CN1325832A - High-strength foam silicon carbide ceramics and its preparing process - Google Patents
High-strength foam silicon carbide ceramics and its preparing process Download PDFInfo
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Abstract
A high-strength silicon carbide foam ceramic with relative density higher than 90% and 10 nm-10 microns of average grain size is prepared from the high-molecular material with high carbon residual rate after pyrolysis as raw materials and foam polyurethane plastic as skeleton through pulping, solidifying, pyrolyzing and siliconizing. Its advantages include high density and strength, easily controlled porosity and size, and low cost.
Description
The present invention relates to thyrite, a kind of technology of preparing with foam silicon carbide ceramics of higher mechanical strength is provided especially.
High-temperature filter is the main application of foam silicon carbide ceramics, and its history is with decades-long.In recent years, progressively obtain paying attention in the application aspect matrix material and the electric heating.Yet because the problem that the preparation method exists makes that the physical strength of foam silicon carbide ceramics is not high, these new application only are in the exploratory stage.
Up to now, the foam silicon carbon pottery is produced by following four kinds of methods, that is: powder sintering, solid state reaction sintering process, contain silicone resin pyrolysis method and vapour deposition process.
Powder sintering can be divided into two kinds of different processes again.One, be at first to contain the carborundum powder of a certain amount of sintering aid and the slurry of linking agent (as the ethyl silicate hydrolyzed solution) furnishing suitable concn, soak then and hang on the polyamine fat vacuole foam, solidify drying after, deviate from linking agent and polyamine fat resin 200--500 ℃ of scope.Then, temperature being raised to 1500--2200 ℃ carries out sintering and just obtains the spumescence silicon carbide ceramics; Another kind method is with after containing the carborundum powder and strain shape whipping agent uniform mixing of sintering aid, with mold pressing or pouring type moulding.Deviate from whipping agent by fusing or vaporization, then carry out high temperature sintering to obtain the spumescence silicon carbide ceramics.
The solid state reaction sintering process is with strain shape whipping agent and silica flour and carbon dust uniform mixing aftershaping.Deviate from whipping agent by fusing or vaporization, behind the pyroreaction sintering, promptly obtain the spumescence silicon carbide ceramics.
Contain the silicone resin pyrolysis method and be and earlier the organosilicon presoma is made high-molecular gel, obtain the foamed silicone resin that contains after deviating from the organic solvent in the gel, after abundant preoxidation, carry out pyrolysis and promptly get the spumescence silicon carbide ceramics.
Vapour deposition process is silicon carbide is deposited on the netlike carbon fiber knitted body and to obtain the spumescence silicon carbide ceramics with chemical gaseous phase depositing process.
Above method, or exist foams intensity low, or exist volume of voids and size to be difficult to control or to face cost of manufacture cross problems such as height.These problems make the application of foam silicon carbon pottery, and particularly new application is subjected to restriction in various degree.
The object of the present invention is to provide a kind of high-strength foam silicon carbide ceramics and preparation method thereof, with silicon carbide ceramics density foam height, the intensity height of this method preparation, volume of voids and size are easy to control, and cost of manufacture is lower.
The invention provides a kind of high-strength foam silicon carbide ceramics, it is characterized in that: the relative density of this foam silicon carbide ceramics muscle is greater than 90%, and average grain size is at 10nm~10 μ m.
The present invention also provides the preparation method of above-mentioned high-strength foam silicon carbide ceramics, it is characterized in that can keep the macromolecular material of high carbon residue rate after the pyrolysis be raw material, is skeleton with the polyurethane foamed plastic, and preparation process is as follows:
(1) macromolecular material is made slurry, the porous plastics skeleton that will be cut into desired shape and size again immerses in the slurry, after the taking-up, goes out redundant sizing agent with modes such as extruding, air-blowings;
(2) hope material in thermal environment or acidic medium, fully solidify the foam behind the above-mentioned soaking paste material;
(3) the porous plastics pyrolysis after will solidifying, pyrolysis is carried out under nitrogen, argon gas or other protection of inert gas, and temperature rise rate 1-10 ℃/min, pyrolysis temperature 800-1400 ℃, soaking time 10min~300min;
(4) the spumescence presoma after the pyrolysis is carried out siliconising and handle, siliconising is carried out under protective atmosphere or vacuum, and temperature 1400-1900 ℃, soaking time 10min-300min.
