CN101274852B - Method for preparing MgALON-based compound material by using boron-rich slag - Google Patents
Method for preparing MgALON-based compound material by using boron-rich slag Download PDFInfo
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- CN101274852B CN101274852B CN2008100115160A CN200810011516A CN101274852B CN 101274852 B CN101274852 B CN 101274852B CN 2008100115160 A CN2008100115160 A CN 2008100115160A CN 200810011516 A CN200810011516 A CN 200810011516A CN 101274852 B CN101274852 B CN 101274852B
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Abstract
The invention provides a method for preparing an MgAlON base composite material by making use of boron-rich slag, which is characterized in that: in the first step, boron-rich slag containing 30 to 40 percent of MgO is taken as main material; the massive boron-rich slag is processed into boron-rich slag powder which is then fine-ground and sieved; the sieved boron-rich slag powder is mixed with an aluminum contained compound and carbon black and made into mixed blank which is then pressed to obtain round blank; the round blank is sintered to obtain MgAlON composite powder; in the second step, the prepared MgAlON composite powder is mixed with an additive and then pressed to obtain round blank which is then sintered to obtain the MgAlON base composite material. The preparation method of MgAlON base composite material of the invention is characterized in that: metallurgical slag is utilized as raw material to prepare the MgAlON base composite material, which reduces the production cost thereof; the synthesized MgAlON base composite material has various excellent performances and can be wildly applied in such fields as metallurgy and ceramics, etc. The preparation method of the invention has simple technique, low production cost and vital significance in comprehensive utilization of the boron-rich slag.
Description
Technical field
The invention belongs to materials science field, particularly a kind ofly utilize rich boron slag to prepare the method for MgAlON based composites.
Background technology
MgAlON (magnesium A Long) can regard MgO or MgAl as
2O
4Solid solution enters the solid solution that γ-AlON lattice forms, and has spinel structure, belongs to cubic system.The MgAlON material has the performance of a lot of excellences, and research in recent years all is proven in theoretical and production application, adopts MgAlON might become a kind of novel high-performance refractory material as the composite refractory in conjunction with mutually development.MgAlON is a kind of typical oxymtride material, and it has poor wettability to molten iron, even the slag of the high basicity of slag, high FeO content is had good resistance to fouling, lower thermal expansivity has good thermal shock resistance.
The method of at present synthetic MgAlON mainly contains three kinds: thermit reduction, reaction sintering and discharge plasma sintering method.Thermit reduction is passed through Al
2O
3, Al and MgO or MgAl
2O
4Directly synthesize MgAlON in nitrogen, solid-solid reaction mechanism is introduced in this reaction, but the cost height, complex process, energy consumption is big, is difficult for industrial-scale production; Reaction sintering passes through Al
2O
3, at high temperature directly reaction was synthetic after AlN and MgO powder mixed, and this method synthesis temperature height needs the time long, the cost of manufacture height, the AlN in the raw material is expensive; The discharge plasma sintering method can make solid solution reaction carry out rapidly, Reaction time shorten, but preparing needed raw material cost height, complex process is because the restriction of equipment is difficult to suitability for industrialized production.
More than three kinds of methods to adopt with the pure reagent be the synthetic method of raw material, the cost of manufacture height; Rich boron slag is as a kind of waste residue in the metallurgy industry, poor activity, boron in the slag is not easily separated, utilizes that lixiviation process exists processing cost height, deficiency in economic performance, treatment capacity is limited, added value of product is low and secondary is discarded and problem such as pollution, is difficult to realize the industrial applications scale.
Summary of the invention
At the deficiencies in the prior art, the invention provides and a kind ofly utilize rich boron slag to prepare the method for MgAlON based composites.It is that 30～40% rich boron slag is a main raw material that the first step adopts MgO content, earlier the rich boron slag of bulk is made rich boron ground-slag, then with the fine grinding of rich boron ground-slag, screening; Rich boron ground-slag after the screening is mixed with aluminum contained compound and carbon black, be prepared into the mixing blank; To mix blank then and be pressed into round base, be prepared into the MgAlON composite granule through oversintering; Second step mixed the MgAlON composite granule for preparing with additive, be pressed into round base, was prepared into the MgAlON based composites through oversintering.
