CN107337453A - A kind of method that combination gas-solid reaction method prepares recrystallized silicon carbide porous ceramics - Google Patents
A kind of method that combination gas-solid reaction method prepares recrystallized silicon carbide porous ceramics Download PDFInfo
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- CN107337453A CN107337453A CN201710471111.4A CN201710471111A CN107337453A CN 107337453 A CN107337453 A CN 107337453A CN 201710471111 A CN201710471111 A CN 201710471111A CN 107337453 A CN107337453 A CN 107337453A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 63
- 238000000034 method Methods 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 46
- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 26
- 239000007787 solid Substances 0.000 title claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 238000001953 recrystallisation Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 11
- 238000010792 warming Methods 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 230000006698 induction Effects 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims abstract description 6
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 5
- 239000011812 mixed powder Substances 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000000748 compression moulding Methods 0.000 claims description 2
- 235000019580 granularity Nutrition 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- 239000000284 extract Substances 0.000 abstract 1
- 238000009702 powder compression Methods 0.000 abstract 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 229910021426 porous silicon Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000001133 acceleration Effects 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
- 239000012298 atmosphere Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 235000012041 food component Nutrition 0.000 description 1
- 239000005417 food ingredient Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000012535 impurity Substances 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
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 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
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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Abstract
The invention discloses a kind of method that combination gas-solid reaction method prepares recrystallized silicon carbide porous ceramics, comprise the following steps：1) SiO powder is placed in crucible bottom, green compact will be formed according to mass percent after the mixed-powder compression molding of 70~95wt% carborundum and 5~30wt% nano carbon black, green compact are placed in the middle part of crucible, crucible is placed in multifunctional sintering furnace again, it is passed through argon gas, gas-solid reaction is carried out in 1650 DEG C~1800 DEG C insulations within 1~3 hour, obtains pre-sintered body；2) pre-sintered body is put into induction sintering furnace, porous SiC ceramics can be obtained in 1~3 hour by being warming up to 1900 DEG C~2100 DEG C recrystallization processing under an argon atmosphere.The carborundum porous ceramics that the present invention obtains can be widely applied to the fields such as Diesel exhaust particles extracts filter or catalyst carrier.
Description
Technical field
The present invention relates to a kind of method that combination gas-solid reaction method prepares recrystallized silicon carbide porous ceramics, suitable for various
Filter separator, catalyst carrier, sound-absorbing material and biomedical material etc..
Background technology
In recent years, diesel vehicle relies on is able to fast development in economy, dynamic property and greenhouse gas emission etc. advantage.
But the exhaust particulate thing exhaust emission of diesel vehicle has turned into restricts its bottleneck factor further developed.Particulate filter
(DPF) it is one of maximally effective post-processing technology generally acknowledged at present.DPF uses the exotic material of specific structure, in trapped exhaust gas
Particulate matter, and carry out filter regeneration in good time, it is granular material discharged so as to reduce.The material applied to DPF is mainly violet at present
Green stone and carborundum, compared with cordierite filtering material, SiC has more excellent heat-resisting, decay resistance and heat conductivility, machine
Tool intensity is also higher, can bear more severe regenerative environ-ment.
At present, the preparation method of recrystallized silicon carbide is mixed according to a certain percentage with the SiC particulate of thickness different-grain diameter,
Fine grained evaporates under high temperature, a kind of sintering method that cohesion occurs in coarse grained neck location and is sintered.Due to
There was only carborundum in raw material, without grain boundary impurities phase, therefore its bearing capacity is high, and thermal shock resistance is good, has excellent high temperature
Anti-oxidant and corrosion resistance；And do not shunk in sintering process, part complex-shaped, that precision is higher can be prepared.These
Advantage becomes a kind of important exhaust gas from diesel vehicle particle filtering material.Chinese patent 201220402621.9 is micro- with carborundum
Powder, rare-earth yttrium auxiliary agent are raw material, by slurrying, moulding by casting, recrystallized silicon carbide ceramic member are made at 2450 DEG C.It is Chinese special
For profit 201310466924.6 with carborundum powder, carbon dust and silica flour are raw material, obtain base substrate using die press technology for forming, are then placed in
Sintered in induction furnace, 2-5h is incubated at 1400-1700 DEG C, then be warming up to 2500 DEG C and carry out recrystallization and handle to obtain recrystallization carbon
SiClx product.In the above method, the silicon-carbide particle that is provided in raw material is micron-sized, and recrystallization sintering temperature is very high, need to be
More than 2200 DEG C, energy consumption is larger, and production cost is high, and equipment requirement is high.
