CN114351064A - Preparation method of GH4169 alloy tube bar with surface ultrafine grain structure - Google Patents
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Abstract
The invention relates to the field of nickel-based high-temperature alloy preparation processes, in particular to a preparation method of a GH4169 alloy tube bar with a surface ultrafine grain structure. The method comprises the following steps: (1) carrying out solution treatment on the GH4169 alloy forged tube bar, wherein the solution temperature is 1020-1050 ℃, the heat preservation time is 30-50 min, and cooling to room temperature by water; (2) carrying out aging treatment on the GH4169 alloy pipe and bar subjected to the solution treatment, wherein the aging temperature is 910-930 ℃, the aging time is 20-24 h, and cooling the obtained product to room temperature by water; (3) and rolling the solution aging GH4169 alloy tube bar by adopting a cross wedge rolling processing technology to obtain the GH4169 alloy tube bar with the surface ultrafine grain structure. The method provided by the invention can simply and efficiently prepare the GH4169 alloy tube bar with the surface grain size of more than ASTM grade 12.
Description
Technical Field
The invention relates to the field of nickel-based high-temperature alloy preparation processes, in particular to a preparation method of a GH4169 alloy tube bar with a surface ultrafine grain structure.
Background
The GH4169 alloy (corresponding to the American mark Inconel 718) is a typical material in nickel-based high-temperature alloy, is one of the most widely applied materials in an aeroengine due to excellent fatigue resistance, creep resistance, corrosion resistance and oxidation resistance at 650 ℃, and is mainly applied to important hot-end power structure materials in the aeroengine, such as: compressor blades, turbine disks, and the like.
The excellent service performance is inseparable from the microstructure. The domestic scholars study the influence of fine grains (10 mu m) and coarse grains (90 mu m) on the mechanical and high-cycle fatigue properties of the Inconel 718 alloy, and the results show that the yield strength and the tensile strength of the alloy are increased along with the reduction of the grain size and the alloy is subjected to the same cycle number (10 mu m)7) The fatigue strength of fine-grained alloys is 1.6 times that of coarse-grained alloys (Du Jinhui. Rare Metal Materials and Engineering [ J ]],2014,43(8):1830-1834.). Therefore, the grain refinement contributes to the improvement of the strength and fatigue properties of the GH4169 alloy. For GH4169 alloy, through solution aging treatment, the pre-precipitated delta phase has the effect of hindering the grain growth in the thermal deformation process.
In the aerospace field, compared with extrusion and forging, the advantage of using a rolling process for blade blank making is embodied as follows: the method has the advantages of simplifying construction technology, greatly improving production efficiency, ensuring that the stress direction of a roller and a blade is consistent when the roller and the blade work, having fine crystal grains and good mechanical property, and improving the fatigue strength of the blade by more than 12 percent (Chengming, research progress of GH4169 alloy main plastic processing technology, Chinese material progress, 2016.). Compared with the defects of difficult design, manufacture and installation of a die of a roller type rolling mill and great debugging difficulty, the plate type wedge cross rolling has no defects except no-load return stroke. Therefore, the plate type cross wedge rolling has good application prospect, and the experiments related to the invention are all carried out on the plate type cross wedge rolling mill.
Disclosure of Invention
The invention aims to provide a preparation method of a GH4169 alloy tube bar with a surface ultrafine grain structure, which comprises the steps of carrying out wedge cross rolling on a GH4169 alloy tube bar subjected to solution aging treatment, and obtaining the GH4169 alloy tube bar with the surface ultrafine grain structure under the interaction of a complex stress state, a delta phase and dynamic recrystallization.
The technical scheme of the invention is as follows:
a preparation method of GH4169 alloy tube and bar with ultra-fine grain structure on the surface comprises the steps of pre-precipitating a delta phase from the GH4169 alloy tube and bar through solution aging treatment, and preparing the GH4169 alloy tube and bar with the grain size of the surface reaching ASTM12 grade through the subsequent wedge cross rolling processing process, complex stress state, delta phase and dynamic recrystallization interaction.
The preparation method of the GH4169 alloy tube bar with the surface ultrafine grain structure comprises the following steps:
A. selecting a group of parameters within a given temperature and time range to carry out solution treatment on the GH4169 alloy tube bar to obtain the GH4169 alloy tube bar with uniform structure;
B. selecting a group of parameters for aging treatment of the GH4169 alloy tube and bar subjected to solution treatment within a given temperature range and time to obtain a GH4169 alloy tube and bar with a pre-precipitated delta phase;
C. the GH4169 alloy tube and bar subjected to solid solution and aging treatment is rolled by using a cross wedge rolling process, a group of parameters are selected within a given rolling process and a given die parameter range, and the GH4169 alloy tube and bar with the surface ultrafine grain structure is obtained under the action of complex heat and force coupling.
