CN104387113B - A kind of fibre-reinforced ceramic element and preparation method thereof - Google Patents
A kind of fibre-reinforced ceramic element and preparation method thereof Download PDFInfo
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- CN104387113B CN104387113B CN201410657087.XA CN201410657087A CN104387113B CN 104387113 B CN104387113 B CN 104387113B CN 201410657087 A CN201410657087 A CN 201410657087A CN 104387113 B CN104387113 B CN 104387113B
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Abstract
The invention discloses a kind of fibre-reinforced ceramic element and preparation method thereof, by the method for chemical vapor infiltration (CVI) on porous ceramic support, prepare a kind of fibre-reinforced surface filtration film; The two is integrated by sintering, and the final ceramic element formed, in gasification dust removal by filtration technological process, has low pressure drop and is easy to the characteristic of pulse gas jet regeneration.
Description
Technical field
The present invention relates to stupalith production technical field, particularly fibre-reinforced ceramic element of one and preparation method thereof.
Background technology
Much more the ceramic element used at high temperature under high pressure carries out the mechanism of filtration, purification to high temperature rough gas, to be described in numerous document.In the high-efficiency cleaning of coal utilizes, need the key issue solved to be exactly high temperature filtration dedusting technology, pyroceramic filter core is considered to address this problem the most effective approach.But surface has the core component of filter core as filtration unit of filtering membrane, and its failure phenomenon but occurs now and then, and one of them important reason is exactly surface film plug-hole or comes off.Core of the present invention is exactly in the surface film of filter core, add the ceramic fiber of some amount, reaches the object improving surface film intensity, prevents from, among pulse gas jet regeneration cleaning, surface film obscission occurring; Simultaneously by picking of raw material, the aperture of control table facial mask, guarantees that filtration is unimpeded.
The ultimate principle of ceramic element work is, the high temperature dust raw gas that gasification produces is through the filtration of filter core, and harmful big dust particle is filtered, and clean coal gas enters into next link and uses; Stopped that the dust granules filtered can be piled up gradually on the surface film of filter core by surface film, this just have impact on the filtration efficiency of filter core, and filtration pressure drop is increased.Like this, for guaranteeing the normal operation of equipment, will clear up in time and finally change ceramic element.
Under normal conditions, filter core can by oppositely pressurization, and the method for pulse backblowing gets rid of the ash cake be attached on surface film.But the time one is long, powder dust particle not only at the surface deposition of surface film, also can be able to enter among film body and supporter simultaneously.Along with the prolongation of filter core duration of service, have increasing dust granules and enter among film body and supporter.These dust granules deposit in inside gradually, form so-called " bridge formation " phenomenon.Because back flushing is carried out from inside to outside, dust granules will be removed through the very long path of membranous wall, just needs larger pressure just can complete, so the preliminary examination pressure drop of filter core will be caused to raise, and comes off to surface film, and finally cause filter core to lose efficacy.Before filter core is scrapped, we wish more long-range work-ing life, and this just requires that prepared filter core more easily cleans.And the standard cleaned up be exactly pressure drop stablize, the long lifetime.So whether filter core can fast and efficiently be rinsed, and ensure that surface film is complete, can just determine equipment run well by expection requirement.
Summary of the invention
The object of the invention is the shortcoming in order to overcome above-mentioned background technology, a kind of fibre-reinforced ceramic element and preparation method thereof is provided.
