CN101551012A - A carbonaceous silicon carbide sealed ring and preparation method thereof - Google Patents
A carbonaceous silicon carbide sealed ring and preparation method thereof Download PDFInfo
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- CN101551012A CN101551012A CNA2009100988759A CN200910098875A CN101551012A CN 101551012 A CN101551012 A CN 101551012A CN A2009100988759 A CNA2009100988759 A CN A2009100988759A CN 200910098875 A CN200910098875 A CN 200910098875A CN 101551012 A CN101551012 A CN 101551012A
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Abstract
The invention discloses a preparation method of carbonaceous silicon carbide sealed ring, taking silicon carbide powder, yttrium aluminum garnet and carbon powder as the main raw material, includes the following steps in sequence: 1) adding the main raw material, binder, and dispersant in the deionized water, performing ball mill mixing, and then confecting into a water-based silicon carbide compound slurry; 2) using spray granulation process to performing spray drying to the water-based silicon carbide compound slurry; 3) adding the obtained silicon carbide granulation powder into an annular mold, and adopting prepressing and cold isostatic pressing end pressing two-step mode molding; 4) placing the obtained high-density sealed ring blank body into a vacuum non-pressure fritting furnace for sintering, to obtain the carbonaceous silicon carbide sealed ring. The invention also provides a carbonaceous silicon carbide sealed ring prepared by the above method, which has low friction coefficient, low wear rate, large bending strength, superior fracture toughness and other characteristics.
Description
Technical field
The bright a kind of carbonaceous silicon carbide sealed and preparation method thereof that relates to of we.
Background technique
Reveal, hang down specific (special) requirements such as wear extent, long lifetime, commentaries on classics distance and tracing ability in order to satisfy zero of mechanical seal, machinery sealing material must have thermal property, decay resistance and the tribological property etc. of high strength, high elastic modulus (rigidity), high hardness, excellence.Silicon carbide ceramics is a kind of machinery sealing material of novel, superior performance, and it is in light weight, specific strength is high, capability of resistance to radiation is strong, the hardness height, wear-resistant, group is good to performance, chemical stability height, corrosion-resistant, heat-conducting property is good, thermal shock resistance good.As machinery sealing material of new generation, silicon carbide ceramics has been defined as since metal, aluminium oxide, cemented carbide basic sealing material of the 4th generation in the world.But silicon carbide ceramics is not so good as graphite as machinery sealing material in self-lubricating property, causes its poor-performing of anti-the dry friction, has reduced its reliability to a certain extent, has limited its application in the special operation condition field.
Usually improve the dry friction performance of silicon carbide ceramics though have units such as in silicon carbide ceramics, adding nickel, titanium or graphite, but still have following problem:
1) adds the self lubricity that metal, graphite improve silicon carbide ceramics at present, mostly its matrix is silicon carbide reaction-sintered, because there are causes such as free silica, silica in silicon carbide reaction-sintered, ceramic combination property is not high, is progressively replaced by pressureless sintering silicon carbide.
2) because the difference of specific gravity of metal, graphite and silicon carbide is bigger, dispersal mechanism also is not quite similar, the mode that adopts conventional mechanical ball milling to mix is difficult to obtain the uniform composite powder of composition, cause silicon carbide ceramics to be not easy sintering, and microstructure is inhomogeneous, influences final mechanical property, frictional behaviour and wear rate.
3) graphite and metallic element are weak back phases with respect to silicon carbide, the intensity of the silicon carbide ceramics of metal-containing or graphite, fracture toughness all can decrease, how guaranteeing that silicon carbide ceramics obtains not reduce its mechanical property in the good dry friction performance, this becomes the major issue of puzzlement dry friction silicon carbide sealing material preparation.
Therefore, be necessary to develop a kind of method that can prepare the silicon carbide ceramic seal material of low coefficient of friction and wear rate,, guarantee the not obvious reduction of resistance to flexure, fracture toughness of this silicon carbide ceramics simultaneously to improve the self-lubricating property of silicon carbide mechanical seal ring.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of carbonaceous silicon carbide sealed and preparation method thereof, characteristic such as the silicon carbide sealed ring produced of method has low coefficient of friction, low wear rate thus, resistance to flexure is big, fracture toughness is good.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of carbonaceous silicon carbide sealed, with weight percentage is that 82%～90% silicon carbide powder, 8%～10% yttrium aluminum garnet and 2%～8% carbon dust are formed main material, may further comprise the steps successively:
1), above-mentioned main material, Bond, dispersing agent are joined in the deionized water, after ball milling mixes, is mixed with solid concentration and is 40%～60% water base silicon carbide compound slurry; The weight of Bond, dispersing agent is respectively 0.5%～3%, 0.5%～1.5% of main material;
2), adopt atomizing granulating technology that water base silicon carbide compound slurry is carried out spray drying, obtain silicon carbide granulating powder;
3), above-mentioned silicon carbide granulating powder put into ring mould adopt 140～180MPa dry-pressing precompressed and the moulding of 230～270MPa cold isostatic pressing end pressing two-step mode, obtain highdensity seal ring base substrate;
4), the seal ring base substrate of above-specified high density is put into vacuum non-pressure sintering furnace, be warming up to 1900 ℃～2000 ℃ insulations 1～1.5 hour, sintering finishes, and obtains carbonaceous silicon carbide sealed.
