CN114293261B - Vacuum induction smelting process for ultra-high purity DD419 single crystal superalloy master alloy - Google Patents
Vacuum induction smelting process for ultra-high purity DD419 single crystal superalloy master alloy Download PDFInfo
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Abstract
The invention belongs to the technical field of alloy smelting, and particularly relates to a vacuum induction smelting process for an ultra-high purity DD419 single crystal superalloy master alloy, which is used for preparing the ultra-high purity DD419 single crystal superalloy master alloy through step-by-step feeding, primary refining, secondary refining and tertiary refining. The invention can remove O and N greatly by refining at high temperature once; al is added step by step, so that deep O removal can be realized; by reasonably controlling the Re size of the metal and the three refining processes, the Re component in the master alloy is uniform and has no segregation; adopting a desulfurization process, and reacting a desulfurizing agent with the interior of the alloy melt to remove S; the content of O, N, S and inclusions in the melt can be reduced to the maximum extent by adopting two ceramic filter screens with different specifications for filtering. By adopting the feeding mode and the vacuum induction smelting process, the smelting preparation of the ultra-high purity DD419 single crystal superalloy master alloy can be realized, wherein the O content in the prepared master alloy is lower than 4ppm, the N content is lower than 2ppm, the S content is lower than 4ppm, and the inclusion content is controlled to be 0.5 level.
Description
Technical Field
The invention belongs to the technical field of alloy smelting, and particularly relates to a vacuum induction smelting process for an ultra-high purity DD419 single crystal superalloy master alloy.
Background
DD419 single crystal superalloy is widely used as advanced aeroengine turbine blade material due to its excellent high temperature comprehensive properties. Along with the improvement of the temperature bearing capacity and the service life requirements of the DD419 single-crystal superalloy master alloy, the purity requirements of the DD419 single-crystal master alloy are higher and higher, and particularly the control requirements of the gas element O, N and the impurity element S are more strict. The ultra-high purity DD419 superalloy master alloy is a basic guarantee for obtaining the DD419 monocrystal superalloy casting which has excellent performance and meets the service condition.
The DD419 single crystal superalloy is a typical second generation single crystal superalloy, is equivalent to the foreign single crystal superalloy brand CMSX-4, has obvious gap between the current domestic content control of the DD419 single crystal alloy O, N, S and the foreign single crystal superalloy, and severely restricts the practical application and the further development of the DD419 single crystal superalloy in China.
The DD419 monocrystal superalloy contains 2.5-3.5 wt% Re element and no C element. The metal Re belongs to rare noble metals, is high in price, and is fed and smelted with other raw materials simultaneously, if the whole furnace alloy is scrapped due to the disqualification of other individual elements, the economic loss is serious, so that after the smelting alloying is finished, re element is added after all other elements are qualified by sampling and detecting, and the economic loss caused by the scrapping of the alloy can be avoided. In addition, the Re density of the metal is high, the melting point is high, and the Re content in the alloy ingot is easily unqualified or the composition segregation is easily caused by the later addition of the metal; if the refining temperature is increased and the refining time is prolonged to ensure the melting of the metal Re, the O content in the melt is increased, and how to realize the rapid and uniform melting of the metal Re in the melt needs to reasonably control the specification and the size of the metal Re and the refining process. In addition, the DD419 single crystal alloy does not contain C element, can not realize C deoxidation, is difficult to deoxidize during smelting, and is very important to deoxidize through a vacuum smelting process and a step-by-step Al adding process. Therefore, in order to realize the smelting preparation of the ultra-high purity DD419 single crystal superalloy master alloy, the development of a reasonable material distribution and feeding mode and a corresponding vacuum smelting process has very important engineering significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a vacuum induction smelting process for an ultra-high purity DD419 single crystal superalloy master alloy. By adopting the feeding mode and the vacuum induction melting process provided by the invention, the content of O in the DD419 monocrystal superalloy prepared by melting is lower than 4ppm, the content of N is lower than 2ppm, the content of S is lower than 4ppm, and the content of inclusion is 0.5 level.
