CN102503521B - Preparation method of high-strength silicon carbide porous ceramic - Google Patents
Preparation method of high-strength silicon carbide porous ceramic Download PDFInfo
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- CN102503521B CN102503521B CN 201110375104 CN201110375104A CN102503521B CN 102503521 B CN102503521 B CN 102503521B CN 201110375104 CN201110375104 CN 201110375104 CN 201110375104 A CN201110375104 A CN 201110375104A CN 102503521 B CN102503521 B CN 102503521B
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 95
- 239000000919 ceramic Substances 0.000 title claims abstract description 71
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 229910021431 alpha silicon carbide Inorganic materials 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052710 silicon Inorganic materials 0.000 claims description 17
- 239000010703 silicon Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 12
- XGNZNBRDPPLKTC-UHFFFAOYSA-N aluminium diboride Chemical compound [Al]1B=B1 XGNZNBRDPPLKTC-UHFFFAOYSA-N 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- -1 silicon carbide compound Chemical class 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 238000001272 pressureless sintering Methods 0.000 abstract 1
- 241000264877 Hippospongia communis Species 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000006872 improvement Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011800 void material Substances 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 206010020852 Hypertonia Diseases 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910007948 ZrB2 Inorganic materials 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of a high-strength silicon carbide porous ceramic. Raw materials are composed of 98%-99% of mixture of alpha-silicon carbide powder and beta-silicon carbide powder, 0.1%-1.0% of aluminum diboride and 0.5%-1% of polycarbosilane, by weight percent. The method comprises the following steps: 1) adding the raw materials into an organic dispersing solvent, ball-milling, mixing and drying; 2) dry-pressing and forming the obtained silicon carbide compound powder under the 45-55 MPa; and 3) placing a silicon carbide blank into a vacuum pressure-less sintering furnace, for sintering at two steps, thereby obtaining the high-strength silicon carbide porous ceramic. The preparation method is simple and the prepared silicon carbide porous ceramic is characterized by high mechanical strength, suitable porosity, and the like.
Description
Technical field
The bright a kind of high-strength carborundum porous ceramics and preparation method thereof that relates to of we specifically, relates to the Carboround material preparation method of purposes such as a kind of purifying vehicle exhaust, high temperature filtration, heat exchange.
Background technology
Carborundum porous ceramics is to form by carry out artificial controlled pore-creating in the silicon carbide ceramics matrix, novel silicon carbide functional materials with certain porosity, it not only has the high strength of silicon carbide itself, anticorrosive, anti-oxidant, physical and chemical performance such as heat-shock resistance and high thermal resistance, but also possesses low density, high strength, high porosity, hypertonicity, specific surface area is big, good characteristics such as thermal insulation, can be used as the high temperature gas cleaning device, the solid particle filter of diesel emission, filter for molten metal, heat exchanger, sensor, insulation and sound-proof material, the support of the catalyst of vehicle exhaust etc. have obtained using widely in the modern industry field.
Obtain the existing more report of patent of ceramic honey comb and preparation thereof about carborundum porous ceramics.Reported silicon carbide ceramics and the lqiuid phase sintering method thereof that contains the synthetic C-B-Al compound phase of reaction as publication number CN1369463.CN101333112 has reported the combustion synthesis method of preparation carborundum porous ceramics.CN101323524 has reported a kind of preparation method of oriented hole silicon carbide porous ceramic.CN1442392 has reported with the yeast powder to be the preparation method of the carborundum porous ceramics of pore-forming material.CN102219543A has reported a kind of preparation method who can be used as the carborundum porous ceramics of high-temperature smoke strainer.CN1769241 has reported that in-situ reaction prepares the carborundum porous ceramics of mullite bonded.CN1654432 has reported a kind of preparation method of silicon nitride/silicon carbide porous ceramic.CN201780040U has reported the silicon carbide honeycomb ceramics heat exchanger.CN1807356 and CN101747078A have reported the manufacture method of high purity silicon carbide honeycomb ceramic body using nanometer silicon carbide as sintering adjuvant.CN102010222A has reported a kind of carborundum porous ceramics and preparation method thereof.CN101607158 has reported a kind of silicon carbide porous ceramic filter and manufacture method thereof.CN101406782 has reported preparation method and the extrusion equipment of silicon carbide porous ceramic filtering element.CN1341578 has reported a kind of method for preparing silicon carbide porous ceramic pipe.
