CN103641482A - Preparation method for self-lubricating silicon carbide ceramic sealing material - Google Patents
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Abstract
The invention relates to a preparation method for a silicon carbide ceramic, and particularly relates to a preparation method for a self-lubricating silicon carbide ceramic sealing material. The preparation method includes the steps of mixing raw materials, carrying out spay granulation, carrying out compression molding, sintering in vacuum, processing the vacuum sintered blank according to drawing requirements, and thus obtaining the self-lubricating silicon carbide ceramic sealing piece finished product. The preparation method has the beneficial effects that a silicon carbide slurry and a lubricant are mixed by a wet method, the difficulty of difficult molding caused by dry-method mixing is overcome, the lubricant can be uniformly distributed inside the silicon carbide substrate, and uniformity of the material internal lubricant is ensured; because the adopted lubricant has a certain strength, the seal ring failure problem caused because a silicon carbide seal ring is stripped due to insufficient lubricating phase strength during a using process is avoided; and the lubricant is subjected to high temperature impurity removal, the purity of the silicon carbide ceramic sealing material can be effectively guaranteed, and the mechanical strength of the product is improved.
Description
Affiliated technical field
The present invention relates to a kind of preparation method of silicon carbide ceramics, particularly a kind of preparation method of self-lubricating silicon carbide ceramic seal material.
Background technology
Silicon carbide sealing member in use, due to the unusual Gao Keda planeness 0.0009mm of rotating ring and stationary ring two seal face planenesses, very easily produce adhesive phenomenon, under static state during starting outfit, because the suction-combining force of rotating ring and stationary ring two seal faces is very large, easily make sealing member produce even fracture of wearing and tearing, thereby affect the work-ing life of product.
Chinese patent disclosed " a kind of silicon carbide carbonized complex phase ceramic sealing material and preparation method thereof " by name, in publication number CN 101591169A, in related silicon carbide carbonized complex phase ceramic sealing material, lubricant is graphite, although graphite lubricity is splendid, but because the graphite adding in silicon carbide ceramics sintering can not occur under the condition of 2,000 degree high temperature, therefore the character of graphite in silicon carbide ceramics does not change, graphite-phase is weak rear phase for silicon carbide, its hardness, the character of all respects such as intensity relatively a little less than, at silicon carbide ceramics closure material, carry out in the process of post-production, there will be some pittings, thereby affected the overall performance of material.
Chinese patent disclosed " conventional sintered microporous carborundum graphite self-lubricating seal ring and manufacture method thereof " by name, in publication number CN 101255330A, related lubricant is also graphite, there is the same defect with last patent, in the time of simultaneously due to micropore and graphite, exist, will affect the overall performance of material.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, the object of this invention is to provide that a kind of self-lubricating effect is good, the preparation method of hardness, intensity is high, frictional coefficient is little self-lubricating silicon carbide ceramic seal material.
Technical scheme of the present invention is: a kind of preparation method of self-lubricating silicon carbide ceramic seal material, and the method comprises the following steps:
1) mixing of raw material: by weight percentage by submicron order α type silicon carbide 70-90%, norbide 0.1-3%, resin 3-15%, organic matter binding agent 5-20%, lubricant 0.5-10%, put into mixer and add pure water to carry out wet-mixed, after 6-48 hour, the slip mixing is crossed to 60-120 mesh sieve;
2) mist projection granulating: slip after sieving in above-mentioned steps is carried out to granulation by mist projection granulating tower, mist projection granulating tower inlet temperature 180-260 ℃, temperature out 60-120 ℃, premix powder after granulation sieves with 60-120 mesh sieve, and the premix powder loose density of producing reaches 0.85-0.90 g/cm
3, mobility reaches 8-11 s/30g;
3) compression molding: choose mould according to required article shape, above-mentioned premix powder is packed in mold cavity, carry out mold pressing premolding with 50-200MPa pressure; Or after above-mentioned mold pressing premolding, then wait static pressure with 200-300MPa pressure, obtain molded blank;
4) vacuum sintering: the blank that above-mentioned steps is prepared, to put into vacuum sintering furnace and carry out vacuum sintering, sintering step is: blank is packed into after vacuum sintering furnace, sintering oven is vacuumized, when vacuum tightness reaches 3-5 * 10
-2after Pa, to logical argon gas in sintering oven, to normal pressure, heat, the pass of Heating temperature and time is: room temperature to 800 ℃, 5-8 hour, insulation 0.5-1 hour, from 800 ℃ to 2000-2300 ℃, 6-9 hour, is incubated 1 to 2 hour, furnace cooling, is down to room temperature and comes out of the stove afterwards;
5) processing: by the blank after above-mentioned vacuum sintering by drawing, obtain self-lubricating silicon carbide ceramic seal part finished product after processing.