Technical scheme of the present invention is:
1, the preparation of MgAlON composite granule:
With the fragmentation of the boron-rich slag physics of bulk, make then Powderedly with the slag of sampling machine after with fragmentation, obtain boron-rich ground-slag; With ball mill above-mentioned boron-rich ground-slag is carried out fine grinding, even with raw material in order to guarantee experiment until raw material reaches below the 74 μ m, sieve with 200 mesh standard sieves.
Rich boron ground-slag after the screening, aluminum contained compound and carbon black are mixed, and the mixing quality percentage is: rich boron slag 10～30%, aluminum contained compound 40～60%, carbon black 10～35%; The material that mixes places the urethane ball grinder, is medium ball milling wet mixing 24h with dehydrated alcohol, guarantees to mix, and the add-on of dehydrated alcohol is as the criterion with submergence urethane ball and mixture; After the wet mixing that slip is air-dry under 60 ℃, do again after the material drying to be mixed and mix 4h, last, compound is put into loft drier dry 3h under 110 ℃, remove moisture residual in the compound and dehydrated alcohol, obtain mixing blank.
To mix blank and put into punching block, single shaft is to being pressed into round base; With pack into plumbago crucible and place sintering oven (MoSi of the mixing blank that suppresses
2Resistance furnace) place, zone of constant temperature, sintering temperature is 1400～1500 ℃; Constant temperature time 4～10h; All the time feed high pure nitrogen in the sintering process in the stove to prevent sample generation oxidation and thermolysis; Cool to room temperature after the insulation with the furnace.
Be below the 74 μ m with improved grinding to mean particle size after sintering is finished, place then in the retort furnace that constant temperature 4h heat-treats in 700 ℃ of air, is cooled to room temperature subsequently, remove remaining carbon black, be prepared into the MgAlON composite granule.
2, the preparation of MgAlON based composites:
With synthetic MgAlON composite granule and additive Y
2O
3Fully mix additive Y
2O
3Consumption be 0.5～1% of raw material total amount; Mixed material is put into punching block, and single shaft is to being pressed into round base; Should justify then base and put into black-fead crucible, place sintering furnace (MoSi
2Resistance furnace) place, zone of constant temperature, in sintering furnace, pass into high pure nitrogen to prevent sample generation oxidation and thermal decomposition, speed with 15～20 ℃/min is warming up to sintering temperature, sintering temperature is 1500～1550 ℃, constant temperature 2～2.5 hours, speed with 10～15 ℃/min is cooled to room temperature then, obtains material and is the MgAlON based composites.
The XRD testing result shows that main phase is MgAlON, O '-Sialon, BN and CaAl in the synthetic MgAlON composite granule
4O
7Main phase in the synthetic MgAlON based composites is that MgAlON, O '-Sialon and BN also have a small amount of Al in addition
5Y
3O
12And CaYAl
3O
7
The present invention carries out the integral body recycling in conjunction with the thought of valuable resource comprehensive utilization in grandidierite and the complex ore slag to boron-rich slag, obtains high value-added product to be desirably on the basis of reducing secondary pollution; Utilize the characteristics on boron-rich slag self chemical composition, adopt special process method that it is not utilized this slag with integrally having new discarded and pollution and increment.
It is boron-rich slag primary raw material that the present invention adopts metallurgical slag, adds aluminum contained compound, adopts the standby MgAlON based composites of carbothermal reduction-nitridation legal system, and institute obtains that BN and O '-Sialon have obvious antioxidation for this material in the material; The method of utilizing boron-rich slag to prepare the MgAlON based composites of the present invention has reduced the production cost of material, effectively utilizes the solid waste in the metallurgy industry, and does not produce new discarded object and pollution, is conducive to curb environmental pollution.The present invention is not only simple for process, and equipment requirements is low, and the reaction times is short, is fit to large-scale industrialization production.
Embodiment
The invention process adopts the oil company, Fushun to produce carbon black as reductive agent, and the carbon black fineness is 30～40nm, and the mass percentage content of carbon is 96.70%; The high pure nitrogen purity that adopts is greater than 99.999%.
The sintering oven that the invention process adopts is MoSi
2Resistance furnace, boiler tube are alundum tube, specification Φ 80 * 70 * 1000mm.
The temperature control that the invention process adopts and temperature measuring equipment are XMTA-1 type digital readout temperature controller and the PtRh6-PtRh30 thermocouple through calibrating.
