CN102815958A - Preparation method of ceramizable resin matrix composite material - Google Patents
Preparation method of ceramizable resin matrix composite material Download PDFInfo
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- CN102815958A CN102815958A CN2012103091145A CN201210309114A CN102815958A CN 102815958 A CN102815958 A CN 102815958A CN 2012103091145 A CN2012103091145 A CN 2012103091145A CN 201210309114 A CN201210309114 A CN 201210309114A CN 102815958 A CN102815958 A CN 102815958A
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Abstract
Belonging to the technical field of composite materials, the invention discloses a preparation method of a ceramizable resin matrix composite material. The method includes: selecting an appropriate reinforcing material and ceramizable additive-containing resin, then dipping the reinforcing material into a resin adhesive solution, and when the reinforcing material is evenly dipped, placing the reinforcing material into a die, and conducting heating pressing to mold the composite material. The ceramizable additive within the composite material can have chemical change at a temperature higher than 600DEG C so as to form ceramics, thus greatly improving the ablation resistance of the composite material, reducing the shortcomings of excessive ablation and interlaminar cracking in high temperature resin matrix composite materials, reducing the production cycle and material cost, as well as substantially improving the machining properties of ceramic materials.
Description
Technical field
The invention belongs to technical field of composite materials, particularly a kind of preparation method that can the potteryization polymer matrix composites.
Background technology
Aircraft carries out gliding type maneuvering flight on a large scale in the endoatmosphere; Environment when its Working environment belongs to typical middle temperature, long boat; The large area region temperature is in 600 ℃~1200 ℃ scopes; Common ablative-type protective coating polymer matrix composites ablation amount under this Working environment is excessive, can not satisfy the requirement of aircraft aerodynamic configuration.
Can the potteryization polymer matrix composites be a kind of novel heat insulation materials, it be that in the new type high temperature resin of anti-the ablation, add can potteryization additive, the matrix material for preparing through dipping and the molding mode suppressed.In low thermophase, rely on the ablation resistance solar heat protection of the resin of anti-ablation the self; When envrionment temperature surpass material can potteryization temperature spot after, material carries out the pottery transformation, dependence stupalith self thermotolerance plays the thermal protection effect.But because density that at present can the potteryization polymer matrix composites is 1.6g/cm
3~1.7g/cm
3, thermal conductivity is 0.6W (mK
-1), can't satisfy the demand of preventing heat-insulation integrative; Though ceramic matric composite has high temperature resistant, oxidation resistant characteristics simultaneously, its cost is high, thermal conductivity is high, anti-heat insulation structural complex design, and large-area applications receives certain limitation.
Summary of the invention
The purpose of this invention is to provide a kind of can heat-insulation integrative, and can large-area applications can the potteryization polymer matrix composites the preparation method.
The technical scheme that the present invention adopted is:
A kind of preparation method that can the potteryization polymer matrix composites may further comprise the steps:
(1) silane coupling agent is dissolved with solvent, can the potteryization additive adds in the silane coupler solution, under 60~80 ℃, stir, up to do not have reunite till, filter with dry removing and desolvate, what obtain surface-treated can the potteryization additive;
(2) resin of anti-the ablation is dissolved with solvent; Can joining in the resin solution of anti-the ablation by the potteryization additive of the surface-treated that step (1) is obtained; Both are mixed; Processing can the potteryization resin adhesive liquid, and what do not have reunion in can the potteryization resin adhesive liquid can potteryization additive or other visible impurity;
(3) with step (2) obtain can potteryization resin adhesive liquid lay-up, dry after thorough the strongthener dipping is all even;
(4) strongthener that step (3) dipping is obtained is put in the mould, with the mould matched moulds, is to carry out under 0~80 ℃ in temperature through pressuring method during matched moulds;
(5) according to the curing system of the resin of anti-the ablation, the curing that heats up, said curing system is: be incubated 1h, 1h to 110 ℃ of intensification down at 90 ℃; Be incubated 1h, 1h to 140 ℃ of intensification down at 110 ℃; Be incubated 1h, 1h to 180 ℃ of intensification down at 140 ℃; Be incubated 2h, 1h to 200 ℃ of intensification down at 180 ℃; At 200 ℃ of insulation 1h;
(6) solidify finish after, the demoulding when treating that mould is reduced to room temperature, and the overlap that polishing can the potteryization polymer matrix composites.
