CN112126875B - Multi-level heterostructure dual-phase alloy and hot rolling method thereof - Google Patents
Multi-level heterostructure dual-phase alloy and hot rolling method thereof Download PDFInfo
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Abstract
The invention discloses a multi-level heterostructure dual-phase alloy and a hot rolling method thereof, wherein a zirconium-niobium alloy is kept at a temperature of 700-beta transition temperature for 10-60 min under an argon atmosphere, then the alloy is subjected to rolling deformation with a single-pass reduction of 10-30%, and the alloy is kept at the temperature and the atmosphere for 1-10 min again after every 1-3 passes until the total rolling reduction rate reaches 60-100%. And annealing the rolled zirconium-niobium alloy at the temperature and in the atmosphere for 1-30 min, and cooling to room temperature at different rates. Finally, stress annealing is carried out on the annealed zirconium-niobium alloy at the temperature of 300-500 ℃ in an argon atmosphere for 0.5-2 h, and air cooling is carried out to room temperature; the multi-level heterostructure dual-phase zirconium-niobium alloy prepared by the method has high plasticity, the yield strength is not less than 658MPa, the tensile strength is not less than 880MPa, and the fracture elongation is not less than 17.6%.
Description
Technical Field
The invention belongs to the field of metal materials, and particularly relates to a multi-level heterostructure dual-phase alloy and a hot rolling method thereof.
Background
The zirconium alloy has the advantages of low thermal neutron absorption cross section, good high-temperature water corrosion resistance, excellent comprehensive mechanical property, higher heat conductivity and the like, is widely applied to the cladding tube of a nuclear reactor fuel assembly, and is an irreplaceable key structural material for developing nuclear power and nuclear power ships. However, with the gradual extension of the refueling period of nuclear fuel in nuclear power plants and nuclear power vessels and the gradual increase of the operating power of reactors, the service performance, especially the mechanical property (<500MPa), of the existing zirconium alloy cladding material cannot meet the actual requirement, so that the research and development of a zirconium alloy material with more excellent mechanical property becomes one of the problems to be solved in the field of nuclear industry.
The Chinese invention patent CN102965605A introduces a method for preparing a high-strength plastic nano-structure zirconium alloy material by liquid nitrogen low-temperature rolling, which has the advantages of high tensile strength (>836MPa) and good uniform elongation (> 6%). But has the disadvantages of long process flow: placing a zirconium alloy plate rolled at low temperature by liquid nitrogen in boron nitride powder to be pressed into a columnar sheet, and placing the columnar sheet in a muffle furnace for drying; then mixing and pressing the oxidized fault powder and the diluted water glass into a columnar zirconium nitride sheet, and putting the columnar zirconium nitride sheet into a muffle furnace for drying; finally, the dolomite sheet, the zirconium plate boron nitride sheet and the zirconium oxide sheet are stacked in the columnar hole of the pyrophyllite cube, and the pyrophyllite cube is placed in a cubic press and subjected to high-pressure treatment.
Chinese patent CN110195199A describes a three-dimensional layered zirconium alloy, which contains a large number of phase interfaces, and has a certain resistance to dislocation slip during the plastic deformation of zirconium alloy, so as to improve the strength of zirconium alloy. But the defects that the zirconium alloy needs to be compressed by 75 percent in a single pass, the deformation is huge, and the requirement on the forging capability of mechanical equipment is high; secondly, the alpha phase and the beta phase of the layered structure accord with the Burges relationship of crystallography, the interface is in a coherent or semi-coherent state, and the barrier effect on dislocation slip in the plastic deformation process of the zirconium alloy is weaker, so that the strength of the zirconium alloy is improved by a smaller amplitude (less than or equal to 693 MPa).
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a multi-level heterostructure dual-phase alloy and a hot rolling method thereof, the method can reasonably utilize the blocking effect of various interfaces on dislocation slippage, improve the strength of the zirconium alloy, simultaneously improve the strain strengthening capability of the alloy by utilizing the heterostructure, and keep higher fracture elongation, and the hot rolling method has the advantages of simple process, short flow and low requirement on equipment.
