CN101653964B - Cold isostatic pressing method of large-size cylindrical thin silicon carbide ceramic biscuit - Google Patents
Cold isostatic pressing method of large-size cylindrical thin silicon carbide ceramic biscuit Download PDFInfo
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- CN101653964B CN101653964B CN2009101525010A CN200910152501A CN101653964B CN 101653964 B CN101653964 B CN 101653964B CN 2009101525010 A CN2009101525010 A CN 2009101525010A CN 200910152501 A CN200910152501 A CN 200910152501A CN 101653964 B CN101653964 B CN 101653964B
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Abstract
The invention discloses a cold isostatic pressing method of a large-size cylindrical thin silicon carbide ceramic biscuit. The method comprises the following steps: (1) mechanically stirring and mixing a saturated tetramethyl ammonium hydroxide aqueous solution and silicon carbide powder, adding a polyving akohol aqueous solution and an acrylamide aqueous solution, mechanically stirring and mixing, adding graphite powder and carbon powder for ball milling so as to obtain a mixed slurry; (2) drying, pulverizing and granulating the mixed slurry and then dieforming the mixed slurry by an oil press so as to obtain a cylindrical biscuit; (3) repeatedly soaking the biscuit by a methylene diacrylamide aqueous solution and then drying the biscuit; (4) carrying out polymerization and crosslinking heat treatment; and (5) putting the cylindrical biscuit in alloy clamp moulds in the same shape for cold isostatic pressing. The invention realizes the high-intensity bonding of powder by utilizing the synergistic action of the viscosity of the polyving akohol, the polymerization of acrylamide monomers and the crosslinking of the methylene diacrylamide. The step of using the alloy clamp moulds in the same shape for cold isostatic pressing improves and homogenizes the density of the biscuit, reinforces the bonding effect and maintains the precise cylindrical surface shape of the biscuit, thus the large-size cylindrical thin silicon carbide ceramic biscuit can be obtained.
Description
Technical field
The present invention relates to a kind of large-size cylindrical thin silicon carbide ceramic biscuit cold isostatic pressing method.
Background technology
A committed step of the whole ballistic resistant sheet manufacturing process of reaction sintering silicon carbide ceramic is the shaping of large-size cylindrical thin silicon carbide and carbon dust mixed powder biscuit.Use the physical bond intensity of single binding agent low, can not support the deadweight of large-size cylindrical thin biscuit; Density reduced after increase binding agent dosage caused the biscuit degreasing; So need to use compound binding agent, and, under the prerequisite that does not increase binding agent dosage, realize the powder high strength bond through monomer polymerization and crosslinked chemical bonding.Single way stempressing can not guarantee that the biscuit density is even, must and improve biscuit density and intensity by the isostatic cool pressing homogenizing; Isostatic cool pressing easily causes the biscuit segment of a cylinder crooked and lose shape, must be in similar shape metal splint grinding tool isostatic cool pressing, obtain high strength, accurate conformal large-size cylindrical thin silicon carbide ceramic element.
Summary of the invention
The purpose of invention is to overcome the deficiencies in the prior art, and a kind of large-size cylindrical thin silicon carbide ceramic biscuit cold isostatic pressing method is provided.
The large-size cylindrical thin silicon carbide ceramic biscuit cold isostatic pressing method comprises the steps:
1) be that 15% TMAH saturated aqueous solution places ball grinder with 1～3 weight portion mass percent concentration, adding 30～40 weight portion particle diameters are carborundum and 20～60 microns carborundum of 10～20 weight portion particle diameters of 100～200 microns, add and two kinds of pure water that the carborundum cumulative volume is identical, stirred 1～3 hour, add 2～4 weight portion mass percent concentrations and be 7% polyvinyl alcohol water solution and 1～3 weight portion mass percent concentration and be 15% acrylamide aqueous solution, stirred 2～8 hours, add 20～25 weight portion graphite powders, the aluminium oxide abrading-ball that the activated carbon powder of 20～40 weight portions and above-mentioned solid gross mass are 1.5～2.5 times, wherein, above-mentioned solid comprises two kinds of carborundum, activated carbon powder and graphite powder, ball milling 12～24 hours obtains mixed slurry;
2) mixed slurry is placed in 80 ℃ of baking ovens 3-8 hour drying after, pulverize granulation, the hydraulic press die forming, pressure is 10～20MPa, obtaining length is 300～500 millimeters, width is 250～400 millimeters, and thickness is 6～10 millimeters, and wide is 200～2000 millimeters cylinder biscuit to radius of curvature;
3) spraying mass percent concentration on cylinder biscuit surface is 1.5～2.5% methylene diacrylamide saturated aqueous solution, after soaking fully to the cylinder biscuit, places in 80 ℃ of baking ovens 40 minutes, so repeats 3～5 times; Place heat-treatment furnace, 180 ℃ of insulations of heat treatment temperature 3 hours are taken out;
4) will place identical shaped aluminium alloy template die through heat treated cylinder biscuit, carry out 80～200MPa isostatic cool pressing.
