CN117684032B - Preparation process of novel high-temperature nickel alloy with fine grain size - Google Patents
Preparation process of novel high-temperature nickel alloy with fine grain size Download PDFInfo
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Abstract
The invention belongs to the field of metal material processing, and in particular relates to a preparation process of a novel high-temperature nickel alloy with fine grain size, which comprises 7 steps of S1: weighing according to the high-temperature nickel alloy raw material powder formula, and processing to obtain uniformly refined nickel-based mixed powder; s2: placing the mixed powder into a stainless steel sleeve, carrying out degassing treatment, and then placing into a hot isostatic press for sintering to form a bar blank; s3: smelting the rod blank in a smelting furnace, refining at high temperature and low temperature, remelting and refining, and casting into alloy ingots; s4: annealing the alloy ingot, forging and rolling to prepare an alloy wire rod; s5: carrying out surface treatment on the alloy wire rod; s6: multiple pass drawing-annealing; s7: and (5) carrying out solid solution-aging treatment. The high-temperature nickel alloy prepared by the process has fine grain size and small grade difference, and has great industrial value.
Description
Technical Field
The invention belongs to the field of metal material processing, and particularly relates to a preparation process of a fine grain size high-temperature nickel alloy.
Background
With the progress of heavy industry technology in China, nuclear industry and aerospace technology in China are also developed, the requirements on the performance of metal materials are higher, the working environments of the nuclear industry and aircrafts are harsh, and new and higher requirements on the high strength of the metal materials are provided for a long time under the working environments of high temperature and high pressure.
Ni is used as a main element of the current high-temperature alloy material, is an alloy element which can not only improve the strength of the alloy material but also not obviously weaken the plasticity of the material, and has extremely excellent high-temperature resistance, oxidation resistance and corrosion resistance.
In practical application, a workpiece obtained by processing the high-temperature nickel alloy for multiple times can generate a cracking phenomenon, metallographic analysis shows that the alloy grain size with the cracking problem is of grade 4-6, the alloy grain size is abnormal coarse grains, the grain size difference of products in the same batch is overlarge, and if the product with larger grain size difference is not subjected to differentiation treatment, the obtained product has inconsistent performance, and the performance of the material is directly influenced.
The grain size of the metal material has great influence on the mechanical property and the technological property of the metal, generally, the finer and more uniform the grains are in a normal temperature state, the better the comprehensive performance of the material is, and the performance of the material can be primarily judged through the grain size. The finer the grain of the metal, the higher its strength and hardness. Because the finer the metal grains, the larger the total area of grain boundaries, the more dislocation barriers, and the more grains with different orientations that need to be coordinated, the higher the resistance to plastic deformation of the metal.
The finer the grain of the metal, the higher its plasticity and toughness. Because the finer the grains, the more the number of grains per unit volume, the more the number of grains involved in deformation, the more uniform the deformation, resulting in greater plastic deformation before fracture. The strength and the plasticity are increased simultaneously, and the work consumed by the metal before fracture is also larger, so that the toughness is also better. Therefore, the development of a preparation process of the fine grain size high-temperature nickel alloy is significant.
Disclosure of Invention
The invention aims to provide a preparation process of a fine-grain-size high-temperature nickel alloy, aiming at the problems that the grains of the high-temperature nickel alloy produced in the prior art are coarse and the grade difference is large, and the performance of a product is seriously affected.
In order to achieve the above purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
A preparation process of a fine grain size high temperature nickel alloy comprises the following steps:
S1: weighing according to the mass percentage of the high-temperature nickel alloy raw material powder formula, and processing to obtain uniformly refined nickel-based mixed powder;
s2: placing the mixed powder into a stainless steel sleeve, reserving a certain space, degassing, and then placing into a hot isostatic pressing machine to sinter into a bar blank;
s3: smelting the rod blank in a smelting furnace, refining at high temperature and low temperature, remelting and refining, and casting into alloy ingots;
s4: annealing the alloy ingot, forging and rolling to prepare an alloy wire rod;
S5: carrying out surface treatment on the alloy wire rod;
S6: multiple pass drawing-annealing;
s7: and (5) carrying out solid solution-aging treatment.
