CN102643095A - SiC honeycomb ceramics material and preparation method thereof - Google Patents

SiC honeycomb ceramics material and preparation method thereof Download PDF

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Publication number
CN102643095A
CN102643095A CN2012101097289A CN201210109728A CN102643095A CN 102643095 A CN102643095 A CN 102643095A CN 2012101097289 A CN2012101097289 A CN 2012101097289A CN 201210109728 A CN201210109728 A CN 201210109728A CN 102643095 A CN102643095 A CN 102643095A
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honey comb
combed
ceramic honey
sic
powder
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CN102643095B (en
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张劲松
田冲
杨振明
曹小明
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The invention belongs to the field of a porous ceramic material and a preparation technology thereof, particularly relates to a SiC honeycomb ceramics material which is thin in porous wall, high in strength, high in specific surface, low in expansion, high in heat conductivity, high in thermal shock resistance, and controllable in structure and a preparation method of the SiC honeycomb ceramics material. The SiC honeycomb ceramics material has a continuous and single integrated structure which is similar to the shape of a honeycomb, and is provided with a plurality of in-parallel passageways along the axial direction, wherein the shapes of the passageways can be triangular, wavelike and the like; the number of pores in each unit area, which form into a honeycomb structure, can be controlled in a range of 100/cm<2> to 5/cm<2>, and the thickness of the pore walls can be controlled in a range of 0.2mm to 2mm; the pore walls can be in an impact structure, and have a micro-pore structure as well; and the invention takes organic resin and SiC powder as main raw material, and the main raw material is prepared into a single-layer structure by a mould pressing technology and is assembled into the honeycomb structure, and is reacted, infiltrated and sintered into a final product after being pyrolyzed. The preparation technology provided by the invention is simple in technology, convenient to operate, free from complex equipment, and low in manufacture cost.

Description

A kind of SiC ceramic honey comb material and preparation method thereof
Technical field
The invention belongs to porous ceramic film material and preparing technical field thereof, be specially SiC ceramic honey comb material of a kind of stephanoporate thin wall, HS, high-ratio surface, low bulk, high heat conduction, thermal shock resistance height, controllable structure and preparation method thereof.
Background technology
Ceramic honey comb has continuous single one-piece construction, and many parallel passages are arranged vertically, and the shape of passage can be circle, square, trilateral, sexangle, waveform etc., gains the name because being similar to favose structure.Therefore, with general block ceramic phase ratio, ceramic honey comb has characteristics such as void content height, specific surface area is big, erosion resistance is strong, weight is lighter; For general granular carrier; Have that gas-flow resistance is little, the unit geometrical surface is big, bulk specific gravity is little, pressure fall little, diffusion length is little, be beneficial to the advantage such as leave away of entering and the resultant of reactant, therefore be specially adapted to adsorb and the support of the catalyst of various uses; In addition, because fluid can be through the hole that runs through upper and lower surfaces on the ceramic honey comb partition, the partition of ceramic honey comb capable of using carries out heat exchange and chemical reaction.At present, ceramic honey comb has been applied to the aspects such as purification, purifying vehicle exhaust and noise elimination, WWT, petrochemical refinery and molten metal filtration of industrial gaseous waste.
Ceramic honey comb can be processed by various material, mainly contains trichroite, mullite, aluminium titanates, silit and silicon nitride etc.Wherein, the SiC ceramic honey comb has the thermal conductivity height, volume density is little, specific surface area is high and high temperature resistant, characteristics such as chemicalstability good, intensity height, therefore is suitable for the environment of high temperature, burn into oxidation, and application prospect is more extensive.
But existing problems were a lot of when extruding shaping technique prepared the SiC ceramic honey comb at present, low precision, distortion, rimose possibility height during moulding; Mould is made difficulty, serious wear, and the life-span is low; The drying process organic composition must discharge totally fully, controls the bad biscuit damage that is prone to cause, and yielding in the sintering, intensity is not high, and above reason causes the material prepn cost high, and performance is not high, has therefore limited applying of this kind ceramic honey comb.
