CN101397209B - Fusible pattern moulding method of silicon carbide with complicated shape - Google Patents

Fusible pattern moulding method of silicon carbide with complicated shape Download PDF

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Publication number
CN101397209B
CN101397209B CN2008102319783A CN200810231978A CN101397209B CN 101397209 B CN101397209 B CN 101397209B CN 2008102319783 A CN2008102319783 A CN 2008102319783A CN 200810231978 A CN200810231978 A CN 200810231978A CN 101397209 B CN101397209 B CN 101397209B
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insulation
paraffin
resol
vacuumize
rate
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CN101397209A (en
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乔冠军
徐顺建
李�杰
李涤尘
高积强
王红洁
杨建锋
王继平
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Xian Jiaotong University
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Xian Jiaotong University
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Abstract

The invention discloses a method for moulding and shaping complex-shaped carborundum. According to the requirements of the actual shape of a carborundum moulded piece, a paraffin female die is designed and processed; then phenolic resin mixture is poured in the die and is solidified for shaping at room temperature. Later, by deep solidification and carbonization, the multi-hole carbon blanker with the shape of the moulded piece is prepared. However, the paraffin die is melted during deep solidification and removed automatically; meanwhile, the melted paraffin is collected for recycling. Finally, siliconizing is carried out on the multi-hole carbon blanker, and the moulded piece of carborundum with the designed shape is prepared, which can be applied to use in the environments of corruption, abrasion, oxidation and high temperature. The method effectively solves the problems of complex shaping and net shaping of carborundum, and is characterized by low cost, one-step shaping, easy industrial production, not requiring demoulding and repeated utilization to die material, etc.

Description

A kind of fusible pattern moulding method of complicated shape silicon carbide
Technical field
The present invention relates to the moulding process that a kind of difficulty adds ceramic objects, particularly a kind of fusible pattern moulding method of complicated shape silicon carbide.
Background technology
Silicon carbide ceramics is a kind of material with good over-all properties.It is little that silicon carbide ceramics has density, and thermal conductivity is high, and thermal expansivity is low, good thermal shock, and good in oxidation resistance, characteristics such as hot strength is big, and is corrosion-resistant are able to use at numerous industrial circles.For example be used to prepare rocket combustion chamber's inwall, nozzle and nose cone in space flight and aviation industry; Be used to prepare turbocharger rotor in automotive industry.Yet the preparation of the silit of complex-shaped, clean moulding is the gordian technique that the restriction silicon carbide ceramics is applied always.It is that carbon raw material is prepared the porous carbon idiosome that USP (3859421,1975) proposes with the furfuryl alcohol resin first, subsequently idiosome is carried out the idiosome that machining obtains having silit product geometrical shape.Constant basically because of geometrical dimension before and after the idiosome siliconising, promptly make the silit product of design shape after the idiosome siliconising.But, but adopt machining to give the complicated forming ability that the certain geometrical shape of porous idiosome has limited this technology to a certain extent.It is carbon raw material that Chinese patent (CN1609054A) discloses with the photosensitive resin, in conjunction with the photocureable rapid shaping technology, makes the silit product of complicated shape.Because of having adopted rapid shaping technique, its complicated forming ability is improved.But there is certain limitation in this method, and both the price of photosensitive resin was higher and the carbon residue rate is lower, was unfavorable for suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of geometrical shape, have that the demoulding of need not, moulding stock can reuse, the fusible pattern moulding method of the complicated shape silicon carbide of low-cost, disposal molding by mould control silit product.
For achieving the above object, the technical scheme that the present invention adopts is:
1) curing molding: manufacture the paraffin former according to silit product profile, by 1:0.33~1:3 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:1~1:3 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 4~10% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample;
2) deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 100~180 ℃ of insulation 8h, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously;
3) carbonization: at N 2Carry out carbonization under the gas shiled, rise to 700~1000 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome;
4) siliconising: in crucible, put into the industrial silicon grain; The porous carbon idiosome is flat on the silicon grain; Then crucible is put into vacuum oven; Vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize, continue to be heated to 1450~1550 ℃ with same heat-up rate subsequently, insulation 30~.120min;
4) row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.
The present invention is that 2130# heat-reactive phenolic resin (production of Xi'an resin processing plant) is a carbon raw material with finished product resol; With returnable paraffin is mould; Earlier according to actual requirement design of product and processing mold; Be poured into the resol mixture in the mould, obtain the regulatable porous carbon idiosome of pore structure through curing molding, deep and firmization, carbonization, further complex-shaped silit product is prepared in siliconising.Realization is by the geometrical shape of mould control silit product, and mould itself then can be removed voluntarily and reclaim because of fusion in deep and firmization process.
Embodiment
Embodiment 1: curing molding: manufacture the paraffin former according to silit product profile, by the 1:2 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:1 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 8% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample; Deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 150 ℃, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously; Carbonization: at N 2Carry out carbonization under the gas shiled, rise to 900 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome; Siliconising: in crucible, put into the industrial silicon grain; The porous carbon idiosome is flat on the silicon grain, then crucible is put into vacuum oven, vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize; Continue to be heated to 1500 ℃ with same heat-up rate subsequently, insulation 70min; Row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.
Embodiment 2: curing molding: manufacture the paraffin former according to silit product profile, by the 1:0.5 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:3 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 5% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample; Deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 120 ℃, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously; Carbonization: at N 2Carry out carbonization under the gas shiled, rise to 700 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome; Siliconising: in crucible, put into the industrial silicon grain; With the porous carbon idiosome. be flat on the silicon grain, then crucible put into vacuum oven, vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize; Continue to be heated to 1480 ℃ with same heat-up rate subsequently, insulation 85min; Row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.
Embodiment 3: curing molding: manufacture the paraffin former according to silit product profile, by the 1:1 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:1.3 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 10% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample; Deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 180 ℃, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously; Carbonization: at N 2Carry out carbonization under the gas shiled, rise to 1000 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome; Siliconising: in crucible, put into the industrial silicon grain; The porous carbon idiosome is flat on the silicon grain, then crucible is put into vacuum oven, vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize; Continue to be heated to 1520 ℃ with same heat-up rate subsequently, insulation 60min; Row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.
Embodiment 4: curing molding: manufacture the paraffin former according to silit product profile, by the 1:3 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:1.6 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 6% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample; Deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 130 ℃, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously; Carbonization: at N 2Carry out carbonization under the gas shiled, rise to 800 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome; Siliconising: in crucible, put into the industrial silicon grain; The porous carbon idiosome is flat on the silicon grain, then crucible is put into vacuum oven, vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize; Continue to be heated to 1450 ℃ with same heat-up rate subsequently, insulation 120min; Row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.
Embodiment 5: curing molding: manufacture the paraffin former according to silit product profile, by the 1:0.33 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:2 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 4% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample; Deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 100 ℃, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously; Carbonization: at N 2Carry out carbonization under the gas shiled, rise to 750 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome; Siliconising: in crucible, put into the industrial silicon grain; The porous carbon idiosome is flat on the silicon grain, then crucible is put into vacuum oven, vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize; Continue to be heated to 1550 ℃ with same heat-up rate subsequently, insulation 30min; Row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.
Embodiment 6: curing molding: manufacture the paraffin former according to silit product profile, by the 1:1.5 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:2.5 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 7% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample; Deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 160 ℃, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously; Carbonization: at N 2Carry out carbonization under the gas shiled, rise to 950 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome; Siliconising: in crucible, put into the industrial silicon grain; The porous carbon idiosome is flat on the silicon grain, then crucible is put into vacuum oven, vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize; Continue to be heated to 1460 ℃ with same heat-up rate subsequently, insulation 100min; Row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.
Embodiment 7: curing molding: manufacture the paraffin former according to silit product profile, by the 1:2.6 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:2.8 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 9% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample; Deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 110 ℃, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously; Carbonization: at N 2Carry out carbonization under the gas shiled, rise to 850 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome; Siliconising: in crucible, put into the industrial silicon grain; The porous carbon idiosome is flat on the silicon grain, then crucible is put into vacuum oven, vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize; Continue to be heated to 1540 ℃ with same heat-up rate subsequently, insulation 50min; Row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.

