CN102030533A - Low-friction-factor silicon carbide ceramic sealing element and preparation method thereof - Google Patents

Low-friction-factor silicon carbide ceramic sealing element and preparation method thereof Download PDF

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CN102030533A
CN102030533A CN 201010538042 CN201010538042A CN102030533A CN 102030533 A CN102030533 A CN 102030533A CN 201010538042 CN201010538042 CN 201010538042 CN 201010538042 A CN201010538042 A CN 201010538042A CN 102030533 A CN102030533 A CN 102030533A
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silicon carbide
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carbide ceramic
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CN102030533B (en
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杨辉
郭兴忠
张冬梅
郑志荣
高黎华
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a low-friction-factor silicon carbide ceramic sealing element which is prepared from a main raw material, polyvinyl alcohol and tetramethyl ammonium hydroxide, wherein the main raw material comprises 65-75% of silicon carbide, 5-10% of boron nitride, 5-10% of fluoridized graphite, 5-10% of molybdenum disulfide and 10% of yttrium aluminium garnet; the polyvinyl alcohol accounts for 2.5-3.5 wt% of the main raw material; and the tetramethyl ammonium hydroxide accounts for 1.5-2.5 wt% of the main raw material. The preparation method comprises the following steps: (1) carrying out ball milling to mix the main raw material, polyvinyl alcohol, tetramethyl ammonium hydroxide and deionized water; (2) carrying out spray granulation on the obtained slurry; (3) putting the obtained granules in a mold, and carrying out dry pressing for primary molding; and (4) carrying out pressureless liquid-phase sintering on the obtained blank to obtain the low-friction-factor silicon carbide ceramic sealing element. The sealing element has the advantages of low friction factor, favorable thermal properties and favorable mechanical properties.

Description

Silicon carbide ceramic seal spare of low-friction coefficient and preparation method thereof
Technical field
The present invention relates to a kind of silicon carbide ceramic seal spare and preparation method thereof.
Background technology
Silicon carbide (SiC) pottery is a kind of stupalith of typical covalent bonds, C and Si bond distance in the SiC crystalline structure, covalency is strong, lattice imperfection is little, and this covalent bonding feature makes that silicon carbide ceramics has that hot strength is big, high temperature creep is little, hardness is high, wear-resisting, corrosion-resistant, anti-oxidant, high heat conductance and characteristics such as high conductivity and Heat stability is good; Obtained a large amount of application in high-tech sectors such as machinery, chemical industry, the energy, military projects.For example, as high temperature, wear-resisting, corrosion-resistant mechanical seal parts, various emery wheels and mould.
Silicon carbide ceramics has obtained using widely as sealing material of new generation at present, but silicon carbide ceramics does not have self-lubricated function, therefore, when the hard but not self-lubricating material of silicon carbide ceramic seal spare and another contacts when producing relative movement, if there is not lubricating fluid, easy inefficacy causes the generation of accident because frictional coefficient is very big in meeting.At publication number is in the patent of CN101255330A, carborundum powder with 90~96%, 2~8% Graphite Powder 99 and 2~5% polyvinyl alcohol constitutive material, promptly, reduced dry friction coefficient to a certain extent by adding C, pore-creating, but sacrificed its mechanical property, and along with the increase of C content, the mechanical property of the formation material of micropore obviously descends.Therefore, needing to seek reasonably, prescription makes the silicon carbide ceramic seal spare that has good lubricity and mechanical property concurrently with sintering schedule.At publication number is in the patent of CN101551012A, informs carborundum powder with 82~90%, 2~8% carbon dust and 8~10% yttrium aluminum garnet constitutive material; But it exists the defective that lubricity and mechanical property have much room for improvement too.
Summary of the invention
The technical problem to be solved in the present invention provides silicon carbide ceramic seal spare of a kind of low-friction coefficient and preparation method thereof, the sealing part not only has lower frictional coefficient but also has good thermal property and mechanical property, thereby guarantees its safe reliability as sealing material.
In order to solve the problems of the technologies described above, the invention provides a kind of silicon carbide ceramic seal spare of low-friction coefficient, the sealing part is by main raw material, form as the polyvinyl alcohol of binding agent with as the Tetramethylammonium hydroxide of dispersion agent, and main raw material is grouped into by the one-tenth of following weight content: 65%~75% silicon carbide (SiC), 5%~10% boron nitride (BN), 5%~10% fluorographite, 5~10% molybdenumdisulphide (MoS 2) and 10% yttrium aluminum garnet; Polyvinyl alcohol accounts for 2.5~3.5% of main raw material gross weight, and Tetramethylammonium hydroxide accounts for 1.5~2.5% of main raw material gross weight.
