CN101913878A - Method for preparing silicon carbide particle-reinforced silicon nitride composite ceramic parts - Google Patents
Method for preparing silicon carbide particle-reinforced silicon nitride composite ceramic parts Download PDFInfo
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- CN101913878A CN101913878A CN 201010230573 CN201010230573A CN101913878A CN 101913878 A CN101913878 A CN 101913878A CN 201010230573 CN201010230573 CN 201010230573 CN 201010230573 A CN201010230573 A CN 201010230573A CN 101913878 A CN101913878 A CN 101913878A
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Abstract
The invention discloses a method for preparing silicon carbide particle-reinforced silicon nitride composite ceramic parts, and belongs to the technical field of ceramic part preparation. The method comprises the following steps of: mixing SiC powder, Si3N4 powder, a sintering acid and a paraffin base multicomponent binder into a uniform feed; and performing solvent-thermal debinding and presintering at the temperature of between 1,150 and 1,200 DEG C on a preformed blank obtained by injection molding of the feed, and sintering in a vacuum carbon tube furnace at the temperature of between 1,800 and 1,900 DEG C and at the normal pressure in the Ar atmosphere to prepare SiCp/Si3N4 composite ceramic parts. The method for preparing the silicon carbide particle-reinforced silicon nitride composite ceramic parts has the advantages of direct preparation of SiCp/Si3N4 composite ceramic products with complicated geometry, uniform texture, high dimensional accuracy and no need of subsequent processing, achievement of integrated molding of the SiCp/Si3N4 materials and the parts, and establishment of low-cost preparation technology for the SiCp/Si3N4 composite ceramic parts with complicated shapes and high dimensional accuracy.
Description
Technical field
The invention belongs to composite ceramics parts preparing technical field, particularly provide a kind of and prepared SiC particles reinforced silicon nitride (SiCp/Si with injection molding process
3N
4) method of complex phase ceramic part, realize preparation low-cost, the high-performance ceramic base composite material parts.
Background technology
SiCp/Si
3N
4Material has as the required hear resistance of high-temperature structural material, resistance to sudden heating, wearability and corrosion resistance, and than metal light, the needs that satisfy the fields such as nuclear energy, petrochemical industry, Aero-Space, national defence have great importance.The fragility that ceramic material itself is intrinsic and high rigidity, although traditional powder metallurgy die pressing technology is simple, the shaping base that mold pressing forms is Density inhomogeneity often, the complex-shaped degree of parts also has been subjected to certain restriction; Also there are the shortcomings such as manufacturing cycle is long, dimensional accuracy is low in the precursor cracking process except being subjected to the restriction of parts complexity; The complicated form part that can be shaped though casting and press filtration are shaped is owing to the problems such as shaping density lack of homogeneity and dimensional accuracy are low have limited its range of application.And when adopting Powder Injection Molding Technology, because the shape of injection base substrate near the net shape of goods, has not only solved SiCp/Si
3N
4The structural homogenity problem of material, the difficulty that has solved simultaneously its complex parts shapes problem, has realized SiCp/Si
3N
4Material and part integral forming.
The basic craft course of injection forming is: the ceramic powder and the organic binder bond that at first will have specified particle size and configuration of surface mix, and make feeding.Take organic binder bond as carrier, so that feeding has flowability at a certain temperature, feeding is shaped at the effect current downflow loading mould cavity of power and heat on injection machine, obtains injecting base substrate, obtains subsequently complete fine and close or near fully dense product through degreasing and sintering.But the injection forming automatic production, management in the production process and control are also very convenient, the suitable production in enormous quantities in enormous quantities; Each position density of goods is even, the geometric accuracy height.
Summary of the invention
The object of the present invention is to provide a kind of SiCp/Si of preparation
3N
4The method of composite material parts has solved SiCp/Si
3N
4Even, the difficult processing of tissue odds in the composite ceramics part production process, high in cost of production problem have realized having complex-shaped and the high SiCp/Si of dimensional accuracy
3N
4The low cost preparation of composite ceramics part.
