CN100384781C - Method for preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process - Google Patents
Method for preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process Download PDFInfo
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- CN100384781C CN100384781C CNB2006101192339A CN200610119233A CN100384781C CN 100384781 C CN100384781 C CN 100384781C CN B2006101192339 A CNB2006101192339 A CN B2006101192339A CN 200610119233 A CN200610119233 A CN 200610119233A CN 100384781 C CN100384781 C CN 100384781C
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Abstract
The invention discloses a preparing method of carborundum porous ceramic through gel parcel-freezing drying technique, which comprises the following steps: preparing alumina sol; using alumina sol to parcel the carborundum particle; controlling the solid sol content; freezing sol slurry; drying; moulding; sintering; possessing oriental and mutual connecting pore with hole opening rate at 40-90% and aperture at 1-500 um; connecting carborundum through mullite; dispersing aluminium isopropoxide and carborundum particle in the isopropanol; hydrolyzing aluminium isopropoxide to form alumina sol slurry; adding adhesive and defoamer; casting; moulding; removing air to form vacuum; freezing to dry; forming porous blank; detackifying; sintering in the air; oxidizing carborundum particle surface into silica and alumina to obtain mullite; combining carborundum particle to obtain the porous carborundum ceramics.
Description
Technical field
The present invention relates to a kind of method of preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process, a kind of more precisely method of utilizing the glue wrapping-freeze drying process to prepare the carborundum porous ceramics with directional hole structure and high porosity belongs to the porous ceramics field.
Background technology
Vehicle exhaust, Industrial fumes and chemical emission bring serious pollution to environment, press for the strainer and the catalyst support material of high temperature resistant, the heat shock resistance of exploitation, high permeability.Carborundum porous ceramics also has low thermal coefficient of expansion, high thermal conductance and excellent mechanical property, thereby is one of optimal strainer and support of the catalyst candidate materials except good high-temperature performance and penetrating quality are arranged.
The foam impregnation method is the carborundum porous ceramics method commonly used of preparation wide aperture, eyed structure hole.CN200410067101 adopts MgO-Al
2O
3-SiO
2System is as helping the burning system, under 1200 ℃～1400 ℃ temperature, realize sintering, prepared that ultimate compression strength is regulated and control in 500 μ m～4mm scope in more than the 1.0MPa and aperture, refractoriness is at 1580 ℃～1730 ℃ mesh silicon carbide ceramics the mesh porous silicon carbide ceramic.
Add the carborundum porous ceramics that pore-forming material can prepare porosity and controllable aperture.CN3116370 is pore-forming material with the yeast powder, is sintering aid with aluminum oxide, Suzhou soil and wilkinite, and 1100～1350 ℃ of sintering under air atmosphere obtain void content 45～65%, volume density 0.95～1.50g/cm
3Carborundum porous ceramics.The mullite that CN200510029152 is pore-forming material with graphite, generate with the silicon carbide reaction in is the carborundum porous ceramics in conjunction with phase, the bending strength of porous ceramics can reach more than the 20MPa, open porosity 20～70%, 0.1～30 micron in aperture, volume density 1.0～2.2g/cm3, thermal expansivity 6～9 * 10
-6K
-1(0～800 ℃) can be used for materials such as liquids and gases strainer under normal temperature, high temperature and the high corrosive environment and high-temperature catalytic agent carrier.
The novel method of preparation carborundum porous ceramics is bionical technology.CN200610012550 is with the carbonization under the protection of argon gas of exsiccant farm crop fruit, material after the carbonization is by siliconising, carbothermic reduction, carry out silication, in air, handled 1～4 hour under 600～800 ℃ of temperature, with hydrochloric acid and hydroflouric acid washing, obtain carborundum porous ceramics again to similar macro morphology of farm crop fruit and microtexture; The SiC particle diameter is between 0.2～.5cm, and pore structure is the honeycomb fashion cell structure, and hole communicates, and the aperture is between 0.01～500 μ m.