The invention is realized by the following technical scheme:
a hot rolling method of a multi-level heterostructure dual-phase alloy comprises the following steps:
step 1, preserving the temperature of an alloy in an alpha + beta two-phase region between 700 and beta transition temperature for 10-60 min under an argon atmosphere to form an equiaxial alpha phase and an equiaxial beta phase in the alloy;
step 3, annealing the alloy obtained in the step 2 at 700-beta transition temperature and in an argon atmosphere for 1-30 min, and cooling to room temperature;
and 4, performing stress annealing on the alloy obtained in the step 3 at the temperature of 300-500 ℃ in an argon atmosphere for 0.5-2 h, and then performing air cooling to room temperature to obtain the multi-level heterostructure biphase alloy.
Preferably, in the step 2, the time interval from the rolling deformation of the alloy to the furnace returning and heat preservation is less than 2 min.
Preferably, the cooling rate after annealing in step 3 is >25 ℃/s or <25 ℃/s.
Preferably, the multi-level heterostructure dual phase alloy prepared when the cooling rate is >25 ℃/s is as follows:
the alloy comprises an alpha and alpha 'dual-phase structure, wherein the alpha phase in the dual-phase structure is a micron-sized isometric crystal structure, the alpha' phase is a submicron-sized prism-shaped lamellar structure and a lath-shaped lamellar structure, and the prism-shaped lamellar structure contains nanoscale twin crystal lamella which are parallel to each other.
Preferably, the lamellar structure α' phase is transformed from an equiaxed β phase upon cooling at a rate >25 ℃/s.
Preferably, the multi-level heterostructure dual phase alloy prepared when the cooling rate is <25 ℃/s is as follows:
the alloy comprises an alpha and beta double-phase structure, wherein the alpha phase in the double-phase structure is a micron-sized isometric crystal structure and a submicron-sized lamellar structure, the beta phase is a nanoscale lamellar structure, and the alpha phase of the lamellar structure and the beta phase of the lamellar structure are parallel to each other.
Preferably, the lamellar structure alpha phase and lamellar structure beta phase, which are parallel to each other, are transformed when the equiaxed beta phase is cooled at a rate <25 ℃/s.
A multi-level heterostructure biphase alloy prepared by the hot rolling method comprises alpha and alpha 'biphase structures, wherein the alpha phase is a micron-sized equiaxial crystal structure, the alpha' phase is a submicron prism-shaped lamellar structure and a lath-shaped lamellar structure, the prism-shaped lamellar structure contains nanometer-sized twin crystal lamella, and the twin crystal lamella are parallel to each other;
or comprises alpha and beta double-phase structures, the alpha phase is a micron-sized isometric crystal structure and a submicron-sized lamellar structure, the beta phase is a nanoscale lamellar structure, and the alpha phase of the lamellar structure and the beta phase of the lamellar structure are mutually parallel.
Preferably, the volume fraction of the micron-sized equiaxed alpha phase is 80% or less and is not 0.
Preferably, the alloy is a zirconium alloy or a titanium alloy.
Compared with the prior art, the invention has the following beneficial technical effects:
the hot rolling method of the multi-level heterostructure dual-phase alloy provided by the invention is characterized in that the multi-level heterostructure dual-phase alloy is subjected to hot rolling and cooling in an alpha + beta two-phase region, a certain content of equiaxial alpha phase is reserved, a submicron and nanoscale fine lamellar structure phase is generated, a coarse soft phase and a fine hard phase are not uniformly deformed in the plastic deformation process, in order to keep the continuity of deformation, dislocation can be accumulated near an interface at one side of the soft phase, the accumulated dislocation backs to a harder phase and reacts on a dislocation source, the microscopic internal stress is called back stress, when the back stress is large enough, the dislocation source can be stopped, and the back stress can simultaneously improve the processing hardening capacity and the strain strengthening capacity of the alloy, so that the alloy shows better strength and plastic combination. Meanwhile, the alpha' phase formed in the cooling process contains high-density dislocation, and the dislocation strengthening is also beneficial to improving the alloy strength. Therefore, the alpha + alpha' dual-phase alloy has higher strength, the alloy prepared by the method has small grain size, can fully strengthen the back stress of the alloy with the heterostructure, has uniform stress distribution, and avoids local stress concentration and premature cracking, thereby obtaining higher strength and keeping excellent plasticity. The hot rolling method has the advantages of simple process, short flow and low requirement on equipment.
