CN104326752A - Low-temperature normal-pressure liquid-phase sintering preparation method of SiC ceramic - Google Patents
Low-temperature normal-pressure liquid-phase sintering preparation method of SiC ceramic Download PDFInfo
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- CN104326752A CN104326752A CN201410508580.5A CN201410508580A CN104326752A CN 104326752 A CN104326752 A CN 104326752A CN 201410508580 A CN201410508580 A CN 201410508580A CN 104326752 A CN104326752 A CN 104326752A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
The invention relates to a low-temperature normal-pressure liquid-phase sintering preparation method of SiC ceramic. (1): at 1450-1650 DEG C, an Al2O3-Y2O3-CaO oxide system sintering assistant is added and a reaction between a SiO2 oxidation layer on the surface of SiC powder is carried out to form a liquid phase in a certain viscosity for promoting sintering densification of the SiC ceramic, thereby obtaining high-strength SiC ceramic. (2) Without a pre-oxidation process during oxidation of the SiC powder, the oxidation of the SiC powder is carried out directly during the sintering process of the SiC ceramic, wherein an oxidation degree of the SiC is controlled by control of a pre-embedded powder and a sintering temperature. (3) In the method, sintering of the SiC ceramic is carried out in air. Compared with a sintering furnace with a protective atmosphere, a common box-typed sintering furnace is greatly reduced in device cost. In addition, because the protective atmosphere is unnecessary, the sintering temperature of the SiC ceramic is low so that a sintering efficiency is increased and preparation cost of the SiC ceramic is reduced. The low-temperature normal-pressure liquid-phase sintering preparation method of the SiC ceramic includes following steps: material blending, material mixing, moulding, glue arranging and powder embedding and sintering.
Description
technical field:
The technology of the present invention relates to ceramic production technology, particularly a kind of low-temperature atmosphere-pressure sintering technology of SiC ceramic.The invention provides a kind of new technical scheme, the program contributes to the requirement of the agglomerating plant reduced when preparing SiC ceramic, SiC raw material powder need not preoxidation, and obtain high performance SiC ceramic goods at a lower temperature, reduces the energy consumption in SiC ceramic production process and production cost.
background technology:
SiC ceramic material has that hot strength is large, high-temperature oxidation resistance is strong, abrasion resistance properties is good, thermal conductivity is large, the premium properties of resistance to chemical attack, be applied in the fields such as automobile, chemical industry, mechanical seal, space flight and aviation, as engine component, mechanical sealing member and corrosion barrier etc. increasingly extensively.In addition, the application of SiC ceramic material in the field such as power electronics, communication is also shown up prominently, and market is progressively expanded.
Application in SiC ceramic material different field has different requirements to its performance, and preparation method is thus also different.The preparation technology of SiC ceramic can be divided into several classes such as reaction sintering, normal pressure-sintered and hot pressed sintering.According to the state of sintering aid in sintering process, normal pressure-sinteredly solid state sintering and liquid phase sintering can be divided into again.Consider to the requirement of equipment and production cost, normal pressure lqiuid phase sintering method in sintering process, forms eutectic liquid phase by sintering aid, Accelerative mass transfer process, acceleration of sintering densification, thus while reducing sintering temperature greatly, maintain higher mechanical property.The room-temperature mechanical property of normal pressure LIQUID PHASE SINTERED SiC CERAMICS material is general all apparently higher than the SiC ceramic material adopting normal pressure solid-phase sintering process to prepare at a higher temperature, and therefore normal pressure lqiuid phase sintering method has very large advantage in prepared by SiC ceramic material.