Chinese patent 200610008498.1 gives a kind of method for preparing high-purity silicon carbide honeycomb ceramics body, this method
The SiC for being respectively adopted 23 μm and 30nm obtains green compact, 1800 as ceramic aggregate and sintering aid by extruding-out process
DEG C lower temperature under realize sintering.This method make use of nanometer silicon carbide surface energy larger and the less spy of diffusion coefficient
Point, hence it is evident that can reduce sintering temperature, while can acceleration of sintering neck area increase, and then obtain the porous silicon carbide of high intensity
Ceramics.But it is too high directly to prepare porous silicon carbide ceramic cost from Neon SiC powder；On the other hand, nanometer powder is difficult to
It is uniformly dispersed, is unfavorable for the uniformity and final performance of material structure.
The content of the invention
Present invention aim to address the problem of existing recrystallized silicon carbide sintering temperature is high, cost is high, it is contemplated that at present
Prepare in recrystallized silicon carbide process and be not directed to gas-solid reaction technique, there is provided one kind combines gas-solid reaction method and prepares weight
The method of crystalline silicon carbide porous ceramics.
To achieve the above objectives, the present invention, which adopts the following technical scheme that, is achieved：
A kind of method that combination gas-solid reaction method prepares recrystallized silicon carbide porous ceramics, comprises the steps：
1) according to mass percent by 70~95wt% carborundum and the mixed-powder mould of 5~30wt% nano carbon black
Green compact are formed after molded, SiO powder is placed in crucible bottom, green compact are placed in the middle part of crucible, then crucible are placed on multi-functional
In sintering furnace, argon gas is passed through, gas-solid reaction is carried out within 1~3 hour in 1650 DEG C~1800 DEG C insulations, obtains pre-sintered body, wherein
The mol ratio of SiO and nano carbon black is 1:1；
2) pre-sintered body is put into induction sintering furnace, be warming up under an argon atmosphere at 1900 DEG C~2100 DEG C recrystallizations
Reason obtains porous SiC ceramics in 1~3 hour.
Further improve of the invention is that in step 1), carborundum has two kinds of particle diameters, respectively 3.5 μm and 14 μm, adopts
With Monosized powder or two kinds of grain size distributions.
Further improve of the invention is that in step 1), the pressure of compression molding is 80~120MPa.
Further improve of the invention is that in step 1), argon atmospheric pressure is 2~3atm.
Further improve of the invention is that in step 2), argon atmospheric pressure is 0.5~1atm.
Of the invention further improve is, 1100 DEG C of heating is risen to from room temperature in step 1), in multifunctional sintering furnace
Speed is 500~700 DEG C/h, and the programming rate for being warming up to sintering temperature from 1100 DEG C is 200~300 DEG C/h.
Further improve of the invention is, in step 2), rises to the heating of sintering temperature in induction sintering furnace from room temperature
Speed is 2000~3000 DEG C/h.