Improvement as the preparation method of carbonaceous silicon carbide sealed of the present invention: Bond is a polyvinyl alcohol, and dispersing agent is a TMAH.
Further improvement as the preparation method of carbonaceous silicon carbide sealed of the present invention: carbon dust is a plumbago.
Further improvement as the preparation method of carbonaceous silicon carbide sealed of the present invention: the spray-dired process conditions step 2) are: water base silicon carbide compound slurry flow is 3～5Kg/h, and the hot blast inlet temperature is 200 ℃～250 ℃.
Further improvement as the preparation method of carbonaceous silicon carbide sealed of the present invention: ball milling mixed 12～24 hours in the step 1).
Further improvement as the preparation method of carbonaceous silicon carbide sealed of the present invention: the size of grain of silicon carbide powder is 0.5 μ m～2.5 μ m, and the size of grain of carbon dust (plumbago) is 0.5 μ m～3.5 μ m.
Further improvement as the preparation method of carbonaceous silicon carbide sealed of the present invention: adopt 160MPa dry-pressing precompressed and 250MPa cold isostatic pressing end pressing in the step 3).
In the preparation method of carbonaceous silicon carbide sealed of the present invention: the outlet temperature step 2) is generally 70 ℃～80 ℃.Solid concentration is that 40%～60% water base silicon carbide slip is meant: (main material) ÷ (main material+Bond+dispersing agent+deionized water)=40%～60%, above-mentioned percentage is weight percentage.
Carbonaceous silicon carbide sealed of the present invention can be according to the required special mould of putting into the different-diameter size of reality, thereby obtains the seal ring of different size.
The present invention also provides prepared according to the method described above carbonaceous silicon carbide sealed simultaneously.
The carbonaceous silicon carbide sealed of the present invention's preparation has the following advantages:
1) introduced the superior graphite of self-lubricating property after, the dry friction performance of carbonaceous silicon carbide sealed obviously improves, its friction factor is 0.1～0.2.
2) adopt aqueous slurries and spray granulation, graphite being evenly distributed in silicon carbide substrate helps to improve the self lubricity of silicon carbide.
3) adopt yttrium aluminum garnet as sintering aid, not only reduced the sintering temperature of seal ring, but also overcome the problem that graphite brings silicon carbide ceramics sintering variation;
4) carbonaceous silicon carbide sealed of the present invention, its body is close to be 3.15～3.20g/cm
3, hardness is 90～91HRA, and resistance to flexure is 400～450MPa, and fracture toughness is 3.5～4.0MPam
1/2
In sum, carbonaceous silicon carbide sealed of the present invention can be when improving self-lubricating property, also guaranteed that performances such as resistance to flexure, fracture toughness are equal to carbon-free conventional seal ring substantially.
Embodiment
The preparation method of embodiment 1, a kind of carbonaceous silicon carbide sealed, silicon carbide powder, yttrium aluminum garnet, plumbago are mixed with main material in proportion, the prescription of this main material is formed and weight percentage is: 82% silicon carbide powder, 10% yttrium aluminum garnet and 8% plumbago, the size of grain 1.75 μ m of this silicon carbide powder, the size of grain 1.8 μ m of plumbago, carry out following steps successively:
1), the polyvinyl alcohol of above-mentioned main material, main material weight 3%, the TMAH of main material weight 1.5% are joined in the deionized water, ball milling mixed 24 hours, was mixed with the solid phase weight content and is 40% water base silicon carbide compound slurry;
I.e. (main material) ÷ (main material+polyvinyl alcohol+TMAH+deionized water)=40% (weight ratio).