The particle diameter of above-mentioned submicron order α type silicon carbide is 0.50-0.60 micron, and purity is greater than 99%.
Above-mentioned resin is: one or more in acrylic resin, resol, polyamide resin, epoxy resin composite; Described organic binder bond is: one or more in polyvinyl alcohol, dextrin, carboxymethyl cellulose composite.
The particle diameter of above-mentioned norbide is 0.5-2.0 micron, and purity is greater than 90%.
Above-mentioned lubricant is: one or more in tungsten disulfide, hexagonal boron nitride, carbon graphite composite.
The granularity of above-mentioned lubricant is 5-20 micron, purity >=90 %.
At above-mentioned lubricant, through high temperature removal of impurities, process; High temperature removal of impurities process is: lubricant is put into vacuum sintering furnace, when suction reaches 3-5 * 10
-2pa post-heating, heat-processed is: normal temperature-400 ℃, 3 hours, 400-1000 ℃, 5 hours, are then incubated after 20-60 minutes furnace cooling.
The self-lubricating silicon carbide ceramic seal material of above-mentioned preparation, its density is 2.85-3.06 g/cm
3, HRA hardness 88-92, three-point bending resistance intensity is 210-400Mpa, friction is 0.20-0.30.。
The beneficial effect of technical scheme of the present invention is: 1, silicon carbide slurry and lubricant adopt wet-mixed, in mixing process, lubricant and binding agent can carry out effective combination, in pressing process lubricant can with the good combination of matrix, overcome the difficulty of the easy-formation not that dry mixed causes, in addition, owing to adopting wet-mixed, lubricant can be uniformly distributed in silicon carbide substrate inside, the homogeneity that guarantees material internal lubricant, its frictional coefficient can reach 0.2-0.3; 2, because the lubricant adopting has certain intensity, avoided silicon carbide sealed ring in use, because lubricated phase insufficient strength produces, peeled off, the problem that causes wear ring to lose efficacy; 3, due to the tungsten disulfide to as lubricant, hexagonal boron nitride, mechanical carbon, carry out high temperature removal of impurities, can effectively guarantee the purity of silicon carbide ceramic seal material, improved the physical strength of product.
Embodiment
Embodiment 1:
First the tungsten disulfide as lubricant is carried out to high temperature removal of impurities processing, treating processes is: tungsten disulfide is put into vacuum sintering furnace, when suction reaches 3 * 10
-2after Pa, heat, heat-processed is: normal temperature-400 ℃, and 3 hours, 400-1000 ℃, 5 hours, be then incubated 20 minutes, stand-by after furnace cooling.
1) mixing of raw material: α type silicon carbide powder 70 ㎏ that to get particle diameter and be 0.6 micron, purity be 99.5%, particle diameter is boron carbide powder 3 ㎏ that 2 microns, purity are 91%, acrylic resin 15 ㎏, tungsten disulfide 10 ㎏, polyvinyl alcohol 5 ㎏, above-mentioned raw materials is put into mixer and add pure water, mix after 49 hours, cross 120 mesh sieves;
2) spraying is dry: the slip after sieving is carried out to granulation by mist projection granulating tower; 260 ℃ of mist projection granulating tower inlet temperatures, 120 ℃ of temperature outs; Dried material is crossed after 120 mesh sieves, and obtaining loose density is 0.90g/cm
3, the material that mobility is 11s/30g;
3) compression molding: choose annular rigid die, above-mentioned pelletizing is packed in mold cavity, with after the premolding of 50MPa pressure, then put into equal pressing equipment, carry out isostatic cool pressing with 300MPa pressure, obtain molded blank;
4) vacuum sintering: molded blank prepared by above-mentioned steps is put into vacuum sintering furnace and vacuumized, when vacuum tightness reaches 3 * 10
-2after Pa, to logical argon gas in sintering oven, to normal pressure, heat, from room temperature to 800 ℃, 5 hours used times, are incubated 1 hour after being warmed up to 800 ℃, then continue to be warming up to 2000 ℃, heating-up time is 7 hours, be incubated after 1 hour, stop heating and come out of the stove after cooling to room temperature with the furnace, obtaining the density of product after sintering is 2.85 g/cm
3, HRA hardness 88, three-point bending resistance intensity is 210Mpa;
5) processing: by the blank after above-mentioned vacuum sintering by drawing, obtain self-lubricating silicon carbide ceramic seal part finished product after processing, product frictional coefficient is 0.26.