Preferably, said strongthener is a fibre integral fabric.
Further, when said strongthener was the staple length yarn, its preparation method was:
(1) silane coupling agent is dissolved with solvent; Can the potteryization additive and low density filler add in the silane coupler solution, under 60~80 ℃ of temperature, stir, until do not have reunite till; Carry out drying and remove and to desolvate, what obtain surface-treated can the potteryization additive;
(2) resin of anti-the ablation is dissolved with solvent; The surface-treated that step (1) is obtained can the potteryization additive and low density filler join in the resin solution of anti-the ablation; Both are mixed; Processing can the potteryization resin adhesive liquid, and what do not have reunion in can the potteryization resin adhesive liquid can potteryization additive or other visible impurity;
(3) with the staple length yarn be put into that step (2) obtains can the potteryization resin adhesive liquid in; Stir and rub; Requiring to mix churning time is 50min~60min, and PM mixes and is no less than 20 times, needs to guarantee that the staple length yarn can the potteryization resin adhesive liquid be soaked into even after mixing finishes;
(4) will flood good staple length yarn and evenly spread out, the weight≤100g of silk group of staple length yarn is fluffy; And the interval that 10mm~20mm should be arranged between the silk group; Place 15 ℃~30 ℃ then, dry in the environment of the ventilation cleaning of humidity≤75%, the air dried time is no less than 24h;
(5) the silk group that will dry is torn by hand, and requires the floss and the powdery substance that produce are disposed when tearing thread, and maximum pack is no more than 20 after tearing;
(6) the silk group that step (5) dipping is obtained, with the mould matched moulds, carries out insulation 1h by one one, put in the mould uniformly under 60~80 ℃ during matched moulds through pressuring method;
(7) according to the curing system of the resin of anti-the ablation, the curing that heats up, said curing system is: be incubated 1h, 1h to 110 ℃ of intensification down at 90 ℃; Be incubated 1h, 1h to 140 ℃ of intensification down at 110 ℃; Be incubated 1h, 1h to 180 ℃ of intensification down at 140 ℃; Be incubated 2h, 1h to 200 ℃ of intensification down at 180 ℃; At 200 ℃ of insulation 1h;
(8) solidify finish after, treat that mould naturally cools to the demoulding when being not less than 30 ℃, and the overlap that polishing can the potteryization polymer matrix composites.
Preferably, said solvent is absolute ethyl alcohol or acetone.
Preferably, said step (3) can be carried out under the environment of vacuum or pressurization.
Further, the mould in said (4) before the dress mould, evenly wiping or spraying releasing agent in the die cavity of mould.
Further, the mould in said (6) before the dress mould, evenly wiping or spraying releasing agent in the die cavity of mould.
Further, in the said intensification solidified process, the mold cavity size does not change.
Preferably, said low density filler is hollow glass micropearl, hollow silicon dioxide microballoon or hollow phenolic aldehyde microballoon.
Further; Said step (4) is: will flood good staple length yarn and evenly spread out and be placed on the desk that is covered with clean plastic cloth, the weight≤100g of silk group of staple length yarn is fluffy; And the interval that 10mm~20mm should be arranged between the silk group; Place 15 ℃~30 ℃ then, dry in the environment of the ventilation cleaning of humidity≤75%, the air dried time is no less than 24h.
The present invention has the following advantages:
That utilizes that method of the present invention prepares can have light weight, high-strength, anti-ablation and heat insulation advantage by the potteryization polymer matrix composites; Under>600 ℃ of high temperature aerobic environments; Can realize the potteryization transformation by the potteryization additive, material is converted into resistant to elevated temperatures fiber reinforced ceramic matrix material.And through the preparation of this forming method can the potteryization polymer matrix composites; Need not to change existing moulding process, equipment and mould; Production cycle, cost, workability and thermal insulation all are superior to ceramic base thermal protection matrix material, have wide through engineering approaches application prospect.
Description of drawings
Below in conjunction with accompanying drawing the present invention is described further.
