CN104072147A - Preparation method of silicon nitride honeycomb ceramics - Google Patents
Preparation method of silicon nitride honeycomb ceramics Download PDFInfo
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Abstract
The invention discloses a preparation method of silicon nitride honeycomb ceramics. The preparation method comprises the following steps: 1) preparing silicon nitride honeycomb blank bodies with parallel pore passages; 2) dumping or degreasing the silicon nitride honeycomb blank bodies; and 3) calcining the silicon nitride honeycomb blank bodies to obtain the silicon nitride honeycomb ceramics with pore passage inner wall extending whisker structures. The ceramic matrix part particles prepared by the method are tightly bonded and whiskers grow on the honeycomb pore inner walls. The honeycomb ceramics have the excellent properties such as high strength, low density, high temperature resistance, chemical corrosion resistance and the like and are suitable for filtration and purification of various fluids. According to the used honeycomb ceramics, filtered matters are easily obtained by adopting various methods and the honeycomb ceramics can be reused. The preparation method is simple in process, is low in equipment requirements, is convenient in operation control, has high production efficiency and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to material technology field, particularly, relate to and a kind ofly having the preparation method of the silicon nitride honeycomb pottery of " whisker intert parallel duct " structure.
Background technology
Ceramic honey comb has the pore texture of parallel perforation, 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 dwindle advantages such as filtering volume, at the aspects such as purifying treatment of the filtration of the filtration, purification of industrial gaseous waste, motor-vehicle tail-gas and other life waste gas, the heat exchange of metallurgical industry and molten metal, the toxic gas of mining industry and liquid, have a wide range of applications.
Ceramic honey comb has the special channel architecture that is parallel to each other.Pore-forming principle based on different, the preparation of ceramic honey comb mainly contains the several methods such as mould extrusion moulding, impregnation sintering and lyophilize.
Extrusion moulding is first prepared mould according to the size of required honeycomb hole and shape (trilateral, rhombus, rectangle, hexagon etc.), then prepares by the extrusion of ceramic size the ceramic honey comb that high-sequential is arranged in duct.U.S. Corning company and Japanese NGK company are comparatively ripe in this technical grasp, have realized industrialization and have produced.The ceramic honey comb of preparation is mainly used in vehicle exhaust and heat accumulation block materials.The greatest problem of the method is that material aperture is limited by the preparation of mould, is difficult to prepare aperture at the cellular material of tens micron dimensions.The up-to-date ceramic honey comb product of Corning company can be prepared at most 1200 through holes on the cross section of 1 square inch, is that current known the method can be prepared the limit in ceramic honey comb aperture, and further reduced bore is very difficult.
Impregnation sintering method is that the tinsel that first thickness is about to 0.1mm is rolled into spination paillon foil, is sticked into after through-hole structure, then this through-hole structure matrix is entered in ceramic size with binding agent, and final drying, sintering are prepared into ceramic honey comb.The problem of the method and mould extrusion moulding are similar, are all mechanical hole fabrication technique, and aperture is subject to the restriction of spination paillon foil rolling process, and further reduced bore is very difficult.
Freeze drying process is relatively new ceramic honey comb moulding process, not yet realizes at present large-scale commercial production.First this technique add the volatile materials of the easy crystallization high temperature of low temperature such as water, amphene, camphor in ceramic size, then ceramic size is injected to the container that is placed on the surrounding heat insulation bottom heat conduction on refrigerant, by controlling thermograde, realize the solvent continuously-directional crystallization in slurry, simultaneously separated with powder granule.After lyophilize, ice crystal distils under vacuum, and the microtexture that ice crystal forms is retained, thereby obtains having the base substrate of directed through-hole structure, then makes porous ceramics through sintering.The method is by chemicrystallization, distillation and phase disengagement method pore-forming, has broken away from mechanical processing technique restriction, and 80 microns of left and right can be down in the ceramic honey comb aperture of preparation.Yet, in the freezing casting process of this technique, be difficult to the synchronous change of the thermograde of control same level, cause the straight parallel general character in duct of prepared ceramic honey comb poor, this is the subject matter of the method, and in addition, this technique exists a series of technology barriers in large-scale application fashion, processing condition and process are difficult to accurate control, have restricted it and have applied on a large scale.
