CN1442392A - Preparation method of silicon carbide porous ceramic using yeast powder as pore forming agent - Google Patents
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Abstract
A process using yeast powder as pore-forming agent for preparing porous silicon carbide ceramics includes such steps as proportionally mixing SiC, Al2O3, Suzhou clay, bentone and alcohol for 6-24 hr to obtain slurry, sieving the yeast powder by 6 gradient classes, mixing with said slurry, backing, die pressing to form under 20-100 MPa, sintering at 1100-1350 deg.C, and holding the temp for 1-5 hr. Its advantages are easy control, uniform pore diameters, high porosity (45-65%) and low volume density (0.95-1.5 g/cu.cm).
Description
Technical field
The present invention relates to a kind of is the carborundum porous ceramics preparation method of pore-forming material with the yeast powder, belongs to the porous ceramics field.
Background technology
As everyone knows, porous ceramics is to be a kind of critical function material of principal phase with the pore, comprises two kinds of perforate and closed pores.Perforate pottery duct is inner to produce all physical influences with outer surface because of fluid flows through, thereby produces purification, filtration, effect such as even.For example: utilize the even perviousness of porous ceramics, can make various strainers, tripping device etc.; Utilize the specific surface area of porous ceramics prosperity, can make porous electrode, support of the catalyst, heat exchanger etc.; Utilize high temperature resistant, the corrosion resistance characteristic of porous ceramics, but the preparing high-temp gas purifier, diesel emission solid particle filter, filter for molten metal.In a word, porous ceramics is widely used in industries such as metallurgy, chemical industry, the energy, environmental protection, biology.Its pore structure is depended in the performance of porous ceramics and application, and pore structure comprises aperture, pore size distribution, porosity, hole shape etc.Wherein aperture and pore size distribution are the porous ceramics important parameters.The porous ceramics performance can be improved in the control aperture, thereby optimizes intensity and void content, both can prolong porous ceramics work-ing life, can improve the porous ceramics result of use again.According to the purpose of using with to the requirement of material property, successfully develop multiple preparation technology, as adding pore-forming material method, foaming, organic foam body impregnation technology, sol gel process etc.The pore-forming material method is a kind of important process of preparation porous ceramics.This technology can prepare complex-shaped goods, can produce the porous article of various air hole structures.This technology is by selecting pore-forming material for use, in base substrate, occupy certain space, pore-forming material leaves matrix and forms pore and come producing porous ceramic behind the sintering, or selects the pore-forming material that can not get rid of in the matrix sintering for use, burns till back water, acid or alkaline solution and leaches pore-forming material and form porous ceramics.People such as Lyckfeldt (O.Lyckfeldt and J.M.F.Ferreira, Journal of the EuropeanCeramic Society, 18,1998,131-140) prepared Al as pore-forming material with starch
2O
3Porous ceramics, porosity are 23～70%, and the aperture is mainly 10-80 μ m, but the range of aperture size of this method preparation is narrower.People such as Tatsuki (Jian-Feng Yang, Guo-Jun Zhang, Nanoki Kondo, Tatsuki Ohji, Acta Materialia 50,2002 4831-4840) prepares Si with carbon dust
3N
4Porous ceramics is at Si
3N
4The surface generates SiC nano-powder and SiO
2Si behind the sintering
3N
4The porous ceramics void content is at 50-60%, and linear shrinkage has only 2～3%, aperture size 0.1～1 μ m, though can prepare the wider porous ceramics of range of aperture size, the porous ceramics size of preparation is smaller.Again, the Y of Mitusui Engineering and Shipbuilding Co.Ltd (Jpn.Kokai Tokkyo Koho, JP59,156,952) with 60%
2O
3Stable ZrO
2With 40% Y
2O
3Mix, behind 1150 ℃ of sintering, dipping is 5 hours in the hot hydrochloric acid of 30wt%, has made porous ZrO
2Pottery, but cost is too high, is not suitable for industrial production.
