CN101805201A - Preparation method of porous silicon carbide ceramics with high thermal shock resistance - Google Patents
Preparation method of porous silicon carbide ceramics with high thermal shock resistance Download PDFInfo
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- CN101805201A CN101805201A CN 201010152549 CN201010152549A CN101805201A CN 101805201 A CN101805201 A CN 101805201A CN 201010152549 CN201010152549 CN 201010152549 CN 201010152549 A CN201010152549 A CN 201010152549A CN 101805201 A CN101805201 A CN 101805201A
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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 height, 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 arranged, cold working such as cutting, boring easily, have micropore (the skeleton volume accounts for 30%) in, the skeleton big with the contact area of liquid.
Porous silicon carbide ceramic will obtain application more and more widely in some harsh fields (as strong corrosive media, high temperature, high radiation property etc.).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 high temperature gas cooled reactor in nuclear energy field especially Tsing-Hua University's independent research, can filter the high temperature helium that contains graphite granule in the radioactive liquid waste that produces in the high temperature gas cooled reactor fuel element preparation process and the high temperature gas cooled reactor etc. as strainer.Porous silicon carbide ceramic can have the premium properties of porous ceramics 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.As 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 have a kind ofly been used Al under 1400~1550 ℃
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 porous ceramics, but can reduce its open-cell porosity, and the porous ceramics 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 overmolding, 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 are as additive, wherein, the precursor powder, aluminum oxide, silicon-dioxide, the quality of yttrium oxide is 100 than scope: (0.5~10): (0.1~5): (0.1~5), mix through powder, pressure forming, after four step process of charing processing and sintering, obtain porous silicon carbide ceramics with high thermal shock resistance, concrete processing step is as follows:
(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 as follows: 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 standby 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 to form when high temperature has promoted sintering reaction to carry out, reduced sintering temperature (1200~1800 ℃), and after cooling, 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 is all kept 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 height, pore size be 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
The invention will be further described below in conjunction with embodiment:
Embodiment 1
The precursor powder and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 0.5: 0.1: 0.1, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 2: 0.3: 0.1, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 2: 0.3: 0.3, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 3: 1: 0.5, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 4: 2: 1, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 5: 3: 2, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 6: 4: 3, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 7: 4: 3, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 8: 4: 5, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 9: 4: 3, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 and aluminum oxide, silicon-dioxide, the yttrium oxide that bag are mixed silicon-resin core shell structure that technology makes mix, and the mixing quality ratio is 100: 10: 5: 5, and adopt ball mill that it was mixed 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 and handle under argon gas atmosphere, 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 a kind 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 a kind 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 a kind of porous silicon carbide ceramics with high thermal shock resistance according to claim 1, it is characterized in that the pressure molding condition is as follows: 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 a kind 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 as follows: 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 a kind 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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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN102500748A (en) * | 2011-10-25 | 2012-06-20 | 中南大学 | Method for preparing aluminum silicon carbide composite material |
CN104058782A (en) * | 2014-07-18 | 2014-09-24 | 厦门大学 | Method for preparing silicon carbide mesoporous ceramic |
CN110330343A (en) * | 2019-07-12 | 2019-10-15 | 清华大学 | A method of nanocrystalline silicon carbide ceramics is prepared using Core-shell Structure Nanoparticles |
CN110526713A (en) * | 2019-08-27 | 2019-12-03 | 广东工业大学 | A kind of porous silicon carbide ceramic and its preparation method and application |
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2010
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN102500748A (en) * | 2011-10-25 | 2012-06-20 | 中南大学 | Method for preparing aluminum silicon carbide composite material |
CN104058782A (en) * | 2014-07-18 | 2014-09-24 | 厦门大学 | Method for preparing silicon carbide mesoporous ceramic |
CN110330343A (en) * | 2019-07-12 | 2019-10-15 | 清华大学 | A method of nanocrystalline silicon carbide ceramics is prepared using Core-shell Structure Nanoparticles |
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 |
CN110526713A (en) * | 2019-08-27 | 2019-12-03 | 广东工业大学 | A kind of porous silicon carbide ceramic and its preparation method and application |
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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