CN110983110B - High-fluidity high-temperature alloy and preparation method thereof - Google Patents
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- C—CHEMISTRY; METALLURGY
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- C22C19/00—Alloys based on nickel or cobalt
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- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
Abstract
The invention provides a high-fluidity high-temperature alloy and a preparation method thereof, belonging to the technical field of high-temperature alloys, wherein the preparation method comprises the following steps: burdening the components of the required high-temperature alloy; ball-milling and tabletting the metal powder after the material mixing to obtain metal sheets; then putting the metal sheet into a vacuum arc melting furnace for melting and casting to obtain a high-temperature alloy section; and finally, placing the obtained high-temperature alloy section in a heat treatment furnace to perform three-step performance heat treatment of solid solution, high-temperature aging and low-temperature aging, thus obtaining the high-fluidity high-temperature alloy. The invention provides a high-fluidity high-temperature alloy and a preparation method thereof, and the alloy has the advantages of excellent high fluidity and excellent high-temperature mechanical property compared with the existing material.
Description
Technical Field
The invention belongs to the technical field of high-temperature alloys, and particularly relates to a high-fluidity high-temperature alloy and a preparation method thereof.
Background
Society is now rapidly developing at unprecedented rates, relying heavily on the materials, information, and energy industries in the process of development. With the rapid development of the aircraft industry and the automobile industry, superalloys are the main materials for aircraft engine impellers, turbine disks, guide rings, diffusers, casings and other structural components, which face unprecedented challenges.
The cost and performance advantages of large complex castings to replace the assembled parts now make their use increasingly widespread. But for large complex thin-walled castings, forming is a critical issue. In the forming process, casting defects such as hot cracks, under-pouring, cold shut, shrinkage cavities and the like are easily formed. To eliminate these drawbacks, it is not practical to increase the casting temperature and the mold shell temperature too much to improve the fluidity of the alloy. The fluidity is one of important casting performances of the cast alloy, and factors influencing the fluidity of the metal mainly comprise: the solidification range, density, specific heat, thermal conductivity, latent heat of crystallization, viscosity, surface tension, etc. of the metal.
The research of high-temperature alloy casting in China is started late, the high-temperature alloy casting is more laggard compared with developed countries such as Europe and America, a plurality of key parts always depend on import, and the engine industry in China cannot make breakthrough progress late. In view of the above, it is desirable to develop a high temperature alloy having good fluidity in a liquid state to solve the above problems.
Disclosure of Invention
In order to overcome the defects, the invention provides a high-fluidity high-temperature alloy and a preparation method of the high-fluidity high-temperature alloy.
In order to achieve the purpose of the invention, the technical scheme of the invention is as follows:
a high-fluidity superalloy, characterized by: the raw materials and the mixture ratio are as follows by mass percent:
wherein the purities of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni are all more than or equal to 99.99 percent; cu3The purity of Al is more than 95.0%.
Wherein the grain sizes of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni are all 7.5-9.5 mu m; cu3The particle size of Al is 10-50 nm.
A preparation method of high-fluidity high-temperature alloy comprises the following specific steps:
s1, material preparation: weighing high-purity powder Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni according to the proportion, and weighing 0.05-0.12% of high-purity nano Cu3Al powder is used;
s2, ball milling, mixing and tabletting: putting the weighed high-purity powder of S1 into a ball mill for ball milling for at least 24 hours to obtain mixed powder, then putting the mixed powder into a press machine, and pressing the mixed powder into a metal sheet at the high pressure of 50-100 MPa and the temperature of 1400-1600 ℃ to obtain a metal sheet;
s3, vacuum melting, namely putting the metal sheet obtained in the step S2 into a vacuum arc melting furnace for melting under the melting condition of a.5 × 10-2～1×10-3A low vacuum state of MPa; b. the smelting temperature is 1600-1700 ℃; c. magnetic stirring is adopted in the smelting process; d. the smelting time is 0.2-0.4 hours;
s4, adding high-purity nano Cu after smelting and before casting3Al powder, and then casting and molding;
s5, performance heat treatment: placing the casting obtained in the S4 into a heat treatment furnace for solid solution-high temperature aging-low temperature aging 3-step performance heat treatment, wherein the performance heat treatment comprises the following specific processes: a. solution heat treatment: preserving the heat for 2-4 h at 1250-1350 ℃, and then air-cooling to room temperature; b. high-temperature aging heat treatment: keeping the temperature of 1050-1200 ℃ for 8-14 h, and then air-cooling to room temperature; c. low-temperature aging heat treatment: keeping the temperature at 750-850 ℃ for 15-20 h, and then air-cooling to room temperature.
