CN106045521A - Method using hot pressed sintering to prepare dry-gas-seal rotating ring - Google Patents
Method using hot pressed sintering to prepare dry-gas-seal rotating ring Download PDFInfo
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- CN106045521A CN106045521A CN201610369366.5A CN201610369366A CN106045521A CN 106045521 A CN106045521 A CN 106045521A CN 201610369366 A CN201610369366 A CN 201610369366A CN 106045521 A CN106045521 A CN 106045521A
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Abstract
The invention discloses a method using hot pressed sintering to prepare a dry-gas-seal rotating ring. The method includes: using 88-92wt% of submicron alpha-SiC micro-powder, 5-7wt% of aluminum oxide and 3-5wt% of yttrium oxide as the base materials; evenly mixing the base materials, dispersing agent, deionized water, binder and lubricating agent to obtain slurry; performing spray granulation on the slurry, and sealing and aging; sequentially performing pressing, drying, pre-sintering and lathing on powder after the aging to obtain a green body; performing high-temperature hot pressed sintering on the green body to obtain the dry-gas-seal rotating ring.
Description
Technical field
The present invention relates to a kind of method that hot-pressing sintering technique prepares high-end seal ring of dry gas (dry gas seals rotating ring).
Background technology
Dry gas seals i.e. " dry operating air seal " (Dry Running gas seals), is fluting Sealing Technology to be used
A kind of Novel shaft end in air seal seals, and belongs to non-contact seals.Offer outside end face fluid dynamic pressure groove (2.5～
10 μm) rotating ring rotate time, fluid dynamic pressure groove pumps into seal face the high_voltage isolation gas of outside diameter (referred to as upstream side)
Between, external diameter it is gradually increased to groove footpath gas film pressure, and is gradually reduced, because of end face film to inner radius gas film pressure from groove footpath
Pressure increases the closing force making formed opening force more than acting on sealing ring, forms the thinnest one layer gas between friction pair
Film (1～3 μm) is so that seal operation is under contactless state.The sealing of the air film total blockage that formed relatively low pressure is situated between
Matter leakage path, it is achieved that the zero leakage of sealing medium or zero effusion.
Crane John Inc. of Britain takes the lead in being applied to dry gas seals the gas conveying of ocean platform the latter stage seventies
On equipment and succeed.Dry gas seals initially occurs for solving high-speed centrifugal compressor axle head sealing problem, by
In sealing contactless operation, therefore seal friction auxiliary material is not limited by PV value, is particularly suitable for high speed and high pressure equipment
Shaft end seal, the producer that current domestic dry gas seals makes with Sichuan day machine, that Chengdu one leads to achievement is more, imported product is such as from about
Writing brush Crane, FOX, Bo Geman etc..
Typical dry gas sealing structure, is made up of rotating ring (rotating ring), stationary ring, spring, sealing ring, spring base and axle sleeve,
Rotating ring sealing surface is through grinding, polishing, and processes the fluid dynamic pressure groove of special role in the above.Rotating ring is dry gas
The core component sealed, because it typically utilizes laser process fluid indent on polished end face, is prepared as accordingly
This is higher, and dry gas seals is mainly used in the shaft end seal of high speed and high pressure equipment simultaneously, and the working condition safety of use requires the highest, peace
Before dress uses, rotating ring will be tested through high speed bench tests, 1.2-1.5 times of the most actually used rotating speed,
Generally up to 12000-18000r/min, run up the high requirement proposing rotating ring, except strict machining and
Mill machining accuracy, proposes high requirement to material simultaneously, and higher mechanical strength, any pore can not be contained, at present in surface
Domestic general main pressureless sintering silicon carbide ceramic (SSiC) uses as rotating ring, but is as using the increase of the diameter of axle,
The raising of centrifugal force when rotary speed and operating, domestic dry gas seals rotating ring is extremely difficult to requirement, and domestic western gas east is sent, pipe
Road distribution pressure is designed as 10MPa, and caliber is at about 1000mm, and natural gas line circuit is grown up 30000km, in order to ensure gas
Flow, a compressor station need to be set up every a segment distance, use two large-scale compressors to carry out supercharging, due to home products very
Difficulty meets requirement, and mainly by Saint-Gobain of France, Germany matches the internationally famous business monopolies such as thinkling sound Tyke, Germany ESK.
