CN108546834B - Purification smelting method for nickel-based high-temperature alloy master alloy - Google Patents
Purification smelting method for nickel-based high-temperature alloy master alloy Download PDFInfo
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Abstract
A purification smelting method of a nickel-based superalloy master alloy comprises the following steps: (1) Performing hydrochloric acid and ultrasonic treatment on a metal raw material; preparing CaO-CaF2Pre-melting slag; uniformly mixing pre-melted slag and pure nickel powder and briquetting; (2) putting the raw materials and the pressing block into a crucible together, and vacuumizing; c, Nb, Ti and Al are added after melting; filling argon, adding B and Zr until the alloy liquid is melted again, and then pouring the alloy liquid into a steel mould to obtain a high-temperature alloy ingot; removing oxide skin and a riser of the cast ingot to obtain a high-temperature alloy concentrate; (3) putting the fine material into a copper crucible; vacuumizing, melting and quickly solidifying to obtain the high-temperature alloy master alloy. The invention carries out slag refining during vacuum induction smelting, and has low sulfur and phosphorus content; the copper crucible can avoid the pollution of the crucible to the alloy melt; magnetic suspension can promote the floating of nonmetallic inclusion; the contents of oxygen and nitrogen are low, so that the quantity of non-metallic inclusions formed in the cooling and solidification processes of the alloy liquid is reduced; the existing mature smelting equipment is utilized, and the operation is convenient.
Description
Technical Field
The invention belongs to the field of high-temperature alloy purification smelting, and relates to nickel-based high-temperature alloy smelting.
Background
The nickel-based high-temperature alloy is the preferred material of hot end parts (blades and turbine discs) of the aircraft engine, and the purity of the master alloy is a key factor influencing the service life of the master alloy. The purity of the master alloy comprises harmful elements such as oxygen, nitrogen, sulfur, phosphorus and the like and nonmetallic inclusions. Currently, the purification melting technology of superalloy master alloy is mainly Vacuum Induction Melting (VIM). The vacuum induction melting technology has the advantages of mature technology, simplicity, convenience and feasibility, and is widely applied to industrial production. However, for high temperature alloys requiring very high purity, the VIM technique still has the following disadvantages: pollution problems of ceramic crucibles; harmful elements such as sulfur, phosphorus and the like cannot be removed; non-metallic inclusions cannot be effectively removed.
The Vacuum Magnetic suspension smelting technology (VMLM) adopts a copper crucible as a reactor, molten steel is in a suspension state in the smelting process, and the pollution of the crucible wall to the molten steel is avoided; the large Lorentz force generated by the induction can well remove the inclusions; has the characteristics of high speed and high efficiency.
Aiming at the defects of Vacuum Induction Melting (VIM), the invention provides a purification melting technology of a nickel-based superalloy master alloy, namely a duplex melting technology of vacuum induction melting and vacuum magnetic suspension melting (VIM + VMLM).
Disclosure of Invention
The invention aims to provide a purification smelting technology of a nickel-based superalloy master alloy, and aims to improve the purity of the nickel-based superalloy master alloy. The chemical composition range of the nickel-based high-temperature alloy comprises a high-temperature alloy with nickel as a main element in the standard of GB/T14992-2005 high-temperature alloy and classification and mark of intermetallic compound high-temperature materials.
A method for purifying and smelting a nickel-based superalloy master alloy is characterized in that the superalloy comprises a superalloy taking nickel as a main element in the Standard of GB/T14992-2005 Classification and trade mark of superalloy and intermetallic compound superalloy; the specific process steps are as follows:
(1) raw material pretreatment and briquetting: the method comprises the following steps of pretreating blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, pure aluminum, pure titanium, pure iron, high-purity graphite, boron and zirconium serving as raw materials, wherein the purity of each raw material is more than 99.9%; preparation of CaF25-20 wt.% CaO-CaF2Melting the slag, preserving heat for 10-30 min, cooling, and mechanically crushing into pre-melted slag with the granularity of 0.1-5 mm; uniformly mixing pre-melted slag and pure nickel powder according to the mass ratio of 1: 1-1: 5, and pressing into blocks; baking the briquettes in a heat treatment furnace before use at the temperature of 200-300 ℃ for 6-10 hours to remove water in the briquettes;
(2) weighing the raw materials in the step (1) in proportion, and firstly, metal blocks of Ni, Cr, Co, W, Mo and Fe with lower affinity with O, N and CaO-CaF2Putting the pre-melted slag briquettes into a crucible for vacuum induction melting, and carrying out vacuum melting to obtain a high-temperature alloy ingot, wherein the briquettes account for 3-9 wt% of the alloy raw materials; the crucible is made of magnesium oxide;
(3) removing oxide skin and a riser of the high-temperature alloy ingot prepared in the step (2) to obtain a high-temperature alloy concentrate;
(4) and (4) putting the high-temperature alloy concentrate prepared in the step (3) into a copper crucible of a vacuum magnetic suspension smelting furnace to be smelted to obtain the high-temperature alloy master alloy.