The beneficial effect that the present invention compared with prior art has is:
1) selecting TMAH is dispersant, and carborundum and carbon dust are had identical dispersion effect.
2) selecting polyvinyl alcohol and acrylamide monomer is compound binding agent, methylene diacrylamide is a crosslinking agent, crosslinked by heat treatment realization acrylamide monomer polymerization and methylene diacrylamide, realize chemical bonding, act synergistically with the polyvinyl alcohol physical bond, produce the strong effect of cohering,, obtain high strength large-size cylindrical thin reaction sintering silicon carbide ceramic ballistic resistant sheet biscuit again through cold isometrical pressure cohesive action;
3) for overcoming compound binding agent and carbon dust affinity is strong, with inhomogeneous the cohering that causes a little less than the carborundum affinity, designed elder generation carborundum powder has been mixed with adhesive, add the processing step of graphite and carbon dust again, realized that heterogeneous powder granule uniformity coheres;
4) after the homotype aluminium alloy template die isostatic cool pressing, improve and homogenizing biscuit density, strengthen bond effect, and keep base substrate segment of a cylinder linearity and cambered surface radius of curvature, reach complete conformal.
The specific embodiment
The large-size cylindrical thin silicon carbide ceramic biscuit cold isostatic pressing method comprises the steps:
1) be that 15% TMAH saturated aqueous solution places ball grinder with 1～3 weight portion mass percent concentration, adding 30～40 weight portion particle diameters are carborundum and 20～60 microns carborundum of 10～20 weight portion particle diameters of 100～200 microns, add and last two kinds of pure water that the carborundum volume is identical, stirred 1～3 hour, add 2～4 weight portion mass percent concentrations and be 7% polyvinyl alcohol water solution and 1～3 weight portion mass percent concentration and be 15% acrylamide aqueous solution, stirred 2～8 hours, add 20～25 weight portion graphite powders, the aluminium oxide abrading-ball that the activated carbon powder of 20～40 weight portions and above-mentioned solid gross mass are 1.5～2.5 times, ball milling 12～24 hours, obtain mixed slurry, wherein solid comprises two kinds of carborundum, activated carbon powder and graphite powder;
2) mixed slurry is placed in 70～90 ℃ of baking ovens 3-8 hour, pulverize granulation, oil pressure is shaped, and pressure is 10～20MPa, and obtaining length is 300～500 millimeters, width is 250～400 millimeters, and thickness is 6～10 millimeters, and wide is 200～2000 millimeters cylinder biscuit to radius of curvature;
3) spraying mass percent concentration on cylinder biscuit surface is 1.5～2.5% methylene diacrylamide saturated aqueous solution, after soaking fully to the cylinder biscuit, places in 70～90 ℃ of baking ovens 10～40 minutes, so repeats 3～5 times; Place heat-treatment furnace, 180 ℃ of insulations of heat treatment temperature 3 hours are taken out;
4) will place identical shaped aluminium alloy template die through heat treated cylinder biscuit, carry out 80～200MPa isostatic cool pressing.
Principle of the present invention is:
The pure and mild acrylamide of using polythene (monomer) compound binding agent and methylene diacrylamide crosslinking agent, through monomer polymerization and crosslinked chemical bonding and polyvinyl alcohol physical bond synergy, under the prerequisite that does not increase binding agent dosage, realize the powder high strength bond.Single way stempressing can not guarantee that the biscuit density is even, must and improve the biscuit density by the isostatic cool pressing homogenizing; Isostatic cool pressing easily causes the bending of biscuit segment of a cylinder and loses shape, needs isostatic cool pressing in similar shape metal splint grinding tool, obtains high strength, accurate conformal large-size cylindrical thin silicon carbide ceramic biscuit.