Preferably, the high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0%, nb:2.0-3.0%, Y:0.30-0.35%, al:1.0-2.0% and Ni balance.
Preferably, the treatment process in the step S1 is to add raw material powder except Y, al powder into ethanol, magnetically stir for 2h at 2000r/min, and then place the raw material powder into 50KHz ultrasonic treatment for 2h to obtain ethanol suspension; filtering, taking insoluble substances, and placing the insoluble substances in a drying oven at 80 ℃ for drying treatment for 2 hours to obtain mixed powder; putting the mixed powder into a ball milling tank, adding long-chain fatty acid, and putting the ball milling tank on a high-energy ball mill for ball milling treatment, wherein the grinding balls are corundum balls, and the mass ratio of the grinding balls is 5-8:1, ball milling process is carried out for 5-10 hours, and the rotating speed of a ball milling tank is 150 200r/min;
The dosage ratio of the long-chain fatty acid to the total mass of the raw material powder is 2g:100g.
Preferably, the long chain fatty acid is myristic acid or lauric acid.
Preferably, the degassing treatment process in the step S2 is that the furnace temperature is kept at 660 700 ℃, the vacuum degree is less than 0.1Pa, and the temperature is kept for 6-8 hours; the sintering process is to heat to 1220 1280 ℃ at a heating rate of 25 ℃/min, then apply 150MPa gas pressure to the surface, and keep the surface at constant pressure and constant temperature for 4 hours and cool along with the furnace, thus obtaining cylindrical powder sintered rod blank with phi of 40-50 mm.
Preferably, the high-temperature refining in the step S3 is carried out at 1750-1850 ℃ for 30-45min, and the heating rate is 15-25 ℃/min; cooling to 1650-1700 ℃ and refining and smelting for 15-25min at low temperature; adding the treated Y powder and Al powder in the later stage of low-temperature refining, and uniformly stirring; the remelting is electroslag remelting, and the temperature of a melting furnace is 1750-1850 ℃.
Preferably, the annealing process in the step S4 is to heat to 1000-1050 ℃ and keep the temperature for 20-35h; the forging process is that an alloy blank I is formed by cogging and forging at 900-950 ℃, the forging ratio is 3-4, an alloy blank II is formed by forging at 1000-1050 ℃ after tempering and heating for 1-2h at 950-1000 ℃, the forging ratio is 7-8, and an alloy blank III is formed by forging at 1000-1050 ℃, and the forging ratio is 3-4; the rolling process is to heat-preserving for 0.5-1.5h at 1000-1050 ℃ and hot-rolling for phi 4.0-5.0mm alloy wire rod at 950-1100 ℃; the temperature rising rate in the step S4 is 10-15 ℃/min.
Preferably, the S5 surface treatment is to heat the alloy wire rod to 950 ℃ and keep the temperature for 1.5 hours, and the alloy wire rod is subjected to oil cooling for softening treatment, pickling and then ultrasonic cleaning.
Preferably, the drawing-annealing in the step S6 is performed, a lubricant is added before drawing, and then the drawing processing is performed for multiple times, so that an alloy wire with the diameter of phi 1.0-1.5mm is obtained; the annealing is to carry out vacuum annealing after carrying out drawing for 9-11 times, and the annealing temperature is 850-950 ℃.
Preferably, the solid solution-aging treatment in the step S7 is to heat to 950-1000 ℃ in a nitrogen environment, keep the temperature for 2-3h, continue to heat to 1020-1070 ℃, keep the temperature for 2-3h, and rapidly quench to obtain solid solution alloy; the aging is heating to 800-850 ℃, preserving heat for 3-8h, air cooling, heating to 750-770 ℃ again, preserving heat for 10-15h, and air cooling; the temperature rising rate of the solid solution-aging treatment is 3-5 ℃/min.
The invention has the following beneficial effects:
(1) The invention provides a preparation process of fine grain size high-temperature nickel alloy, which adopts a ball milling method to refine powder grains in a metal powder stage and reduces atomic stacking density in an initial stage of raw materials; meanwhile, long-chain fatty acid is used as a ball milling medium, and the ball milling medium has three functions: firstly, the particles can react and adsorb on the surfaces of the particles to form an organic protective layer which has lubricating effect; secondly, the existence of the organic protective layer solves the problem of agglomeration caused by the increase of surface activity after the powder particles are thinned after ball milling; and thirdly, volatilizing, carbonizing and separating out the organic protective layer in the later high-temperature smelting process, wherein carbon is a deoxidizer, so that the metal mixed solution can be further purified, and the purity is ensured. In addition, the grinding balls are made of corundum, are mainly made of alumina, and cannot introduce other impurities in the ball milling and refining process.
