CN101913878B - 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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- CN101913878B CN101913878B CN2010102305735A CN201010230573A CN101913878B CN 101913878 B CN101913878 B CN 101913878B CN 2010102305735 A CN2010102305735 A CN 2010102305735A CN 201010230573 A CN201010230573 A CN 201010230573A CN 101913878 B CN101913878 B CN 101913878B
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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 component preparing technical field, particularly provide a kind of and prepared silicon-carbide particle enhancing 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 thermotolerance of high-temperature structural material, resistance to sudden heating, wear resistance and erosion resistance, and lighter than metal, and the needs that satisfy fields such as nuclear energy, petrochemical complex, aerospace, national defence have great importance.Inherent fragility of stupalith own and high firmness, though traditional powder metallurgy compression molding technology is simple, the shaping base that mold pressing forms often density unevenness is even, the complex-shaped degree of parts has also received certain restriction; Also there are shortcomings such as preparation cycle is long, dimensional precision is low in the precursor cracking process except that receiving the restriction of parts complexity; The complicated form part that can be shaped though casting and press filtration are shaped is owing to problems such as shaping density uniformity difference and dimensional precision are low have limited its range of application.And when adopting the powder injection forming technology, because the shape of injection base substrate near the net shape of goods, has not only solved SiCp/Si
3N
4The homogeneity of structure problem of material, the difficulty that has solved its complicated shape simultaneously 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 process feeding.With the organic binder bond is carrier; Make feeding have flowability at a certain temperature; Feeding is shaped at power and hot effect current downflow loading mould cavity on injection machine, obtains injecting base substrate, obtains complete fine and close or approaching fully dense product through degreasing and sintering subsequently.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, and geometric accuracy is high.
Summary of the invention
The object of the present invention is to provide a kind of preparation SiCp/Si
3N
4The method of composite material parts has solved SiCp/Si
3N
4Problems such as even, the difficult processing of the tissue odds in the composite ceramics part production process, cost height have realized having complex-shaped and the high SiCp/Si of dimensional precision
3N
4The low cost preparation of composite ceramics part.
Preparation technology of the present invention is: mixing evenly ceramic powder and sticker, granulation, injection forming will be injected green compact degreasing, sintering more subsequently, make SiCp/Si
3N
4The composite ceramics part.Concrete technology is:
1, mixes 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 yttrium 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 per-cent is SiC: Si
3N
4: sintering aid=(5～20): (70～85): (5～10);
2, the configuration of paraffinic base multicomponent sticker: the composition of sticker 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 uniform mixing;
3, mixing: as will to have added the silicon nitride powder of a certain amount of sintering aid and the paraffinic base multicomponent sticker 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 forming: the back gained feeding of will granulating is injected on CJ80E type injection moulding machine, and injection temperature is 170～185 ℃, and injection pressure is 90～110Mpa, and die 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 trieline; Skimming temp is 20～50 ℃, takes out base substrate after degreasing is accomplished and in thermostatic drying chamber, dries, and 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 heat-processed 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 temperature rise rates; After 1400 ℃ 3～5 ℃/min; Sintering atmosphere is Ar, and sintered compact is handled 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 homogeneous microstructure, dimensional precision is high, 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 precision
3N
4The low-cost technology of preparing of composite ceramics part.
Embodiment
Embodiment 1: the SiCp/Si that contains 5wt%SiC, tonburden 58vol%
3N
4Composite material parts
The massfraction of each composition of raw material is 5%SiC+85%Si
3N
4+ 4.3%Al
2O
3+ 5.7%Y
2O
3, sticker is adopted as heteropolymer paraffinic base sticker, and each constituent element weight fraction is 65%PW+25%HDPE+10%SA, and the powder tonburden 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 proportional mixing, be solvent with the absolute ethyl alcohol, ball milling 16h in the corundum ball grinder.Then that ball milling is good ceramic powder and sticker are 58% preparation by the ceramic powder volume(tric)fraction, on SK2160 type open type plastic purificating set 140 ℃ mixing evenly.Use PSJ32 type single screw extrusion machine extrusion granulator subsequently again, on CJ80E type injection moulding machine, adopting injection pressure 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 compact promptly obtains specific density and reaches 97% through subsequent disposal, dimensional precision up to ± 0.2% with comprehensive mechanical property SiCp/Si preferably
3N
4The composite ceramics special-shaped part.
Embodiment 2: the SiCp/Si that contains 10wt%SiC, tonburden 50vol%
3N
4Composite material parts
The massfraction of each composition of raw material is 10%SiC+80%Si
3N
4+ 4.3%Al
2O
3+ 5.7%Y
2O
3, sticker is adopted as heteropolymer paraffinic base sticker, and each constituent element weight fraction is 63%PW+27%HDPE+10%SA, and the powder tonburden is 50vol%.
With granularity 0.8 μ m high purity nitrogenize silicon powder, the silicon carbide powder of granularity 0.09 μ m, sintering aid proportional mixing, be solvent with the absolute ethyl alcohol, ball milling 16h in the corundum ball grinder.Then that ball milling is good ceramic powder and sticker are 58% preparation by the ceramic powder volume(tric)fraction, on SK2160 type open type plastic purificating set 140 ℃ mixing evenly, use PSJ32 type single screw extrusion machine extrusion granulator subsequently again; On CJ80E type injection moulding machine, adopting injection pressure is 100MPa; It is peaked 60% that 180 ℃ of injection temperatures, injection speed remain on system, and dwell pressure is 100MPa; Die temperature is 30 ℃ an optimal injection parameter; Inject base substrate, carry out solvent degreasing, hot degreasing and under Ar atmosphere then in 1200 ℃ of presintering at 40 ℃, 8h; Under mobile Ar atmosphere, normal pressure-sintered at 1800 ℃ at last at vacuum carbon tube furnace.Sintered compact promptly obtains specific density and reaches 98% through subsequent disposal, dimensional precision up to ± 0.2% with comprehensive mechanical property SiCp/Si preferably
3N
4The composite ceramics special-shaped part.
