CN101747075B - Porous conductive MAX phase ceramics and preparation method and use thereof - Google Patents
Porous conductive MAX phase ceramics and preparation method and use thereof Download PDFInfo
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- CN101747075B CN101747075B CN2008102295134A CN200810229513A CN101747075B CN 101747075 B CN101747075 B CN 101747075B CN 2008102295134 A CN2008102295134 A CN 2008102295134A CN 200810229513 A CN200810229513 A CN 200810229513A CN 101747075 B CN101747075 B CN 101747075B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 37
- 238000001272 pressureless sintering Methods 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000005056 compaction Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000012071 phase Substances 0.000 abstract description 29
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 4
- 239000012876 carrier material Substances 0.000 abstract description 3
- 229910009818 Ti3AlC2 Inorganic materials 0.000 abstract 1
- 229910009817 Ti3SiC2 Inorganic materials 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 26
- 239000000758 substrate Substances 0.000 description 8
- 239000002184 metal Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 238000001238 wet grinding Methods 0.000 description 6
- 239000000969 carrier Substances 0.000 description 5
- 239000011888 foil Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- HEHRHMRHPUNLIR-UHFFFAOYSA-N aluminum;hydroxy-[hydroxy(oxo)silyl]oxy-oxosilane;lithium Chemical compound [Li].[Al].O[Si](=O)O[Si](O)=O.O[Si](=O)O[Si](O)=O HEHRHMRHPUNLIR-UHFFFAOYSA-N 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 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
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052670 petalite Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Abstract
The invention relates to a porous conductive ceramics, in particular to a porous conductive MAX phase (Ti3SiC2, Ti3AlC2 or Ti2AlC) ceramics with a through hole structure, and a preparation method and a use thereof. The porosity of the porous ceramics is adjustable within the range of 20-65%, the ceramics comprises a through hole structure, and the openporosity is more than 85%. The preparation method comprises the steps of taking MAX phase ceramic powder as a raw material, molding, carrying out pressureless sintering in an atmosphere furnace, keeping the sintering temperature at 1200-1400 DEG C, and leading the sintering time to be 0.5-3 hours. The MAX phase conductive ceramics with the through hole structure prepared by the pressureless sintering method can be used as a catalyst carrier material for automobile exhaust purification. The invention can solve the problems of liquid phase, a large number of closed pores in the generated hole and the like during the sintering process by optimizing the molding pressure, the sintering temperature and the time precise control of the porosity.
Description
Technical field
The present invention relates to the porous, electrically conductive pottery, be specially a kind of porous conductive MAX phase (Ti with through hole structure
3SiC
2, Ti
3AlC
2Or Ti
2AlC) pottery.
Background technology
Nowadays, automobile quantity increases sharply, and causes the emission of automobile wastes amount to grow with each passing day.Carbon monoxide in the tail gas (CO), hydrocarbon (C
xH
y), oxynitrides (NO
x), material such as sulfur dioxide, solid particle and aldehydes has the taste of intense stimulus property or carcinogenesis arranged, and become the important source of atmospheric pollution.
Be to reduce the pollution of tail gas, mainly adopt the outer measures of machine such as emission controls by improving combustion measure such as exhaust gas recirculation, late ignition time and efficient catalytic technology.The efficient catalytic technology is with CO, C before tail gas is discharged cylinder entering atmosphere
xH
y, NO
xBe converted into CO
2, H
2O, N
2The three-way catalytic converter that is adopted is made up of shell, carrier and catalyst three parts.Wherein carrier is a part and parcel, and two kinds of ceramic monolith and metallic carriers are arranged.At present, what use in a large number is cellular monoblock type ceramic monolith, and its material is cordierite, mullite, α-Al
2O
3, traditional ceramics such as zirconia, aluminium titanates, titanium dioxide, mullite, petalite, spodumene, alumino-silicate and magnesium silicate.Except widely used ceramic monolith, progress into people's the visual field by the metal foil carriers of stainless steel or alloy material making.Compare with ceramic monolith, conductive metal foil can electrical heating, can reduce the cold-starting automobile time, discharge of harmful gases amount when significantly having reduced startup.Although the metal foil carriers function admirable, complex forming technology, especially carrier and catalyst activity layer tack are poor.
At present, the subject matter that the catalyst carrier of using faces is: the non-conductive or poorly conductive of traditional ceramics carrier, be difficult for electrical heating, and thermal shock resistance is bad; The metal foil carriers good conductivity can electrical heating, but big with catalyst activity layer difference of thermal expansion coefficients, active layer peels off from carrier easily.