Summary of the invention
The objective of the invention is to seek a kind of novel pore-forming material (yeast powder), prepare low cost, aperture size and be about 50-500 μ m, a plurality of gradient porous ceramics that size range is wider.The objective of the invention is to implement by following technological process:
(1) the present invention is to cross 30-40 order (mesh diameter 600-450 μ m), 40-50 order (mesh diameter 450-355 μ m), 50-60 order (mesh diameter 355-280 μ m), 60-75 order (mesh diameter 280-200 μ m), 75-120 order (mesh diameter 200-125 μ m), the yeast powder of the sieve of 120-300 order (mesh diameter 125-50 μ m) is as pore-forming material, forms pore thereby constantly get rid of in sintering process, prepares porous ceramics.Pore size is relevant with the yeast powder particle diameter, because yeast powder is soluble in water, is insoluble to ethanol, therefore in order to prevent the yeast powder dissolving, particle diameter is diminished, and does not have the due effect of pore-forming material, so select for use ethanol as dispersion medium.
(2) concrete technology is: at first press SiC powder: Al
2O
3: Suzhou soil: wilkinite=1: 0.05-0.3: 0.06-0.2: 0.03-0.1 (quality), ethanol adds as dispersion medium by material powder total mass 25%～55%, uses Al
2O
3Ball is expected powder: Al as mill ball
2O
3Ball=1: 2 (quality) mixed 6～24 hours; Secondly, with the 30-40 order, 40-50 order, 50-60 order, the 60-75 order, the 75-120 order, 120-300 purpose sieve is divided into 6 gradients, by 40～60% of material opaque amount yeast powder joined mixing in the slurry, after the oven dry, dry-pressing formed with 20-100Mpa pressure on sheet-leveling machine; Sintering under atmospheric air atmosphere at last, sintering temperature be from 1100～1350 ℃, soaking time 1～5 hour.The characteristics of this technology except yeast powder than-as the optional size range of pore-forming material wide, the carborundum porous ceramics pore size distribution that makes is more even.Porosity between 45～65%, volume density 0.95～1.50g/cm
3Between, bending strength is the highest can be greater than 25mpa.
(3) by screening, yeast powder can be divided into a plurality of size gradients.Fig. 1, Fig. 2, Fig. 3, Fig. 4 were the 30-40 mesh sieves, the 40-50 mesh sieve, the 50-60 mesh sieve, the yeast powder optical microphotograph pattern and the size distribution of 60-75 mesh sieve, the yeast powder particle diameter of as can be seen from the figure crossing the 30-40 mesh sieve mainly is distributed between the 550-700 μ m, the yeast powder particle diameter of crossing the 40-50 mesh sieve mainly is distributed between the 350-500 μ m, and the yeast powder particle diameter of crossing the 50-60 mesh sieve mainly is distributed between the 250-400 μ m, and the yeast powder particle diameter of crossing the 60-75 mesh sieve mainly is distributed between the 150-300 μ m.Particle size is to characterize with equivalent diameter.Fig. 5, Fig. 6 were the 75-120 mesh sieves, cross the yeast powder optical microphotograph pattern and the size distribution of 120-300 mesh sieve, the yeast powder particle diameter of crossing the 75-120 mesh sieve mainly is distributed between the 100-200 μ m, and the yeast powder particle diameter of crossing the 120-300 mesh sieve mainly is distributed between the 50-150 μ m.
The pore-forming material size is divided into the different size gradient after sieving, and regulates by screening as can be seen from Figure 11-16 that the pore size of porous ceramics is feasible behind the sintering.Carborundum porous ceramics aperture among Figure 11 mainly is distributed in 400-550 μ m, carborundum porous ceramics aperture among Figure 12 mainly is distributed in 350-450 μ m, carborundum porous ceramics aperture among Figure 13 mainly is distributed in 280-350 μ m, carborundum porous ceramics aperture among Figure 14 mainly is distributed in 180-250 μ m, carborundum porous ceramics aperture among Figure 15 mainly is distributed in-100-180 μ m, and the carborundum porous ceramics aperture among Figure 16 mainly is distributed in 50-120 μ m.In a word, along with reducing of sieve mesh size, the size of isolating yeast powder also reduces, and the porous ceramics aperture of preparation presents certain gradient and reduces trend.
