CN103274693A - Porous silicon carbide ceramic provided with novel pore wall structure and preparation method thereof - Google Patents
Porous silicon carbide ceramic provided with novel pore wall structure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a porous silicon carbide ceramic and a preparation method thereof, in particular to a porous silicon carbide ceramic provided with a novel pore wall structure and a preparation method thereof, and aims to solve the technical problems that the porous silicon carbide ceramic prepared by the conventional method has low mechanical property and specific surface area. The porous silicon carbide ceramic is prepared by silicon carbide powder, a sintering aid, deionized water, a dispersant, a binder and a defoamer. The preparation method comprises the following steps: 1, preparing slurry; 2, preparing a porous silicon carbide ceramic green ware body; 3, preparing a pre-oxidation porous silicon carbide ceramic ware body; 4, preparing the porous silicon carbide ceramic bound with baryta feldspar in situ; and 5, performing high-heat treatment. According to the prepared porous silicon carbide ceramic, the porosity can reach 20 vol%-82 vol%, and the pore diameter ranges from 0.1 mum to 300 mum; the bending strength can reach 63 MPa when the porosity is 48 vol%; and rod-shaped silicon carbide particles are grown in situ in the pore wall. The preparation method is used for preparing the porous silicon carbide ceramic provided with the novel pore wall structure.
Description
Technical field
The present invention relates to porous silicon carbide ceramic and preparation method thereof.
Background technology
Porous silicon carbide ceramic because have low density, perviousness is good, specific surface area is big, high temperature resistant, corrosion-resistant, premium properties such as chemical stability is good and anti-oxidant, thermal shock resistance is good, it is with a wide range of applications in all many-sides such as tripping device, various strainer, support of the catalyst, porous electrode, heat exchangers, and uses gradually and fields such as metallurgy, chemical industry, the energy, environmental protection and biology.Therefore, the preparation about porous silicon carbide ceramic becomes one of focus of present porous ceramics area research.
At present, the research of porous silicon carbide ceramic mainly concentrates in preparation method's the improvement, to realize being control to porosity and pore texture.At present oneself method of exploitation mainly contains: powder metallurgic method, the pore-forming material method of adding, whipping agent method, with biological templates such as timber through high temperature cabonization afterreaction sintering process, organic foam plastic as template, precursor cracking process etc.Among the existing porous silicon carbide ceramic preparation method, powder metallurgic method technology is comparatively simple, but is difficult to realize the design to porosity and pore size, and the porous SiC pottery porosity of preparation is generally 20～50vol%; Adding the pore-forming material method is to get rid of pore-forming material to form pore texture in preparation process, though porosity and aperture are controlled within the specific limits, be difficult to prepare the porous silicon carbide ceramic of high porosity equally, porosity is generally below 50vol%, in addition, the eliminating of pore-forming material is unfriendly to environment; And the formation owing to hole depends on the bubble that whipping agent produces in the whipping agent method, can not realize the effective control to pore dimension and pattern; Adopt the porous silicon carbide of biological template method preparation to make pottery, therefore its pore texture, is difficult to obtain the good porous silicon carbide product of repeatability by the structure control of biological template; Organic foam plastic has bigger aperture size as the porous silicon carbide of template preparation, can not satisfy the service requirements of multiple occasion.Utilize Polycarbosilane can prepare porous silicon carbide ceramic at a lower temperature as precursor, but preparation cost is very high, yields poorly.Therefore, develop new preparation method, realize effective control of porous silicon carbide ceramic porosity and pore structure particularly necessary better.
The sintering character of silicon carbide is poor, and the mechanical property of prepared porous silicon carbide ceramic is lower, has seriously limited the application of porous silicon carbide ceramic.Hole wall structure has bigger influence to many-sided performance of porous silicon carbide ceramic: the density that improves hole wall is conducive to increase its mechanical property; And rationally change the porous silicon carbide ceramic that hole wall structure can obtain to have different specific surface areas, thereby influence the dotted point of catalyzer on the filter effect of porous silicon carbide ceramic and the support of the catalyst.Yet, also lack research for the control of the middle hole wall structure of porous silicon carbide.Given this, exploitation has the porous silicon carbide ceramic of novel hole wall structure, has the important research meaning.
