CN104072111B - A kind of preparation method of cellular alumina pottery - Google Patents
A kind of preparation method of cellular alumina pottery Download PDFInfo
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- CN104072111B CN104072111B CN201410120658.6A CN201410120658A CN104072111B CN 104072111 B CN104072111 B CN 104072111B CN 201410120658 A CN201410120658 A CN 201410120658A CN 104072111 B CN104072111 B CN 104072111B
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Abstract
The invention discloses a kind of preparation method of cellular alumina pottery, comprise the cellular alumina base substrate that step 1) preparation has parallel channels; 2) binder removal of cellular alumina base substrate or degreasing; 3) Calcined polishing aluminum oxide honeycomb body, obtains the cellular alumina pottery with duct inner wall extend whisker structure.The obtained ceramic matrix partial particulate of the inventive method combines closely, and honeycomb hole inwall grows into whisker, and this ceramic honey comb has the premium propertiess such as high temperature resistant, resistance to chemical attack, is applicable to filtration and the purification of multiple fluid.Ceramic honey comb after using is easy to adopt multiple method to remove filtrate, reusable.Preparation method's technique of the present invention is simple, low for equipment requirements, convenient operation and control, and production efficiency is high, is applicable to large-scale industrial and produces.
Description
Technical field
The present invention relates to field of material technology, particularly, relate to one and have the preparation method of the cellular alumina pottery of " duct inner wall extend whisker " structure.
Background technology
Ceramic honey comb has parallel through pore texture, have that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, be conducive to counting of particle and discharge with gas and to reduce advantages such as filtering volume, have a wide range of applications in the purifying treatment etc. of the filtration, purification of industrial gaseous waste, motor-vehicle tail-gas and other life waste gas, the heat exchange of metallurgical industry and the filtration of molten metal, the toxic gas of mining industry and liquid.
What the technology of preparing of current ceramic honey comb was the most ripe is extrusion moulding, namely the first size according to required honeycomb hole and shape (trilateral, rhombus, rectangle, hexagon etc.) prepare mould, then prepare the ceramic honey comb of duct arrangement high-sequential by the extrusion of ceramic size.Corning company of the U.S. and Japanese NGK company have realized industrialization and have produced, and the ceramic honey comb of preparation is mainly used in vehicle exhaust and heat accumulation block materials.
To be material aperture limit by the preparation of mould for the greatest problem of the method, is difficult to prepare the cellular material of aperture in tens micron dimensions, thus limits the further performance of the performance such as honeycomb ceramic filter, heat accumulation.The up-to-date ceramic honey comb product of Corning company can prepare 1200 through holes at most on the cross section of 1 square inch, and be the limit that current known the method can prepare ceramic honey comb aperture, further reduced bore is very difficult.This is focus in the preparation research of ceramic honey comb and difficult point.
Namely the aperture of enable further reduction ceramic honey comb is reduced to micron dimension, its aperture reduce the increase suddenly that gas will be caused by resistance, thus reduce its working efficiency.That is, single honeycomb structure is relied on to be difficult to the small-bore required by the filtration of solution subparticle and to keep air-flow this contradiction unimpeded simultaneously.
Whisker is the single crystal of a kind of high strength beard shape synthesized under manual control condition, and its crystalline structure is more complete, and subsurface defect is few, and its strength and modulus is all close to ideal crystal.Therefore, whisker Chang Zuowei reinforcing component join metal matrix, ceramic base and polymer-based in the effect of its activeness and quietness.Modal whisker has Si
3n
4, SiC, Al
2o
3deng.But at present about the research of whisker mainly concentrate on whisker preparation and in matrix activeness and quietness effect, rarely have report about the research of whisker in other purposes.In the preparation research of whisker, report is had to point out to utilize hole can growth in situ whisker, as patent CN102251284A (a kind of method preparing beta-alumina whisker), and document (Ji Xiaoli, Xu Fei, power is national, Wan Weiwei, On In-situ Synthesis of Mullite Whisker strengthens foam silicon carbide ceramics, Chinese powder technology, 2011,17 (3): 33-36) and document (Lv Chenjing, Tian Xiushu, Han Yufang, fabricated in situ contains Al
2o
3whisker Al
2o
3the research of/Ti-Al matrix material mechanism), but former concerns is in the preparation of whisker, and rear both pay close attention to the reinforced effects of whisker to matrix or foam base plate.Meanwhile, the porous body prepared by above document and the hole in parts are closed pore, are difficult to use in filtration.