Can say, the preparation difficult point of ceramic honey comb and focus concentrate on the hole count of further increase unit surface always, in the research of reduced bore.Yet, it is pointed out that the aperture that enables further to reduce ceramic honey comb is reduced to micron dimension, its aperture dwindle the increase suddenly that will cause gas to pass through resistance, thereby reduce filtration efficiency.That is, relying on single honeycomb structure to be difficult to solve subparticle filters desired small-bore and keeps unimpeded this contradiction of air-flow simultaneously.
Whisker is the single crystal of a kind of high strength beard shape synthetic under manual control condition, and its crystalline structure is more complete, and subsurface defect is few, and its strength and modulus all approaches ideal crystal.Therefore, whisker Chang Zuowei reinforcing component join metal matrix, ceramic base and polymer-based in it strengthens toughness reinforcing effect.Modal whisker has Si
3n
4, SiC, Al
2o
3deng.Yet the current research about whisker mainly concentrates on the preparation of whisker and matrix is strengthened on toughening effect, and the research about whisker in other purposes rarely has report.In the preparation research of whisker, there is report to point out to utilize the hole can growth in situ whisker, as patent CN102251284A (a kind of method of preparing beta-silicon nitride whisker), and document (Ji Xiaoli, Xu Fei, power its people, Wan Weiwei, On In-situ Synthesis of Mullite Whisker And strengthens foam silicon carbide ceramics, Chinese powder technology, 2011,17 (3): 33-36) and document (Lv Chenjing, Tian Xiushu, Han Yufang, the synthetic Al that contains of original position
2o
3whisker Al
2o
3the research of/Ti-Al matrix material mechanism), yet former concerns is in the preparation of whisker, and both pay close attention to the reinforced effects of whisker to matrix or foam base plate afterwards.Meanwhile, porous body and the hole in parts that above document is prepared are closed pore, are difficult to use in filtration.
The present invention is based on hole the principle that space can growth in situ whisker is provided, select Si
3n
4for raw material, by controlling sintering condition, prepare the New Si of " duct inner wall extend whisker "
3n
4ceramic honey comb.The present invention is intended to utilize parallel duct to guarantee the unimpeded of fluid, utilizes the whisker of duct inner wall extend to increase the filtration to fine particle.The present invention synthesizes whisker at honeycomb structure situ first, and has developed whisker new application in filtration and field of purification in conjunction with honeycomb structure.
Summary of the invention
The preparation method who the invention provides a kind of silicon nitride honeycomb pottery, comprises the following steps:
1) preparation has the silicon nitride honeycomb base substrate in parallel duct and is dried;
2) dried base substrate is carried out to organic eliminating;
3) calcining silicon nitride honeycomb base substrate, obtains body portion particle in conjunction with tight, and hole inner wall extend has the silicon nitride honeycomb pottery of whisker.
Wherein, in step 1), there is the silicon nitride honeycomb base substrate employing extrusion moulding preparation in parallel duct.In the art, extruding forming method is to prepare the method that ceramic honey comb is conventional, can directly prepare silicon nitride honeycomb base substrate.
In the inventive method, in step 1), silicon nitride honeycomb 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 make to have the silicon nitride honeycomb base substrate in parallel duct.
In a plurality of embodiment of the present invention, be to adopt self-control Multi needle to become punch die, make the silicon nitride honeycomb base substrate with parallel duct.
In the inventive method, in step 1), take beta-silicon nitride powder as raw material, and add sintering agent, shaping medium, dispersion agent to mix, prepare silicon nitride base substrate.