Macromolecular material described in the inventive method can be selected from one or more of Resins, epoxy, resol, furfuryl resin.Can also sneak into the carborundum powder of mean particle size 10nm-10 μ m and make raw material in described macromolecular material, add-on is the 5-90% volume, is good with the 40-60% volume.
Curing described in the inventive method can be selected from oxidisability mineral acids such as sulfuric acid, nitric acid, perchloric acid with acidic medium, and is comparatively suitable with sulfuric acid, sulphuric acid soln concentration 10-80%, preferably 30-50%.Can also add solidifying agent five Lip rivers and take off product in material resin, content is the 1-50% of weight resin, is good with 5-10%, thermofixation under 150-250 ℃ of temperature, time 1-3 hour.
In the pyrolytic process of the inventive method, pyrolysis temperature is preferably in 1000-1200 ℃, temperature rise rate 2-4 ℃/min.
The inventive method is to make the suitable slurry of concentration behind carborundum powder and the macromolecular solution uniform mixing particularly.Select the polyurethane foamed plastic in suitable aperture, and be cut into desired shape and size, then it is immersed in the slurry.After the taking-up, go out redundant sizing agent, to keep the connectedness of hole with modes such as extruding, air-blowings.In thermal environment or acidic medium, fully solidify.Placing vacuum or special atmosphere oven to carry out polyamine fat the foams after solidifying deviates from and the resin pyrolysis, obtains the composite foam shape presoma with original equiform silicon carbide of foam polyamine fat and RESEARCH OF PYROCARBON.RESEARCH OF PYROCARBON in the presoma and liquid-state silicon or gaseous state pasc reaction form silicon carbide, simultaneously original silicon carbide powder closely are connected to form the compact silicon carbide muscle of high bond strength.What process obtained thus is high strength foam silicon carbon pottery.The present invention has following characteristics.
1, high strength.The reaction of siliconising in the pyrolysis carbon skeleton that the present invention adopts forms the foam silicon carbide ceramics method, and the muscle of foamed ceramics is had near 100% relative density and the even fine and closely woven microstructure (seeing accompanying drawing 1,2,3) of 0.5-2 μ m.This is that other method institute is inaccessiable except that the gas phase deposition method, but cost is far below gas-phase deposition, and the thickness of muscle is more easy to control simultaneously.Thereby this method can obtain high foam silicon carbon intensity with low preparation cost.
2, do not need mould can realize nearly end form moulding, reduce the preparation tooling cost.These characteristics are mainly by following two aspect reason decisions: the first, and as the primary template of foamed ceramics, polyurethane foamed plastic very easily is processed into arbitrary shape; The second, forming silicon carbide reaction-sintered by the reaction of siliconising in carbon skeleton almost is the process of a no deformation rate.
3, foamed ceramics pass, aperture, porosity are easily controlled.Polyamine fat vacuole foam resin is as the primary template that obtains final foamed ceramics, at first utilize the pyrolytic reaction of high carbon output rate resin to make the foamy carbon skeleton that contains certain proportion silicon carbide, then obtain the geometry high strength spumescence silicon carbide ceramics similar by carrying out liquid state or gaseous state siliconising reactivity thereon to original foamed resin.