According to the document delivered, the sintering temperature that normal pressure LIQUID PHASE SINTERED SiC CERAMICS is is at 1750-1900 DEG C, though low compared with the sintering temperature of more than 2000 DEG C of normal pressure solid state sintering, also still very high, high to the requirement of equipment.Further, normal pressure LIQUID PHASE SINTERED SiC CERAMICS generally also needs the protective atmospheres such as logical nitrogen or argon gas, to stop SiC powder and the sintering aid vigorous reaction when high temperature, adds the complicacy of sintering process, too increases manufacturing cost.Therefore, select lower sintering temperature, realize SiC ceramic without the sintering under atmosphere protection, to reduce production cost as far as possible, be the target that SiC ceramic prepares industry pursuit always.Zhu Yumei etc. [Zhu Yumei, Li Zhihong. ceramic journal, 1999,20 (2): 99-103] surface of SiC preoxidation formation SiO is proposed
2zone of oxidation, and then 1580 DEG C of sintering prepare SiC ceramic in nitrogen atmosphere.The SiC ceramic material density adopting the method to prepare is low, and three-point bending strength only has 120 MPa.Long Zhizhou etc. [Long Zhizhou, Han Minfang. material engineering, 2008,6:48-52] attempt sintered sic complex phase ceramic in atmosphere, but SiC content wherein only has 30-50wt% at most, and density is poor, performance is also lower, does not reach the requirement of industrial applications.Jin Zhihao etc. [Wang Qian, Jin Zhihao. Southwest Jiaotong University's journal, 2006,36 (9): 971-974] propose to adopt SiO
2, Al
2o
3, the oxide addition such as MgO, CaO 1530-1600 DEG C of sintering preparation SiC ceramic material in air atmosphere, but the three-point bending resistance intensity of this material, only has 42 MPa.By the paper delivered and published patent retrieval, low-temperature sintering SiC ceramic material compactness is lower in air atmosphere, and bending strength is not high yet, cannot meet the requirement that SiC uses as structural part, is mostly used as fire-resistant (mill) material.Up till now, there is not yet the bibliographical information at structural parts such as air atmosphere low temperature sintering SiC ceramic mechanical sealing members.In addition, sintered sic pottery, there will be the oxidation of SiC unavoidably in atmosphere, and along with the rising of temperature, degree of oxidation also can aggravate.Excessive oxidation, reduces the amount of principal crystalline phase in SiC ceramic, exacerbates the reaction of SiC and sintering aid, and the structure of SiC ceramic and performance also can be subject to larger disadvantageous effect.Therefore, the control of SiC oxidation is crucial, adopts suitable powder to bury firing technique, can alleviate SiC oxidation, but effective SiC ceramic powder embedded sintering technique also rarely has report.
For the deficiency of above-mentioned existing normal pressure-sintered SiC ceramic technology of preparing, the present invention proposes the low-temperature atmosphere-pressure liquid phase sintering preparation method of a new high strength SiC ceramic, can realize in atmosphere, prepare the SiC ceramic material used as structural part under sintering temperature and low.
Summary of the invention
Technical problem to be solved by this invention be to provide a kind of production process simple, produce that equipment is simple and easy, the oxide compound of the high and low cost of production efficiency is in conjunction with the preparation method of SiC ceramic and goods.The present invention adopts Al
2o
3-Y
2o
3-CaO oxide sintering aid, and be placed in air and sinter, the SiO that sintering aid and surface of SiC are formed
2zone of oxidation reaction forms polynary sintering aid system, reduces its liquid phase forming temperature, promotes the densification of SiC ceramic at a lower temperature, the SiC ceramic material that processability is excellent.
The scheme that technical solution problem of the present invention adopts is:
The present invention relates to a kind of low-temperature atmosphere-pressure liquid phase sintering preparation method of SiC ceramic, it is characterized in that: SiC material powder and oxide sintering aid powder are made slurry by the method after wet mixing; Slurry, at 100-120 DEG C of dry 3-4 h, crosses 80-100 mesh sieve after pulverizing, after adding binder, and homogeneous heating in 90-100 DEG C of water-bath, every 2-3 min stirs once, altogether stirring in water bath 30-60 min; To be cooled after room temperature after 80-100 mesh sieve, powder mix adopts unidirectional pressing mode to be shaped; At 580-600 DEG C of insulation 20-30 min binder removal; Last powder embedded sintering, furnace cooling obtains high strength SiC ceramic sample.
The low-temperature atmosphere-pressure liquid phase sintering preparation method of described a kind of SiC ceramic, is characterized in that, two kinds of SiC powders of described SiC material powder to be median size be 3.5-7 μm and 0.5 μm are obtained by mixing, and the mass ratio of two kinds of powders is 1-4:1.
The low-temperature atmosphere-pressure liquid phase sintering preparation method of described a kind of SiC ceramic, is characterized in that, described oxide sintering aid is Al
2o
3-Y
2o
3-CaO system.
The low-temperature atmosphere-pressure liquid phase sintering preparation method of described a kind of SiC ceramic, is characterized in that, in described SiC material powder and oxide sintering aid powder, both weight percents are respectively 60-90 wt% and 40-10 wt%.
The low-temperature atmosphere-pressure liquid phase sintering preparation method of described a kind of SiC ceramic, it is characterized in that, described is make water base paste mixture by SiC material powder and oxide sintering aid powder blending means, adopts ball milling hybrid mode, ball-milling medium is high-purity agate ball, and ball grinder material is Al
2o
3ceramic material: ball: water three part by weight is that 1:2-3:0.35 is obtained by mixing, ball milling parameter is rotating speed 300-360 r/min, Ball-milling Time 6-12 h.
The low-temperature atmosphere-pressure liquid phase sintering preparation method of described a kind of SiC ceramic, is characterized in that, described binder is solid paraffin, and its addition is the 3-8% of SiC and oxygen oxide sintering aid powder gross weight.
