CN102653846A - Large-thickness easy-to-weld quenched and tempered high-strength steel plate for hydroelectricity and manufacturing method thereof - Google Patents
Large-thickness easy-to-weld quenched and tempered high-strength steel plate for hydroelectricity and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a large-thickness easy-to-weld quenched and tempered high-strength steel plate used for hydroelectricity, and also relates to a manufacturing method of the steel plate. The large-thickness easy-to-weld quenched and tempered high-strength steel plate used for hydroelectricity disclosed by the invention is composed of the following chemical components in percentage by weight: 0.15%-0.18% of C, 0.15%-0.35% of Si, 0.90%-1.00% of Mn, less than or equal to 0.012% of P, less than or equal to 0.005% of S, 1.52%-1.60% of Ni, 0.30%-0.40% of Cr, 0.020%-0.030% of Nb, 0.020%-0.050% of Al, 0.20%-0.30% of Mo, 0.055%-0.065% of V, 0.0007%-0.0015% of B, 0.015%-0.025% of Ti, and the balance of Fe and inevitable impurities. The manufacturing method of the steel plate comprises the following steps of: electric furnace smelting, LF (ladle furnace)/VD (vacuum distillation) refining, die casting, ingot heating, rolling, water cooling after rolling, thermal stacking, and heat treatment to obtain a finished product. The maximum thickness of the large-thickness easy-to-weld quenched and tempered high-strength steel plate used for hydroelectricity disclosed by the invention can achieve 230 mm; and the large-thickness easy-to-weld quenched and tempered high-strength steel plate has the characteristics of good welding performance, low yield ratio, good low-temperature impact tenacity and good thickness directional property, and has wide application prospects.
Description
Technical field
The present invention relates to a kind of water power with big thickness easy-weld hardening high-strength steel plate, relate to a kind of working method of this steel plate simultaneously.
Background technology
The maximum hydraulic generator unit of at present external rated output is 700MW, totally 23.700MW that China has put into operation and above hydraulic generator unit have reached nearly 50; Estimate also having 35 rated output is the generating of will before 2015, going into operation of 700MW and above hydraulic generator unit, and wherein maximum rated power is to 8 800MW hydraulic generator units in power station, tame dam and 18 770MW hydraulic generator units in small stream Luo Du power station.
The application of huge water wheel generator group relates to unit and support equipment manufacturing.Unit capacity and operating head polishing all are higher than the Three Gorges unit, therefore steel plate thickness and performance demands are further improved, and have exceeded the used steel plate scope of existing hydraulic generator unit.Because the thickness (the thickest 230mm that reaches) of super large, higher welding property requirement, but lower ring plate depends on import with big thickness 500MPa level weld hardening high-strength steel plate all the time on the hydraulic generator unit seat ring.
Summary of the invention
To the problems referred to above, the purpose of this invention is to provide a kind of water power with big thickness easy-weld hardening high-strength steel plate and working method thereof, to improve thickness, welding property, anti-lamellar tearing performance, intensity and the low-temperature impact toughness of steel plate.
For realizing above purpose, the technical scheme that the present invention adopted is that a kind of water power is made up of following components in weight percentage with big thickness easy-weld hardening high-strength steel plate: C:0.15%～0.18%, Si:0.15%～0.35%; Mn:0.90%～1.00%, P≤0.012%, S≤0.005%; Ni:1.52%～1.60%, Cr:0.30%～0.40%, Nb:0.020%～0.030%; Al:0.020%～0.050%, Mo:0.20%～0.30%, V:0.055%～0.065%; B:0.0007%～0.0015%, Ti:0.015%～0.025%, surplus is Fe and unavoidable impurities.
The maximum ga(u)ge of said steel plate is 230mm.