The MAX phase ceramics is (like Ti
3SiC
2, Ti
3AlC
2, Ti
2AlC) contain covalent bond and metallic bond, the advantage of integrated pottery and metal is like thermal shock resistance and the good electrical conductivity and the workability ability of high mechanical strength, excellence.These performances have overcome the deficiency of traditional ceramics carrier and metal foil carriers just simultaneously, make the MAX phase ceramics (like Ti
3SiC
2, Ti
3AlC
2, Ti
2AlC) be with a wide range of applications as catalyst carrier material.But it is up to the present, very limited to the research report of porous MAX phase ceramics both at home and abroad.The method of existing preparation porous MAX phase ceramics adopts approach (document 1, S.A.Firstov, the E.P.Pechkovsky.Powder Metall.Met.Ceram.42:424 (2003) of reaction-sintered; Document 2, Z.M.Sun, A.Murugaiah, T.Zhen, A.G.Zhou, M.W Barsoum.Acta Mater., 53:4359 (2005)).Because in the process of sintering, have liquid phase to generate, there is a large amount of closed pores in the hole of generation,, will reduces the catalyst activity layer and on the carrier hole wall, effectively utilize area if as catalyst carrier material.For the porous MAX phase ceramics that obtains to have the through hole structure (like Ti
3SiC
2, Ti
3AlC
2, Ti
2AlC), it is necessary avoiding in sintering process, occurring liquid phase.
Summary of the invention
The object of the present invention is to provide a kind of preparation to have the porous conductive MAX phase (Ti of through hole structure
3SiC
2, Ti
3AlC
2, Ti
2AlC) pottery and preparation method thereof, and its purposes is proposed, liquid phase appears in solution in sintering process, and there are a large amount of problems such as closed pore in the hole of generation.
Technical scheme of the present invention is:
A kind of porous conductive MAX phase ceramics has the through hole structure through the pressureless sintering porous conductive MAX phase ceramics, and the porosity is between 20-65%, and apparent porosity is at 85%-100%.
The preparation method of said porous conductive MAX phase ceramics is a raw material with MAX phase ceramics powder, after the moulding, in atmosphere furnace, do not have (the being normal pressure) sintering of pressure and obtains porous ceramics, and heating rate 5-20 ℃/min, sintering temperature 1200-1400 ℃, sintering time 0.5-3 hour.Thereby, prepare porous conductive MAX phase ceramics with through hole structure through pressureless sintering.
Said MAX phase ceramics is Ti
3SiC
2, Ti
3AlC
2Or Ti
2AlC.
Said cold moudling or the cold isostatic compaction of being shaped to.Wherein, cold moudling is at 20-60MPa pressure, 5-20 minute compacted under; Cold isostatic compaction is at 50-200MPa pressure, 5-20 minute compacted under.
Said pressureless sintering is carried out in argon gas or vacuum atmosphere.
The purposes of said porous conductive MAX phase ceramics, the MAX conductive ceramic phase with through hole structure for preparing through pressureless sintering method can be used as the catalyst carrier for purifying automobile exhaust material.
Advantage of the present invention is:
1, the inventive method can prepare porous MAX conductive ceramic phase.
2, the hole of the porous MAX phase ceramics of the present invention's preparation has the pore structure of perforation, and the perforate porosity is more than 85%.
3, the porous MAX phase ceramics of the present invention's preparation can accurately be controlled porosity through optimizing briquetting pressure, sintering temperature and sintering time, and porosity is adjustable between 20-65%.
Description of drawings
Fig. 1 .Ti
3SiC
2Photo behind 1200 ℃ of sintering.
Fig. 2 .Ti
3SiC
2Photo behind 1300 ℃ of sintering.
The specific embodiment
Through embodiment the present invention is detailed below.
Embodiment 1.
Ti
3SiC
2The moulding in 5 minutes of under 25MPa pressure, colding pressing is then dried in powder (granularity 2-5 micron) wet-milling 2 hours in the planetary ball mill jar in room temperature.Base substrate after the cold moudling was put into the atmosphere furnace sintering 2 hours.Atmosphere is argon gas, 10 ℃/min of heating rate, 1200 ℃ of sintering temperatures.Thereby, the MAX phase ceramics of acquisition porous, electrically conductive, porosity 54% behind the sintering, the perforate porosity 98%.Behind the sintering, porous ceramics has kept the profile of base substrate preferably, and is as shown in Figure 1.
Embodiment 2.