Summary of the invention
The object of the present invention is to provide SiC ceramic honey comb material of a kind of high-strength, high-ratio surface, controllable structure and preparation method thereof; Said ceramic honey comb material has the fundamental characteristics of SiC pottery, as intensity is high, thermal expansivity is low, resistance to chemical attack, anti-oxidant, high-temperature stable good, thermal shock resistance is strong etc.; The characteristics that have high-ratio surface, low volume density, high porosity simultaneously; Said preparing method's technology is simple, and cost is low.
Technical scheme of the present invention is:
A kind of SiC ceramic honey comb material, said ceramic honey comb material is SiC, has continuous single honeycombed one-piece construction, and parallel passage is arranged vertically, the shape of passage is trilateral or waveform; The unit surface hole count of forming honey-combed is controlled at 100~5/cm 2Between, pore wall thickness is controlled between 0.2~2mm.
Said SiC ceramic honey comb material, the hole wall structure of forming honey-combed is a dense structure, perhaps adopts pore-creating technology to become a micron vesicular structure.
Said SiC ceramic honey comb preparation methods is raw material with powder of solid particles with the macromolecular material that has than high carbon output rate, adopts mold pressing to prepare individual layer cellular unit combination back pyrolysis, sintering, and it is following specifically to prepare process:
(1) preparation of raw material
With powder of solid particles, macromolecular material, solidifying agent by mass percentage example be (70wt%~20wt%): (20wt%~70wt%): (1wt%~10wt%) be dissolved in the organic solvent altogether; Ball milling after mechanical stirring; Filter; Get slip, said slurry solution solute is 5~80% of a total mass; After certain amount of organic solvent in the air-dry removal slip, making the organic solvent mass content after air-dry is between 10~15%;
Powder of solid particles is carborundum powder, silica flour or the two mixed powder; Macromolecular material is selected from a kind of of epoxy resin, resol and furfuryl resin or several kinds; Solidifying agent is: tosic acid, urotropine, oxalic acid or Hydrocerol A;
(2) compression molding and assembling
Above-mentioned raw materials evenly is coated on the Z 150PH non-woven fabrics, is layered on back matched moulds on the one side of splitting forming mould of heating then, become the individual layer cellular unit of mold shape; Perhaps; Adopt the gear pair roller of heating; Non-woven fabrics after applying is pushed curing molding between pair roller be the individual layer cellular unit with profile of tooth; Then requisite number purpose individual layer cellular unit is got up with the bonding folded buttress of slip, solidify bonding slip and make it fixedly to become the honey-combed precast body, the preheating temperature of splitting forming mould or gear pair roller is 120-180 ℃;
(3) pyrolysis
With the pyrolysis under the protective atmosphere of argon gas, nitrogen or other rare gas element of honey-combed precast body, perhaps pyrolysis under vacuum condition generates the carbonaceous honey-combed, and the Z 150PH non-woven fabrics is burnt therebetween; Wherein, 1~10 ℃ of temperature rise rate PM is warming up to 800~1200 ℃, is incubated 0.5~2 hour;
(4) liquid phase reaction infiltration
The carbonaceous honey-combed that pyrolysis is obtained reacts melting infiltration sintering; The raw material of selecting for use in the reaction sintering infiltration is a silicon, and the sintering siliconising is perhaps carried out in sintering siliconising under the protective atmosphere of argon gas, nitrogen or other rare gas element under vacuum condition; Temperature rise rate is 5~15 ℃ of PMs; Melt temperature is: 1400~1900 ℃, be incubated 0.5~5 hour, and get SiC ceramic honey comb material.
Said organic solvent is ethanol or formaldehyde, and solvent quality concentration is between 50-90%.
Said silica flour and carborundum powder purity are more than 95%, and mean particle size is 10nm~25 μ m.
Said curing agent content is 1~10% of a high molecular material resin quality; Under 100~250 ℃ of temperature, solidify 1~10 minute time.
Said compression molding mould is split cavity or gear mesh roller die tool, and mould molding is shaped as the individual layer of required honey-combed, and the single layer structure of compression moulding is trilateral or waveform; Wall thickness is controlled between 0.2~2mm, and the unit surface hole count that is assembled into honey-combed can be controlled in 100~5/cm 2Between.