How overcoming legacy cellular pottery working efficiency to the dependence of aperture and unit surface hole count, and then increase the filtration of pottery to fine particle, and ensure the unimpeded of fluid, is that current honeycomb ceramic filter and field of purification are to the new demand of ceramic structure.
Summary of the invention
The invention provides a kind of preparation method of cellular alumina pottery, comprise the following steps:
1) preparation has the cellular alumina base substrate also drying of parallel channels;
2) organic eliminating is carried out to dried base substrate;
3) Calcined polishing aluminum oxide honeycomb body, obtains body portion particle and combines closely, and hole inner wall extend has the cellular alumina pottery of whisker.
Wherein, the cellular alumina base substrate in step 1) with parallel channels adopts extrusion moulding preparation.In the art, extruding forming method prepares the conventional method of ceramic honey comb, can directly prepare cellular alumina base substrate.
In the inventive method, in step 1), cellular alumina base substrate also can adopt dry pressing, gel casting forming method or direct coagulation casting method first to prepare biscuit, then adopts mechanical hole building method to obtain the cellular alumina base substrate with parallel channels.
In embodiments of the invention, be adopt Multi needle to become punch die, the obtained cellular alumina base substrate with parallel channels.
In the inventive method, be raw material with alumina powder jointed in step 1), and add sintering agent, shaping medium, dispersion agent mix, and prepares cellular alumina base substrate base substrate.
Described alumina powder jointed particle diameter 0.5 μm ~ 3 μm, accounts for total powder 65 ~ 75wt%.
Described sintering agent is kaolin, CaCO
3, BaCO
3, MgCO
3, talcum, rhombspar and/or wollastonite, wherein, kaolin content is 9 ~ 20%, CaCO of total powder quality
3content is 0 ~ 3%, BaCO of total powder quality
3content is 0 ~ 3%, MgCO of total powder quality
3content is 0 ~ 3% of total powder quality, and talc content is 0 ~ 2% of total powder quality, and rhombspar content is 0 ~ 9% of total powder quality, and wollastonite content is 0 ~ 2% of total powder quality.
Described total powder is the summation of aluminum oxide, sintering agent, shaping medium, dispersion agent powder.
Dispersion agent is mainly used in the colloidal formation such as gel injection molding and forming technology, direct coagulation casting technique, and the present invention does not also rely on specific dispersion agent, as long as dispersion agent can make ceramic powder suitably disperse in sauce.The example of some operable dispersion agents is ammonium polyacrylate, ammonium citrate, ammonium polymethacrylate etc.
According to different forming methods, select corresponding shaping medium.Extrusion moulding generally selects water, polyvinyl alcohol, poly-hydroxyl ethanol acid etc. as shaping medium.Gel casting forming selects water base acrylamide polymers to be shaping medium, and wherein monomer is acrylamide, and linking agent is N, N '-methylene-bisacrylamide, and initiator is 8% ammonium persulfate solution, and catalyzer is N,N,N′,N′ tetramethylethylene diamine.Direct coagulation casting selects urea and urease to be shaping medium.
Raw alumina powder involved in the present invention, sintering agent powder and the additive such as dispersion agent, shaping medium are common commercial powder, its purity is commercial level, but further according to adjusting the requirement of product purity, also can adopt the grade reagents such as analytical pure.
The powder granularity of raw alumina powder involved in the present invention, sintering agent powder and dispersion agent, shaping medium etc. is more little is more conducive to sintering, preferably less than 2.0 μm powders, but is not limited thereto scope.
According to different forming methods, additive such as dispersion agent, shaping reagent etc. can be different, and the solid load of base substrate also can be different.
In the inventive method, step 2) in the drying of cellular alumina base substrate be that room temperature is dried in the shade or 40 DEG C ~ 60 DEG C oven dry, the parallel construction in maintenance honeycomb duct.
According to different forming methods, its time of drying/temperature/humidity is different, to keep base substrate indeformable for standard.Because organic content in different forming method base substrate is different, so it is different to get rid of organic program.In extrusion moulding, dry-pressing formed prepared base substrate, organic content is higher, depending on base substrate size, need the 1 little independent degreasing process up to 1 day, and in gel casting forming and the base substrate prepared by direct coagulation casting, organic content is lower, is easy to binder removal in rapid heating condition before sintering.This process is familiar with by those skilled in the art.