(2) The invention provides a preparation process of fine grain size high temperature nickel alloy, which adopts a chemical treatment method, nb powder is added into an alloy formula, and Y powder and Al powder are added in the smelting process. When Nb element is heated before forging, carbon nitrogen compound particles forming trace Nb are pinned to migrate to prevent the growth of grains. The Al element is a strong deoxidizer on one hand, can supplement insufficient deoxidizing capability of carbon, and further reduces the oxygen content of the metal mixed solution; on the other hand, dispersed gamma' phase can be formed to refine crystal grains. The Y element is enriched on the surface of the crystal boundary in the solidification process due to the small equilibrium distribution coefficient, so that the growth of crystals is prevented, and more cores are formed in the solidification process of the high-temperature molten metal, thereby achieving the purpose of grain refinement; for the same material, the finer the as-cast grains of the alloy, the finer the grains of the rolled product; secondly, the oxygen sulfide is formed by coordination reaction with O, S and other elements in the smelting process, the melting point is very high and stable, the oxygen sulfide can be removed after sedation, and the obtained alloy has higher purity and has the impurity removal and purification effects.
(3) The invention provides a preparation process of fine grain size high-temperature nickel alloy, which adopts gradient heating and multiple forging, namely a thermomechanical treatment process. On one hand, the multiple forging plays a role in mechanical crushing, eliminates primary coarse grains and improves the as-cast structure; on the other hand, the deformation recrystallization process is generated, new grains are re-nucleated and grown at the original coarse grain boundary, and the grains are fully refined.
(4) The invention provides a preparation process of fine grain size high-temperature nickel alloy, which adopts graded solid solution treatment, and maintains the temperature for a period of time at different temperatures, thereby regulating and controlling the grain size distribution uniformity of grains, effectively controlling the grain size uniformity and reducing the grain size difference. The size, the number and the distribution of the strengthening phases are adjusted by adopting the graded aging treatment, and coarse gamma 'phases and fine gamma' phases are dispersed and separated out simultaneously, so that the method has the best comprehensive performance.
(5) The invention provides a preparation process of fine grain size high-temperature nickel alloy, which adopts larger heating and cooling rate in the refining-remelting-forging-hot rolling process to destroy coarse grains which are preferentially generated, thereby achieving refined and uniform fine grains.
(6) The invention provides a preparation process of fine grain size high temperature nickel alloy, which combines a ball milling method, a chemical treatment method (namely adding a grain refiner), a thermomechanical treatment process and rapid temperature rise and reduction and fractional multiple solid solution-aging treatment to obtain a high temperature nickel alloy product with fine grain size and small grade difference.
Detailed Description
The present invention will be described in detail with reference to examples. It is to be understood that the following examples are illustrative of embodiments of the present invention and are not intended to limit the scope of the invention.
Example 1
A preparation process of a fine grain size high temperature nickel alloy comprises the following steps:
S1: weighing according to the mass percentage of the high-temperature nickel alloy raw material powder formula, and processing to obtain uniformly refined nickel-based mixed powder;
The high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0%, nb:2.2%, Y:0.35%, al:1.5% and Ni balance.
The treatment process in the step S1 is that raw material powder except Y, al powder is added into ethanol, and after being magnetically stirred for 2 hours at 2000r/min, the raw material powder is placed in 50KHz ultrasonic treatment for 2 hours, so as to obtain ethanol suspension; filtering, taking insoluble substances, and placing the insoluble substances in a drying oven at 80 ℃ for drying treatment for 2 hours to obtain mixed powder; placing the mixed powder into a ball milling tank, adding myristic acid, and placing the ball milling tank on a high-energy ball mill for ball milling treatment, wherein the grinding balls are corundum balls, and the mass ratio of the grinding balls is 7:1, ball milling process is carried out for 10 hours, and the rotating speed of a ball milling tank is 150r/min;
the dosage ratio of the myristic acid to the total mass of the raw material powder is 2g:100g.