Embodiment 1
1) be that 15% TMAH saturated aqueous solution places ball grinder with 1 weight portion mass percent concentration, add 30 weight portion particle diameters and be sic powder and 20 microns carborundum of 10 weight portion particle diameters of 100 microns, add the pure water identical with above-mentioned solid volume, mechanical agitation 1 hour, add 2 weight portion mass percent concentrations and be 7% polyvinyl alcohol water solution and 1 weight portion mass percent concentration and be 15% acrylamide aqueous solution, mechanical agitation 2 hours, the activated carbon powder that adds 20 weight portion graphite powders and 20 weight portions, aluminium oxide abrading-ball with 1.5 times of above-mentioned solid gross masses, ball milling 12 hours obtains mixed slurry;
2) mixed slurry is placed in 70 ℃ of baking ovens 3 hours, pulverize, granulation, oil pressure is shaped, and pressure is 10MPa, and obtaining length is 300 millimeters, and width is 250 millimeters, and thickness is 6 millimeters, and wide is 200 millimeters cylinder biscuit to radius of curvature;
3) spraying mass percent concentration on cylinder biscuit surface is 1.5% methylene diacrylamide saturated aqueous solution, after soaking fully to the cylinder biscuit, places in 80 ℃ of baking ovens 40 minutes, so repeats 3 times; Place heat-treatment furnace, 180 ℃ of insulations of heat treatment temperature 3 hours are taken out.
4) will place identical shaped aluminium alloy template die through heat treated cylinder biscuit, carry out the 80MPa isostatic cool pressing.
Embodiment 2
1) be that 15% TMAH saturated aqueous solution places ball grinder with 3 weight portion mass percent concentrations, add 40 weight portion particle diameters and be sic powder and 60 microns carborundum of 20 weight portion particle diameters of 200 microns, add the pure water identical with above-mentioned solid volume, mechanical agitation 3 hours, add 4 weight portion mass percent concentrations and be 7% polyvinyl alcohol water solution and 3 weight portion mass percent concentrations and be 15% acrylamide aqueous solution, mechanical agitation 8 hours, the activated carbon powder that adds 25 weight portion graphite powders and 40 weight portions, aluminium oxide abrading-ball with 1.5 times of above-mentioned solid gross masses, ball milling 24 hours obtains mixed slurry;
2) mixed slurry is placed in 90 ℃ of baking ovens 8 hours, pulverize, granulation, oil pressure is shaped, and pressure is 20MPa, and obtaining length is 500 millimeters, and width is 400 millimeters, and thickness is 10 millimeters, and wide is 2000 millimeters cylinder biscuit to radius of curvature;
3) spraying mass percent concentration on cylinder biscuit surface is 2.5% methylene diacrylamide saturated aqueous solution, after soaking fully to the cylinder biscuit, places in 80 ℃ of baking ovens 40 minutes, so repeats 5 times; Place heat-treatment furnace, 180 ℃ of insulations of heat treatment temperature 3 hours are taken out.
4) will place identical shaped aluminium alloy template die through heat treated cylinder biscuit, carry out the 200MPa isostatic cool pressing.
Embodiment 3
1) be that 15% TMAH saturated aqueous solution places ball grinder with 2 weight portion mass percent concentrations, add 30 weight portion particle diameters and be sic powder and 40 microns carborundum of 10 weight portion particle diameters of 150 microns, add the pure water identical with above-mentioned solid volume, mechanical agitation 2 hours, add 3 weight portion mass percent concentrations and be 7% polyvinyl alcohol water solution and 1 weight portion mass percent concentration and be 15% acrylamide aqueous solution, mechanical agitation 2 hours, the activated carbon powder that adds 20 weight portion graphite powders and 20 weight portions, aluminium oxide abrading-ball with 2 times of above-mentioned solid gross masses, ball milling 12 hours obtains mixed slurry;
2) mixed slurry is placed in 80 ℃ of baking ovens 5 hours, pulverize, granulation, oil pressure is shaped, and pressure is 10MPa, and obtaining length is 300 millimeters, and width is 250 millimeters, and thickness is 6 millimeters, and wide is 200 millimeters cylinder biscuit to radius of curvature;
3) spraying mass percent concentration on cylinder biscuit surface is 1.5% methylene diacrylamide saturated aqueous solution, after soaking fully to the cylinder biscuit, places in 80 ℃ of baking ovens 40 minutes, so repeats 3 times; Place heat-treatment furnace, 180 ℃ of insulations of heat treatment temperature 3 hours are taken out.