Step 2) in organism eliminating is carried out to dried base substrate, temperature is at 500 DEG C ~ 800 DEG C, and the time is 0.5 ~ 3h.
In the inventive method, calcined by cellular alumina base substrate in step 3), calcining temperature is 1580 DEG C ~ 1600 DEG C, insulation 1h ~ 3h.
Preferably, calcined by cellular alumina base substrate in step 3), calcining temperature is 1600 DEG C, insulation 3h.
The present invention proposes on the framework of ceramic honey comb base substrate, hole is utilized to grow the principle of whisker, preparing hole wall is the filtration that the whisker stretched in this novel texture cellular alumina ceramic channel walls of cellular alumina pottery of " whisker intert parallel channels " novel texture of whisker effectively can carry out fine particle, and its original basic honeycomb parallel via holes structure in turn ensure that the smoothness of fluid.
The present invention is based on hole provides space can the principle of growth in situ whisker, selects Al
2o
3for raw material, by controlling sintering condition, prepare the novel oxidized aluminium ceramic honey comb of " duct inner wall extend whisker ".The present invention, according to the pattern feature of whisker, utilizes the whisker of duct inner wall extend to increase filtration to fine particle, utilizes parallel channels to ensure the unimpeded of fluid simultaneously, overcomes the dependence of legacy cellular pottery working efficiency to aperture and unit surface hole count.The present invention first at honeycomb structure situ synthesizing whisker, and develops whisker and is filtering and the new opplication of field of purification in conjunction with honeycomb structure.
Production technique of the present invention is simple, low for equipment requirements, convenient operation and control, and production efficiency is high, is applicable to large-scale industrial and produces.The ceramic honey comb prepared by method of the present invention is alumina material, there is the premium propertiess such as high temperature resistant, resistance to chemical attack, be applicable to filtration and the purification of multiple fluid, as the filtration, purification of fine particle in air, waste gas that various commercial run produces, its other life waste gas of motor-vehicle tail-gas, also can be used for the tabular adsorbent of analysis chromatographic column, to the filtration of the heat exchange of metallurgical industry and molten metal, to the toxic gas of mining industry and the purifying treatment etc. of liquid.Scanning electron microscope (SEM) shows ceramic honey comb body portion particle of the present invention and combines closely, and honeycomb hole inwall grows into whisker, forms parallel channels.This structure makes ceramic honey comb of the present invention can be kept the smoothness of fluid in use by straight channels, and the whisker of passing hole channel inner wall extend filters further, cleansing fluid.
Accompanying drawing explanation
Fig. 1 is the SEM photo of alumina-ceramic " duct inner wall extend whisker ".
Fig. 2 is the XRD figure spectrum of alumina-ceramic " duct inner wall extend whisker ".
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.Without departing from the spirit and substance of the case in the present invention, the amendment do the inventive method, step or condition or replacement, all belong to scope of the present invention.
If do not specialize, chemical feedstocks used in embodiment is conventional commercial raw material, the conventional means that technique means used in embodiment is well known to those skilled in the art.
Cellular alumina pottery and performance thereof are prepared in embodiment 1 extrusion moulding
Get the aluminum oxide powder that 216g particle diameter is 3 μm, 60g kaolin, 9gCaCO
3, 9gBaCO
3with 6g wollastonite, mix, obtain powdered mixture.The acid of water, polyvinyl alcohol and poly-hydroxyl ethanol is pressed the weight ratio mixing of 70:10:20, stir obtained homogeneous solution, solution is mixed with the weight ratio of above-mentioned powder mixture according to 100:70, fully mixing 0.75 hour of normal temperature in the mixing roll (BL-6175-B) at normal temperatures and pressures, under normal temperature and pressure old 3 hours, obtain pug.Pug is crossed 60 mesh sieves and carry out filtration, purification, honeycomb biscuit is extruded by honeycomb ceramic extruding machine (BL-6177), 40 DEG C of dryings 6 hours, after dry, sample is at 600 DEG C of binder removal organics removal 2h, then the honeycomb biscuit after binder removal is put into retort furnace (BTF-1700C), be warming up to 1580 DEG C of insulations 3 hours with 10 DEG C/min, be there is the cellular alumina pottery of " duct inner wall extend whisker " structure.Fig. 1 is shown in by its SEM photo, and XRD figure is shown in Fig. 2.SEM picture shows the obtained cellular alumina ceramic matrix partial particulate of the present embodiment and combines closely, and honeycomb hole inwall grows into whisker, forms parallel channels.