In order to achieve the technical effects, the invention adopts the following technical scheme: an ultra-high purity DD419 single crystal superalloy master alloy vacuum induction melting process, wherein the DD419 single crystal superalloy comprises the following chemical components: 6.2 to 6.8 weight percent of Cr,0.3 to 0.9 weight percent of Mo,0.7 to 1.2 weight percent of Ti,5.3 to 5.8 weight percent of Al,9 to 10 weight percent of Co,0.07 to 0.15 weight percent of Hf,2.5 to 3.5 weight percent of Re,6.1 to 7.0 weight percent of Ta,6.0 to 6.8 weight percent of W and the balance of Ni, and the method specifically comprises the following steps:
(1) Feeding: charging all raw materials Ni, cr, co, mo, ta and W with lower affinity to O and N into a crucible according to the chemical composition of DD419 single crystal superalloy;
(2) Primary refining: after all the raw materials in the step (1) are added into a crucible, vacuumizing the crucible, heating the crucible by power, and heating the crucible in a step heating mode until the vacuum degree reaches 5 multiplied by 10 -2 Refining once at 1660-1680 deg.c for 30-40 min;
(3) Secondary refining: after the melt is cooled to surface conjunctiva after the primary refining is finished, adding Ti, hf and partial Al into the melt according to the chemical components of DD419 single crystal superalloy, when the vacuum degree reaches 1X 10 -1 Secondary refining is carried out when Pa and the temperature reaches 1470-1500 ℃, the refining time is 15-20 min, the stirring power is 260-300 kW, and after the secondary refining is finished, the chemical composition detection of the melt is carried out along with furnace sampling;
(4) And (3) refining for three times: after the sampling and detecting result in the step (3) is qualified, cooling the melt to surface conjunctiva, adding Re and residual Al into the melt according to the chemical components of the DD419 single crystal superalloy, and when the vacuum degree reaches 1 multiplied by 10 -1 When Pa and the temperature reaches 1530-1550 ℃, refining is carried out for three times, the refining time is 10-15 min, and the stirring power is 280-320 kW;
(5) After the three refining is finished, adding a desulfurizing agent into the melt, and pouring when the vacuum degree reaches 5Pa and the temperature reaches 1480-1520 ℃, so as to finish alloy smelting and obtain the ultra-high purity DD419 single crystal superalloy.
Further, the step heating in the step (1) is specifically:
when the vacuum degree reaches 20Pa, the power is 40-60 kW to exhaust the raw materials; when the vacuum degree reaches 5Pa, the power is sent to 150-200 kW, the power is kept for 20-25 min, the power is lifted to 350-400 kW, the power is kept for 30-40 min, the power is continuously lifted to 500-550 kW, the power is continuously lifted to 570-590 kW after all raw materials are completely melted, and the temperature of the melt is 1580-1600 ℃ and the temperature is kept for 15-20 min.
Further, the feeding sequence of the raw materials in the step (1) is as follows: the addition amount of Ni before adding part Ni, W, ta, mo, cr, co and the rest Ni, W is 20-40% of the required amount.
Further, the amount of Al added in step (3) was 99% of the desired amount.
Further, the desulfurizing agent is nickel-calcium alloy, and the adding amount of the desulfurizing agent is 0.5-1.0% of the total mass of the alloy.
Further, the raw material Re is a block metal, the length and width of the block metal Re are 15-30 mm, and the thickness of the block metal Re is 10-15 mm.
Further, when the step (5) is performed, a ceramic filter screen is adopted for filtering, the ceramic filter screen is assembled into a chute for use, and the ceramic filter screen is assembled in a mode of 15-20PPI+20-30 PPI.
Further, the ultra-high purity DD419 single crystal superalloy has an O content of less than 4ppm, an N content of less than 2ppm, an S content of less than 4ppm and an inclusion content of 0.5 level.