Described beta-silicon nitride powder particle diameter 0.5 μ m～2.5 μ m, untreated or process oxide treatment.In step 1), beta-silicon nitride powder addition is the 65～90wt% that comprises the powder gross weight of silicon nitride powder, sintering agent and dispersion agent.
Described sintering agent is aluminum oxide powder and yttrium oxide powder, aluminum oxide powder particle diameter 0.3 μ m～5.0 μ m, the 2-4wt% that addition is beta-silicon nitride powder; Yttrium oxide particle diameter is 0.1 μ m～5.0 μ m, the 6-8wt% that addition is beta-silicon nitride powder.
Dispersion agent is mainly used in the colloidal formation techniques such as gel injection molding and forming technology, direct coagulation casting, and the present invention does not also rely on specific dispersion agent, as long as dispersion agent can be so that ceramic powder suitably disperses in sauce.Operable dispersion agent is ammonium polyacrylate, Tetramethylammonium hydroxide, ammonium citrate, ammonium polymethacrylate, Tetramethyl Ethylene Diamine, Sodium hexametaphosphate 99 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.It is shaping medium that gel casting forming is selected water base acrylamide polymerization system, and wherein monomer is acrylamide, and linking agent is N, N '-methylene-bisacrylamide, and initiator is 8% ammonium persulfate solution, catalyzer is N,N,N′,N′ tetramethylethylene diamine.It is shaping medium that direct coagulation casting is selected urea and urease.
The additives such as raw material beta-silicon nitride powder involved in the present invention, sintering agent powder and dispersion agent, shaping medium are common commercial powder, its purity is commercial level, but can, further according to the requirement of product purity is adjusted, also can adopt the rank reagent such as analytical pure.
The more little sintering that is more conducive to of powder granularity of raw material beta-silicon nitride powder involved in the present invention, sintering agent powder and dispersion agent, shaping medium etc., the preferred following powder of 2.0 μ m, but be not limited to this scope.
According to different forming methods, additive can be different as dispersion agent, shaping medium etc., and the solid load of base substrate also can be different.
In the inventive method, step 2) in, silicon nitride honeycomb base substrate is dry, and room temperature is dried in the shade or 40 ℃～60 ℃ oven dry, keeps the parallel construction in honeycomb duct.
Step 2) in, dried base substrate is carried out to organism eliminating, temperature is at 500 ℃～800 ℃, and the time is 0.5～3 hour.
According to different forming methods, its time of drying/temperature/humidity is different, take that to keep base substrate indeformable be standard.Because of organic content difference in different forming method base substrates, 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 independent degreasing program of 1 hour to 1 day, and in the prepared base substrate of gel casting forming and direct coagulation casting, organic content is lower, is easy to binder removal in the rapid heating condition before sintering.This process is familiar with by those skilled in the art.
In the inventive method, in step 3), silicon nitride honeycomb base substrate is calcined, calcining temperature is 1650 ℃～1750 ℃, insulation 0.5h～3h.
Preferably, in step 3), silicon nitride honeycomb base substrate is calcined, calcining temperature is 1700 ℃, and soaking time is 3h.
The present invention also provides above-mentioned preparation method preparation-obtained silicon nitride honeycomb pottery.
The present invention proposes on the framework of ceramic honey comb base substrate, utilize the principle of hole growth whisker, prepare hole wall and be the silicon nitride honeycomb pottery of " whisker intert parallel duct " novel texture of whisker, the whisker stretching in this novel texture silicon nitride honeycomb pottery duct can effectively carry out the filtration of fine particle, and its original basic honeycomb parallel via holes structure has guaranteed the smoothness of fluid.
The ceramic honey comb of " duct inner wall extend whisker " novel texture proposed by the invention, is not only applicable to silicon nitride, is also applicable to generate the material such as silicon carbide, aluminum oxide of whisker under similar or catalytic condition simultaneously.The ceramic honey comb of " duct inner wall extend whisker " novel texture of preparation, is not limited to pore size, increases the efficiency such as filtration by hole, separation, enrichment by aperture inner wall extend whisker.Ceramic honey comb after use is easy to adopt several different methods to remove filtrate, reusable.
