conventional unless otherwise indicated.
Example 1
① The chemical components of the adopted nickel-based superalloy are as follows: c.ltoreq.0.08, cr: 17-20%, W: 4-5%, mo: 4-5%, al: 1-1.5%, ti: 2.2-2.8%, and the balance of Ni and some unavoidable impurity elements. The electrode bar with the diameter of 420mm is prepared through the procedures of vacuum induction smelting, pouring, annealing, sawing, peeling, baking, welding and the like.
② The electrode rod in the step ① is taken as a consumable electrode to be placed into a consumable furnace with the ingot diameter of phi 508mm, a furnace door is closed, vacuumizing is started, and when the vacuum degree and the leak rate reach the requirements, namely, the vacuum degree is less than 0.1Pa, and the leak rate is less than 0.1Pa/min, power can be transmitted to start smelting. The self-consuming smelting arcing stage is controlled by adopting current and voltage within 0-20 min, the current in the arcing stage is gradually increased from 4.5kA to 7.5kA and then stabilized, the voltage is gradually increased from 22V to 24V and then stabilized, and the helium pressure in the arcing stage is 0Pa.
③ The self-consuming smelting is carried out in a steady-state smelting stage within 21-730 min, the steady-state smelting stage adopts the control of molten drop and smelting speed, the number of molten drops is 7.0/s, the smelting speed is 3.8kg/min, helium is filled when the smelting time reaches 100min, and the helium pressure is increased to 600Pa and then the smelting time reaches 150min and is stable. The smelting melting speed is reduced from 1/3 height position from the top of the ingot to reduce the heat input of the head position of the ingot, namely the melting speed is gradually reduced from 3.8kg/min in the steady-state smelting stage to 3.5kg/min in the heat-sealing top stage.
④ And the time of 731-820 min is a self-consumed smelting heat-sealing top stage, the heat-sealing top stage adopts molten drop and melting speed control, the number of the molten drops is 11-16 1/s, and the melting speed is 1.5-3.5 kg/min. The early stage of heat-seal top smelting is carried out within the period of 731-764 min, the smelting speed is gradually reduced from 3.5kg/min to 1.7kg/min, and the flow rate of the used helium is 0.08-0.12L/min. The later smelting stage of the heat-seal roof is carried out within 765-820 min, namely the low melting speed heat-preservation smelting stage (the smelting time is 55 min), the melting speed is gradually reduced from 1.7kg/min to 1.5 kg/min, and the flow rate of the used helium is 0.05-0.08L/min.
⑤ And cooling the ingot in a crystallizer for 120min after the heat capping is finished, removing the ingot, and obtaining the consumable ingot after air cooling.
Comparative example 1
The only difference from example 1 is that: the melting speed is not reduced to reduce the heat input of the head position of the ingot in the later stage of steady-state smelting, namely, the melting speed from the position 1/3 of the height of the top of the ingot to the heat-seal top stage is kept at 3.8kg/min, the flow control is not adopted in the heat-seal top stage, the pressure control is adopted, and the helium pressure of 600Pa is maintained in the whole heat-seal top stage. Meanwhile, the low melting speed heat preservation smelting time in the heat capping stage is 70min.
Comparative example 2
The only difference from example 1 is that: the smelting speed in the steady-state smelting stage is 2.9kg/min, namely, smelting is carried out by adopting a smaller smelting speed, a molten pool is obviously not on the side in the smelting process under the condition, the surface quality of an ingot is poor, and the skinning amount of the ingot is large.
Comparative example 3
The only difference from example 1 is that: the smelting speed in the steady-state smelting stage is 4.6kg/min, namely, smelting is performed by adopting a larger smelting speed, the depth of a smelting pool and a pasty area are large under the condition, the local solidification time of the alloy is long, and serious segregation defects appear in the cast ingot.
Comparative example 4
The only difference from example 1 is that: the helium pressure in the steady-state smelting stage is 900Pa, and in this case, the helium breaks through a metal molten pool in the smelting process, so that the vacuum degree in the smelting process is obviously more than 0.1Pa, and the cooling effect of the helium, the electric arc and the stability of the molten pool are affected.
Comparative example 5
The only difference from example 1 is that: the helium pressure in the steady-state smelting stage is 300Pa, and in this case, the cooling effect of the filled helium is weak, so that the local solidification time of the alloy cannot be reduced, and the segregation problem of the cast ingot is relieved.
Comparative example 6
The only difference from example 1 is that: the number of molten drops in the steady-state stage is controlled to be 8.6/s, namely smelting is carried out by adopting a shorter arc length. In this case, the shorter arc length increases the temperature of the surface of the molten metal pool, and increases the local solidification time and segregation tendency of the ingot.
Comparative example 7
The only difference from example 1 is that: the number of molten drops in the steady-state smelting stage is controlled to be 6.4/s, namely smelting is carried out by adopting a longer arc length. Under the condition, the stability of the arc length is poor, the arc deviation phenomenon is easy to occur in the smelting process, the arc energy and the instability of a molten pool are increased, and the problem of ingot segregation is obvious.