Further, the pretreatment of the step (1) is: pretreating the metal raw material in a 5 vol.% hydrochloric acid aqueous solution to remove surface oxides, wherein the pretreatment time is 20-40 min; and (3) putting various metal raw materials subjected to hydrochloric acid treatment into absolute ethyl alcohol for ultrasonic treatment, wherein the treatment time is 10-20 min.
Further, the vacuum melting step in the step (2) is as follows: vacuum-pumping to 5 × 10-1Pa～5×10-3Pa, smelting; c is added after the melt is melted down, and refining is carried out for 15-30 min; adding strong nitride and oxide to form elements Nb, Ti and Al, and heating until the added materials are completely melted; and filling argon to 1.0-2.0 kPa, adding easily burnt and volatile trace elements B and Zr, and stirring simultaneously until the alloy liquid is completely melted again and then pouring into a steel die.
Further, the smelting step in the step (4) is as follows: vacuum-pumping to 5 × 10-3Pa, then filling high-purity argon to 0.01Pa, and repeating the step for three times to clean the vacuum chamber; melting at 1350-1450 deg.c for 10-20 min; and (3) adopting a water cooling mode to carry out rapid solidification.
The invention adopts a vacuum induction melting and vacuum magnetic suspension melting duplex melting process (VIM + VMLM), and has the following advantages compared with the prior art:
(1) CaO-CaF is added during vacuum induction smelting2Pre-melting slag, performing slag refining, and having low sulfur and phosphorus contents;
(2) the copper crucible can avoid the pollution of the crucible material to the alloy melt at high temperature during vacuum magnetic suspension smelting;
(3) the non-metallic inclusion can be promoted to float upwards by the Lorentz force generated by magnetic suspension, so that the non-metallic inclusion is effectively removed;
(4) the contents of oxygen and nitrogen are low, so that the quantity of non-metallic inclusions such as oxides, nitrides and the like formed in the processes of cooling and solidifying the alloy liquid is reduced;
(5) the method utilizes the existing mature smelting equipment and is convenient to operate.
Detailed Description
Example 1: FGH96 high-temperature alloy master alloy pure purification smelting
Blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, pure aluminum, pure titanium, high-purity graphite, boron, zirconium and the like are used as raw materials, and the purity of each raw material is more than 99.9%; pretreating the metal raw material in a 5 vol.% hydrochloric acid aqueous solution to remove surface oxides, wherein the pretreatment time is 30 min; then, various metal raw materials are put into absolute ethyl alcohol for ultrasonic treatment, and the treatment time is 15 min. Preparation of CaF210 wt.% CaO-CaF2And slag is subjected to premelting treatment, is kept for 25min after being completely melted, is cooled and is mechanically crushed into premelted slag with the granularity of 1 mm. And then uniformly mixing the pre-melted slag and the pure nickel powder according to the ratio of 1:1, and briquetting. The briquettes were baked at 220 ℃ for 7 hours before use to remove moisture. Firstly, putting elements Ni, Cr, Co, W, Mo and Fe with low affinity with O, N and a briquetting into a crucible of a vacuum induction melting furnace, wherein the briquetting accounts for wt.3% of the alloy raw materials; vacuum-pumping to 5 × 10-2Pa, smelting; c is added after the melt is melted down, and refining is carried out for 25 min; adding strong nitride and oxide to form elements Nb, Ti and Al, and heating until the added materials are completely melted; filling argon to 1.5kPa, finally adding easily burnt and volatile trace elements B and Zr, stirring simultaneously until the alloy liquid is completely melted again, and pouring into a steel die to obtain a high-temperature alloy ingot; removing oxide skin and a riser of the high-temperature alloy cast ingot to obtain a high-temperature alloy concentrate; putting the high-temperature alloy concentrate into a copper crucible of a vacuum magnetic suspension smelting furnace, and vacuumizing to 5 multiplied by 10-3Pa, then filling high-purity argon to 0.01Pa, and repeating the step for three times to clean the vacuum chamber; remelting at 1350-1450 ℃ for 10-20 min; and (3) rapidly solidifying in a water cooling mode to obtain the high-temperature alloy master alloy.
