CN101805201B - Preparation method of porous silicon carbide ceramics with high thermal shock resistance - Google Patents
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- CN101805201B CN101805201B CN2010101525494A CN201010152549A CN101805201B CN 101805201 B CN101805201 B CN 101805201B CN 2010101525494 A CN2010101525494 A CN 2010101525494A CN 201010152549 A CN201010152549 A CN 201010152549A CN 101805201 B CN101805201 B CN 101805201B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 46
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 38
- 230000035939 shock Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000002243 precursor Substances 0.000 claims abstract description 22
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 21
- 239000011258 core-shell material Substances 0.000 claims abstract description 20
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 92
- 229910052786 argon Inorganic materials 0.000 claims description 46
- 238000002156 mixing Methods 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 24
- 229960001866 silicon dioxide Drugs 0.000 claims description 18
- 238000003763 carbonization Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 239000011435 rock Substances 0.000 claims description 2
- 238000009725 powder blending Methods 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 17
- 238000001816 cooling Methods 0.000 description 12
- 238000009413 insulation Methods 0.000 description 11
- 239000000758 substrate Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 229920003987 resole Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound 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
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of porous silicon carbide ceramics with high thermal shock resistance, belonging to the technical field of preparation of porous silicon carbide ceramics. Precursor powder, aluminum oxide, silicon dioxide and yttrium oxide of a core-shell structure of the silicon-resin prepared by the current coat mix process are mixed according to the mass ratio range of 100:(0.5-10):(0.1-5), and then, the mixed powder is treated by pressure forming, carbonizing and sintering to obtain the porous silicon carbide ceramics with high thermal shock resistance. The invention lowers the sintering temperature to 1200-1800 DEG C, obviously increases the thermal conductivity of the ceramics, improves the thermal shock resistance, and loses 6.5-30% of strength after 30 times of thermal shock at 800 DEG C. The prepared porous silicon carbide ceramics have the characteristics that the porosity is greater than 80%, the average pore size is 100-300mu m, and the pore size distribution is uniform. The method has the advantages of simple processes, little additive amount of assistants and obvious effect.
Description
Technical field
The invention belongs to the porous silicon carbide ceramic preparing technical field, particularly a kind of preparation method of porous silicon carbide ceramics with high thermal shock resistance.
Background technology
Porous silicon carbide ceramic has following characteristics: have uniform tridimensional network, void content high, have cold working such as big continuous hole, the pressure-losses are little, energising is heatable (littler than resistance, resistivity is generally 1-2 Ω cm under the room temperature situation), high thermal resistance is good, thermal conductivity is high, good resistance to chemical corrosion, cutting, boring easily, with the contact area of liquid greatly, have micropore (the skeleton volume accounts for 30%) in the skeleton.
(like strong corrosive media, high temperature, high radiation property etc.) will obtain application more and more widely to porous silicon carbide ceramic in some harsh fields.As in field of metallurgy, it can be used as filter for molten metal, iron notch, tap hole, cold slide rail and distiller etc.; In silicate industry porous silicon carbide ceramic can be in a large number as the liner of various kilns and saggar etc.; In chemical industry, can be used as oil gas generator, incinerator and oil gasification device etc.; Can be on space technology as rocket nozzle and high-temperature fuel gas turbine blade etc.; In the HTGR in nuclear energy field especially Tsing-Hua University's independent research, can filter the HTGR fuel element and prepare the high temperature helium that contains graphite granule in the radioactive liquid waste that produces in the process and the HTGR etc. as strainer.Porous silicon carbide ceramic can have the premium properties of ceramic foam and carbofrax material concurrently, is a kind of important functional material, can be widely used in filtering flow, especially is considered to one of optimal candidate material as the diesel engine vent gas strainer.