Said SiC ceramic honey comb preparation methods adopts carborundum powder or carborundum powder and silica flour mixed powder, and when wherein adopting mixed powder, the two mass ratio is (20~90%): (80~10%).
The present invention mixes the air-dry slip of processing with powder of solid particles (carborundum powder, silica flour or the two mixed powder) with the polymer of high carbon output rate; Slip is evenly applied the Z 150PH non-woven fabrics; Then it is layered on matched moulds pressurization in back on the one side of splitting forming mould of heating; Make the slip compact curing, become individual layer cellular unit, perhaps adopt the profile of tooth pair roller extrusion molding of heating with mold shape; After with the individual layer cellular unit that obtains the bonding folded buttress of slip with dilution, solidify the back and fixedly become the honey-combed precast body.
Honey-combed precast body after solidifying is carried out pyrolysis in vacuum or inert atmosphere furnace, obtain and the equiform carbon honey-combed of forming by solid powder particle and RESEARCH OF PYROCARBON of honey-combed precast body.
In the reaction sintering infiltration; It is overheated that silicon melt is melted under vacuum or protective atmosphere; And then the carbon of carbon honey-combed and gas phase or liquid-phase silicone reaction generate silit, and combine and obtain high-strength, high-ratio surface, controllable structure SiC ceramic honey comb material with original silicon-carbide particle in the carbon honey-combed.
The present invention is avoiding traditional preparation process SiC ceramic honey comb extrusion process poor controllability, on the high basis of cost, has developed a kind of high-strength, high-ratio surface, controllable structure SiC ceramic honey comb material and technology of preparing thereof, has following advantage:
1, the honeycomb pass is controlled.The compression molding mould is a split cavity in the SiC ceramic honey comb preparation methods according to the invention; Mould molding is shaped as the individual layer shape of required honey-combed; When making, mould can be shaped as trilateral, waveform etc. by the designing mould fluting; Shown in accompanying drawing 1, mould fluting spacing and fluting size can be regulated, and then are made as corresponding shape in that the single layer structure of slip compression moulding is controlled; Control just can be adjusted pore wall thickness in the die clearance up and down again; Perhaps adopt profile of tooth pair roller extrusion process to prepare cellular unit; The pair roller profile of tooth can be a trilateral, also can be waveform, roller adjustable gaps joint; Cellular unit shape, controllable thickness, the unit surface hole count that is assembled into honey-combed can be controlled in 100~5/cm 2Between, hole wall can be controlled between 0.2~2mm.
2, the SiC ceramic honey comb strength of materials is good.The present invention adopts the organic polymer pyrolysis to obtain carbon matrix precursor and liquid phase reaction melting infiltration sintering technology; The silicon carbide powder particle mortise of adding in silit that the carbon that the resin pyrolysis obtains generates in the infiltration reaction and the slip, thereby silicon carbide ceramics phase particle bonding strength is high, has strong interaction; Homogeneous microstructure is fine and closely woven; Guaranteed that material has high mechanical property, avoided traditional pressureless sintering method prepare SiC stupalith SiC particle combine not firm, the shortcoming that intensity is not high.
3, the hole wall structure of SiC ceramic honey comb material can be controlled, and both can obtain fine and close hole wall, also can obtain a micron porous hole wall.Can add the pore-creating raw material in the preparation of raw material of the present invention, the control soaking time obtains a micron porous hole wall structure in sintering, also can not add the pore-creating raw material, directly obtains the ceramic honey comb material of fine and close hole wall behind the sintering.
4, technology is simple, and cost is low.Preparation technology is loaded down with trivial details in legacy cellular pottery extruding, the old-extrusion molding-drying-firing process that comprises that main raw material synthesize-mixes, and every step process requires all very strict, and raw material should be beneficial to extrusion molding and be beneficial to sintering again, and component is complicacy very; Extrusion process requires very high to mould, Mould Machining is difficult, the life-span is low, cost is high; Drying process is complicated, easy of crack; Sintering process control difficulty, the risk of distortion is high, and yield rate is low thus, and the material prepn cost is high.And the present invention prepares the SiC ceramic honey comb, and raw material is prepared easily; No extrusion process, Mould Machining is simple, the life-span is high; After the moulding in pyrolysis and the sintering process pottery not fragile, yield rate is high, technology is simple, and is with low cost.