Above-mentioned patent obtains fine progress at porous ceramics or ceramic honey comb and application facet, but porous ceramics adopts organism pore-creating or reaction in to come pore-creating or foaming pore-creating mostly, aspect ceramic honey comb, add a large amount of organism, though this pore-creating is satisfactory for result, but directly can cause the reduction of porous ceramics or ceramic honey comb physical strength, physical strength is about 20MPa mostly, though there are some porous ceramics energy can reach 50MPa, but apparent porosity is very low (only being about 20%) obviously, and these all greatly limit the application of porous ceramics or ceramic honey comb.Exploitation physical strength height, the moderate carborundum porous ceramics of void content have become the developing direction in this field.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of high-strength carborundum porous ceramics; This method technology is simple, and prepared carborundum porous ceramics has characteristics such as physical strength height, porosity be moderate.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of high-strength carborundum porous ceramics, be 98%~99% the mixture of being formed by alpha-silicon carbide powder and silicon B-carbide powder, 0.1%~1.0% aluminium diboride and 0.5%~1% Polycarbosilane constitutive material with weight percentage, may further comprise the steps successively:
1), above-mentioned raw materials is joined in organic dispersion solvent, ball milling carried out drying 22~26 hours at 35~45 ℃ after mixing, and obtained silicon carbide composite powder body;
2), above-mentioned silicon carbide composite powder body is carried out dry-pressing formed under 45~55MPa, obtain the silicon carbide base substrate;
3), above-mentioned silicon carbide base substrate is put into vacuum non-pressure sintering furnace, carry out two-step sintering, obtain the high-strength carborundum porous ceramics.
Improvement as the preparation method of high-strength carborundum porous ceramics of the present invention: in the mixture of being formed by alpha-silicon carbide powder and silicon B-carbide powder, the weight content of alpha-silicon carbide powder is 50%~90%, and the weight content of silicon B-carbide powder is 10%~50%.
Further improvement as the preparation method of high-strength carborundum porous ceramics of the present invention: two-step sintering is: be warming up to 1450~1500 ℃ of vacuum outgass 3~5 hours earlier, be warming up to 2150~2250 ℃ of sintering 30~60 minutes under argon shield then.
Further improvement as the preparation method of high-strength carborundum porous ceramics of the present invention: organic dispersion solvent is the mixed solvent of being made up of ethanol, dimethylbenzene and normal hexane.The volume ratio of ethanol, dimethylbenzene and normal hexane can be 1: 3~and 4: 5~6.The ratio of organic dispersion solvent and raw material allocates arbitrarily that (general solid-liquid ratio with raw material formation is: 1g raw material/3~5 milliliter organic dispersion solvent).
Further improvement as the preparation method of high-strength carborundum porous ceramics of the present invention: the ball milling mixing time of step 1) is 24~28 hours.
Method technology of the present invention is simple, and prepared carborundum porous ceramics physical strength height, porosity are moderate, is purifying vehicle exhaust carrier, high temperature filtration, heat exchange desirable material.
High-strength carborundum porous ceramics of the present invention has the following advantages:
1) utilize the carborundum grain growth to realize the densification of silicon carbide ceramics, at high temperature, silicon B-carbide can change alpha-silicon carbide into and promote the carborundum grain growth, and aluminium diboride also can promote the carborundum grain growth, utilize the transformation of silicon carbide crystalline phase and aluminium diboride can both promote the acting in conjunction of carborundum grain growth, thereby realize the sintering of carborundum porous ceramics, this is different from other and adopts sintering aid to carry out the method for sintering.
2) utilize Polycarbosilane to carry out suitable pore-creating, made carborundum porous ceramics that certain porosity is arranged owing to utilize the grain growing mode to carry out sintering, the recycling Polycarbosilane at high temperature is cracked into SiC, and produce suitable hole by it, and carborundum porous ceramics is carried out pore-creating control, realize the controlled of carborundum porous ceramics porosity.