2), adopt atomizing granulating technology that water base silicon carbide compound slurry is carried out spray drying, concrete process conditions are: water base silicon carbide slip flow is 5Kg/h, and the hot blast inlet temperature is 220 ℃, 80 ℃ of outlet temperatures; Get silicon carbide granulating powder;
3), above-mentioned silicon carbide granulating powder put into ring mould adopt 160MPa dry-pressing precompressed and the moulding of 250MPa cold isostatic pressing end pressing two-step mode, obtain highdensity seal ring base substrate;
4), the seal ring base substrate of above-specified high density is put into vacuum non-pressure sintering furnace, be warming up to 2000 ℃ of insulations 1.0 hours; Sintering finishes, and gets carbonaceous silicon carbide sealed.
Its friction factor is 0.1, and volume density is 3.15g/cm
3, hardness is 90HRA, and resistance to flexure is 410MPa, and fracture toughness is 3.6MPam
1/2
Embodiment 2: a kind of preparation method of carbonaceous silicon carbide sealed, silicon carbide powder, yttrium aluminum garnet, plumbago are mixed with main material in proportion, the prescription of this main material is formed and weight percentage is: 90% silicon carbide powder, 8% yttrium aluminum garnet and 2% plumbago, the size of grain 1.75 μ m of this silicon carbide powder, the size of grain 1.8 μ m of plumbago, carry out following steps successively:
1), the polyvinyl alcohol of above-mentioned main material, main material weight 0.5%, the TMAH of main material weight 0.5% are joined in the deionized water, ball milling mixed 12 hours, was mixed with the solid phase weight content and is 60% water base silicon carbide slip;
I.e. (main material) ÷ (main material+polyvinyl alcohol+TMAH+deionized water)=60% (weight ratio).
2), adopt atomizing granulating technology that water base silicon carbide slip is carried out spray drying, concrete process conditions are: water base silicon carbide slip flow is 3Kg/h, and the hot blast inlet temperature is 220 ℃, 80 ℃ of outlet temperatures; Get silicon carbide granulating powder;
3), above-mentioned silicon carbide granulating powder put into ring mould adopt 160MPa dry-pressing precompressed and the moulding of 250MPa cold isostatic pressing end pressing two-step mode, obtain highdensity silicon carbide biscuit;
4), the seal ring base substrate of above-specified high density is placed in the vacuum non-pressure sintering furnace, be warming up to 1900 ℃ of insulations 1.5 hours; Sintering finishes, and gets carbonaceous silicon carbide sealed.
Its friction factor is 0.15, and body is close to be 3.20g/cm
3, hardness is 91HRA, and resistance to flexure is 450MPa, and fracture toughness is 4.0MPam
1/2
Embodiment 3: a kind of preparation method of carbonaceous silicon carbide sealed, silicon carbide powder, yttrium aluminum garnet, plumbago are mixed with main material in proportion, the prescription of this main material is formed and weight percentage is: 87% silicon carbide powder, 8% yttrium aluminum garnet and 5% plumbago, the size of grain 1.3 μ m of this silicon carbide powder, the size of grain 2 μ m of plumbago, carry out following steps successively:
1), the polyvinyl alcohol of above-mentioned main material, main material weight 1.2%, the TMAH of main material weight 1.2% are joined in the deionized water, ball milling mixed 16 hours, was mixed with the solid phase weight content and is 50% water base silicon carbide slip;
I.e. (main material) ÷ (main material+polyvinyl alcohol+TMAH+deionized water)=50% (weight ratio).
2), adopt atomizing granulating technology that water base silicon carbide slip is carried out spray drying, concrete process conditions are: water base silicon carbide slip flow is 4Kg/h, and the hot blast inlet temperature is 240 ℃, 80 ℃ of outlet temperatures; Get silicon carbide granulating powder;
3), above-mentioned silicon carbide granulating powder put into ring mould adopt 160MPa dry-pressing precompressed and the moulding of 250MPa cold isostatic pressing end pressing two-step mode, obtain highdensity silicon carbide biscuit;
4), the seal ring base substrate of above-specified high density is placed in the vacuum non-pressure sintering furnace, be warming up to 1950 ℃ of insulations 1.0 hours; Sintering finishes, and gets carbonaceous silicon carbide sealed.