The present invention also provides the preparation method of the silicon carbide ceramic seal spare of above-mentioned low-friction coefficient simultaneously, may further comprise the steps successively:
1) be 65%~75% silicon carbide (SiC), 5%~10% boron nitride (BN), 5%~10% fluorographite, 5~10% molybdenumdisulphide (MoS, with weight percentage 2) and 10% yttrium aluminum garnet form main raw material; Main raw material, polyvinyl alcohol, Tetramethylammonium hydroxide and deionized water are carried out ball milling mix, be mixed with solid load and be 40%~60% slurry; That is the weight ratio of, (main raw material+polyvinyl alcohol+Tetramethylammonium hydroxide)/(main raw material+polyvinyl alcohol+Tetramethylammonium hydroxide+deionized water)=40%~60%;
Polyvinyl alcohol accounts for 2.5~3.5% of main raw material gross weight, and Tetramethylammonium hydroxide accounts for 1.5~2.5% of main raw material gross weight.
2), slurry is carried out mist projection granulating, obtain amyloplastid;
3), place mould to carry out the dry-pressing once shaped amyloplastid, forming pressure is 100~150MPa, obtains base substrate;
4), above-mentioned base substrate is had the hydraulic fluid phase sintering, temperature is not 1750 ℃~2000 ℃, is incubated 2~3 hours; Obtain the silicon carbide ceramic seal spare of low-friction coefficient.
Improvement as the preparation method of the silicon carbide ceramic seal spare of low-friction coefficient of the present invention: the ball milling blended time is 2~4 hours in the step 1); Step 2) in the mist projection granulating: the flow of described slip is 2~3kg/h, and the hot blast inlet temperature is 200~250 ℃.
The silicon carbide ceramic seal spare of low-friction coefficient of the present invention belongs to a kind of no hydraulic fluid phase sintering silicon carbide ceramics self-lubricating material.
The effect of the silicon carbide ceramic seal spare of low-friction coefficient of the present invention is:
1), boron nitride (BN) has good thermal stability and lower thermal expansion, higher thermal conductivity.Hexagonal boron nitride and the crystal structure of graphite are more close, laminate structure for similar graphite, but it does not at high temperature have the such load ruckbildung of image-stone China ink, it can image-stone the same dry method car easily of China ink, mill, plane, cobalt, cut, grind, and because BN is finer and close more than graphite, so working accuracy is higher, can reach 0.01 millimeter.But, can be used for making the component of complicated shape owing to this processing characteristics.
2), fluorine carbon bond bound energy is stronger in the fluorographite, the distance between layer and the layer is more much bigger than graphite, therefore is easy to shear at interlayer, in High Temperature High Pressure with there is not the lubricity under the aqueous vapor condition good.With boron nitride and fluorographite, MoS 2Mixing effect, thus constitute high temperature lubricant.Because the mechanical property of boron nitride, fluorographite all obviously is better than graphite, thus thus the silicon carbide sealing member of Zhi Zaoing not only mechanical property obviously improve and lubricity excellence.
The salient features index of the silicon carbide ceramic seal spare of low-friction coefficient of the present invention is as follows:
Volume density 2.5-3.0g/cm 3, void content 2%-10%, ultimate compression strength is greater than 1500MPa, and folding strength is greater than 300MPa, and frictional coefficient is less than 0.15.
In sum, the silicon carbide ceramic seal spare of low-friction coefficient of the present invention can guarantee that mechanical property has low frictional coefficient again.
Embodiment
The present invention is described further below in conjunction with specific embodiment, and the part among all embodiment is all represented weight part.
Silicon carbide is selected silicon carbide powder (purity>98%, median size are 0.76 μ m) for use, and boron nitride is selected hexagonal boron nitride particles (HBN, median size is less than 5 μ m, purity is>97%), fluorine carbon ratio 0.7-1.14, the MoS of fluorographite for use 2Purity be 98.5%.