Produce the pressureless sintering silicon carbide ceramic of preparation at present, mainly use B4C and C is as sintering aid, normal pressure-sintered
Prepared by technique, silicon carbide ceramics prepared by this technique, and consistency is high, and hardness is up to 92HRA, but uses carbon prepared by this technique
SiClx pottery, three-point bending resistance intensity and fracture toughness are relatively low, and when internal diameter is more than 300mm, owing to product size is relatively big, density is difficult to
Reach 3.12g/cm3Above, testing under 15000r/min high speed bench tests, product is easy to break into pieces, it is impossible to by test, only
Diameter of axle ＜ 300mm environment can be used for use.
Summary of the invention
The technical problem to be solved in the present invention is to provide and a kind of uses hot pressed sintering to prepare high-end dry gas seals rotating ring
Method, uses the method for the present invention can solve that existing pressureless sintering silicon carbide ceramic three-point bending resistance intensity is low, fracture toughness is low, whole
The problem of body structural integrity difference.
In order to solve above-mentioned technical problem, the present invention provides a kind of side using hot pressed sintering to prepare dry gas seals rotating ring
Method, comprises the following steps:
1) pressing blank powder, is prepared:
Aluminium oxide (Al with submicron alpha-SiC micropowder, 5～the 7wt% of 88～92wt%2O3), 3～the yittrium oxide of 5wt%
Based on expect；
First basestocks and dispersant are joined in ball mill, be subsequently adding deionized water as solvent, be stirred ball
Mill, is subsequently adding binding agent and lubricant, uniformly after mixing, obtains slurry；
Described dispersant accounts for the 0.5%-1% (preferably 0.8wt%) of basestocks gross weight；
Described binding agent accounts for the 5%-12% (preferably 10wt%) of basestocks gross weight；
Described lubricant accounts for the 1%-4% (preferably 3wt%) of basestocks gross weight；
Described deionized water accounts for the 50%-80% (preferably 60～70wt%) of basestocks gross weight；
Submicron alpha-SiC micropowder refers to D50It is the α-SiC of 0.4～1.0 μm；
Alumina powder D50About 1 μm, yittrium oxide D50About 1.2 μm；
Described slurry is carried out mist projection granulating, obtains the mist projection granulating powder that can cross 80 mesh, by described mist projection granulating powder in room temperature
Old 4～6 days of lower seal (preferably 5 days)；
2), the compacting of base substrate:
By step 1) the old rear powder of gained suppresses, and obtains base substrate；
3), base substrate is dried:
Base substrate is dried 1～4h in 80～120 DEG C, obtains dried base substrate；
4), base substrate pre-burning:
Dried base substrate (pure carbon base substrate) is at flowing N2Under the protection of gas, with the intensification of 80～120 DEG C/h in Muffle furnace
Speed rises to 600～900 DEG C of binder removals (purpose be so that additive pyrolysis devolatilization in base substrate)；
5), car system:
By step 4) base substrate carries out car system after the pre-burning of gained, obtains biscuit；
Particularly as follows: carry out car system according to the shrinkage factor calculated, base substrate car after pre-burning being made the size of needs, this belongs to normal
Rule technology；
6), high temperature hot pressing sintering:
Biscuit is put into graphite jig with the form that levels stacking is put, between the biscuit that every two-layer is adjacent, arranges two
Graphite paper and a Graphite pad, described Graphite pad is between two graphite papers；
Remarks illustrate: in graphite jig, be positioned at end face and be positioned at bottom surface be biscuit；
The above-mentioned graphite jig equipped with biscuit is loaded in vacuum resistance furnace (vacuum graphite resistance furnace) and carries out hot pressed sintering,
It is warming up to 1500 DEG C with 150～200 DEG C/h under vacuum, is then shut off vacuum pump, be filled with argon, continue with 100～150 DEG C/h liter
Temperature, to 1800 DEG C～1900 DEG C, keeps 1～2h under the pressure of 20～30Mpa；Obtain seal ring of dry gas (dry gas seals rotating ring).
The hot pressed sintering that uses as the present invention prepares the improvement of method of dry gas seals rotating ring:
Described step 1) in,
Described dispersant is Tetramethylammonium hydroxide；
Described binding agent be mass concentration be the polyvinyl alcohol water solution of 10%；
Described lubricant is glycerol.
The hot pressed sintering that uses as the present invention prepares the further improvements in methods of dry gas seals rotating ring:
Described step 1) in,
First submicron alpha-SiC micropowder, aluminium oxide, yittrium oxide and dispersant are joined in ball mill, be subsequently adding from
Sub-water, as solvent, is stirred ball milling 3～5h, is then sequentially added into binding agent and lubricant, then uniform stirring ball every 1h
Mill 3～5h, obtains slurry.