S2: placing the mixed powder in a stainless steel sleeve, reserving a distance space with the upper and lower 20mm, carrying out degassing treatment under the conditions that the furnace temperature is kept at 700 ℃ and the vacuum degree is less than 0.1Pa and is kept for 6 hours, then placing the mixed powder in a hot isostatic pressing machine, heating to 1280 ℃ at a heating rate of 25 ℃/min, then applying the gas pressure of 150MPa to the surface, and keeping the temperature for 4 hours under constant pressure and constant temperature and cooling along with the furnace to obtain a cylindrical powder sintering bar blank with the diameter of 40 mm.
S3: smelting the rod blank in a smelting furnace at 1800 ℃ for 30min at a heating rate of 20 ℃/min; cooling to 1650 ℃ and refining and smelting for 25min at low temperature; adding the ball-milled Y powder and Al powder before finishing low-temperature refining, and uniformly stirring; then adopting electroslag remelting refining, wherein the temperature of a melting furnace is 1850 ℃, the filling coefficient is 0.4, and casting into an alloy ingot;
S4: annealing the alloy ingot, wherein the process is to heat to 1050 ℃, and preserving heat for 20 hours; forging after annealing, wherein the process is that an alloy blank I is formed by cogging and forging at 950 ℃, the forging ratio is 4, an alloy blank II is formed by forging at 1050 ℃ after tempering and heating at 1000 ℃ for 1h, the forging ratio is 7, and an alloy blank III is formed by forging at 1050 ℃, and the forging ratio is 4; then rolling, wherein the process is to heat-preserving for 0.5h at 1050 ℃ and hot-rolling into phi 4.0mm alloy wire rods at 1100 ℃; the temperature rising rate is 15 ℃/min.
S5: heating the alloy wire rod to 950 ℃, preserving heat for 1.5h, performing oil cooling for softening treatment, washing with acid (5 wt% of hydrofluoric acid, 10wt% of nitric acid and 85wt% of water) at 70 ℃ for 1h, quickly lifting after pickling, and immersing in water at 80 ℃ for cleaning; then the mixture is subjected to ultrasonic treatment for 2 hours at 50 KHz.
S6: adding a lubricant (80% calcium stearate and 20% lime powder) before drawing, and carrying out multi-pass drawing processing to obtain an alloy wire with the diameter of 1.0 mm; the annealing is to carry out vacuum annealing after carrying out drawing for 10 times, and the annealing temperature is 850 ℃.
S7: heating to 980 ℃ in a nitrogen environment, preserving heat for 2.5h, continuously heating to 1050 ℃, preserving heat for 2.5h, and rapidly performing water quenching to obtain solid-solution alloy; the aging is heating to 850 ℃, preserving heat for 3 hours, air-cooling, heating to 760 ℃ again, preserving heat for 12 hours, and air-cooling; the temperature rising rate of the solid solution-aging treatment is 4 ℃/min.
Example 2
A preparation process of a fine grain size high temperature nickel alloy comprises the following steps:
S1: weighing according to the mass percentage of the high-temperature nickel alloy raw material powder formula, and processing to obtain uniformly refined nickel-based mixed powder;
The high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0%, nb: 3.0%, Y:0.30%, al:1.0% and Ni balance.
The treatment process in the step S1 is that raw material powder except Y, al powder is added into ethanol, and after being magnetically stirred for 2 hours at 2000r/min, the raw material powder is placed in 50KHz ultrasonic treatment for 2 hours, so as to obtain ethanol suspension; filtering, taking insoluble substances, and placing the insoluble substances in a drying oven at 80 ℃ for drying treatment for 2 hours to obtain mixed powder; placing the mixed powder into a ball milling tank, adding myristic acid, and placing the ball milling tank on a high-energy ball mill for ball milling treatment, wherein the grinding balls are corundum balls, and the mass ratio of the grinding balls is 5:1, ball milling process is carried out for 10 hours, and the rotating speed of a ball milling tank is 200r/min;
the dosage ratio of the myristic acid to the total mass of the raw material powder is 2g:100g.
