CN101560104A - Preparation method for silicon carbide ceramic tube or rod - Google Patents
Preparation method for silicon carbide ceramic tube or rod Download PDFInfo
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Abstract
The invention relates to a preparation method for a silicon carbide ceramic tube or rod. An extrusion moulding method is adopted to form a blank body; a normal pressure sintering method is adopted for sintering; and submicron level silicon carbide powder and additives are taken as main raw materials. The preparation method comprises the following steps: 1) carrying out ball milling on the main raw materials by a dry method, adding water, a dispersant, a plasticizer, a lubricant and a liquid state binder, and then carrying out ball milling by a wet method; 2) adopting a spray granulation process to granulate silicon carbide slurry; 3) extruding the blank body by a one-shot direct extrusion moulding method after vacuum pug, corrosion, and vacuum pug; 4) drying the molded blank body by a stage drying mechanism; and 5) placing the blank body of the silicon carbide ceramic tube or rod in a vacuum furnace and carrying out sintering for two times by taking argon gas as protective gas. The high temperature resisting strength and the corrosion resistance of the silicon carbide ceramic tube or rod prepared by the method are both better than those of a reactive sintered product. Compared with a hot press sintering method, the method has lower limit on the product shape and size, and lower cost. The method is suitable for the industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method, the preparation method of particularly a kind of silicon carbide ceramic or rod.
Background technology
Silicon carbide ceramics has many good characteristics as a kind of high-temperature structural ceramics, as mechanics wear-resisting, that thermal conductivity is high, heat-resisting, corrosion-resistant and good and thermal property etc.Silicon carbide ceramics has been widely used in industrial circle and national defense industry such as machinery, electronics, petrochemical complex, metallurgy, and has been confirmed as the 4th kind of basic material since metal, aluminum oxide, Wimet in the world.
Silicon carbide ceramic or rod because its constructional feature, adopt generally that chemical gas phase is synthetic, the method for isostatic pressing, injection forming, injection molding and extrusion molding comes molding blank, but still there is following problem in aforesaid method:
1) chemical gas phase synthetic method is by depositing silicon carbide layer on the clavate graphite, high temperature oxidation is removed graphite and is obtained carborudum tube or rod then, as the patent No. is that 90109657.1 " tubular silicon carbide structures and preparation method thereof " discloses a kind of making method that adopts the tubular silicon carbide structures of chemical gas phase synthetic method, but this method is difficult to make heavy-walled carborudum tube and production cost height, is difficult to realize large-scale production.
2) though isostatic pressing can mold fine and close base substrate, a kind of silicon carbide roller rod manufacturing method of isostatic pressing is disclosed as the patent No. 99120189.2 " silicon carbide roller used for roller kiln and manufacture method thereof ", but its cost is higher, and can not realize serialization production, and productive rate is lower.
3) prerequisite of injection forming is the stable suspension liquid that will obtain high solid loading, and often adds multiple additives in the silicon carbide ceramics batching, therefore is difficult to realize even, stable high solid loading suspension liquid.
4) there is long, the restive shortcoming of degreasing time in injection molding.
5) extrusion molding is the method for a kind of low cost, continuous production vitrified pipe or rod, but is difficult to mold fine and close base substrate.The general employing requires base substrate loose reaction sintering or hot pressed sintering to carry out sintering.And the reaction sintering product is owing to exist more free silica, and its intensity, solidity to corrosion and high-temperature stability are relatively poor.Then cost is higher for the mode of employing hot pressed sintering, and the shape of product is very limited.