The invention name of the application "DD419" in the ultra-high purity DD419 single crystal superalloy master alloy vacuum induction smelting process "only refers to the brand of a metal, and the metal components corresponding to the brand are the components: "6.2-6.8 wt% Cr, 0.3-0.9 wt% Mo, 0.7-1.2 wt% Ti, 5.3-5.8 wt% Al, 9-10 wt% Co, 0.07-0.15 wt% Hf, 2.5-3.5 wt% Re, 6.1-7.0 wt% Ta, 6.0-6.8 wt% W, the balance Ni,".
Compared with the prior art, the technical scheme of the embodiment of the invention has the beneficial effects that:
(1) The invention adopts one-time high-temperature refining, and simultaneously, the melt is greatly deo and N-removed under the high vacuum condition.
(2) The Re element in the prepared master alloy is uniformly distributed and has no segregation by reasonably controlling the Re specification and size of the raw material and the three refining processes.
(3) According to the invention, the raw material Re is added at the end of alloying, so that economic loss caused by unqualified other elements can be effectively reduced.
(4) The invention adopts a mode of adding Al step by step to realize deep O removal.
(5) According to the invention, the alloy liquid is filtered by adopting 15-20 PPI+20-30 PPI ceramic filter screens with two different specifications during casting, so that the content of O, N, S and inclusions in the alloy can be reduced to the greatest extent.
(6) By adopting the feeding mode and the vacuum induction smelting process provided by the invention, the content of O in the DD419 monocrystal superalloy prepared by smelting is lower than 4ppm, the content of N is lower than 2ppm, the content of S is lower than 4ppm, and the content of inclusions is 0.5 level.
Detailed Description
The technical scheme of the invention is further described in detail below with reference to examples.
Example 1
The DD419 single crystal superalloy of the embodiment comprises the following element components in percentage by weight: 6.2wt% Cr,0.3 wt% Mo,0.7 wt% Ti,5.3 wt% Al, 9.0wt% Co,0.07 wt% Hf,2.5 wt% Re,6.1 wt% Ta,6.0 wt% W, the balance Ni, and single furnace melting 2000kg of the alloy.
The vacuum induction smelting process of the ultra-high purity DD419 monocrystal superalloy master alloy specifically comprises the following steps:
(1) Feeding: according to the chemical composition of DD419 single crystal superalloy, all raw materials Ni, cr, co, mo, ta and W with lower affinity to O and N are filled into a crucible, and the filling sequence is as follows: 20% of the required Ni, W, ta, mo, cr, co and the rest Ni;
(2) Primary refining: after the raw materials are all added into the crucible, vacuumizing and power-feeding heating are carried out, and a step heating mode is adopted for heating, specifically: when the vacuum degree reaches 20Pa, the raw materials are exhausted by delivering 40kW of power; when the vacuum degree reaches 5Pa, the power is sent to 150kW for 25min, the power is lifted to 350kW for 40min, the power is continuously lifted to 500kW, and the vacuum degree is kept until allAfter the raw materials are completely melted, continuously increasing the power to 570kW, and keeping the melt temperature at 1580 ℃ for 20min; when the vacuum degree reaches 5X 10 -2 Refining for 40min at 1660deg.C under Pa;
(3) Secondary refining: after the melt is cooled to surface conjunctiva after the primary refining is finished, adding 99% of Ti, hf and required Al into the melt according to the chemical components of the DD419 single crystal superalloy; when the vacuum degree reaches 1X 10 -1 Secondary refining is carried out when Pa and the temperature reaches 1470 ℃, the refining time is 20min, and the stirring power is 260kW; after secondary refining is finished, sampling along with a furnace to detect chemical components of the melt;
(4) And (3) refining for three times: after the sampling detection result in the step (3) is qualified, cooling the melt to form a surface film, adding Re and residual Al into the melt according to the chemical composition of the DD419 single crystal superalloy, wherein the raw material Re is blocky metal, and the blocky metal Re has the length and the width of 15mm and the thickness of 10mm; when the vacuum degree reaches 1X 10 -1 When Pa, refining temperature is 1530 ℃, refining is carried out for three times, refining time is 15min, and stirring power is 280kW; after the three refining is finished, adding a desulfurizing agent nickel-calcium alloy into the melt, wherein the adding amount of the desulfurizing agent is 0.5 weight percent of the total mass of the alloy;
(5) Before alloy casting, a 15+30PPI ceramic filter screen is assembled into a chute for use, and casting is carried out when the vacuum degree reaches 5Pa and the temperature is 1480 ℃, so that alloy smelting is completed, and the ultra-high purity DD419 single crystal superalloy is obtained.