S2: placing the mixed powder in a stainless steel sleeve, reserving a distance space of 20mm from top to bottom, carrying out degassing treatment under the conditions that the furnace temperature is kept at 660 ℃, the vacuum degree is less than 0.1Pa, and keeping for 8 hours, then placing the mixed powder in a hot isostatic pressing machine, heating to 1220 ℃ at a heating rate of 25 ℃/min, then applying gas pressure of 150MPa to the surface, and keeping for 6 hours under constant pressure and constant temperature for cooling along with the furnace, thus obtaining a cylindrical powder sintered rod blank with the diameter of 50 mm.
S3: smelting the rod blank in a smelting furnace at 1850 ℃ for 30min at a heating rate of 25 ℃/min; cooling to 1700 ℃ and refining and smelting for 15min at low temperature; adding the ball-milled Y powder and Al powder before finishing low-temperature refining, and uniformly stirring; then adopting electroslag remelting refining, wherein the temperature of a melting furnace is 1850 ℃, the filling coefficient is 0.4, and casting into an alloy ingot;
s4: annealing the alloy ingot, wherein the process is to heat to 1000 ℃ and preserve heat for 35 hours; forging after annealing, wherein the process is that an alloy blank I is formed by cogging and forging at 900 ℃, the forging ratio is 3, an alloy blank II is formed by forging at 1000 ℃ after tempering and heating for 2 hours at 950 ℃, the forging ratio is 8, and an alloy blank III is formed by forging at 1000 ℃, and the forging ratio is 4; then rolling, wherein the process is to keep the temperature at 1000 ℃ for 1.5h, and hot-roll the alloy wire rod with the diameter of phi 5.0mm at 950 ℃; the temperature rising rate is 10 ℃/min.
S5: heating the alloy wire rod to 950 ℃, preserving heat for 1.5h, performing oil cooling for softening treatment, washing with acid (5 wt% of hydrofluoric acid, 10wt% of nitric acid and 85wt% of water) at 70 ℃ for 1h, quickly lifting after pickling, and immersing in water at 80 ℃ for cleaning; then the mixture is subjected to ultrasonic treatment for 2 hours at 50 KHz.
S6: adding a lubricant (80% calcium stearate and 20% lime powder) before drawing, and carrying out multi-pass drawing processing to obtain an alloy wire with the diameter of 1.5 mm; the annealing is to carry out vacuum annealing after carrying out drawing for 9 passes, and the annealing temperature is 950 ℃.
S7: heating to 950 ℃ in a nitrogen environment, preserving heat for 3 hours, continuously heating to 1020 ℃, preserving heat for 3 hours, and rapidly performing water quenching to obtain solid solution state alloy; the aging is heating to 830 ℃, preserving heat for 5 hours, air-cooling, heating to 770 ℃ again, preserving heat for 10 hours, and air-cooling; the temperature rising rate of the solid solution-aging treatment is 3 ℃/min.
Example 3
A preparation process of a fine grain size high temperature nickel alloy comprises the following steps:
S1: weighing according to the mass percentage of the high-temperature nickel alloy raw material powder formula, and processing to obtain uniformly refined nickel-based mixed powder;
The high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0%, nb:2.0%, Y:0.30%, al:2.0% and Ni balance.
The treatment process in the step S1 is that raw material powder except Y, al powder is added into ethanol, and after being magnetically stirred for 2 hours at 2000r/min, the raw material powder is placed in 50KHz ultrasonic treatment for 2 hours, so as to obtain ethanol suspension; filtering, taking insoluble substances, and placing the insoluble substances in a drying oven at 80 ℃ for drying treatment for 2 hours to obtain mixed powder; putting the mixed powder into a ball milling tank, adding lauric acid, and putting the ball milling tank on a high-energy ball mill for ball milling treatment, wherein the grinding balls are corundum balls, and the mass ratio of the balls is 8:1, ball milling process is carried out for 5 hours, and the rotating speed of a ball milling tank is 180r/min;
The dosage ratio of lauric acid to the total mass of the raw material powder is 2g:100g.