4) will place identical shaped aluminium alloy template die through heat treated cylinder biscuit, carry out the 80MPa isostatic cool pressing.
Embodiment 4
1) be that 15% TMAH saturated aqueous solution places ball grinder with 2.5 weight portion mass percent concentrations, add 30 weight portion particle diameters and be sic powder and 20 microns carborundum of 10 weight portion particle diameters of 100 microns, add the pure water identical with above-mentioned solid volume, mechanical agitation 1 hour, add 2 weight portion mass percent concentrations and be 7% polyvinyl alcohol water solution and 1 weight portion mass percent concentration and be 15% acrylamide aqueous solution, mechanical agitation 2 hours, the activated carbon powder that adds 20 weight portion graphite powders and 20 weight portions, aluminium oxide abrading-ball with 1.5 times of above-mentioned solid gross masses, ball milling 12 hours obtains mixed slurry;
2) mixed slurry is placed in 70 ℃ of baking ovens 3 hours, pulverize, granulation, oil pressure is shaped, and pressure is 10MPa, and obtaining length is 300 millimeters, and width is 250 millimeters, and thickness is 6 millimeters, and wide is 200 millimeters cylinder biscuit to radius of curvature;
3) spraying mass percent concentration on cylinder biscuit surface is 1.5% methylene diacrylamide saturated aqueous solution, after soaking fully to the cylinder biscuit, places in 80 ℃ of baking ovens 40 minutes, so repeats 3 times; Place heat-treatment furnace, 180 ℃ of insulations of heat treatment temperature 3 hours are taken out.
4) will place identical shaped aluminium alloy folder through heat treated cylinder biscuit. carry out the 80MPa isostatic cool pressing.
Embodiment 5
1) be that 15% TMAH saturated aqueous solution places ball grinder with 2 weight portion mass percent concentrations, add 30 weight portion particle diameters and be sic powder and 20 microns carborundum of 10 weight portion particle diameters of 100 microns, add the pure water identical with above-mentioned solid volume, mechanical agitation 1 hour, add 2 weight portion mass percent concentrations and be 7% polyvinyl alcohol water solution and 1 weight portion mass percent concentration and be 15% acrylamide aqueous solution, mechanical agitation 2 hours, the activated carbon powder that adds 20 weight portion graphite powders and 20 weight portions, aluminium oxide abrading-ball with 1.5 times of above-mentioned solid gross masses, ball milling 12 hours obtains mixed slurry;
2) mixed slurry is placed in 70 ℃ of baking ovens 3 hours, pulverize, granulation, oil pressure is shaped, and pressure is 10MPa, and obtaining length is 300 millimeters, and width is 250 millimeters, and thickness is 6 millimeters, and wide is 200 millimeters cylinder biscuit to radius of curvature;
3) spraying mass percent concentration on cylinder biscuit surface is 1.5% methylene diacrylamide saturated aqueous solution, after soaking fully to the cylinder biscuit, places in 80 ℃ of baking ovens 40 minutes, so repeats 3 times; Place heat-treatment furnace, 180 ℃ of insulations of heat treatment temperature 3 hours are taken out.
4) will place identical shaped aluminium alloy folder through heat treated cylinder biscuit, carry out the 80MPa isostatic cool pressing.