Claims (1)

1. the fusible pattern moulding method of a complicated shape silicon carbide is characterized in that:
1) curing molding: manufacture the paraffin former according to silit product profile, by 1:0.33~1:3 weight ratio terepthaloyl moietie and starch are mixed then and process pore-forming agent; The weight ratio of pressing 1:1~1:3 again is with 2130# heat-reactive phenolic resin and pore-forming agent mixing and stirring; The benzene sulfonyl chloride that adds resol and terepthaloyl moietie gross weight 4~10% subsequently mixes processes the resol mixture; The resol miscellany is poured in the paraffin former, shelves under the room temperature and make this mixture solidified moulding obtain sample;
2) deep and firmization: the sample of curing molding is 60 ℃ in initial temperature is warming up to 100~180 ℃ of insulation 8h, temperature rise rate is 20 ℃/12h, reclaims fusion paraffin simultaneously;
3) carbonization: at N 2Carry out carbonization under the gas shiled, rise to 700~1000 ℃ of insulation 1h by room temperature, temperature rise rate is 50 ℃/h, cools to the furnace after the completion insulation to stop to supply N below 300 ℃ 2, process the porous carbon idiosome;
4) siliconising: in crucible, put into the industrial silicon grain; The porous carbon idiosome is flat on the silicon grain; Then crucible is put into vacuum oven; Vacuumize and be heated to 1000 ℃ with 8 ℃/min heat-up rate after stop to vacuumize, continue to be heated to 1450~1550 ℃ with same heat-up rate subsequently, insulation 30~120min;
4) row's silicon: vacuumize once more after the insulation, and be warming up to 1650 ℃, be incubated 10~30min, promptly make the silit product of design shape after the cooling.
CN2008102319783A 2008-10-28 2008-10-28 Fusible pattern moulding method of silicon carbide with complicated shape Expired - Fee Related CN101397209B (en)

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CN101655009B (en) * 2009-07-23 2012-08-15 西安科技大学 Method for manufacturing annular test-piece from cylindrical rock-soil material sample
CN111331763A (en) * 2020-02-24 2020-06-26 沈阳中航迈瑞特工业有限公司 Preparation process of reverse mold material for resin mold

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1051591C (en) * 1992-12-29 2000-04-19 斯格特纸业公司 Non-creped web and method for making same
CN101148360A (en) * 2007-08-14 2008-03-26 西安交通大学 Customized forming method for gradient porous structure ceramic
CN101209922A (en) * 2007-12-21 2008-07-02 西安交通大学 Forming method for lost foam of complicated shape silicon carbide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1051591C (en) * 1992-12-29 2000-04-19 斯格特纸业公司 Non-creped web and method for making same
CN101148360A (en) * 2007-08-14 2008-03-26 西安交通大学 Customized forming method for gradient porous structure ceramic
CN101209922A (en) * 2007-12-21 2008-07-02 西安交通大学 Forming method for lost foam of complicated shape silicon carbide

Non-Patent Citations (1)

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Title
JP特开2003-313059A 2003.11.06

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