In recent years, freezing pouring technology has obtained great concern as the novel method of preparation porous material, and this technology can realize the effective control to the porosity of porous material and pore texture.Yet, adopt the porous silicon carbide ceramic of this method preparation still to have the lower shortcoming of performance, its hole wall structure is comparatively single, generally is to realize by accumulation and the sintering of silicon-carbide particle, therefore is difficult to reach densification; In addition, because the high stability of silicon carbide, original position grows long bar-shaped carborundum grain in fine and close hole wall, thereby the porous silicon carbide with high-specific surface area yet there are no bibliographical information, if the porous silicon carbide of this structure is applied in strainer and the tripping device, is expected to improve and filters and the effect of separating, be applied on the support of the catalyst, increased the dotted point of catalyzer, improved catalytic effect, therefore had broad application prospects.
Summary of the invention
The present invention will solve the technical problem that the porous silicon carbide ceramic mechanical property is low, specific surface area is low of existing method preparation, and a kind of porous silicon carbide ceramic with novel hole wall structure and preparation method thereof is provided.
A kind of porous silicon carbide ceramic with novel hole wall structure is raw material with silicon carbide powder and sintering aid, adopt freezing casting moulding, sintering is prepared from after drying, in the slurry of freezing cast, according to volume percent, the mixed powder of silicon carbide powder and sintering aid is 5～60%, and deionized water is 95～40%; The mass ratio of the mixed powder of silicon carbide powder and sintering aid, dispersion agent, binding agent and defoamer is 1:(0.001～0.03): (0.005～0.03): (0.001～0.01); The massfraction of sintering aid is 1～50% in the mixed powder of silicon carbide powder and sintering aid.
Prepare above-mentioned a kind of method with porous silicon carbide ceramic of novel hole wall structure, it is characterized in that a kind of preparation method with porous silicon carbide ceramic of novel hole wall structure, specifically prepare according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24～25 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 5～60%, and deionized water is 95～40%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:(0.001～0.03): (0.005～0.03): (0.001～0.01);
Described in the step 1 in the mixed powder massfraction of sintering aid be 1～50%;
Sintering aid is Al in the step 1
2O
3, BaO and rare earth oxide mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 1～5%; Perhaps sintering aid is Al
2O
3, BaCO
3With the mixing of rare earth oxide, wherein Al
2O
3With BaCO
3The ratio of amount of substance be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 1～5%; Wherein rare earth oxide is Y
2O
3, Gd
2O
3, Lu
2O
3, Eu
2O
3, CeO
2And Sm
2O
3In one or more press the combination of arbitrary proportion;
Dispersion agent is Tetramethylammonium hydroxide or ammonium citrate in the step 1;
Binding agent is gelatin, polyvinyl alcohol or polyvinyl butyral acetal in the step 1;
Defoamer is propyl carbinol or the trimethyl carbinol in the step 1;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgased again 30 minutes, obtain sample, take out sample then, solidified 3～60 minutes under-200 ° of C～-10 ° C in temperature, be-10～40 ° of C in temperature again, pressure is lyophilize 1～4 day under the environment of 1～600Pa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 1～20 ° of C/min then, be heated to 800～1300 ° of C, be incubated 10～360 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charge into rare gas element, the control temperature rise rate is 1～20 ° of C/min, be heated to 1200～1500 ° of C, be incubated 0.5～4 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.2～3MPa, controlling temperature rise rate then is 1～20 ° of C/min, be warming up to 1700～1900 ° of C, be incubated 0.5～4 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure.