The hot pressed sintering that uses as the present invention prepares the further improvements in methods of dry gas seals rotating ring:
Described step 1) in, during mist projection granulating, controlling inlet temperature is 200～260 DEG C, and outlet temperature is at 80～120 DEG C.
The hot pressed sintering that uses as the present invention prepares the further improvements in methods of dry gas seals rotating ring:
Described step 6) in, after holding (that is, insulation, the pressurize) time of 1～2h arrives, pressure release is lowered the temperature with stove, treats that furnace temperature drops
To 150 DEG C, open fire door；Obtain seal ring of dry gas.
The hot pressed sintering that uses as the present invention prepares the further improvements in methods of dry gas seals rotating ring:
Described step 2) in, first use four-column hydraulic press (such as 500t four-column hydraulic press) under the pressure of 25MPa
Suppress, then carry out isostatic pressed process in 200MPa.
The hot pressed sintering that uses as the present invention prepares the further improvements in methods of dry gas seals rotating ring: with 90wt%
Submicron alpha-SiC micropowder, the aluminium oxide of 6wt%, 4wt% yittrium oxide based on expect.
The method that the employing hot pressed sintering of the present invention prepares dry gas seals rotating ring, by using high-purity sub-micro SiC micropowder,
Use Al2O3And Y2O3As liquid-phase sintering auxiliary agent, obtain even structure consistency in combination with hot-pressing sintering technique high, mechanical
The sintered body that intensity is high.
The present invention has following technical advantage: using liquid-phase sintering auxiliary agent to be sintered, liquid-phase sintering auxiliary agent can improve
The fracture toughness of product and bending strength；Use liquid phase sintering silicon carbide ceramic prepared by hot-pressing sintering technique, it is possible to achieve produce
The basic densification of product, ensures that product microstructure is uniform simultaneously, and mechanical strength is high.
Detailed description of the invention
Embodiment 1, a kind of method using hot pressed sintering to prepare high-end seal ring of dry gas (dry gas seals rotating ring), successively
Follow the steps below:
1), the preparation of pressing blank powder:
First by the submicron (D of 90wt%50=0.7 μm) α-SiC, the alumina powder (D of 6wt%50=1 μm) and 4wt%
Yittrium oxide (D50=1.2 μm), based on material join in the ball milling that liner is polyurethane, add basestocks 0.8wt% point
Powder Tetramethylammonium hydroxide and the deionized water of basestocks 60wt%, after ball grinding stirring 4h, be then sequentially added into base every 1h
The polyvinyl alcohol water solution (mass concentration of polyvinyl alcohol is 10%) of plinth material 10wt%, adds the glycerol ball of basestocks 3wt%
Mill stirring 4h, carries out mist projection granulating by the slip of mix homogeneously, and the inlet temperature controlling mist projection granulating is 250 DEG C, outlet temperature
Being 100 DEG C, atomizing disk rotating speed is 8000r/min, the pelletizing prepared is passed through 80 mesh sieve, is then charged into plastic bag and enters
Row seals old, suppresses under room temperature after old 5 days.
In the present invention, room temperature generally refers to 15～25 DEG C.
2), the compacting (molding) of base substrate:
Pressing blank as requested, suppresses, then in isostatic cool pressing on four-column hydraulic press under the pressure of 25MPa
In machine, the pressure static pressure with 200MPa processes 30min.
3), base substrate is dried:
Base substrate is dried at 110 DEG C 3h, to its moisture less than 1%.
4), base substrate pre-burning:
Dried base substrate is at flowing N2Under the protection of gas, in Muffle furnace, rise to 900 with the programming rate of 100 DEG C/h
DEG C, insulation 2h carries out de-waxing, so that the additive pyrolysis devolatilization in base substrate is clean.
5), car system:
By the biscuit after pre-burning, according to the size required on product drawing, car internal-and external diameter and height, and leave mill processing
Surplus (surplus is generally 1%)；This step belongs to routine techniques.