In sum, the carborundum porous ceramics that with the yeast powder is pore-forming material prepares provided by the invention has the following advantages:
(1) yeast powder has certain wear resistance, like this with the mixing raw materials process in can keep granularity.But yeast powder is not again that extremely difficulty grinds, and can obtain the yeast powder of different grain size size range so again, thereby the porous ceramics pore diameter range of preparation is wide, and aperture ratio is more even.
(2) yeast powder low price can be realized low cost, large-scale production application.
(3) the yeast powder temperature of decomposing fully is than general pore-forming material height, the sealing when this helps to reduce afterwards high temperature sintering of hole.
Description of drawings
1-1 was the optical microphotograph pattern of the yeast powder of 30-40 mesh sieve among Fig. 1, and 1-2 is relevant particle size distribution figure, and X-coordinate is particle size (equivalent diameter) among the figure, and unit is mm; Ordinate zou is a granule number.
2-1 was the optical microphotograph pattern of the yeast powder of 40-50 mesh sieve among Fig. 2, and 2-2 is relevant particle size distribution figure, and X-coordinate is particle size (equivalent diameter) among the figure, and unit is mm; Ordinate zou is a granule number.
3-1 was the optical microphotograph pattern of the yeast powder of 50-60 mesh sieve among Fig. 3, and 3-2 is relevant particle size distribution figure, and X-coordinate is particle size (equivalent diameter) among the figure, and unit is mm; Ordinate zou is a granule number.
4-1 was the optical microphotograph pattern of the yeast powder of 60-75 mesh sieve among Fig. 4, and 4-2 is relevant particle size distribution figure, and X-coordinate is particle size (equivalent diameter) among the figure, and unit is mm; Ordinate zou is a granule number.
5-1 was that the yeast powder of 75-120 mesh sieve amplifies 13 times optical microphotograph pattern among Fig. 5,5-3 was that the yeast powder of 75-120 mesh sieve amplifies 80 times optical microphotograph pattern, 5-2 is relevant particle size distribution figure, and X-coordinate is particle size (equivalent diameter) among the figure, and unit is mm; Ordinate zou is a granule number.
6-1 was that the yeast powder of 120-300 mesh sieve amplifies 13 times optical microphotograph pattern among Fig. 6,6-3 was that the yeast powder of 120-300 mesh sieve amplifies 80 times optical microphotograph pattern, 6-2 is relevant particle size distribution figure, and X-coordinate is particle size (equivalent diameter) among the figure, and unit is mm; Ordinate zou is a granule number.
7-1 is the SEM photo of yeast powder granule-morphology among Fig. 7, and 7-2 is the SEM photo of yeast powder cross-section morphology.
Fig. 8 is the thermogravimetric curve of yeast powder, and in the time of 900 ℃, yeast powder is substantially no longer weightless.X-coordinate is a temperature among the figure, unit ℃; Ordinate zou is a weight percentage.
Fig. 9 is a slurry dry powder TG-DSC curve, at 217.8 ℃ an endotherm(ic)peak is arranged as can be known by the DSC curve, at 1176.1 ℃, 1298.1 ℃, 1346.1 ℃ exothermic peak is arranged; Shown in the TG curve, temperature during less than 1176.1 ℃ weight reduce, when temperature during greater than 1176.1 ℃, because the SiC oxidation, weight increases.X-coordinate is a temperature among the figure, unit ℃; Ordinate zou is two coordinates, and the left side is DSC, and unit is mW/mg, and the right is a weight percentage, the wt% of unit.Reaction in temperature-rise period is as follows: 1176.1 ℃ are risen:
Or
1298.1 ℃ rise:
Figure 10 is to be pore-forming material with the yeast powder among Fig. 2, at 1300 ℃ of following sintering, is incubated 3 hours porous ceramics hole breaking of muscle and tendon face shape appearance figure.1,2,3,4 places are analyzed as can be known by EDS among the figure, and crystalline phase is respectively aluminum oxide, silicon carbide, mullite, silicon-dioxide.