Simultaneously, technical scheme of the present invention has also adopted the working method of a kind of water power with big thickness easy-weld hardening high-strength steel plate, comprises the steps:
(1) smelts: will contain following weight percent C:0.15%～0.18%, Si:0.15%～0.35%, Mn:0.90%～1.00%; P≤0.012%, S≤0.005%, Ni:1.52%～1.60%; Cr:0.30%～0.40%, Nb:0.020%～0.030%, Al:0.020%～0.050%; Mo:0.20%～0.30%, V:0.055%～0.065%, B:0.0007%～0.0015%; The molten steel of Ti:0.015%～0.025% component is earlier through electrosmelting; Send into the refining of LF refining furnace, when liquid steel temperature meets or exceeds 1640 ± 10 ℃, change the vacuum outgas of VD stove over to and handle, add CaSi piece>=100kg/ stove or Fe-Ca line 400～450m change inclusion morphology before the VD;
(2) die casting: adopt the Large Flat ingot mold to pour into a mould, and adopt the protection of inert gas cast;
(3) heating: maximum heating temperature is 1240 ℃, and soaking temperature is 1180～1200 ℃, and be 24～30h total heat-up time, soaking time >=5h;
(4) rolling: adopt high temperature recrystallize technology controlling and process rolling technology, start rolling temperature is 1000～1050 ℃, and low speed heavy reduction rolling, single pass draught are 10～20%, and finishing temperature is 940 ± 20 ℃, and the accumulative total draft is 70～80%;
(5) roll the back water-cooled: quick water-cooled to 780 after steel plate rolls～810 ℃;
(6) thermal reactor buttress: timely wind sheltering stacking after the water-cooled, the stacking temperature is 650～680 ℃, the stacking time is 72h, obtains the steel plate bullion;
(7) thermal treatment:
Intercritical hardening: the steel plate bullion is carried out heat tracing at 760 ℃～800 ℃ handle; Put into quenching bath water medium quenching then fast; Water temperature is not higher than 25 ℃ before the steel plate entry, and water temperature is not higher than 30 ℃ after the water outlet, and the steel plate entry time is controlled between 60～70min;
Tempering: tempering temperature is between 660～680 ℃, and soaking time obtains the finished product steel plate at 3.5～4.0min/mm.
Vacuum tightness≤66.6Pa that the described vacuum outgas of step (1) is handled, vacuum hold-time>=25min.
The described teeming temperature of step (2) is 1545～1555 ℃, and the minimum thickness of band steel cover half is 780mm.
Big thickness easy-weld hardening high-strength steel of the present invention adopts carbon, manganese solution strengthening; Add minor N b, V crystal grain thinning, its carbonitride plays dispersion-strengthened action; Nickel both can guarantee the low-temperature flexibility of steel as main strengthening element, also can improve the welding property of steel; Through follow-up rational heat treatment technology, steel plate has big thickness and good performance.
Each component of steel plate and content effect in the present invention are:
C:0.15%～0.18%, carbon produces remarkably influenced to ys, tensile strength, the welding property of steel.Carbon can significantly improve armor plate strength through the gap solid solution, for the thick steel plate of 230mm, guarantees that a certain amount of carbon content is necessary, but the too high welding property and the toughness that can influence steel again of carbon content.
As reductive agent and reductor, simultaneously Si also can play the solution strengthening effect in steelmaking process for Si:0.15%～0.35%, silicon, but silicon can cause the toughness of steel to descend when excessive, causes weld seam fusion area fragility.
Mn:0.90%～1.00%, manganese is with low cost, can increase toughness, intensity and the hardness of steel, improves the hardening capacity of steel, improves the hot workability of steel; The manganese amount is too high, produces segregation easily at the large steel ingot center, and the eutectoid point carbon content of steel is reduced, thereby increases the content of organizing Medium pearlite, and is unfavorable to toughness.
Ni:1.52%～1.60%, nickel are principal character elements of the present invention, and nickel is dissolved in austenite, suppress austenite recrystallization, and refine austenite crystal grain improves the steel plate low-temperature flexibility.The nickel that adds certain amount in addition can also improve weldableness and notch toughness.
Cr:0.30%-0.40%, chromium are the principal elements that carbide forms, and increase austenitic stability, reduce critical cooling velocity, improve hardening capacity, temper resistance and impelling strength, can reduce weldableness but add-on is more.
Mo:0.20%-0.30%, the carbide of molybdenum is dissolved in austenite, improves the intensity of steel, improves hardening capacity, stops austenite to be grown up, and improves temper resistance, eliminates temper brittleness.
P≤0.012%, S≤0.005%: in the ordinary course of things, p and s all is a harmful element in the steel, increases the fragility of steel.Phosphorus reduces welding property, reduces plasticity, makes the cold-bending property variation; Sulphur reduces the ductility and the toughness of steel, is forging and causing when rolling crackle.Therefore, should reduce the content of p and s in steel as far as possible.