Preparation technology of the present invention is: mixing evenly ceramic powders and binding agent, granulation, injection moulding will be injected green compact degreasing, sintering more subsequently, make SiCp/Si
3N
4The composite ceramics part.Concrete technology is:
1, mixed powder: with SiC powder (particle diameter is 0.01~0.1 μ m), Si
3N
4(sintering aid is by Al with sintering aid for powder (particle diameter is 0.3~1.0 μ m)
2O
3: Y
2O
3Form aluminium oxide Al
2O
3With yittrium oxide Y
2O
3Mass ratio is 4: 5) place the corundum ball grinder with certain rotating speed ball milling 16 hours, reach and mix.Wherein each powder quality percentage is SiC: Si
3N
4: sintering aid=(5~20): (70~85): (5~10);
2, the configuration of paraffinic base multicomponent binding agent: the composition of binding agent is: paraffin (PW), high density polyethylene(HDPE) (HDPE), stearic acid (SA).Each constituent element weight percent is PW: HDPE: SA=(60~70): (25~30): (5~10).Three kinds of constituent elements are added blend in the thermostat, reach even mixing;
3, mixing: as will to have added the silicon nitride powder of a certain amount of sintering aid and the paraffinic base multicomponent binding agent mixing 1~1.5h on opening rubber mixing machine that is prepared, melting temperature is 135~150 ℃, on SK2160 type twin-screw mixer forcing machine, granulate again, make feeding further even, the ratio of the silicon nitride powder of sintering aid and multicomponent polymer-paraffin based binder powder (percent by volume) is 50~60: 40~50.
4, injection moulding: the gained feeding is injected at CJ80E type injection machine after will granulating, and injection temperature is 170~185 ℃, and injection pressure is 90~110Mpa, and mold temperature is 20~50 ℃, obtains SiCp/Si
3N
4The composite ceramics preform;
5, degreasing and presintering: adopt two step degreasing methods of solvent degreasing+hot degreasing, at first with SiCp/Si
3N
4The composite ceramics preform is dipped in and carries out solvent degreasing 8~12h in the trichloro-ethylene, skimming temp is 20~50 ℃, the taking-up base substrate was dried in thermostatic drying chamber after degreasing was finished, hot degreasing is carried out in vacuum tube furnace, skimming temp is between 30~600 ℃, be heated at last and carry out presintering 0.5~1h between 1100~1200 ℃, obtain the presintering base, whole heating process atmosphere is Ar;
6, sintering: with the presintering base place vacuum sintering furnace in 1800~1900 ℃ normal pressure-sintered, insulation 0.5~1h is 5~7 ℃/min before 1400 ℃ of the heating rates, be 3~5 ℃/min after 1400 ℃, sintering atmosphere is Ar, and sintered body is processed through follow-up finishing, obtains SiCp/Si
3N
4The composite ceramics part.
The invention has the advantages that:
Can directly prepare the SiCp/Si of complex geometry
3N
4Composite ceramic articles; The goods even tissue, the dimensional accuracy height, and need not following process; Can realize SiCp/Si
3N
4The integral forming of material and part; Set up and had complex-shaped and the high SiCp/Si of dimensional accuracy
3N
4The low-cost technology of preparing of composite ceramics part.
Embodiment
Embodiment 1: the SiCp/Si that contains 5wt%SiC, useful load 58vol%
3N
4Composite material parts
The mass fraction of each composition of raw material is 5%SiC+85%Si
3N
4+ 4.3%Al
2O
3+ 5.7%Y
2O
3, binding agent is adopted as heteropolymer paraffinic base binding agent, and each constituent element weight fraction is 65%PW+25%HDPE+10%SA, and powder loading is 58vol%.