S2: placing the mixed powder in a stainless steel sleeve, reserving a distance space of 20mm from top to bottom, carrying out degassing treatment under the conditions that the furnace temperature is maintained at 680 ℃, the vacuum degree is less than 0.1Pa and the temperature is maintained for 7 hours, then placing the mixed powder in a hot isostatic pressing machine, heating to 1250 ℃ at a heating rate of 25 ℃/min, then applying gas pressure of 150MPa to the surface, and maintaining the temperature for 5 hours at constant pressure and constant temperature for cooling along with the furnace to obtain a cylindrical powder sintered rod blank with phi 45 mm.
S3: smelting the rod blank in a smelting furnace at 1750 ℃ for 45min at a heating rate of 15 ℃/min; cooling to 1650 ℃ and refining and smelting for 20min at low temperature; adding the ball-milled Y powder and Al powder before finishing low-temperature refining, and uniformly stirring; then adopting electroslag remelting refining, wherein the temperature of a melting furnace is 1750 ℃, the filling coefficient is 0.4, and casting into an alloy ingot;
S4: annealing the alloy ingot, wherein the process is to heat to 1020 ℃, and preserving heat for 28 hours; forging after annealing, wherein the process is that an alloy blank I is formed by cogging and forging at 950 ℃, the forging ratio is 4, an alloy blank II is formed by forging at 1050 ℃ after tempering and heating at 1000 ℃ for 1h, the forging ratio is 8, and an alloy blank III is formed by forging at 1050 ℃, and the forging ratio is 3; then rolling, wherein the process is to heat-preserving for 1h at 1030 ℃ and hot-rolling into phi 4.5mm alloy wire rods at 1050 ℃; the temperature rising rate is 12 ℃/min.
S5: heating the alloy wire rod to 950 ℃, preserving heat for 1.5h, performing oil cooling for softening treatment, washing with acid (5 wt% of hydrofluoric acid, 10wt% of nitric acid and 85wt% of water) at 70 ℃ for 1h, quickly lifting after pickling, and immersing in water at 80 ℃ for cleaning; then the mixture is subjected to ultrasonic treatment for 2 hours at 50 KHz.
S6: adding a lubricant (80% calcium stearate and 20% lime powder) before drawing, and carrying out multi-pass drawing processing to obtain an alloy wire with the diameter of 1.0 mm; the annealing is vacuum annealing after 11 passes of drawing, and the annealing temperature is 900 ℃.
S7: heating to 1000 ℃ in a nitrogen environment, preserving heat for 2 hours, continuously heating to 1070 ℃, preserving heat for 2 hours, and rapidly performing water quenching to obtain solid solution state alloy; the aging is heating to 800 ℃, preserving heat for 8 hours, air-cooling, heating to 750 ℃ again, preserving heat for 15 hours, and air-cooling; the temperature rising rate of the solid solution-aging treatment is 5 ℃/min.
Comparative examples 1-15 are all compared to example 1:
Comparative example 1
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: s1, the high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0% and Ni balance.
Comparative example 2
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: s1, the high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0%, Y:0.35%, al:1.5% and Ni balance.
Comparative example 3
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: s1, the high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0%, nb:2.2%, al:1.5% and Ni balance.
Comparative example 4
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: s1, the high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0%, nb:2.2%, Y:0.35% and Ni balance.
Comparative example 5
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: and S1, refining the nickel-based mixed powder by a ball milling method.
Comparative example 6
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: myristic acid in S1 was replaced with absolute ethanol.
Comparative example 7
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: myristic acid in S1 was replaced with stearic acid.
Comparative example 8
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: and (3) replacing the grinding ball material in the step (S1) with a hard alloy ball by corundum.
Comparative example 9
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: and S4, cogging and forging to obtain an alloy blank I at 950 ℃ with a forging ratio of 4.
Comparative example 10
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: and S4, the forging process is that the forging is performed at 950 ℃ to form an alloy blank I, the forging ratio is 2, the alloy blank II is formed at 1050 ℃ after tempering and heating at 1000 ℃ for 1h, the forging ratio is 3, and the alloy blank III is formed at 1050 ℃ and the forging ratio is 2.
Comparative example 11
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: and S6, the drawing pass is 5.
Comparative example 12
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: s7, heating to 980 ℃ in a nitrogen environment, preserving heat for 2.5 hours, and rapidly performing water quenching to obtain a solid solution state alloy; the aging is heating to 850 ℃, preserving heat for 3 hours and air cooling; the temperature rising rate of the solid solution-aging treatment is 4 ℃/min.