In the preparation method of the GH4169 alloy tube bar with the surface ultrafine grain structure, in the wedge cross rolling process, dynamic recrystallization is expanded from the surface layer to the heart of a rolled piece, and the dynamic recrystallization mechanism is discontinuous dynamic recrystallization; the rolling force and the reduction of area are in positive correlation, the reduction of area is improved, dynamic recrystallization is expanded to the center of a rolled piece, and the GH4169 alloy tube bar with the surface and the center of an ultrafine grain structure is obtained.
According to the preparation method of the GH4169 alloy tube bar with the ultrafine grain structure on the surface, through solution aging treatment, the delta phase pre-precipitated on the surface layer of the GH4169 alloy tube bar is changed into a short rod or a particle in the rolling process and distributed on a crystal boundary to provide more nucleation mass points as dynamic recrystallization, so that the generation of the dynamic recrystallization is promoted, and the fine grains can be obtained.
According to the preparation method of the GH4169 alloy tube bar with the ultrafine grain structure on the surface, the delta phase is pre-precipitated, so that the deformation activation energy of the GH4169 alloy tube bar is increased, and the deformation expansion towards the center is inhibited.
In the preparation method of the GH4169 alloy tube and bar with the ultrafine grain structure on the surface, in the step A, GH4169 alloy forging tube and bar is selected, solid solution treatment is carried out, the selected temperature range is 1020-1050 ℃, the heat preservation time is 30-50 min, water cooling is carried out to the room temperature, and the grain size of the GH4169 alloy tube and bar is 60-100 mu m.
In the preparation method of the GH4169 alloy tube bar with the ultrafine grain structure on the surface, in the step B, the temperature range selected for aging treatment is 910-930 ℃, the heat preservation time is 20-24 h, and the bar is cooled to room temperature by water.
In the step C, the GH4169 alloy tube bar subjected to solid solution and aging treatment is subjected to wedge cross rolling, the GH4169 alloy tube bar is kept at 950-1050 ℃ for 20-40 min before rolling, and the GH4169 alloy tube bar is cooled to room temperature after rolling.
In the step C, the GH4169 alloy tube bar with the ultra-fine grain structure on the surface is subjected to cross wedge rolling, the cross wedge rolling process conditions and the die parameter range which need to be met are as follows, the rolling speed is 300-500 mm/s, the forming angle is 28-32 degrees, the spreading angle is 6-8 degrees, the grain size of the surface of the GH4169 alloy tube bar is 2-5 mu m, and the grain size of the core of the GH4169 alloy tube bar is 20-30 mu m.
The design principle of the invention is as follows:
compared with other forming methods, the cross wedge rolling process is characterized in that a rolled piece is subjected to radial compression deformation and axial extension deformation simultaneously in the deformation process, so that the plastic forming capability of metal can be fully exerted. As the GH4169 alloy tube and bar are subjected to complex stress action in the cross wedge rolling process, dislocation can be deposited close to delta phase, and the lamellar delta phase of the pre-precipitation sheet of the GH4169 alloy tube and bar subjected to the solution aging treatment is broken and dissolved into granules/short bars. In the rolling process, under the combined action of axial tensile deformation generated by axial force, compression deformation generated by radial pressure and torsional deformation generated by circumferential shearing force, the GH4169 alloy tube bar is dynamically recrystallized from the surface layer to the centripetal part step by step, and the dynamic recrystallization mechanism is discontinuous dynamic recrystallization. In addition, the spheroidized delta phase is uniformly distributed in the grain boundary in a granular/short rod shape during the rolling process, a large number of nucleation mass points are provided for dynamic recrystallization, and the granular/short rod-shaped delta phase distributed in the grain boundary plays a role in inhibiting the growth of grains, so that the characteristics are beneficial to preparing the GH4169 alloy tube bar material with the ultrafine grain structure on the surface.
The invention has the advantages and beneficial effects that:
1. the invention realizes the preparation of GH4169 alloy pipe or bar with surface ultrafine grain structure based on the mutual combination of heat treatment and cross wedge rolling processing, and fully utilizes the advanced process (not only can spheroidize delta phase in the rolling process, but also can influence the generation of dynamic recrystallization together with the spheroidized delta phase) of cross wedge rolling which can generate complex stress to obtain the forming method for simply and efficiently preparing the GH4169 alloy pipe or bar with surface ultrafine grain structure.