Comparative example 8
The only difference from example 1 is that: the steady state melting stage begins to reduce the melting rate of the melt at a height of 1/5 of the top of the ingot to reduce the heat input at the head of the ingot, i.e., the melting rate gradually decreases from 3.8kg/min in the steady state melting stage to 3.5kg/min in the heat seal topping stage. Under the condition, the melting speed reducing position is closer to the top of the ingot during steady-state smelting, the reduced melting speed does not obviously reduce the heat input of the head of the ingot, the black spot defect of the head of the ingot is effectively reduced, and a small amount of black spot defects still exist in head macroscopic inspection.
Comparative example 9
The only difference from example 1 is that: the steady state melting stage begins to reduce the melting rate of the melt at a height of 1/2 from the top of the ingot to reduce the heat input at the head of the ingot, i.e., the melting rate gradually decreases from 3.8kg/min in the steady state stage to 3.5kg/min in the heat seal top stage. Under the condition, the melting speed reducing position in the steady-state melting stage is far away from the top of the ingot, the reduced melting speed can reduce the heat input of the head of the ingot, but the whole melting time is increased by about 120min, and the production period and the cost are obviously increased.
Comparative example 10
The only difference from example 1 is that: when the smelting speed is reduced from a position 1/3 of the height from the top of the ingot in the steady-state smelting stage, the smelting speed is gradually reduced from 3.8kg/min to 3.6kg/min in the heat-sealing top stage, and the smelting speed is reduced by only 0.2kg/min. In this case, the reduced melting rate did not significantly reduce the heat input to the ingot head, which was inspected for the presence of a small number of black spot defects.
Comparative example 11
The only difference from example 1 is that: when the smelting speed is reduced from a position 1/3 of the height from the top of the ingot in the steady-state smelting stage, the smelting speed is gradually reduced from 3.8kg/min to 3.0kg/min in the heat-sealing top stage, and the smelting speed is reduced by 0.8kg/min. In this case, a large melt rate change causes a small number of white spot defects to appear in the head macroscopic inspection.
Comparative example 12
The only difference from example 1 is that: the maximum helium flow rate of the heat-seal top stage is 0.13L/min, and under the condition, a molten pool is obviously broken in the heat-seal top stage, the vacuum degree in the smelting process is obviously more than 0.1Pa, and an electric arc and the molten pool are unstable.
Comparative example 13
The only difference from example 1 is that: the maximum helium flow rate of the heat-seal top stage is 0.04L/min, and in the heat-seal top stage, a molten pool is not obviously broken, but the helium cooling effect of the molten pool is weaker, and the segregation tendency of cast ingots is large.
Comparative example 14
The only difference from example 1 is that: the heat-sealing top has the low melting speed and heat preservation time of 35min, and under the condition, the quantity of alloy liquid used for feeding is small, the trend of increasing the shrinkage cavity size of the head of the ingot is obvious, and the head cutting quantity of the ingot is increased.
Comparative example 15
The only difference from example 1 is that: the heat-sealing low melting speed heat preservation time is 75min, and in this case, the input arc energy of the head of the ingot is increased, and the local solidification time of the alloy and the segregation tendency of the ingot are increased.
Example 2
The only difference from example 1 is that: the chemical components of the nickel-based superalloy adopted in the (1) are as follows: c.ltoreq.0.08, cr: 17-21%, ni: 50-55%, co less than or equal to 1%, mo: 2.8-3.3%, al: 0.2-0.8%, ti: 0.65-1.15%, nb: 4.75-5.5%, and the balance of Fe and unavoidable impurity elements. (2) The melting speed is 4.0kg/min in the steady-state melting stage of consumable smelting. (3) The melting rate gradually decreases from 4.0kg/min to 3.5kg/min during the steady state melting phase, i.e. from a position 1/3 height from the top of the ingot to the heat seal top phase.
Comparative example 16
The only difference from example 2 is that: the melting speed is not reduced to reduce the heat input of the head position of the ingot in the later stage of steady-state smelting, namely, the melting speed from the position 1/3 of the height of the top of the ingot to the heat-seal top stage is kept to be 4.0kg/min, the flow control is not adopted in the heat-seal top stage, the pressure control is adopted, and the helium pressure of 600Pa is maintained in the whole heat-seal top stage. And meanwhile, the low melting speed heat preservation smelting time of the heat seal top is 70min.
Example 3
The only difference from example 1 is that: (1) The current in the arcing stage is gradually increased from 4.0kA to 8.0kA and then is stable; (2) The melting speed in the steady-state melting stage is 3.0kg/min, and the number of molten drops is 3 1/s; (3) The melting speed of the heat sealing top stage is 1.5kg/min, and the number of molten drops is controlled to be 10 1/s.