The porous silicon carbide ceramic that obtains in the step 5 has novel hole wall structure, and original position grows long bar-shaped carborundum grain in the hole wall, and its diameter is 1～5um, and length-to-diameter ratio is 2～5; The porous silicon carbide ceramic porosity can reach 20vol%～82vol%, and the aperture is 0.1～300 μ m; When void content was 48v0l%, bending strength can reach 63MPa.
The invention has the beneficial effects as follows:
(1) can realize effective control to porous ceramics porosity and aperture structure, adopt water-based slurry to prepare porous ceramics, the generation of unharmful substance is environmentally friendly in the preparation process.
(2) present method is passed through porous ceramics base substrate pre-oxidation treatment, (＜1500 ° of C) obtains the porous silicon carbide material of celsian-felspar original position combination then at low temperatures, because celsian-felspar has high-melting-point (1780 ° of C), makes porous ceramics can satisfy the high temperature service requirements.
(3) the inventive method can realize the porous silicon carbide ceramic of hole wall densification, has realized the raising of material mechanical performance; And realized the growth in situ of long bar-shaped single-crystal silicon carbide in hole wall first, formed new porous silicon carbide hole wall structure, compared with the hole wall structure of being formed by the silicon-carbide particle of irregular shape, improved the specific surface area of porous silicon carbide.Be applied in strainer and the tripping device, be expected to improve and filter and the effect of separating; Be applied on the support of the catalyst, increased the dotted point of catalyzer, improve catalytic effect, have broad application prospects.
(4) among the present invention owing to adopt colloidal formation technology, do not have and press or gas pressure sintering, can prepare the porous silicon carbide product of complicated shape, be suitable for producing in batches.
The porous silicon carbide ceramic of the present invention preparation can be controlled the variation of material void content by regulating solid load in the freezing casting process, improves the solid load of slurry, and the void content of porous silicon carbide ceramic descends.By regulating freezing temp and freezing mode, can control pore size and the pore texture of porous silicon carbide ceramic, freezing temp is more low, and solidification rate is more big, and aperture size is more little; The pore texture that adopts the directional freeze mode to obtain to align.The porous ceramics void content of gained can reach 20vol%～80vol%, and the aperture is 0.1～300 μ m; Obtained fine and close hole wall structure, and original position grows long bar-shaped carborundum grain in the hole wall, its diameter is 1～5 μ m, and length-to-diameter ratio is 2～5; Prepared porous silicon carbide ceramic has excellent mechanical property, and when porosity was 48vol%, bending strength can reach 63MPa.
The present invention is for the preparation of the porous silicon carbide ceramic with novel hole wall structure.
Description of drawings
The XRD diffraction spectrogram of the porous silicon carbide ceramic of the celsian-felspar original position combination that Fig. 1 obtains for embodiment one step 4, wherein " ◆ " represents α-SiC, and " ▲ " represents the porous silicon carbide ceramic of celsian-felspar original position combination, and Fig. 2 is sem photograph;
Fig. 3 is the sem photograph of the porous silicon carbide ceramic with novel hole wall structure of embodiment one preparation, and Fig. 4 is gas cell distribution figure.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of porous silicon carbide ceramic with novel hole wall structure of present embodiment is raw material with silicon carbide powder and sintering aid, adopt freezing casting moulding, through thousand dry after sintering be prepared from, in the slurry of freezing cast, according to volume percent, the mixed powder of silicon carbide powder and sintering aid is 5～60%, and deionized water is 95～40%; The mass ratio of the mixed powder of silicon carbide powder and sintering aid, dispersion agent, binding agent and defoamer is 1:(0.001～0.03): (0.005～0.03): (0.001～0.01); The massfraction of sintering aid is 1～50% in the mixed powder of silicon carbide powder and sintering aid.