Comparative example 13
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: s7, heating to 980 ℃ in a nitrogen environment, preserving heat for 2.5 hours, continuously heating to 1100 ℃, preserving heat for 2.5 hours, and rapidly performing water quenching to obtain solid solution state alloy; the aging is heating to 850 ℃, preserving heat for 3 hours, air-cooling, heating to 760 ℃ again, preserving heat for 12 hours, and air-cooling; the temperature rising rate of the solid solution-aging treatment is 4 ℃/min.
Comparative example 14
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: s7, heating to 980 ℃ in a nitrogen environment, preserving heat for 2.5 hours, continuously heating to 1000 ℃, preserving heat for 2.5 hours, continuously heating to 1050 ℃, preserving heat for 2.5 hours, and rapidly performing water quenching to obtain solid solution state alloy; the aging is heating to 850 ℃, preserving heat for 3 hours, air-cooling, heating to 760 ℃ again, preserving heat for 12 hours, and air-cooling; the temperature rising rate of the solid solution-aging treatment is 4 ℃/min.
Comparative example 15
The preparation process of the fine grain size high temperature nickel alloy is the same as in embodiment 1, except that: the heating rate in S2, S3 and S4 is 5 ℃/min.
Physical properties of nickel alloys prepared by the preparation process of fine grain size high temperature nickel alloys according to examples 1 to 3 of the present invention and comparative examples 1 to 15 were measured, respectively, and the results are shown in table 1.
Table 1 physical test performance of various examples
It can be observed from examples 1-3 that the preparation process of the fine grain size high temperature nickel alloy combines a ball milling method, a chemical treatment method (namely adding a grain refiner), a thermomechanical treatment process and rapid temperature rise and reduction and classification multiple solid solution-aging treatment to obtain a high temperature nickel alloy product with fine grain size and small grade difference, and the fine grain size and small grade difference are reflected in good mechanical properties.
As can be seen from example 1 and comparative examples 1 to 4, the fine grain size high temperature nickel alloy of the present invention can be produced by adding a grain refiner to refine grains to some extent and reduce the level difference. It can be observed from example 1 and comparative examples 5 to 6 that the ball milling method has an important effect on the initial ion refinement, and has a wrapping and anti-agglomeration effect on metal ions after ball milling treatment, and finally, the ball milling method is better in various performance indexes. From example 1 and comparative examples 7 to 8, it can be observed that myristic acid is better as a ball milling medium, and is suspected to have smaller molecular weight, higher carboxyl density, stronger adsorption to the surface of metal particles and better dispersibility; it can be observed from example 8 that the corundum has alumina as the main component, no pollution to the metal particle powder and better final properties. It can be seen from example 1 and comparative examples 9 to 10 that a suitable forging process has an important effect on the size and distribution of grains, and can mechanically crush, eliminate primary coarse grains, recrystallize and sufficiently refine them. From example 1 and comparative example 11, it can be seen that the number of cold drawing passes was larger and the grain size was finer. It can be seen from example 1 and comparative examples 12 to 14 that the grain size after 2 solid solution-aging treatments was optimal and the grade difference was minimum; and the temperature has a larger influence on the grain size. As can be seen from example 1 and comparative example 15, rapid temperature changes can destroy coarse grains which are preferentially generated, thereby achieving fine and uniform fine grains.
The test method comprises the following steps:
(1) Hardness: the load is 150kg.
(2) Mechanical property test: the test temperature is 23+/-5 ℃ according to GB/T228-2002 'method for room temperature tensile test of metallic materials'.
(3) Grain size: the test was performed as described in GB/T6394-2017.