4, silicon, carbon react completely, and both unit " dead skin is hollow " did not have remaining silicon again." dead skin is hollow " is meant that sample surfaces forms silicon carbide, and the inside is still unreacted carbon, and this is that the conventional carbon precast body prepares the serious problems that the silicon carbide ceramics method exists by siliconising.Present method adopts the way of adding an amount of silicon carbide powder in material resin, prevents effectively that not only the resin pyrolysis from forming fine and close carbon-coating and stoping the interior infiltration of silicon thermotropism disintegration to form " dead skin is hollow ", also restricts the formation of remaining silicon simultaneously.
The present invention proposes a kind of new, cheap, high strength foam silicon carbon ceramic preparation in a word.In the method, polymer pyrolysis and reaction sintering are organically combined, and make the foam silicon carbon of preparing have void density and characteristics such as pore dimension is easily controlled, ceramic muscle density height (can reach 100%), muscle condition of surface can arbitrarily design, foams intensity height.These characteristics will make the foam silicon carbon pottery obtain more widely application.Below by embodiment in detail the present invention is described in detail.
Accompanying drawing 1 is the section microstructure (scale is 200 μ m) of foam silicon carbon pottery muscle
Accompanying drawing 2 is the microstructure (scale is 10 μ m) of foam silicon carbon pottery muscle inside
Accompanying drawing 3 is the microstructure (scale is 50 μ m) on foam silicon carbon pottery muscle surface
Embodiment 1
Universal heat-reactive phenolic resin (phenol formaldehyde resin) being dissolved in the dehydrated alcohol, making slurry solution, is that the polyurethane foamed plastic of 2mm immerses in the above-mentioned slip with the aperture, soaks after 1 minute and takes out, and extrudes unnecessary slip.Then immerse concentration and be in 40% the aqueous sulfuric acid and solidify the washing after drying.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 2 ℃/min of temperature rise rate, 1100 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1500 ℃ of temperature of reaction, soaking time 1 hour promptly gets the foam silicon carbon pottery, muscle density 95%, 1.1 microns of silicon carbide average crystal grain granularities.
Embodiment 2
Resins, epoxy and the mean particle size that with the trade mark is EP0141-310 is that 2 microns carborundum powder is uniformly mixed to form resin/silicon carbide volume than the slip that is 1/9.With the aperture is that the polyurethane foamed plastic of 2mm immerses in the above-mentioned slip, soaks after 1 minute and takes out, and extrudes unnecessary slip.Then, wash after drying 60 ℃ of curing.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 2 ℃/min of temperature rise rate, 1100 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1500 ℃ of temperature of reaction, soaking time 1 hour promptly gets the foam silicon carbon pottery, muscle density 93%, 1.8 microns of silicon carbide average crystal grain granularities.
Embodiment 3
With weight ratio respectively is that 50% heat-reactive phenolic resin and furfuryl resin are dissolved in the dehydrated alcohol altogether, makes slurry solution, is that 2 microns carborundum powder evenly adds in the above-mentioned solution again with mean particle size, forms resin/silicon carbide volume than the slip that is 1/9.With the aperture is that the polyurethane foamed plastic of 2mm immerses in the above-mentioned slip, soaks after 1 minute and takes out, and extrudes unnecessary slip.Then immerse concentration and be in 40% the aqueous sulfuric acid and solidify the washing after drying.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 2 ℃/min of temperature rise rate, 1100 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1500 ℃ of temperature of reaction, soaking time 1 hour promptly gets the foam silicon carbon pottery, muscle density 98%, 1.8 microns of silicon carbide average crystal grain granularities.
Embodiment 4
With weight ratio respectively is that 50% heat-reactive phenolic resin and furfural are dissolved in the dehydrated alcohol altogether, makes slurry solution, is that 2 microns carborundum powder evenly adds in the above-mentioned solution again with mean particle size, forms resin/silicon carbide volume than the slip that is 4/6.With the aperture is that the polyurethane foamed plastic of 2mm immerses in the above-mentioned slip, soaks after 1 minute and takes out, and extrudes unnecessary slip.Then immerse concentration and be in 40% the aqueous sulfuric acid and solidify the washing after drying.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 3 ℃/min of temperature rise rate, 1100 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1550 ℃ of temperature of reaction, soaking time 1 hour promptly gets the foam silicon carbon pottery, muscle density 99%, 1.8 microns of silicon carbide average crystal grain granularities.