Ti
3AlC
2Isostatic cool pressing moulding in 20 minutes under 200MPa pressure is then dried in powder (granularity 2-5 micron) wet-milling 10 hours in the planetary ball mill jar in room temperature.Base substrate behind the cold isostatic compaction was put into the atmosphere furnace sintering 0.5 hour.Atmosphere is argon gas, 10 ℃/min of heating rate, 1400 ℃ of sintering temperatures.Thereby, the MAX phase ceramics of acquisition porous, electrically conductive, porosity 20% behind the sintering, the perforate porosity 85%.
Embodiment 3.
Ti
2The moulding in 10 minutes of under 20MPa pressure, colding pressing is then dried in AlC powder (granularity 2-5 micron) wet-milling 5 hours in the planetary ball mill jar in room temperature.Base substrate after the cold moudling was put into the atmosphere furnace sintering 0.5 hour.Atmosphere is that (vacuum is 10 to vacuum
-2Pa), 5 ℃/min of heating rate, 1200 ℃ of sintering temperatures.Thereby, the MAX phase ceramics of acquisition porous, electrically conductive, porosity 60% behind the sintering, the perforate porosity 98%.
Embodiment 4.
Ti
3SiC
2The moulding in 20 minutes of under 25MPa pressure, colding pressing is then dried in powder (granularity 2-5 micron) wet-milling 2 hours in the planetary ball mill jar in room temperature.Base substrate after the cold moudling was put into the atmosphere furnace sintering 2 hours.Atmosphere is argon gas, 10 ℃/min of heating rate, 1300 ℃ of sintering temperatures.Thereby, the MAX phase ceramics of acquisition porous, electrically conductive, porosity 46% behind the sintering, the perforate porosity 95%.Behind the sintering, porous ceramics has kept the profile of base substrate well, and is as shown in Figure 2.
Embodiment 5.
Ti
3AlC
2The moulding in 15 minutes of under 40MPa pressure, colding pressing is then dried in powder (granularity 2-5 micron) wet-milling 1 hour in the planetary ball mill jar in room temperature.Base substrate after the cold moudling was put into the atmosphere furnace sintering 3 hours.Atmosphere is argon gas, 15 ℃/min of heating rate, 1350 ℃ of sintering temperatures.Thereby, the MAX phase ceramics of acquisition porous, electrically conductive, porosity 36% behind the sintering, the perforate porosity 92%.
Embodiment 6.
Ti
2The moulding in 5 minutes of under 30MPa pressure, colding pressing is then dried in AlC powder (granularity 2-5 micron) wet-milling 5 hours in the planetary ball mill jar in room temperature.Base substrate after the cold moudling was put into the atmosphere furnace sintering 1 hour.Atmosphere is argon gas, 20 ℃/min of heating rate, 1300 ℃ of sintering temperatures.Thereby, the MAX phase ceramics of acquisition porous, electrically conductive, porosity 45% behind the sintering, the perforate porosity 95%.
Embodiment result shows that the present invention can accurately control porosity through optimizing briquetting pressure, sintering temperature and time, and the MAX conductive ceramic phase with through hole structure for preparing through pressureless sintering method can be used as the catalyst carrier for purifying automobile exhaust material.
Claims (2)
1. porous conductive MAX phase ceramics, it is characterized in that: have the through hole structure through the pressureless sintering porous conductive MAX phase ceramics, the porosity is between 20-65%, and apparent porosity is at 85%-100%;
Said MAX phase ceramics is Ti
3SiC
2, Ti
3AlC
2Or Ti
2AlC;
With MAX phase ceramics powder is raw material, and after the moulding, pressureless sintering obtains porous ceramics in atmosphere furnace, heating rate 5-20 ℃/min, and sintering temperature 1200-1400 ℃, sintering time 0.5-3 hour; Thereby, prepare porous conductive MAX phase ceramics with through hole structure through pressureless sintering;
Said cold moudling or the cold isostatic compaction of being shaped to;
Cold moudling is at 20-60MPa pressure, 5-20 minute compacted under; Cold isostatic compaction is at 50-200MPa pressure, 5-20 minute compacted under;
Said pressureless sintering is carried out in argon gas or vacuum atmosphere.
2. according to the purposes of the described porous conductive MAX phase ceramics of claim 1, it is characterized in that: the MAX conductive ceramic phase with through hole structure through the pressureless sintering method preparation can be used as the catalyst carrier for purifying automobile exhaust material.
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CN101747075B true CN101747075B (en) | 2012-05-23 |
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EP0659480A1 (en) * | 1993-12-27 | 1995-06-28 | SUT-SYSTEM- UND UMWELTTECHNIK GmbH | Metallic carrier with sintered cellular structure |
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