CN106064946A - Mechanical seal SiC/ graphite diphase ceramic material and preparation method thereof - Google Patents
Mechanical seal SiC/ graphite diphase ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of mechanical seal SiC/ graphite diphase ceramic material, comprise the following steps: with silicon carbide powder 100 parts, boron carbide 0.1 part～1 part, graphite powder 5 parts～30 parts, binding agent 0.5 part～15 parts, pressing aid lubricant 0.5 part～5 parts, 0.5 part～1.5 parts constitutive materials of dispersant；The ball milling that adds water raw material mixes, and is configured to the water base silicon carbide compound slurry that solid phase weight content is 40%～60%；Slurry is spray-dried, the graphitiferous silicon carbide granulating powder forming processes of gained, and the base substrate of gained is placed in vacuum non-pressure sintering furnace, it is warming up to 2000 DEG C～2100 DEG C, it is incubated 1 hour～1.5 hours, after terminating, obtain mechanical seal SiC/ graphite diphase ceramic material.
Description
Technical field
The present invention relates to a kind of mechanical seal SiC/ graphite diphase ceramic material and preparation method thereof.
Background technology
In order to meet the particular/special requirements such as the zero leakage of mechanical seal, low abrasion amount, long-life, machinery sealing material must have
Have high intensity, high elastic modulus, high rigidity, excellent thermal property and decay resistance etc..Silicon carbide ceramics is a kind of novel
The machinery sealing material of superior performance, it is lightweight, intensity is high, capability of resistance to radiation is strong；There is certain self lubricity, friction system
Number is low；Hardness is high, wear-resistant, group is good to performance；Chemical stability is high, corrosion-resistant；Heat conductivility is excellent, thermal shock resistance
Good.As a new generation's machinery sealing material, carborundum has been confirmed as since metal, aluminum oxide, hard alloy the in the world
Four generation materials substantially sealed off.But silicon carbide ceramics is not so good as graphite as machinery sealing material in self-lubricating property, cause it resistance to dry
Frictional behaviour is poor, reduces its reliability to a certain extent, limits its application in special operation condition field.
Although the existing dry friction adding the units such as nickel, titanium or graphite usually to improve silicon carbide ceramics in silicon carbide ceramics
Can, but still there is problems in that
(1) being currently fed metal, graphite to improve the self lubricity of silicon carbide ceramics, its matrix mostly is reaction-sintered carbonization
Silicon, owing to there is the reason such as free silica, silica in silicon carbide reaction-sintered, pottery combination property is not high, progressively by nothing
Pressure sintered silicon carbon is replaced.
(2) owing to metal, graphite are relatively big with the difference of specific gravity of carborundum, dispersal mechanism is also not quite similar, and uses routine
The mode of machinery ball milling mixing is difficult to obtain the uniform composite granule of composition, causes ceramic post sintering not fine and close, and affects final
Mechanical property.
(3) graphite and metallic element are weak phase for carborundum, contain metal or graphitic carbon SiClx pottery intensity,
Fracture toughness all can decrease.Do not reduce its mechanical energy while how guaranteeing that silicon carbide ceramics obtains good dry friction performance
Power, this becomes major issue prepared by a puzzlement dry friction carborundum encapsulant.
Therefore, it is necessary to exploitation mechanical seal SiC/ graphite diphase ceramic material, to improve carborundum mechanical seal material
The self-lubricating property of material, guarantees that the bending strength of thyrite, fracture toughness can not substantially reduce simultaneously.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of mechanical seal SiC/ graphite diphase ceramic material and system thereof
Preparation Method, the material mixture ratio of gained of the present invention is reasonable, has low-friction coefficient, low wear rate, bending strength is big, fracture toughness is excellent
The characteristic such as good.