In sum, the invention provides a kind of high-strength, high-ratio surface, controllable structure SiC ceramic honey comb material and technology of preparing thereof.This kind ceramic honey comb has been realized high-performance and has organically combined cheaply that preparation process is simple, and controllability is high, and yield rate is high.
Description of drawings
Fig. 1 is that the present invention splits the mould synoptic diagram.
Fig. 2 is a profile of tooth pair roller synoptic diagram of the present invention.
Among the figure, 1 patrix; 2 counterdies; Nest unit, 3 individual layer peak; Serrated roller on 4; 5 lower toothed rollers.
Embodiment
The material of ceramic honey comb material of the present invention is SiC, and the ceramic honey comb material has continuously the single favose one-piece construction that is similar to, and many parallel passages are arranged vertically, and the shape of passage can be trilateral, waveform etc.; The unit surface hole count of forming honey-combed can be controlled in 100~5/cm 2Between, pore wall thickness can be controlled between 0.2~2mm.Honeycomb porous structure is controlled, and the hole wall structure of forming honey-combed can be dense structure, also can adopt pore-creating technology to become a micron vesicular structure.
Ceramic honey comb preparation methods technology of the present invention is simple, mainly comprises feedstock production, mold pressing unit formation, assembling and pyrolysis and firing process.
This preparation method is raw material with powder of solid particles with the macromolecular material that has than high carbon output rate, and mold pressing prepares individual layer cellular unit combination back pyrolysis, sintering, and it is following specifically to prepare process:
(1) powder of solid particles (carborundum powder, silica flour or the two powder mix), macromolecular material, solidifying agent and organic solvent in certain ratio are mixed, ball milling after mechanical stirring filters, and gets slip, and said slurry solution solute is 5~80% of a total mass; After certain amount of organic solvent in the air-dry removal slip, making the organic solvent mass content after air-dry is between 10~15%.
The macromolecular material that adopts is selected from a kind of of epoxy resin, resol and furfuryl resin or several kinds; Powder of solid particles can be carborundum powder, silica flour or the two mixed powder; Silica flour and carborundum powder purity are more than the 95wt%, and mean particle size is 10nm~25 μ m; Organic solvent can be ethanol, formaldehyde etc., between the solvent quality concentration 50-90%; Solidifying agent is: tosic acid, urotropine, oxalic acid or Hydrocerol A etc.; Content is 1~10% of high molecular material resin quality; Under 100~250 ℃ of temperature, solidify; 1~10 minute time, the mass percent example is (70wt%~20wt%): (20wt%~70wt%): (1wt%~10wt%) between powder of solid particles, macromolecular material and the solidifying agent.As adopting carborundum powder and silica flour mixed powder, the two mass ratio is (20~90%): (80~10%).
(2) compression molding and assembling
Step (1) is obtained raw material evenly to be coated on the Z 150PH non-woven fabrics; Be layered on back matched moulds on the one side of splitting forming mould (seeing accompanying drawing 1) of heating then; In addition certain pressure is depressed into the spacing place that mould is subscribed then, and making macromolecular material is that the slip of tackiness agent can compact curing under pressure, becomes the individual layer cellular unit of mold shape; Perhaps adopt the gear pair roller (seeing accompanying drawing 2) of heating; Non-woven fabrics after applying is pushed curing molding between pair roller be the individual layer cellular unit with profile of tooth, then the slip bonding folded buttress of requisite number purpose individual layer cellular unit with dilution got up, and solidifies bonding slip and make it fixedly to become the honey-combed precast body.The preheating temperature of splitting forming mould or gear pair roller here is 120-180 ℃.
As shown in Figure 1, the compression molding mould is the mould of splitting of patrix 1 and counterdie 2, and mould molding is shaped as the nest unit, individual layer peak 3 of required honey-combed, and nest unit, individual layer peak 3 structures of compression moulding can be trilateral, waveform etc.As shown in Figure 2, the profile of tooth pair roller is that last serrated roller 4, lower toothed roller 5 are oppositely arranged structure, and the individual layer cellular unit 3 that the profile of tooth pair roller is produced is a profile of tooth.