Its friction factor is 0.13, and body is close to be 3.18g/cm
3, hardness is 91HRA, and resistance to flexure is 430MPa, and fracture toughness is 3.8MPam
1/2
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (8)
1, a kind of preparation method of carbonaceous silicon carbide sealed is characterized in that with weight percentage being that 82%～90% silicon carbide powder, 8%～10% yttrium aluminum garnet and 2%～8% carbon dust are formed main material, may further comprise the steps successively:
1), above-mentioned main material, Bond, dispersing agent are joined in the deionized water, after ball milling mixes, is mixed with solid concentration and is 40%～60% water base silicon carbide compound slurry; The weight of described Bond, dispersing agent is respectively 0.5%～3%, 0.5%～1.5% of main material;
2), adopt atomizing granulating technology that water base silicon carbide compound slurry is carried out spray drying, obtain silicon carbide granulating powder;
3), above-mentioned silicon carbide granulating powder put into ring mould adopt 140～180MPa dry-pressing precompressed and the moulding of 230～270MPa cold isostatic pressing end pressing two-step mode, obtain highdensity seal ring base substrate;
4), the seal ring base substrate of above-specified high density is put into vacuum non-pressure sintering furnace, be warming up to 1900 ℃～2000 ℃ insulations 1～1.5 hour, sintering finishes, and obtains carbonaceous silicon carbide sealed.
2, the preparation method of carbonaceous silicon carbide sealed according to claim 1 is characterized in that: described Bond is a polyvinyl alcohol, and described dispersing agent is a TMAH.
3, the preparation method of carbonaceous silicon carbide sealed according to claim 1 and 2 is characterized in that: described carbon dust is a plumbago.
4, the preparation method of carbonaceous silicon carbide sealed according to claim 3, it is characterized in that: the spray-dired process conditions described step 2) are: water base silicon carbide compound slurry flow is 3～5Kg/h, and the hot blast inlet temperature is 200 ℃～250 ℃.
5, the preparation method of carbonaceous silicon carbide sealed according to claim 4 is characterized in that: ball milling mixed 12～24 hours in the described step 1).
6, the preparation method of carbonaceous silicon carbide sealed according to claim 5 is characterized in that: the size of grain of described silicon carbide powder is 0.5 μ m～2.5 μ m, and the size of grain of carbon dust is 0.5 μ m～3.5 μ m.
7, the preparation method of carbonaceous silicon carbide sealed according to claim 6 is characterized in that: adopt 160MPa dry-pressing precompressed and 250MPa cold isostatic pressing end pressing in the described step 3).
8, according to the prepared carbonaceous silicon carbide sealed of any one method in the claim 1～7.
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| CNA2009100988759A CN101551012A (en) | 2009-05-21 | 2009-05-21 | A carbonaceous silicon carbide sealed ring and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104987076A (en) * | 2015-06-17 | 2015-10-21 | 宁波东联密封件有限公司 | High-toughness silicon carbide ceramic and low-temperature sintering technology thereof |
| CN106064946A (en) * | 2016-05-31 | 2016-11-02 | 台州东新密封有限公司 | Mechanical seal SiC/ graphite diphase ceramic material and preparation method thereof |
| CN104505990B (en) * | 2014-09-15 | 2017-02-15 | 横店集团东磁股份有限公司 | Preparation method for sintering permanent magnetic ferrite ring of brushless motor |
| CN108546128A (en) * | 2018-05-19 | 2018-09-18 | 奉化市飞固凯恒密封工程有限公司 | A kind of silicon carbide ceramics non-pressure sintering technology |
| CN114043763A (en) * | 2021-09-17 | 2022-02-15 | 大同新成新材料股份有限公司 | Forming method of isostatic pressing small graphite block |
-
2009
- 2009-05-21 CN CNA2009100988759A patent/CN101551012A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104505990B (en) * | 2014-09-15 | 2017-02-15 | 横店集团东磁股份有限公司 | Preparation method for sintering permanent magnetic ferrite ring of brushless motor |
| 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 |
| CN104987076A (en) * | 2015-06-17 | 2015-10-21 | 宁波东联密封件有限公司 | High-toughness silicon carbide ceramic and low-temperature sintering technology thereof |
| CN106064946A (en) * | 2016-05-31 | 2016-11-02 | 台州东新密封有限公司 | Mechanical seal SiC/ graphite diphase ceramic material and preparation method thereof |
| CN108546128A (en) * | 2018-05-19 | 2018-09-18 | 奉化市飞固凯恒密封工程有限公司 | A kind of silicon carbide ceramics non-pressure sintering technology |
| CN108546128B (en) * | 2018-05-19 | 2020-11-20 | 奉化市飞固凯恒密封工程有限公司 | Silicon carbide ceramic pressureless sintering process |
| CN114043763A (en) * | 2021-09-17 | 2022-02-15 | 大同新成新材料股份有限公司 | Forming method of isostatic pressing small graphite block |
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Application publication date: 20091007 |