In order to solve above-mentioned technical problem, the present invention provides the system of a kind of mechanical seal SiC/ graphite diphase ceramic material
Preparation Method, comprises the following steps:
(1), by silicon carbide powder 100 parts, boron carbide 0.1 part～1 part, graphite powder 5 parts～30 parts, binding agent 0.5 part～
15 parts, pressing aid lubricant 0.5 part～5 parts, 0.5 part～1.5 parts constitutive materials of dispersant；Above-mentioned part is mass parts；
Add after raw material is uniformly mixed to deionized water, after ball milling mixes 12 hours～24 hours, be configured to solid phase
Weight content is the water base silicon carbide compound slurry of 40%～60%；
Solid phase weight content refers to: (raw material) ÷ (raw material+deionized water)=40%～60%, above-mentioned percentage is weight
Percentage；
(2), use atomizing granulating technology to be spray-dried above-mentioned water base silicon carbide compound slurry, obtain graphitiferous carbon
SiClx pelletizing；
(3) the two of 120MPa dry-pressing precompressed and 200Mpa cold isostatic pressing end pressing is used to above-mentioned graphitiferous silicon carbide granulating powder
Step mode is molded, it is thus achieved that highdensity SiC/ graphite complex phase ceramic base substrate；
(4) it is placed on the encapsulant base substrate of above-specified high density in vacuum non-pressure sintering furnace, be warming up to 2000 DEG C～2100
DEG C, it is incubated 1 hour～1.5 hours, after terminating, obtain mechanical seal SiC/ graphite diphase ceramic material.
Improvement as the mechanical seal of the present invention preparation method with SiC/ graphite diphase ceramic material:
Described step 1) in:
Binding agent is polyvinyl alcohol；
Pressing aid lubricant is polyoxyethylene, it may be assumed that PEO, poly (ethylene oxide), PEO；
Dispersant is amino alcohol, polyvinylpyrrolidone, TMAH.
Improvement further as the mechanical seal of the present invention preparation method with SiC/ graphite diphase ceramic material:
Described step 2) mist projection granulating: hot wind inlet temperature is 200 DEG C～230 DEG C；Outlet temperature is at 80～120 DEG C.
The present invention provides the mechanical seal utilizing said method to be prepared SiC/ graphite complex phase ceramic material also simultaneously
Material.
The silicon carbide ceramics that employing method is produced has that low-friction coefficient, low wear rate, bending strength be big, fracture toughness
The characteristic such as excellent.
Mechanical seal SiC/ graphite complex phase ceramic of the present invention and preparation method thereof, has the advantage that
(1) SiC/ graphite complex phase ceramic sealing material, reasonable mixture ratio, low-friction coefficient, low wear rate can be made it have, resist
The characteristics such as curved intensity is big, fracture toughness is excellent, bulk density is 2.65g/cm3～2.95g/cm3, and hardness HRA is 88～91, anti-
Curved intensity is 210MPa～280MPa, and elastic modelling quantity is 230GPa～270GPa.
(2) after introducing the superior graphite powder of self-lubricating property, the dry friction performance of SiC/ graphite complex phase ceramic sealing material
Substantially being improved, its coefficient of friction is only 0.01～0.02.
(3) preparation method uses water base silicon carbide slurry and spray granulation, makes graphite powder equal in silicon carbide substrate
Even distribution, is favorably improved the self lubricity of carborundum.
(4) use boron carbide as sintering aid, not only reduce the sintering temperature of encapsulant, but also overcome stone
Ink powder brings the problem of degradation after silicon carbide ceramics sintering.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
Embodiment 1:
A kind of SiC/ graphite complex phase ceramic sealing material, silicon carbide powder is matrix, carborundum powder, boron carbide and graphite powder
For main material, each constituent mass proportioning is: silicon carbide powder 100Kg, boron carbide 1Kg, graphite powder 30Kg, gathering as binding agent
Vinyl alcohol 3Kg, as the polyoxyethylene 0.5kg of pressing aid lubricant, dispersant 1.5Kg.
Dispersant be following any one: amino alcohol, polyvinylpyrrolidone, TMAH.