The mass percent of the rich boron slag main component that the invention process adopts sees Table 1.
The main component of the boron-rich slag of table 1 experiment
| Composition | B 2O 3 | SiO 2 | MgO | Al 2O 3 | CaO | TFe | P 2O 5 | S |
| Content/% | 12.01 | 28.03 | 34.55 | 7.30 | 15.03 | 1.18 | 0.02 | 0.60 |
Embodiment 1:
With the fragmentation of the boron-rich slag physics of bulk, make then Powderedly with the slag of MZ-100 vibrating mill after with fragmentation, obtain boron-rich ground-slag; With ball mill with the speed of 120r/min with above-mentioned boron-rich ground-slag ball milling 72h, until raw material reaches below the 74 μ m, sieve with 200 mesh standard sieves then.
Rich boron ground-slag after the screening, aluminum contained compound and carbon black are mixed wherein rich boron slag 30g, Al (OH)
360g, carbon black 10g; The material that mixes places the urethane ball grinder, is the speed ball milling wet mixing 24h of medium with 120r/min with dehydrated alcohol, guarantees to mix; Use 101-1 type electric drying oven with forced convection air-dry under 60 ℃ slip after the wet mixing, do again after the material drying to be mixed and mix 4h, last, compound is put into loft drier dry 3h under 110 ℃, remove moisture residual in the compound and dehydrated alcohol and obtain mixing blank.
To mix blank and put into punching block, place an order at 250MPa pressure with 769YP-15A type powder compressing machine that axially to be pressed into diameter be roundlet base about 15mm, pressurize 5min; With pack into plumbago crucible and place MoSi of the mixing blank that suppresses
2Place, the zone of constant temperature of resistance furnace feeds under the condition of nitrogen 400mL/min in reaction system continuously, adopts normal pressure-sintered method, carries out temperature control with XMTA-1 type digital display temperature controller, 1450 ℃ of sintering temperatures, constant temperature precision ± 1 ℃, constant temperature 4h; Cool to room temperature after the insulation with the furnace.
Be below the 74 μ m with improved grinding to mean particle size after sintering is finished, place then in the retort furnace that constant temperature 4h heat-treats in 700 ℃ of air, is cooled to room temperature subsequently, remove remaining carbon black, obtain the MgAlON composite granule.
With the MgAlON composite granule that obtains and 0.5% the additive Y that accounts for powder quality
2O
3Fully mix, again material is put into punching block, with the 769YP-15A type powder compressing machine unidirectional roundlet base that diameter is 15mm, pressurize 5min of being pressed under 250MPa pressure; The roundlet base of compacting is packed in the graphite crucible, then crucible is placed MoSi with crucible tongs
2The place, zone of constant temperature of resistance furnace is at MoSi
2Pass into high pure nitrogen in the resistance furnace, nitrogen flow is 50mL/min, is warming up to sintering temperature with the speed of 20 ℃/min, sintering temperature is 1500 ℃, constant temperature precision ± 1 ℃, constant temperature 2h, speed with 15 ℃/min is cooled to room temperature then, obtains material and is the MgAlON based composites.
This MgAlON composite volume density is 2.13g/cm
3, dimension formula hardness 13GPa, normal temperature compression strength is 462Mpa, material begins the oxidation weight gain temperature in air be 988 ℃.
Embodiment 2:
The preparation of boron-rich ground-slag and fine grinding and screening are with embodiment 1.
Rich boron ground-slag after the screening, aluminum contained compound and carbon black are mixed wherein rich boron slag 30g, Al (OH)
340g, carbon black 30g; The material that mixes places the urethane ball grinder, is the speed ball milling wet mixing 24h of medium with 120r/min with dehydrated alcohol, guarantees to mix; Use 101-1 type electric drying oven with forced convection air-dry under 60 ℃ slip after the wet mixing, do again after the material drying to be mixed and mix 4h, last, compound is put into loft drier dry 3h under 110 ℃, remove moisture residual in the compound and dehydrated alcohol and obtain mixing blank.