The low-temperature atmosphere-pressure liquid phase sintering preparation method of described a kind of SiC ceramic, is characterized in that, described press forming pressure is 270-400 MPa, dwell time 30-60 s.
The low-temperature atmosphere-pressure liquid phase sintering preparation method of described a kind of SiC ceramic, is characterized in that, described buried powder covers by the powder mix of SiC powder, Graphite Powder 99 and oxidate powder on SiC biscuit.
The low-temperature atmosphere-pressure liquid phase sintering preparation method of described a kind of SiC ceramic, it is characterized in that, described sintering sinters in atmosphere, sintering process is: less than 1000 DEG C, temperature rise rate: 4-6 DEG C/min, temperature rise rate more than 1000 DEG C: 2-3 DEG C/min, sintering temperature 1450-1650 DEG C, soaking time is 30-90 min, after sintering, and sample furnace cooling.
Compared with the prior art, advantage applies of the present invention exists:
The present invention need not adopt surface of SiC pre-oxidation process; also need not sinter under atmosphere protection; surface of SiC zone of oxidation is formed in SiC ceramic unprotect atmosphere sintering process; and react form low melting point liquid phase with the oxide compound sintering agent added; promote SiC ceramic sintering; reduce operation, reduce manufacturing cost.
Accompanying drawing explanation
Fig. 1 is the microstructure photo after the embodiment of the present invention 1 sinters.
Fig. 2 is the microstructure photo after the embodiment of the present invention 2 sinters.
Embodiment
embodiment 1
To be averaged particle diameter be SiC powder 15.75g, the median size of 3.5 μm is SiC powder 5.25g, CaO powder 3.33g, Al of 0.5 μm
2o
3powder 3.96g, Y
2o
3powder 1.71g, high-purity agate ball ball 75g, distilled water 10.5g, be placed in Al
2o
3in the ball grinder of ceramic material, with the speed ball milling 10h of 360r/min on planetary ball mill, make slurry.By slurry at 100 DEG C of thermostatic drying chamber inner drying 4h, after grinding is broken, cross 80 mesh sieves, in the powder after sieving, add 1.5g solid paraffin, homogeneous heating in 100 DEG C of water-baths, stir once every 3min, be total to stirring in water bath 40min; To be cooled after room temperature after 80 mesh sieves, powder mix adopts unidirectional pressing mode, and compacting pressure is 400MPa, pressurize 60s, is pressed into 40mm × 4.5mm × 3.5mm long strip shape sample; By this sample 580 DEG C of insulation 30 min binder removals in draft glue discharging furnace, by the sample graphite after binder removal and Y
2o
3(15wt%)+Al
2o
3(25wt%) powder mix of+SiC (60wt%) is covered buried powder and is placed in chamber type sintering stove and sinters, less than 1000 DEG C temperature rise rates, 5 DEG C/min, more than 1000 DEG C temperature rise rates, 2.5 DEG C/min, after reaching sintering temperature 1600 DEG C, insulation 60min, then furnace cooling.Specimen surface is polished, tests its void content and three-point bending resistance intensity.
The performance of the SiC ceramic of preparation: apparent porosity is 0.18%, three-point bending resistance intensity 360MPa.
embodiment 2
The preparation method of the present embodiment is with embodiment 1, and different oxide sintering aid total contents is 20 wt%, and sintering temperature is 1575 DEG C.
The performance of the SiC ceramic of preparation: apparent porosity is 0.21%, three-point bending resistance intensity 330 MPa.
Claims (9)
1. the present invention relates to a kind of low-temperature atmosphere-pressure liquid phase sintering preparation method of SiC ceramic, it is characterized in that: SiC material powder and oxide sintering aid powder are made slurry by the method after wet mixing; Slurry, at 100-120 DEG C of dry 3-4 h, crosses 80-100 mesh sieve after pulverizing, after adding binder, and homogeneous heating in 90-100 DEG C of water-bath, every 2-3 min stirs once, altogether stirring in water bath 30-60 min; To be cooled after room temperature after 80-100 mesh sieve, powder mix adopts unidirectional pressing mode to be shaped; At 580-600 DEG C of insulation 20-30 min binder removal; Last powder embedded sintering, furnace cooling obtains high strength SiC ceramic sample.
2. the low-temperature atmosphere-pressure liquid phase sintering preparation method of a kind of SiC ceramic according to claim 1, it is characterized in that, two kinds of SiC powders of described SiC material powder to be median size be 3.5-7 μm and 0.5 μm are obtained by mixing, and the mass ratio of two kinds of powders is 1-4:1.
3. the low-temperature atmosphere-pressure liquid phase sintering preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, described oxide sintering aid is Al
2o
3-Y
2o
3-CaO system.
4. the low-temperature atmosphere-pressure liquid phase sintering preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, in described SiC material powder and oxide sintering aid powder, both weight percents are respectively 60-90 wt% and 40-10 wt%.