When S4 casting, Fe is dispersed and distributed in the casting3An Al phase; s5 property Heat treated, Fe3The Al phase is completely dissolved in the matrix structure.
S4 castingIn the casting, Fe is dispersed and distributed3Al phase and Cu3Al phase, Cu3Al in an atomic ratio of 3.57 to 7.68%, Fe3Al accounts for 3.66-7.21% of the atomic ratio.
The high-fluidity high-temperature alloy manufactured by the invention has the characteristics of high fluidity and excellent high-temperature mechanical property. The high-fluidity high-temperature alloy provided by the invention has Fe dispersed and distributed in the microstructure during casting3Al phase for regulating components and improving high-temperature fluidity of the alloy, and Fe after heat treatment3Al phase is completely dissolved in matrix structure in a solid solution mode, the high-temperature mechanical property of the alloy is improved, and the high-temperature alloy can be promoted to have the characteristics of high fluidity and excellent high-temperature mechanical property.
Compared with the existing material, the high-fluidity high-temperature alloy provided by the invention has the advantages of excellent high fluidity and excellent high-temperature mechanical property.
(1): high fluidity: the high fluidity of superalloys is one of the necessary physical characteristics for casting complex or ultra-thin castings. The invention utilizes a specific preparation process to prepare liquid iron and Cu in the process of casting the high-temperature alloy3Al reacts to obtain the ultrafine Fe which is dispersed and distributed in the microstructure of the material3Al increases the Cu content in the liquid alloy on one hand, reduces the Fe content in the liquid alloy on the other hand, and has the characteristic of adjusting the high-temperature low-viscosity high-fluidity of the liquid alloy. Fe3The Al phase is dispersed and distributed in the microstructure of the high-temperature alloy, so that the defects of overhigh viscosity and poor liquidity of the high-temperature alloy in a molten state can be effectively overcome, and the liquidity of the high-temperature alloy in the molten state is greatly improved.
The molten metal is rich in iron during casting, and Cu is added before casting3Post-reaction of Al powder Cu3Al+Fe＝Fe3On one hand, 3.57-7.68 mol of copper is introduced into the liquid alloy without Cu, so that the viscosity of the liquid alloy can be greatly reduced, and the fluidity is increased; on the other hand Fe3Al is a high-temperature compound, and the formation of the Al can reduce the Fe content in the liquid alloy by 3.66-7.21 mol, and further reduce the viscosity of the liquid alloyThe fluidity is increased, the defects of overhigh viscosity and poor fluidity of the high-temperature alloy in a molten state can be effectively overcome, and the fluidity of the high-temperature alloy in the molten state is greatly improved.
(2): excellent high-temperature mechanical properties: the high-temperature mechanical property is an important property of the high-temperature alloy and determines the application condition of the high-temperature alloy. The invention enables Fe formed during casting to be subjected to performance heat treatment through a specific preparation process3Al phase is completely dissolved in matrix structure in a solid mode, so that the cast section has excellent high-temperature comprehensive mechanical properties.
(3): the preparation method comprises the following steps: the invention adopts a mode of ball milling high-purity powder, tabletting and vacuum melting to prepare the high-temperature alloy. In the process, the high-energy ball milling can achieve the aim of uniformly mixing high-purity powder on one hand. On the other hand, the defects of the alloy powder can be increased, and the energy of the alloy powder is improved.
(4): the performance heat treatment method comprises the following steps: the invention adopts 3 steps of performance heat treatment of solid solution, high temperature aging and low temperature aging, and the specific process of the performance heat treatment is as follows: a. solution heat treatment: preserving the heat for 2-4 h at 1250-1350 ℃, and then air-cooling to room temperature; b. high-temperature aging heat treatment: keeping the temperature of 1050-1200 ℃ for 8-14 h, and then air-cooling to room temperature; c. low-temperature aging heat treatment: keeping the temperature at 750-850 ℃ for 15-20 h, and then air-cooling to room temperature. The process adopts three-step performance heat treatment modes of solid solution, high temperature aging and low temperature aging to greatly improve the fluidity and high temperature mechanical property of the high temperature alloy.