Embodiment 2:
First the hexagonal boron nitride as lubricant is carried out to high temperature removal of impurities processing, treating processes is: hexagonal boron nitride is put into vacuum sintering furnace, when suction reaches 3 * 10
-2after Pa, heat, heat-processed is: normal temperature-400 ℃, and 3 hours, 400-1000 ℃, 5 hours, be then incubated 20 minutes, stand-by after furnace cooling.
1) mixing of raw material: α type silicon carbide powder 90 ㎏ that to get particle diameter and be 0.5 micron, purity be 99.6%, particle diameter is boron carbide powder 0.1 ㎏ that 0.5 micron, purity are 92%, resol 3 ㎏, dextrin 5 ㎏, hexagonal boron nitride 1.9 ㎏, above-mentioned raw materials is put into mixer and add pure water, mix after 6 hours, cross 60 mesh sieves;
2) spraying is dry: the slip after sieving is carried out to granulation by mist projection granulating tower; 180 ℃ of mist projection granulating tower inlet temperatures, 60 ℃ of temperature outs; Dried material is crossed after 60 mesh sieves, and obtaining loose density is 0.85g/cm
3, the material that mobility is 8s/30g;
3) compression molding: choose annular rigid die, above-mentioned pelletizing is packed in mold cavity, with after the premolding of 200MPa pressure, obtain molded blank;
4) vacuum sintering: molded blank prepared by above-mentioned steps is put into vacuum sintering furnace and vacuumized, when vacuum tightness reaches 4 * 10
-2after Pa, to logical argon gas in sintering oven, to normal pressure, heat, from room temperature to 800 ℃, 6 hours used times, are incubated 1 hour after being warmed up to 800 ℃, then continue to be warming up to 2300 ℃, heating-up time is 8 hours, be incubated after 2 hours, stop heating and come out of the stove after cooling to room temperature with the furnace, obtaining the density of product after sintering is 3.0g/cm
3, HRA hardness 90, three-point bending resistance intensity is 368 Mpa.
5) processing: by the blank after above-mentioned vacuum sintering by drawing, obtain self-lubricating silicon carbide ceramic seal part finished product after processing.Product frictional coefficient can reach 0.20.
Embodiment 3:
First the carbon graphite as lubricant is carried out to high temperature removal of impurities processing, treating processes is: carbon graphite is put into vacuum sintering furnace, when suction reaches 3 * 10
-2after Pa, heat, heat-processed is: normal temperature-400 ℃, and 3 hours, 400-1000 ℃, 5 hours, be then incubated 20, stand-by after furnace cooling.
