CN108913922B - Purification smelting method of nickel-based directionally solidified columnar crystal and monocrystal high-temperature alloy master alloy - Google Patents
Purification smelting method of nickel-based directionally solidified columnar crystal and monocrystal high-temperature alloy master alloy Download PDFInfo
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Abstract
The invention belongs to the technical field of high-temperature alloy preparation, and particularly relates to a purification smelting method of a nickel-based directionally solidified columnar crystal and single crystal high-temperature alloy master alloy. The invention comprehensively controls the raw materials, the crucible material, the pure purification smelting process control and the like, reduces the alloy refining temperature in the smelting process, further reduces the element loss and slows down the crucible reaction, and can realize more accurate control of the alloy components and reduce the content of impurity elements. And simultaneously, after the alloying period is finished, a deoxidizing and desulfurizing agent is added, so that impurity elements such as O, S in the alloy are reduced as much as possible. The method can control the total amount of O, N, S impurity elements in the nickel-based directionally solidified columnar crystal and single crystal superalloy master alloy within 5ppm, and simultaneously control the total amount of trace impurity elements such As As, Bi, Pb, Sn, Sb and the like within 5ppm, thereby greatly improving the purity of the nickel-based directionally solidified columnar crystal and single crystal superalloy.
Description
Technical Field
The invention belongs to the technical field of high-temperature alloy preparation, and particularly relates to a purification smelting method of a nickel-based directionally solidified columnar crystal and single crystal high-temperature alloy master alloy.
Background
With the continuous development of the aircraft engine and gas turbine industries, the usage amount of the high-temperature alloy is more and more, and the requirement of continuously increasing the inlet air temperature in front of a turbine is to increase the thrust, improve the efficiency and reduce the oil consumption, so that higher requirements are provided for the high-temperature alloy and the process thereof. Compared with common isometric crystal high-temperature alloy, the directional solidification column crystal and single crystal high-temperature alloy greatly improves the use temperature, the service life, the tissue stability and the comprehensive mechanical property due to the unique chemical components and the structural property. The alloying degree of the directionally solidified columnar crystal and single crystal high-temperature alloy is very high in design, the adding proportion of high-specific-gravity refractory metal elements such as W, Mo, Ta, Hf, Re and the like is continuously improved, so that the content of harmful gases and impurity elements is difficult to control in the smelting process, and the impurities formed by the harmful gases and the impurity elements can seriously increase the rejection rate and reduce the service life of the material.
How to improve the purity of nickel-based directionally solidified columnar crystals and single crystal high-temperature alloys and further exert the application potential of the material becomes an important subject to be researched urgently. Most of the patents in the aspect of the disclosed high-temperature alloy purification smelting process adopt 1600 DEG CAnd the high-temperature refining, for example, the high-temperature refining at 1614-1624 ℃ is adopted in the patent with the publication number of CN106319255A, the high-temperature refining temperature in the patent with the publication number of CN1360071A is 1650 ℃, the high-temperature refining temperature in the patent with the publication number of CN1552928A is 1600-1650 ℃, the high-temperature refining has certain effect on removing deoxidation, denitrification and other low-melting-point volatile impurity elements, but the high-temperature refining also has the following defects: (1) aggravate the crucible reaction: the reaction of the alloy liquid and the refractory material on the inner surface of the crucible is violent at higher temperature, and the common crucible contains MgO and Al2O3、SiO2、ZrO、Fe2O3The compounds intensify the [ C ] in the materials and the alloy liquid under the conditions of high temperature and high vacuum]The pollution of the crucible material to the alloy liquid is caused; meanwhile, the erosion degree of the crucible material is higher, and the service life of the crucible is shortened. (2) Under the conditions of high temperature and high vacuum, alloy elements such as Cr, Al and the like with higher saturated vapor pressure volatilize more seriously, thereby causing great loss of the alloy elements.
In published patents, it is also reported that high temperature alloy purification melting is performed by using crucible materials such as calcium oxide and yttrium oxide, for example, in patent publication No. CN1360071A, the crucible material is calcium oxide, and in patent publication No. CN103498063A, the crucible material is yttrium oxide. Although the crucibles made of these materials can remove O and S to a certain extent, they have problems of high cost and difficulty in storage, and thus are difficult to be industrially popularized.
Therefore, the purity of the nickel-based directionally solidified columnar crystals and the single crystal superalloy can be more effectively controlled by comprehensively considering the aspects of raw material purity, crucible material, smelting process control and the like.