The present invention has the advantage that：
The present invention can synthesize nano SiC using gas-solid reaction in micron SiC aggregate situ first, have higher vapor pressure
Nano SiC can promote recrystallize sintering process in evaporation-coacervation process, recrystallization temperature is greatly lowered, compared to
2200~2400 DEG C of tradition recrystallization sintering, the present invention can realize recrystallization sintering at 1900 DEG C, meanwhile, nano SiC can promote
The increase of sintered neck area between micron SiC particle, the intensity of material is increased substantially, it is thick using 14 μm of 64wt.%
Silicon-carbide particle and 16wt.% 3.5 μm of thick silicon-carbide particles carry out grading, 20wt.% nano carbon black are added, by 1700
DEG C gas-solid reaction and 2000 DEG C recrystallization sintering, the porous SiC porosity be 40%, intensity can reach 95.6MPa.The opposing party
The composition proportion such as face, content, carborundum particle diameter and grading by regulating and controlling nano carbon black, and briquetting pressure and sintering atmosphere pressure
The sintering process parameters such as power, it can obtain that there are the different porositys and the porous silicon carbide ceramic of mechanical property.Compared to tradition weight
Crystalline, porous silicon nitride ceramics, it is of the invention using cheap silicon monoxide powder, silicon carbide micro-powder, nano carbon black as primary raw material,
Cost can be significantly reduced, save the energy.
Brief description of the drawings
Fig. 1 is the SEM figures of sample after the recrystallization sintering of embodiment 8.
Fig. 2 is the XRD of sample after the recrystallization sintering of embodiment 6.
Fig. 3 is gas-solid reaction schematic diagram.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Carborundum porous ceramics of the present invention, embodiment composition is as shown in table 1, in the embodiment 1~12 shown in table 1,
Micrometer silicon carbide silicon serves as skeleton in base substrate, and as the coarse granule in recrystallization process, nano carbon black serves as the carbon of gas-solid reaction
Source, silicon monoxide serve as the silicon source of gas-solid reaction, and the nanometer silicon carbide synthesized by gas-solid reaction is used as in recrystallization process
Fine grained.
The raw material composition of 1. carborundum porous ceramics of the present invention of table
The sintering process parameter of 2. carborundum porous ceramics of the present invention of table
The embodiment of table 1 is the preparation method of carborundum porous ceramics, first by carborundum powder and nano carbon black as described in table 1 not
Weighed respectively with composition, be prepared into uniform mixed-powder by the use of absolute ethyl alcohol as solvent wet mixing, then rotate mixed-powder
Dry, place into 70 DEG C of baking oven and thoroughly dry, 200 mesh sieves are crossed after drying, pour into mortar plus a little mass fraction is 5%
PVA be ground, cross 80 mesh sieves be granulated, be put into the compressing green compact sample for obtaining embodiment 1~12 of metal die, be molded
Stress control is in 80~120MPa.SiO powder is placed in crucible bottom, green compact are placed in the middle part of crucible, then crucible is placed on more
In function sintering furnace, first rise to 1100 DEG C with 500~700 DEG C/h programming rate under an argon atmosphere, then with 200~300 DEG C/
H programming rate is warming up to 1650 DEG C~1800 DEG C insulations and carries out gas-solid reaction in 1~3 hour, obtains pre-sintered body；Then will be pre-
Sintered body is put into induction sintering furnace, under an argon atmosphere with 2000~3000 DEG C/h programming rate be warming up to 1900 DEG C~
2100 DEG C of recrystallization processing obtain sintered body in 1~3 hour.
The formulation of technique is in order at considered below：Raw material carborundum powder footpath uses a kind of granularity or two kinds of grain size distributions,
It can be filled in compared with small size particle in the space of greater particle size particle, obtain the sample of different green densities, and then realize gas
The regulation and control of porosity.The pressure of green compact shaping should be controlled in 80~120MPa, and in the case where food ingredient determines, body crack defects are excellent
Bad to be determined by precast body briquetting pressure, it directly affects the intensity and density of green compact, and the quality of green compact performance decides burning
Gained end properties after knot.Gas-solid reaction technique be 1650 DEG C~1800 DEG C be incubated 1~3 hour, sintering temperature it is too high or
Soaking time is oversize all to cause the nanometer silicon carbide particle diameter of generation excessive, do not have the effect for reducing recrystallization temperature.Tie again
Brilliant technique needs the matched well of temperature and time, and the time is short when temperature is high, time length when temperature is low.