1) mixing of raw material: α type silicon carbide powder 80 ㎏ that to get particle diameter and be 0.55 micron, purity be 99.2%, particle diameter is boron carbide powder 2 ㎏ that 0.5 micron, purity are 91%, polyamide resin 6 ㎏, carboxymethyl cellulose 7 ㎏, carbon graphite 0.5 ㎏, above-mentioned raw materials is put into mixer and add pure water, mix after 6 hours, cross 80 mesh sieves;
2) spraying is dry: the slip after sieving is carried out to granulation by mist projection granulating tower; 200 ℃ of mist projection granulating tower inlet temperatures, 80 ℃ of temperature outs; Dried material is crossed after 100 mesh sieves, and obtaining loose density is 0.88g/cm
3, the material that mobility is 9s/30g;
3) compression molding: choose annular rigid die, above-mentioned pelletizing is packed in mold cavity, with after the premolding of 100MPa pressure, then put into equal pressing equipment, carry out isostatic cool pressing with 200MPa pressure, obtain molded blank;
4) vacuum sintering: molded blank prepared by above-mentioned steps is put into vacuum sintering furnace and vacuumized, when vacuum tightness reaches 5 * 10
-2after Pa, to logical argon gas in sintering oven, to normal pressure, heat, from room temperature to 800 ℃, 8 hours used times, are incubated 0.5 hour after being warmed up to 800 ℃, then continue to be warming up to 2215 ℃, heating-up time is 9 hours, be incubated after 1.5 hours, stop heating and come out of the stove after cooling to room temperature with the furnace, obtaining the density of product after sintering is 3.06g/cm
3, HRA hardness 92, three-point bending resistance intensity is 400 Mpa.
5) processing: by the blank after above-mentioned vacuum sintering by drawing, obtain self-lubricating silicon carbide ceramic seal part finished product after processing.Product frictional coefficient can reach 0.30.
Example 4:
High temperature removal of impurities as the tungsten disulfide of lubricant, hexagonal boron nitride, mechanical carbon is processed as previously mentioned.
1) mixing of raw material: α type silicon carbide powder 78 ㎏ that to get particle diameter and be 0.55 micron, purity be 99.8%, particle diameter is boron carbide powder 2 ㎏ that 1 micron, purity are 92%, epoxy resin 11 ㎏, carboxypolymethylene alcohol, each 3 ㎏ of methyl fiber, tungsten disulfide, hexagonal boron nitride, each 0.5 ㎏ of mechanical carbon, above-mentioned raw materials is put into mixer and add pure water, mix after 6 hours, cross 80 mesh sieves;
2) spraying is dry: the slip after sieving is carried out to granulation by mist projection granulating tower; 240 ℃ of mist projection granulating tower inlet temperatures, 100 ℃ of temperature outs; Dried material is crossed after 100 mesh sieves, and obtaining loose density is 0.89g/cm
3, the material that mobility is 10s/30g;
3) compression molding: choose annular rigid die, above-mentioned pelletizing is packed in mold cavity, with after the premolding of 80MPa pressure, then put into equal pressing equipment, carry out isostatic cool pressing with 220MPa pressure, obtain molded blank;
4) vacuum sintering: molded blank prepared by above-mentioned steps is put into vacuum sintering furnace and vacuumized, when vacuum tightness reaches 4 * 10
-2after Pa, to logical argon gas in sintering oven, to normal pressure, heat, from room temperature to 800 ℃, 5 hours used times, are incubated 1 hour after being warmed up to 800 ℃, then continue to be warming up to 2215 ℃, heating-up time is 7 hours, be incubated after 2 hours, stop heating and come out of the stove after cooling to room temperature with the furnace, obtaining the density of product after sintering is 3.06g/cm
3, HRA hardness 92, three-point bending resistance intensity is 400Mpa.
5) processing: by the blank after above-mentioned vacuum sintering by drawing, obtain self-lubricating silicon carbide ceramic seal part finished product after processing.Product frictional coefficient can reach 0.25.
Embodiment 5:
As the tungsten disulfide of lubricant, the high temperature removal of impurities of hexagonal boron nitride process as previously mentioned.