Disclosure of Invention
The invention aims to provide a pure smelting method of a nickel-based directionally solidified column crystal and single crystal superalloy master alloy, aiming at the problem that high-value superalloy such as nickel-based directionally solidified column crystal and single crystal is more sensitive to harmful gas such as O, N, S and impurity elements. The method controls the aspects of raw material purity, crucible material, purification smelting process control and the like, can control the total amount of O, N, S impurity elements in the nickel-based oriented single crystal superalloy within 5ppm, and can control the total amount of trace impurity elements such As As, Bi, Pb, Sn, Sb and the like within 5ppm, thereby greatly improving the purity of the nickel-based oriented single crystal superalloy.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the purification smelting method of the nickel-based directionally solidified columnar crystal and single crystal high temperature alloy master alloy selects the raw material with higher purity; simultaneously, a high-purity alumina or magnesia crucible with good thermal stability and purity of more than 92 percent is selected; the method comprises the following steps:
(1) charging: the charging sequence in the crucible is from bottom to top, and the charging sequence sequentially comprises: 20-30% of total amount of all Co and Ni, 0.01-0.03% of C, all Cr, all Mo, all W, all Ta, all Re and the rest Ni; charging the rest raw materials such as C, Al, Ti, all Hf, NiB, Zr and the like into a charging chamber; adding a deoxidizing and desulfurizing agent from a feeding chamber after the feeding is finished in the alloying period;
the charging sequence is not limited to a certain grade of alloy, if the alloy does not contain one or more elements, the raw material charging process can be eliminated during charging;
(2) melting period: smelting by using a vacuum induction furnace, when the vacuum degree is less than or equal to 1.33Pa, sending power section by section and heating until furnace burden is molten down, and continuing heating after the furnace burden is molten down;
(3) and (3) refining period: when the temperature reaches 140-180 ℃ above the liquidus temperature of the alloy, refining is started, wherein the refining time is determined according to the capacity of a vacuum induction furnace, and the refining time of a 250Kg vacuum furnace is 10-40 min;
(4) and (3) alloying period: after the refining period is finished, stopping power, reducing the temperature, freezing until the temperature reaches 20-60 ℃ above the temperature of the alloy liquidus, adding the rest raw materials such as C, Al, Ti, all Hf, NiB, Zr and the like from a feeding chamber, and stirring and melting down the raw materials at high power; when the temperature reaches 100-140 ℃ above the temperature of the alloy liquidus line, refining; the refining time is determined according to the capacity of the vacuum induction furnace, and the refining time of a 250Kg vacuum furnace is 10-20 min;
(5) and (3) a deoxidation and desulfurization period: after the alloying period is finished, stopping power, reducing the temperature and freezing, and filling argon gas for 5-30 kPa during the period; when the temperature reaches 20-60 ℃ above the liquidus temperature of the alloy, adding a deoxidizing and desulfurizing agent into the feeding chamber, and stirring and melting down the alloy at high power; when the temperature reaches 60-100 ℃ above the temperature of the alloy liquidus line, refining; the refining time is determined according to the capacity of the vacuum induction furnace, and the refining time of a 250Kg vacuum furnace is 5-15 min;
(6) and (3) pouring period: and after the deoxidation and the desulfurization are finished, the power is cut off to reduce the temperature, the vacuum is pumped to less than or equal to 1.33Pa, the mixture is stirred with high power, and when the temperature reaches 100-120 ℃ above the liquidus temperature of the alloy, the mixture is poured.
Wherein, the raw materials with higher purity are respectively: ni9999, metallic chromium GHCr-1, metallic chromium GHCr-2, metallic cobalt Co9998, metallic tantalum GDT-1, GDT-2, GDT-3, hafnium sponge HHf-01, metallic rhenium Re-04, refined aluminum ingot for remelting of Al99.99 and higher, 0AGrade titanium sponge.
In the step (5), the deoxidizing and desulfurizing agent is Y and nickel-calcium alloy, the addition amount of Y is 0.02-0.1% of the weight ratio of the alloy, the addition amount of nickel-calcium alloy is 0.5-1.0% of the weight ratio of the alloy, and the calcium content in the nickel-calcium alloy is 5-30%.
Due to the adoption of the technical scheme, compared with the prior art, the invention has at least the following beneficial effects:
(1) the invention selects the high-purity alumina or magnesia crucible with better thermal stability and purity of more than 92 percent, and can reduce the impurities brought into the alloy liquid by the crucible reaction.
(2) The invention provides a high-purity raw material aiming at nickel-based directionally solidified column crystal and single crystal superalloy master alloy, and controls impurity elements from the source, thereby effectively reducing the impurity content in the nickel-based directionally solidified and single crystal superalloy master alloy and improving the purity of the alloy.