With the highly purified silicon nitride powder of granularity 0.58 μ m, granularity 0.09 μ m silicon carbide powder, sintering aid is mixed in proportion, and is solvent with the dehydrated alcohol, ball milling 16h in the corundum ball grinder.The ceramic powders that ball milling is good and binding agent are 58% preparation by the ceramic powders volume fraction then, on SK2160 type open type plastic purificating set 140 ℃ mixing evenly.Use PSJ32 type single screw extrusion machine extrusion granulator subsequently again, adopting injection pressure on CJ80E type injection moulding machine is 100MPa, 170 ℃ of injection temperatures, injection speed remains on system peaked 60%, dwell pressure is 100MPa, and die temperature is 30 ℃ an optimal injection parameter, injects base substrate, carry out solvent degreasing at 40 ℃, 8h, hot degreasing and under Ar atmosphere then in 1200 ℃ of presintering; Under mobile Ar atmosphere, normal pressure-sintered at 1800 ℃ at last at vacuum carbon tube furnace.Sintered body namely obtains relative density and reaches 97% through subsequent treatment, and dimensional accuracy is up to ± 0.2% and comprehensive mechanical property SiCp/Si preferably
3N
4The composite ceramics special-shaped part.
Embodiment 2: the SiCp/Si that contains 10wt%SiC, useful load 50vol%
3N
4Composite material parts
The mass fraction of each composition of raw material is 10%SiC+80%Si
3N
4+ 4.3%Al
2O
3+ 5.7%Y
2O
3, binding agent is adopted as heteropolymer paraffinic base binding agent, and each constituent element weight fraction is 63%PW+27%HDPE+10%SA, and powder loading is 50vol%.
Silicon carbide powder, the sintering aid of granularity 0.8 μ m high purity nitrogenize silicon powder, granularity 0.09 μ m are mixed in proportion, and are solvent with the dehydrated alcohol, ball milling 16h in the corundum ball grinder.Then that ball milling is good ceramic powder and binding agent are 58% preparation by the ceramic powder volume fraction, on SK2160 type open type plastic purificating set 140 ℃ mixing evenly, use PSJ32 type single screw extrusion machine extrusion granulator subsequently again, adopting injection pressure on CJ80E type injection moulding machine is 100MPa, 180 ℃ of injection temperatures, injection speed remains on system peaked 60%, dwell pressure is 100MPa, die temperature is 30 ℃ an optimal injection parameter, inject base substrate, carry out solvent degreasing at 40 ℃, 8h, hot degreasing and under Ar atmosphere then in 1200 ℃ of presintering; Under mobile Ar atmosphere, normal pressure-sintered at 1800 ℃ at last at vacuum carbon tube furnace.Sintered body namely obtains relative density and reaches 98% through subsequent treatment, and dimensional accuracy is up to ± 0.2% and comprehensive mechanical property SiCp/Si preferably
3N
4The composite ceramics special-shaped part.
Embodiment 3: the SiCp/Si that contains 20wt%SiC, useful load 58%
3N
4Composite material parts
The mass fraction of each composition of raw material is 5%SiC+85%Si
3N
4+ 4.3%Al
2O
3+ 5.7%Y
2O
3, binding agent is adopted as heteropolymer paraffinic base binding agent, and its each constituent element percentage by weight is PW: HDPE: SA=65: 25: 10, powder loading was 58vol%.
With silicon nitride powder, the granularity 0.09 μ m silicon carbide powder of granularity 0.58 μ m high-purity alpha phase>93%, sintering aid is mixed in proportion, and is solvent with the dehydrated alcohol, ball milling 16h in the corundum ball grinder.Then that ball milling is good ceramic powder and binding agent are 58% preparation by the ceramic powder volume fraction, on SK2160 type open type plastic purificating set 140 ℃ mixing evenly, use PSJ32 type single screw extrusion machine extrusion granulator subsequently again, adopting injection pressure on CJ80E type injection moulding machine is 100MPa, 170 ℃ of injection temperatures, injection speed remains on system peaked 60%, dwell pressure is 100MPa, die temperature is 30 ℃ an optimal injection parameter, inject base substrate, carry out solvent degreasing at 40 ℃, 8h, hot degreasing and under Ar atmosphere then in 1200 ℃ of presintering; Under mobile Ar atmosphere, normal pressure-sintered at 1900 ℃ at last at vacuum carbon tube furnace.Sintered body namely obtains relative density and reaches 97% through subsequent treatment, and dimensional accuracy is up to ± 0.2% and comprehensive mechanical property SiCp/Si preferably
3N
4The composite ceramics special-shaped part.