Embodiment 3: the SiCp/Si that contains 20wt%SiC, tonburden 58%
3N
4Composite material parts
The massfraction of each composition of raw material is 5%SiC+85%Si
3N
4+ 4.3%Al
2O
3+ 5.7%Y
2O
3, sticker is adopted as heteropolymer paraffinic base sticker, and its each constituent element weight percent is PW: HDPE: SA=65: 25: 10, the powder tonburden was 58vol%.
With silicon nitride powder, granularity 0.09 μ m silicon carbide powder, the sintering aid proportional mixing of granularity 0.58 μ m high-purity alpha phase＞93%, be solvent with the absolute ethyl alcohol, ball milling 16h in the corundum ball grinder.Then that ball milling is good ceramic powder and sticker are 58% preparation by the ceramic powder volume(tric)fraction, on SK2160 type open type plastic purificating set 140 ℃ mixing evenly, use PSJ32 type single screw extrusion machine extrusion granulator subsequently again; On CJ80E type injection moulding machine, adopting injection pressure is 100MPa; It is peaked 60% that 170 ℃ of injection temperatures, injection speed remain on system, and dwell pressure is 100MPa; Die temperature is 30 ℃ an optimal injection parameter; Inject base substrate, carry out solvent degreasing, hot degreasing and under Ar atmosphere then in 1200 ℃ of presintering at 40 ℃, 8h; Under mobile Ar atmosphere, normal pressure-sintered at 1900 ℃ at last at vacuum carbon tube furnace.Sintered compact promptly obtains specific density and reaches 97% through subsequent disposal, dimensional precision up to ± 0.2% with comprehensive mechanical property SiCp/Si preferably
3N
4The composite ceramics special-shaped part.
Claims (1)
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 that has 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, massfraction is Al
2O
3: Y
2O
3=4: 5; Said 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%;
The configuration of b, paraffinic base multicomponent sticker: the composition of sticker is that paraffin is that PW, high density polyethylene(HDPE) are that HDPE, Triple Pressed 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 forming: the back gained feeding of will granulating is injected on CJ80E type injection moulding machine, and injection temperature is 170～185 ℃, and injection pressure is 90～110MPa, and die temperature is 20～50 ℃, obtains SiC
p/ Si
3N
4The composite ceramics preform;
E, degreasing and presintering: adopt two step degreasing methods of solvent degreasing+hot degreasing, at first with SiC
p/ Si
3N
4The composite ceramics preform is dipped in and carries out solvent degreasing 8～12h in the trieline; Skimming temp is 20～50 ℃, takes out base substrate after degreasing is accomplished and in thermostatic drying chamber, dries, and 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 heat-processed 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 temperature rise rates; After 1400 ℃ 3～5 ℃/min; Sintering atmosphere is Ar, and sintered compact is handled through follow-up finishing, obtains SiC
p/ Si
3N
4The composite ceramics part.
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| CN2010102305735A CN101913878B (en) | 2010-07-19 | 2010-07-19 | Method for preparing silicon carbide particle-reinforced silicon nitride composite ceramic parts |
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| CN101913878B true CN101913878B (en) | 2012-06-27 |
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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 |
| CN102992778B (en) * | 2012-09-11 | 2014-06-25 | 廖文宏 | Precision ceramic with jade texture and preparation method thereof |
| CN104045350B (en) * | 2013-03-11 | 2015-06-17 | 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 |
| EP3036195B1 (en) | 2013-08-19 | 2020-07-01 | University Of Utah Research Foundation | Producing a titanium product |
| WO2015175726A1 (en) | 2014-05-13 | 2015-11-19 | University Of Utah Research Foundation | Production of substantially spherical metal powers |
| CN104258741B (en) * | 2014-09-24 | 2017-09-22 | 中山市瑞邦红利塑料工业有限公司 | A kind of ceramic film support with filtering function and its preparation method and application |
| 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 |
| 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 |
| CN108439995B (en) * | 2018-05-24 | 2020-12-22 | 中南大学 | Complex phase ceramic and preparation method thereof |
| 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 |
| US10907239B1 (en) | 2020-03-16 | 2021-02-02 | University Of Utah Research Foundation | Methods of producing a titanium alloy product |
| CN113548903B (en) * | 2021-08-27 | 2022-12-23 | 广东工业大学 | Silicon carbide reinforced silicon nitride ceramic and preparation method thereof |
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| CN101037336A (en) * | 2007-04-29 | 2007-09-19 | 北京科技大学 | Method for preparing carborundum whisker reinforced carborundum composite material element |
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| US6350713B1 (en) * | 1998-11-24 | 2002-02-26 | Dow Corning Corporation | Ceramic matrix composites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101037336A (en) * | 2007-04-29 | 2007-09-19 | 北京科技大学 | Method for preparing carborundum whisker reinforced carborundum composite material element |
Non-Patent Citations (1)
| Title |
|---|
| 张勇等.SPS工艺制备SiCp/Si3N4复相陶瓷及其力学性能的研究.《粉末冶金工业》.2008,第18卷(第2期),第1-5页. * |
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