Al:0.020%～0.050%, aluminium are reductors commonly used in the steel.Add a spot of aluminium in the steel, but crystal grain thinning improves impelling strength.Aluminium also has oxidation-resistance and corrosion resistance, too high hot workability, welding property and the machinability that then influences steel.
Nb:0.020%～0.030%, the adding of niobium are in order to promote the grain refining of steel rolling microstructure, can improve intensity and toughness simultaneously that niobium can pass through to suppress the effective refinement microstructure of austenite recrystallization, and the precipitation strength matrix in the controlled rolling process.Niobium can reduce the superheated susceptivity and the temper brittleness of steel.In the welding process, the alligatoring that gathers and separate out austenite crystal in the time of can hindering heating partially of niobium, boron atom, and guarantee to obtain more tiny heat affected zone tissue after the welding, improve welding property.
V:0.055%～0.065%, vanadium are the good reductors of steel.But add vanadium thinning microstructure crystal grain in the steel, improve intensity and toughness.The carbide that vanadium and carbon form can improve anti-hydrogen-type corrosion ability under HTHP.
Ti:0.015%～0.025%, titanium are good reductors.Add carbide, nitride or carbonitride that Ti can form Ti with C, N element in the steel, these compounds have good grain refining effect.
B:0.0007%～0.0015%, boron increase hardening capacity, and its effect is higher more than 100 times than chromium, manganese, cause hot-shortly but boron steel is prone to separate out boride at crystal boundary, and weldableness are caused bigger infringement.
The present invention has the following advantages: Steel Alloy content 1. of the present invention is lower; Optimize the proportioning of element in the steel plate through adjustment; Can guarantee under the low-carbon-equivalent condition that steel plate has favorable tissue, over-all properties and welding property; Can also reduce the cost, enhance one's market competitiveness, reach the target of substituting imports with production; 2. the working method of steel plate of the present invention adopts that the recrystallize type is rolling to be aided with quick refrigerative technology, has solved the mill milling insufficient pressure and causes the problem of the thick inequality of crystal grain, the high comprehensive performance of steel plate; Be applicable to the manufacturing of lower ring plate on the huge power unit seat ring, and can be applied to other and require steel plate to have the making of the structural part of better weldableness, have a extensive future; 3. armor plate strength of the present invention is higher, and ys is more than 440MPa, and tensile strength is between 540MPa～720MPa; 0 ℃ of impact of collision merit KV
2Be not less than 50 joules, 0 ℃ transverse impact merit KV
2Be not less than 30 joules; Steel plate Z to the stretching relative reduction in area greater than 35%; 4. the steel plate maximum ga(u)ge can reach 230mm; 5. to be organized as with tempering troostite+tempering ferrite bainite be the complex tissue of main and a small amount of granular ferrite to steel plate.
Description of drawings
Fig. 1. grooves of welding joints synoptic diagram (20mm);
Fig. 2. welding joint hardness test point synoptic diagram.
Embodiment
Embodiment 1
The water power of present embodiment is with big thickness easy-weld hardening high-strength steel plate, and thickness is 230mm, is made up of following components in weight percentage: C:0.16%, Si:0.27%; Mn:0.91%, P:0.009%, S:0.001%, Al:0.043%; Nb:0.026%, V:0.061%, Ni:1.58%, Cr:0.34%; Ti:0.021%, Mo:0.25%, B:0.0013%, surplus is iron and unavoidable impurities.