The multi-level heterostructure two-phase alloy provided by the invention fully utilizes the blocking effect of multi-scale and multi-morphology crystal grain interfaces on dislocation slippage, remarkably improves the tensile strength (>880MPa) of the alloy, and meanwhile, heterostructures with different hardness and softness can coordinate deformation of two sides of the interface and avoid stress concentration, so that the alloy also keeps higher elongation at break (> 17.6%).
Drawings
FIG. 1 is an EBSD photograph of the zirconium niobium alloy structure of example 1 of the present invention.
FIG. 2 is a transmission electron micrograph of a structure of a zirconium niobium alloy according to example 1 of the present invention.
FIG. 3 is a graph of the engineering strain-engineering stress-strain elongation of the zirconium niobium alloy of example 1 of the present invention.
FIG. 4 is an EBSD photograph of the zirconium niobium alloy structure of example 2 of the present invention.
FIG. 5 is a transmission electron micrograph of a structure of a zirconium niobium alloy according to example 2 of the present invention.
FIG. 6 is a graph of the engineering strain-engineering stress-strain elongation of a zirconium niobium alloy of example 2 of the present invention.
FIG. 7 is a transmission electron micrograph of a structure of a zirconium niobium alloy according to example 4 of the present invention.
FIG. 8 is a tensile diagram of the engineering strain-engineering stress of the zirconium niobium alloy of example 4 of the present invention.
FIG. 9 is a transmission electron micrograph of a structure of a zirconium niobium alloy according to a comparative example of the present invention.
FIG. 10 is a tensile strain diagram of engineering strain versus engineering stress for a zirconium niobium alloy of a comparative example of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to the attached drawings, which are illustrative, but not limiting, of the present invention.
Example 1:
a hot rolling method of a multi-layer heterostructure two-phase zirconium-niobium alloy comprises the following steps:
step 1, maintaining a Zr-2.5Nb alloy plate with the thickness of 7mm in a furnace filled with argon at the temperature of 815 ℃ for 30 min;
and 2, taking out the sample for rolling, wherein the single-pass reduction is 20%, and after every two passes of rolling, the sample is thermally insulated again for 1min at 815 ℃ in a furnace filled with argon, and the total rolling reduction rate is 75%.
And 3, annealing the sample in a furnace filled with argon at 815 ℃ for 5min after rolling, and cooling to room temperature at the speed of 25 ℃/s after annealing.
And 4, stress relief annealing the deformed and annealed sample for 1h at 400 ℃ in a furnace filled with argon to obtain the multi-level heterostructure two-phase zirconium-niobium alloy.
As shown in FIG. 1, the structure of the crystal comprises 2-5 μm equiaxed alpha phase and 0.15-0.25 μm flaky alpha' phase, and the volume fraction of the equiaxed alpha phase is 40%. The further magnified transmission electron microscope photo shows that the prism-shaped flaky alpha' phase also comprises a twin crystal lamella layer with the thickness of 30-60 nm, as shown in figure 2; the mechanical property test shows that the yield strength of the zirconium-niobium alloy reaches 607MPa, the tensile strength reaches 808MPa, the elongation at break reaches 16%, and the tensile curve is shown in figure 3.
Example 2:
a hot rolling method of a multi-layer heterostructure two-phase zirconium-niobium alloy comprises the following steps:
step 1, preserving heat of a Zr-2.5Nb alloy plate with the thickness of 7mm for 30min in a furnace filled with argon at 860 ℃;
and 2, taking out the sample for rolling, wherein the single-pass reduction is 20%, and after every two passes of rolling, the sample is thermally insulated again for 1min at 860 ℃ in a furnace filled with argon, and the total rolling reduction rate is 75%.
And 3, annealing the sample in a furnace filled with argon at 860 ℃ for 5min after rolling, and cooling to room temperature at the speed of 25 ℃/s after annealing.
And 4, stress relief annealing the deformed and annealed sample for 1h at 400 ℃ in a furnace filled with argon. And obtaining the multi-layer heterostructure biphase zirconium-niobium alloy.