1) mixing of raw material: α type silicon carbide powder 76 ㎏ that to get particle diameter and be 0.55 micron, purity be 99.8%, particle diameter is boron carbide powder 1.5 ㎏ that 1.8 microns, purity are 92%, acrylic resin, resol, each 2 ㎏ of polyamide resin, dextrin 8 ㎏, carboxymethyl cellulose 4 ㎏, tungsten disulfide 1.5 ㎏, hexagonal boron nitride 5 ㎏, above-mentioned raw materials is put into mixer and add pure water, mix after 6 hours, cross 80 mesh sieves;
2) spraying is dry: the slip after sieving is carried out to granulation by mist projection granulating tower; 240 ℃ of mist projection granulating tower inlet temperatures, 100 ℃ of temperature outs; Dried material is crossed after 100 mesh sieves, and obtaining loose density is 0.89g/cm
3, the material that mobility is 10s/30g;
3) compression molding: choose annular rigid die, above-mentioned pelletizing is packed in mold cavity, with after the premolding of 80MPa pressure, then put into equal pressing equipment, carry out isostatic cool pressing with 220MPa pressure, obtain molded blank;
4) vacuum sintering: molded blank prepared by above-mentioned steps is put into vacuum sintering furnace and vacuumized, when vacuum tightness reaches 3 * 10
-2after Pa, to logical argon gas in sintering oven, to normal pressure, heat, from room temperature to 800 ℃, 7 hours used times, are incubated 0.6 hour after being warmed up to 800 ℃, then continue to be warming up to 2215 ℃, heating-up time is 8 hours, be incubated after 2 hours, stop heating and come out of the stove after cooling to room temperature with the furnace, obtaining the density of product after sintering is 2.98g/cm
3, HRA hardness 90, three-point bending resistance intensity is 350Mpa.
5) processing: by the blank after above-mentioned vacuum sintering by drawing, obtain self-lubricating silicon carbide ceramic seal part finished product after processing.Product frictional coefficient can reach 0.26.
In the above-described embodiments, the purity of unreceipted raw material is technical grade.
Claims (8)
1. a preparation method for self-lubricating silicon carbide ceramic seal material, the method comprises the following steps:
1) mixing of raw material: by weight percentage by submicron order α type silicon carbide 70-90%, norbide 0.1-3%, resin 3-15%, organic matter binding agent 5-20%, lubricant 0.5-10%, put into mixer and add pure water to carry out wet-mixed, after 6-48 hour, the slip mixing is crossed to 60-120 mesh sieve;
2) mist projection granulating: slip after sieving in above-mentioned steps is carried out to granulation by mist projection granulating tower, mist projection granulating tower inlet temperature 180-260 ℃, temperature out 60-120 ℃, premix powder after granulation sieves with 60-120 mesh sieve, and the premix powder loose density of producing reaches 0.85-0.90 g/cm
3, mobility reaches 8-11 s/30g;
3) compression molding: choose mould according to required article shape, above-mentioned premix powder is packed in mold cavity, carry out mold pressing premolding with 50-200MPa pressure; Or after above-mentioned mold pressing premolding, then wait static pressure with 200-300MPa pressure, obtain molded blank;
4) vacuum sintering: the blank that above-mentioned steps is prepared, to put into vacuum sintering furnace and carry out vacuum sintering, sintering step is: blank is packed into after vacuum sintering furnace, sintering oven is vacuumized, when vacuum tightness reaches 3-5 * 10
-2after Pa, to logical argon gas in sintering oven, to normal pressure, heat, the pass of Heating temperature and time is: room temperature to 800 ℃, 5-8 hour, insulation 0.5-1 hour, from 800 ℃ to 2000-2300 ℃, 6-9 hour, is incubated 1 to 2 hour, furnace cooling, is down to room temperature and comes out of the stove afterwards;
5) processing: by the blank after above-mentioned vacuum sintering by drawing, obtain self-lubricating silicon carbide ceramic seal part finished product after processing.
2. the preparation method of self-lubricating silicon carbide ceramic seal material according to claim 1, is characterized in that the particle diameter of above-mentioned submicron order α type silicon carbide is 0.50-0.60 micron, and purity is greater than 99%.
3. the preparation method of self-lubricating silicon carbide ceramic seal material according to claim 2, is characterized in that above-mentioned resin is: one or more in acrylic resin, resol, polyamide resin, epoxy resin composite; Described organic binder bond is: one or more in polyvinyl alcohol, dextrin, carboxymethyl cellulose composite.
4. the preparation method of self-lubricating silicon carbide ceramic seal material according to claim 3, is characterized in that the particle diameter of above-mentioned norbide is 0.5-2.0 micron, and purity is greater than 90%.
5. the preparation method of self-lubricating silicon carbide ceramic seal material according to claim 4, is characterized in that above-mentioned lubricant is: one or more in tungsten disulfide, hexagonal boron nitride, carbon graphite composite.