Technical scheme of the present invention is: a kind of fibre-reinforced ceramic element, this filter core is made up of supporter and surface film two portions, described surface film is coated on supporter, described supporter contains major ingredient silicon carbide, auxiliary material binding agent and pore-forming material, described silicon carbide major ingredient is the fine graded silicon carbide of particle diameter, and particle diameter is 250 ~ 300 μm; Described binding agent contains clay, kaolin and feldspar, and the weight percent proportioning between three is clay: 4 ~ 8%, kaolin: 4 ~ 8%, feldspar: 2 ~ 4%; Described pore-forming material be content higher than 90% camwood knag; The raw material that described surface film adopts is particle diameter is 50 μm of mullites, minimum 40 μm of described supporter aperture, maximum 50 μm; The minimum 0.2mm of thickness of described surface film, maximum 0.4mm, its aperture need be less than supporter aperture, and concrete numerical value is minimum 4 μm, maximum 5 μm;
A preparation method for fibre-reinforced ceramic element, the method is as follows:
(1) SiC ceramic supporter is prepared: in supporter, the weight percent of described silicon carbide major ingredient is 85 ~ 90%, the weight percent of described binding agent is 10 ~ 15%, the volume percent of described pore-forming material is 30 ~ 40%, binding agent and pore-forming material is added in fine graded major ingredient silicon carbide powder, be made into mixed powder, add deionized water and be made into slurry; After the mixing of slurry ball milling, drying obtains powder, Vacuum Heat type casting moulding; Base substrate after shaping is carried out pressureless sintering, and sintering temperature is 1250 ~ 1280
?c, soaking time 2 hours, atmosphere is air atmosphere, obtains porous SiC ceramics supporter with stove naturally cooling;
(2) SiC fiber preform is manufactured: the method utilizing chemical vapor infiltration, resol and Polycarbosilane according to weight percent 1:1, put into RESEARCH OF PYROCARBON reactor, and carry out oozing Si process, when there being 0.5 ~ 1.0 μm of thick carbon laydown on heater strip, shut-down operation, reactor cuts out and removal medium, whole operating process is all carried out in 1000 DEG C of isothermal reaction stills, and the weight control of monofilament SiC fiber is within 1.00 ~ 1.10g scope;
(3) be that mullite, the 24g binding agent of 50 μm is even in certain deionized water for stirring the SiC fiber preform of above-mentioned for 20g preparation, 100g particle diameter, make the coating suspension slip of surface film; When supporter applied atop surface film, supporter can not be immersed among slip, but will repeatedly brush gently; Only in this way operation can guarantee that the feed particles in surface film can not enter among supporter, and then affects the strainability of filter core;
(4) after the surface film slip being mixed with SiC fiber preform is coated to supporter; dry 1 hour for 150 DEG C in the baking oven having air draft; the floating dust on surface film is removed with nylon brush after dry; afterwards the supporter after film put into N2 protection stove burn till in 1300 DEG C; be incubated 4 hours, the fibre-reinforced ceramic element of SiC after coming out of the stove, can be obtained.
This filter core shape is one end is blind head, and the other end is slot opening.
The invention has the beneficial effects as follows: by being the ceramic element with double-layer structure obtained by the present invention: supporter and with fibre-reinforced surface film; The aperture of surface film is less than the particle diameter of institute's Chalk-dust filtering particle, guarantees that most dust granules can not enter supporter or be trapped on surface film; The surface film of preparation is fibre-reinforced by SiC, ensure that surface film has enough intensity in pulse cleaning process; The thickness of surface film is between 0.2 ~ 0.4mm, and mean pore size is within 4 ~ 5 μm of scopes, and because surface film powder particles used have passed through strict control, surface film uniform pore diameter, improves filter core pulse cleaning efficiency; And for supporter, require the large of Pore Diameter Specific Surface film, ensure the filtration efficiency of filter core; Desired strength is enough high, ensures the ultimate compression strength of filter core; Ceramic element prepared by the present invention not only intensity is high, simultaneously low pressure drop, corrosion-resistant.