Embodiment two: what present embodiment and embodiment one were different is: described sintering aid is Al
2O
3, BaO and rare earth oxide mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be silicon carbide powder and sintering aid the mixed powder quality 1～5%; Perhaps sintering aid is Al
2O
3, BaCO
3With the mixing of rare earth oxide, wherein Al
2O
3With BaCO
3The ratio of amount of substance be 1:1, the quality of rare earth oxide be silicon carbide powder and sintering aid the mixed powder quality 1～5%; Wherein rare earth oxide is Y
2O
3, G
D2O
3, Lu
2O
3, Eu
2O
3, CeO
2And Sm
2O
3In one or more press the combination of arbitrary proportion.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: described dispersion agent is Tetramethylammonium hydroxide or ammonium citrate.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: described defoamer is propyl carbinol or the trimethyl carbinol.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is: described binding agent is gelatin, polyvinyl alcohol or polyvinyl butyral acetal.Other is identical with embodiment one.
Embodiment six: preparation embodiment five described a kind of methods with porous silicon carbide ceramic of novel hole wall structure specifically prepare according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24～25 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 5～60%, and deionized water is 95～40%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:(0.001～0.03): (0.005～0.03): (0.001～0.01);
Described in the step 1 in the mixed powder massfraction of sintering aid be 1～50%;
Sintering aid is Al in the step 1
2O
3, BaO and rare earth oxide mixing, Al wherein
20
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 1～5%; Perhaps sintering aid is Al
2O
3, BaCO
3With the mixing of rare earth oxide, wherein Al
2O
3With BaCO
3The ratio of amount of substance be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 1～5%; Wherein rare earth oxide is Y
2O
3, Gd
2O
3, Lu
2O
3, Eu
2O
3, CeO
2And Sm
2O
3In one or more press the combination of arbitrary proportion;
Dispersion agent is Tetramethylammonium hydroxide or ammonium citrate in the step 1;
Binding agent is gelatin, polyvinyl alcohol or polyvinyl butyral acetal in the step 1;
Defoamer is propyl carbinol or the trimethyl carbinol in the step 1;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgased again 30 minutes, obtain sample, take out sample then, solidified 3～60 minutes under-200 ° of C～-10 ° C in temperature, be-10～40 ° of C in temperature again, pressure is lyophilize 1～4 day under the environment of 1～600Pa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 1～20 ° of C/min then, be heated to 800～1300 ° of C, be incubated 10～360 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charge into rare gas element, the control temperature rise rate is 1～20 ° of C/min, be heated to 1200～1500 ° of C, be incubated 0.5～4 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.2～3MPa, controlling temperature rise rate then is 1～20 ° of C/min, be warming up to 1700～1900 ° of C, be incubated 0.5～4 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure.
Embodiment seven: what present embodiment and embodiment six were different is: the median size that is silicon carbide powder in the step 1 is 0.4～100Um.Other is identical with embodiment six.
Embodiment eight: what present embodiment and embodiment six were different is: solidification mode adopts and evenly solidifies or ask solidification mode surely in the step 2.Other is identical with embodiment six.
Embodiment nine: what present embodiment and embodiment six were different is: rare gas element is nitrogen or argon gas in the step 4.Other is identical with embodiment six.
Embodiment ten: what present embodiment and embodiment six were different is: high purity inert gas is high pure nitrogen or high-purity argon gas in the step 5.Other is identical with embodiment six.
Adopt following examples and contrast experiment to verify beneficial effect of the present invention:
Embodiment one:
A kind of preparation method with porous silicon carbide ceramic of novel hole wall structure of present embodiment specifically prepares according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 30%, and deionized water is 70%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:0.006:0.01:0.001;
Wherein, silicon carbide powder is 4.2um for the commercially available prod median size; The massfraction of sintering aid is 20% in the mixed powder, and sintering aid is Al
2O
3, BaO and rare earth oxide mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 3%, rare earth oxide is Y
2O
3; Dispersion agent is Tetramethylammonium hydroxide; Binding agent is gelatin; Defoamer is propyl carbinol;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgases 30 minutes again, obtains sample, taking out sample then, solidified 10 minutes under-70 ° of C in temperature, is 40 ° of C in temperature again, pressure is lyophilize 2 days under the environment of lPa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 10 ° of C/min then, be heated to 850 ° of C, be incubated 120 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charges into rare gas element, and the control temperature rise rate is 10 ° of C/min, be heated to 1300 ° of C, be incubated 1 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination; Wherein, rare gas element is nitrogen;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.5MPa, controlling temperature rise rate then is 10 ° of C/min, be warming up to 1800 ° of C, be incubated 1 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure; Wherein, rare gas element is nitrogen.