Embodiment 2:
A kind of SiC/ graphite complex phase ceramic sealing material, silicon carbide powder is matrix, carborundum powder, boron carbide and graphite powder
For main material, each constituent mass proportioning is: silicon carbide powder 100Kg, boron carbide 0.1Kg, graphite powder 5Kg, as binding agent
Polyvinyl alcohol is 0.5Kg, as the polyoxyethylene 5kg of pressing aid lubricant, dispersant 0.5Kg.
Dispersant be following any one: amino alcohol, polyvinylpyrrolidone, TMAH.
Embodiment 3:
A kind of SiC/ graphite complex phase ceramic sealing material, silicon carbide powder is matrix, carborundum powder, boron carbide and graphite powder
For main material, each constituent mass proportioning is: silicon carbide powder 100Kg, boron carbide 0.55Kg, graphite powder 17.5Kg, as bonding
The polyvinyl alcohol of agent is 1.75Kg, as the polyoxyethylene 3kg of pressing aid lubricant, dispersant 1Kg.
Dispersant be following any one: amino alcohol, polyvinylpyrrolidone, TMAH.
Embodiment 4:
A kind of SiC/ graphite complex phase ceramic sealing material, silicon carbide powder is matrix, carborundum powder, boron carbide and graphite powder
For main material, each constituent mass proportioning is: silicon carbide powder 100Kg, boron carbide 0.5Kg, graphite powder 20Kg, as binding agent
Polyvinyl alcohol is 1Kg, as the polyoxyethylene 2.5kg of pressing aid lubricant, dispersant 1.2Kg.
Dispersant be following any one: amino alcohol, polyvinylpyrrolidone, TMAH.
Embodiment 5:
A kind of SiC/ graphite complex phase ceramic sealing material, silicon carbide powder is matrix, carborundum powder, boron carbide and graphite powder
For main material, each constituent mass proportioning is: silicon carbide powder 100Kg, boron carbide 0.8Kg, graphite powder 10Kg, as binding agent
Polyvinyl alcohol is 0.8Kg, as the polyoxyethylene 1.5kg of pressing aid lubricant, dispersant 0.9Kg.
Dispersant be following any one: amino alcohol, polyvinylpyrrolidone, TMAH.
Embodiment 6:
A kind of SiC/ graphite complex phase ceramic sealing material, silicon carbide powder is matrix, carborundum powder, boron carbide and graphite powder
For main material, each constituent mass proportioning is: silicon carbide powder 100Kg, boron carbide 0.2Kg, graphite powder 6Kg, as binding agent
Polyvinyl alcohol is 0.6Kg, as the polyoxyethylene 1.2kg of pressing aid lubricant, dispersant 0.6Kg.
Dispersant be following any one: amino alcohol, polyvinylpyrrolidone, TMAH.
Embodiment 7:
A kind of SiC/ graphite complex phase ceramic sealing material, silicon carbide powder is matrix, carborundum powder, boron carbide and graphite powder
For main material, each constituent mass proportioning is: silicon carbide powder 100Kg, boron carbide 0.9Kg, graphite powder 29Kg, as binding agent
Polyvinyl alcohol is 2.9Kg, as the polyoxyethylene 4.9kg of pressing aid lubricant, dispersant 1.4Kg.
Dispersant be following any one: amino alcohol, polyvinylpyrrolidone, TMAH.