Embodiment
The present embodiment is a kind of fibre-reinforced ceramic element, this filter core is made up of supporter and surface film two portions, described surface film is coated on supporter, described supporter contains major ingredient silicon carbide, auxiliary material binding agent and pore-forming material, described silicon carbide major ingredient is the fine graded silicon carbide of particle diameter, and particle diameter is 250 ~ 300 μm; Described binding agent contains clay, kaolin and feldspar, and the weight percent proportioning between three is clay: 4 ~ 8%, kaolin: 4 ~ 8%, feldspar: 2 ~ 4%; Described pore-forming material be content higher than 90% camwood knag; The raw material that described surface film adopts is particle diameter is 50 μm of mullites, minimum 40 μm of described supporter aperture, maximum 50 μm; The minimum 0.2mm of thickness of described surface film, maximum 0.4mm, its aperture need be less than supporter aperture, and concrete numerical value is minimum 4 μm, maximum 5 μm;
A preparation method for fibre-reinforced ceramic element, the method is as follows:
(1) SiC ceramic supporter is prepared: in supporter, the weight percent of described silicon carbide major ingredient is 85 ~ 90%, the weight percent of described binding agent is 10 ~ 15%, the volume percent of described pore-forming material is 30 ~ 40%, binding agent and pore-forming material is added in fine graded major ingredient silicon carbide powder, be made into mixed powder, add deionized water and be made into slurry; After the mixing of slurry ball milling, drying obtains powder, Vacuum Heat type casting moulding; Base substrate after shaping is carried out pressureless sintering, and sintering temperature is 1250 ~ 1280
?c, soaking time 2 hours, atmosphere is air atmosphere, obtains porous SiC ceramics supporter with stove naturally cooling;
(2) SiC fiber preform is manufactured: the method utilizing chemical vapor infiltration, resol and Polycarbosilane according to weight percent 1:1, put into RESEARCH OF PYROCARBON reactor, and carry out oozing Si process, when there being 0.5 ~ 1.0 μm of thick carbon laydown on heater strip, shut-down operation, reactor cuts out and removal medium, whole operating process is all carried out in 1000 DEG C of isothermal reaction stills, and the weight control of monofilament SiC fiber is within 1.00 ~ 1.10g scope;
(3) be that mullite, the 24g binding agent of 50 μm is even in certain deionized water for stirring the SiC fiber preform of above-mentioned for 20g preparation, 100g particle diameter, make the coating suspension slip of surface film; When supporter applied atop surface film, supporter can not be immersed among slip, but will repeatedly brush gently; Only in this way operation can guarantee that the feed particles in surface film can not enter among supporter, and then affects the strainability of filter core;
(4) after the surface film slip being mixed with SiC fiber preform is coated to supporter; dry 1 hour for 150 DEG C in the baking oven having air draft; the floating dust on surface film is removed with nylon brush after dry; afterwards the supporter after film put into N2 protection stove burn till in 1300 DEG C; be incubated 4 hours, the fibre-reinforced ceramic element of SiC after coming out of the stove, can be obtained.
This filter core shape is one end is blind head, and the other end is slot opening.
The porosity of the SiC fiber reinforced ceramic filter core prepared by the inventive method is 39.2%, and intensity reaches 26.2MPa, can ensure the service requirements to filter core under high-temperature and high-pressure conditions completely.
Claims (3)
1. a fibre-reinforced ceramic element, it is characterized in that this filter core is made up of supporter and surface film two portions, described surface film is coated on supporter, described supporter contains major ingredient silicon carbide, auxiliary material binding agent and pore-forming material, described silicon carbide major ingredient is the fine graded silicon carbide of particle diameter, and particle diameter is 250 ~ 300 μm; Described binding agent contains clay, kaolin and feldspar, and the weight percent proportioning between three is clay: 4 ~ 8%, kaolin: 4 ~ 8%, feldspar: 2 ~ 4%; Described pore-forming material be content higher than 90% camwood knag; The raw material that described surface film adopts is particle diameter is 50 μm of mullites, and adds SiC fiber preform; Minimum 40 μm of described supporter aperture, maximum 50 μm; The minimum 0.2mm of thickness of described surface film, maximum 0.4mm, its aperture need be less than supporter aperture, and concrete numerical value is minimum 4 μm, maximum 5 μm.