The preparation method of the silicon carbide ceramic seal spare of embodiment 1, a kind of low-friction coefficient, carry out following steps successively:
1), with 65 parts of silicon carbide, 5 parts of boron nitride, 10 parts of fluorographites, 10 parts of MoS 2Mix with 10 parts of yttrium aluminum garnets, form main raw material; Add 3 parts of polyvinyl alcohol, 2 parts of Tetramethylammonium hydroxide and 105 parts of deionized waters then, mechanical ball milling 3 hours; Be mixed with solid load and be 50% slurry;
2), slurry is carried out mist projection granulating, processing condition are as follows: the flow of slip is 2.5kg/h, and the hot blast inlet temperature is 220 ℃; Obtain amyloplastid;
3), place mould to carry out the dry-pressing once shaped amyloplastid, forming pressure is 150MPa, obtains base substrate;
4), above-mentioned base substrate is had the hydraulic fluid phase sintering, temperature is not 2000 ℃, is incubated 2 hours; Obtain the silicon carbide ceramic seal spare of low-friction coefficient.
The volume density 2.5g/cm of this low-friction coefficient silicon carbide ceramic seal spare 3, void content 10%, ultimate compression strength is 1700MPa, and folding strength is 310MPa, and frictional coefficient is 0.1.
The preparation method of the silicon carbide ceramic seal spare of embodiment 2, a kind of low-friction coefficient, carry out following steps successively:
1), with 75 parts of silicon carbide, 5 parts of boron nitride, 5 parts of fluorographites, 5 parts of MoS 2Mix with 10 parts of yttrium aluminum garnets, form main raw material; Add 3 parts of polyvinyl alcohol, 2 parts of Tetramethylammonium hydroxide and 155 parts of deionized waters then, mechanical ball milling 4 hours; Be mixed with solid load and be 40% slurry;
2), slurry is carried out mist projection granulating, processing condition are as follows: the flow of slip is 3kg/h, and the hot blast inlet temperature is 250 ℃; Obtain amyloplastid;
3), place mould to carry out the dry-pressing once shaped amyloplastid, forming pressure is 120MPa, obtains base substrate;
4), above-mentioned base substrate is had the hydraulic fluid phase sintering, temperature is not 1750 ℃, is incubated 3 hours; Obtain the silicon carbide ceramic seal spare of low-friction coefficient.
The volume density 3.0g/cm of this low-friction coefficient silicon carbide ceramic seal spare 3, void content 2.0%, ultimate compression strength is 1800MPa, and folding strength is 360MPa, and frictional coefficient is 0.15.
The preparation method of the silicon carbide ceramic seal spare of embodiment 3, a kind of low-friction coefficient, carry out following steps successively:
1), with 70 parts of silicon carbide, 10 parts of boron nitride, 5 parts of fluorographites, 5 parts of MoS 2Mix with 10 parts of yttrium aluminum garnets, form main raw material; Add 3 parts of polyvinyl alcohol, 2 parts of Tetramethylammonium hydroxide and 70 parts of deionized waters then, mechanical ball milling 3 hours; Be mixed with solid load and be 60% slurry;
2), slurry is carried out mist projection granulating, processing condition are as follows: the flow of slip is 2.5kg/h, and the hot blast inlet temperature is 200 ℃; Obtain amyloplastid;
3), place mould to carry out the dry-pressing once shaped amyloplastid, forming pressure is 130MPa, obtains base substrate;
4), above-mentioned base substrate is had the hydraulic fluid phase sintering, temperature is not 1800 ℃, is incubated 2.5 hours; Obtain the silicon carbide ceramic seal spare of low-friction coefficient.
The volume density 2.7g/cm of this low-friction coefficient silicon carbide ceramic seal spare 3, void content 6.0%, ultimate compression strength is 1750MPa, and folding strength is in 340MPa, and frictional coefficient is 0.14.
The preparation method of the silicon carbide ceramic seal spare of embodiment 4, a kind of low-friction coefficient, carry out following steps successively:
1), with 68 parts of silicon carbide, 7 parts of boron nitride, 7 parts of fluorographites, 8 parts of MoS 2Mix with 10 parts of yttrium aluminum garnets, form main raw material; Add 3 parts of polyvinyl alcohol, 2 parts of Tetramethylammonium hydroxide and 105 parts of deionized waters then, mechanical ball milling 3 hours; Be mixed with solid load and be 50% slurry;
2), slurry is carried out mist projection granulating, processing condition are as follows: the flow of slip is 2.5kg/h, and the hot blast inlet temperature is 220 ℃; Obtain amyloplastid;
3), place mould to carry out the dry-pressing once shaped amyloplastid, forming pressure is 100MPa, obtains base substrate;
4), above-mentioned base substrate is had the hydraulic fluid phase sintering, temperature is not 1750 ℃, is incubated 3 hours; Obtain the silicon carbide ceramic seal spare of low-friction coefficient.