To mix blank and put into punching block, place an order at 250MPa pressure with 769YP-15A type powder compressing machine that axially to be pressed into diameter be roundlet base about 15mm, pressurize 5min; With pack into plumbago crucible and place MoSi of the mixing blank that suppresses
2Place, the zone of constant temperature of resistance furnace feeds under the condition of nitrogen 800mL/min in reaction system continuously, adopts normal pressure-sintered method, carries out temperature control with XMTA-1 type digital display temperature controller, 1500 ℃ of sintering temperatures, constant temperature precision ± 1 ℃, constant temperature 6h; Cool to room temperature after the insulation with the furnace.
Be below the 74 μ m with improved grinding to mean particle size after sintering is finished, place then in the retort furnace that constant temperature 4h heat-treats in 700 ℃ of air, is cooled to room temperature subsequently, remove remaining carbon black, obtain the MgAlON composite granule.
With the MgAlON composite granule that obtains and 1% the additive Y that accounts for powder quality
2O
3Fully mix, again material is put into punching block, with the 769YP-15A type powder compressing machine unidirectional roundlet base that diameter is 15mm, pressurize 5min of being pressed under 250MPa pressure; The roundlet base of compacting is packed in the graphite crucible, then crucible is placed MoSi with crucible tongs
2The place, zone of constant temperature of resistance furnace is at MoSi
2Pass into high pure nitrogen in the resistance furnace, nitrogen flow is 70mL/min, is warming up to sintering temperature with the speed of 15 ℃/min, sintering temperature is 1510 ℃, constant temperature precision ± 1 ℃, constant temperature 2.5h, speed with 10 ℃/min is cooled to room temperature then, obtains material and is the MgAlON based composites.
The bulk density of this MgAlON composite is 2.82g/cm
3, dimension formula hardness 17GPa, normal temperature compression strength is 493MPa, material begins oxidizing temperature in air be 998 ℃.
Embodiment 3:
The preparation of boron-rich ground-slag and fine grinding and screening are with embodiment 1.
Boron-rich ground-slag, aluminum contained compound after the screening and carbon black are mixed boron-rich slag 30g wherein, Al
2O
350g, carbon black 20g; The material that mixes places polyurethane ball-milling pot, with absolute ethyl alcohol be medium with the speed wet ball-milling 24h of 120r/min, guarantee to mix; After the wet mixing that slip is air-dry under 60 ℃ with 101-1 type electric drying oven with forced convection, do again mixed 4h after the material drying to be mixed, last, compound is put into drying box in 110 ℃ of lower dry 3h, remove moisture residual in the compound and absolute ethyl alcohol and obtain mixing blank.
To mix blank and put into punching block, place an order at 250MPa pressure with 769YP-15A type powder compressing machine that axially to be pressed into diameter be roundlet base about 15mm, pressurize 5min; With pack into plumbago crucible and place MoSi of the mixing blank that suppresses
2Place, the zone of constant temperature of resistance furnace feeds under the condition of nitrogen 600mL/min in reaction system continuously, adopts normal pressure-sintered method, carries out temperature control with XMTA-1 type digital display temperature controller, 1400 ℃ of sintering temperatures, constant temperature precision ± 1 ℃, constant temperature 8h; Cool to room temperature after the insulation with the furnace.
Be below the 74 μ m with improved grinding to mean particle size after sintering is finished, place then in the retort furnace that constant temperature 4h heat-treats in 700 ℃ of air, is cooled to room temperature subsequently, remove remaining carbon black, obtain the MgAlON composite granule.
With the MgAlON composite granule that obtains and 1% the additive Y that accounts for powder quality
2O
3Fully mix, again material is put into punching block, with the 769YP-15A type powder compressing machine unidirectional roundlet base that diameter is 15mm, pressurize 5min of being pressed under 250MPa pressure; The roundlet base of compacting is packed in the graphite crucible, then crucible is placed MoSi with crucible tongs
2The place, zone of constant temperature of resistance furnace is at MoSi
2Pass into high pure nitrogen in the resistance furnace, nitrogen flow is 60mL/min, is warming up to sintering temperature with the speed of 20 ℃/min, sintering temperature is 1520 ℃, constant temperature precision ± 1 ℃, constant temperature 2.5h, speed with 15 ℃/min is cooled to room temperature then, obtains material and is the MgAlON based composites.
The bulk density of this MgAlON composite is 2.73g/cm
3, dimension formula hardness 15GPa, normal temperature compression strength is 475MPa, material begins oxidizing temperature in air be 998 ℃.