Claims (2)
1. a method for preparing silicon carbide particle-reinforced silicon nitride composite ceramic parts is characterized in that, preparation technology is:
A, mixed powder: with SiC powder, Si
3N
4Powder and sintering aid place the corundum ball grinder with certain rotating speed ball milling 14-18 hour, the silicon nitride powder with sintering aid that obtains mixing; Wherein each powder quality mark is (5~20) %SiC+ (70~85) %Si
3N
4+ (5~10) % sintering aid; Sintering aid is by Al
2O
3: Y
2O
3Form, mass fraction is Al
2O
3: Y
2O
3=4: 5;
The configuration of b, paraffinic base multicomponent binding agent: the composition of binding agent is that paraffin is that PW, high density polyethylene(HDPE) are that HDPE, stearic acid are SA, and each constituent element weight percent is PW: HDPE: SA=(60~70): (25~30): (5~10); Three kinds of constituent elements are added blend in the thermostat, reach uniform ingredients;
C, mixing: will add the silicon nitride powder of a certain amount of sintering aid and the multicomponent polymer-paraffin based binder mixing 1~1.5h on opening rubber mixing machine that is prepared, melting temperature is 135~150 ℃, on SK2160 type twin-screw mixer forcing machine, granulate again, make feeding further even; The ratio of the silicon nitride powder of sintering aid and multicomponent polymer-paraffin based binder powder volume percentage ratio is 50~60: 40~50;
D, injection moulding: the gained feeding is injected at CJ80E type injection machine after will granulating, and injection temperature is 170~185 ℃, and injection pressure is 90~110Mpa, and mold temperature is 20~50 ℃, obtains SiCp/Si
3N
4The composite ceramics preform;
E, degreasing and presintering: adopt two step degreasing methods of solvent degreasing+hot degreasing, at first with SiCp/Si
3N
4The composite ceramics preform is dipped in and carries out solvent degreasing 8~12h in the trichloro-ethylene, skimming temp is 20~50 ℃, the taking-up base substrate was dried in thermostatic drying chamber after degreasing was finished, hot degreasing is carried out in vacuum tube furnace, skimming temp is between 30~600 ℃, be heated at last and carry out presintering 0.5~1h between 1100~1200 ℃, obtain the presintering base, whole heating process atmosphere is Ar;
F, sintering: with the presintering base place vacuum sintering furnace in 1800~1900 ℃ normal pressure-sintered, insulation 0.5~1h is 5~7 ℃/min before 1400 ℃ of the heating rates, be 3~5 ℃/min after 1400 ℃, sintering atmosphere is Ar, and sintered body is processed through follow-up finishing, obtains SiCp/Si
3N
4The composite ceramics part.
2. according to the described a kind of silicon carbide particle-reinforced silicon nitride composite ceramic parts method for preparing of claim 1, it is characterized in that: Si
3N
4The particle diameter of raw material is 0.3~1.0 μ m, purity>99%; The SiC particle diameter is 0.01~0.1 μ m, purity>99%.
