CN1528704A - Iolite-base composite ceramic with oxygen-storage function and preparing method thereof - Google Patents
Iolite-base composite ceramic with oxygen-storage function and preparing method thereof Download PDFInfo
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Abstract
The invention discloses a new cordierite composite ceramic with oxygen-storage capability and preparing method, able to adopt powder sintering process and glass crystallization to prepare it, by critical control of sintering process, able to form rare-earth oxide, titanium oxide, ferric oxide, zirconium oxide, etc on the cordierite substrate, therefore it has oxygen-storage capability (OSC) essential for ternary catalysis and a certain auxiliary catalysis capability, and it can improve the catalytic conversion effect of harmful components such as CO, C-H and NxO. It is applied to prepare catalyst carrier in car tail-gas converter. Its porosity is 30-50%, its thermal expansion coefficient 1.5-3.5X10 to the power -6/deg.C, its bend strength 15-40MPa and its maximum oxygen storage capacity 0.06mmol/g.
Description
Technical field:
The present invention relates to a kind of iolite-base composite ceramics and preparation method thereof, belong to field of inorganic materials, be applicable to the catalytic carrier material of preparation automobile exhaust purifier with storage oxygen function (OSC).
Background technology:
Along with increasing sharply of automobile pollution, a large amount of obnoxious flavoures that motor vehicle emission goes out and can suck solid particulate and atmospheric environment and human health have been produced ill effect.Exhaust purifier is installed is considered to comparatively effective measures with the catalyzed conversion of realizing obnoxious flavour.Exhaust purifier is by honeycomb-like cordierite pottery (2MgO2Al
2O
35SiO
2) carrier and its go up the catalyst layer composition of coating.Because the range of temperature of tail gas is bigger, require carrier that the ability of certain intensity and higher opposing thermal shock is arranged.
In the three-way emission control of vehicle exhaust, the oxygen concn (air-fuel ratio is about 14.7) in the control tail gas is constant, is the key that realizes three-way emission control.CeO
2And sosoloid has unique storage oxygen function (OSC), but because the contained CeO of catalyst coatings
2Measure limitedly, when air-fuel ratio fluctuation was big, its effect became not obvious.Even so three-element catalytic is difficult to also guarantee that various compositions all have higher turnover ratio simultaneously.In addition, because residing Working environment is very abominable, cleaner is very strict to the requirement of cordierite carrier and its surface catalyst layer.Catalyst coat and cordierite carrier must be in conjunction with firm, and granules of catalyst is grown up, come off in can not be under arms and dissolves in carrier.Because the coating number of times is more, this is quite difficult on preparation technology.The coating quality of Catalytic Layer is to the exhaust fume catalytic changing effect and play decisive role work-ing life.Adopt trichroite-oxide compound composite ceramics carrier, can save the process of coating oxide compound, and these oxide compounds can not grow up owing to be subjected to the constraint of trichroite matrix on every side, thereby improve the bonding strength of catalyst life and coating and cordierite carrier.
In Chinese patent, relate to the also few of cordierite ceramic solid support material.CN 1210835, and CN 1033455 has only reported the preparation method of single-phase cordierite ceramic.About patent application: application number is 01145537.3, and publication number is CN1358689A, has related to a kind of performance with trichroite composite ceramics of storage oxygen function.
Summary of the invention:
The objective of the invention is to utilize the synthetic technology of oxide ceramics, prepare this iolite-base composite ceramics,, make oxide particle evenly separate out matrix in porous cordierite ceramic by choose reasonable raw material and optimal preparation technology with storage oxygen function.Utilize cordierite ceramic carrier and the higher characteristics of top coat mesoporosity rate, make oxide particle participate in the adjusting and the promoting catalysis of oxygen concn in the atmosphere, thereby improve the catalyticing purifying effect of objectionable constituent in the tail gas.
Purpose of the present invention is implemented by following technical scheme: the porosity of iolite-base composite ceramics is that 30-50%, thermal expansivity are 1.5-3.5 * 10
-6/ ℃, flexural strength is 15-40MPa, oxygen storage capacity is up to 0.06mmol/g.