3) physical strength of carborundum porous ceramics can reach more than the 60MPa, void content is between 40%~55%, be enough to satisfy purifying vehicle exhaust carrier, high temperature filtration, heat exchange to the requirement of the mechanical property of materials and void content, and production technique is simple, can adapt to suitability for industrialized production.
In sum, the present invention utilizes silicon B-carbide at high temperature to change alpha-silicon carbide into can promote the carborundum grain growth, and aluminium diboride promotes the trend of carborundum grain growth, and the sintering of realization carborundum porous ceramics, and utilize the Polycarbosilane Pintsch process to become SiC and realize pore-creating, thereby prepare physical strength height, the moderate carborundum porous ceramics of void content.This method technology is simple, and prepared carborundum porous ceramics physical strength height, porosity are moderate, is purifying vehicle exhaust carrier, high temperature filtration, heat exchange desirable material.
Embodiment
The median size of used alpha-silicon carbide powder, silicon B-carbide powder, aluminium diboride is respectively 0.7~0.8 μ mm, 0.2~0.3 μ m, 0.4~0.6 μ m in following examples, and Polycarbosilane is liquid.
The preparation method of embodiment 1, a kind of high-strength carborundum porous ceramics is 49.5% alpha-silicon carbide powder, 49.4% silicon B-carbide powder, 0.1% aluminium diboride and 1.0% Polycarbosilane constitutive material with weight percentage, carries out following steps successively:
1), above-mentioned raw materials is joined in organic dispersion solvent that ethanol, dimethylbenzene, normal hexane forms according to 1: 4: 5 volume ratio, ball milling mixed after 24 hours, and 40 ℃ of dryings 24 hours obtain silicon carbide composite powder body; The solid-liquid ratio of raw material and organic dispersion solvent is 1g/3ml;
2), dry-pressing formed under 50MPa to silicon carbide composite powder body, obtain the silicon carbide base substrate;
3), above-mentioned silicon carbide base substrate is put into vacuum non-pressure sintering furnace, be warming up to 1500 ℃ of vacuum outgass 4 hours earlier, be warming up to 2200 ℃ of sintering 45 minutes under argon shield then, be prepared from carborundum porous ceramics.
This carborundum porous ceramics physical strength is 61MPa, and porosity is 55%.
The preparation method of embodiment 2, a kind of high-strength carborundum porous ceramics is 88.65% alpha-silicon carbide powder, 9.85% silicon B-carbide powder, 0.5% aluminium diboride and 1.0% Polycarbosilane constitutive material with weight percentage, carries out following steps successively:
1), above-mentioned raw materials is joined in organic dispersion solvent that ethanol, dimethylbenzene, normal hexane forms according to 1: 3: 6 volume ratio, ball milling mixed after 24 hours, and 40 ℃ of dryings 24 hours obtain silicon carbide composite powder body; The solid-liquid ratio of this raw material and organic dispersion solvent is 1g/5ml;
2), dry-pressing formed under 50MPa to silicon carbide composite powder body, obtain the silicon carbide base substrate;
3), above-mentioned silicon carbide base substrate is placed in the vacuum non-pressure sintering furnace, be warming up to 1500 ℃ of vacuum outgass 3 hours earlier, be warming up to 2200 ℃ of sintering 50 minutes under argon shield then, be prepared from carborundum porous ceramics.
This carborundum porous ceramics physical strength is 65MPa, and porosity is 55%.