The preparation method of porous silicon carbide has bibliographical information both at home and abroad always.Like Chinese patent (application number: 200610119233.9) reported a kind of method of preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process; This method gained porous silicon carbide ceramic has the pore texture of orientation, interconnection; Porosity is higher, but complex process, purity is not high." Materials Characterization, 2008,59 (2): 140-143 " have been reported and a kind ofly under 1400～1550 ℃, have been used Al
2O
3Make additive, make the reaction of oxidized silicon-dioxide that forms of silicon carbide and aluminum oxide generate mullite and form the sintering neck, obtain that pore size distribution is narrower, the carborundum porous ceramics of mean pore size 1.9 μ m.Improve sintering temperature and can increase the intensity of ceramic foam, but can reduce its open-cell porosity, and the ceramic foam purity that this method obtains is not high.Chinese patent (application number: 200510076993.1) adopt bag to mix prepared and have the precursor powder of silicon-resin core shell structure, obtain the porous silicon carbide ceramic of high porosity (greater than 80%) again through moulding, carbonization and high temperature sintering prepared in reaction.This method technology is simple, production efficiency is high, energy-conservation, Environmental compatibility good, be a kind of method that can prepare porous silicon carbide ceramic with high porosity, but sintering temperature is higher, the product heat-shock resistance is relatively poor.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of porous silicon carbide ceramics with high thermal shock resistance; It is characterized in that the silicon-resin core shell structure precursor powder that mixes prepared with existing bag is a raw material; And in above-mentioned raw materials, add aluminum oxide, silicon-dioxide and yttrium oxide as additive; Wherein, the quality of precursor powder, aluminum oxide, silicon-dioxide, yttrium oxide is 100 than scope: (0.5～10): (0.1～5): (0.1～5), and after powder mixing, pressure forming, charing processing and four step process of sintering; Obtain porous silicon carbide ceramics with high thermal shock resistance, concrete process step is following:
(1) will have the silicon-resin core shell structure precursor powder that wraps mixed prepared is 100 according to quality than scope with aluminum oxide, silicon-dioxide and yttrium oxide: (0.5～10): (0.1～5): mix (0.1～5); Method for mixing is manual or mechanical stirring, ball milling or rocks and make it even that mixing time is 5 minutes～24 hours;
(2) mixed powder gets ceramic green through pressure forming, the pressure molding condition: mixed powder is 50～140 ℃ through the green compact mold temperature of pressure forming, and compacting pressure is 0.5～50MPa, and soaking time is 20～120min;
(3) ceramic green carries out the charing processing, and the charing treatment process condition is following: carbonization temperature is 600～1000 ℃, and temperature rise rate is 0.3～3 ℃/min; Argon flow amount is 5～200ml/min, and soaking time is 1～4h.
(4) charing is carried out sintering after handling, and sintering carries out in argon gas atmosphere or vacuum, air pressure: 0～20MPa, and temperature rise rate: 1-20 ℃/min, sintering temperature: 1200～1800 ℃, soaking time: 1～4 hour, obtain porous silicon carbide ceramics with high thermal shock resistance.
Existing bag mixes the silicon-resin core shell structure precursor powder of prepared; With silica flour, resol and alcohol is raw material, and above-mentioned raw materials is by mass ratio 1: (0.25～1.1): 2 are mixed into slurry adopts bag to mix technology to wrap to mix and obtain silicon powder surface and coat silicon-resin core shell structure precursor powder that complete sum coats imperfect resin again.Its concrete preparation process can be the step that preparation resol bag mixes the powder of silica flour in 200510076993.1 the patent with reference to application number.It is subsequent use to prepare silicon-resin core shell structure precursor powder.
Beneficial effect of the present invention is: the present invention mixes prepared at bag to have on the basis of silicon-resin core shell structure precursor powder; Add additive aluminum oxide, silicon-dioxide and yttrium oxide; The liquid phase of utilizing additive when high temperature, to form has promoted sintering reaction to carry out, and has reduced sintering temperature (1200～1800 ℃), and after cooling, has formed new solid phase; Obviously increased ceramic thermal conductivity, thereby made its heat-shock resistance improve (30 losss of strength 6.5～30% of 800 ℃ of thermal shocks).And the high porosity of original technology (greater than 80%), mean pore size all is able to keep in advantages such as 100～300 μ m and even aperture distribution.