Example 4
The only difference from example 1 is that: (1) The melting speed in the steady-state melting stage is 4.5kg/min, and the number of molten drops is 10/s; (2) The melting speed of the heat sealing top stage is 1.5kg/min, and the number of molten drops is controlled to be 18/s.
Example 5
The only difference from example 1 is that: the number of droplets in the steady-state smelting stage is 6.5/s.
Example 6
The only difference from example 1 is that: the number of drops in the steady-state smelting stage is 8.5/s.
Example 7
The only difference from example 1 is that: the helium pressure in the steady-state smelting stage is increased to 400Pa and then is stable.
Example 8
The only difference from example 1 is that: the helium pressure in the steady-state smelting stage is increased to 800Pa and then tends to be stable.
Example 9
The only difference from example 1 is that: the smelting melting rate starts to be reduced at a position 1/4 of the height from the top of the ingot.
The invention analyzes the low power condition of some of the alloy forging bars of the examples and the comparative examples. As can be seen from FIG. 2, the forged bars obtained in the examples were inferior in the absence of black spot defect to those obtained in the comparative examples. That is, the invention systematically optimizes the smelting process to control heat input and heat loss, namely, properly reduces smelting melting speed in the later stage of steady-state smelting, adopts proper helium flow control in different stages of the heat-sealing stage, reduces low melting speed heat preservation time in the heat-sealing stage, obviously reduces heat input of the head of an ingot, increases cooling of the head of the ingot, reduces local solidification time of alloy at the head of the ingot, and effectively reduces black spot defect at the head of the ingot.
In conclusion, the method provided by the invention can obviously reduce the black spot defect of the nickel-based superalloy consumable ingot, reduce the end cutting amount of the product, and improve the product qualification rate and the yield.
The formation of the nickel-based superalloy consumable ingot black spot is mainly in the smelting stage, so that other working procedure steps of vacuum consumable smelting (such as preparation of consumable electrode rods and the like) and related parameters thereof are adopted in the common use in the field, and the invention is not particularly limited.
Finally, it should be noted that: the embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (10)
1.A method for preparing a high-homogeneity nickel-base superalloy, comprising: preparing a nickel-based superalloy consumable ingot by a vacuum consumable remelting smelting process, wherein the vacuum consumable remelting smelting process comprises an arcing stage, a steady-state smelting stage and a heat-sealing top stage, and the vacuum consumable remelting smelting process comprises the following steps of:
In the arcing stage, the current is controlled to be 4.0-8.0 kA, and the voltage is controlled to be 22.0-24.0V;
In the steady-state smelting stage, inert gas is filled into the consumable furnace, the inert gas is controlled by pressure, the smelting speed is kept stable in the early stage of steady-state smelting, the smelting speed starts to be reduced in the later stage of steady-state smelting, the smelting speed is controlled to be 3.0-4.5 kg/min, and the number of molten drops is controlled to be 3-10 1/s;
In the heat-sealing top stage, inert gas adopts flow control, the melting speed is controlled to be 1.5-4.0 kg/min, and the number of molten drops is controlled to be 10-18 1/s;
And after the heat capping stage is finished, discharging the nickel-based superalloy from the furnace after vacuum cooling, and obtaining the nickel-based superalloy consumable ingot.
2. The method of preparing a high homogenized nickel base superalloy as in claim 1, wherein the vacuum consumable remelting process comprises: and (3) placing the consumable electrode into a consumable furnace, closing a furnace door, starting vacuumizing, starting power transmission smelting when the vacuum degree is less than 0.10Pa and the leak rate is less than 0.10Pa/min, and entering an arcing stage.
3. The method for producing a high-homogeneity nickel-base superalloy according to claim 1, wherein the maximum pressure of the inert gas charged during the steady-state melting stage is in the range of 400 to 800Pa.
4. The method for producing a high-homogenized nickel-base superalloy according to claim 1, wherein the number of droplets is controlled to be 6.5-8.5/s during the steady-state melting phase.
5. The method for producing a high homogenized nickel base superalloy according to claim 1, wherein the lowering of the melting rate is started at a position 1/4 to 1/3 height from the top of the ingot in the later stage of steady state melting.
6. The method for producing a high-homogenized nickel-base superalloy according to claim 1 or 5, wherein the melting speed reduction is in the range of 0.3-0.7 kg/min at the late stage of steady state melting.
7. The method for producing a high-homogeneity nickel-base superalloy according to claim 1, wherein the flow rate of the inert gas is controlled to be 0.05 to 0.12l/min at the heat-seal top stage.
8. The method for producing a high-homogeneity nickel-base superalloy according to claim 7, wherein the flow rate of the inert gas is controlled to be 0.08 to 0.12l/min in the early stage of heat-sealing and 0.05 to 0.08l/min in the later stage of heat-sealing.
9. The method for preparing the high-homogeneity nickel-base superalloy according to claim 1, wherein the smelting time is 40-60 min in the later stage of heat capping.
10. A high homogeneity nickel-base superalloy, characterized in that it is produced by the production method according to any of claims 1-9.
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