Purpose of the present invention is implemented by following technical scheme: its preparation process comprises: the preparation of (1), non-crystalline state powder; (2), the preparation of crystalline, powder; (3), according to the specific non-crystalline state powder and the ratio of crystalline, powder, the ball mill ball milling of packing into; (4), add solid pore former particle according to different ratios again, ball milling under the nitrogen atmosphere protection is made the mixed powder raw material that sintered ceramic is used; (5), the mixed powder with preparation is shaped insulation at a certain temperature under certain pressure; Stove is chilled to room temperature, can prepare the trichroite-multivariant oxide composite ceramics that contains different porosities;
(1), the preparation of non-crystalline state powder: the composition that contains aluminium, magnesium, silicon, lanthanum, cerium, iron, zirconium, titanium in the raw material of this powder, atomic ratio is an aluminium: magnesium: silicon=(3-5): (1-3): (4-6), the atomic ratio of lanthanum, cerium, iron, zirconium, titanium is (0-7): (1-15): (0-7): (0-7): (0-7), optimum content is, (2-5): (4-12): (2-5): (2-5): (2-5).Above-mentioned metal adds with the form of oxide compound respectively, and the effect of iron, zirconium, titanium mainly is the sintering character of regulating pottery.Per-cent according to the total mass of the oxide compound total mass of the aluminium of aforementioned proportion, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound is 20-60: 40-80, the best is 30-50: 70-50, according to above-mentioned component batching, after the high temperature melting, the melt quenching chilling, obtain the non-crystalline state particle, put into the ball mill ball milling 3-12 hour, obtain the non-crystalline state powder;
(2), the preparation of crystalline, powder: with the inorganic salt such as oxide compound, oxyhydroxide, carbonate, nitrate and muriate of aluminium, magnesium, silicon, according to atomic ratio, aluminium: magnesium: silicon=(3-5): (1-3): proportion ingredient (4-6); Put into the ball mill ball milling 3-12 hour, and obtained crystalline, powder;
(3), the mass percent ratio according to described non-crystalline state powder and described crystalline, powder is (10-60): (40-90) batching, optimum content is (20-50): (50-80).Pack into ball mill ball milling 3-12 hour;
(4), solid pore former particle is joined in the above-mentioned powder, the volume percent of the add-on of solid pore former and crystalline, powder, the total add-on of non-crystalline state powder is (10-50): (50-90); Optimum value is (20-40): (80-60).The solid pore former can be class low ignition point materials such as carbon, polystyrene, polyvinyl chloride and hard PVC, and granularity requirements is the 50-700 micron; Granularity the best is the 150-500 micron.Under the nitrogen atmosphere protection, continued ball milling 2-8 hour, make the mixed powder raw material that sintered ceramic is used; (5) mixed powder with preparation is shaped under the certain pressure of 20-60PMa, the best 30-50PMa of its pressure, and sintering temperature is 900-1400 ℃, the best is 950-1350 ℃.Be incubated 2-8 hour, stove is chilled to room temperature, can prepare the trichroite-multivariant oxide composite ceramics that contains different porosities.
Advantage of the present invention is: prepared iolite-base composite ceramics carrier material has storage oxygen function and helps catalysis.By choose reasonable raw material type and component and optimal preparation technology, make oxide particle evenly separate out matrix in porous cordierite ceramic, utilize cordierite ceramic carrier and the higher characteristics of top coat mesoporosity rate, make oxide particle participate in the adjusting and the promoting catalysis of oxygen concn in the atmosphere, thereby improve the catalyticing purifying effect of objectionable constituent in the vehicle exhaust.