2. a preparation method for fibre-reinforced ceramic element, is characterized in that the method is as follows:
(1) SiC ceramic supporter is prepared: in supporter, the weight percent of described silicon carbide major ingredient is 85 ~ 90%, the weight percent of described binding agent is 10 ~ 15%, the volume percent of described pore-forming material is 30 ~ 40%, binding agent and pore-forming material is added in fine graded major ingredient silicon carbide powder, be made into mixed powder, add deionized water and be made into slurry; After the mixing of slurry ball milling, drying obtains powder, Vacuum Heat type casting moulding; Base substrate after shaping is carried out pressureless sintering, and sintering temperature is 1250 ~ 1280 DEG C, soaking time 2 hours, and atmosphere is air atmosphere, obtains porous SiC ceramics supporter with stove naturally cooling;
(2) SiC fiber preform is manufactured: the method utilizing chemical vapor infiltration, resol and Polycarbosilane according to weight percent 1:1, put into RESEARCH OF PYROCARBON reactor, and carry out oozing Si process, when there being 0.5 ~ 1.0 μm of thick carbon laydown on heater strip, shut-down operation, reactor cuts out and removal medium, whole operating process is all carried out in 1000 DEG C of isothermal reaction stills, and the weight control of monofilament SiC fiber is within 1.00 ~ 1.10g scope;
(3) be that mullite, the 24g binding agent of 50 μm is even in certain deionized water for stirring the SiC fiber preform of above-mentioned for 20g preparation, 100g particle diameter, make the coating suspension slip of surface film; When supporter applied atop surface film, supporter can not be immersed among slip, but will repeatedly brush gently; Only in this way operation can guarantee that the feed particles in surface film can not enter among supporter, and then affects the strainability of filter core;
(4) after the surface film slip being mixed with SiC fiber preform is coated to supporter, dry 1 hour for 150 DEG C in the baking oven having air draft, remove the floating dust on surface film with nylon brush after dry, afterwards the supporter after film is put into N
2burn till in 1300 DEG C in the stove of protection, be incubated 4 hours, the fibre-reinforced ceramic element of SiC after coming out of the stove, can be obtained.
3. the fibre-reinforced ceramic element of one according to claim 1, it is characterized in that this filter core shape be one end is blind head, the other end is slot opening.
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| CN107089836A (en) * | 2016-08-25 | 2017-08-25 | 邱和忠 | Ion activity multi-microporous ceramic filter core composition of raw materials and its manufacturing process |
| CN107663088B (en) * | 2017-08-03 | 2020-11-10 | 浙江理工大学 | Preparation method of low-temperature sintered acid-alkali-resistant porous silicon carbide ceramic membrane |
| EP3647459A1 (en) | 2018-10-31 | 2020-05-06 | Petroceramics S.p.A. | Method and an assembly by chemical vapor infiltration of porous components |
| IT201800009953A1 (en) | 2018-10-31 | 2020-05-01 | Petroceramics Spa | Method and assembly of infiltration and rapid vapor deposition of porous components |
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| CN1683284A (en) * | 2004-04-13 | 2005-10-19 | 杨颖辉 | Method for quick preparing fiber reinforced ceramic base composite material or carbon/carbon composite material |
| CN101475400B (en) * | 2008-01-04 | 2013-02-13 | 广州锐得森特种陶瓷科技有限公司 | Floamed ceramic reinforcing fiber porous ceramic |
| CN103086732B (en) * | 2013-01-21 | 2014-12-03 | 天津师范大学 | Fiber enhanced silicon carbide porous ceramic and preparation method and application thereof |
| CN103111132B (en) * | 2013-02-25 | 2014-12-24 | 中国石油大学(北京) | Manufacturing device of filtering tube applied to high-temperature gas filtration and method of filtering tube |
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