The preparation method of embodiment the 8th, a kind of SiC/ graphite complex phase ceramic sealing material is (according to embodiment 1～embodiment 7 institute
The formula stated), follow the steps below successively:
(1) add after silicon carbide powder, boron carbide, graphite powder, binding agent, pressing aid lubricant, dispersant proportioning in proportion
Entering in deionized water, after ball milling mixes 12 hours, being configured to solid phase mass content is 40% water base graphitiferous silicon carbide compound
Slurry；
(2) atomizing granulating technology is used to carry out spray granulating and drying to above water base graphitiferous silicon carbide compound slurry,
To graphitiferous silicon carbide granulating powder；Hot wind inlet temperature is 200 DEG C, and outlet temperature is 80 DEG C；
(3) two step sides of 120MPa dry-pressing precompressed and 200MPa isostatic cool pressing are used to above-mentioned graphitiferous silicon carbide granulating powder
Formula is molded, it is thus achieved that highdensity encapsulant base substrate；
(4) being placed on above-specified high density encapsulant base substrate in vacuum non-pressure sintering furnace, being warming up to 2000 DEG C, insulation 1 is little
When, after terminating, obtain SiC/ graphite complex phase ceramic sealing material.
The preparation method of embodiment the 9th, a kind of SiC/ graphite complex phase ceramic sealing material is (according to embodiment 1～embodiment 7 institute
The formula stated), follow the steps below successively:
(1) add after silicon carbide powder, boron carbide, graphite powder, binding agent, pressing aid lubricant, dispersant proportioning in proportion
Entering in deionized water, after ball milling mixes 12 hours, being configured to solid phase mass content is 40% water base silicon carbide compound slurry；
(2) use atomizing granulating technology to carry out spray granulating and drying to above water base silicon carbide compound slurry, obtain carbonization
Silicon pelletizing；Hot wind inlet temperature is 230 DEG C, and outlet temperature is 120 DEG C；
(3) 120MPa dry-pressing precompressed is used to become with the two step approach of 200MPa isostatic cool pressing above-mentioned silicon carbide granulating powder
Type, it is thus achieved that highdensity encapsulant base substrate；
(4) being placed on above-specified high density encapsulant base substrate in vacuum non-pressure sintering furnace, being warming up to 2100 DEG C, insulation 1 is little
When, obtain SiC/ graphite complex phase ceramic sealing material after terminating.
The preparation method of embodiment the 10th, a kind of SiC/ graphite complex phase ceramic sealing material is (according to embodiment 1～embodiment 7
Described formula), follow the steps below successively:
(1) add after silicon carbide powder, boron carbide, graphite powder, binding agent, pressing aid lubricant, dispersant proportioning in proportion
Entering in deionized water, after ball milling mixes 12 hours, being configured to solid phase mass content is 40% water base silicon carbide compound slurry；
(2) use atomizing granulating technology to carry out spray granulating and drying to above water machine silicon carbide compound slurry, obtain carbonization
Silicon pelletizing；Hot wind inlet temperature is 225 DEG C；Outlet temperature is 110 DEG C；
(3) 120MPa dry-pressing precompressed is used to become with the two step approach of 200MPa isostatic cool pressing above-mentioned silicon carbide granulating powder
Type, it is thus achieved that highdensity encapsulant base substrate；
(4) being placed on above-specified high density encapsulant base substrate in vacuum non-pressure sintering furnace, being warming up to 2050 DEG C, insulation 1 is little
When, obtain SiC/ graphite complex phase ceramic sealing material after terminating.
The preparation method of embodiment the 11st, a kind of SiC/ graphite complex phase ceramic sealing material, follows the steps below successively:
(1) by silicon carbide powder 100kg, boron carbide 1kg, graphite powder 30kg, polyvinyl alcohol 3kg, polyoxyethylene 0.5kg,
Amino alcohol 1.5kg, joins in deionized water, and after ball milling mixes 24 hours, being configured to solid phase mass content is 40% water base carbon
SiClx composite mortar；
(2) use atomizing granulating technology to carry out spray granulating and drying to above water base silicon carbide compound slurry, obtain containing stone
Ink silicon carbide granulating powder；Hot wind inlet temperature is 220 DEG C, and outlet temperature is 110 DEG C；
(3) 120MPa dry-pressing precompressed is used to become with the two step approach of 200MPa isostatic cool pressing above-mentioned silicon carbide granulating powder
Type, it is thus achieved that highdensity encapsulant base substrate；
(4) being placed on above-specified high density encapsulant base substrate in vacuum non-pressure sintering furnace, being warming up to 2000 DEG C, insulation 1 is little
When, obtain SiC/ graphite complex phase ceramic sealing material after terminating.