(3) The purification smelting process reduces the refining temperature of the alloy, further reduces the reaction of the alloy liquid and the crucible refractory material in the smelting process, and further reduces the secondary pollution caused by the crucible reaction; meanwhile, the loss of alloy elements with higher saturated vapor pressure in the smelting process is reduced, and the element yield is improved.
(4) The invention provides a novel deoxidizing and desulfurizing agent and a deoxidizing and desulfurizing process, which can effectively reduce the content of O, S and other impurities in alloy.
(5) The nickel-based directionally solidified columnar crystals and the single crystal high temperature alloy master alloy produced by the pure smelting process have extremely low harmful gas and impurity contents, and the yield and the service life of the nickel-based directionally solidified columnar crystals and the single crystal high temperature alloy blades can be greatly improved. The total amount of O, N, S impurity elements in the nickel-based directionally solidified columnar crystals and the single crystal superalloy can be controlled within 5ppm, and the total amount of trace impurity elements such As As, Bi, Pb, Sn, Sb and the like can be controlled within 5 ppm.
(6) The purification smelting process is simple, easy to operate and capable of realizing industrial production and popularization.
Detailed Description
The invention is further illustrated by the following examples. In the following detailed description, certain exemplary embodiments of the present invention are described by way of illustration only. Needless to say, a person skilled in the art realizes that the described embodiments can be modified in various different ways without departing from the spirit and scope of the present invention. Accordingly, the description is illustrative in nature and not intended to limit the scope of the claims.
In the embodiments 1 and 2, 250Kg of vacuum induction furnace equipment is adopted to carry out purification smelting on the nickel-based directionally solidified column crystals and the single crystal superalloy.
Example 1:
the DZ125 nickel-based directional solidification columnar crystal high-temperature alloy produced by the pure smelting process is examined to be 1377 ℃ in the liquid phase line temperature of the alloy in Chinese aviation material handbook. The alloy comprises the following chemical components in percentage by mass: 0.09% of C, 8.9% of Cr, 10% of Co, 7% of W, 2% of Mo, 5.1% of Al, 0.95% of Ti, 3.8% of Ta, 1.5% of Hf, 0.015% of B, 0.04% of Zr and the balance of Ni.
The specific implementation steps of the embodiment are as follows:
1. selection of high-purity raw materials: ni9999, metal chromium of GHCr-1 and GHCr-2, metal cobalt of Co9998, metal tantalum of GDT-1, GDT-2 and GDT-3, sponge hafnium of HHf-01, refined aluminum ingot for remelting of Al99.99 and higher marks, 0A-grade sponge titanium, C, W, Mo, Zr and the like are all selected from high marks with HB/Z131 specified grade, and B is selected from high-purity nickel-boron intermediate alloy produced by the company;
2. selecting a crucible: selecting a high-purity magnesium oxide crucible with the purity of 95 percent;
3. the smelting method comprises the following steps:
(1) charging: the charging sequence in the crucible is from bottom to top, and the charging sequence sequentially comprises: 20-30% of total amount of all Co and Ni, 0.01-0.03% of C, all Cr, all Mo, all W, all Ta and the rest Ni; the rest raw materials of C, Al, Ti, all Hf, NiB, Zr and the like are filled into a feeding chamber, and a deoxidizing and desulfurizing agent is added into the feeding chamber after the feeding in the alloying period is finished;
(2) melting period: when the vacuum degree is less than or equal to 1.33Pa, the power is sent section by section to heat up the furnace burden to be molten down, and the temperature is continuously raised after the high power of the molten down is achieved;
(3) and (3) refining period: when the temperature reaches 1517-1557 ℃, refining for 10-40 min;
(4) and (3) alloying period: after the refining period is finished, stopping power, reducing the temperature, freezing until the temperature reaches 1397-1437 ℃, adding the rest raw materials such as C, Al, Ti, all Hf, NiB, Zr and the like into a feeding chamber, and stirring and melting down the raw materials at high power; when the temperature reaches 1477-1517 ℃, refining for 10-20 min;
(5) and (3) a deoxidation and desulfurization period: after the alloying period is finished, stopping power, reducing the temperature and freezing, and filling argon gas for 5-30 kPa during the period; when the temperature reaches 1397-1437 ℃, adding a deoxidizing and desulfurizing agent from a feeding chamber, and stirring at high power to melt down; when the temperature reaches 1437-1477 ℃, refining for 5-15 min;
(6) and (3) pouring period: and after the deoxidation and the desulfurization are finished, the power is cut off to reduce the temperature, the vacuum is pumped to less than or equal to 1.33Pa, the mixture is stirred with high power, and when the temperature reaches 1477-1497 ℃ above the liquidus temperature of the alloy, the mixture is poured.