Embodiment 4:
The preparation of boron-rich ground-slag and fine grinding and screening are with embodiment 1.
Boron-rich ground-slag, aluminum contained compound after the screening and carbon black are mixed boron-rich slag 10g wherein, Al
2O
360g, carbon black 30g; The material that mixes places polyurethane ball-milling pot, with absolute ethyl alcohol be medium with the speed wet ball-milling 24h of 120r/min, guarantee to mix; After the wet mixing that slip is air-dry under 60 ℃ with 101-1 type electric drying oven with forced convection, do again mixed 4h after the material drying to be mixed, last, compound is put into drying box in 110 ℃ of lower dry 3h, remove moisture residual in the compound and absolute ethyl alcohol and obtain mixing blank.
To mix blank and put into punching block, place an order at 250MPa pressure with 769YP-15A type powder compressing machine that axially to be pressed into diameter be roundlet base about 15mm, pressurize 5min; With pack into plumbago crucible and place MoSi of the mixing blank that suppresses
2Place, the zone of constant temperature of resistance furnace feeds under the condition of nitrogen 700mL/min in reaction system continuously, adopts normal pressure-sintered method, carries out temperature control with XMTA-1 type digital display temperature controller, 1450 ℃ of sintering temperatures, constant temperature precision ± 1 ℃, constant temperature 9h; Cool to room temperature after the insulation with the furnace.
Be below the 74 μ m with improved grinding to mean particle size after sintering is finished, place then in the retort furnace that constant temperature 4h heat-treats in 700 ℃ of air, is cooled to room temperature subsequently, remove remaining carbon black, obtain the MgAlON composite granule.
With the MgAlON composite granule that obtains and 0.5% the additive Y that accounts for powder quality
2O
3Fully mix, again material is put into punching block, with the 769YP-15A type powder compressing machine unidirectional roundlet base that diameter is 15mm, pressurize 5min of being pressed under 250MPa pressure; The roundlet base of compacting is packed in the graphite crucible, then crucible is placed MoSi with crucible tongs
2The place, zone of constant temperature of resistance furnace is at MoSi
2Pass into high pure nitrogen in the resistance furnace, nitrogen flow is 70mL/min, is warming up to sintering temperature with the speed of 20 ℃/min, sintering temperature is 1540 ℃, constant temperature precision ± 1 ℃, constant temperature 2h, speed with 10 ℃/min is cooled to room temperature then, obtains material and is the MgAlON based composites.
The volume density 2.56g/cm of this MgAlON matrix material
3, dimension formula hardness 16GPa, normal temperature ultimate compression strength is 447Mpa, material begins oxidizing temperature in air be 979 ℃.
Embodiment 5:
The preparation of boron-rich ground-slag and fine grinding and screening are with embodiment 1.
Rich boron ground-slag after the screening, aluminum contained compound and carbon black are mixed wherein rich boron slag 20g, Al (OH)
345g, carbon black 35g; The material that mixes places the urethane ball grinder, is the speed ball milling wet mixing 24h of medium with 120r/min with dehydrated alcohol, guarantees to mix; Use 101-1 type electric drying oven with forced convection air-dry under 60 ℃ slip after the wet mixing, do again after the material drying to be mixed and mix 4h, last, compound is put into loft drier dry 3h under 110 ℃, remove moisture residual in the compound and dehydrated alcohol and obtain mixing blank.
To mix blank and put into punching block, place an order at 250MPa pressure with 769YP-15A type powder compressing machine that axially to be pressed into diameter be roundlet base about 15mm, pressurize 5min; With pack into plumbago crucible and place MoSi of the mixing blank that suppresses
2Place, the zone of constant temperature of resistance furnace feeds under the condition of nitrogen 500mL/min in reaction system continuously, adopts normal pressure-sintered method, carries out temperature control with XMTA-1 type digital display temperature controller, 1500 ℃ of sintering temperatures, constant temperature precision ± 1 ℃, constant temperature 10h; Cool to room temperature after the insulation with the furnace.
Be below the 74 μ m with improved grinding to mean particle size after sintering is finished, place then in the retort furnace that constant temperature 4h heat-treats in 700 ℃ of air, is cooled to room temperature subsequently, remove remaining carbon black, obtain the MgAlON composite granule.