Embodiment 1: amorphous powder is a feedstock production with aluminium, magnesium, silicon, lanthanum, cerium, iron, zirconium, titanyl compound, aluminium: magnesium: the Siliciumatom ratio is 3: 1: 6, the atomic ratio of lanthanum, cerium, iron, zirconium, titanium is 0: 5: 0: 1: 4, the per-cent of the total mass of the oxide compound total mass of aluminium, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound is 60: 40, after 1600 ℃ of fusings, the melt quenching chilling obtains the non-crystalline state particle, put into the ball mill ball milling 10 hours, and obtained the non-crystalline state powder.In the crystalline, powder, aluminium: magnesium: silicon adds with the form of oxide compound, and aluminium: magnesium: the Siliciumatom ratio is 4: 2: 5, puts into the ball mill ball milling 5 hours, obtains crystalline, powder.The mass percent of non-crystalline state powder and crystalline, powder is 10: 90 batchings.The volume ratio of the mixed powder of polystyrene and above-mentioned non-crystalline state powder and crystalline, powder is 10: 90.The granularity of polystyrene is 50 microns; Will be under the nitrogen atmosphere protection by polystyrene, non-crystalline state powder and the crystalline, powder of said ratio, ball milling was shaped under the pressure of 20MPa after 2 hours, 950 ℃ of sintering 8 hours.
Embodiment 2: amorphous powder is a feedstock production with aluminium, magnesium, silicon, lanthanum, cerium, iron, zirconium, titanyl compound, aluminium: magnesium: the Siliciumatom ratio is 4: 2: 4, the atomic ratio of lanthanum, cerium, iron, zirconium, titanium is 1: 10: 7: 0: 1, the per-cent of the total mass of the oxide compound total mass of aluminium, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound is 50: 50, after 1600 ℃ of fusings, the melt quenching chilling obtains the non-crystalline state particle, put into the ball mill ball milling 5 hours, and obtained the non-crystalline state powder.In the crystalline, powder, aluminium: magnesium adds with muriatic form: silicon adds with the form of silicon oxide, and aluminium: magnesium: the Siliciumatom ratio is 3: 3: 6, puts into the ball mill ball milling 8 hours, obtains crystalline, powder.The mass percent of non-crystalline state powder and crystalline, powder is 20: 80 batchings.The volume ratio of the mixed powder of polyvinyl chloride and above-mentioned non-crystalline state powder and crystalline, powder is 20: 80.The granularity of polyvinyl chloride is 100 microns; Will be under the nitrogen atmosphere protection by polyvinyl chloride, non-crystalline state powder and the crystalline, powder of said ratio; behind the ball milling 10 hours, under the pressure of 40MPa, be shaped 1150 ℃ of sintering 6 hours; obtain porosity after stove is cold and be 15% composite ceramic body, thermal expansivity is 1.9 * 10
-6/ ℃, flexural strength is 24MPa, the oxygen storage capacity of its powder is 0.015mmol/g.
Embodiment 3: amorphous powder is a feedstock production with aluminium, magnesium, silicon, lanthanum, cerium, iron, zirconium, titanyl compound, aluminium: magnesium: the Siliciumatom ratio is 5: 3: 2, the atomic ratio of lanthanum, cerium, iron, zirconium, titanium is 5: 12: 1: 7: 0, the per-cent of the total mass of the oxide compound total mass of aluminium, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound is 40: 60, after 1600 ℃ of fusings, the melt quenching chilling obtains the non-crystalline state particle, put into the ball mill ball milling 6 hours, and obtained the non-crystalline state powder.In the crystalline, powder, aluminium: magnesium adds with the form of nitrate: silicon adds with the form of silicon oxide, and aluminium: magnesium: the Siliciumatom ratio is 3: 3: 6, puts into the ball mill ball milling 8 hours, obtains crystalline, powder.The mass percent of non-crystalline state powder and crystalline, powder is 30: 70 batchings.The volume ratio of the mixed powder of polystyrene and above-mentioned non-crystalline state powder and crystalline, powder is 25: 75.The granularity of polystyrene is 450 microns; Will be under the nitrogen atmosphere protection by polystyrene, non-crystalline state powder and the crystalline, powder of said ratio; behind the ball milling 12 hours, under the pressure of 50MPa, be shaped 1250 ℃ of sintering 5 hours; obtain porosity after stove is cold and be 20% composite ceramic body, thermal expansivity is 2.5 * 10
-6/ ℃, flexural strength is 20MPa, the oxygen storage capacity of its powder is 0.020mmol/g.