Summary of the invention
The technical problem to be solved in the present invention provides the preparation method of a kind of silicon carbide ceramic or rod, adopt extrusion process to come the moulding dense green, adopt normal pressure-sintered mode to carry out sintering, the silicon carbide ceramic or the rod of this method preparation have characteristics such as wear-resistant, high temperature resistant, corrosion-resistant, that fracture toughness property is good, and suitable suitability for industrialized production.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the preparation method that a kind of silicon carbide ceramic or rod are provided, with the silicon carbide in submicro level powder of weight percent 60%-98.5%, the additive composition main raw material of 1.5%-40%, be 100% with main raw material weight; Described additive comprises solid state sintering auxiliary agent, liquid phase sintering auxiliary agent or compound additive; Described solid state sintering auxiliary agent is norbide and carbon, and described liquid phase sintering auxiliary agent is aluminum oxide, yttrium oxide, and described compound additive is norbide, aluminum oxide, yttrium oxide, lanthanum trioxide, may further comprise the steps successively:
1), with main raw material dry ball milling 1 hour;
2), the back of will dry grinding is incorporated as acrylic resin wet ball grinding 4-9 hour again of oleic acid, the 1%-3% of polyoxyethylene glycol, the 0.5%-1.5% of Tetramethylammonium hydroxide, the 0.2%-1.5% of water, the 0.5%-1.5% of main raw material weight 100%-150% in the main raw material successively, is configured to the silicon carbide slurry that solid content is 40%-55%;
3), the silicon carbide slurry after adopting drying process with atomizing to wet-milling carries out granulation, obtains silicon carbide granulating powder; Described spraying drying adopts spray-drier to carry out, and processing parameter is: inlet temperature is 220-250 ℃, and temperature out is 75-120 ℃, and atomizing pressure is 0.8-1.5MPa;
4), be 100% with the weight of granulation powder, be added to the water of granulation powder weight 13%-17% in the granulation powder after spraying drying, in vacuum deairing machine, carry out vacuum pugging;
5), the pug behind the vacuum pugging is sealed old 12-48 hour with plastic box;
6), old back pug once more behind the vacuum pugging, is squeezed out silicon carbide ceramic or excellent base substrate with the extrusion under vacuum machine;
7), base substrate is placed in 60-100 ℃ the baking oven dry 6-12 hour, it is dry again 2-5 hour to 120-150 ℃ to improve temperature then;
8), base substrate after the drying is carried out preliminary working, obtain silicon carbide ceramic or rod;
9), base substrate after the preliminary working is placed in the vacuum oven, does shielding gas with argon gas and carry out pre-burning, be warming up to 600-1000 ℃ of insulation 1-3 hour, take out behind the furnace cooling, obtain blank;
10), blank is placed in the vacuum oven, does shielding gas with argon gas and carry out normal pressure-sinteredly, be warming up to 1850-2200 ℃ of insulation 1-3 hour, take out behind the furnace cooling, obtain constant pressure sintering silicon carbide pipe or rod;
11) carborudum tube behind the sintering or rod are carried out precision work, obtain finished product.
According to the product requirement difference, can select different sintering processings: normal pressure solid state sintering, normal pressure liquid phase sintering.Its additive also has different choice, and described additive comprises solid state sintering auxiliary agent, liquid phase sintering auxiliary agent or compound additive; Solid state sintering auxiliary agent commonly used is norbide and carbon; Liquid phase sintering auxiliary agent commonly used is two or more the mixture in aluminum oxide, yttrium oxide, aluminium, yttrium aluminum garnet, rare earth oxide, the magnesium oxide; Compound additive commonly used is at least a in norbide, yttrium oxide, aluminum oxide, aluminium nitride, rare earth oxide, various whisker and the fiber.
Described dispersion agent also can be ammonium polyacrylate; Described softening agent also can be a kind of in sucrose fat, the paraffin common plasticizers; Described lubricant also can be stearic acid; Described liquid adhesive also can be a kind of in polyvinyl alcohol, arab resin, the ether of cellulose binding agent commonly used.