SiC/ graphite diphase ceramic material coefficient of friction is 0.01, and bulk density is 2.65g/cm3, hardness is 89HRA, anti-
Curved intensity 220MPa, elastic modelling quantity 240GPa.
The preparation method of embodiment the 12nd, a kind of SiC/ graphite complex phase ceramic sealing material, follows the steps below successively:
(1) by silicon carbide powder 100kg, boron carbide 0.1kg, graphite powder 5kg, polyvinyl alcohol 0.5kg, polyoxyethylene 5kg,
Amino alcohol 0.5kg, joins in deionized water, and after ball milling mixes 12 hours, being configured to solid phase mass content is 60% water base carbon
SiClx composite mortar；
(2) use atomizing granulating technology to carry out spray granulating and drying to above water base silicon carbide compound slurry, obtain containing stone
Ink silicon carbide granulating powder；Hot wind inlet temperature is 220 DEG C, and outlet temperature is 110 DEG C；
(3) two step sides of 120MPa dry-pressing precompressed and 200MPa isostatic cool pressing are used to above-mentioned graphitiferous silicon carbide granulating powder
Formula is molded, it is thus achieved that highdensity encapsulant base substrate；
(4) it is placed on above-specified high density encapsulant base substrate in vacuum non-pressure sintering furnace, is warming up to 2000 DEG C, be incubated 1.5
Hour, obtain SiC/ graphite complex phase ceramic sealing material after terminating.
SiC/ graphite complex phase ceramic sealing material coefficient of friction is 0.02, and bulk density is 2.91g/cm3, hardness is
91HRA, bending strength 255MPa, elastic modelling quantity 270GPa.
The preparation method of embodiment the 13rd, a kind of SiC/ graphite complex phase ceramic sealing material, comprises the following steps successively:
(1) by silicon carbide powder 100kg, boron carbide 0.15kg, graphite powder 15kg, polyvinyl alcohol 1.2kg, polyoxyethylene
1.5kg, amino alcohol 1.2kg, join in deionized water, and ball milling mixed after 16 hours, and it is 40% water base for being configured to solid concentration
Silicon carbide compound slurry；
(2) use atomizing granulating technology to carry out spray granulating and drying to above water base silicon carbide compound slurry, obtain containing stone
Ink silicon carbide granulating powder；Hot wind inlet temperature is 220 DEG C, and outlet temperature is 110 DEG C；
(3) two step sides of 120MPa dry-pressing precompressed and 200MPa isostatic cool pressing are used to above-mentioned graphitiferous silicon carbide granulating powder
Formula is molded, it is thus achieved that highdensity encapsulant base substrate；
(4) being placed on above-specified high density encapsulant base substrate in vacuum non-pressure sintering furnace, being warming up to 2050 DEG C, insulation 1 is little
When, obtain SiC/ graphite complex phase ceramic sealing material after terminating.
Graphitiferous carborundum composite-phase ceramic material friction coefficient is 0.015, and bulk density is 2.86g/cm3, hardness is
91HRA, bending strength 240MPa, elastic modelling quantity 250GPa.
The 14th, embodiment makes the amino alcohol in embodiment 12 into polyvinylpyrrolidone, and weight is constant；Remaining is equal to reality
Execute example 12.
SiC/ graphite complex phase ceramic sealing material coefficient of friction is 0.02, and hardness is 90HRA, bending strength 250MPa, bullet
Property modulus 260GPa.
The 15th, embodiment makes the amino alcohol in embodiment 12 into TMAH, and weight is constant；Remaining is equal to reality
Execute example 12.