Because the filter-carrier material must have bigger rate of permeation, carrying intravital requirement by pressing with the quilt that reduces inside and outside the carrier smoothly to satisfy fluid, so the filter-carrier porous ceramics must possess high porosity, and require hole to align.Yet, with above-mentioned all methods be difficult to obtain porosity greater than 80%, the aperture is 0.1～100 μ m and carborundum porous ceramics with directional hole structure.The gel refrigeration drying forming method utilizes unique hole of the vesicular structure of gel itself and the ice pellets distillation back formation that the colloid interior orientation is grown simultaneously, obtain having high hole, the porous ceramics of pore directional profile, be the desirable technology of preparation strainer porous material.So constitute design of the present invention.
Summary of the invention
Based on the above-mentioned state of the art, the objective of the invention is to prepare the carborundum porous ceramics that high porosity, hole align with gelatin wrapping-freeze drying process easy and simple to handle.The invention provides the method for preparing carborundum porous ceramics, comprise the sintering of base substrate after the preparation, alumina sol of alumina sol are to the lyophilize moulding of the control of the parcel of silicon-carbide particle, colloidal sol solid content, colloidal sol slurry and moulding.Core of the present invention is the colloidal sol slurry by preparation aluminum oxide micelle packaged silicon carbide particles, the slurry directly-forming that utilizes freeze-drying to make then to freeze is porous body, obtains the mullite bonded carborundum porous ceramics that high porosity and hole align behind the sintering.The present invention is dispersed in the aluminum isopropylate solution by silicon carbide, it is the alumina sol slurry of nucleation centre that the aluminum isopropylate hydrolysis obtains forming with the silicon-carbide particle, PVB (polyvinyl butyral acetal), resol (solid content 30-70%) or PVA (polyvinyl alcohol) binding agent during as moulding, sodium polymethacrylate (or potassium) is as defoamer.The degasification of colloidal sol slurry cast molding final vacuum, cryogenic freezing, strip after freezing is put into the freeze drier lyophilize, unsticking, sintering then, the silicon-dioxide and the aluminum oxide reaction that obtain by silicon-carbide particle surface oxidation under the high temperature generate mullite, thereby the based on silicon carbide particle obtains the carborundum porous ceramics of mullite bonded.
The method of preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process provided by the invention is characterized in that comprising the sintering of base substrate after the preparation, alumina sol of alumina sol are to the lyophilize moulding of the control of the parcel of silicon-carbide particle, colloidal sol solid content, colloidal sol slurry and moulding; Also be
1. the ratio with mass ratio 1: 0.5～1 after aluminum isopropylate being ground is dissolved in the Virahol, and with aluminum isopropylate: the weight ratio of silicon carbide=1: 0.3～0.8 adds 0.1～100 micron carborundum powder in aluminum isopropylate solution, ultrasonic mixing magnetic agitation 20 minutes after 0.5～8 hour, then solution is placed under 70-100 ℃ the environment mechanical stirring and adds the deionized water hydrolysis, add the acetic acid dispergator after 20 minutes, obtaining with the silicon-carbide particle is the alumina sol slurry of the heterogeneous nucleation in center, is cooled to normal temperature;
2. then with aluminum isopropylate: silicon carbide: binding agent: the mass ratio of defoamer=1: 0.3～0.8: 0.01～0.1: 0.005～0.1 adds binding agent PVA, PVB or resol and defoamer, and mechanical stirring, forms finely dispersed slurry;
3. the slurry for preparing is poured into cast molding in the mould of desired shape rapidly, and put into vacuum drying oven and more than 10 minutes, eliminate the bubble in the slurry in the following vacuum outgas of normal temperature 100Pa;
4. then sample is placed＜-10 ℃ cryogenic refrigerator, kept 4～48 hours, sample is freezed fully, sample after freezing is transferred in the freeze drier fast, lyophilize under the environment of 0～80 ℃ and 5～100Pa makes the ice pellets distillation in the frozen block, thereby forms the porous base substrate;
5. the base substrate after the lyophilize ℃ removes binding agent with the temperature rise rate to 600 that is lower than 2 ℃/min in air, remove organism volatile matter wherein, sample after the unsticking is put into High Temperature Furnaces Heating Apparatus, under air atmosphere, rise to 1400～1600 ℃ of reaction sinterings with 5 ℃/min, furnace cooling behind the sintering obtains the porous ceramics of mullite bonded silicon carbide.