In conclusion, the invention provides the high-fluidity high-temperature alloy and the preparation method thereof, and the alloy has the advantages of excellent high fluidity and excellent high-temperature mechanical property compared with the existing material.
Drawings
FIG. 1 is a structural diagram of a superalloy of the present invention.
Detailed Description
The invention is further illustrated by the figures and examples.
Example 1:
according to the requirement of the required hot cracking resistant high-temperature alloy, the prepared high-fluidity high-temperature alloy comprises the following components in percentage by mass (wt.%):
wherein the purities of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni are all more than or equal to 99.99 percent; cu3The purity of Al is more than 95.0%.
Wherein the grain sizes of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni are all about 7.5 μm; cu3The particle size of Al is about 10 nm.
A preparation method of high-fluidity high-temperature alloy comprises the following specific steps:
s1, material preparation: weighing the high-purity powder according to the proportion, wherein the particle size of the high-purity powder is about 7.5 mu m; then 0.05 percent of high-purity nano Cu is weighed3Al powder for use, high purity nano Cu3The grain diameter of the Al powder is about 10 nm;
s2, ball milling, mixing and tabletting: putting the weighed powder of S1 into a ball mill for ball milling for 24h to obtain mixed powder, then putting the mixed powder into a press, and pressing and molding under the high pressure of 50MPa and the temperature of 1400 ℃ to obtain a metal sheet;
s3, vacuum melting, namely putting the metal sheet obtained in the step S2 into a vacuum arc melting furnace for melting under the melting condition of a.5 × 10-2A low vacuum state of MPa; b. the smelting temperature is 1600 ℃; c. magnetic stirring is adopted in the smelting process; d. the smelting time is 0.4 hour;
s4, adding high-purity nano Cu after smelting and before casting3Al powder, and then casting and molding;
s5, performance heat treatment: placing the casting obtained in the S4 into a heat treatment furnace for solid solution-high temperature aging-low temperature aging 3-step performance heat treatment, wherein the performance heat treatment comprises the following specific processes: a. solution heat treatment: preserving the heat for 2 hours at 1250 ℃, and then cooling the mixture to room temperature in air; b. high-temperature aging heat treatment: keeping the temperature at 1050 ℃ for 8h, and then cooling the mixture to room temperature in air; c. low-temperature aging heat treatment: keeping the temperature at 750 ℃ for 15h, and then cooling to room temperature in air.
When S4 casting, Fe is dispersed and distributed in the casting3An Al phase; s5 PerformanceAfter heat treatment, Fe3The Al phase is completely dissolved in the matrix structure.
When S4 casting, Fe is dispersed and distributed in the casting3Al phase and Cu3Al phase, Cu3Al in an atomic ratio of 3.57 to 7.68%, Fe3Al accounts for 3.66-7.21% of the atomic ratio.
The alloy prepared by the method is cut into samples by linear cutting and is tested for high-temperature mechanical property and fluidity.
Example 2:
according to the requirement of the required hot cracking resistant high-temperature alloy, the prepared high-fluidity high-temperature alloy comprises the following components in percentage by mass (wt.%):
wherein the purities of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni are all more than or equal to 99.99 percent; cu3The purity of Al is more than 95.0%.
Wherein the grain sizes of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni are all about 8.0 μm; cu3The particle size of Al is about 30 nm.