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Cited By (13)
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CN102717081A (en) * | 2012-06-20 | 2012-10-10 | 北京科技大学 | Method for preparing miniature mold by powder micro injection forming method |
CN102992778A (en) * | 2012-09-11 | 2013-03-27 | 廖文宏 | Precision ceramic with jade texture and preparation method thereof |
CN104045350A (en) * | 2013-03-11 | 2014-09-17 | 中国科学院上海硅酸盐研究所 | Method for preparing silicon nitride /silicon carbide ceramic composite by use of reaction sintering process |
CN104258741A (en) * | 2014-09-24 | 2015-01-07 | 马嘉 | Ceramic membrane supporting body with filtering function and preparation method and application of ceramic membrane supporting body |
CN105420581A (en) * | 2015-11-10 | 2016-03-23 | 太仓捷公精密金属材料有限公司 | Ceramic metal material |
CN105451916A (en) * | 2014-05-13 | 2016-03-30 | 犹他大学研究基金会 | Production of substantially spherical metal powers |
CN105669206A (en) * | 2015-12-31 | 2016-06-15 | 南方科技大学 | Porous silicon carbide ceramic and preparation method thereof |
CN107216154A (en) * | 2017-06-19 | 2017-09-29 | 青岛科技大学 | A kind of mixed material being molded for ceramic 3D printing and preparation method thereof |
CN108439995A (en) * | 2018-05-24 | 2018-08-24 | 中南大学 | A kind of complex phase ceramic and preparation method thereof |
CN109465970A (en) * | 2018-11-08 | 2019-03-15 | 北京星航机电装备有限公司 | A kind of silicon nitride complex phase ceramics high temperature resistant composite thin-wall curved-surface structure part processing method |
US10689730B2 (en) | 2013-08-19 | 2020-06-23 | University Of Utah Research Foundation | Methods of producing a titanium product |
US10907239B1 (en) | 2020-03-16 | 2021-02-02 | University Of Utah Research Foundation | Methods of producing a titanium alloy product |
CN113548903A (en) * | 2021-08-27 | 2021-10-26 | 广东工业大学 | Silicon carbide reinforced silicon nitride ceramic and preparation method thereof |
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Cited By (18)
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CN102992778A (en) * | 2012-09-11 | 2013-03-27 | 廖文宏 | Precision ceramic with jade texture and preparation method thereof |
CN104045350A (en) * | 2013-03-11 | 2014-09-17 | 中国科学院上海硅酸盐研究所 | Method for preparing silicon nitride /silicon carbide ceramic composite by use of reaction sintering process |
US10689730B2 (en) | 2013-08-19 | 2020-06-23 | University Of Utah Research Foundation | Methods of producing a titanium product |
CN105451916A (en) * | 2014-05-13 | 2016-03-30 | 犹他大学研究基金会 | Production of substantially spherical metal powers |
US10130994B2 (en) | 2014-05-13 | 2018-11-20 | University Of Utah Research Foundation | Production of substantially spherical metal powders |
CN105451916B (en) * | 2014-05-13 | 2018-12-18 | 犹他大学研究基金会 | The preparation of substantially spherically-shaped metal powder |
CN104258741A (en) * | 2014-09-24 | 2015-01-07 | 马嘉 | Ceramic membrane supporting body with filtering function and preparation method and application of ceramic membrane supporting body |
CN105420581A (en) * | 2015-11-10 | 2016-03-23 | 太仓捷公精密金属材料有限公司 | Ceramic metal material |
CN105669206A (en) * | 2015-12-31 | 2016-06-15 | 南方科技大学 | Porous silicon carbide ceramic and preparation method thereof |
CN105669206B (en) * | 2015-12-31 | 2018-10-23 | 南方科技大学 | porous silicon carbide ceramic and preparation method thereof |
CN107216154A (en) * | 2017-06-19 | 2017-09-29 | 青岛科技大学 | A kind of mixed material being molded for ceramic 3D printing and preparation method thereof |
CN108439995A (en) * | 2018-05-24 | 2018-08-24 | 中南大学 | A kind of complex phase ceramic and preparation method thereof |
CN108439995B (en) * | 2018-05-24 | 2020-12-22 | 中南大学 | Complex phase ceramic and preparation method thereof |
CN109465970A (en) * | 2018-11-08 | 2019-03-15 | 北京星航机电装备有限公司 | A kind of silicon nitride complex phase ceramics high temperature resistant composite thin-wall curved-surface structure part processing method |
CN109465970B (en) * | 2018-11-08 | 2020-07-28 | 北京星航机电装备有限公司 | Method for processing silicon nitride complex phase ceramic high temperature resistant composite material thin wall curved surface structural member |
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CN113548903A (en) * | 2021-08-27 | 2021-10-26 | 广东工业大学 | Silicon carbide reinforced silicon nitride ceramic and preparation method thereof |
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