The volume density 2.6g/cm of this low-friction coefficient silicon carbide ceramic seal spare 3, void content 7.0%, ultimate compression strength is 1700MPa, and folding strength is 380MPa, and frictional coefficient is 0.13.
In order to prove superior performance of the present invention place, the contriver has also carried out following contrast experiment:
Comparative Examples 1, be that the patent of CN101255330A prepares self-lubricating seal ring, volume density 2.6~2.9g/cm3, knoop hardness 2600~2800Kg/mm2, bending strength>140MPa, ultimate compression strength>1700MPa. void content 4~7% according to publication number.Its frictional coefficient is about 0.27.
Comparative Examples 2, be that the patent of CN101551012A prepares silicon carbide sealed ring according to publication number, its body is close to be 3.15~3.20g/cm 3, hardness is 90~91HRA, and bending strength is 400~450MPa, and fracture toughness property is 3.5~4.0MPam 1/2Its frictional coefficient is also more much bigger than Comparative Examples 1, that is, self lubricity is relatively poor.
Comparative Examples 3, the main raw material among the embodiment 1 is made into to be mixed by 65 parts of silicon carbide, 25 parts of fluorographites and 10 parts of yttrium aluminum garnets, all the other are with embodiment 1.
The volume density 2.5g/cm of this silicon carbide ceramic seal spare 3, void content 8.9%, ultimate compression strength is 1200MPa, and folding strength is 210MPa, and frictional coefficient is 0.19.
Comparative Examples 4, the main raw material among the embodiment 1 is made into to be mixed by 65 parts of silicon carbide, 25 parts of boron nitride and 10 parts of yttrium aluminum garnets, all the other are with embodiment 1.
The volume density 2.61g/cm of this silicon carbide ceramic seal spare 3, void content 8.5%, ultimate compression strength is 1500MPa, and folding strength is 280MPa, and frictional coefficient is 0.17.
Comparative Examples 5, the main raw material among the embodiment 1 is made into to be mixed by 65 parts of silicon carbide, 25 parts of molybdenumdisulphide and 10 parts of yttrium aluminum garnets, all the other are with embodiment 1.
The volume density 2.71g/cm of this silicon carbide ceramic seal spare 3, void content 8.3%, ultimate compression strength is 1400MPa, and folding strength is 270MPa, and frictional coefficient is 0.16.
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 (3)

1. the silicon carbide ceramic seal spare of low-friction coefficient, it is characterized in that: described sealing member is by main raw material, form as the polyvinyl alcohol of binding agent with as the Tetramethylammonium hydroxide of dispersion agent, and described main raw material is grouped into by the one-tenth of following weight content: 65%~75% silicon carbide, 5%~10% boron nitride, 5%~10% fluorographite, 5~10% molybdenumdisulphide and 10% yttrium aluminum garnet; Described polyvinyl alcohol accounts for 2.5~3.5% of main raw material gross weight, and Tetramethylammonium hydroxide accounts for 1.5~2.5% of main raw material gross weight.
2. the preparation method of the silicon carbide ceramic seal spare of low-friction coefficient as claimed in claim 1 is characterized in that may further comprise the steps successively:
1) be that 65%~75% silicon carbide, 5%~10% boron nitride, 5%~10% fluorographite, 5~10% molybdenumdisulphide and 10% yttrium aluminum garnet are formed main raw material, with weight percentage; Main raw material, polyvinyl alcohol, Tetramethylammonium hydroxide and deionized water are carried out ball milling mix, be mixed with solid load and be 40%~60% slurry;
Described polyvinyl alcohol accounts for 2.5~3.5% of main raw material gross weight, and Tetramethylammonium hydroxide accounts for 1.5~2.5% of main raw material gross weight.