Example 2: FGH96 high-temperature alloy master alloy pure purification smelting
Using blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, pure aluminum and pure aluminumTitanium, high-purity graphite, boron, zirconium and the like are used as raw materials, and the purity of each raw material is more than 99.9%; pretreating the metal raw material in a 5 vol.% hydrochloric acid aqueous solution to remove surface oxides, wherein the pretreatment time is 30 min; then, various metal raw materials are put into absolute ethyl alcohol for ultrasonic treatment, and the treatment time is 15 min. Preparation of CaF215 wt.% CaO-CaF2And slag is subjected to premelting treatment, is kept for 25min after being completely melted, is cooled and is mechanically crushed into premelted slag with the granularity of 1 mm. And then uniformly mixing the pre-melted slag and the pure nickel powder according to the ratio of 1:2, and briquetting. The briquettes were baked at 230 ℃ for 8 hours before use to remove moisture. Firstly, putting elements Ni, Cr, Co, W, Mo and Fe with low affinity with O, N and a briquetting into a crucible of a vacuum induction smelting furnace, wherein the briquetting accounts for 5 wt% of alloy raw materials; vacuum-pumping to 5 × 10-2Pa, smelting; c is added after the melt is melted down, and refining is carried out for 25 min; adding strong nitride and oxide to form elements Nb, Ti and Al, and heating until the added materials are completely melted; filling argon to 1.5kPa, finally adding easily burnt and volatile trace elements B and Zr, stirring simultaneously until the alloy liquid is completely melted again, and pouring into a steel die to obtain a high-temperature alloy ingot; removing oxide skin and a riser of the high-temperature alloy cast ingot to obtain a high-temperature alloy concentrate; putting the high-temperature alloy concentrate into a copper crucible of a vacuum magnetic suspension smelting furnace, and vacuumizing to 5 multiplied by 10-3Pa, then filling high-purity argon to 0.01Pa, and repeating the step for three times to clean the vacuum chamber; remelting at 1350-1450 ℃ for 10-20 min; and (3) rapidly solidifying in a water cooling mode to obtain the high-temperature alloy master alloy.
Example 3: GH4169 high-temperature alloy master alloy pure smelting
Blocky pure nickel, pure chromium, pure molybdenum, pure niobium, pure aluminum, pure titanium, pure iron, high-purity graphite, boron, zirconium and the like are used as raw materials, and the purity of each raw material is more than 99.9%; pretreating the metal raw material in a 5 vol.% hydrochloric acid aqueous solution to remove surface oxides, wherein the pretreatment time is 25 min; then various metal raw materials are put into absolute ethyl alcohol for ultrasonic treatment,the treatment time was 15 min. Preparation of CaF2CaO-CaF with percentage content of weight.10 percent2And slag is subjected to premelting treatment, is kept for 25min after being completely melted, is cooled and is mechanically crushed into premelted slag with the granularity of 1 mm. And then uniformly mixing the pre-melted slag and the pure nickel powder according to the ratio of 1:1, and briquetting. The briquettes were baked at 220 ℃ for 7 hours before use to remove moisture. Firstly, putting elements Ni, Cr, Mo and Fe with low affinity with O, N and a briquetting into a crucible of a vacuum induction smelting furnace, wherein the briquetting accounts for 3 wt% of alloy raw materials; vacuum-pumping to 5 × 10-2Pa, smelting; c is added after the melt is melted down, and refining is carried out for 25 min; adding strong nitride and oxide to form elements Nb, Ti and Al, and heating until the added materials are completely melted; filling argon to 1.5kPa, finally adding easily burnt and volatile trace elements B and Zr, stirring simultaneously until the alloy liquid is completely melted again, and pouring into a steel die to obtain a high-temperature alloy ingot; removing oxide skin and a riser of the high-temperature alloy cast ingot to obtain a high-temperature alloy concentrate; putting the high-temperature alloy concentrate into a copper crucible of a vacuum magnetic suspension smelting furnace, and vacuumizing to 5 multiplied by 10-3Pa, then filling high-purity argon to 0.01Pa, and repeating the step for three times to clean the vacuum chamber; remelting at 1350-1450 ℃ for 10-20 min; and (3) rapidly solidifying in a water cooling mode to obtain the high-temperature alloy master alloy.