Fig. 1 provides for the embodiment of the invention 1 a kind of can the preparation method of potteryization polymer matrix composites in the structural representation of mould matched moulds;
A kind of low density that Fig. 2 provides for the embodiment of the invention 2 can the preparation method of potteryization polymer matrix composites in the structural representation of mould matched moulds.
Embodiment
Preparing method that can potteryization polymer matrix composites 2 may further comprise the steps:
(1) silane coupling agent is dissolved with absolute ethyl alcohol; Can add in the silane coupler solution by the potteryization additive; Under 60 ℃, stir, till not having reunion, filter with dry removing and desolvate; What obtain surface-treated can the potteryization additive, can the potteryization additive be the mixture of silicate, nitride, carbide;
(2) resin of anti-the ablation is dissolved with absolute ethyl alcohol; Can joining in the resin solution of anti-the ablation by the potteryization additive of the surface-treated that step (1) is obtained; Both are mixed; Processing can the potteryization resin adhesive liquid, and what do not have reunion in can the potteryization resin adhesive liquid can potteryization additive or other visible impurity;
(3) under vacuum environment, with step (2) obtain can potteryization resin adhesive liquid impregnation of fibers integral fabric, dry after thorough the fibre integral fabric dipping is all even;
(4) with reference to Fig. 1, the fibre integral fabric that step (3) dipping obtains is put in the mould 1,, at room temperature carry out during matched moulds mould 1 matched moulds through pressuring method, before the dress mould in the die cavity of mould 1 even wiping releasing agent;
(5) according to the curing system of the resin of anti-the ablation, the curing that heats up, said curing system is: be incubated 1h, 1h to 110 ℃ of intensification down at 90 ℃; Be incubated 1h, 1h to 140 ℃ of intensification down at 110 ℃; Be incubated 1h, 1h to 180 ℃ of intensification down at 140 ℃; Be incubated 2h, 1h to 200 ℃ of intensification down at 180 ℃; At 200 ℃ of insulation 1h, in the intensification solidified process, the mold cavity size does not change;
(6) solidify finish after, the demoulding when treating that mould 1 is reduced to room temperature, and the overlap that polishing can potteryization polymer matrix composites 2.
Moulding can have the high-strength light characteristic of fiber reinforced polymer composites by the potteryization polymer matrix composites at normal temperatures as stated above; Under>600 ℃ of high temperature aerobic environments; Can realize the potteryization transformation by the potteryization additive, material is converted into resistant to elevated temperatures fiber reinforced ceramic matrix material.And through the preparation of this forming method can the potteryization polymer matrix composites, cost is relatively low, workability and structural safety performance are superior to ceramic base thermal protection matrix material, have wide through engineering approaches application prospect.
When strongthener was the staple length yarn, the preparation method that low density can potteryization polymer matrix composites 4 was:
(1) silane coupling agent is dissolved with acetone; Can the potteryization additive and the hollow silicon dioxide microballoon add in the silane coupler solution, under 80 ℃ of temperature, stir, until do not have reunite till; Carry out drying and remove and to desolvate, what obtain surface-treated can the potteryization additive;
(2) resin of anti-the ablation is dissolved with acetone; The surface-treated that step (1) is obtained can the potteryization additive and the hollow silicon dioxide microballoon join in the resin solution of anti-the ablation; Both are mixed; Processing can the potteryization resin adhesive liquid, and what do not have reunion in can the potteryization resin adhesive liquid can potteryization additive or other visible impurity;
(3) under pressurized conditions; With the staple length yarn be put into that step (2) obtains can the potteryization resin adhesive liquid in; Stir and rub; Requiring to mix churning time is 50min, and PM mixes and is no less than 20 times, needs to guarantee that the staple length yarn can the potteryization resin adhesive liquid be soaked into even after mixing finishes;
(4) will flood good staple length yarn evenly spreads out and is placed on the desk that is covered with clean plastic cloth; Weight≤the 100g of silk group of staple length yarn; Fluffy, and the interval of 20mm should be arranged between the silk group, place 15 ℃ then; Dry in the environment of the ventilation cleaning of humidity≤75%, the air dried time is no less than 24h;
(5) the silk group that will dry is torn by hand, and requires the floss and the powdery substance that produce are disposed when tearing thread, and maximum pack is no more than 20 after tearing;
(6) with reference to Fig. 2; The silk group that step (5) dipping is obtained, one one, put in the mould 3 uniformly, through pressuring method with mould 3 matched moulds; Under 60 ℃, carry out during matched moulds; Insulation 1h evenly sprays releasing agent in the die cavity of mould 3 before the dress mould, the device of exerting pressure is a press 5;
(7) according to the curing system of the resin of anti-the ablation, the curing that heats up, said curing system is: be incubated 1h, 1h to 110 ℃ of intensification down at 90 ℃; Be incubated 1h, 1h to 140 ℃ of intensification down at 110 ℃; Be incubated 1h, 1h to 180 ℃ of intensification down at 140 ℃; Be incubated 2h, 1h to 200 ℃ of intensification down at 180 ℃; At 200 ℃ of insulation 1h;
(8) solidify finish after, treat that mould naturally cools to the demoulding when being not less than 30 ℃, and the overlap that polishing can potteryization polymer matrix composites 4.