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 of preparing by method of the present invention is silicon nitride material, there is the premium propertiess such as high strength, low density, high temperature resistant, resistance to chemical attack, be applicable to filtration and the purification of multiple fluid, the waste gas producing as fine particle in air, various commercial run, the filtration, purification of its other life waste gas of motor-vehicle tail-gas, also can be used for analyzing the tabular adsorbent of use chromatographic column, to the filtration of the heat exchange of metallurgical industry and molten metal, to the purifying treatment of the toxic gas of mining industry and liquid etc.Scanning electron microscope (SEM) shows that ceramic honey comb body portion particle of the present invention is in conjunction with tight, and honeycomb hole inwall grows into whisker, forms parallel duct.This structure makes ceramic honey comb of the present invention can by straight-through duct, keep the smoothness of fluid in use, and the whisker of passing hole channel inner wall extend further filters, cleansing fluid.
Accompanying drawing explanation
Fig. 1 is silicon nitride ceramics " duct inner wall extend whisker " the SEM photo that embodiment 1 makes.
Fig. 2 is silicon nitride ceramics " the duct inner wall extend whisker " XRD figure that embodiment 1 makes.
Embodiment
Following examples are used for illustrating 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 modification that the inventive method, step or condition are done or replacement, all belong to scope of the present invention.
If do not specialize, in embodiment, chemical feedstocks used is conventional marketable material, the conventional means that in embodiment, technique means used is well known to those skilled in the art.
Silicon nitride honeycomb pottery and performance thereof are prepared in embodiment 1 extrusion moulding
Getting 200g particle diameter is 2 μ m silicon nitride powders, and 5g particle diameter is that 3 μ m aluminum oxide and 15g particle diameter are 2 μ m yttrium oxide, mixes, and obtains powdered mixture.Water, polyvinyl alcohol and the acid of poly-hydroxyl ethanol being pressed to the weight ratio of 70:10:20 mixes, stirring makes homogeneous solution, solution is mixed according to the weight ratio of 100:70 with above-mentioned powder mixture, normal temperature fully mixing 0.75 hour in mixing roll (BL-6175-B) at normal temperatures and pressures, under normal temperature and pressure old 3 hours, obtain pug.Pug is crossed to 60 mesh sieves and carry out filtration, purification, by honeycomb ceramic extruding machine (BL-6177), extrude the honeycomb biscuit with parallel duct, 40 ℃ are dried 6 hours, after dry, sample is removed organism 2h at 600 ℃ of binder removals, then the honeycomb biscuit after binder removal is put into sintering oven, with 10 ℃/min, be warming up to 1700 ℃, under the nitrogen pressure of 0.5MPa, sintering is 2.5 hours, is had " duct inner wall extend whisker " structure silicon nitride honeycomb pottery.Fig. 1 is shown in by its SEM photo, and XRD figure is shown in Fig. 2.The silicon nitride honeycomb ceramic matrix part particle that scanning electron microscope (SEM) demonstration the present embodiment makes is in conjunction with tight, and honeycomb hole inwall grows into whisker, forms parallel duct.