The XRD diffraction spectrogram of the porous silicon carbide ceramic of the celsian-felspar original position combination that the present embodiment step 4 obtains as shown in Figure 1, wherein " ◆ " represents α-SiC, " ▲ " represents the porous silicon carbide ceramic of celsian-felspar original position combination, sem photograph is as shown in Figure 2; The sem photograph of the porous silicon carbide ceramic with novel hole wall structure of present embodiment preparation as shown in Figure 3, gas cell distribution figure is as shown in Figure 4.
The porosity of the porous silicon carbide ceramic with novel hole wall structure of present embodiment preparation is 48v0l%, and its bending strength is 63MPa.
Embodiment two:
A kind of preparation method with porous silicon carbide ceramic of novel hole wall structure of present embodiment specifically prepares according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 30%, and deionized water is 70%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:0.006:0.01:0.001;
Wherein, silicon carbide powder is 4.2 μ m for the commercially available prod median size; The massfraction of sintering aid is 20% in the mixed powder, and sintering aid is Al
2O
3, BaO and rare earth oxide mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 3%, rare earth oxide is Gd
2O
3; Dispersion agent is Tetramethylammonium hydroxide; Binding agent is gelatin; Defoamer is propyl carbinol;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgases 30 minutes again, obtains sample, taking out sample then, solidified 10 minutes under-70 ° of C in temperature, is 40 ° of C in temperature again, pressure is lyophilize 2 days under the environment of lPa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 10 ° of C/min then, be heated to 850 ° of C, be incubated 120 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charges into rare gas element, and the control temperature rise rate is 10 ° of C/min, be heated to 1300 ° of C, be incubated 1 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination; Wherein, rare gas element is nitrogen;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.5MPa, controlling temperature rise rate then is 10 ° of C/min, be warming up to 1800 ° of C, be incubated 1 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure; Wherein, rare gas element is nitrogen.
The porosity of the porous silicon carbide ceramic with novel hole wall structure of present embodiment preparation is 53v0l%, and its bending strength is 58MPa.
Embodiment three:
A kind of preparation method with porous silicon carbide ceramic of novel hole wall structure of present embodiment specifically prepares according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 30%, and deionized water is 70%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:0.006:0.01:0.001;
Wherein, silicon carbide powder is 4.2 μ m for the commercially available prod median size; The massfraction of sintering aid is 20% in the mixed powder, and sintering aid is Al
2O
3, BaO and rare earth nitride mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 3%, rare earth oxide is Lu
2O
3Dispersion agent is Tetramethylammonium hydroxide; Binding agent is gelatin; Defoamer is propyl carbinol;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgases 30 minutes again, obtains sample, taking out sample then, solidified 10 minutes under-70 ° of C in temperature, is 40 ° of C in temperature again, pressure is lyophilize 2 days under the environment of lPa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 10 ° of C/min then, be heated to 850 ° of C, be incubated 120 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charges into rare gas element, and the control temperature rise rate is 10 ° of C/min, be heated to 1300 ° of C, be incubated 1 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination; Wherein, rare gas element is nitrogen;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.5MPa, controlling temperature rise rate then is 10 ° of C/min, be warming up to 1800 ° of C, be incubated 1 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure; Wherein, rare gas element is nitrogen.