Embodiment 5
With weight ratio respectively is that 50% heat-reactive phenolic resin and furfuryl resin are dissolved in the dehydrated alcohol altogether, makes slurry solution, is that 2 microns carborundum powder evenly adds in the above-mentioned solution again with mean particle size, forms resin/silicon carbide volume than the slip that is 5/5.With the aperture is that the polyurethane foamed plastic of 2mm immerses in the above-mentioned slip, soaks after 1 minute and takes out, and extrudes unnecessary slip.Then immerse concentration and be in 40% the aqueous sulfuric acid and solidify the washing after drying.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 3 ℃/min of temperature rise rate, 1050 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1600 ℃ of temperature of reaction, soaking time 1 hour promptly gets the foam silicon carbon pottery, and the muscle density is greater than 99%, 1.8 microns of silicon carbide average crystal grain granularities.
Embodiment 6
With weight ratio respectively is that 50% heat-reactive phenolic resin and furfuryl resin are dissolved in the dehydrated alcohol altogether, makes slurry solution, is that 1.5 microns carborundum powder evenly adds in the above-mentioned solution again with mean particle size, forms resin/silicon carbide volume than the slip that is 6/4.With the aperture is that the polyurethane foamed plastic of 1mm immerses in the above-mentioned slip, soaks after 1 minute and takes out, and extrudes unnecessary slip.Then immerse concentration and be in 50% the aqueous sulfuric acid and solidify the washing after drying.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 2 ℃/min of temperature rise rate, 1100 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1650 ℃ of temperature of reaction, soaking time 2 hours promptly gets the foam silicon carbon pottery, and the muscle density is greater than 99%, 1.3 microns of silicon carbide average crystal grain granularities.
Embodiment 7
Five Lip rivers that weight ratio is respectively 30% and 65% heat-reactive phenolic resin and furfuryl resin and 5% are taken off product and are dissolved in the dehydrated alcohol altogether, make slurry solution, the carborundum powder that with mean particle size is 2 microns more evenly adds in the above-mentioned solution, forms resin/silicon carbide volume than the slip that is 3/7.With the aperture is that the polyurethane foamed plastic of 2mm immerses in the above-mentioned slip, soaks after 1 minute and takes out, and extrudes unnecessary slip and dry.In baking oven, dried 1-3 hour down for 150-220 ℃.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 2 ℃/min of temperature rise rate, 1100 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1500 ℃ of temperature of reaction, soaking time 1 hour promptly gets the foam silicon carbon pottery, muscle density 96%, 1.7 microns of silicon carbide average crystal grain granularities.
Embodiment 8
Five Lip rivers that weight ratio is respectively 30% and 65% heat-reactive phenolic resin and furfuryl resin and 5% are taken off product and are dissolved in the dehydrated alcohol altogether, make slurry solution, the carborundum powder that with mean particle size is 10 microns more evenly adds in the above-mentioned solution, forms resin/silicon carbide volume than the slip that is 6/4.With the aperture is that the polyurethane foamed plastic of 2mm immerses in the above-mentioned slip, soaks after 1 minute and takes out, and extrudes unnecessary slip and dry.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 3 ℃/min of temperature rise rate, 1200 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1600 ℃ of temperature of reaction, soaking time 2 hours promptly gets the foam silicon carbon pottery, muscle density 98%, 6.8 microns of silicon carbide average crystal grain granularities.