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (1)
1. A preparation process of a fine grain size high temperature nickel alloy is characterized in that: the method comprises the following steps:
S1: weighing according to the mass percentage of the high-temperature nickel alloy raw material powder formula, and processing to obtain uniformly refined nickel-based mixed powder;
s2: placing the mixed powder into a stainless steel sleeve, reserving a certain space, degassing, and then placing into a hot isostatic pressing machine to sinter into a bar blank;
s3: smelting the rod blank in a smelting furnace, refining at high temperature and low temperature, remelting and refining, and casting into alloy ingots;
s4: annealing the alloy ingot, forging and rolling to prepare an alloy wire rod;
S5: carrying out surface treatment on the alloy wire rod;
S6: multiple pass drawing-annealing;
S7: carrying out solid solution-aging treatment;
The high-temperature nickel alloy raw material powder comprises the following components in percentage by mass: cr:15.0%, co:4.0%, mo:5.0%, fe:6.0%, nb:2.0-3.0%, Y:0.30-0.35%, al:1.0-2.0%, ni balance;
The treatment process in the step S1 is that raw material powder except Y, al powder is added into ethanol, and after being magnetically stirred for 2 hours at 2000r/min, the raw material powder is placed in 50KHz ultrasonic treatment for 2 hours, so as to obtain ethanol suspension; filtering, taking insoluble substances, and placing the insoluble substances in a drying oven at 80 ℃ for drying treatment for 2 hours to obtain mixed powder; putting the mixed powder into a ball milling tank, adding long-chain fatty acid, and putting the ball milling tank on a high-energy ball mill for ball milling treatment, wherein the grinding balls are corundum balls, and the mass ratio of the grinding balls is 5-8:1, ball milling process is carried out for 5-10h, and the rotating speed of a ball milling tank is 150-200r/min;
The dosage ratio of the long-chain fatty acid to the total mass of the raw material powder is 2g:100g;
The long-chain fatty acid is myristic acid or lauric acid;
the degassing treatment process in the step S2 is that the furnace temperature is kept at 660-700 ℃, the vacuum degree is less than 0.1 Pa, and the temperature is kept for 6-8 hours; the sintering process is that heating is carried out at a heating rate of 25 ℃/min to 1220-1280 ℃, then gas pressure of 150MPa is applied to the surface, and the surface is kept for 4-6h and cooled along with the furnace at constant pressure and constant temperature, thus obtaining cylindrical powder sintered rod blank with phi of 40-50 mm;
The high-temperature refining in the step S3 is carried out at 1750-1850 ℃ for 30-45min, and the heating rate is 15-25 ℃/min; cooling to 1650-1700 ℃ and refining and smelting for 15-25min at low temperature; adding the treated Y powder and Al powder in the later stage of low-temperature refining, and uniformly stirring; the remelting is electroslag remelting, and the temperature of a melting furnace is 1750-1850 ℃;
The annealing process in the step S4 is heating to 1000-1050 ℃, and preserving heat for 20-35h; the forging process is that an alloy blank I is formed by cogging and forging at 900-950 ℃, the forging ratio is 3-4, an alloy blank II is formed by forging at 1000-1050 ℃ after tempering and heating for 1-2h at 950-1000 ℃, the forging ratio is 7-8, and an alloy blank III is formed by forging at 1000-1050 ℃, and the forging ratio is 3-4; the rolling process is to heat-preserving for 0.5-1.5h at 1000-1050 ℃ and hot-rolling for phi 4.0-5.0 mm alloy wire rod at 950-1100 ℃; the temperature rising rate in the step S4 is 10-15 ℃/min;
The S5 surface treatment is to heat the alloy wire rod to 950 ℃ and keep the temperature for 1.5 hours, perform softening treatment by oil cooling, perform acid washing, and then perform ultrasonic cleaning;
the drawing-annealing in the step S6 is carried out, a lubricant is added before drawing, and then the drawing processing is carried out for multiple times, so that the alloy wire with the diameter of phi 1.0-1.5mm is obtained; the annealing is to carry out vacuum annealing after carrying out drawing for 9-11 times, and the annealing temperature is 850-950 ℃;
In the step S7, the solid solution-aging treatment is carried out under the nitrogen environment, the temperature is heated to 950-1000 ℃, the heat preservation is carried out for 2-3 hours, the heating is continued to 1020-1070 ℃, the heat preservation is carried out for 2-3 hours, and the solid solution alloy is obtained by rapid water quenching; the aging is heating to 800-850 ℃, preserving heat for 3-8h, air cooling, heating to 750-770 ℃ again, preserving heat for 10-15h, and air cooling; the temperature rising rate of the solid solution-aging treatment is 3-5 ℃/min.
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