2), described slurry is carried out mist projection granulating, obtain amyloplastid;
3), place mould to carry out the dry-pressing once shaped amyloplastid, forming pressure is 100~150MPa, obtains base substrate;
4), above-mentioned base substrate is had the hydraulic fluid phase sintering, temperature is not 1750 ℃~2000 ℃, is incubated 2~3 hours; Obtain the silicon carbide ceramic seal spare of low-friction coefficient.
3. the preparation method of the silicon carbide ceramic seal spare of low-friction coefficient according to claim 2, it is characterized in that: the ball milling blended time is 2~4 hours in the described step 1); Step 2) in the mist projection granulating: the flow of described slip is 2~3kg/h, and the hot blast inlet temperature is 200~250 ℃.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250538A (en) * 2011-06-03 2011-11-23 武汉理工大学 Normal-temperature solidifying wear-resistance coating and preparation method thereof
CN102432294A (en) * 2011-09-08 2012-05-02 浙江晟翔电子科技有限公司 Preparation method of multiphase ceramic powder
CN105236981A (en) * 2015-10-09 2016-01-13 安徽东迅密封科技有限公司 Silicon carbide/molybdenum disulfide composite ceramic and preparation method thereof
CN105236987A (en) * 2015-10-09 2016-01-13 安徽东迅密封科技有限公司 Silicon carbide/molybdenum disulfide composite ceramic and preparation method thereof
CN105384442A (en) * 2015-10-27 2016-03-09 合肥龙多电子科技有限公司 Self-lubricated high-thermally-conductive aluminum nitride-silicon carbide composite baseplate material for circuit board and preparation method of self-lubricated high-thermally-conductive aluminum nitride-silicon carbide composite baseplate material
CN105801123A (en) * 2016-03-03 2016-07-27 刘佩佩 Self-lubricated silicon metal ceramic material for bearing and preparation method of self-lubricated silicon metal ceramic material
CN106083056A (en) * 2016-06-12 2016-11-09 台州东新密封有限公司 The method of carborundum/molybdenum disilicide composite ceramics is prepared in pressureless sintering
CN109265175A (en) * 2018-10-22 2019-01-25 三明学院 A kind of high-strength ceramic product and preparation method thereof

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CN1454398A (en) * 2000-08-18 2003-11-05 全球热电公司 High temperature gas seals
CN100999411A (en) * 2006-12-30 2007-07-18 浙江大学 Aluminium nitride reinforced sibicon carbide ceramic and its preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1454398A (en) * 2000-08-18 2003-11-05 全球热电公司 High temperature gas seals
CN100999411A (en) * 2006-12-30 2007-07-18 浙江大学 Aluminium nitride reinforced sibicon carbide ceramic and its preparation method

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250538A (en) * 2011-06-03 2011-11-23 武汉理工大学 Normal-temperature solidifying wear-resistance coating and preparation method thereof
CN102250538B (en) * 2011-06-03 2013-11-20 武汉理工大学 Normal-temperature solidifying wear-resistance coating and preparation method thereof
CN102432294A (en) * 2011-09-08 2012-05-02 浙江晟翔电子科技有限公司 Preparation method of multiphase ceramic powder
CN105236981A (en) * 2015-10-09 2016-01-13 安徽东迅密封科技有限公司 Silicon carbide/molybdenum disulfide composite ceramic and preparation method thereof
CN105236987A (en) * 2015-10-09 2016-01-13 安徽东迅密封科技有限公司 Silicon carbide/molybdenum disulfide composite ceramic and preparation method thereof
CN105384442A (en) * 2015-10-27 2016-03-09 合肥龙多电子科技有限公司 Self-lubricated high-thermally-conductive aluminum nitride-silicon carbide composite baseplate material for circuit board and preparation method of self-lubricated high-thermally-conductive aluminum nitride-silicon carbide composite baseplate material
CN105801123A (en) * 2016-03-03 2016-07-27 刘佩佩 Self-lubricated silicon metal ceramic material for bearing and preparation method of self-lubricated silicon metal ceramic material
CN106083056A (en) * 2016-06-12 2016-11-09 台州东新密封有限公司 The method of carborundum/molybdenum disilicide composite ceramics is prepared in pressureless sintering
CN109265175A (en) * 2018-10-22 2019-01-25 三明学院 A kind of high-strength ceramic product and preparation method thereof
CN109265175B (en) * 2018-10-22 2021-05-25 三明学院 High-strength ceramic product and preparation method thereof

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