The carborundum porous ceramics obtained by the above method, with the bending strength of three-point bending method measure at room temperature；Use Ah
Base Mead drainage determines open pore rate；Microscopic structure is observed on sample section with SEM；Use X-ray diffraction
Instrument analyzes the thing phase composition of sintered body.The results of property of these porositys and bending strength is as shown in table 2.
The performance of the carborundum porous ceramics sintered body of the present invention of table 2.
As can be seen from Table 2 embodiment 7 using 80wt% carborundum powder (80wt%14 μm of+20wt%3.5 μm of SiC) and
20wt% nano carbon black is as raw material, briquetting pressure 120MPa, by 1700 DEG C of insulation 2h gas-solid reactions, then at 2000 DEG C
Lower insulation 1.5h carries out recrystallization processing, and the porosity~40.4% of gained porous SiC ceramics material, intensity is up to 95.6MPa.
From accompanying drawing 1 as can be seen that forming well-developed sintering neck between micrometer silicon carbide silicon grain, combine discrete micron particles
Form porous ceramics.
The XRD for the porous SiC ceramics material that Fig. 2 is obtained by embodiment 8.As illustrated, recrystallized by high temperature, institute
That obtain is mutually single 6H-SiC.
Claims (7)
1. a kind of method that combination gas-solid reaction method prepares recrystallized silicon carbide porous ceramics, it is characterised in that including following steps
Suddenly：
1) mixed-powder of 70~95wt% carborundum and 5~30wt% nano carbon black is molded into according to mass percent
Green compact are formed after type, SiO powder is placed in crucible bottom, green compact are placed in the middle part of crucible, then crucible is placed on multi-functional sintering
In stove, be passed through argon gas, 1650 DEG C~1800 DEG C insulation 1~3 hour carry out gas-solid reaction, obtain pre-sintered body, wherein SiO and
The mol ratio of nano carbon black is 1:1；
2) pre-sintered body is put into induction sintering furnace, is warming up to 1900 DEG C~2100 DEG C recrystallization processing 1 under an argon atmosphere
Obtain porous SiC ceramics within~3 hours.
2. the method that a kind of combination gas-solid reaction method according to claim 1 prepares recrystallized silicon carbide porous ceramics, its
It is characterised by, in step 1), carborundum there are two kinds of particle diameters, respectively 3.5 μm and 14 μm, using Monosized powder or two kinds of granularities
Grading.
3. the method that a kind of combination gas-solid reaction method according to claim 1 prepares recrystallized silicon carbide porous ceramics, its
It is characterised by, in step 1), the pressure of compression molding is 80~120MPa.
4. the method that a kind of combination gas-solid reaction method according to claim 1 prepares recrystallized silicon carbide porous ceramics, its
It is characterised by, in step 1), argon atmospheric pressure is 2~3atm.
5. the method that a kind of combination gas-solid reaction method according to claim 1 prepares recrystallized silicon carbide porous ceramics, its
It is characterised by, in step 2), argon atmospheric pressure is 0.5~1atm.
6. the method that a kind of combination gas-solid reaction method according to claim 1 prepares recrystallized silicon carbide porous ceramics, its
It is characterised by, in step 1), it is 500~700 DEG C/h to rise to 1100 DEG C of programming rate from room temperature in multifunctional sintering furnace, from
1100 DEG C of programming rates for being warming up to sintering temperature are 200~300 DEG C/h.
7. the method that a kind of combination gas-solid reaction method according to claim 1 prepares recrystallized silicon carbide porous ceramics, its
It is characterised by, in step 2), it is 2000~3000 DEG C/h to rise to the programming rate of sintering temperature from room temperature in induction sintering furnace.
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