(3) pyrolysis
With the pyrolysis under protective atmosphere (argon gas, nitrogen or other rare gas element) or vacuum condition of honey-combed precast body, generate the carbonaceous honey-combed, the Z 150PH non-woven fabrics is burnt removal therebetween.Wherein, 1~10 ℃ of temperature rise rate PM is warming up to 800~1200 ℃, is incubated 0.5~2 hour.
(4) liquid phase reaction infiltration
The carbonaceous honey-combed that pyrolysis is obtained reacts the melting infiltration sintering siliconising; Sintering carries out under protective atmosphere (argon gas, nitrogen or other rare gas element) or vacuum condition; Temperature rise rate is 5~15 ℃ of PMs; Melt temperature is: 1400~1900 ℃, be incubated 0.5~5 hour, and get SiC ceramic honey comb material.Can access fine and close or micron porous hole wall structure through the control sintering time, the raw material of selecting for use in the reaction sintering infiltration is a silicon.Like soaking time is that sintering obtains fine and close hole wall structure below 2 hours, removes like soaking time pore-creating raw material such as remaining Si in then can be with hole wall more than 2 hours, forms micrometer level porous hole wall structure.
Experiment shows, in above-mentioned embodiment and parameter area, all can realize the object of the invention.Through embodiment the present invention is detailed below.
Embodiment 1
The mean particle size 5 μ m carborundum powders, ammonia resol, the tosic acid that mass ratio are respectively 60%: 35%: 5% are dissolved in the absolute ethyl alcohol altogether, and ball milling after mechanical stirring filters, slip, said slurry solution solute is 80% of a total mass; Certain ethanol in the air-dry removal slip, making the organic solvent mass content after air-dry is 10%.This raw material evenly is coated on the Z 150PH non-woven fabrics, is layered on then on the one side of splitting mould with triangle fluting that is heated to 120 ℃, matched moulds is forced into spacing place; The spacing gap that guarantees is 0.3mm between the mould, is incubated 1 minute after fixing, and die sinking can obtain having the beading individual layer cellular unit of triangular slot; After mode prepares some blade units according to this; These unit are bonding with the folded buttress of slip, can obtain the ceramic honey comb precast body after solidifying firmly, its perforate be shaped as trilateral; After with the pyrolysis under argon shield of this precast body, generate the carbonaceous ceramic honey comb; Wherein the temperature rise rate PM is 2 ℃, is warming up to 1200 ℃, is incubated 0.5 hour.After the pyrolysis, carry out the siliconising of vacuum reaction melting infiltration sintering, 1650 ℃ of temperature of reaction, temperature rise rate is 10 ℃/minute, is incubated 1 hour, the infiltration raw material is Si, gets fine and close SiC ceramic honey comb material.
The technical indicator of present embodiment gained SiC ceramic honey comb material is following:
Unit surface hole count: 100 holes/cm 2Surface volume ratio: 4800m -1Density: 0.4g/cm 3Porosity: 85%; Compressive strength (being parallel to the hole): 70MPa; Thermal expansivity: 4.7 * 10 -6/ ℃; The strong acid-base resistance corrosion; 1000 ℃ of following shrend experiments can stand 10 circulations and not damage not oxidation.