Example 4: GH4169 high-temperature alloy master alloy pure smelting
Blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, pure aluminum, pure titanium, pure iron, high-purity graphite, boron, zirconium and the like are used as raw materials, and the purity of each raw material is more than 99.9%; pretreating the metal raw material in a 5 vol.% hydrochloric acid aqueous solution to remove surface oxides, wherein the pretreatment time is 35 min; then, various metal raw materials are put into absolute ethyl alcohol for ultrasonic treatment, and the treatment time is 15 min. Preparation of CaF2CaO-CaF with percentage content of wt.15%2And slag is subjected to premelting treatment, is kept for 25min after being completely melted, is cooled and is mechanically crushed into premelted slag with the granularity of 1 mm. Then uniformly mixing the pre-melted slag and the pure nickel powder according to the ratio of 1:2, and briquetting. The briquettes were baked at 270 ℃ for 7 hours before use to remove moisture. Firstly, putting elements Ni, Cr, Co, W, Mo and Fe with low affinity with O, N and a briquetting into a crucible of a vacuum induction smelting furnace, wherein the briquetting accounts for 5 wt% of alloy raw materials; vacuum-pumping to 5 × 10-2Pa, smelting; c is added after the melt is melted down, and refining is carried out for 20 min; adding strong nitride and oxide to form elements Nb, Ti and Al, and heating until the added materials are completely melted; filling argon to 1.5kPa, finally adding easily burnt and volatile trace elements B and Zr, stirring simultaneously until the alloy liquid is completely melted again, and pouring into a steel die to obtain a high-temperature alloy ingot; removing oxide skin and a riser of the high-temperature alloy cast ingot to obtain a high-temperature alloy concentrate; putting the high-temperature alloy concentrate into a copper crucible of a vacuum magnetic suspension smelting furnace, and vacuumizing to 5 multiplied by 10-3Pa, then filling high-purity argon to 0.01Pa, and repeating the step for three times to clean the vacuum chamber; remelting at 1350-1450 ℃ for 10-20 min; and (3) rapidly solidifying in a water cooling mode to obtain the high-temperature alloy master alloy.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. The invention is also suitable for the purification smelting of other nickel-based high-temperature alloy master alloys. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (3)
1. A method for purifying and smelting a nickel-based superalloy master alloy is characterized in that the superalloy comprises a superalloy taking nickel as a main element in the Standard of GB/T14992-2005 Classification and trade mark of superalloy and intermetallic compound superalloy; the specific process steps are as follows:
(1) raw material pretreatment and briquetting: using blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium and pure aluminumThe method comprises the following steps of pretreating pure titanium, pure iron, high-purity graphite, boron and zirconium serving as raw materials, wherein the purity of each raw material is more than 99.9%; preparation of CaF25-20 wt.% CaO-CaF2Melting the slag, preserving heat for 10-30 min, cooling, and mechanically crushing into pre-melted slag with the granularity of 0.1-5 mm; uniformly mixing pre-melted slag and pure nickel powder according to the mass ratio of 1: 1-1: 5, and pressing into blocks; baking the briquettes in a heat treatment furnace before use at the temperature of 200-300 ℃ for 6-10 hours to remove water in the briquettes;
(2) weighing the raw materials in the step (1) in proportion, and firstly, metal blocks of Ni, Cr, Co, W, Mo and Fe with lower affinity with O, N and CaO-CaF2Putting the pre-melted slag briquettes into a crucible for vacuum induction melting, and carrying out vacuum melting to obtain a high-temperature alloy ingot, wherein the briquettes account for 3-9 wt% of the alloy raw materials; the crucible is made of magnesium oxide;
(3) removing oxide skin and a riser of the high-temperature alloy ingot prepared in the step (2) to obtain a high-temperature alloy concentrate;
(4) putting the high-temperature alloy concentrate prepared in the step (3) into a copper crucible of a vacuum magnetic suspension smelting furnace to be smelted to obtain a high-temperature alloy master alloy;
the pretreatment in the step (1) is as follows: pretreating the metal raw material in a 5 vol.% hydrochloric acid aqueous solution to remove surface oxides, wherein the pretreatment time is 20-40 min; and (3) putting various metal raw materials subjected to hydrochloric acid treatment into absolute ethyl alcohol for ultrasonic treatment, wherein the treatment time is 10-20 min.
2. The pure purification smelting method of the nickel-based superalloy master alloy as claimed in claim 1, wherein the vacuum smelting step in the step (2) is: vacuum-pumping to 5 × 10-1Pa～5×10-3Pa, smelting; c is added after the melt is melted down, and refining is carried out for 15-30 min; adding strong nitride and oxide to form elements Nb, Ti and Al, and heating until the added materials are completely melted; and filling argon to 1.0-2.0 kPa, adding easily burnt and volatile trace elements B and Zr, and stirring simultaneously until the alloy liquid is completely melted again and then pouring into a steel die.
3. The pure purification smelting method of the nickel-based superalloy master alloy as claimed in claim 1, wherein the smelting step in the step (4) is: vacuum-pumping to 5 × 10-3Pa, then filling high-purity argon to 0.01Pa, and repeating the step for three times to clean the vacuum chamber; melting at 1350-1450 deg.c for 10-20 min; and (3) adopting a water cooling mode to carry out rapid solidification.
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| CN106636848B (en) * | 2017-01-18 | 2018-06-15 | 东南大学 | A kind of preparation method of wear-resisting erosion resistance nickel-base alloy silk material |
| CN106884110B (en) * | 2017-03-27 | 2018-11-09 | 东南大学 | A kind of method that high vacuum electric arc furnaces prepares nickel base superalloy |
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