The water power of present embodiment is following with the step that can weld the large thickness quenched high strength steel working method:
(1) smelts: will contain following weight percent C:0.16%, Si:0.27%, Mn:0.91%, P:0.009%; S:0.001%, Al:0.043%, Nb:0.026%, V:0.061%; Ni:1.58%, Cr:0.34%, Ti:0.021%, Mo:0.25%; The molten steel of B:0.0013% component is sent into the refining of LF refining furnace earlier through electrosmelting, when liquid steel temperature meets or exceeds 1640 ℃, changes the vacuum outgas of VD stove over to and handles, and adds Fe-Ca line 450m before the VD and changes inclusion morphology; The vacuum tightness 66.6Pa of VD stove, vacuum hold-time 25min guarantees effective eliminating of inclusion, gas, guarantees the pure of molten steel;
(2) die casting: adopt Large Flat ingot mold (minimum thickness 780mm) to pour into a mould, teeming temperature is 1550 ℃, and adopts the protection of inert gas cast;
(3) heating: 1240 ℃ of maximum heating temperatures, 1200 ℃ of soaking temperatures, total 29 hours heat-up times, soaking time 6h;
(4) rolling: adopt high temperature recrystallize technology controlling and process rolling technology, 1020 ℃ of start rolling temperatures, low speed heavy reduction rolling, single pass draught are 18%, 950 ℃ of finishing temperatures, the accumulative total draft is 75%;
(5) roll the back water-cooled: steel plate rolls fast water-cooled to 785 ℃ of back;
(6) thermal reactor buttress: timely wind sheltering stacking after the water-cooled, 650 ℃ of stacking temperature, stacking time 72h obtains the steel plate bullion;
(7) thermal treatment:
Intercritical hardening: the steel plate bullion is carried out heat tracing at 780 ℃ handle, go into the quenching bath water medium then fast and quench, water temperature is 13 ℃ before the steel plate entry, and water temperature is 23 ℃ after the water outlet, and the steel plate entry time is controlled at 70min;
Tempering: tempering temperature is at 680 ℃, and soaking time 3.5min/mm obtains the finished product steel plate.
The mechanical property of the steel plate of this instance: ys 493MPa, tensile strength: 626MPa, 0 ℃ of impact of collision merit KV
2Average 100J, 0 ℃ of transverse impact merit KV
2Average 85J, Z is average 45% to performance.
Embodiment 2
The water power of present embodiment is with big thickness easy-weld hardening high-strength steel plate, and thickness is 200mm, is made up of following components in weight percentage: C:0.17%, Si:0.30%; Mn:0.95%, P:0.010%, S:0.002%, Al:0.030%; Nb:0.022%, V:0.055%, Ni:1.60%, Cr:0.30%; Ti:0.018%, Mo:0.27%, B:0.0015%, surplus is iron and unavoidable impurities.
The water power of present embodiment is following with the step that can weld the large thickness quenched high strength steel working method:
(1) smelts: will contain following weight percent C:0.17%, Si:0.30%, Mn:0.95%, P:0.010%; S:0.002%, Al:0.030%, Nb:0.022%; V:0.055%, Ni:1.60%, Cr:0.30%; Ti:0.018%, Mo:0.27%, the molten steel of B:0.0015% component is earlier through electrosmelting; Send into the refining of LF refining furnace, when liquid steel temperature meets or exceeds 1640 ℃, change the vacuum outgas of VD stove over to and handle, add CaSi >=120kg/ stove before the VD and change inclusion morphology; The vacuum tightness 66.6Pa of VD stove, vacuum hold-time 25min guarantees effective eliminating of inclusion, gas, guarantees the pure of molten steel;
(2) die casting: adopt Large Flat ingot mold (minimum thickness 780mm) to pour into a mould, teeming temperature is 1548 ℃, and adopts the protection of inert gas cast;
(3) heating: 1240 ℃ of maximum heating temperatures, 1180 ℃ of soaking temperatures, total 27 hours heat-up times, soaking time 6h;
(4) rolling: adopt high temperature recrystallize technology controlling and process rolling technology, 1050 ℃ of start rolling temperatures, low speed heavy reduction rolling, single pass draught are 20%, 945 ℃ of finishing temperatures, the accumulative total draft is 77%;
(5) roll the back water-cooled: steel plate rolls fast water-cooled to 790 ℃ of back;
(6) thermal reactor buttress: timely wind sheltering stacking after the water-cooled, 660 ℃ of stacking temperature, stacking time 72h obtains the steel plate bullion;
(7) thermal treatment:
Intercritical hardening: the steel plate bullion is carried out heat tracing at 780 ℃ handle, go into the quenching bath water medium then fast and quench, water temperature is 18 ℃ before the steel plate entry, and water temperature is 27 ℃ after the water outlet, and the steel plate entry time is controlled at 65min;
Tempering: tempering temperature is at 680 ℃, and soaking time 3.5min/mm obtains the finished product steel plate.
The mechanical property of the steel plate of this instance: ys 475MPa, tensile strength: 605MPa, 0 ℃ of impact of collision merit KV
2Average 95J, 0 ℃ of transverse impact merit KV
2Average 80J, Z is average 43.5% to performance.