Embodiment 2
Mass ratio was respectively 50%: 10%: 35%: 5% mean particle size 5 μ m carborundum powders and mean particle size are that 3 μ m silica flours, ammonia resol, tosic acid are dissolved in the absolute ethyl alcohol altogether; Ball milling after mechanical stirring; Filter, get slip, said slurry solution solute is a total mass 75%; Certain ethanol in the air-dry removal slip, making the organic solvent mass content after air-dry is 15%.This raw material evenly is coated in the Z 150PH non-woven fabrics, and the back is pushed in being heated to the wavy profile of tooth pair roller of 150 ℃ have and is passed by, and guarantees between the up-down rollers that the gap is 0.3mm; Roll-in speed is 1m/1min; Obtain having the beading individual layer cellular unit of wavy groove, after mode prepares some blade units according to this, that these unit are bonding with the folded buttress of slip; Can obtain the ceramic honey comb precast body after solidifying firmly; Its perforate be shaped as waveform, after with the pyrolysis under argon shield of this precast body, generate the carbonaceous ceramic honey comb; Wherein the temperature rise rate PM is 2 ℃, is warming up to 900 ℃, is incubated 0.5 hour.After the pyrolysis, carry out the siliconising of vacuum reaction melting infiltration sintering, 1750 ℃ of temperature of reaction; Temperature rise rate is 10 ℃/minute, is incubated 2.5 hours, in this sintering process; The carbon reaction generates SiC in infiltration raw material Si and the carbonaceous ceramic honey comb, and SiC in the raw material is combined, and continues in the back in the vacuum heat-preserving; Remaining Si can be removed in Si that adds in the slip raw material and the reaction, makes hole wall become porous, must have the SiC ceramic honey comb material of porous hole wall.
The technical indicator of present embodiment gained SiC ceramic honey comb material is following:
Unit surface hole count: 75 holes/cm 2Surface volume ratio: 3600m -1Density: 0.5g/cm 3Porosity: 85%; Hole wall is a vesicular structure, and porosity is about 40%; Compressive strength (being parallel to the hole): 86MPa; Thermal expansivity: 4.7 * 10 -6/ ℃; The strong acid-base resistance corrosion; 1000 ℃ of following shrend experiments can stand 10 circulations and not damage not oxidation.
Embodiment 3
Mass ratio was respectively 60%: 20%: 15%: 5% mean particle size 1.5 μ m carborundum powders, ammonia resol, epoxy resin, tosic acid are dissolved in the absolute ethyl alcohol altogether; Ball milling after mechanical stirring; Filter, get slip, said slurry solution solute is 60% of a total mass; Certain ethanol in the air-dry removal slip, making the organic solvent mass content after air-dry is 12%.This raw material evenly is coated on the Z 150PH non-woven fabrics, is layered on then on the one side of splitting mould with triangle fluting that is heated to 180 ℃, matched moulds is forced into spacing place; The spacing gap that guarantees is 0.8mm between the mould, is incubated 1 minute after fixing, and die sinking can obtain having the beading individual layer cellular unit of triangular slot; After mode prepares some blade units according to this; These unit are bonding with the folded buttress of slip, can obtain the ceramic honey comb precast body after solidifying firmly, its perforate be shaped as trilateral; After with the pyrolysis under argon shield of this precast body, generate the carbonaceous ceramic honey comb; Wherein the temperature rise rate PM is 5 ℃, is warming up to 800 ℃, is incubated 2 hours.After the pyrolysis, carry out the siliconising of vacuum reaction melting infiltration sintering, 1850 ℃ of temperature of reaction, temperature rise rate is 15 ℃/minute, is incubated 1.5 hours, the infiltration raw material is Si, gets fine and close SiC ceramic honey comb material.
The technical indicator of present embodiment gained SiC ceramic honey comb material is following:
Unit surface hole count: 50 holes/cm 2Surface volume ratio: 2000m -1Density: 0.8g/cm 3Porosity: 75%; Compressive strength (being parallel to the hole): 85MPa; Thermal expansivity: 4.7 * 10 -6/ ℃; The strong acid-base resistance corrosion; 1000 ℃ of following shrend experiments can stand 10 circulations and not damage not oxidation.

Claims (8)

1. SiC ceramic honey comb material, it is characterized in that: said ceramic honey comb material is SiC, has continuous single honeycombed one-piece construction, and parallel passage is arranged vertically, the shape of passage is trilateral or waveform; The unit surface hole count of forming honey-combed is controlled at 100~5/cm 2Between, pore wall thickness is controlled between 0.2~2mm.
2. by the said SiC ceramic honey comb of claim 1 material, be characterised in that: the hole wall structure of forming honey-combed is a dense structure, perhaps adopts pore-creating technology to become a micron vesicular structure.