As shown in FIG. 4, the structure of the crystal comprises 2-5 μm equiaxed alpha phase and 0.17-0.32 μm flaky alpha' phase, and the volume fraction of the equiaxed alpha phase is 25%. The further magnified transmission electron micrograph shows that the prismatic flaky alpha' phase also contains a twin crystal lamella layer with a thickness of 30-60 nm, as shown in FIG. 5. The mechanical property test shows that the yield strength of the multi-scale and multi-morphology heterostructure zirconium-niobium alloy reaches 658MPa, the tensile strength reaches 880MPa, the elongation at break reaches 17.6%, and the tensile curve is shown in FIG. 6.
Example 3:
a hot rolling method of a multi-layer heterostructure two-phase zirconium-niobium alloy comprises the following steps:
step 1, a 7mm thick Zr-2.5Nb alloy plate is kept warm for 30min in a furnace filled with argon at 880 ℃.
And 2, taking out the sample for rolling, wherein the single-pass reduction is 20%, and after every two passes of rolling, the sample is thermally insulated again for 1min at 860 ℃ in a furnace filled with argon, and the total rolling reduction rate is 75%.
And 3, annealing the sample in a furnace filled with argon at 880 ℃ for 5min after rolling, and cooling to room temperature at the speed of 25 ℃/s after annealing.
And 4, stress relief annealing the deformed and annealed sample for 1h at 400 ℃ in a furnace filled with argon to obtain the multi-level heterostructure two-phase zirconium-niobium alloy.
The dual-phase zirconium-niobium alloy structure comprises 2-5 mu m of equiaxial alpha phase and 0.17-0.32 mu m of flaky alpha' phase, and the volume fraction of the equiaxial alpha phase is 12%. The further magnified transmission electron microscope photo shows that the prism-shaped flaky alpha' phase also contains a twin crystal lamella layer with the thickness of 30-60 nm. Mechanical property tests show that the yield strength of the multi-scale and multi-morphology heterostructure zirconium-niobium alloy reaches 645MPa, the tensile strength reaches 797MPa, and the fracture elongation reaches 15.9%.
Example 4:
a hot rolling method of a multi-layer heterostructure two-phase zirconium-niobium alloy comprises the following steps:
step 1, preserving heat of a Zr-2.5Nb alloy plate with the thickness of 7mm for 30min in a furnace filled with argon at the temperature of 910 ℃,
and 2, taking out the sample for rolling, wherein the single-pass reduction is 20%, and after every two passes of rolling, the sample is thermally insulated for 1min again in a furnace filled with argon at 910 ℃, and the total rolling reduction rate is 75%.
And 3, annealing the sample in a furnace filled with argon at 910 ℃ for 2min after rolling, and cooling to room temperature at the rate of 3 ℃/s after annealing.
And 4, stress relief annealing the deformed and annealed sample for 1h at 400 ℃ in a furnace filled with argon to obtain the multi-level heterostructure two-phase zirconium-niobium alloy.
As shown in FIG. 7, the structure includes 2 to 5 μm of equiaxed alpha phase, 0.14 to 0.3 μm thick flaky alpha phase and 10 to 30nm thick flaky beta phase. Wherein the flaky alpha phase and the flaky beta phase are parallel to each other. At this time, the total volume of the equiaxed α phases in the sample was 1%. Mechanical property tests show that the yield strength of the multi-layer heterostructure dual-phase zirconium-niobium alloy reaches 605MPa, the tensile strength reaches 812MPa, the elongation at break reaches 14.2%, and the tensile curve is shown in figure 8.
Example 5:
a hot rolling method of a multi-layer heterostructure two-phase zirconium-niobium alloy comprises the following steps:
step 1, keeping the temperature of a Zr-2.5Nb alloy plate with the thickness of 7mm in a furnace filled with argon at 700 ℃ for 60min,
and 2, taking out the sample for rolling, wherein the single-pass reduction is 30%, and the sample is subjected to heat preservation again for 10min at 700 ℃ in a furnace filled with argon after every three passes of rolling, and the total rolling reduction rate is 100%.
And 3, annealing the sample in a furnace filled with argon at 700 ℃ for 30min after rolling, and cooling to room temperature at the speed of 26 ℃/s after annealing.
And 4, performing stress relief annealing on the deformed and annealed sample in a furnace filled with argon at 500 ℃ for 2 hours to obtain the multi-level heterostructure two-phase zirconium-niobium alloy.