The low density of moulding can have light weight, high-strength, anti-ablation and heat insulation advantage by the potteryization polymer matrix composites as stated above; Under>600 ℃ of high temperature aerobic environments; Can realize the potteryization transformation by the potteryization additive, material is converted into resistant to elevated temperatures staple fibre and strengthens ceramic composite.And the low density through the preparation of this forming method can the potteryization polymer matrix composites; Need not to change existing moulding process, equipment and mould; Production cycle, cost, workability and thermal insulation all are superior to ceramic base thermal protection matrix material, have wide through engineering approaches application prospect.
Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although the present invention is specified with reference to preferred embodiment; Those of ordinary skill in the art is to be understood that; Can make amendment or be equal to replacement technical scheme of the present invention, and not break away from the spirit and the scope of technical scheme of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (10)
- One kind can the potteryization polymer matrix composites the preparation method, it is characterized in that, may further comprise the steps:(1) silane coupling agent is dissolved with solvent, can the potteryization additive adds in the silane coupler solution, under 60~80 ℃, stir, up to do not have reunite till, filter with dry removing and desolvate, what obtain surface-treated can the potteryization additive;(2) resin of anti-the ablation is dissolved with solvent; Can joining in the resin solution of anti-the ablation by the potteryization additive of the surface-treated that step (1) is obtained; Both are mixed; Processing can the potteryization resin adhesive liquid, and what do not have reunion in can the potteryization resin adhesive liquid can potteryization additive or other visible impurity;(3) with step (2) obtain can potteryization resin adhesive liquid lay-up, dry after thorough the strongthener dipping is all even;(4) strongthener that step (3) dipping is obtained is put in the mould, with the mould matched moulds, is to carry out under 0~80 ℃ in temperature through pressuring method during matched moulds;(5) according to the curing system of the resin of anti-the ablation, the curing that heats up, said curing system is: be incubated 1h, 1h to 110 ℃ of intensification down at 90 ℃; Be incubated 1h, 1h to 140 ℃ of intensification down at 110 ℃; Be incubated 1h, 1h to 180 ℃ of intensification down at 140 ℃; Be incubated 2h, 1h to 200 ℃ of intensification down at 180 ℃; At 200 ℃ of insulation 1h;(6) solidify finish after, the demoulding when treating that mould is reduced to room temperature, and the overlap that polishing can the potteryization polymer matrix composites.
- 2. preparation method that can the potteryization polymer matrix composites according to claim 1 is characterized in that said strongthener is a fibre integral fabric.