This ceramic honey comb aperture is 0.5mm, and void content is 68%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 9MPa, axial compression strength 21MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the cellular alumina that prepared by the present invention pottery has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, be conducive to counting of particle to discharge with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 2 gel casting forming prepares cellular alumina pottery and performance thereof
By monomeric acrylamide and linking agent N, N '-methylene-bisacrylamide water-soluble, monomer concentration is 15wt%, crosslinker concentration is 0.5wt%, forms monomer premixed liquid, in 100ml monomer premixed liquid, adds the aluminum oxide powder that 140g particle diameter is 1 μm, 40g kaolin, 6gMgCO
3, 6gBaCO
3with 4g talcum, dispersion agent is ammonium citrate 2g, stirs and obtains uniform ceramic size, catalyst n is added in above-mentioned slurry, N, N ', N '-Tetramethyl Ethylene Diamine 25 μ l, then stir, then add initiator 8% ammonium persulfate solution 50 μ l, after stirring, inject mould at once, and self-control Multi needle is become punch die (syringe needle φ=2mm, 4 hole/square centimeters) insert in slurry, be the demoulding after gel until slurry, obtain honeycomb and to wet base.Wet base is put into baking oven 50 DEG C of dryings 24 hours, dry base substrate is put into retort furnace (BTF-1700C), 1600 DEG C are warming up to speed 10 DEG C/min, organism completes eliminating in temperature-rise period, 1600 DEG C sinter 2 hours, are had the cellular alumina pottery of " duct inner wall extend whisker " structure.The SEM photo of the cellular alumina pottery that the present embodiment prepares and XRD figure and the obtained cellular alumina ceramic-like of embodiment 1 are seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 68%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 9MPa, axial compression strength 21MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the cellular alumina pottery of preparation has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, is conducive to counting of particle and discharges with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 3 is dry-pressing formed prepares cellular alumina pottery and performance thereof
Be 3 μm of aluminum oxide powders by 210g particle diameter, 60g kaolin, 6gBaCO
3mix with 18g rhombspar powder, add alcohol and abrading-ball wet-milling 24 hours, after drying and screening, add using material 5wt% paraffin after sieving as forming agent, rectangular sample (long 10cm is pressed in punching block, wide 5cm, high 5cm), pressure is 100MPa, the Multi needle of press-in self-control subsequently becomes punch die (syringe needle φ=2mm, 4 hole/square centimeters) and extract, obtained honeycomb body, this honeycomb body is put into draft glue discharging furnace be warming up to 800 DEG C and be incubated dewaxing in 3 hours, dry base substrate is put into retort furnace (BTF-1700C), 1600 DEG C of sintering 2.5 hours are warming up to speed 10 DEG C/min.Be there is the cellular alumina pottery of " duct inner wall extend whisker " structure.The SEM photo of the cellular alumina pottery that the present embodiment prepares and XRD figure and the obtained cellular alumina ceramic-like of embodiment 1 are seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 62%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 10MPa, axial compression strength 21MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the cellular alumina pottery of preparation has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, is conducive to counting of particle and discharges with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 4 direct coagulation casting prepares cellular alumina pottery and performance thereof
Be that alumina powder jointed and 8.5g sintering agent aluminum oxide powder and the 255g yttrium oxide powder of 1 μm mixes by 340g particle diameter, add 100ml deionized water fully to stir, slurry is cooled to about 5 DEG C, add analytically pure urea 1g and urease 20unit/mg, be stirred well to evenly, slurry is warming up to 25 DEG C, punch die is become to put into slurry Multi needle, static 1 hour, slurry curing, take out self-control Multi needle and become punch die (syringe needle φ=2mm, 4 hole/square centimeters), obtained cellular alumina base substrate.Base substrate is put into baking oven 40 DEG C of dryings 12 hours, dry base substrate is put into dry base substrate is put into retort furnace (BTF-1700C), 1600 DEG C are warming up to speed 10 DEG C/min, organism completes eliminating in temperature-rise period, 1600 DEG C sinter 3 hours, are had the cellular alumina pottery of " duct inner wall extend whisker " structure.The SEM photo of the cellular alumina pottery that the present embodiment prepares and XRD figure and the obtained cellular alumina ceramic-like of embodiment 1 are seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 72%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 12MPa, axial compression strength 28MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the cellular alumina pottery of preparation has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, is conducive to counting of particle and discharges with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 5 gel casting forming cellular alumina pottery and performance thereof