The present invention has reduced the reaction sintering temperature, and has obtained advantages such as maintenance existing product porosity is high, pore size is controlled, and thermal conductivity is higher, the better porous silicon carbide ceramic of heat-shock resistance.Present method technology is simple, and additive dosage is few, and effect is obvious.
Embodiment
Below in conjunction with embodiment the present invention is described further:
Embodiment 1
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 0.5: 0.1: 0.1, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 100 ℃, heat-insulation pressure keeping 20min makes green compact under the 1MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 5ml/min, 0.5 ℃/min of temperature rise rate, 600 ℃ of carbonization temperatures are incubated 4 hours.At last base substrate is carried out vacuum sintering in the stove of crossing with the high-purity argon air purge, 5 ℃/min of temperature rise rate, 1200 ℃ of sintering temperatures are incubated 4 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 2
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 2: 0.3: 0.1, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 80 ℃, heat-insulation pressure keeping 30min makes green compact under the 5MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 5ml/min, 0.5 ℃/min of temperature rise rate, 600 ℃ of carbonization temperatures are incubated 3 hours.At last base substrate is carried out vacuum sintering in the stove of crossing with the high-purity argon air purge, 2 ℃/min of temperature rise rate, 1300 ℃ of sintering temperatures are incubated 4 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 3
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 2: 0.3: 0.3, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 140 ℃, heat-insulation pressure keeping 40min makes green compact under the 7.5MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 15ml/min, 1 ℃/min of temperature rise rate, 700 ℃ of carbonization temperatures are incubated 3 hours.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min; 10 ℃/min of temperature rise rate; 1400 ℃ of sintering temperatures are incubated 4 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 4
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 3: 1: 0.5, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 130 ℃, heat-insulation pressure keeping 40min makes green compact under the 7.5MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 15ml/min, 2 ℃/min of temperature rise rate, 800 ℃ of carbonization temperatures are incubated 2 hours.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min; 10 ℃/min of temperature rise rate; 1400 ℃ of sintering temperatures are incubated 4 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 5
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 4: 2: 1, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 100 ℃, heat-insulation pressure keeping 60min makes green compact under the 10MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 15ml/min, 2 ℃/min of temperature rise rate, 800 ℃ of carbonization temperatures are incubated 2 hours.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min; 15 ℃/min of temperature rise rate; 1500 ℃ of sintering temperatures are incubated 3 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 6
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 5: 3: 2, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 110 ℃, heat-insulation pressure keeping 40min makes green compact under the 7.5MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 20ml/min, 3 ℃/min of temperature rise rate, 800 ℃ of carbonization temperatures are incubated 2 hours.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min; 15 ℃/min of temperature rise rate; 1500 ℃ of sintering temperatures are incubated 2.5 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 7
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 6: 4: 3, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 50 ℃, heat-insulation pressure keeping 120min makes green compact under the 8MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 25ml/min, 3 ℃/min of temperature rise rate, 900 ℃ of carbonization temperatures are incubated 2 hours.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min; 15 ℃/min of temperature rise rate; 1600 ℃ of sintering temperatures are incubated 2.5 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 8
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 7: 4: 3, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 60 ℃, heat-insulation pressure keeping 120min makes green compact under the 8MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 25ml/min, 3 ℃/min of temperature rise rate, 900 ℃ of carbonization temperatures are incubated 2 hours.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min; 20 ℃/min of temperature rise rate; 1600 ℃ of sintering temperatures are incubated 2 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 9
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 8: 4: 5, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 110 ℃, heat-insulation pressure keeping 60min makes green compact under the 8MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 25ml/min, 2 ℃/min of temperature rise rate, 900 ℃ of carbonization temperatures are incubated 1.5 hours.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min; 15 ℃/min of temperature rise rate; 1700 ℃ of sintering temperatures are incubated 2 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 10
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 9: 4: 3, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 130 ℃, heat-insulation pressure keeping 40min makes green compact under the 8MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 25ml/min, 1 ℃/min of temperature rise rate, 1000 ℃ of carbonization temperatures are incubated 1 hour.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min; 10 ℃/min of temperature rise rate; 1700 ℃ of sintering temperatures are incubated 1.5 hours, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Embodiment 11
The precursor powder that bag is mixed silicon-resin core shell structure that technology makes mixes with aluminum oxide, silicon-dioxide, yttrium oxide, and the mixing quality ratio is 100: 10: 5: 5, and adopt ball mill to make its mixing 24 hours.Again with mixed powder at 140 ℃, heat-insulation pressure keeping 20min makes green compact under the 8MPa.Then green compact are carried out charing under argon gas atmosphere and handle, argon flow amount 25ml/min, 1 ℃/min of temperature rise rate, 1000 ℃ of carbonization temperatures are incubated 1 hour.At last base substrate is carried out high temperature sintering in argon gas atmosphere, air pressure is a normal atmosphere, argon flow amount 100ml/min, and 5 ℃/min of temperature rise rate, 1800 ℃ of sintering temperatures are incubated 1 hour, and furnace cooling makes the high porous silicon carbide ceramic with high porosity of heat-shock resistance.