6), high temperature sintering:
The biscuit made by car loads in hot pressing graphite jig, and the form that biscuit is put with levels stacking puts into graphite jig
In, two graphite papers and a Graphite pad are set between the biscuit that every two-layer is adjacent, described Graphite pad is positioned at two graphite
Between paper；In graphite jig, be positioned at end face and be positioned at bottom surface be biscuit；By the above-mentioned graphite mo(u)ld equipped with biscuit
Tool loading vacuum graphite resistance furnace carries out hot pressed sintering, is warming up to 1500 DEG C with 200 DEG C/h under vacuum, is then shut off vacuum
Pump, is filled with argon, continues to be warming up to 1860 DEG C with 150 DEG C/h, keeps 1h under the pressure of 25Mpa；Then pressure release, stops heating
Insulation, furnace cooling；Treat that furnace temperature is down to 150 DEG C, open fire door；Obtain seal ring of dry gas (dry gas seals rotating ring).
7), performance detection
Detection bulk density is 3.26g/cm3, three-point bending resistance intensity is 680Mpa, and fracture toughness is 6.5GPa, hardness
(HRA) being 92, high speed bench tests, run up under 18000r/min 60s, any exception does not occur, meets dry gas seals
Ring uses requirement.
Embodiment 2:
By " submicron (D50=0.7 μm) α-SiC of 90wt%, the alumina powder (D50 of 6wt% in embodiment 1 step 1
=1 μm) and the yittrium oxide (D50=1.2 μm) of 4wt% " change " submicron (D of 95wt% into50=0.7 μm) α-SiC, 3wt%
Alumina powder (D50=1 μm) and the yittrium oxide (D of 2wt%50=1.2 μm) "；Remaining is equal to embodiment 1.
Its performance test results is as follows: bulk density is 3.21g/cm3, three-point bending resistance intensity is 520Mpa, fracture toughness
For 5.0GPa, hardness (HRA) is 92, high speed bench tests, and run up under 18000r/min 60s, any exception does not occur,
Meet seal ring of dry gas and use requirement.
Embodiment 3:
By " submicron (D50=0.7 μm) α-SiC of 90wt%, the alumina powder (D50 of 6wt% in embodiment 1 step 1
=1 μm) and the yittrium oxide (D50=1.2 μm) of 4wt% " change " submicron (D50=0.7 μm) α-SiC, the 8wt% of 90wt% into
Alumina powder (D50=1 μm) and the yittrium oxide (D50=1.2 μm) of 2wt% "；Remaining is equal to embodiment 1.
Its performance test results is as follows: bulk density is 3.24g/cm3, three-point bending resistance intensity is 600Mpa, fracture toughness
For 5.5GPa, hardness (HRA) is 91.5, high speed bench tests, and run up under 18000r/min 60s, does not occur any different
Often, meet seal ring of dry gas and use requirement.
Every mechanical performance of the seal ring of dry gas of above-described embodiment 1～embodiment 3 gained is described in table 1 below.
Table 1
Comparative example 1, by " submicron (the D of 90wt% in embodiment 150=0.7 μm) α-SiC " make into " α of 90wt%-
SiC(D50=3.0 μm) ", remaining is equal to embodiment 1.
Comparative example 2, by " submicron (the D of 90wt% in embodiment 150=0.7 μm) α-SiC, the alumina powder of 6wt%
(D50=1 μm) and the yittrium oxide (D of 4wt%50=1.2 μm) " change " submicron (D of 94wt% into50=0.7 μm) α-SiC,
Alumina powder (the D of 6wt%50=1 μm) "；Remaining is equal to embodiment 1.
Comparative example 3, by " submicron (the D of 90wt% in embodiment 150=0.7 μm) α-SiC, the alumina powder of 6wt%
(D50=1 μm) and the yittrium oxide (D of 4wt%50=1.2 μm) " change " submicron (D of 100wt% into50=0.7 μm) α-SiC ", its
More than be equal to embodiment 1.
Comparative example 4, by " submicron (the D of 90wt% in embodiment 150=0.7 μm) α-SiC, the alumina powder of 6wt%
(D50=1 μm) and the yittrium oxide (D of 4wt%50=1.2 μm) " change " submicron (D of 96wt% into50=0.7 μm) α-SiC,
Boron carbide (the D of 1wt%50=1 μm) and the nanometer carbon black (D of 3wt%50=200nm) "；Remaining is equal to embodiment 1.
Comparative example 5, by the step 6 in embodiment 1) high temperature sintering changes into as follows: the biscuit made by car loads graphite earthenware
Crucible, loads in normal pressure-sintered stove, begins to shut off fire door, heats up with 200 DEG C/min, is warming up to 1500 DEG C and is filled with argon, so
Rear continuation is warming up to 1930 DEG C with 150 DEG C/min, and insulation 1h stops heating, and furnace cooling, remaining is equal to embodiment 1.
The properties detection data of above-mentioned all comparative examples are described in table 2 below.