In this case, the structure contains 2 to 5 μm of equiaxed alpha phase and 0.13 to 0.22 μm of flaky alpha' phase, and the volume fraction of the equiaxed alpha phase is 79%. Further magnifying and observing to find that the prism-shaped flaky alpha' phase also comprises a twin crystal lamella with the thickness of 30-60 nm; the mechanical property test shows that the yield strength of the zirconium-niobium alloy reaches 546MPa, the tensile strength reaches 725MPa, the elongation at break reaches 21%, and the tensile curve is shown in figure 3.
Example 6:
a hot rolling method of a multi-layer heterostructure two-phase zirconium-niobium alloy comprises the following steps:
step 1, keeping the temperature of a Zr-2.5Nb alloy plate with the thickness of 7mm in a furnace filled with argon at 700 ℃ for 10min,
and 2, taking out the sample to be rolled, wherein the single-pass reduction is 10%, the temperature of the sample after each pass of rolling is maintained for 1min in a furnace filled with argon again at 700 ℃, and the total rolling reduction rate is 60%.
And 3, annealing the sample in a furnace filled with argon at 700 ℃ for 1min after rolling, and cooling to room temperature at the speed of 24 ℃/s after annealing.
And 4, stress relief annealing the deformed and annealed sample in a furnace filled with argon at 300 ℃ for 0.5h to obtain the multi-level heterostructure two-phase zirconium-niobium alloy. Example 7:
a hot rolling method of a multi-layer heterostructure two-phase zirconium-niobium alloy comprises the following steps:
step 1, keeping the temperature of a Zr-2.5Nb alloy plate with the thickness of 7mm in a furnace filled with argon at 700 ℃ for 60min,
and 2, taking out the sample for rolling, wherein the single-pass reduction is 10%, and the sample is subjected to heat preservation again for 1min at 700 ℃ in a furnace filled with argon after every three passes of rolling, and the total rolling reduction rate is 60%.
And 3, annealing the sample in a furnace filled with argon at 700 ℃ for 30min after rolling, and cooling to room temperature at the speed of 1 ℃/s after annealing.
And 4, stress relief annealing the deformed and annealed sample in a furnace filled with argon at 300 ℃ for 0.5h to obtain the multi-level heterostructure two-phase zirconium-niobium alloy.
Comparative examples
This comparative example is essentially the same as the method of examples 1-7 above, except for the process parameters, particularly the stress relief annealing temperature and time in step 4
A hot rolling method of a multi-layer heterostructure two-phase zirconium-niobium alloy comprises the following steps:
step 1, preserving the heat of a Zr-2.5Nb alloy plate with the thickness of 7mm for 30min in a furnace filled with argon at 860 ℃.
And 2, taking out the sample and rolling the sample, wherein the single-pass reduction is 20%, the sample is subjected to heat preservation again for 1min at 860 ℃ in a furnace filled with argon after every two-pass rolling, and the total rolling reduction rate is 75%.
And 3, annealing the sample in a furnace filled with argon at 860 ℃ for 5min after rolling, and cooling to room temperature at the speed of 25 ℃/s after annealing.
And 4, annealing the deformed and annealed sample at 580 ℃ in a furnace filled with argon for stress relief annealing for 10 hours to obtain the coarse zirconium-niobium alloy with the isometric structure.
As shown in FIG. 9, the mechanical property test shows that the yield strength of the zirconium niobium alloy with the structure reaches 502MPa, the tensile strength reaches 575MPa, the elongation at break reaches 42.5%, and the tensile curve is shown in FIG. 10.