The concrete implementation step of technology: 1. aluminum isopropylate is ground the back by 100～300 eye mesh screens, ratio with mass ratio 1: 0.5～1 is dissolved in the Virahol then, and with aluminum isopropylate: the weight ratio of silicon carbide=1: 0.3～0.8 adds 0.1～100 micron carborundum powder in aluminum isopropylate solution, adopt two kinds of sic raw materials: commercially available initial carborundum powder or preoxidation carborundum powder, preoxidation silicon carbide are that initial carborundum powder obtains in 1000～1300 ℃ of insulations oxidation in 1～12 hour in air; Ultrasonic mixing magnetic agitation more than 20 minutes after 0.5～8 hour, then solution is placed under 70-100 ℃ the environment mechanical stirring and adds the deionized water hydrolysis, add the acetic acid dispergation more than 20 minutes, obtaining with the silicon-carbide particle is the alumina sol slurry of the heterogeneous nucleation in center, stops the water-bath postcooling to normal temperature; 2. then with aluminum isopropylate: silicon carbide: binding agent: the weight ratio of defoamer=1: 0.3～0.8: 0.01～0.1: 0.005～0.1 adds binding agent PVA, PVB or resol and defoamer n-Octanol, and mechanical stirring, thereby form finely dispersed slurry; 3. the slurry for preparing is poured into cast molding in the mould of definite shape rapidly, and put into vacuum drying oven and more than 10 minutes, eliminate the bubble in the slurry in the following vacuum outgas of normal temperature 100Pa; 4. then sample place cryogenic refrigerator (＜-10 ℃=, kept 4～48 hours, sample is freezed fully, freezing good sample is transferred in the freeze drier fast, lyophilize under the environment of 0～80 ℃ and 5～100Pa makes the ice pellets distillation in the frozen block, thereby forms the porous base substrate; 5. the base substrate after the lyophilize in air with the temperature rise rate to 600 that is lower than 2 ℃/min ℃ 1～12 hour unsticking of insulation, remove organism volatile matter wherein, sample after the unsticking is put into the high temperature retort furnace, under air atmosphere, rise to 1～24 hour reaction sintering of 1400～1600 ℃ of insulations with 5 ℃/min, furnace cooling obtains the mullite bonded carborundum porous ceramics then.Concrete technical process as shown in Figure 1.Shrinking percentage before and after the sintering is-0.4～7.3%, and the silicon carbide oxidation ratio is 9.7～28.2%.
Use the invention provides the typical microstructure of mullite bonded carborundum porous ceramics of method preparation shown in Fig. 2 and 3.The open-celled structure that porous ceramics has higher porosity and is interconnected, open porosity is 1～500 μ m for the 40-90% aperture size, hole aligns significantly; Along with the increase of solid content, porosity reduces, and the aperture of directed macropore diminishes, and the hole orientation ratio reduces, and the combination of the hole muscle between the hole strengthens.Fig. 4 shows that the preoxidation of silicon carbide has a significant impact the phase composite of porous ceramics before the adding colloidal sol slurry, and behind the employing preoxidation silicon carbide, the content of mullite and cristobalite all increases.
Fig. 5 is for showing, along with the rising of sintering temperature, the open porosity of porous material reduces, and volume density increases; And SiC particulate pre-oxidation treatment has reduced open porosity, has improved the volume density of sample.Fig. 6 shows, increases the intensity that the slurry solid content can improve porous ceramics to a great extent.Fig. 7 shows that the raising of solid content increases the volume density of porous ceramics, and open porosity reduces.
In sum, utilizing the present invention to prepare carborundum porous ceramics has the following advantages:
(1) use collosol and gel to be convenient to prepare the porous ceramics in the micron order aperture that high porosity, hole align in conjunction with cryodesiccated technology;
(2) owing to the combination that obtains porous ceramics is that mullite, matrix are silicon carbide mutually, so porous ceramics has excellent high;
(3) with SiC be matrix, with the SiO of sol alumina and SiC particle surface oxidation generation
2The mullite that reaction generates is in conjunction with phase, has even, directed interconnected pores structure;
(4) generation of mullite on the silicon-carbide particle surface makes carborundum porous ceramics have higher high temperature oxidation resistent susceptibility.