Embodiment 4: amorphous powder is a feedstock production with aluminium, magnesium, silicon, lanthanum, cerium, iron, zirconium, titanyl compound, aluminium: magnesium: the Siliciumatom ratio is 4: 3: 4, the atomic ratio of lanthanum, cerium, iron, zirconium, titanium is 7: 14: 0: 0: 7, the per-cent of the total mass of the oxide compound total mass of aluminium, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound is 30: 70, after 1600 ℃ of fusings, the melt quenching chilling obtains the non-crystalline state particle, put into the ball mill ball milling 4 hours, and obtained the non-crystalline state powder.In the crystalline, powder, aluminium: magnesium adds with the form of oxyhydroxide: silicon adds with the form of silicon oxide, and aluminium: magnesium: the Siliciumatom ratio is 3: 3: 6, puts into the ball mill ball milling 8 hours, obtains crystalline, powder.The mass percent of non-crystalline state powder and crystalline, powder is 35: 65 batchings.The volume ratio of the mixed powder of PVC powder and above-mentioned non-crystalline state powder and crystalline, powder is 30: 70.The granularity of PVC is 200 microns; Will be under the nitrogen atmosphere protection by PVC powder, non-crystalline state powder and the crystalline, powder of said ratio; behind the ball milling 12 hours, under the pressure of 40MPa, be shaped 1350 ℃ of sintering 4 hours; obtain porosity after stove is cold and be 16% composite ceramic body, thermal expansivity is 2.1 * 10
-6/ ℃, flexural strength is 23MPa, the oxygen storage capacity of its powder is 0.031mmol/g.
Embodiment 5: amorphous powder is a feedstock production with aluminium, magnesium, silicon, lanthanum, cerium, iron, zirconium, titanyl compound, aluminium: magnesium: the Siliciumatom ratio is 5: 2: 5, the atomic ratio of lanthanum, cerium, iron, zirconium, titanium is 3: 15: 0: 1: 1, the per-cent of the total mass of the oxide compound total mass of aluminium, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound is 40: 60, after 1600 ℃ of fusings, the melt quenching chilling obtains the non-crystalline state particle, put into the ball mill ball milling 6 hours, and obtained the non-crystalline state powder.In the crystalline, powder, aluminium: magnesium, silicon add with the form of oxide compound: aluminium: magnesium: the Siliciumatom ratio is 3: 4: 4, puts into the ball mill ball milling 3 hours, obtains crystalline, powder.The mass percent of non-crystalline state powder and crystalline, powder is 40: 60 batchings.The volume ratio of the mixed powder of carbon dust and above-mentioned non-crystalline state powder and crystalline, powder is 35: 65.The granularity of carbon dust is 600 microns; Will be under the nitrogen atmosphere protection by carbon dust, non-crystalline state powder and the crystalline, powder of said ratio; behind the ball milling 10 hours, under the pressure of 55MPa, be shaped 1250 ℃ of sintering 6 hours; obtain porosity after stove is cold and be 29% composite ceramic body, thermal expansivity is 1.6 * 10
-6/ ℃, flexural strength is 21MPa, the oxygen storage capacity of its powder is 0.057mmol/g.
Embodiment 6: amorphous powder is a feedstock production with aluminium, magnesium, silicon, lanthanum, cerium, iron, zirconium, titanyl compound, aluminium: magnesium: the Siliciumatom ratio is 3: 2: 4, the atomic ratio of lanthanum, cerium, iron, zirconium, titanium is 5: 15: 1: 1: 1, the per-cent of the total mass of the oxide compound total mass of aluminium, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound is 40: 60, after 1600 ℃ of fusings, the melt quenching chilling obtains the non-crystalline state particle, put into the ball mill ball milling 6 hours, and obtained the non-crystalline state powder.In the crystalline, powder, aluminium: magnesium, silicon add with the form of oxide compound: aluminium: magnesium: the Siliciumatom ratio is 3: 4: 4, puts into the ball mill ball milling 3 hours, obtains crystalline, powder.The mass percent of non-crystalline state powder and crystalline, powder is 40: 60 batchings.The volume ratio of the mixed powder of polystyrene and above-mentioned non-crystalline state powder and crystalline, powder is 35: 65.The granularity of polystyrene is 350 microns; Will be under the nitrogen atmosphere protection by polyvinyl chloride, non-crystalline state powder and the crystalline, powder of said ratio; behind the ball milling 10 hours, under the pressure of 35MPa, be shaped 1400 ℃ of sintering 2 hours; obtain porosity after stove is cold and be 27% composite ceramic body, thermal expansivity is 1.6 * 10
-6/ ℃, flexural strength is 21MPa, the oxygen storage capacity of its powder is 0.047mmol/g.