Claims (6)
1. the preparation method of a porous silicon carbide ceramics with high thermal shock resistance; It is characterized in that the silicon-resin core shell structure precursor powder that mixes prepared with existing bag is a raw material; And in above-mentioned raw materials, add aluminum oxide, silicon-dioxide and yttrium oxide as additive; After powder mixing, pressure forming, charing processing and four step process of sintering; Obtain porous silicon carbide ceramics with high thermal shock resistance, wherein, the quality of precursor powder, aluminum oxide, silicon-dioxide, yttrium oxide is 100 than scope: (0.5～10): (0.1～5): (0.1～5).
2. the preparation method of porous silicon carbide ceramics with high thermal shock resistance according to claim 1 is characterized in that the powder blending means is manual or mechanical stirring, ball milling or rocks and make it even.
3. the preparation method of porous silicon carbide ceramics with high thermal shock resistance according to claim 1 is characterized in that the powder mixing time is 5 minutes～24 hours.
4. the preparation method of porous silicon carbide ceramics with high thermal shock resistance according to claim 1; It is characterized in that the pressure molding condition is following: mixed powder is 50～140 ℃ through the green compact mold temperature of pressure forming; Compacting pressure is 0.5～50MPa, and soaking time is 20～120min.
5. the preparation method of porous silicon carbide ceramics with high thermal shock resistance according to claim 1, it is characterized in that the charing treatment process condition is following: carbonization temperature is 600～1000 ℃, temperature rise rate is 0.3～3 ℃/min; Argon flow amount is 5～200ml/min, and soaking time is 1～4h.
6. the preparation method of porous silicon carbide ceramics with high thermal shock resistance according to claim 1; It is characterized in that sintering carries out air pressure in argon gas atmosphere or vacuum: 0～20MPa, temperature rise rate: 1-20 ℃/min; Sintering temperature: 1200～1800 ℃, soaking time: 1～4 hour.
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| CN102303978A (en) * | 2011-06-03 | 2012-01-04 | 清华大学 | Method for preparing porous silicon carbide ceramic with high strength |
| CN102500748B (en) * | 2011-10-25 | 2013-10-23 | 中南大学 | Method for preparing aluminum silicon carbide composite material |
| CN104058782B (en) * | 2014-07-18 | 2015-10-14 | 厦门大学 | The preparation method of the mesoporous pottery of a kind of silicon carbide |
| CN110330343B (en) * | 2019-07-12 | 2021-07-27 | 清华大学 | Method for preparing nanocrystalline silicon carbide ceramic by utilizing core-shell structure nanoparticles |
| CN110526713B (en) * | 2019-08-27 | 2022-03-11 | 广东工业大学 | Porous silicon carbide ceramic and preparation method and application thereof |
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Non-Patent Citations (2)
| Title |
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| Limin Shi et al..Fabrication of high purity porous SiC ceramics using coat mix process.《Materials Science and Engineering A》.2007,第460-461卷第645-647页. * |
| 王艳香等.不同烧结助剂对网眼碳化硅多孔陶瓷性能的影响.《硅酸盐学报》.2008,第36卷(第S1期),第108-112页. * |
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