The porosity of the porous silicon carbide ceramic with novel hole wall structure of present embodiment preparation is 52vol%, and its bending strength is 5lMPa.
Embodiment four:
A kind of preparation method with porous silicon carbide ceramic of novel hole wall structure of present embodiment specifically prepares according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 10%, and deionized water is 90%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:0.006:0.01:0.001;
Wherein, silicon carbide powder is 4.2 μ m for the commercially available prod median size; The massfraction of sintering aid is 20% in the mixed powder, and sintering aid is Al
2O
3, BaO and rare earth oxide mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 3%, rare earth oxide is Y
2O
3Dispersion agent is the tetramethyl-oxyammonia; Binding agent is gelatin; Defoamer is propyl carbinol;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgases 30 minutes again, obtains sample, taking out sample then, solidified 10 minutes under-70 ° of C in temperature, is 40 ° of C in temperature again, pressure is lyophilize 2 days under the environment of lPa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 10 ° of C/min then, be heated to 850 ° of C, be incubated 120 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charges into rare gas element, and the control temperature rise rate is 10 ° of C/min, be heated to 1300 ° of C, be incubated 1 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination; Wherein, rare gas element is nitrogen;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.5MPa, controlling temperature rise rate then is 10 ° of C/min, be warming up to 1800 ° of C, be incubated 1 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure; Wherein, rare gas element is nitrogen.
The porosity of the porous silicon carbide ceramic with novel hole wall structure of present embodiment preparation is 78vol%, and its bending strength is 16MPa.
Embodiment five:
A kind of preparation method with porous silicon carbide ceramic of novel hole wall structure of present embodiment specifically prepares according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 20%, and deionized water is 80%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:0.006:0.01:0.001;
Wherein, silicon carbide powder is 4.2 μ m for the commercially available prod median size; The massfraction of sintering aid is 20% in the mixed powder, and sintering aid is Al
2O
3, BaO and rare earth nitride mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 3%, rare earth oxide is Y
2O
3Dispersion agent is Tetramethylammonium hydroxide; Binding agent is gelatin; Defoamer is propyl carbinol;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgases 30 minutes again, obtains sample, taking out sample then, solidified 10 minutes under-70 ° of C in temperature, is 40 ° of C in temperature again, pressure is lyophilize 2 days under the environment of lPa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 10 ° of C/min then, be heated to 850 ° of C, be incubated 120 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charges into rare gas element, and the control temperature rise rate is 10 ° of C/min, be heated to 1300 ° of C, be incubated 1 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination; Wherein, rare gas element is nitrogen;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.5MPa, controlling temperature rise rate then is 10 ° of C/min, be warming up to 1800 ° of C, be incubated 1 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure; Wherein, rare gas element is nitrogen.
The porosity of the porous silicon carbide ceramic with novel hole wall structure of present embodiment preparation is 71vol%, and its bending strength is 19MPa.
Embodiment six:
A kind of preparation method with porous silicon carbide ceramic of novel hole wall structure of present embodiment specifically prepares according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 30%, and deionized water is 70%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:0.006:0.01:0.001;
Wherein, silicon carbide powder is 4.2 μ m for the commercially available prod median size; The massfraction of sintering aid is 10% in the mixed powder, and sintering aid is Al
2O
3, BaO and rare earth oxide mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 3%, rare earth oxide is Y
2O
3Dispersion agent is the tetramethyl-oxyammonia; Binding agent is gelatin; Defoamer is propyl carbinol;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgases 30 minutes again, obtains sample, taking out sample then, solidified 10 minutes under-70 ° of C in temperature, is 40 ° of C in temperature again, pressure is lyophilize 2 days under the environment of lPa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 1O ° of C/min then, be heated to 850 ° of C, be incubated 120 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charges into rare gas element, and the control temperature rise rate is 10 ° of C/min, be heated to 1300 ° of C, be incubated 1 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination; Wherein, rare gas element is nitrogen;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.5MPa, controlling temperature rise rate then is 10 ° of C/min, be warming up to 1800 ° of C, be incubated 1 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure; Wherein, rare gas element is nitrogen.