Compared with prior art, the invention has the advantages that:
(1), the present invention's material before pugging has mixed through dry ball milling-wet ball grinding-technologies such as spraying drying, again through two sections puggings, make old back pug moisture content homogeneous, particles dispersed is even, base substrate densification after the moulding, intensity height, drying is not broken, and the yield rate height is better than generally directly pugging-old pug and base substrate without ball milling-spraying drying.
(2), the present invention adopts once the directly method of extrusion molding, can large batch ofly mold the carborudum tube or the excellent dense green of various size, and cost is lower, is better than methods such as injection molding, injection forming, compression moulding and extruding back compression moulding earlier.
(3), the present invention adopts normal pressure-sintered mode, product high temperature strength, erosion resistance are better than the reaction sintering product; And compare with the hot pressed sintering mode, the geomery of product is limited less and cost is lower, is more suitable for suitability for industrialized production.
(4), according to the excellent product performance that the present invention makes, its bending strength is that 450-620MPa, fracture toughness property are 5.4-7.2MPam
1/2, hardness is 2800-3400HK0.1.
Description of drawings
Below in conjunction with accompanying drawing embodiments of the invention are further described.
Accompanying drawing is a production scheme of the present invention;
Embodiment
Embodiment 1
1), with median size be 0.5 micron, weight percent is 98.5% carborundum powder, 1% Graphite Powder 99,0.5% boron carbide powder dry ball milling 1 hour;
2), the back of will dry grinding water, 0.2% Tetramethylammonium hydroxide, 1% polyoxyethylene glycol, 0.5% oleic acid, 2% the polyvinyl alcohol wet ball grinding 8 hours again that is incorporated as main raw material weight 100% in the powder successively, be configured to solid content and be 50% silicon carbide slurry;
3), the silicon carbide slurry after adopting drying process with atomizing to wet-milling carries out granulation, obtains silicon carbide granulating powder; Described spraying drying adopts spray-drier to carry out, and processing parameter is: inlet temperature is that 230 ℃, temperature out are that 105 ℃, atomizing pressure are 1.2MPa;
4), be 100% with the weight of granulation powder, the water that is added to granulation powder weight 13% in the granulation powder after spraying drying carries out vacuum pugging in vacuum deairing machine;
5), the pug behind the vacuum pugging is sealed old 18 hours with plastic box;
6), old back pug once more behind the vacuum pugging, is gone out the silicon carbide ceramic base substrate with the extrusion molding of extrusion under vacuum machine;
7), the silicon carbide ceramic base substrate is placed in 65 ℃ the baking oven dry 12 hours, improve temperature to 125 then ℃ dry 3 hours again;
8) base substrate after the drying is carried out preliminary working, obtain silicon carbide ceramic;
9) base substrate after the preliminary working is placed in the vacuum oven, does shielding gas with argon gas and carry out pre-burning, be warming up to 900 ℃ of insulations 2 hours, take out behind the furnace cooling, obtain blank;
10) blank is placed in the vacuum oven, does shielding gas with argon gas and carry out the normal pressure-sintered 2150 ℃ of insulations 1.5 hours that are warming up to, take out behind the furnace cooling, obtain normal pressure solid-phase sintered silicon carbide pipe;
11) carborudum tube behind the sintering is carried out precision work, obtain finished product.
The density of this silicon carbide ceramic is 3.14g/cm
3, bending strength 490MPa, fracture toughness property 5.6MPam
1/2, hardness 3218HK0.1.