2. The delta phase precipitated by the solid solution aging treatment can provide nucleation particles for new recrystallization, and has the function of pinning a grain boundary to inhibit grain growth. Complex stress is generated in the rolling process, so that the rolled piece has stress action in all directions of deformation, the deformation energy storage at the crystal boundary is increased, the deformation activation energy is provided for complete recrystallization, and the GH4169 alloy product with excellent mechanical property can be obtained by processing through the process.
3. The method provided by the invention can simply and efficiently prepare the GH4169 alloy tube bar with the surface grain size of more than ASTM grade 12.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
FIG. 2 is a microstructure of solution treated GH4169 bar stock.
FIG. 3 shows the microstructure of the surface layer of a solution treated GH4169 alloy rolled piece after cross wedge rolling.
FIG. 4 is a microstructure of solution aged GH4169 bar stock.
FIG. 5 shows the microstructure of the surface layer of a solution aging treated GH4169 alloy rolled piece after cross wedge rolling.
Detailed Description
As shown in figure 1, in the implementation process of specifically obtaining GH4169 alloy tube and bar materials with ultrafine grain structures on the surfaces, GH4169 alloy tube and bar materials are selected for carrying out experiments, and rolling experiments are carried out on a plate type wedge cross rolling mill, wherein the method comprises the following steps: (1) carrying out solution treatment on the GH4169 alloy forged tube bar, wherein the solution temperature is 1020-1050 ℃, the heat preservation time is 30-50 min, and cooling to room temperature by water; (2) aging the GH4169 alloy tube and bar subjected to the solution treatment at 910-930 ℃ for 20-24 h, cooling the tube and bar to room temperature by water, and pre-precipitating a delta phase from a microstructure; (3) and rolling the solution aging GH4169 alloy tube bar by adopting a cross wedge rolling processing technology to obtain the GH4169 alloy tube bar with the surface ultrafine grain structure.
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Example 1
In the embodiment, the preparation method of the GH4169 alloy bar with the surface ultrafine grain structure comprises the following steps:
step 1: the method comprises the steps of selecting a GH4169 alloy forging bar, carrying out solution treatment at the temperature of 1035 +/-5 ℃ for 30min, and then carrying out water cooling to room temperature to eliminate element segregation and second phases in the original material to obtain the GH4169 alloy tube bar with fine and uniform grain structure, wherein the grain size of the GH4169 alloy forging bar is 60-100 mu m.
Step 2: and carrying out wedge cross rolling on the GH4169 alloy forged bar after the solution treatment, keeping the temperature of the GH4169 alloy tube bar at 1000 ℃ for 30min before rolling, and cooling the GH4169 alloy tube bar to room temperature after rolling. A set of data of the rolling process and the die parameters is selected, and the specific contents are shown in table 1.
Table 1 main process and mould parameters during the test
As shown in FIG. 2, the microstructure of the solution-treated bar was an equiaxed structure with a small amount of carbide (NbC) on the γ phase as a matrix. As shown in FIG. 3, the solid solution GH4169 alloy is cross-wedge rolled to obtain a microstructure of the surface layer of the rolled piece, the volume fraction of recrystallized grains of the surface layer of the rolled piece is about 95%, the microstructure is a completely dynamic recrystallization structure, and the average grain size of the surface layer of the rolled piece is 16 μm. In the cross wedge rolling process, the distribution characteristics of the microstructure of the rolled piece are related to the special deformation characteristics in the cross wedge rolling forming process, the rolled piece rotates under the action of friction force under the special stress state, and at the moment, the rolled piece not only generates axial stretching and radial compression deformation, but also generates circumferential torsion deformation. In the embodiment, the reduction of area is selected to be 50%, the rolling force of a rolled piece is large, the deformation in each direction is large, the deformation energy storage at the crystal boundary is high, and the deformation activation energy required by the dynamic recrystallization can be provided.
Example 2
In the embodiment, the preparation method of the GH4169 alloy bar with the surface ultrafine grain structure comprises the following steps:
step 1: the method comprises the steps of selecting a GH4169 alloy forging bar, carrying out solution treatment at the temperature of 1035 +/-5 ℃ for 30min, and then carrying out water cooling to room temperature to eliminate element segregation and second phases in the original material to obtain the GH4169 alloy tube bar with fine and uniform crystal grains, wherein the grain size of the GH4169 alloy forging bar is 60-100 mu m.