Example 2
The DD419 single crystal superalloy of the embodiment comprises the following element components in percentage by weight: 6.5wt% Cr, 0.6wt% Mo, 1.0wt% Ti, 5.5wt% Al, 9.6wt% Co, 0.10wt% Hf, 3.0wt% Re, 6.5wt% Ta, 6.4wt% W, the balance Ni, and single furnace melting 2000kg of alloy.
A vacuum induction smelting process for ultra-high purity DD419 single crystal superalloy master alloy comprises the following steps:
(1) Feeding: all raw materials Ni, cr, co, mo, ta and W with lower affinity to O and N are filled into a crucible according to the chemical composition of DD419 single crystal superalloy, and the filling sequence is as follows: 30% of the required Ni, W, ta, mo, cr, co and the rest Ni;
(2) Primary refining: after the raw materials are all added into the crucible, vacuumizing and power-feeding heating are carried out, and a step heating mode is adopted for heating, specifically: when the vacuum degree reaches 20Pa, the raw materials are exhausted by delivering 50kW of power; when the vacuum degree reaches 5Pa, the power is sent to 180kW and kept for 22min, the power is lifted to 380kW and kept for 35min, the power is continuously lifted to 530kW, after all the raw materials are completely melted, the power is continuously lifted to 580kW, and the temperature of the melt is 1590 ℃ and kept for 18min; when the vacuum degree reaches 5X 10 -2 Refining for 35min at 1670deg.C under Pa;
(3) Secondary refining: after the melt is cooled to surface conjunctiva after the primary refining is finished, adding 99 percent of Ti, hf and the required Al into the melt according to the chemical components of the DD419 single crystal superalloy, and when the vacuum degree reaches 1 multiplied by 10 -1 Secondary refining is carried out at the Pa and the temperature of 1490 ℃ for 18min, and the stirring power is 280kW; after secondary refining is finished, sampling along with a furnace to detect chemical components of the melt;
(4) And (3) refining for three times: after the sampling and detecting result in the step (3) is qualified, cooling the melt to form a film on the surface, adding Re and the rest Al into the melt according to the chemical composition of the DD419 single crystal superalloy, wherein the Re is bulk metal, and the Re length and the Re width of the bulk metal are 25mm and the thickness is 13mm; when the vacuum degree reaches 1X 10 -1 At Pa, refining temperature of 1540 ℃, refining for three times, refining time of 13min and stirring power of 300kW; after the three refining is finished, adding a desulfurizing agent nickel-calcium alloy into the melt, wherein the adding amount of the desulfurizing agent is 0.8wt% of the total mass of the alloy;
(5) Before alloy casting, a 15+20PPI ceramic filter screen is assembled into a chute for use, and casting is carried out when the vacuum degree reaches 5Pa and the temperature is 1500 ℃, so that alloy smelting is completed, and the ultra-high purity DD419 single crystal superalloy is obtained.
Example 3
In the embodiment, the content of the element components in the DD419 single crystal superalloy is as follows: 6.8wt% Cr, 0.9wt% Mo, 1.2wt% Ti, 5.8wt% Al, 10.0wt% Co, 0.15wt% Hf, 3.5wt% Re, 6.9wt% Ta, 6.8wt% W, ni, the balance being, single furnace smelted 2000kg alloy.