With the MgAlON composite granule that obtains and 1% the additive Y that accounts for powder quality
2O
3Mix, again blank is put into punching block, with the 769YP-15A type powder compressing machine unidirectional roundlet base that diameter is 15mm, pressurize 5min of being pressed under 250MPa pressure; The roundlet base of compacting is packed in the graphite crucible, then crucible is placed MoSi with crucible tongs
2The place, zone of constant temperature of resistance furnace is at MoSi
2Pass into high pure nitrogen in the resistance furnace, nitrogen flow is 50mL/min, is warming up to sintering temperature with the speed of 15 ℃/min, sintering temperature is 1550 ℃, constant temperature precision ± 1 ℃, constant temperature 2.5h, speed with 15 ℃/min is cooled to room temperature then, obtains material and is the MgAlON based composites.
The bulk density of this MgAlON composite is 2.26g/cm
3, dimension formula hardness 15GPa, normal temperature compression strength is 463Mpa, material begins oxidizing temperature in air be 985 ℃.
Claims (2)
1. method of utilizing boron-rich slag to prepare the MgAlON based composites is characterized in that: the first step adopts and contains MgO30～40%, SiO
220～30%, B
2O
310～15% boron-rich slag is primary raw material, earlier the boron-rich slag of bulk is made boron-rich ground-slag, with ball mill boron-rich ground-slag is carried out fine grinding, until fineness is below the 74 μ m, sieves with 200 mesh standard sieves then; Boron-rich ground-slag after the screening is mixed with aluminum contained compound and carbon black, be prepared into the mixing blank; To mix then blank and be pressed into round base, be prepared into the MgAlON composite granule through oversintering; Second step mixes the MgAlON composite granule for preparing with additive, be pressed into round base, is prepared into the MgAlON based composites through oversintering; The preparation method of described mixing blank mixes the boron-rich ground-slag after the screening with aluminum contained compound and carbon black, mixed proportion is: boron-rich slag 20～30%, aluminum contained compound 40～60%, carbon black 10～35%; Then the material that mixes is placed polyurethane ball-milling pot, take absolute ethyl alcohol as medium wet mixing 24h, guarantee to mix; After the wet mixing that slip is air-dry under 60 ℃, place again polyurethane ball-milling pot to do mixed 4h after the material drying to be mixed, last, mixed material is put into drying box in 110 ℃ of lower dry 3h, remove moisture residual in the compound and absolute ethyl alcohol and obtain mixing blank; The preparation method of described MgAlON composite granule puts into punching block with the mixing blank, and single shaft is to being pressed into round base; With the round base that the suppresses black-fead crucible of packing into, insert the sintering furnace zone of constant temperature, sintering temperature is 1400～1500 ℃, constant temperature time 4～10h; All the time pass into nitrogen in the sintering process in the stove and prevent sample generation oxidation and thermal decomposition; Cool to room temperature after the insulation with the furnace; After sintering is finished material ground to form the powder below the 75 μ m, place then in the Muffle furnace, constant temperature 4h heat-treats in 700 ℃ of air, is cooled to subsequently room temperature, obtains the MgAlON composite granule; The preparation method of described MgAlON based composites is with synthetic MgAlON composite granule and the additive Y that accounts for oeverall quality 0.5～1%
2O
3Fully mix, single shaft is to being pressed into round base, briquetting pressure 250MPa, pressurize 5min; Put into then graphite crucible and carry out high temperature sintering, speed with 15～20 ℃/min is warming up to firing temperature, sintering temperature is 1500～1550 ℃, passes into all the time high pure nitrogen in the sintering process to prevent sample generation oxidation and thermal decomposition, temperature retention time 2～2.5 hours; Speed with 10～15 ℃/min is cooled to room temperature, obtains the MgAlON based composites.
2. the method for utilizing boron-rich slag to prepare the MgAlON based composites according to claim 1, it is characterized in that described aluminum contained compound: aluminum contained compound is that purity is not less than 98% Al (OH)
3Or Al
2O
3
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|---|---|---|---|
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| CN102825649B (en) * | 2012-07-18 | 2014-08-13 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic bisque by gel casting and molding |
| CN112225564B (en) * | 2019-07-15 | 2022-01-04 | 中国科学院上海硅酸盐研究所 | Aluminum oxynitride transparent ceramic and preparation method thereof |
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