Claims (9)
1, a kind of iolite-base composite ceramics with storage oxygen function is characterized in that the porosity of iolite-base composite ceramics is that 30-50%, thermal expansivity are 1.5-3.5 * 10
-6/ ℃, flexural strength is 15-40MPa, oxygen storage capacity is up to 0.06mmol/g.
2, a kind of preparation method with iolite-base composite ceramics of storage oxygen function according to claim 1 is characterized in that its preparation process comprises: the preparation of (1), non-crystalline state powder; (2), the preparation of crystalline, powder; (3), according to the specific non-crystalline state powder and the ratio of crystalline, powder, the ball mill ball milling of packing into; (4), add solid pore former particle according to different ratios again, ball milling under the nitrogen atmosphere protection is made the mixed powder raw material that sintered ceramic is used; (5), the mixed powder with preparation is shaped insulation at a certain temperature under certain pressure; Stove is chilled to room temperature, can prepare the trichroite-multivariant oxide composite ceramics that contains different porosities;
(1), the preparation of non-crystalline state powder: the composition that contains aluminium, magnesium, silicon, lanthanum, cerium, iron, zirconium, titanium in the raw material of this powder, according to atomic ratio, aluminium: magnesium: silicon=(3-5): (1-3): (4-6), the atomic ratio of lanthanum, cerium, iron, zirconium, titanium is (0-7): (1-15): (0-7): (0-7): (0-7), above-mentioned metal adds with the form of oxide compound respectively, and wherein the effect of iron, zirconium, titanium mainly is to regulate the sintering character of pottery and play the catalytic effect that helps.Per-cent according to the total mass of the oxide compound total mass of the aluminium of aforementioned proportion, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound is 20-60: 40-80, according to above-mentioned component batching, after the high temperature melting, the melt quenching chilling, obtain the non-crystalline state particle, put into the ball mill ball milling, obtain the non-crystalline state powder;
(2), the preparation of crystalline, powder: with the inorganic salt such as oxide compound, oxyhydroxide, carbonate, nitrate and muriate of aluminium, magnesium, silicon, according to atomic ratio, aluminium: magnesium: silicon=(3-5): (1-3): proportion ingredient (4-6); Put into the ball mill ball milling, obtain crystalline, powder;
(3), the mass percent ratio according to described non-crystalline state powder and described crystalline, powder is (10-60): (40-90) batching, the ball mill ball milling of packing into;
(4), the volume percent of the add-on of solid pore former and crystalline, powder, the total add-on of non-crystalline state powder is (10-50): (50-90); The solid pore former can be some low ignition point materials such as carbon, polystyrene, polyvinyl chloride, hard PVC powder.The solid organic matters granularity is the 50-800 micron; The best is the 100-600 micron.Under the nitrogen atmosphere protection, solid pore former, crystalline, powder and non-crystalline state powder are continued ball milling, make the mixed powder raw material that sintered ceramic is used.
(5) mixed powder with preparation is shaped under the certain pressure of 20-70PMa, and sintering temperature is 900 ℃-1400 ℃, is incubated 2-8 hour, and stove is chilled to room temperature, can prepare the trichroite-multivariant oxide composite ceramics that contains different porosities.
3, a kind of preparation method according to claim 2 with iolite-base composite ceramics of storage oxygen function, it is characterized in that atomic ratio the best of lanthanum, cerium, iron, zirconium, titanium is in the non-crystalline state powder: (2-5): (4-12): (2-5): (2-5): (2-5).