Step 2: and (3) aging the GH4169 alloy forged bar subjected to solution treatment, heating the bar to 920 ℃ in a resistance furnace, preserving the heat for 24 hours, performing delta phase pre-precipitation treatment, and cooling the bar to room temperature by water to obtain an aged structure.
And step 3: and carrying out wedge cross rolling on the GH4169 alloy forged bar subjected to solid solution and aging treatment, keeping the temperature of the GH4169 alloy tube bar at 1000 ℃ for 30min before rolling, and cooling the GH4169 alloy tube bar to room temperature after rolling. A set of data of the rolling process and the die parameters is selected, and the specific contents are shown in table 1.
As shown in fig. 4, the microstructure of the solution aging bar contains a large amount of sheet-like/long needle-like δ -phase widmanstatten structures, and the content and morphology of the precipitated δ -phase are different in different oriented grains. As shown in FIG. 5, the surface microstructure of the solution aged GH4169 alloy rolled piece by cross wedge rolling. The delta phase morphology is changed from an initial lamellar/long needle shape into a short rod shape/granular shape, the delta phase pre-precipitated in the cross wedge rolling forming process is mainly subjected to torsional fracture, and the spheroidization degree of the delta phase is in positive correlation with the reduction of area, because large local orientation differences are generated between grains and inside the grains of a rolled piece in the cross wedge rolling forming process, the dislocation density at the positions is increased, the dislocation provides a channel for Nb diffusion, the delta phase nucleation free energy is reduced, and the nucleation rate is increased. And the dynamic recrystallization mainly nucleates around the delta phase, is distributed in a strip shape along the delta phase direction, and is compared with the microstructure of the surface layer of a solid solution GH4169 alloy cross wedge rolled piece under the same rolling process condition, the result shows that the surface grain size of the solid solution aging GH4169 alloy cross wedge rolled piece is obviously fine, the average grain size of the surface layer of the rolled piece is only 2 mu m and is obviously lower than the surface grain size of the solid solution GH4169 alloy cross wedge rolled piece by 16 mu m, because the delta phase hinders dislocation movement in the deformation process, a high-density dislocation area is formed around the delta phase, the lamellar delta phase is spheroidized in the deformation process, the spheroidized delta phase provides nucleation particles for new recrystallization, and in addition, the pinning crystal grain boundary of the delta phase inhibits the growth of crystal grains, so the surface grain size of the delta phase aging GH4169 alloy cross wedge rolled piece is obviously finer than that of the solid solution crystal grains.
The results of the above examples show that the invention makes full use of the spheroidization of the sheet delta produced by time effect in the wedge cross rolling process which produces complex stress, and makes the complex stress and the spheroidized delta phase jointly act in the process of dynamic recrystallization, so that the preparation method of the GH4169 alloy forged bar with the surface ultrafine grain structure appears. The advantages of the preparation method are clearly shown by selecting GH4169 alloy forged bars in the two embodiments, and the method is not limited to GH4169 alloy forged bars and is also suitable for GH4169 alloy pipes. Any creation that does not exceed the scope of the present invention shall be protected by the present invention.
Claims (9)
1. A preparation method of a GH4169 alloy tube bar with a surface ultrafine grain structure is characterized in that the GH4169 alloy tube bar is subjected to solid solution aging treatment to pre-precipitate a delta phase, and then the GH4169 alloy tube bar with the surface grain size reaching ASTM12 grade is prepared through a wedge cross rolling process, a complex stress state, delta phase and dynamic recrystallization interaction.
2. The method for preparing GH4169 alloy tube and bar materials with ultra-fine grain structure on the surface according to claim 1, which comprises the following steps:
A. selecting a group of parameters within a given temperature and time range to carry out solution treatment on the GH4169 alloy tube bar to obtain the GH4169 alloy tube bar with uniform structure;
B. selecting a group of parameters for aging treatment of the GH4169 alloy tube and bar subjected to solution treatment within a given temperature range and time to obtain a GH4169 alloy tube and bar with a pre-precipitated delta phase;
C. the GH4169 alloy tube and bar subjected to solid solution and aging treatment is rolled by using a cross wedge rolling process, a group of parameters are selected within a given rolling process and a given die parameter range, and the GH4169 alloy tube and bar with the surface ultrafine grain structure is obtained under the action of complex heat and force coupling.