5. the low-temperature atmosphere-pressure liquid phase sintering preparation method of a kind of SiC ceramic according to claim 1, it is characterized in that, described is make water base paste mixture by SiC material powder and oxide sintering aid powder blending means, adopt ball milling hybrid mode, ball-milling medium is high-purity agate ball, and ball grinder material is Al
2o
3ceramic material: ball: water three part by weight is that 1:2-3:0.35 is obtained by mixing, ball milling parameter is rotating speed 300-360 r/min, Ball-milling Time 6-12 h.
6. the low-temperature atmosphere-pressure liquid phase sintering preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, described binder is solid paraffin, and its addition is the 3-8% of SiC and oxygen oxide sintering aid powder gross weight.
7. the low-temperature atmosphere-pressure liquid phase sintering preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, described press forming pressure is 270-400 MPa, dwell time 30-60 s.
8. the low-temperature atmosphere-pressure liquid phase sintering preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, described buried powder covers by the powder mix of SiC powder, Graphite Powder 99 and oxidate powder on SiC biscuit.
9. the low-temperature atmosphere-pressure liquid phase sintering preparation method of a kind of SiC ceramic according to claim 1, it is characterized in that, described sintering sinters in atmosphere, sintering process is: less than 1000 DEG C, temperature rise rate: 4-6 DEG C/min, temperature rise rate more than 1000 DEG C: 2-3 DEG C/min, sintering temperature 1450-1650 DEG C, soaking time is 30-90 min, after sintering, and sample furnace cooling.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104452080A (en) * | 2014-12-18 | 2015-03-25 | 鑫立达机器（常熟）有限公司 | High-stable frame |
| CN105461313A (en) * | 2015-11-19 | 2016-04-06 | 湖南航天诚远精密机械有限公司 | A sintering method of a silicon carbide structural member skeleton |
| CN105801124A (en) * | 2016-03-11 | 2016-07-27 | 天津大学 | Silicon carbide ceramic composite microwave absorption material with structure-function integration |
| CN106673660A (en) * | 2016-12-09 | 2017-05-17 | 中国科学院上海硅酸盐研究所 | Liquid-phase sintered SiC non-linear resistance ceramic and preparation method thereof |
| CN116675538A (en) * | 2023-05-30 | 2023-09-01 | 中国科学院上海硅酸盐研究所 | Method for preparing SiC ceramic by combining selective laser 3D printing/precursor dipping pyrolysis/liquid phase sintering |
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| CN101613209A (en) * | 2009-07-16 | 2009-12-30 | 中国人民解放军国防科学技术大学 | C fThe high-temperature oxidation resistant coating of/SiC matrix material, coating slurry and preparation method thereof |
| CN102807391A (en) * | 2012-08-29 | 2012-12-05 | 哈尔滨工业大学 | Method for preparing porous silicon carbide ceramic |
| CN104291825A (en) * | 2014-09-04 | 2015-01-21 | 合肥工业大学 | Preparation method for low temperature sintering of SiC ceramic with synthetic celsian as sintering aid |
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| JPH04104944A (en) * | 1990-08-21 | 1992-04-07 | Nitsukatoo:Kk | Al2o3-sic-zro2 composite sinter |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104452080A (en) * | 2014-12-18 | 2015-03-25 | 鑫立达机器（常熟）有限公司 | High-stable frame |
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| CN105461313A (en) * | 2015-11-19 | 2016-04-06 | 湖南航天诚远精密机械有限公司 | A sintering method of a silicon carbide structural member skeleton |
| CN105801124A (en) * | 2016-03-11 | 2016-07-27 | 天津大学 | Silicon carbide ceramic composite microwave absorption material with structure-function integration |
| CN105801124B (en) * | 2016-03-11 | 2018-06-26 | 天津大学 | A kind of silicon carbide ceramics composite microwave absorbing material of structure-function integration |
| CN106673660A (en) * | 2016-12-09 | 2017-05-17 | 中国科学院上海硅酸盐研究所 | Liquid-phase sintered SiC non-linear resistance ceramic and preparation method thereof |
| CN106673660B (en) * | 2016-12-09 | 2019-12-17 | 中国科学院上海硅酸盐研究所 | Liquid phase sintered SiC nonlinear resistance ceramic and preparation method thereof |
| CN116675538A (en) * | 2023-05-30 | 2023-09-01 | 中国科学院上海硅酸盐研究所 | Method for preparing SiC ceramic by combining selective laser 3D printing/precursor dipping pyrolysis/liquid phase sintering |
| CN116675538B (en) * | 2023-05-30 | 2023-12-22 | 中国科学院上海硅酸盐研究所 | Method for preparing SiC ceramic by combining selective laser 3D printing/precursor dipping pyrolysis/liquid phase sintering |
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