This ceramic honey comb aperture is 0.5mm, and void content is 68%.Method according to GB/T1964 regulation detects, and obtaining horizontal ultimate compression strength is 9MPa, axial compression strength 21MPa.Ceramic honey comb is boiled after 0.5 hour and placed after 24 hours again with 10% salpeter solution, and solution is water white transparency, and resist chemical performance is good.After testing, the silicon nitride honeycomb 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 dwindle filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 2 gel casting formings are prepared silicon nitride honeycomb pottery and performance thereof
By monomer acrylamide and linking agent N, N '-methylene-bisacrylamide is water-soluble, monomer acrylamide concentration is 15wt%, crosslinker concentration is 0.5wt%, form monomer premixed liquid, in 100ml monomer premixed liquid, adding particle diameter is 0.5 μ m beta-silicon nitride powder 230g, the particle diameter that adds silicon nitride powder body burden 2.5% is that the particle diameter of 0.3 μ m sintering agent aluminum oxide powder 5.75g and silicon nitride powder body burden 7.5% is 0.1 μ m yttrium oxide powder 17.25g, dispersion agent is ammonium citrate 2g, stirring obtains solid load and is about 40% ceramic size, in above-mentioned slurry, add catalyst n, N, N ', N '-Tetramethyl Ethylene Diamine 25 μ l, then stir, add again initiator 8% ammonium persulfate solution 50 μ l, after stirring, inject at once mould, and will make Multi needle by oneself and become punch die (syringe needle φ=2mm, 4 hole/square centimeters) insert in slurry, the demoulding after slurry is gel, obtain the wet base of honeycomb.The base that will wet is put into 50 ℃, baking oven and is dried 24 hours, dry base substrate is put into multifunctional sintering furnace (HIGH-MUTLI5000), with speed, 10 ℃/min is warming up to 1650 ℃, and in temperature-rise period, organism completes eliminating, and under the nitrogen pressure of 0.5MPa, 1650 ℃ of sintering are 2 hours.There is " duct inner wall extend whisker " structure silicon nitride honeycomb pottery.The silicon nitride honeycomb ceramic-like that the SEM photo of the silicon nitride honeycomb pottery that the present embodiment prepares and XRD figure and embodiment 1 make seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 65%.Method according to GB/T1964 regulation detects, and obtaining horizontal ultimate compression strength is 13MPa, axial compression strength 28MPa.Ceramic honey comb is boiled after 0.5 hour and placed after 24 hours again with 10% salpeter solution, and solution is water white transparency, and resist chemical performance is good.After testing, the silicon nitride honeycomb 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 dwindle filtration volume, the excellent specific properties such as the smoothness of fluid.
Dry-pressing formed silicon nitride honeycomb pottery and the performance thereof prepared of embodiment 3
By 200g particle diameter, be that 2.5 μ m beta-silicon nitride powders and 5g particle diameter are that 5 μ m sintering agent aluminum oxide powders and 15g particle diameter are that 2 μ m yttrium oxide powders mix, add alcohol and abrading-ball wet-milling 24 hours, after drying and screening, after adding to sieve, material is counted 5wt% paraffin as forming agent, in punching block, be pressed into rectangular sample (long 10cm, wide 5cm, high 5cm), pressure is 120MPa, be pressed into subsequently self-control Multi needle and become punch die (syringe needle φ=2mm, 4 hole/square centimeters) and extract, make honeycomb base substrate, this honeycomb base substrate is put into draft glue discharging furnace and be warming up to 800 ℃ and be incubated dewaxing in 3 hours, dry base substrate is put into multifunctional sintering furnace (HIGH-MUTLI5000), with 10 ℃/min of speed, be warming up to 1700 ℃, under the nitrogen pressure of 0.5MPa, sintering is 1.5 hours.There is " duct inner wall extend whisker " structure silicon nitride honeycomb pottery.The silicon nitride honeycomb ceramic-like that the SEM photo of the silicon nitride honeycomb pottery that the present embodiment prepares and XRD figure and embodiment 1 make seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 62%.Method according to GB/T1964 regulation detects, and obtaining horizontal ultimate compression strength is 10MPa, axial compression strength 21MPa.Ceramic honey comb is boiled after 0.5 hour and placed after 24 hours again with 10% salpeter solution, and solution is water white transparency, and resist chemical performance is good.After testing, the silicon nitride honeycomb 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 dwindle filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 4 direct coagulation castings are prepared silicon nitride honeycomb pottery and performance thereof