The sample is composed of only coarse equiaxed grains, the total grain boundary area of the coarse equiaxed grain sample is small, and the dislocation slip resistance is also small in the stretching deformation process. Meanwhile, the larger the crystal grains, the smaller the number of crystal grains having different orientations, and the smaller the number of propagation of dislocation slip from one crystal grain to another crystal grain having different orientations, i.e., the smaller the hindrance of dislocation slip. Therefore, the sample having only coarse isometric crystals has a low strength and a large tensile strain. In the multi-level heterostructure biphase alloy, the content of submicron and nano-scale crystal grains is larger, the total area of crystal boundaries is large, and the orientations of the crystal grains are different, so that the dislocation slip resistance is larger and the strength is higher in the stretching deformation process, and meanwhile, the local necking fracture of the alloy is easily caused by stress concentration caused by dislocation plug accumulation, and the plasticity is reduced.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. A hot rolling method of a multi-level heterostructure dual-phase alloy is characterized by comprising the following steps:
step 1, in an argon atmosphere, carrying out heat preservation on a Zr-2.5Nb alloy in an alpha + beta two-phase region between 700 ℃ and beta transition temperature for 10-60 min to form an equiaxial alpha phase and an equiaxial beta phase in the alloy;
step 2, carrying out rolling deformation with the single-pass reduction of 10-30% on the alloy obtained in the step 1, and after each 1-3-pass rolling, preserving the temperature of the alloy again for 1-10 min at the temperature of 700-beta transformation temperature and under the argon atmosphere until the total rolling reduction rate of the alloy reaches 60-100%;
step 3, annealing the alloy obtained in the step 2 at 700-beta transition temperature and in an argon atmosphere for 1-30 min, and cooling to room temperature;
and 4, performing stress annealing on the alloy obtained in the step 3 at the temperature of 300-500 ℃ in an argon atmosphere for 0.5-2 h, and then performing air cooling to room temperature to obtain the multi-level heterostructure biphase alloy.
2. A hot rolling method of a multi-level heterostructure two-phase alloy according to claim 1, wherein in step 2, the alloy is kept warm for less than 2min after rolling deformation and after returning to the furnace.
3. A hot rolling process of a multi-level heterostructure dual phase alloy according to claim 1, characterized in that the cooling rate after annealing in step 3 is >25 ℃/s or <25 ℃/s.
4. A hot rolling process of a multi-level heterostructure dual phase alloy according to claim 3, characterized in that the multi-level heterostructure dual phase alloy is prepared with a cooling rate >25 ℃/s as follows:
the alloy comprises an alpha and alpha 'dual-phase structure, wherein the alpha phase in the dual-phase structure is a micron-sized isometric crystal structure, the alpha' phase is a submicron-sized prism-shaped lamellar structure and a lath-shaped lamellar structure, and the prism-shaped lamellar structure contains nanoscale twin crystal lamella which are parallel to each other.
5. A hot rolling process of a multi-level heterostructure dual phase alloy according to claim 4, wherein the lamellar structure α' phase is transformed from equiaxed β phase when cooled at a rate >25 ℃/s.
6. A hot rolling process of a multi-level heterostructure dual phase alloy according to claim 3, characterized in that the multi-level heterostructure dual phase alloy is prepared when the cooling rate is <25 ℃/s as follows:
the alloy comprises an alpha and beta double-phase structure, wherein the alpha phase in the double-phase structure is a micron-sized isometric crystal structure and a submicron-sized lamellar structure, the beta phase is a nanoscale lamellar structure, and the alpha phase of the lamellar structure and the beta phase of the lamellar structure are parallel to each other.
7. A hot rolling process of a multi-level heterostructure two-phase alloy according to claim 6, wherein the mutually parallel lamellar α and β phases are transformed from equiaxed β phases upon cooling at a rate <25 ℃/s.
8. A multi-level heterostructure two-phase alloy prepared by the hot rolling method according to claim 1, wherein the alloy comprises a and a 'two-phase structures, the a phase is a micron-sized equiaxed crystal structure, the a' phase is a submicron-sized prism-shaped lamellar structure and a lath-shaped lamellar structure, the prism-shaped lamellar structure comprises nanometer-sized twin crystal lamella, and the twin crystal lamella are parallel to each other;
or comprises alpha and beta double-phase structures, the alpha phase is a micron-sized isometric crystal structure and a submicron-sized lamellar structure, the beta phase is a nanoscale lamellar structure, and the alpha phase of the lamellar structure and the beta phase of the lamellar structure are mutually parallel.
9. The multi-level heterostructure dual phase alloy of claim 8, wherein the micron-sized equiaxed alpha phase has a volume fraction of 80% or less and is not 0.
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| CN113174551B (en) * | 2021-03-30 | 2022-08-09 | 西安交通大学 | Dual-phase high-strength high-plasticity titanium alloy with heterogeneous laminated structure and preparation method thereof |
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