SiC/ graphite complex phase ceramic sealing material coefficient of friction is 0.02, and hardness is 91HRA, bending strength 255MPa, bullet
Property modulus 265GPa.
It is finally noted that, above citing is only several instantiations of the present invention.Obviously, the present invention does not limits
In above example, can also have many deformation.Those of ordinary skill in the art directly can derive from present disclosure
Or associate all of deformation, it is all considered as protection scope of the present invention.
Claims (4)
1. the mechanical seal preparation method of SiC/ graphite diphase ceramic material, it is characterised in that comprise the following steps:
(1), with silicon carbide powder 100 parts, boron carbide 0.1 part～1 part, graphite powder 5 parts～30 parts, binding agent 0.5 part～15 parts,
Pressing aid lubricant 0.5 part～5 parts, 0.5 part～1.5 parts constitutive materials of dispersant；Above-mentioned part is mass parts；
Add after raw material is uniformly mixed to deionized water, after ball milling mixes 12 hours～24 hours, be configured to solid phase weight
Content is the water base silicon carbide compound slurry of 40%～60%；
(2), use atomizing granulating technology to be spray-dried above-mentioned water base silicon carbide compound slurry, obtain graphitiferous carborundum
Pelletizing；
(3) two step sides of 120MPa dry-pressing precompressed and 200Mpa cold isostatic pressing end pressing are used to above-mentioned graphitiferous silicon carbide granulating powder
Formula is molded, it is thus achieved that highdensity SiC/ graphite complex phase ceramic base substrate；
(4) it is placed on the encapsulant base substrate of above-specified high density in vacuum non-pressure sintering furnace, is warming up to 2000 DEG C～2100 DEG C, protect
Temperature 1 hour～1.5 hours, after terminating, obtains mechanical seal SiC/ graphite diphase ceramic material.
2. the preparation method of mechanical seal SiC/ graphite diphase ceramic material according to claim 1, it is characterised in that:
Described step 1) in:
Binding agent is polyvinyl alcohol；
Pressing aid lubricant is polyoxyethylene；
Dispersant is amino alcohol, polyvinylpyrrolidone, TMAH.
3. the preparation method of mechanical seal SiC/ graphite diphase ceramic material according to claim 2, it is characterised in that:
Described step 2) mist projection granulating: hot wind inlet temperature is 200 DEG C～230 DEG C；Outlet temperature is at 80～120 DEG C.
4. utilize the mechanical seal SiC/ graphite complex phase ceramic material that the method as described in claims 1 to 3 is arbitrary is prepared
Material.
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| CN111138200A (en) * | 2020-01-11 | 2020-05-12 | 浙江东新新材料科技有限公司 | Multiphase composite reinforced low-friction silicon carbide ceramic sealing material and preparation method thereof |
| CN111333428A (en) * | 2020-03-31 | 2020-06-26 | 西安鑫垚陶瓷复合材料有限公司 | Ceramic matrix composite elastic sealing element and forming process thereof |
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| CN116768630A (en) * | 2023-05-22 | 2023-09-19 | 铜陵优必胜新材料科技有限公司 | Preparation method of microporous carbon-containing silicon carbide sealing element |
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| CN112778014A (en) * | 2021-01-12 | 2021-05-11 | 罗焕焕 | High-performance silicon carbide ceramic material and preparation method thereof |
| CN116768630A (en) * | 2023-05-22 | 2023-09-19 | 铜陵优必胜新材料科技有限公司 | Preparation method of microporous carbon-containing silicon carbide sealing element |
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Effective date of registration: 20181101 Address after: 317015 No. 1, 12 road, Beiyang Industrial Park, Shang pan Town, Taizhou, Zhejiang. Applicant after: Zhejiang Xinxin Mstar Technology Ltd Address before: 317015 No. 1, 12 road, Beiyang Industrial Park, Taizhou, Zhejiang. Applicant before: TAIZHOU DONGXIN SEALS CO., LTD. |
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