Claims (1)
1. a large-size cylindrical thin silicon carbide ceramic biscuit cold isostatic pressing method is characterised in that to comprise the steps:
1) be that 15% TMAH saturated aqueous solution places ball grinder with 1～3 weight portion mass percent concentration, adding 30～40 weight portion particle diameters are carborundum and 20～60 microns carborundum of 10～20 weight portion particle diameters of 100～200 microns, add and two kinds of pure water that the carborundum cumulative volume is identical again, stirred 1～3 hour, add 2～4 weight portion mass percent concentrations and be 7% polyvinyl alcohol water solution and 1～3 weight portion mass percent concentration and be 15% acrylamide aqueous solution, stirred 2～8 hours, add 20～25 weight portion graphite powders, the aluminium oxide abrading-ball that the activated carbon powder of 20～40 weight portions and above-mentioned solid gross mass are 1.5～2.5 times, wherein, above-mentioned solid comprises two kinds of carborundum, activated carbon powder and graphite powder, ball milling 12～24 hours obtains mixed slurry;
2) mixed slurry is placed in 80 ℃ of baking ovens 3～8 hours dryings after, pulverize granulation, the hydraulic press die forming, pressure is 10～20MPa, obtaining length is 300～500 millimeters, width is 250～400 millimeters, and thickness is 6～10 millimeters, and wide is 200～2000 millimeters cylinder biscuit to radius of curvature;
3) spraying mass percent concentration on cylinder biscuit surface is 1.5～2.5% methylene diacrylamide saturated aqueous solution, after soaking fully to the cylinder biscuit, places in 80 ℃ of baking ovens 40 minutes, so repeats 3～5 times; Place heat-treatment furnace, 180 ℃ of insulations of heat treatment temperature 3 hours are taken out;
4) will place identical shaped aluminium alloy template die through heat treated cylinder biscuit, carry out 80～200MPa isostatic cool pressing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101525010A CN101653964B (en) | 2009-09-10 | 2009-09-10 | Cold isostatic pressing method of large-size cylindrical thin silicon carbide ceramic biscuit |
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| CN2009101525010A CN101653964B (en) | 2009-09-10 | 2009-09-10 | Cold isostatic pressing method of large-size cylindrical thin silicon carbide ceramic biscuit |
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| CN101653964B true CN101653964B (en) | 2011-05-18 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996028399A1 (en) * | 1995-03-09 | 1996-09-19 | Ins^¿Titut 'joz^¿Ef Stefan' | A process for forming ceramic products from an aqueous suspension with a high solids content |
| US5656218A (en) * | 1995-05-19 | 1997-08-12 | Industrial Technology Research Institute | Method for making high performance self-reinforced silicon carbide using a pressureless sintering process |
| CN1686940A (en) * | 2005-04-07 | 2005-10-26 | 上海交通大学 | Method for forming ceramics biscuits of carbonized bricks |
| CN100999411A (en) * | 2006-12-30 | 2007-07-18 | 浙江大学 | Aluminium nitride reinforced sibicon carbide ceramic and its preparation method |
| CN101100384A (en) * | 2007-07-20 | 2008-01-09 | 浙江大学 | Nanometer composite silicon carbide ceramic and preparation method thereof |
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- 2009-09-10 CN CN2009101525010A patent/CN101653964B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996028399A1 (en) * | 1995-03-09 | 1996-09-19 | Ins^¿Titut 'joz^¿Ef Stefan' | A process for forming ceramic products from an aqueous suspension with a high solids content |
| US5656218A (en) * | 1995-05-19 | 1997-08-12 | Industrial Technology Research Institute | Method for making high performance self-reinforced silicon carbide using a pressureless sintering process |
| CN1686940A (en) * | 2005-04-07 | 2005-10-26 | 上海交通大学 | Method for forming ceramics biscuits of carbonized bricks |
| CN100999411A (en) * | 2006-12-30 | 2007-07-18 | 浙江大学 | Aluminium nitride reinforced sibicon carbide ceramic and its preparation method |
| CN101100384A (en) * | 2007-07-20 | 2008-01-09 | 浙江大学 | Nanometer composite silicon carbide ceramic and preparation method thereof |
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Address after: 313000 Zhejiang city of Huzhou province Deqing County leidian town revitalization Road No. 7 Patentee after: Zhejiang Li Tai composite limited company Address before: 313219 Zhejiang city of Huzhou province Deqing County LEIDIAN Industrial Park revitalization Road No. 7 Patentee before: Zhejiang Light-tough Composite Materials Co., Ltd. |
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Denomination of invention: Cold isostatic pressing of large cylindrical thin SiC ceramic blank Effective date of registration: 20210531 Granted publication date: 20110518 Pledgee: Zhejiang Deqing Rural Commercial Bank Co.,Ltd. leidian sub branch Pledgor: ZHEJIANG LIGHT-TOUGH COMPOSITE MATERIALS Co.,Ltd. Registration number: Y2021330000496 |
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