A preparation method of high-fluidity high-temperature alloy comprises the following specific steps:
s1, material preparation: weighing the high-purity powder according to the proportion, wherein the metal purity is more than or equal to 99.99 percent, and the grain diameter of the high-purity powder is about 8.0 mu m; then 0.09 percent of high-purity nano Cu is weighed3Al powder for use, high purity nano Cu3The grain diameter of the Al powder is about 30 nm;
s2, ball milling, mixing and tabletting: placing the weighed high-purity powder of S1 into a ball mill for ball milling for 24h to obtain mixed powder, then placing the mixed powder into a press, and pressing and molding under the high pressure of 80MPa and the temperature of 1500 ℃ to obtain a metal sheet;
s3, vacuum melting, namely putting the metal sheet obtained in the step S2 into a vacuum arc melting furnace for melting under the melting condition of a.8 × 10-2A low vacuum state of MPa; b. the smelting temperature is 1650 ℃; c. magnetic stirring is adopted in the smelting process; d. the smelting time is 0.3 hour;
s4, adding high-purity nano Cu after smelting and before casting3Al powder, and then casting and molding;
s5, performance heat treatment: placing the casting obtained in the S4 into a heat treatment furnace for solid solution-high temperature aging-low temperature aging 3-step performance heat treatment, wherein the performance heat treatment comprises the following specific processes: a. solution heat treatment: preserving the heat at 1300 ℃ for 3h, and then cooling the mixture to room temperature in air; b. high-temperature aging heat treatment: keeping the temperature at 1100 ℃ for 10h, and then cooling to room temperature in air; c. low-temperature aging heat treatment: keeping the temperature at 800 ℃ for 18h, and then cooling to room temperature in air.
When S4 casting, Fe is dispersed and distributed in the casting3An Al phase; s5 property Heat treated, Fe3The Al phase is completely dissolved in the matrix structure.
When S4 casting, Fe is dispersed and distributed in the casting3Al phase and Cu3Al phase, Cu3Al in an atomic ratio of 3.57 to 7.68%, Fe3Al accounts for 3.66-7.21% of the atomic ratio.
The alloy prepared by the method is cut into samples by linear cutting and is tested for high-temperature mechanical property and fluidity.
Example 3:
according to the requirement of the required hot cracking resistant high-temperature alloy, the prepared high-fluidity high-temperature alloy comprises the following components in percentage by mass (wt.%):
wherein the purities of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni are all more than or equal to 99.99 percent; cu3The purity of Al is more than 95.0%.
Wherein the grain sizes of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni are all about 9.5 μm; cu3The particle size of Al is about 50 nm.
A preparation method of high-fluidity high-temperature alloy comprises the following specific steps:
s1, material preparation: weighing the high-purity powder according to the proportion, wherein the metal purity is more than or equal to 99.99 percent, and the grain diameter of the high-purity powder is about 9.5 mu m; then 0.12 percent of high-purity nano C is weighedu3Al powder for use, high purity nano Cu3The grain diameter of the Al powder is about 50 nm;
s2, ball milling, mixing and tabletting: placing the weighed high-purity powder of S1 into a ball mill for ball milling for 24h to obtain mixed powder, then placing the mixed powder into a press, and pressing the mixed powder into a metal sheet under the high pressure of 100MPa and the temperature of 1600 ℃ to obtain a metal sheet;
s3, vacuum melting, namely putting the metal sheet obtained in the step S2 into a vacuum arc melting furnace for melting under the melting condition of a.1 × 10-3A low vacuum state of MPa; b. the smelting temperature is 1700 ℃; c. magnetic stirring is adopted in the smelting process; d. the smelting time is 0.4 hour;
s4, adding high-purity nano Cu after smelting and before casting3Al powder, and then casting and molding;
s5, performance heat treatment: placing the casting obtained in the S4 into a heat treatment furnace for solid solution-high temperature aging-low temperature aging 3-step performance heat treatment, wherein the performance heat treatment comprises the following specific processes: a. solution heat treatment: preserving the heat for 4 hours at 1350 ℃, and then cooling the mixture to room temperature in air; b. high-temperature aging heat treatment: keeping the temperature at 1200 ℃ for 14h, and then cooling to room temperature in air; c. low-temperature aging heat treatment: keeping the temperature at 850 ℃ for 20h, and then cooling to room temperature in air.
When S4 casting, Fe is dispersed and distributed in the casting3An Al phase; s5 property Heat treated, Fe3The Al phase is completely dissolved in the matrix structure.
When S4 casting, Fe is dispersed and distributed in the casting3Al phase and Cu3Al phase, Cu3Al in an atomic ratio of 3.57 to 7.68%, Fe3Al accounts for 3.66-7.21% of the atomic ratio.
The alloy prepared by the method is cut into samples by linear cutting and is tested for high-temperature mechanical property and fluidity.