By monomeric acrylamide and linking agent N, N '-methylene-bisacrylamide is water-soluble, monomer concentration is 15wt%, crosslinker concentration is 0.5wt%, form monomer premixed liquid, the alumina powder jointed 240g that particle diameter is 1 μm is added in 100ml monomer premixed liquid, add the sintering agent calcium fluoride powder 9.6g of aluminum oxide powder the body burden 4% and Suzhou soil 12g of aluminum oxide powder body burden 5%, dispersion agent is ammonium citrate 1g, stir and obtain the ceramic size that solid load is about 40%, catalyst n is added in above-mentioned slurry, N, N ', N '-Tetramethyl Ethylene Diamine 25 μ l, then stir, add initiator 8% ammonium persulfate solution 50 μ l again, mould is injected at once after stirring, and self-control Multi needle is become punch die (syringe needle φ=2mm, 4 hole/square centimeters) insert in slurry, be the demoulding after gel until slurry, obtain honeycomb to wet base.Wet base is put into baking oven 50 DEG C of dryings 24 hours, dry base substrate is put into retort furnace (BTF-1700C), 1600 DEG C are warming up to speed 10 DEG C/min, organism completes eliminating in temperature-rise period, 1600 DEG C sinter 2 hours, are had the cellular alumina pottery of " duct inner wall extend whisker " structure.The SEM photo of the cellular alumina pottery that the present embodiment prepares and XRD figure and the obtained cellular alumina ceramic-like of embodiment 1 are seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 60%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 8MPa, axial compression strength 18MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the cellular alumina pottery of preparation has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, is conducive to counting of particle and discharges with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. a preparation method for cellular alumina pottery, is characterized in that, described method comprises the following steps:
1) preparation has the cellular alumina base substrate also drying of parallel channels;
2) organic eliminating is carried out to dried base substrate;
3) Calcined polishing aluminum oxide honeycomb body, obtains body portion particle and combines closely, and hole inner wall extend has the cellular alumina pottery of whisker;
Wherein, step 1) in be raw material with alumina powder jointed, and add sintering agent, dispersion agent, shaping medium mix, and prepares aluminum oxide base substrate;
Described alumina powder jointed particle diameter 0.5 μm ~ 3 μm, accounts for total powder 65 ~ 75wt%;
Described sintering agent is kaolin, CaCO
3, BaCO
3, MgCO
3, talcum, rhombspar and/or wollastonite, wherein, kaolin content is 9 ~ 20%, CaCO of total powder quality
3content is 0 ~ 3%, BaCO of total powder quality
3content is 0 ~ 3%, MgCO of total powder quality
3content is 0 ~ 3% of total powder quality, and talc content is 0 ~ 2% of total powder quality, and rhombspar content is 0 ~ 9% of total powder quality, and wollastonite content is 0 ~ 2% of total powder quality;
Step 2) in organism eliminating is carried out to dried base substrate, temperature is at 500 DEG C ~ 800 DEG C, and the time is 0.5 ~ 3h;
Step 3) in calcining temperature be 1580 DEG C ~ 1600 DEG C, insulation 1 ~ 3h.
2. preparation method as claimed in claim 1, is characterized in that, step 1) in there is parallel channels cellular alumina base substrate adopt extrusion moulding preparation.
3. preparation method as claimed in claim 1, it is characterized in that, step 1) in cellular alumina base substrate adopt dry pressing, gel casting forming method or direct coagulation casting method first to prepare biscuit, then adopt mechanical hole building method to obtain the cellular alumina base substrate with parallel channels.
4. the method for claim 1, is characterized in that, step 1) in the drying means of cellular alumina base substrate be that room temperature is dried in the shade or 40 DEG C ~ 60 DEG C oven dry, the parallel construction in maintenance honeycomb duct.
5. according to the preparation-obtained cellular alumina pottery of the arbitrary described preparation method of claim 1-4.
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