The DZ125 nickel-based directionally solidified columnar crystal superalloy master alloy smelted by the process method is extremely low in O, N, S content, and the total amount of trace impurity elements such As As, Bi, Pb, Sn and Sb can be controlled within 5 ppm. Specifically, the results are shown in tables 1 and 2.
TABLE 1O, N, S content (ppm)
| Element(s) | O | N | S | Total of |
| Content (wt.) | 1 | 2 | 1.5 | 4.5 |
TABLE 2 As, Bi, Pb, Sn, Sb contents (ppm)
| Element(s) | As | Bi | Pb | Sn | Sb | Total of |
| Content (wt.) | 1.6 | 0.05 | 0.3 | 2.1 | 0.15 | 4 |
Example 2:
the purifying smelting process of the present invention is used in producing certain grade of second generation nickel base monocrystal high temperature alloy with liquidus temperature 1385 deg.c. The alloy comprises the following chemical components in percentage by mass: 0.06% C, 7.0% Cr, 8.0% Co, 5.0% W, 2.0% Mo, 6.2% Al, 7.0% Ta, 3.0% Re, 0.20% Hf, 0.004% B, and the balance Ni.
The specific implementation steps of the embodiment are as follows:
1. selection of high-purity raw materials: ni9999, metal chromium of GHCr-1 and GHCr-2, metal cobalt of Co9998, metal tantalum of GDT-1, GDT-2 and GDT-3, sponge hafnium of HHf-01, Re-04 metal rhenium, refined aluminum ingots for remelting of Al99.99 and higher marks, C, W, Mo and the like are all selected from HB/Z131 with higher specified grade, and B is selected from high-purity nickel-boron intermediate alloy produced by the company.
2. Selecting a crucible: the high-purity alumina crucible with the purity of 96 percent is selected.
3. The smelting method comprises the following steps:
(1) charging: the charging sequence in the crucible is from bottom to top, and the charging sequence sequentially comprises: 20-30% of the total amount of all Co and Ni, 0.01-0.03% of C, all Cr, all Mo, all W, all Ta, all Re and the rest Ni in the weight ratio of the oriented single crystal nickel-based high-temperature alloy; the residual C, Al, all Hf, NiB and other raw materials are filled into the feeding chamber, and the deoxidizing and desulfurizing agent is added into the feeding chamber after the feeding in the alloying period is finished;
(2) melting period: when the vacuum degree is less than or equal to 1.33Pa, the power is sent section by section to heat up the furnace burden to be molten down, and the temperature is continuously raised after the high power of the molten down is achieved;
(3) and (3) refining period: when the temperature reaches 1525-1565 ℃, refining for 10-40 min;
(4) and (3) alloying period: after the refining period is finished, stopping power, reducing the temperature, freezing until the temperature reaches 1405-1445 ℃, adding the residual C, Al, all Hf, NiB and other raw materials from a feeding chamber, and stirring at high power to melt down; when the temperature reaches 1485-1525 ℃, refining for 10-20 min;
(5) and (3) a deoxidation and desulfurization period: after the alloying period is finished, stopping power, reducing the temperature and freezing, and filling argon gas for 5-30 kPa during the period; when the temperature reaches 1405-1445 ℃, adding a deoxidizing and desulfurizing agent into the feeding chamber, and stirring and melting down the mixture at high power; when the temperature reaches 1445-1485 ℃, refining for 5-15 min;
(6) and (3) pouring period: and after the deoxidation and the desulfurization are finished, the power is cut off to reduce the temperature, the vacuum is pumped to less than or equal to 1.33Pa, the mixture is stirred with high power, and when the temperature reaches 1485-1505 ℃ above the liquidus temperature of the alloy, the mixture is poured.
The second generation single crystal high temperature alloy mother alloy O, N, S with certain grade smelted by the process method has extremely low content, and the total amount of trace impurity elements such As As, Bi, Pb, Sn, Sb and the like can be controlled within 5 ppm. Specifically, the results are shown in tables 3 and 4.
TABLE 3O, N, S content (ppm)
| Element(s) | O | N | S | Total of |
| Content (wt.) | 1 | 1 | 0.5 | 2.5 |
TABLE 4 As, Bi, Pb, Sn, Sb contents (ppm)
| Element(s) | As | Bi | Pb | Sn | Sb | Total of |
| Content (wt.) | 1.4 | 0.05 | 0.1 | 1.6 | 0.1 | 3.25 |
The above description is only an exemplary embodiment of the present invention, and is not intended to limit the scope of the present invention. Any equivalent changes and modifications that can be made by one skilled in the art without departing from the spirit and principles of the invention shall fall within the protection scope of the invention.