3. The method for preparing GH4169 alloy tube or bar with ultra-fine grain structure on the surface according to claim 1 or 2, characterized in that during cross wedge rolling, dynamic recrystallization spreads from the surface layer to the center of the rolled piece, and the dynamic recrystallization mechanism is discontinuous dynamic recrystallization; the rolling force and the reduction of area are in positive correlation, the reduction of area is improved, dynamic recrystallization is expanded to the center of a rolled piece, and the GH4169 alloy tube bar with the surface and the center of an ultrafine grain structure is obtained.
4. The method for preparing GH4169 alloy tube and bar with ultra-fine grain structure on the surface according to claim 1 or 2, wherein the solution aging treatment is performed, the pre-precipitated delta phase on the surface layer of the GH4169 alloy tube and bar becomes short rod-shaped or granular in the rolling process, and is distributed on the grain boundary to provide more nucleation particles as dynamic recrystallization, so as to promote the dynamic recrystallization and be beneficial to obtain fine grains.
5. The method for preparing GH4169 alloy tube or bar with ultra-fine grain structure on the surface according to claim 1 or 2, wherein the pre-precipitated delta phase increases the strain activation energy of the GH4169 alloy tube or bar and inhibits the strain from expanding toward the center.
6. The preparation method of the GH4169 alloy tube and bar with the ultrafine grain structure on the surface as claimed in claim 2, wherein in the step A, the GH4169 alloy forged tube and bar is selected and subjected to solution treatment, the selected temperature range is 1020-1050 ℃, the heat preservation time is 30-50 min, the GH4169 alloy tube and bar is cooled to room temperature by water, and the grain size of the GH4169 alloy tube and bar is 60-100 μm.
7. The preparation method of the GH4169 alloy tube and bar with the ultrafine grain structure on the surface as claimed in claim 2, wherein in the step B, the temperature range for aging treatment is 910-930 ℃, the heat preservation time is 20-24 h, and the temperature is cooled to room temperature by water.
8. The preparation method of the GH4169 alloy tube and bar with the ultrafine grain structure on the surface as claimed in claim 2, wherein in the step C, the GH4169 alloy tube and bar after the solution treatment and the aging treatment is subjected to wedge cross rolling, the heat preservation of the GH4169 alloy tube and bar at 950-1050 ℃ is ensured for 20-40 min before rolling, and the GH4169 alloy tube and bar is cooled to room temperature after rolling.
9. The preparation method of the GH4169 alloy tube and bar with the ultrafine grain structure on the surface according to claim 2 or 5, characterized in that in the step C, the GH4169 alloy tube and bar with the pre-precipitated delta phase is subjected to cross wedge rolling, wherein the cross wedge rolling process conditions and the die parameter ranges are met, the rolling speed is 300-500 mm/s, the forming angle is 28-32 degrees, the widening angle is 6-8 degrees, the grain size of the surface of the GH4169 alloy tube and bar is 2-5 μm, and the grain size of the core of the GH4169 alloy tube and bar is 20-30 μm.
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| CN115821180A (en) * | 2022-12-06 | 2023-03-21 | 浙江浙能技术研究院有限公司 | Method for obtaining GH4169 alloy forging with uniform and fine grain structure |
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| WO2016179780A1 (en) * | 2015-05-11 | 2016-11-17 | 怀集登云汽配股份有限公司 | Efficient near net shape precision forming method of hollow valve blank for engine |
| CN107866512A (en) * | 2017-04-28 | 2018-04-03 | 中国科学院金属研究所 | Difficult-to-deformation material blank-making method based on cross wedge rolling |
| CN108080544A (en) * | 2017-11-23 | 2018-05-29 | 中国航发沈阳黎明航空发动机有限责任公司 | A kind of double installing plate stator blade blank manufacturing process of compressor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016179780A1 (en) * | 2015-05-11 | 2016-11-17 | 怀集登云汽配股份有限公司 | Efficient near net shape precision forming method of hollow valve blank for engine |
| CN107866512A (en) * | 2017-04-28 | 2018-04-03 | 中国科学院金属研究所 | Difficult-to-deformation material blank-making method based on cross wedge rolling |
| CN108080544A (en) * | 2017-11-23 | 2018-05-29 | 中国航发沈阳黎明航空发动机有限责任公司 | A kind of double installing plate stator blade blank manufacturing process of compressor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115821180A (en) * | 2022-12-06 | 2023-03-21 | 浙江浙能技术研究院有限公司 | Method for obtaining GH4169 alloy forging with uniform and fine grain structure |
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