The results of the tests of examples 1 to 3 are shown in Table 1.
TABLE 1 high temperature mechanical Properties and fluidity comparison of high flow superalloys
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the invention.
Claims (5)
1. A high-fluidity superalloy, characterized by: the raw materials and the mixture ratio are as follows by mass percent:
the preparation method of the high-fluidity high-temperature alloy comprises the following steps:
s1, material preparation: weighing high-purity powder Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni according to the proportion, and weighing 0.05-0.12% of high-purity nano Cu3Al powder is used;
s2, ball milling, mixing and tabletting: putting the weighed high-purity powder of S1 into a ball mill for ball milling for at least 24 hours to obtain mixed powder, then putting the mixed powder into a press machine, and pressing the mixed powder into a metal sheet at the high pressure of 50-100 MPa and the temperature of 1400-1600 ℃ to obtain a metal sheet;
s3, vacuum melting, namely putting the metal sheet obtained in the step S2 into a vacuum arc melting furnace for melting under the melting condition of a.5 × 10-2～1×10-3A low vacuum state of MPa; b. the smelting temperature is 1600-1700 ℃; c. magnetic stirring is adopted in the smelting process; d. the smelting time is 0.2-0.4 hours;
s4, adding high-purity nano Cu after smelting and before casting3Al powder, and then casting and molding;
s5, performance heat treatment: placing the casting obtained in the S4 into a heat treatment furnace for solid solution-high temperature aging-low temperature aging 3-step performance heat treatment, wherein the performance heat treatment comprises the following specific processes: a. solution heat treatment: preserving the heat for 2-4 h at 1250-1350 ℃, and then air-cooling to room temperature; b. high-temperature aging heat treatment: keeping the temperature of 1050-1200 ℃ for 8-14 h, and then air-cooling to room temperature; c. low-temperature aging heat treatment: keeping the temperature at 750-850 ℃ for 15-20 h, and then air-cooling to room temperature.
2. The high-fluidity superalloy according to claim 1, wherein the purity of each of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni is 99.99% or more; cu3The purity of Al is more than 95.0%.
3. The high-fluidity superalloy according to claim 1, wherein the grain sizes of Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr, and Ni are each 7.5 to 9.5 μm; cu3The particle size of Al is 10-50 nm.
4. The method for preparing the high-fluidity high-temperature alloy according to any one of claims 1 to 3, which is characterized by comprising the following steps:
s1, material preparation: weighing high-purity powder Cr, Fe, Ti, C, Co, B, Mo, Mn, Zr and Ni according to the proportion, and weighing 0.05-0.12% of high-purity nano Cu3Al powder is used;
s2, ball milling, mixing and tabletting: putting the weighed high-purity powder of S1 into a ball mill for ball milling for at least 24 hours to obtain mixed powder, then putting the mixed powder into a press machine, and pressing the mixed powder into a metal sheet at the high pressure of 50-100 MPa and the temperature of 1400-1600 ℃ to obtain a metal sheet;
s3, vacuum melting, namely putting the metal sheet obtained in the step S2 into a vacuum arc melting furnace for melting under the melting condition of a.5 × 10-2～1×10-3A low vacuum state of MPa; b. the smelting temperature is 1600-1700 ℃; c. magnetic stirring is adopted in the smelting process; d. the smelting time is 0.2-0.4 hours;
s4, adding high-purity nano Cu after smelting and before casting3Al powder, and then casting and molding;
s5, performance heat treatment: placing the casting obtained in the S4 into a heat treatment furnace for solid solution-high temperature aging-low temperature aging 3-step performance heat treatment, wherein the performance heat treatment comprises the following specific processes: a. solution heat treatment: preserving the heat for 2-4 h at 1250-1350 ℃, and then air-cooling to room temperature; b. high-temperature aging heat treatment: keeping the temperature of 1050-1200 ℃ for 8-14 h, and then air-cooling to room temperature; c. low-temperature aging heat treatment: keeping the temperature at 750-850 ℃ for 15-20 h, and then air-cooling to room temperature.
5. The method of claim 4, wherein Fe is dispersed in the casting at S43An Al phase; s5 property Heat treated, Fe3The Al phase is completely dissolved in the matrix structure.
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