11-1 is to be the cross-section morphology SEM photo of the carborundum porous ceramics of pore-forming material preparation with the yeast powder among Fig. 1 among Figure 11, and 11-2 is the graph of pore diameter distribution of the porous ceramics made, and X-coordinate is an aperture size, and unit is μ m; Ordinate zou is a percent by volume, and 11-3 is 1300 ℃ of sintering, is incubated 1 hour carborundum porous ceramics XRD analysis, and crystalline phase is SiC, Al as seen from the figure
2O
3, mullite, SiO
2, X-coordinate is 2-Theta, ordinate zou is an intensity.
12-1 is to be the cross-section morphology SEM photo of the carborundum porous ceramics of pore-forming material preparation with the yeast powder among Fig. 2 among Figure 12, and 12-2 is the graph of pore diameter distribution of the porous ceramics made, and X-coordinate is an aperture size, and unit is μ m; Ordinate zou is a percent by volume, and 12-3 is 1300 ℃ of sintering, is incubated 3 hours carborundum porous ceramics XRD analysis, and crystalline phase is SiC, Al as seen from the figure
2O
3, mullite, SiO
2, X-coordinate is 2-Theta, ordinate zou is an intensity.
13-1 is to be the cross-section morphology SEM photo of the carborundum porous ceramics of pore-forming material preparation with the yeast powder among Fig. 3 among Figure 13, and 13-2 is the graph of pore diameter distribution of the porous ceramics made, and X-coordinate is an aperture size, and unit is μ m; Ordinate zou is a percent by volume, and 13-3 is 1300 ℃ of sintering, is incubated 5 hours carborundum porous ceramics XRD analysis, and crystalline phase is SiC, Al as seen from the figure
2O
3, mullite, SiO
2, X-coordinate is 2-Theta, ordinate zou is an intensity.
14-1 is to be the cross-section morphology SEM photo of the carborundum porous ceramics of pore-forming material preparation with the yeast powder among Fig. 4 among Figure 14, and 14-2 is the graph of pore diameter distribution of the porous ceramics made, and X-coordinate is an aperture size, and unit is μ m; Ordinate zou is a percent by volume, and 14-3 is 1300 ℃ of sintering, is incubated 3 hours carborundum porous ceramics XRD analysis, and crystalline phase is SiC, Al as seen from the figure
2O
3, mullite, SiO
2, X-coordinate is 2-Theta, ordinate zou is an intensity.
15-1 is to be the cross-section morphology SEM photo of the carborundum porous ceramics of pore-forming material preparation with the yeast powder among Fig. 5 among Figure 15, and 15-2 is the graph of pore diameter distribution of the porous ceramics made, and X-coordinate is an aperture size, and unit is μ m; Ordinate zou is a percent by volume, and 15-3 is 1200 ℃ of sintering, is incubated 3 hours carborundum porous ceramics XRD analysis, and crystalline phase is SiC, Al as seen from the figure
2O
3, SiO
2, X-coordinate is 2-Theta, ordinate zou is an intensity.
16-1 is to be the cross-section morphology SEM photo of the carborundum porous ceramics of pore-forming material preparation with the yeast powder among Fig. 6 among Figure 16, and 16-2 is the graph of pore diameter distribution of the porous ceramics made, and X-coordinate is an aperture size, and unit is μ m; Ordinate zou is a percent by volume, and 16-3 is 1100 ℃ of sintering, is incubated 3 hours carborundum porous ceramics XRD analysis, and crystalline phase is SiC, Al as seen from the figure
2O
3, X-coordinate is 2-Theta, ordinate zou is an intensity.