By 340g particle diameter, be that 2 μ m beta-silicon nitride powders and 8.5g particle diameter are that 3 μ m sintering agent aluminum oxide powders and 255g particle diameter are that 3 μ m yttrium oxide powders mix, add 100ml deionized water fully to stir, slurry is cooled to 5 ℃ of left and right, adds analytically pure urea 1g and urease 20unit/mg, be stirred well to evenly, slurry is warming up to 25 ℃, become punch die to put into slurry Multi needle, static 1 hour, slurry curing, take out Multi needle and become punch die, make silicon nitride honeycomb base substrate.Base substrate is put into 40 ℃, baking oven and be dried 12 hours, dry base substrate is put into dry base substrate is put into multifunctional sintering furnace (HIGH-MUTLI5000), with speed, 10 ℃/min is warming up to 1700 ℃, and in temperature-rise period, organism completes eliminating, and under the nitrogen pressure of 0.5MPa, 1700 ℃ of sintering are 3 hours.There is " duct inner wall extend whisker " structure silicon nitride honeycomb pottery.The silicon nitride honeycomb ceramic-like that the SEM photo of the silicon nitride honeycomb pottery that the present embodiment prepares and XRD figure and embodiment 1 make seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 72%.Method according to GB/T1964 regulation detects, and obtaining horizontal ultimate compression strength is 12MPa, axial compression strength 28MPa.Ceramic honey comb is boiled after 0.5 hour and placed after 24 hours again with 10% salpeter solution, and solution is water white transparency, and resist chemical performance is good.After testing, the silicon nitride honeycomb 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 dwindle 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, do not departing under the prerequisite of 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 (10)
1. a preparation method for silicon nitride honeycomb pottery, is characterized in that, described method comprises the following steps:
1) preparation has the silicon nitride honeycomb base substrate in parallel duct and is dried;
2) dried base substrate is carried out to organic eliminating;
3) calcining silicon nitride honeycomb base substrate, obtains body portion particle in conjunction with tight, and hole inner wall extend has the silicon nitride honeycomb pottery of whisker.
2. preparation method as claimed in claim 1, is characterized in that, the silicon nitride honeycomb base substrate in step 1) with parallel duct adopts extrusion moulding preparation.
3. preparation method as claimed in claim 1, it is characterized in that, in step 1), silicon nitride honeycomb base substrate adopts dry pressing, gel casting forming method or direct coagulation casting method first to prepare biscuit, then adopts mechanical hole building method to make to have the silicon nitride honeycomb base substrate in parallel duct.
4. preparation method as claimed in claim 1, is characterized in that, take beta-silicon nitride powder as raw material in step 1), and adds sintering agent, dispersion agent, shaping medium, deionized water to mix, and prepares silicon nitride base substrate.
5. method as claimed in claim 3, is characterized in that, beta-silicon nitride powder particle diameter 0.5 μ m～2.5 μ m described in step 1), and beta-silicon nitride powder addition is the 65～90wt% that comprises the powder gross weight of silicon nitride powder, sintering agent and dispersion agent.
6. method as claimed in claim 3, is characterized in that, described sintering agent is aluminum oxide powder and yttrium oxide powder, aluminum oxide powder particle diameter 0.3 μ m～5.0 μ m, the 2-4wt% that addition is beta-silicon nitride powder; Yttrium oxide particle diameter is 0.1 μ m～5.0 μ m, the 6-8wt% that addition is beta-silicon nitride powder.
7. the method as described in as arbitrary in claim 1～3, is characterized in that, in step 1), the drying means of silicon nitride honeycomb base substrate is that room temperature is dried in the shade or 40 ℃～60 ℃ oven dry, keeps the parallel construction in honeycomb duct.
8. the method for claim 1, is characterized in that step 2) in dried base substrate is carried out to organism eliminating, temperature is at 500 ℃～800 ℃, the time is 0.5～3 hour.
9. the method for claim 1, is characterized in that, in step 3), calcining temperature is 1650 ℃～1750 ℃, insulation 0.5h～3h, pressure 0.5MPa.
10. according to claim 1, require the preparation-obtained silicon nitride honeycomb pottery of described preparation method.
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