Embodiment 2
1) with median size be 0.6 micron, weight percent is 94% carborundum powder, 2% yttrium oxide, 1.5% aluminum oxide, weight percent are 2.5% magnesium oxide dry ball milling 2 hours;
2), the back of will dry grinding water, 0.2% Tetramethylammonium hydroxide, 1% polyoxyethylene glycol, 0.5% oleic acid, 2% the polyvinyl alcohol wet ball grinding 8 hours again that is incorporated as main raw material weight 100% in the powder successively, be configured to solid content and be 50% silicon carbide slurry;
3), adopt drying process with atomizing to the silicon carbide slurry after the wet-milling is carried out granulation, obtain silicon carbide granulating powder; Described spraying drying adopts spray-drier to carry out, and processing parameter is: inlet temperature is that 230 ℃, temperature out are that 105 ℃, atomizing pressure are 1.2MPa;
4), be 100% with the weight of granulation powder, the water that is added to granulation powder weight 15% in the granulation powder after spraying drying carries out vacuum pugging in vacuum deairing machine;
5), the pug behind the vacuum pugging is sealed old 36 hours with plastic box;
6), old back pug is squeezed out the Globar base substrate behind the vacuum pugging once more;
7), the Globar base substrate is placed in 85 ℃ the baking oven dry 6 hours, improve temperature to 145 then ℃ dry 4 hours again;
8), base substrate after the drying is carried out preliminary working, obtain the silicon carbide ceramics rod;
9), base substrate after the preliminary working is placed in the vacuum oven, does shielding gas with argon gas and carry out pre-burning, be warming up to 750 ℃ of insulations 2 hours, take out behind the furnace cooling, obtain blank;
10), blank is placed in the vacuum oven, does shielding gas with argon gas and carry out normal pressure-sinteredly, be warming up to 1900 ℃ of insulations 1.5 hours, take out behind the furnace cooling, obtain normal pressure liquid phase sintering silicon carbide rod;
11), the Globar behind the sintering is carried out precision work, obtain finished product.
The density of this silicon carbide ceramics rod is 3.16g/cm
3, bending strength 602MPa, fracture toughness property 6.9MPam
1/2, hardness 2900HK0.1.
Embodiment 3
1), with median size be 0.5 micron, weight percent is 70% carborundum powder, median size is a boron carbide powder 1 micron, 22%, 4% aluminum oxide powder, 3% yttrium oxide powder, 1% lanthanum trioxide dried bean noodles method ball milling 1 hour;
2), water, 0.2% ammonium polyacrylate, 1% sucrose fat, 0.5% stearic acid, 2% the water soluble acrylic resin wet ball grinding 8 hours again that in ball mill, is incorporated as main raw material weight 100% successively of the powder after will dry grinding, be configured to solid content and be 50% silicon carbide slurry;
3), the silicon carbide slurry after adopting drying process with atomizing to wet-milling carries out granulation, obtains silicon carbide granulating powder; Described spraying drying adopts spray-drier to carry out, and processing parameter is: inlet temperature is 220 ℃, and temperature out is 105 ℃, and atomizing pressure is 1.2MPa;
4), be 100% with the weight of granulation powder, the water that is added to granulation powder weight 14% in the granulation powder after spraying drying carries out vacuum pugging in vacuum deairing machine;
5), the pug behind the vacuum pugging is sealed old 24 hours with plastic box;
6), with old back pug once more behind the vacuum pugging extrusion molding go out the silicon carbide ceramic base substrate;
7), the silicon carbide ceramic base substrate is placed in 65 ℃ the baking oven dry 12 hours, improve temperature to 125 then ℃ dry 3 hours again;
8) base substrate after the drying is carried out preliminary working, obtain carborudum tube;
9) base substrate after the preliminary working is placed in the true stove, does shielding gas with argon gas and carry out pre-burning, be warming up to 800 ℃ of insulations 2 hours, take out behind the furnace cooling, obtain blank;
10) blank is placed in the vacuum oven, with argon gas do shielding gas carry out normal pressure-sintered, be warming up to 1900 ℃ the insulation 2 hours, take out behind the furnace cooling, obtain normal pressure liquid phase sintering compound carbonizing silicone tube;
11) carborudum tube behind the sintering is carried out precision work, obtain finished product.
The density of this silicon carbide ceramic is 2.92g/cm
3, bending strength 550MPa, fracture toughness property 6.2MPam
1/2, hardness 3300HK0.1.