Embodiment 3
The water power of present embodiment is with big thickness easy-weld hardening high-strength steel plate, and thickness is 220mm, is made up of following components in weight percentage: C:0.17%, Si:0.29%; Mn:0.95%, P:0.009%, S:0.001%, Al:0.025%; Nb:0.020%, V:0.063%, Ni:1.60%, Cr:0.30%; Ti:0.020%, Mo:0.28%, B:0.0015%, surplus is iron and unavoidable impurities.
The water power of present embodiment is following with the step that can weld the large thickness quenched high strength steel working method:
(1) smelts: will contain following weight percent C:0.17%, Si:0.29%, Mn:0.95%, P:0.009%; S:0.001%, Al:0.025%, Nb:0.020%; V:0.063%, Ni:1.60%, Cr:0.30%; Ti:0.020%, Mo:0.28%, the molten steel of B:0.0015% component is earlier through electrosmelting; Send into the refining of LF refining furnace, when liquid steel temperature meets or exceeds 1650 ℃, change the vacuum outgas of VD stove over to and handle, add CaSi piece >=120kg/ stove before the VD and change inclusion morphology; The vacuum tightness 66.6Pa of VD stove, vacuum hold-time 25min guarantees effective eliminating of inclusion, gas, guarantees the pure of molten steel;
(2) die casting: adopt Large Flat ingot mold (minimum thickness 780mm) to pour into a mould, teeming temperature is 1548 ℃, and adopts the protection of inert gas cast;
(3) heating: 1235 ℃ of maximum heating temperatures, 1200 ℃ of soaking temperatures, total 27 hours heat-up times, soaking time 6h;
(4) rolling: adopt high temperature recrystallize technology controlling and process rolling technology, 1045 ℃ of start rolling temperatures, low speed heavy reduction rolling, single pass draught are 17%, 930 ℃ of finishing temperatures, the accumulative total draft is 75%;
(5) roll the back water-cooled: steel plate rolls fast water-cooled to 780 ℃ of back;
(6) thermal reactor buttress: timely wind sheltering stacking after the water-cooled, 650 ℃ of stacking temperature, stacking time 72h obtains the steel plate bullion;
(7) thermal treatment:
Intercritical hardening: the steel plate bullion is carried out heat tracing at 780 ℃ handle, go into the quenching bath water medium then fast and quench, water temperature is 15 ℃ before the steel plate entry, and water temperature is 26 ℃ after the water outlet, and the steel plate entry time is controlled at 68min;
Tempering: tempering temperature is at 680 ℃, and soaking time 3.5min/mm obtains the finished product steel plate.
The mechanical property of the steel plate of this instance: ys 480MPa, tensile strength: 615MPa, 0 ℃ of impact of collision merit KV
2Average 96J, 0 ℃ of transverse impact merit KV
2Average 82J, Z is average 41.5% to performance.
Welding performance test:
This is tested used steel plate and is the steel plate described in the embodiment 1.
1. tiltedly Y type groove welding cold cracking test
Because test steel plate thickness is big, so sample is thinned to 50mm when making an experiment.
1.1 welding condition (seeing table 1)
Table 1 cracking test welding condition
| Welding process | Welding material | Specification | Welding current | Weldingvoltage | Welding speed |
| SMAW | J607RH | Φ4.0mm | 170±10A | 24± |
150±10mm/min |
1.2 test-results (seeing table 2)
Table 2 cracking test result
2 welding joint technological property tests
2.1 grooves of welding joints form (see figure 1)
2.2 welding condition (seeing table 3,120 ℃ of preheatings, 20 ℃ of envrionment temperatures)
Table 3 welding condition
The postwelding test plate (panel) is not found welding flaws such as crackle through defect detecting test.
2.3 welding joint mechanical property test-results
By the requirement of JB4708-2000 " steel pressure vessel welding technology evaluation ", welding joint is carried out the relevant mechanical properties check, the result sees table 4.
The mechanical property of table 4 welding joint
2.4 welding joint hardness test result
Welding joint hardness test point position is as shown in Figure 2, and test-results is seen table 5.