- 3. preparation method that can the potteryization polymer matrix composites according to claim 1 is characterized in that when said strongthener was the staple length yarn, its preparation method was:(1) silane coupling agent is dissolved with solvent; Can the potteryization additive and low density filler add in the silane coupler solution, under 60~80 ℃ of temperature, stir, until do not have reunite till; Carry out drying and remove and to desolvate, what obtain surface-treated can the potteryization additive;(2) resin of anti-the ablation is dissolved with solvent; The surface-treated that step (1) is obtained can the potteryization additive and low density filler join in the resin solution of anti-the ablation; Both are mixed; Processing can the potteryization resin adhesive liquid, and what do not have reunion in can the potteryization resin adhesive liquid can potteryization additive or other visible impurity;(3) with the staple length yarn be put into that step (2) obtains can the potteryization resin adhesive liquid in; Stir and rub; Requiring to mix churning time is 50min~60min, and PM mixes and is no less than 20 times, needs to guarantee that the staple length yarn can the potteryization resin adhesive liquid be soaked into even after mixing finishes;(4) will flood good staple length yarn and evenly spread out, the weight≤100g of silk group of staple length yarn is fluffy; And the interval that 10mm~20mm should be arranged between the silk group; Place 15 ℃~30 ℃ then, dry in the environment of the ventilation cleaning of humidity≤75%, the air dried time is no less than 24h;(5) the silk group that will dry is torn by hand, and requires the floss and the powdery substance that produce are disposed when tearing thread, and maximum pack is no more than 20 after tearing;(6) the silk group that step (5) dipping is obtained, with the mould matched moulds, carries out insulation 1h by one one, put in the mould uniformly under 60~80 ℃ during matched moulds through pressuring method;(7) according to the curing system of the resin of anti-the ablation, the curing that heats up, said curing system is: be incubated 1h, 1h to 110 ℃ of intensification down at 90 ℃; Be incubated 1h, 1h to 140 ℃ of intensification down at 110 ℃; Be incubated 1h, 1h to 180 ℃ of intensification down at 140 ℃; Be incubated 2h, 1h to 200 ℃ of intensification down at 180 ℃; At 200 ℃ of insulation 1h;(8) solidify finish after, treat that mould naturally cools to the demoulding when being not less than 30 ℃, and the overlap that polishing can the potteryization polymer matrix composites.
- 4. according to claim 1 or 3 described preparing methods that can the potteryization polymer matrix composites, it is characterized in that said solvent is absolute ethyl alcohol or acetone.
- 5. according to claim 1 or 3 described preparing methods that can the potteryization polymer matrix composites, it is characterized in that said step (3) can be carried out under the environment of vacuum or pressurization.
- 6. preparation method that can the potteryization polymer matrix composites according to claim 1 is characterized in that, the mould in said (4) before the dress mould, evenly wiping or spraying releasing agent in the die cavity of mould.
- 7. preparation method that can the potteryization polymer matrix composites according to claim 3 is characterized in that, the mould in said (6) before the dress mould, evenly wiping or spraying releasing agent in the die cavity of mould.
- 8. according to claim 1 or 3 described preparing methods that can the potteryization polymer matrix composites, it is characterized in that in the said intensification solidified process, the mold cavity size does not change.
- 9. preparation method that can the potteryization polymer matrix composites according to claim 3 is characterized in that said low density filler is hollow glass micropearl, hollow silicon dioxide microballoon or hollow phenolic aldehyde microballoon.
- 10. preparation method that can the potteryization polymer matrix composites according to claim 3 is characterized in that said step (4) is: will flood good staple length yarn and evenly spread out and be placed on the desk that is covered with clean plastic cloth; Weight≤the 100g of silk group of staple length yarn; Fluffy, and the interval of 10mm~20mm should be arranged between the silk group, place 15 ℃~30 ℃ then; Dry in the environment of the ventilation cleaning of humidity≤75%, the air dried time is no less than 24h.