4, a kind of preparation method according to claim 2 with iolite-base composite ceramics of storage oxygen function, it is characterized in that the per-cent of the total mass of the oxide compound total mass of aluminium, magnesium, silicon and lanthanum, cerium, iron, zirconium, titanyl compound the best is 30-50: 70-50 in the non-crystalline state powder.
5, a kind of preparation method with iolite-base composite ceramics of storage oxygen function according to claim 2 is characterized in that the mass percent optimum content of crystalline, powder and non-crystalline state powder is (20-50) in the powder: (50-80).
6, a kind of preparation method according to claim 2 with iolite-base composite ceramics of storage oxygen function, it is characterized in that the add-on of described solid organic matters and crystalline, powder, the total volume percent the best of non-crystalline state powder are (20-40): (80-60).
7, according to claim 2 or 6 described a kind of preparation methods, it is characterized in that solid organic matters can be some low ignition point materials such as carbon, polystyrene, polyvinyl chloride, hard PVC powder with iolite-base composite ceramics of storage oxygen function.Solid organic matters granularity the best is the 100-600 micron.
8, a kind of preparation method with iolite-base composite ceramics of storage oxygen function according to claim 2 is characterized in that, the mixed powder for preparing is shaped under the pressure of best 30-60PMa.
9, a kind of preparation method with iolite-base composite ceramics of storage oxygen function according to claim 2 is characterized in that sintering temperature the best of pottery is 950 ℃-1350 ℃, and best soaking time is 3-7 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101161603B (en) * | 2006-10-12 | 2011-05-11 | 湖南省新化县鑫星电子陶瓷有限责任公司 | An iolite porcelain electronic flat-irons soles with low hot expansion factor |
| CN101687713B (en) * | 2007-06-28 | 2013-05-29 | 康宁股份有限公司 | High porosity ceramic honeycomb article containing rare earth oxide and method of manufacturing same |
| CN103755332A (en) * | 2013-12-30 | 2014-04-30 | 内蒙古工业大学 | Method for preparing cordierite ceramics from desert aeolian sand |
| CN115108815A (en) * | 2021-03-19 | 2022-09-27 | 比亚迪股份有限公司 | Microcrystalline porous ceramic matrix and preparation method thereof, electronic cigarette atomization core and electronic cigarette |
-
2003
- 2003-10-13 CN CN 200310100863 patent/CN1242954C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101161603B (en) * | 2006-10-12 | 2011-05-11 | 湖南省新化县鑫星电子陶瓷有限责任公司 | An iolite porcelain electronic flat-irons soles with low hot expansion factor |
| CN101687713B (en) * | 2007-06-28 | 2013-05-29 | 康宁股份有限公司 | High porosity ceramic honeycomb article containing rare earth oxide and method of manufacturing same |
| CN103755332A (en) * | 2013-12-30 | 2014-04-30 | 内蒙古工业大学 | Method for preparing cordierite ceramics from desert aeolian sand |
| CN103755332B (en) * | 2013-12-30 | 2016-02-03 | 内蒙古工业大学 | Desert wind sand is utilized to prepare the method for cordierite ceramic |
| CN115108815A (en) * | 2021-03-19 | 2022-09-27 | 比亚迪股份有限公司 | Microcrystalline porous ceramic matrix and preparation method thereof, electronic cigarette atomization core and electronic cigarette |
| CN115108815B (en) * | 2021-03-19 | 2023-11-14 | 比亚迪股份有限公司 | Microcrystalline porous ceramic matrix, preparation method thereof, electronic cigarette atomization core and electronic cigarette |
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Assignee: Baotou Beifang Railway Products Co., Ltd. Assignor: Nei Mongol Polytechnical Univ. Contract fulfillment period: 2007.8.15 to 2012.8.15 contract change Contract record no.: 2009150000011 Denomination of invention: Iolite-base composite ceramic with oxygen-storage function and preparing method thereof Granted publication date: 20060222 License type: Exclusive license Record date: 2009.6.22 |
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