Table 5 welding joint hardness test result (HV10)
Claims (5)
1. a water power is characterized in that with big thickness easy-weld hardening high-strength steel plate, is made up of the chemical ingredients of following weight percentage: C:0.15% ~ 0.18%, Si:0.15% ~ 0.35%; Mn:0.90% ~ 1.00%, P≤0.012%, S≤0.005%; Ni:1.52% ~ 1.60%, Cr:0.30% ~ 0.40%, Nb:0.020% ~ 0.030%; Al:0.020% ~ 0.050%, Mo:0.20% ~ 0.30%, V:0.055% ~ 0.065%; B:0.0007% ~ 0.0015%, Ti:0.015% ~ 0.025%, surplus is Fe and unavoidable impurities.
2. water power according to claim 1 uses the maximum ga(u)ge of big thickness easy-weld hardening high-strength steel plate to be 230mm.
3. a water power as claimed in claim 1 is characterized in that with the working method of big thickness easy-weld hardening high-strength steel plate, comprises the steps:
(1) smelts: will contain following weight percent C:0.15% ~ 0.18%, Si:0.15% ~ 0.35%, Mn:0.90% ~ 1.00%, P≤0.012%; S≤0.005%, Ni:1.52% ~ 1.60%, Cr:0.30% ~ 0.40%; Nb:0.020% ~ 0.030%, Al:0.020% ~ 0.050%, Mo:0.20% ~ 0.30%; V:0.055% ~ 0.065%, B:0.0007% ~ 0.0015%, the molten steel of Ti:0.015% ~ 0.025% component is earlier through electrosmelting; Send into the refining of LF refining furnace, when liquid steel temperature meets or exceeds 1640 ± 10 ℃, change the vacuum outgas of VD stove over to and handle, add CaSi piece>=100kg/ stove or Fe-Ca line 400 ~ 450m before the VD;
(2) die casting: adopt the Large Flat ingot mold to pour into a mould, and adopt the protection of inert gas cast;
(3) heating: maximum heating temperature is 1240 ℃, and soaking temperature is 1180 ~ 1200 ℃, and be 24 ~ 30h total heat-up time, soaking time >=5h;
(4) rolling: adopt high temperature recrystallize technology controlling and process rolling technology, start rolling temperature is 1000 ~ 1050 ℃, and low speed heavy reduction rolling, single pass draught are 10 ~ 20%, and finishing temperature is 940 ± 20 ℃, and the accumulative total draft is 70 ~ 80%;
(5) roll the back water-cooled: quick water-cooled to 780 after steel plate rolls ~ 810 ℃;
(6) thermal reactor buttress: timely wind sheltering stacking after the water-cooled, the stacking temperature is 650 ~ 680 ℃, the stacking time is 72h, obtains the steel plate bullion;
(7) thermal treatment:
Intercritical hardening: the steel plate bullion is carried out heat tracing at 760 ℃～800 ℃ handle; Put into quenching bath water medium quenching then fast; Water temperature is not higher than 25 ℃ before the steel plate entry, and water temperature is not higher than 30 ℃ after the water outlet, and the steel plate entry time is controlled between 60 ~ 70min;
Tempering: tempering temperature is between 660 ~ 680 ℃, and soaking time obtains the finished product steel plate at 3.5 ~ 4.0min/mm.
4. water power according to claim 3 is characterized in that with the working method of big thickness easy-weld hardening high-strength steel plate, vacuum tightness≤66.6Pa that the described vacuum outgas of step (1) is handled, vacuum hold-time>=25min.
5. water power according to claim 3 is characterized in that with the working method of big thickness easy-weld hardening high-strength steel plate the described teeming temperature of step (2) is 1545 ~ 1555 ℃, and the minimum thickness of ingot slab mould is 780mm.
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| CN103451562A (en) * | 2013-08-29 | 2013-12-18 | 舞阳钢铁有限责任公司 | Quenched large-thickness easy-to-weld Z-direction high-strength steel plate for water and electricity and production method thereof |
| CN105886909A (en) * | 2016-04-19 | 2016-08-24 | 江阴兴澄特种钢铁有限公司 | Pressure container steel plate resistant to hydrogen induced cracking and manufacturing method thereof |
| CN107177714A (en) * | 2017-07-24 | 2017-09-19 | 攀钢集团江油长城特殊钢有限公司 | Plastic mould generous band steel and preparation method thereof |
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