A vacuum induction smelting process for ultra-high purity DD419 single crystal superalloy master alloy comprises the following steps:
(1) Feeding: all raw materials Ni, cr, co, mo, ta and W with lower affinity to O and N are filled into a crucible according to the chemical composition of DD419 single crystal superalloy, and the filling sequence is as follows: 40% of the required Ni, W, ta, mo, cr, co and the rest Ni;
(2) Primary refining: after the raw materials are all added into the crucible, vacuumizing and power-feeding heating are carried out, and a step heating mode is adopted for heating, specifically: when the vacuum degree reaches 20Pa, the raw materials are exhausted by delivering power of 60kW; when the vacuum degree reaches 5Pa, the power is sent to 200kW and kept for 20min, the power is lifted to 400kW and kept for 30min, the power is continuously lifted to 550kW, after all the raw materials are completely melted, the power is continuously lifted to 590kW, and the temperature of the melt is 1600 ℃ and kept for 15min; when the vacuum degree reaches 5X 10 -2 In Pa, refining for 30min at 1680 deg.C;
(3) Secondary refining: after the primary refining is finished, cooling the melt to a surface conjunctiva, and adding 99% of Ti, hf and required Al into the melt according to the chemical components of the DD419 single crystal superalloy; when the vacuum degree reaches 1X 10 -1 When Pa, refining temperature is 1500 ℃, secondary refining is carried out, refining time is 15min, and stirring power is 300kW; after secondary refining is finished, sampling along with a furnace to detect chemical components of the melt;
(4) And (3) refining for three times: after the sampling and detecting result in the step (3) is qualified, cooling the melt to form a film on the surface, adding Re and the rest Al into the melt according to the chemical composition of the DD419 single crystal superalloy, wherein the Re is bulk metal, and the Re length and the Re width of the bulk metal are both 30mm and the thickness is 15mm; when the vacuum degree reaches 1X 10 -1 When Pa, refining temperature is 1550 ℃, refining is carried out for three times, refining time is 10min, and stirring power is 320kW; after the three refining is finished, adding a desulfurizing agent nickel-calcium alloy into the melt, wherein the adding amount of the desulfurizing agent is 1.0wt% of the total mass of the alloy;
(5) Before alloy casting, a 20+30PPI ceramic filter screen is assembled into a chute for use, and casting is carried out when the vacuum degree reaches 5Pa and the casting temperature is 1520 ℃, so that alloy smelting is completed, and the ultra-high purity DD419 single crystal superalloy is obtained.
The results of measuring O, N, S content and total content and inclusion content in DD419 single crystal superalloy master alloy prepared by smelting in examples 1-3 are shown in Table 1.
Table 1 examples 1-3 preparation of DD419 alloys and foreign advanced level comparison tables
As is clear from Table 1, in the DD419 single crystal superalloy master alloys prepared by smelting in examples 1 to 3 of the present invention, the O content is less than 4ppm, the N content is less than 2ppm, the S content is less than 4ppm, the total content of O and N, S is less than 10ppm, the inclusion content is 0.5 grade, which is equivalent to the advanced foreign level, indicating that the present invention realizes the preparation of the ultra-high purity DD419 single crystal superalloy master alloys.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications and equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, and all such modifications and equivalents are intended to be encompassed in the scope of the claims of the present invention.
Claims (8)
1. The vacuum induction smelting process of the ultra-high purity DD419 single crystal superalloy master alloy is characterized in that the DD419 single crystal superalloy comprises the following chemical components: 6.2 to 6.8wt% of Cr,0.3 to 0.9wt% of Mo,0.7 to 1.2wt% of Ti,5.3 to 5.8wt% of Al,9 to 10wt% of Co,0.07 to 0.15wt% of Hf,2.5 to 3.5wt% of Re,6.1 to 7.0wt% of Ta,6.0 to 6.8wt% of W and the balance of Ni, and the method specifically comprises the following steps:
(1) Feeding: charging all raw materials Ni, cr, co, mo, ta and W with lower affinity to O and N into a crucible according to the chemical composition of DD419 single crystal superalloy;
(2) Primary refining: after all the raw materials in the step (1) are added into a crucible, vacuumizing the crucible, heating the crucible by power, and heating the crucible in a step heating mode until the vacuum degree reaches 5 multiplied by 10 -2 When Pa and the temperature reaches 1660-1680 ℃, refining for 30-40 min;
(3) Secondary refining: after the melt is cooled to surface conjunctiva after the primary refining is finished, adding Ti, hf and partial Al into the melt according to the chemical components of DD419 single crystal superalloy, when the vacuum degree reaches 1X 10 -1 When Pa and the temperature reaches 1470-1500 ℃, secondary refining is carried out, the refining time is 15-20 min, the stirring power is 260-300 kW, and after the secondary refining is finished, the melt chemical component detection is carried out along with furnace sampling;
(4) And (3) refining for three times: after the sampling and detecting result in the step (3) is qualified, cooling the melt to surface conjunctiva, adding Re and residual Al into the melt according to the chemical components of the DD419 single crystal superalloy, and when the vacuum degree reaches 1 multiplied by 10 -1 When Pa and the temperature reaches 1530-1550 ℃, refining for three times, wherein the refining time is 10-15 min, and the stirring power is 280-320 kW;
(5) After the three refining is finished, adding a desulfurizing agent into the melt, and pouring when the vacuum degree reaches 5Pa and the temperature reaches 1480-1520 ℃, so as to finish alloy smelting and obtain the ultra-high purity DD419 single crystal superalloy.