The porosity of the porous silicon carbide ceramic with novel hole wall structure of present embodiment preparation is 62vol%, and its bending strength is 2gMPa.
Embodiment seven:
A kind of preparation method with porous silicon carbide ceramic of novel hole wall structure of present embodiment specifically prepares according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 10%, and deionized water is 90%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:0.006:0.01:0.001;
Wherein, silicon carbide powder is 4.2 μ m for the commercially available prod median size; The massfraction of sintering aid is 10% in the mixed powder, and sintering aid is Al
2O
3, BaO and rare earth nitride mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 3%, rare earth oxide is Y
2O
3Dispersion agent is the tetramethyl-oxyammonia; Binding agent is gelatin; Defoamer is propyl carbinol;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgases 30 minutes again, obtains sample, taking out sample then, solidified 10 minutes under-70 ° of C in temperature, is 40 ° of C in temperature again, pressure is lyophilize 2 days under the environment of lPa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck is levied in the air then, and the control temperature rise rate is 10 ° of C/min, be heated to 850 ° of C, be incubated 120 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charges into rare gas element, and the control temperature rise rate is 10 ° of C/min, be heated to 1300 ° of C, be incubated 1 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination; Wherein, rare gas element is nitrogen;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.5MPa, controlling temperature rise rate then is 10 ° of C/min, be warming up to 1800 ° of C, be incubated 1 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure; Wherein, rare gas element is nitrogen.
The porosity of the porous silicon carbide ceramic with novel hole wall structure of present embodiment preparation is 82vol%, and its bending strength is gMPa.
Claims (10)
1. porous silicon carbide ceramic with novel hole wall structure, it is characterized in that a kind of porous silicon carbide ceramic with novel hole wall structure is raw material with silicon carbide powder and sintering aid, adopt freezing casting moulding, sintering is prepared from after drying, in the slurry of freezing cast, according to volume percent, the mixed powder of silicon carbide powder and sintering aid is 5～60%, and deionized water is 95～40%; The mass ratio of the mixed powder of silicon carbide powder and sintering aid, dispersion agent, binding agent and defoamer is 1:(0.001～0.03): (0.005～0.03): (0.001～0.01); The massfraction of sintering aid is 1～50% in the mixed powder of silicon carbide powder and sintering aid.
2. a kind of porous silicon carbide ceramic with novel hole wall structure according to claim 1 is characterized in that described sintering aid is Al
2O
3, BaO and rare earth oxide mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be silicon carbide powder and sintering aid the mixed powder quality 1～5%; Perhaps sintering aid is Al
2O
3, BaCO
3With the mixing of rare earth oxide, wherein Al
2O
3With BaCO
3The ratio of amount of substance be 1:1, the quality of rare earth oxide be silicon carbide powder and sintering aid the mixed powder quality 1～5%; Wherein rare earth oxide is Y
2O
3, Gd
2O
3, Lu
2O
3, Eu
2O
3, CeO
2And Sm
2O
3In one or more press the combination of arbitrary proportion.
3. a kind of porous silicon carbide ceramic with novel hole wall structure according to claim 1 is characterized in that described dispersion agent is Tetramethylammonium hydroxide or ammonium citrate.
4. a kind of porous silicon carbide ceramic with novel hole wall structure according to claim 1 is characterized in that described defoamer is propyl carbinol or the trimethyl carbinol.
5. a kind of porous silicon carbide ceramic with novel hole wall structure according to claim 1 is characterized in that described binding agent is gelatin, polyvinyl alcohol or polyvinyl butyral acetal.