Embodiment 9
Five Lip rivers that weight ratio is respectively 30% and 65% heat-reactive phenolic resin and furfuryl resin and 5% are taken off product and are dissolved in the dehydrated alcohol altogether, make slurry solution, the carborundum powder that with mean particle size is 5 microns more evenly adds in the above-mentioned solution, and forming resin/silicon carbide weight ratio is 6/4 slip.With the aperture is that the polyurethane foamed plastic of 2mm immerses in the above-mentioned slip, soaks after 1 minute and takes out, and extrudes unnecessary slip and dry.Pyrolysis in protective atmospheres such as argon gas or nitrogen, average 3 ℃/min of temperature rise rate, 1200 ℃ of final pyrolysis temperatures.After the pyrolysis, carry out the vacuum siliconising, 1600 ℃ of temperature of reaction, soaking time 2 hours promptly gets the foam silicon carbon pottery, muscle density 98%, 3.8 microns of silicon carbide average crystal grain granularities.
Claims (11)
1, a kind of high-strength foam silicon carbide ceramics is characterized in that: the relative density of this foam silicon carbide ceramics muscle is greater than 90%, and average grain size is at 10nm~10 μ m.
2, the preparation method of the described high-strength foam silicon carbide ceramics of a kind of claim 1 is characterized in that can keep the macromolecular material of high carbon residue rate after the pyrolysis be raw material, is skeleton with the polyurethane foamed plastic, and preparation process is as follows:
(1) macromolecular material is made slurry, the porous plastics skeleton that will be cut into desired shape and size again immerses in the slurry, after the taking-up, goes out redundant sizing agent with modes such as extruding, air-blowings;
(2) hope material in thermal environment or acidic medium, fully solidify the foam behind the above-mentioned soaking paste material;
(3) the porous plastics pyrolysis after will solidifying, pyrolysis is carried out under nitrogen, argon gas or other protection of inert gas, and temperature rise rate 1-10 ℃/min, pyrolysis temperature 800-1400 ℃, soaking time 10min~300min;
(4) the spumescence presoma after the pyrolysis is carried out siliconising and handle, siliconising is carried out under protective atmosphere or vacuum, and temperature 1400-1900 ℃, soaking time 10min-300min.
3, by the preparation method of the described high-strength foam silicon carbide ceramics of claim 2, it is characterized in that: described macromolecular material is selected from one or more of Resins, epoxy, resol, furfuryl resin.
4, by the preparation method of claim 2 or 3 described high-strength foam silicon carbide ceramics, it is characterized in that: the carborundum powder of sneaking into mean particle size 10nm-10 μ m in described macromolecular material is made raw material, and add-on is the 5-90% volume.
5, by the preparation method of the described high-strength foam silicon carbide ceramics of claim 4, it is characterized in that: the carborundum powder add-on is the 40-60% volume.
6, by the preparation method of the described high-strength foam silicon carbide ceramics of claim 4, it is characterized in that: described curing is selected from oxidisability mineral acids such as sulfuric acid, nitric acid, perchloric acid with acidic medium.
7, by the preparation method of the described high-strength foam silicon carbide ceramics of claim 6, it is characterized in that: described acidic medium is a sulfuric acid, sulphuric acid soln concentration 10-80%.
8, by the preparation method of the described high-strength foam silicon carbide ceramics of claim 7, it is characterized in that: sulphuric acid soln concentration 30-50%.
9, by the preparation method of the described high-strength foam silicon carbide ceramics of claim 4, it is characterized in that: add solidifying agent five Lip rivers and take off product in material resin, content is the 1-50% of weight resin, thermofixation under 150-250 ℃ of temperature, time 1-3 hour.
10, by the preparation method of the described high-strength foam silicon carbide ceramics of claim 9, it is characterized in that: product content 5-10% is taken off in five Lip rivers.
11, by the preparation method of the described high-strength foam silicon carbide ceramics of claim 4, it is characterized in that: in the pyrolytic process, pyrolysis temperature 1000-1200 ℃, temperature rise rate 2-4 ℃/min.
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