Table 2
Finally, in addition it is also necessary to be only several specific embodiments of the present invention it is noted that listed above.Obviously, this
Bright it is not limited to above example, it is also possible to have many deformation.Those of ordinary skill in the art can be from present disclosure
The all deformation directly derived or associate, are all considered as protection scope of the present invention.
Claims (7)
1. the method using hot pressed sintering to prepare dry gas seals rotating ring, is characterized in that comprising the following steps:
1) pressing blank powder, is prepared:
Based on the yittrium oxide of the aluminium oxide of submicron alpha-SiC micropowder, 5～7wt%, 3～the 5wt% of 88～92wt%
Material；
First basestocks and dispersant are joined in ball mill, be subsequently adding deionized water as solvent, be stirred ball milling, so
Rear addition binding agent and lubricant, uniformly after mixing, obtain slurry；
Described dispersant accounts for the 0.5%～1% of basestocks gross weight；
Described binding agent accounts for the 5%～12% of basestocks gross weight；
Described lubricant accounts for the 1%～4% of basestocks gross weight；
Described deionized water accounts for the 50%～80% of basestocks gross weight；
Submicron alpha-SiC micropowder refers to D50It is the α-SiC of 0.4～1.0 μm；
Described slurry is carried out mist projection granulating, obtains the mist projection granulating powder that can cross 80 mesh, by the closeest for described mist projection granulating powder
Seal old 4～6 days；
2), the compacting of base substrate:
By step 1) the old rear powder of gained suppresses, and obtains base substrate；
3), base substrate is dried:
Base substrate is dried 1～4h in 80～120 DEG C, obtains dried base substrate；
4), base substrate pre-burning:
Dried base substrate is at flowing N2Under the protection of gas, in Muffle furnace, rise to 600～900 with the programming rate of 80～120 DEG C/h
DEG C binder removal；
5), car system:
By step 4) base substrate carries out car system after the pre-burning of gained, obtains biscuit；
6), high temperature hot pressing sintering:
Biscuit is put into graphite jig with the form that levels stacking is put, two graphite are set between the biscuit that every two-layer is adjacent
Paper and a Graphite pad, described Graphite pad is between two graphite papers；
The above-mentioned graphite jig equipped with biscuit is loaded in vacuum resistance furnace and carries out hot pressed sintering, with 150～200 DEG C/h under vacuum
It is warming up to 1500 DEG C, is then shut off vacuum pump, be filled with argon, continue to be warming up to 1800 DEG C～1900 DEG C with 100～150 DEG C/h,
1～2h is kept under the pressure of 20～30Mpa；Obtain seal ring of dry gas.
The method that employing hot pressed sintering the most according to claim 1 prepares dry gas seals rotating ring, is characterized in that:
Described step 1) in,
Described dispersant is Tetramethylammonium hydroxide；
Described binding agent be mass concentration be the polyvinyl alcohol water solution of 10%；
Described lubricant is glycerol.
The method that employing hot pressed sintering the most according to claim 2 prepares dry gas seals rotating ring, is characterized in that:
Described step 1) in,
First submicron alpha-SiC micropowder, aluminium oxide, yittrium oxide and dispersant are joined in ball mill, be subsequently adding deionized water
As solvent, be stirred ball milling 3～5h, be then sequentially added into binding agent and lubricant every 1h, then uniform stirring ball milling 3～
5h, obtains slurry.
The method that employing hot pressed sintering the most according to claim 2 prepares dry gas seals rotating ring, is characterized in that:
Described step 1) in, during mist projection granulating, controlling inlet temperature is 200～260 DEG C, and outlet temperature is at 80～120 DEG C.
The method that employing hot pressed sintering the most according to claim 1 prepares dry gas seals rotating ring, is characterized in that:
Described step 6) in, after the retention time of 1～2h arrives, pressure release is lowered the temperature with stove, treats that furnace temperature is down to 150 DEG C, opens fire door；?
Seal ring of dry gas.
The method that employing hot pressed sintering the most according to claim 1 prepares dry gas seals rotating ring, is characterized in that:
Described step 2) in, first use four-column hydraulic press to suppress under the pressure of 25MPa, then carry out in 200MPa
Static pressure processes.
The method that employing hot pressed sintering the most according to claim 1 prepares dry gas seals rotating ring, is characterized in that:
By the submicron alpha-SiC micropowder of 90wt%, the aluminium oxide of 6wt%, 4wt% yittrium oxide based on expect.
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