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Cited By (9)
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CN103449825A (en) * | 2013-08-19 | 2013-12-18 | 航天特种材料及工艺技术研究所 | Micro-ablation insulating material and preparation method thereof |
CN103540155A (en) * | 2013-09-29 | 2014-01-29 | 湖北三江航天红阳机电有限公司 | Preparation method of high-temperature resisting ablative resin matrix composite |
CN109294238A (en) * | 2018-09-13 | 2019-02-01 | 沈阳理工大学 | A kind of high-elastic resistance to ablative-insulative material of lightweight and preparation method thereof |
CN109486201A (en) * | 2018-09-13 | 2019-03-19 | 沈阳理工大学 | The resistance to ablative insulative material of the siliceous boron high polymer base of self-cross linking type and preparation method |
CN110194609A (en) * | 2019-04-22 | 2019-09-03 | 湖南远辉新材料研究院有限公司 | A kind of high temperature resistant, it is anti-oxidant can ceramic resin composite materials and preparation method thereof |
CN111349306A (en) * | 2020-03-16 | 2020-06-30 | 武汉理工大学 | Ceramizable phenolic resin and preparation method and application thereof |
CN112064357A (en) * | 2020-08-27 | 2020-12-11 | 航天特种材料及工艺技术研究所 | Ablation-resistant silicone resin composite material and preparation method thereof |
CN112662311A (en) * | 2020-12-07 | 2021-04-16 | 上海航天设备制造总厂有限公司 | Light high-silicon ceramic resin coating, ceramic coating and preparation method thereof |
CN117165248A (en) * | 2023-10-31 | 2023-12-05 | 南京艾布纳新材料股份有限公司 | Multi-curing polyurethane ceramic sealant and preparation method thereof |
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CN101939359A (en) * | 2007-10-22 | 2011-01-05 | 弗莱克斯伯陶器公司 | Fire resistant flexible ceramic resin blend and composite products formed therefrom |
CN102558666A (en) * | 2010-12-28 | 2012-07-11 | 上海金发科技发展有限公司 | Ceramic fiber reinforced polypropylene complex and preparation method thereof |
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CN103449825A (en) * | 2013-08-19 | 2013-12-18 | 航天特种材料及工艺技术研究所 | Micro-ablation insulating material and preparation method thereof |
CN103540155A (en) * | 2013-09-29 | 2014-01-29 | 湖北三江航天红阳机电有限公司 | Preparation method of high-temperature resisting ablative resin matrix composite |
CN103540155B (en) * | 2013-09-29 | 2016-02-10 | 湖北三江航天红阳机电有限公司 | A kind of preparation method of resistant to elevated temperatures Ablative resin based composites |
CN109486201B (en) * | 2018-09-13 | 2021-03-23 | 沈阳理工大学 | Self-crosslinking type silicon-boron-containing high polymer-based ablation-resistant heat-insulating material and preparation method thereof |
CN109486201A (en) * | 2018-09-13 | 2019-03-19 | 沈阳理工大学 | The resistance to ablative insulative material of the siliceous boron high polymer base of self-cross linking type and preparation method |
CN109294238B (en) * | 2018-09-13 | 2021-03-16 | 沈阳理工大学 | Light high-elastic ablation-resistant heat-insulating material and preparation method thereof |
CN109294238A (en) * | 2018-09-13 | 2019-02-01 | 沈阳理工大学 | A kind of high-elastic resistance to ablative-insulative material of lightweight and preparation method thereof |
CN110194609A (en) * | 2019-04-22 | 2019-09-03 | 湖南远辉新材料研究院有限公司 | A kind of high temperature resistant, it is anti-oxidant can ceramic resin composite materials and preparation method thereof |
CN110194609B (en) * | 2019-04-22 | 2021-07-16 | 湖南远辉新材料研究院有限公司 | High-temperature-resistant and oxidation-resistant ceramizable resin composite material and preparation method thereof |
CN111349306A (en) * | 2020-03-16 | 2020-06-30 | 武汉理工大学 | Ceramizable phenolic resin and preparation method and application thereof |
CN112064357A (en) * | 2020-08-27 | 2020-12-11 | 航天特种材料及工艺技术研究所 | Ablation-resistant silicone resin composite material and preparation method thereof |
CN112662311A (en) * | 2020-12-07 | 2021-04-16 | 上海航天设备制造总厂有限公司 | Light high-silicon ceramic resin coating, ceramic coating and preparation method thereof |
CN112662311B (en) * | 2020-12-07 | 2021-10-01 | 上海航天设备制造总厂有限公司 | Light high-silicon ceramic resin coating, ceramic coating and preparation method thereof |
CN117165248A (en) * | 2023-10-31 | 2023-12-05 | 南京艾布纳新材料股份有限公司 | Multi-curing polyurethane ceramic sealant and preparation method thereof |
CN117165248B (en) * | 2023-10-31 | 2024-02-23 | 南京艾布纳新材料股份有限公司 | Multi-curing polyurethane ceramic sealant and preparation method thereof |
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