6. the described a kind of method with porous silicon carbide ceramic of novel hole wall structure of preparation claim 1 is characterized in that a kind of preparation method with porous silicon carbide ceramic of novel hole wall structure, specifically prepares according to following steps:
One, silicon carbide powder is mixed with sintering aid, obtain mixed powder, again mixed powder is mixed with deionized water, add dispersion agent, binding agent and defoamer then, and adding silicon carbide ball carries out ball milling, the control ball milling time is 24～25 hours, obtain finely dispersed slurry, wherein, according to volume percent, mixed powder is 5～60%, and deionized water is 95～40%; The mass ratio of mixed powder, dispersion agent, binding agent and defoamer is 1:(0.001～0.03): (0.005～0.03) (0.001～0.01);
Described in the step 1 in the mixed powder massfraction of sintering aid be 1～50%;
Sintering aid is Al in the step 1
2O
3, BaO and rare earth oxide mixing, Al wherein
2O
3With the ratio of the amount of substance of BaO be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 1～5%; Perhaps sintering aid is Al
2O
3, BaCO
3With the mixing of rare earth oxide, wherein Al
2O
3With BaCO
3The ratio of amount of substance be 1:1, the quality of rare earth oxide be in the step 1 mixed powder quality 1～5%; Wherein rare earth oxide is Y
2O
3, Gd
2O
3, Lu
2O
3, Eu
2O
3, CeO
2And Sm
2O
3In one or more press the combination of arbitrary proportion;
Dispersion agent is Tetramethylammonium hydroxide or ammonium citrate in the step 1;
Binding agent is gelatin, polyvinyl alcohol or polyvinyl butyral acetal in the step 1;
Defoamer is propyl carbinol or the trimethyl carbinol in the step 1;
Two, the slurry that step 1 is obtained is poured casting in the mould into, outgased again 30 minutes, obtain sample, take out sample then, solidified 3～60 minutes under-200 ° of C～-10 ° C in temperature, be-10～40 ° of C in temperature again, pressure is lyophilize 1～4 day under the environment of 1～600Pa, obtains the porous silicon carbide ceramic green compact;
Three, the porous silicon carbide ceramic green compact that step 2 the obtained processing of coming unstuck, in air, the control temperature rise rate is 1～20 ° of C/min then, be heated to 800～1300 ° of C, be incubated 10～360 minutes and carry out oxide treatment, furnace cooling obtains preoxidation porous silicon carbide ceramic base substrate again;
Four, the preoxidation porous silicon carbide ceramic base substrate that step 3 is obtained is put into the atmosphere heat treatment stove, charge into rare gas element, the control temperature rise rate is 1～20 ° of C/min, be heated to 1200～1500 ° of C, be incubated 0.5～4 hour, furnace cooling again obtains the porous silicon carbide ceramic of celsian-felspar original position combination;
The porous silicon carbide ceramic of the celsian-felspar original position combination that five, step 4 is obtained is put into the gas pressure sintering stove, charge into the high purity inert gas that pressure is 0.2～3MPa, controlling temperature rise rate then is 1～20 ° of C/min, be warming up to 1700～1900 ° of C, be incubated 0.5～4 hour, furnace cooling again obtains having the porous silicon carbide ceramic of novel hole wall structure.
7. a kind of preparation method with porous silicon carbide ceramic of novel hole wall structure according to claim 6, the median size that it is characterized in that silicon carbide powder in the step 1 is 0.4～100um.
8. a kind of preparation method with porous silicon carbide ceramic of novel hole wall structure according to claim 6, it is characterized in that in the step 2 that solidification mode adopts evenly solidifies or asks solidification mode surely.
9. a kind of preparation method with porous silicon carbide ceramic of novel hole wall structure according to claim 6 is characterized in that rare gas element is nitrogen or chlorine in the step 4.
10. a kind of preparation method with porous silicon carbide ceramic of novel hole wall structure according to claim 6 is characterized in that high purity inert gas is high pure nitrogen or high pure nitrogen in the step 5.
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