Claims (3)
1, the preparation method of a kind of silicon carbide ceramic or rod, adopt the method for extrusion molding to come molding blank, adopt normal pressure-sintered method to carry out sintering, it is characterized in that the silicon carbide in submicro level powder with weight percent 60%-98.5%, the additive composition main raw material of 1.5%-40%, is 100% with main raw material weight; Described additive comprises solid state sintering auxiliary agent, liquid phase sintering auxiliary agent or compound additive, and described solid state sintering auxiliary agent is norbide and carbon; Described liquid phase sintering auxiliary agent is aluminum oxide, yttrium oxide, and described compound additive is norbide, aluminum oxide, yttrium oxide, lanthanum trioxide, may further comprise the steps:
1), with main raw material dry ball milling 1 hour;
2), be incorporated as liquid adhesive wet ball grinding 4-9 hour again of lubricant, the 1%-3% of softening agent, the 0.5%-1.5% of dispersion agent, the 0.2%-1.5% of water, the 0.5%-1.5% of main raw material weight 100%-150% in the main raw material after will dry grinding successively, be configured to the silicon carbide slurry that solid content is 40%-55%; Described dispersion agent is a Tetramethylammonium hydroxide, and described softening agent is a polyoxyethylene glycol, and described lubricant is an oleic acid, and described liquid adhesive is an acrylic resin;
3), the silicon carbide slurry after adopting drying process with atomizing to wet-milling carries out granulation, obtain silicon carbide granulating powder, described spraying drying adopts spray-drier to carry out, and processing parameter is: inlet temperature is 220-250 ℃, temperature out is 75-120 ℃, and atomizing pressure is 0.8-1.5MPa;
4), be 100% with the weight of granulation powder, the water that is added to granulation powder weight 13%-17% in the granulation powder after spraying drying carries out vacuum pugging in vacuum deairing machine;
5), the pug behind the vacuum pugging is sealed old 12-48 hour with plastic box;
6), old back pug once more behind the vacuum pugging, is squeezed out carborudum tube or excellent base substrate with the extrusion under vacuum machine;
7), base substrate is placed in 60-100 ℃ the baking oven dry 6-12 hour, it is dry again 2-5 hour to 120-150 ℃ to improve temperature then;
8), base substrate after the drying is carried out preliminary working, obtain carborudum tube or rod;
9), base substrate after the preliminary working is placed in the vacuum oven, does shielding gas with argon gas and carry out pre-burning, be warming up to 600-1000 ℃ of insulation 1-3 hour, take out behind the furnace cooling, obtain blank;
10), with blank in vacuum oven, with argon gas do shielding gas carry out normal pressure-sintered, be warming up to 1850-2200 ℃ the insulation 1-3 hour, take out behind the furnace cooling, obtain constant pressure sintering silicon carbide pipe or rod;
11), carborudum tube behind the sintering or rod are carried out precision work, obtain finished product.
2, the preparation method of silicon carbide ceramic according to claim 1 or rod is characterized in that described additive comprises solid state sintering auxiliary agent, liquid phase sintering auxiliary agent or compound additive; Solid state sintering auxiliary agent commonly used is norbide and carbon; Liquid phase sintering auxiliary agent commonly used is two or more the mixture in aluminum oxide, yttrium oxide, aluminium, yttrium aluminum garnet, rare earth oxide, the magnesium oxide; Compound additive commonly used is at least a in norbide, yttrium oxide, aluminum oxide, aluminium nitride, rare earth oxide, various whisker and the fiber.
3, the preparation method of silicon carbide ceramic according to claim 1 or rod is characterized in that described dispersion agent also can be ammonium polyacrylate; Described softening agent also can be a kind of in sucrose fat, the paraffin common plasticizers; Described lubricant also can be stearic acid; Described liquid adhesive also can be a kind of in polyvinyl alcohol, arab resin, the ether of cellulose binding agent commonly used.
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