6. the preparation method of self-lubricating silicon carbide ceramic seal material according to claim 5, the granularity that it is characterized in that above-mentioned lubricant is 5-20 micron, purity >=90 %.
7. the preparation method of self-lubricating silicon carbide ceramic seal material according to claim 6, is characterized in that above-mentioned lubricant processes through high temperature removal of impurities; High temperature removal of impurities process is: lubricant is put into vacuum sintering furnace, when suction reaches 3-5 * 10
-2pa post-heating, heat-processed is: normal temperature-400 ℃, 3 hours, 400-1000 ℃, 5 hours, are then incubated after 20-60 minutes furnace cooling.
8. the preparation method of self-lubricating silicon carbide ceramic seal material according to claim 7, is characterized in that the self-lubricating silicon carbide ceramic seal material of above-mentioned preparation, and its density is 2.85-3.06 g/cm
3, HRA hardness 88-92, three-point bending resistance intensity is 210-400Mpa, friction is 0.20-0.30.
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| CN103922743A (en) * | 2013-10-25 | 2014-07-16 | 宁夏机械研究院（有限责任公司） | Silicon carbide sealing ring possessing spherical micropore and its preparation method |
| CN104402448A (en) * | 2014-11-19 | 2015-03-11 | 山东宝纳新材料有限公司 | Preparation method of novel non-pressure silicon carbide bearing balls |
| CN104496478A (en) * | 2014-12-08 | 2015-04-08 | 中国船舶重工集团公司第七二五研究所 | Method for preparing self-lubricating silicon carbide sealing material through pressureless sintering |
| CN104844225A (en) * | 2015-06-08 | 2015-08-19 | 齐鲁工业大学 | SiC-coated hexagonal boron nitride composite powder modified self-lubricating ceramic cutter material and preparation method thereof |
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| CN105294108A (en) * | 2015-12-03 | 2016-02-03 | 中国兵器科学研究院宁波分院 | Preparation method of low-cost normal pressure-sintered silicon carbide ceramics |
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| CN109650894A (en) * | 2019-02-15 | 2019-04-19 | 上海华硕精瓷陶瓷股份有限公司 | A kind of preparation method of normal pressure-sintered silicon carbide ceramics part |
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| CN104496478A (en) * | 2014-12-08 | 2015-04-08 | 中国船舶重工集团公司第七二五研究所 | Method for preparing self-lubricating silicon carbide sealing material through pressureless sintering |
| CN104844225A (en) * | 2015-06-08 | 2015-08-19 | 齐鲁工业大学 | SiC-coated hexagonal boron nitride composite powder modified self-lubricating ceramic cutter material and preparation method thereof |
| CN104844225B (en) * | 2015-06-08 | 2016-07-27 | 齐鲁工业大学 | Self-lubrication ceramic cutter material of carborundum cladding hexagonal boron nitride powder modified and preparation method thereof |
| CN104989827A (en) * | 2015-06-17 | 2015-10-21 | 宁波东联密封件有限公司 | Mechanical sealing device for pump |
| CN105294108A (en) * | 2015-12-03 | 2016-02-03 | 中国兵器科学研究院宁波分院 | Preparation method of low-cost normal pressure-sintered silicon carbide ceramics |
| TWI737801B (en) * | 2016-09-27 | 2021-09-01 | 日商北陸成型工業股份有限公司 | Silicon carbide component for plasma processing device and manufacturing method thereof |
| CN107324810A (en) * | 2017-07-14 | 2017-11-07 | 芜湖乾凯材料科技有限公司 | Low friction carbide composite ceramic and preparation method thereof |
| CN109650894A (en) * | 2019-02-15 | 2019-04-19 | 上海华硕精瓷陶瓷股份有限公司 | A kind of preparation method of normal pressure-sintered silicon carbide ceramics part |
| CN114380537A (en) * | 2022-01-25 | 2022-04-22 | 上海德宝密封件有限公司 | Silicon carbide light-weight sealing ring and preparation method thereof |
| CN117756532A (en) * | 2023-12-14 | 2024-03-26 | 宁夏机械研究院股份有限公司 | Silicon carbide material and preparation method thereof |
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