Embodiment
Further specify outstanding feature of the present invention and obvious improvement below by specific embodiment, but the present invention is confined to embodiment by no means.Concrete implementation of processes example 1～6 is as shown in the table,
| Embodiment | SiC | Al 2O 3 | Suzhou soil | Wilkinite | Ethanol | Alumina balls | The order number of sieve | Pore-forming material and material powder mass ratio | Firing temperature | Soaking |
| 1 | 56 | 8 | 20 | 10 | 40 | 190 | 30-40 | 60％ | 1300 | 1 |
| 2 | 56 | 4 | 14 | 6 | 40 | 160 | 40-50 | 60％ | 1300 | 3 |
| 3 | 56 | 8 | 16 | 8 | 40 | 180 | 50-60 | 60％ | 1300 | 5 |
| 4 | 56 | 12 | 14 | 6 | 25 | 180 | 60-75 | 40％ | 1300 | 3 |
| 5 | 56 | 20 | 10 | 4 | 55 | 180 | 75-120 | 50％ | 1200 | 3 |
| 6 | 56 | 32 | 6 | 2 | 40 | 190 | 120-300 | 60％ | 1100 | 3 |
The performance of the carborundum porous ceramics for preparing in the foregoing description is as shown in the table:
| Embodiment | Porosity | Volume density/g/cm 3 | Bending strength/ |
| 1 | 62.6％ | 0.97 | 11.5±1.2 |
| 2 | 61.4％ | 1.10 | 16.8±1.2 |
| 3 | 57.3％ | 1.12 | 18.1±0.9 |
| 4 | 46.9％ | 1.44 | 25.5±1.3 |
| 5 | 60.0％ | 1.15 | 16.2±1.2 |
| 6 | 58.5％ | 1.23 | 16.3±1.1 |
Shown in embodiment 2, SiC, Al
2O
3, Suzhou soil, wilkinite, ethanol batch mixes 12 hours adds the yeast powder that sieves with 40-50 mesh sieve, and yeast powder is 60% with the mass ratio of material powder, remix, the gained slurry is dried in baking oven, crosses behind 20 mesh sieves on vulcanizing press with the 50MPa pressure forming.
Sintering under atmospheric air atmosphere, 1 ℃/minute of temperature rise rate below 900 ℃ is warming up to sintering temperature with 5 ℃/minute speed then.1300 ℃ of firing temperatures, soaking time 3 hours.Goods volume density 1.10g/cm
3, porosity 61.4%, folding strength 16.8 ± 1.2MPa.
Claims (5)
1, a kind of is the preparation method of the carborundum porous ceramics of pore-forming material with the yeast powder, comprising: proportioning, moulding, sintering process is characterized in that:
(1) presses SiC powder: Al
2O
3: Suzhou soil: wilkinite=1: 0.05-0.3: 0.06-0.2: 0.03-0.1 (quality) ratio batching;
(2) as the ethanol of dispersion medium, add, use Al by material powder total mass 25%～55%
2O
3Ball is expected powder: Al as mill ball
2O
3Ball=1: 2 (quality) mixed 6～24 hours;
(3) the pore-forming material yeast powder is six gradients with 30 orders～300 purposes screening, joins mixing in the slurry, oven dry, dry-pressing formed by 40～60% of material opaque amount;
(4) sintering under atmospheric air atmosphere, sintering temperature is 1100～1350 ℃, soaking time 1～5 hour.
2, described by claim 1 is the preparation method of the carborundum porous ceramics of pore-forming material with the yeast powder, it is characterized in that six gradients that described 30 orders～300 mesh sieves divide are 30～40 orders, 40～50 orders, 50～60 orders, 60～75 orders, 75～120 orders and 120～300 orders; Corresponding mesh diameter is respectively 600～450 μ m, 450～355 μ m, 355～280 μ m, 280～200 μ m, 200～125 μ m and 125～50 μ m.