The preparation method of embodiment 3, a kind of high-strength carborundum porous ceramics, by weight percentage be: 68.95% alpha-silicon carbide powder, 29.55% silicon B-carbide powder, 1.0% aluminium diboride and 0.5% Polycarbosilane constitutive material, carry out following steps successively:
1), above-mentioned raw materials is joined in organic dispersion solvent that ethanol, dimethylbenzene, normal hexane forms according to 1: 3.5: 5.5 volume ratio, ball milling mixed after 24 hours, and 40 ℃ of dryings 24 hours obtain silicon carbide composite powder body; The solid-liquid ratio of this raw material and organic dispersion solvent is 1g/5ml;
2), dry-pressing formed under 50MPa to silicon carbide composite powder body, obtain the silicon carbide base substrate;
3), above-mentioned silicon carbide base substrate is placed in the vacuum non-pressure sintering furnace, be warming up to 1500 ℃ of vacuum outgass 5 hours earlier, be warming up to 2200 ℃ of sintering 40 minutes under argon shield then, be prepared from carborundum porous ceramics.
This carborundum porous ceramics physical strength is to more than the 68MPa, and porosity is 42%.
Comparative Examples 1, the silicon B-carbide powder of cancellation among the embodiment 2 make the weight percentage of alpha-silicon carbide powder into 98.5% by 88.65%.All the other are with embodiment 2.
This carborundum porous ceramics physical strength is 41MPa, and porosity is 44%.
Comparative Examples 2, with 88.65% alpha-silicon carbide powder among the embodiment 2,9.85% silicon B-carbide powder corresponding 94% alpha-silicon carbide powder, the 3.5% silicon B-carbide powder of making into respectively.All the other are with embodiment 2.
This carborundum porous ceramics physical strength is to 49MPa, and porosity is 43%.
Comparative Examples 3, with 88.65% alpha-silicon carbide powder among the embodiment 2,9.85% silicon B-carbide powder corresponding 39.4% alpha-silicon carbide powder, the 59.1% silicon B-carbide powder of making into respectively.All the other are with embodiment 2.
This carborundum porous ceramics physical strength is to 45MPa, and porosity is 50%.
Comparative Examples 4, make 0.5% aluminium diboride among the embodiment 2 into 0.5% zirconium diboride.All the other are with embodiment 2.
This carborundum porous ceramics physical strength is to 20MPa, and porosity is 53%.
Comparative Examples 5, make 0.5% aluminium diboride among the embodiment 2 into 0.5% aluminum borate.All the other are with embodiment 2.
This carborundum porous ceramics physical strength is to 25MPa, and porosity is 55%.
The use of aluminium diboride among Comparative Examples 6, the cancellation embodiment 2 makes the content of Polycarbosilane into 1.5% by 1.0%.All the other are with embodiment 2.
This carborundum porous ceramics physical strength is to 15MPa, and porosity is 61%.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (3)
1. the preparation method of high-strength carborundum porous ceramics is characterized in that: be 98%~99% the mixture of being made up of alpha-silicon carbide powder and silicon B-carbide powder, 0.1%~1.0% aluminium diboride and 0.5%~1% Polycarbosilane constitutive material with weight percentage; In the described mixture of being made up of alpha-silicon carbide powder and silicon B-carbide powder, the weight content of alpha-silicon carbide powder is 50% ~ 90%, and the weight content of silicon B-carbide powder is 10% ~ 50%; May further comprise the steps successively:
1), above-mentioned raw materials is joined in organic dispersion solvent, ball milling carried out drying 22 ~ 26 hours at 35 ~ 45 ℃ after mixing, and obtained silicon carbide composite powder body;
2), above-mentioned silicon carbide composite powder body is carried out dry-pressing formed under 45 ~ 55MPa, obtain the silicon carbide base substrate;
3), above-mentioned silicon carbide base substrate is put into vacuum non-pressure sintering furnace, carry out two-step sintering, obtain the high-strength carborundum porous ceramics;
Described two-step sintering is: be warming up to 1450 ~ 1500 ℃ of vacuum outgass 3 ~ 5 hours earlier, be warming up to 2150 ~ 2250 ℃ of sintering 30 ~ 60 minutes under argon shield then.
2. the preparation method of high-strength carborundum porous ceramics according to claim 1 is characterized in that: the mixed solvent of described organic dispersion solvent for being made up of ethanol, dimethylbenzene and normal hexane.
3. the preparation method of high-strength carborundum porous ceramics according to claim 2, it is characterized in that: the ball milling mixing time of described step 1) is 24 ~ 28 hours.
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