3. by the said SiC ceramic honey comb of claim 1 preparation methods; It is characterized in that: is raw material with powder of solid particles with the macromolecular material that has than high carbon output rate; Adopt mold pressing to prepare individual layer cellular unit combination back pyrolysis, sintering, it is following specifically to prepare process:
(1) preparation of raw material
With powder of solid particles, macromolecular material, solidifying agent by mass percentage example be (70wt%~20wt%): (20wt%~70wt%): (1wt%~10wt%) be dissolved in the organic solvent altogether; Ball milling after mechanical stirring; Filter; Get slip, said slurry solution solute is 5~80% of a total mass; After certain amount of organic solvent in the air-dry removal slip, making the organic solvent mass content after air-dry is between 10~15%;
Powder of solid particles is carborundum powder, silica flour or the two mixed powder; Macromolecular material is selected from a kind of of epoxy resin, resol and furfuryl resin or several kinds; Solidifying agent is: tosic acid, urotropine, oxalic acid or Hydrocerol A;
(2) compression molding and assembling
Above-mentioned raw materials evenly is coated on the Z 150PH non-woven fabrics, is layered on back matched moulds on the one side of splitting forming mould of heating then, become the individual layer cellular unit of mold shape; Perhaps; Adopt the gear pair roller of heating; Non-woven fabrics after applying is pushed curing molding between pair roller be the individual layer cellular unit with profile of tooth; Then requisite number purpose individual layer cellular unit is got up with the bonding folded buttress of slip, solidify bonding slip and make it fixedly to become the honey-combed precast body, the preheating temperature of splitting forming mould or gear pair roller is 120-180 ℃;
(3) pyrolysis
With the pyrolysis under the protective atmosphere of argon gas, nitrogen or other rare gas element of honey-combed precast body, perhaps pyrolysis under vacuum condition generates the carbonaceous honey-combed, and the Z 150PH non-woven fabrics is burnt therebetween; Wherein, 1~10 ℃ of temperature rise rate PM is warming up to 800~1200 ℃, is incubated 0.5~2 hour;
(4) liquid phase reaction infiltration
The carbonaceous honey-combed that pyrolysis is obtained reacts melting infiltration sintering; The raw material of selecting for use in the reaction sintering infiltration is a silicon, and the sintering siliconising is perhaps carried out in sintering siliconising under the protective atmosphere of argon gas, nitrogen or other rare gas element under vacuum condition; Temperature rise rate is 5~15 ℃ of PMs; Melt temperature is: 1400~1900 ℃, be incubated 0.5~5 hour, and get SiC ceramic honey comb material.
4. according to the said SiC ceramic honey comb of claim 3 preparation methods, it is characterized in that: said organic solvent is ethanol or formaldehyde, and solvent quality concentration is between 50-90%.
5. according to the said SiC ceramic honey comb of claim 3 preparation methods, it is characterized in that: said silica flour and carborundum powder purity are more than 95%, and mean particle size is 10nm~25 μ m.
6. according to the said SiC ceramic honey comb of claim 3 preparation methods, it is characterized in that: curing agent content is 1~10% of a high molecular material resin quality; Under 100~250 ℃ of temperature, solidify 1~10 minute time.
7. according to the said SiC ceramic honey comb of claim 3 preparation methods, it is characterized in that: the compression molding mould is split cavity or gear mesh roller die tool, and mould molding is shaped as the individual layer of required honey-combed, and the single layer structure of compression moulding is trilateral or waveform; Wall thickness is controlled between 0.2~2mm, and the unit surface hole count that is assembled into honey-combed can be controlled in 100~5/cm 2Between.
8. according to the said SiC ceramic honey comb of claim 3 preparation methods, it is characterized in that: adopt carborundum powder or carborundum powder and silica flour mixed powder, when wherein adopting mixed powder, the two mass ratio is (20~90%): (80~10%).
CN 201210109728 2012-04-16 2012-04-16 SiC honeycomb ceramics material and preparation method thereof Expired - Fee Related CN102643095B (en)

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CN109476560A (en) * 2016-07-29 2019-03-15 日本碍子株式会社 Porous ceramic particle and porous ceramic structure
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