3, described by claim 1 is the preparation method of the carborundum porous ceramics of pore-forming material with the yeast powder, it is characterized in that expecting powder and pore-forming material mixing the oven dry after, dry-pressing formed with 20～100MPa pressure on sheet-leveling machine.
4, described by claim 1 is the preparation method of the carborundum porous ceramics of pore-forming material with the yeast powder, and the intensification that it is characterized in that sintering process is 1 ℃/minute of a temperature rise rate below 900 ℃, is warming up to sintering temperature with 5 ℃/minute speed then.
5, by claim 1,2,3 or 4 described be the preparation method of the carborundum porous ceramics of pore-forming material with the yeast powder, the SiC porous ceramics porosity that it is characterized in that producing between between 45-60%, volume density 0.95～1.50g/cm
3, aperture size is 50-500 μ m.
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| CN100423810C (en) * | 2007-02-07 | 2008-10-08 | 山东理工大学 | Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing method |
| CN101323524B (en) * | 2008-04-15 | 2011-04-06 | 西安交通大学 | Preparation of oriented hole silicon carbide porous ceramic |
| CN102503520A (en) * | 2011-11-21 | 2012-06-20 | 河南科技大学 | Method for preparing SiC foam ceramic filter |
| CN103073330A (en) * | 2013-02-04 | 2013-05-01 | 山东科技大学 | Method for preparing mullite-corundum porous ceramic by taking active yeast as pore forming agent |
| CN103449840A (en) * | 2013-08-28 | 2013-12-18 | 北京中安四海节能环保工程技术有限公司 | Honeycomb ceramic carrier and preparation method thereof |
| CN106167398A (en) * | 2016-07-11 | 2016-11-30 | 岳阳钟鼎热工电磁科技有限公司 | honeycomb ceramic heat accumulator and preparation method thereof |
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| CN100423810C (en) * | 2007-02-07 | 2008-10-08 | 山东理工大学 | Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing method |
| CN101323524B (en) * | 2008-04-15 | 2011-04-06 | 西安交通大学 | Preparation of oriented hole silicon carbide porous ceramic |
| CN102503520A (en) * | 2011-11-21 | 2012-06-20 | 河南科技大学 | Method for preparing SiC foam ceramic filter |
| CN102503520B (en) * | 2011-11-21 | 2013-03-13 | 河南科技大学 | Method for preparing SiC foam ceramic filter |
| CN103073330B (en) * | 2013-02-04 | 2014-02-26 | 山东科技大学 | Method for preparing mullite-corundum porous ceramic by taking active yeast as pore forming agent |
| CN103073330A (en) * | 2013-02-04 | 2013-05-01 | 山东科技大学 | Method for preparing mullite-corundum porous ceramic by taking active yeast as pore forming agent |
| CN103449840A (en) * | 2013-08-28 | 2013-12-18 | 北京中安四海节能环保工程技术有限公司 | Honeycomb ceramic carrier and preparation method thereof |
| CN106167398A (en) * | 2016-07-11 | 2016-11-30 | 岳阳钟鼎热工电磁科技有限公司 | honeycomb ceramic heat accumulator and preparation method thereof |
| CN106365677A (en) * | 2016-08-26 | 2017-02-01 | 宜兴王子制陶有限公司 | Main material for wall-flow type ceramic filter |
| CN106588085A (en) * | 2016-12-22 | 2017-04-26 | 哈尔滨工业大学 | Method for preparing high-temperature-resistant structural SiC porous ceramics |
| CN106588085B (en) * | 2016-12-22 | 2019-07-16 | 哈尔滨工业大学 | A kind of preparation method of high-temperature-resistant structure type SiC porous ceramics |
| CN108409353A (en) * | 2018-03-08 | 2018-08-17 | 武汉理工大学 | The preparation method of SiC porous ceramic film materials as electronic smoke atomizer tobacco tar carrier |
| CN113797948A (en) * | 2021-08-31 | 2021-12-17 | 江西环宇工陶技术研究有限公司 | Catalyst carrier prepared by taking natural clay mineral as raw material and preparation method thereof |
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