2. The ultra-high purity DD419 single crystal superalloy master alloy vacuum induction melting process as claimed in claim 1, wherein the step heating in step (1) is specifically:
when the vacuum degree reaches 20Pa, the power is 40-60 kW, and the raw materials are exhausted; when the vacuum degree reaches 5Pa, the power is sent to 150-200 kW, the power is kept for 20-25 min, the power is lifted to 350-400 kW, the power is kept for 30-40 min, the power is continuously lifted to 500-550 kW, after all raw materials are completely melted, the power is continuously lifted to 570-560 kW, and the temperature of a melt is 1580-1600 ℃ and is kept for 15-20 min.
3. The ultra-high purity DD419 single crystal superalloy master alloy vacuum induction melting process as claimed in claim 1, wherein the raw materials are fed sequentially in the following order in step (1): the addition amount of Ni before adding part Ni, W, ta, mo, cr, co and the rest Ni and W is 20-40% of the required amount.
4. The ultra-high purity DD419 single crystal superalloy master alloy vacuum induction melting process as claimed in claim 1, wherein the amount of Al added in step (3) is 99% of the desired amount.
5. The vacuum induction melting process of an ultra-high purity DD419 single crystal superalloy master alloy according to claim 1, wherein the desulfurizing agent is nickel-calcium alloy, and the adding amount of the desulfurizing agent is 0.5-1.0% of the total mass of the alloy.
6. The vacuum induction melting process of an ultra-high purity DD419 single crystal superalloy master alloy according to claim 1, wherein the raw material Re is a bulk metal, the length and width of the bulk metal Re are 15-30 mm, and the thickness of the bulk metal Re is 10-15 mm.
7. The vacuum induction melting process of the ultra-high purity DD419 single crystal superalloy master alloy according to claim 1, wherein in the casting in the step (5), a ceramic filter screen is adopted for filtering, the ceramic filter screen is assembled into a chute for use, and the ceramic filter screen is assembled in a manner of 15-20 PPI+20-30 PPI.
8. The ultra-high purity DD419 single crystal superalloy master alloy vacuum induction melting process as claimed in claim 1, wherein the ultra-high purity DD419 single crystal superalloy has an O content of less than 4ppm, an n content of less than 2ppm, an s content of less than 4ppm, and an inclusion content of 0.5 grade.
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| RU2274671C1 (en) * | 2004-10-05 | 2006-04-20 | Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" (ФГУП "ВИАМ") | Method of production of the carbon-free casting high-temperature alloys |
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| CN109811155A (en) * | 2017-11-20 | 2019-05-28 | 薛红剑 | A kind of copper base high temperature alloy utilizes electromagnetic induction fast melting technique |
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| RU2274671C1 (en) * | 2004-10-05 | 2006-04-20 | Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" (ФГУП "ВИАМ") | Method of production of the carbon-free casting high-temperature alloys |
| CN107190158A (en) * | 2017-05-19 | 2017-09-22 | 江苏隆达超合金航材有限公司 | Reduce the vacuum induction melting technique of O, N, S content in nickel base superalloy |
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