Description of drawings
Fig. 1 gelatin wrapping-freeze drying process prepares the technical process of mullite bonded carborundum porous ceramics.
Fig. 2 slurry solid content is the section SEM pattern of 4 hours agglomerating porous ceramicss of 25%, 1500 ℃ of insulation.
Fig. 3 slurry solid content is the section SEM pattern of 4 hours agglomerating porous ceramicss of 70%, 1500 ℃ of insulation.
The pre-oxidation treatment of Fig. 4 silicon carbide powder (1200 ℃ are incubated 4 hours) is to the influences of the phase composite of 4 hours agglomerating porous ceramicss of 1500 ℃ of insulations; X-coordinate is 2 times of diffraction angle, and unit is degree, and ordinate zou is the relative value of diffracted intensity.
It is 7.5% preoxidation silicon carbide that Fig. 5 adopts without preoxidation silicon carbide and oxidation ratio, and the slurry solid content is 25% o'clock, and sintering temperature is to the influence of the open porosity and the volume density of porous ceramics.
Fig. 6 adopt oxidation ratio be 7.5% preoxidation silicon carbide add slurry and 1500 ℃, during 4 hours sintering of insulation, the influence of the porous ceramics ultimate compression strength that solid content is right.
Fig. 7 adopt oxidation ratio be 7.5% preoxidation silicon carbide add slurry and 1500 ℃, during 4 hours sintering of insulation, the porous ceramics volume density that solid content is right and the influence of open porosity.
Embodiment
Below by concrete enforcement the present invention is described further, but the present invention is confined to embodiment absolutely not.Process implementing is for example shown in the following table:
| Embodiment | The pre-oxidation treatment of silicon carbide | Slurry solid content (%) | Sintering temperature (℃) | Soaking time (h) | Sublimation drying (h) | Lyophilize pressure (Pa) | The lyophilize temperature (℃) | Volume density (g/cm 3) | Open porosity (%) | Ultimate compression strength (MPa) |
| 1 | Not oxidation | 25 | 1400 | 4 | 48 | 8.5 | 60 | 0.34 | 89.3 | 0.09 |
| 2 | Not oxidation | 25 | 1550 | 4 | 48 | 8.5 | 60 | 0.37 | 87.6 | 0.19 |
| 3 | 7.5% oxidation | 25 | 1550 | 4 | 48 | 8.5 | 60 | 0.44 | 84.9 | 0.43 |
| 4 | 7.5% |
50 | 1500 | 4 | 48 | 8.5 | 60 | 1.49 | 52.8 | 12.3 |
| 5 | 7.5% |
70 | 1500 | 4 | 48 | 8.5 | 60 | 1.09 | 66.2 | 2.5 |
Shown in embodiment 1, concrete processing step: the 40g aluminum isopropylate is ground the back by 200 eye mesh screens, be dissolved in the 30g alcohol then and add the SiC powder (not preoxidation) of 20 microns of 20g, magnetic agitation was mixed 30 minutes, placed 80 ℃ of water-baths then 5 minutes and mechanical stirring, add the sub-water of 200g degranulation, add 10g acetic acid after 1 hour again, kept water-bath, mechanical stirring 1 hour.Stop the water-bath postcooling to normal temperature, add binding agent 0.4g and defoamer 0.1g.And mechanical stirring, form finely dispersed slurry.Slurry is poured into cast molding in the mould of definite shape, and put into vacuum drying oven and keep the 5Pa pressure vacuum degassing 10 minutes, then sample is placed cryogenic refrigerator (20 ℃), kept 24 hours, sample is freezed fully, freeze good sample and be transferred to fast in the freeze drier, lyophilize under the environment of 60 ℃ and 8.5Pa, make the ice pellets distillation, thereby form the porous base substrate.Base substrate after the lyophilize is temperature rise rate to the 600 ℃ 4 hours unstickings of insulation to be lower than 2 ℃/min in air, sample after the unsticking is put into High Temperature Furnaces Heating Apparatus, rise to 4 hours sintering of 1400 ℃ of insulations with 5 ℃/min under air atmosphere, furnace cooling obtains volume density 0.34g/cm then
3, open porosity 89.3%, ultimate compression strength 0.09MPa the mullite bonded carborundum porous ceramics.