Claims (4)
1. The pure purification smelting method of the nickel-based directionally solidified columnar crystal and single crystal high temperature alloy master alloy is characterized by comprising the following steps of: selecting raw materials with higher purity and simultaneously selecting a high-purity alumina or magnesia crucible; the method comprises the following steps:
(1) charging: the charging sequence in the crucible is from bottom to top, and the charging sequence sequentially comprises: 20-30% of total amount of all Co and Ni, 0.01-0.03% of C, all Cr, all Mo, all W, all Ta, all Re and the rest Ni; filling the rest raw materials of C, Al, Ti, all Hf, NiB and Zr into a charging chamber;
(2) melting period: smelting by using a vacuum induction furnace, when the vacuum degree is less than or equal to 1.33Pa, sending power section by section and heating until furnace burden is molten down, and continuing heating after the furnace burden is molten down;
(3) and (3) refining period: when the temperature reaches 140-180 ℃ above the liquidus temperature of the alloy, refining is started;
(4) and (3) alloying period: after the refining period is finished, stopping power, reducing the temperature, freezing until the temperature reaches 20-60 ℃ above the temperature of the alloy liquidus, adding the rest raw materials of C, Al, Ti, all Hf, NiB and Zr into a feeding chamber, and stirring and melting down the raw materials at high power; when the temperature reaches 100-140 ℃ above the temperature of the alloy liquidus line, refining;
(5) and (3) a deoxidation and desulfurization period: after the alloying period is finished, stopping power, reducing the temperature and freezing, and filling argon gas for 5-30 kPa during the period; when the temperature reaches 20-60 ℃ above the liquidus temperature of the alloy, adding a deoxidizing and desulfurizing agent into the feeding chamber, and stirring and melting down the alloy at high power; when the temperature reaches 60-100 ℃ above the temperature of the alloy liquidus line, refining;
(6) and (3) pouring period: and after the deoxidation and the desulfurization are finished, the power is cut off to reduce the temperature, the vacuum is pumped to less than or equal to 1.33Pa, the mixture is stirred with high power, and when the temperature reaches 100-120 ℃ above the liquidus temperature of the alloy, the mixture is poured.
2. The method for purifying and smelting the nickel-based directionally solidified columnar crystal and single crystal superalloy master alloy as claimed in claim 1, wherein the raw materials with higher purity are respectively as follows: ni9999, metallic chromium GHCr-1, metallic chromium GHCr-2, metallic cobalt Co9998, metallic tantalum GDT-1, GDT-2, GDT-3, hafnium sponge HHf-01, metallic rhenium Re-04, refined aluminum ingot for remelting of Al99.99 and higher, 0AGrade titanium sponge.
3. The method for purifying and smelting the nickel-based directionally solidified columnar crystal and single crystal superalloy master alloy as claimed in claim 1, wherein: the crucible is an alumina or magnesia crucible with the purity of more than 92 percent.
4. The method for purifying and smelting the nickel-based directionally solidified columnar crystal and single crystal superalloy master alloy as claimed in claim 1, wherein: in the step (5), the deoxidizing and desulfurizing agent is Y and nickel-calcium alloy, the addition amount of Y is 0.02-0.1% of the weight ratio of the alloy, the addition amount of nickel-calcium alloy is 0.5-1.0% of the weight ratio of the alloy, and the calcium content in the nickel-calcium alloy is 5-30%.
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| CN112522541B (en) * | 2019-09-17 | 2022-03-18 | 东北大学 | Nickel-based alloy desulfurizing agent and preparation method thereof |
| CN111411288B (en) * | 2020-03-19 | 2021-08-20 | 靖江新舟合金材料有限公司 | High-temperature alloy smelting method |
| CN112048631A (en) * | 2020-09-04 | 2020-12-08 | 江苏隆达超合金航材有限公司 | Nickel-chromium intermediate alloy for nickel-based high-temperature alloy and preparation method thereof |
| CN115612877B (en) * | 2022-10-10 | 2023-10-27 | 北京航空材料研究院股份有限公司 | Intelligent vacuum induction melting method for high-temperature alloy master alloy |
| CN117646127B (en) * | 2023-12-01 | 2024-06-28 | 美特林科航空科技(安徽)有限公司 | Purifying smelting method for carbon-free nickel-based monocrystal superalloy |
| CN117363960B (en) * | 2023-12-08 | 2024-03-08 | 成都先进金属材料产业技术研究院股份有限公司 | Low-carbon aluminum-free high-niobium-iron-based superalloy and preparation method thereof |
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