The execution of embodiment 2～5 is undertaken by the processing parameter in the table as embodiment 1, obtains the mullite bonded carborundum porous ceramics of respective performances.
Claims (8)
1. the method for preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process is characterized in that comprising the sintering of base substrate after the preparation, alumina sol of alumina sol are to the lyophilize moulding of the control of the parcel of silicon-carbide particle, colloidal sol solid content, colloidal sol slurry and moulding;
Concrete processing step is:
1. the ratio with mass ratio 1: 0.5～1 after aluminum isopropylate being ground is dissolved in the Virahol, and with aluminum isopropylate: the weight ratio of silicon carbide=1: 0.3～0.8 adds 0.1～100 micron carborundum powder in aluminum isopropylate solution, ultrasonic mixing magnetic agitation 20 minutes after 0.5～8 hour, then solution is placed under 70-100 ℃ the environment mechanical stirring and adds the deionized water hydrolysis, add the acetic acid dispergator after 20 minutes, obtaining with the silicon-carbide particle is the alumina sol slurry of the heterogeneous nucleation in center, is cooled to normal temperature;
2. then with aluminum isopropylate: silicon carbide: binding agent: the mass ratio of defoamer=1: 0.3～0.8: 0.01～0.1: 0.005～0.1 adds binding agent PVA, PVB or resol and defoamer, and mechanical stirring, forms finely dispersed slurry;
3. the slurry for preparing is poured into cast molding in the mould of desired shape rapidly, and put into vacuum drying oven and more than 10 minutes, eliminate the bubble in the slurry in the following vacuum outgas of normal temperature 100Pa;
4. then sample is placed＜-10 ℃ cryogenic refrigerator, kept 4～48 hours, sample is freezed fully, sample after freezing is transferred in the freeze drier fast, lyophilize under the environment of 0～80 ℃ and 5～100Pa makes the ice pellets distillation in the frozen block, thereby forms the porous base substrate;
5. the base substrate after the lyophilize ℃ removes binding agent with the temperature rise rate to 600 that is lower than 2 ℃/min in air, remove organism volatile matter wherein, sample after the unsticking is put into High Temperature Furnaces Heating Apparatus, under air atmosphere, rise to 1400～1600 ℃ of reaction sinterings with 5 ℃/min, furnace cooling behind the sintering obtains the porous ceramics of mullite bonded silicon carbide.
2. by the method for the described preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process of claim 1, the aluminum isopropylate after it is characterized in that grinding is crossed the 100-300 eye mesh screen.
3. press the method for the described preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process of claim 1, it is characterized in that employed sic raw material has two kinds, be respectively the preoxidation carborundum powder that commercially available initial carborundum powder and initial carborundum powder obtained under the condition 1000-1300 ℃ of insulation in 1-12 hour in air.
4. by the method for the described preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process of claim 1, it is characterized in that removing the binding agent soaking time during step 5. is 1-12 hour.
5. by the method for the described preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process of claim 1, it is characterized in that step 5. during the final reaction sintering soaking time be 1-24 hour.
6. by the method for the described preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process of claim 1, it is characterized in that described defoamer is a n-Octanol.
7. by the method for any described preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process among the claim 1-6, it is characterized in that the porous ceramics for preparing is is matrix with SiC, the SiO that obtains with sol alumina and the oxidation of SiC particle surface
2The mullite that reaction generates is in conjunction with phase, has even, directed interconnected pores structure.
8. by the method for any described preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process among the claim 1-6, it is characterized in that the open porosity of the porous ceramics for preparing is 40-90%, aperture size is 1-500 μ m.
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| CN101337817B (en) * | 2008-08-12 | 2010-11-10 | 西安交通大学 | Vacuum freezing and drying process for ceramic cast blank |
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| CN102260092A (en) * | 2011-06-14 | 2011-11-30 | 中国科学院上海硅酸盐研究所 | Method for preparing porous silicon carbide ceramic material |
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