CN104001913A - Press piece type sealing device and method for manufacturing large molybdenum crucible - Google Patents
Press piece type sealing device and method for manufacturing large molybdenum crucible Download PDFInfo
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- CN104001913A CN104001913A CN201410234680.3A CN201410234680A CN104001913A CN 104001913 A CN104001913 A CN 104001913A CN 201410234680 A CN201410234680 A CN 201410234680A CN 104001913 A CN104001913 A CN 104001913A
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Abstract
The invention discloses a method for manufacturing a large molybdenum crucible. The method includes seven steps of molybdenum powder selection, powder loading, pressing forming, rubber mould separating, reshaping, steel mould separating and sintering. A press piece type sealing device comprises a steel mould, a rubber mould, a mould steel plug, a demoulding ring, threaded holes and the like. By means of the method, a large-specification molybdenum crucible product with the inner diameter being 600-650mm, the height being 1300-1400mm and the thickness being 18-22mm can be produced successfully. The finished product is smooth in inner wall and outer wall, regular in appearance and free of gaps. Cold isostatic pressing is adopted in the production process, the product is formed through one step, no press forming waste is produced, the surface is reshaped through a vertical lathe on the steel mould after pressing, the yield is over 85%, and the recovery is over 95%. The recycled turned molybdenum powder can be reutilized, and production cost is greatly reduced. The press piece type sealing device removes risks of waste generation caused by press liquid leakage. By means of the demoulding ring, automatic demoulding of the large molybdenum is achieved, operation difficulty is reduced, and cost is reduced. A step-by-step heating method is adopted in the sintering process, and the outer diameter out-of-roundness of the large molybdenum is lower than 2%.
Description
Technical field
The invention belongs to material preparation method technical field, be specifically related to a kind of preparation method of large-scale molybdenum crucible, the invention still further relates to a kind of tabletting type sealing device for the preparation of large-scale molybdenum crucible.
Background technology
Molybdenum crucible is normally used as cord cage and the heater in various high temperature industrial furnaces, and the fusing point of molybdenum is up to 2610 ℃, and the serviceability temperature of molybdenum crucible is conventionally in 2000 ℃.Because its production cost is well below tungsten crucible, therefore, 2000 ℃ with interior hot environment under, molybdenum crucible substitutes tungsten crucible has become inevitable trend.Along with the development of industrial technology, the dimensions of high temperature industrial furnace is increasing, and the demand of large scale corresponding thereto, large piece weight molybdenum crucible is more and more.Conventionally, the molybdenum crucible that diameter is surpassed to 500mm is called large-scale molybdenum crucible, the powder metallurgic method of the small-sized molybdenum crucible of existing preparation cannot be indiscriminately imitated to the preparation of large-scale molybdenum crucible, because the increase along with molybdenum crucible size, the substance of crucible also increases thereupon, powder metallurgic method mainly adopts manual operation, the increase of size and substance causes original manual operation cannot complete the critical process such as sealing, the demoulding, shaping of molybdenum crucible, once there is careless mistake in these operations, will produce the waste material of hundreds of kilograms, cost allowance is huge.
Current, industrial common employing splicing method or spraying process are produced large-scale molybdenum crucible.
Splicing method is that large-scale molybdenum crucible is broken the whole up into parts, and first prepares the molybdenum product compared with small dimension, then the molybdenum product of above-mentioned small dimension is stitched together, but this method machined splicing difficulty is larger, and the stitching portion between two crucibles exists gap.
Spraying process is to utilize high temperature, high speed flame stream that the powder particle through specially treated is ejected into graphite core mould surface, powder particle obtains the crucible product of given shape in mandrel surface deposition, but this method exists the problem that difficulty of processing is large, yield rate is low, production cost is high.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing large-scale molybdenum crucible, without splicing, one-shot forming just can be produced large-scale molybdenum crucible more than diameter 500mm, and yield rate is high.
Another object of the present invention is to provide a kind of tabletting type sealing device for the preparation of large-scale molybdenum crucible.
The technical solution adopted in the present invention is: tabletting type sealing device, comprise columniform punching block, the arranged outside of punching block has columnar rubber moulding, between rubber moulding and punching block, form Zhuan Fen district, the upper end of rubber moulding is provided with open-topped cylindrical mold steel plug, and the sidewall of mould steel plug and bottom are provided with some through holes; The upper end of the lower end of punching block and mould steel plug is respectively arranged with the first extension, the two ends up and down of rubber moulding are respectively arranged with the second extension, the first extension of relevant position and the second extension are superimposed with each other and together stretch in snap close, lock screw is fixed the first extension and the second extension through snap close, between lock screw and the second extension, is provided with intermediate plate; Along punching block bottom outside, within one week, be evenly arranged at intervals with several stripper rings, stripper rings inside is provided with screw.
Feature of the present invention is also,
The wall thickness of rubber moulding is 5～7mm.
Another technical scheme of the present invention is: prepare the method for large-scale molybdenum crucible, comprise the steps:
The first step, chooses molybdenum powder
Choose particle mean size and be 3.2 μ m～3.8 μ m, pine than being 1.05～1.2g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder that the first step is chosen packs in tabletting type sealing device, and the quality that packs molybdenum powder into is 750～850kg;
The 3rd step, die mould
The tabletting type sealing device that second step is installed to molybdenum powder is put into cold isostatic press, under the pressure of 180～200MPa, and pressurize 6～9 minutes, then release, then tabletting type sealing device is hung out from cold isostatic press;
The 4th step, rubber moulding departs from
Separate opening lock catch, slough rubber moulding, expose the molybdenum crucible pressed compact that place, Zhuan Fen district forms;
The 5th step, shaping
Use lathe to process the molybdenum crucible pressed compact with punching block, lathe jaw is clamped in the bottom of punching block, guarantees that the profile rule of molybdenum crucible pressed compact is without burr;
The 6th step, the punching block demoulding
Stripper bolt is inserted respectively in the screw of stripper rings, then hang stripper bolt with crane, slowly mention, make molybdenum crucible pressed compact separated with punching block;
The 7th step, sintering
The molybdenum crucible pressed compact of the 6th step being sloughed to punching block drops in intermediate frequency furnace, adopts the method for progressively heating to heat molybdenum crucible pressed compact, makes molybdenum crucible.
Feature of the present invention is also,
The progressively method of heating in the 5th step is: first heat and within 6 hours, make furnace temperature rise to 1000 ℃ from room temperature, then be incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 ℃ from 1000 ℃, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 ℃ from 1200 ℃, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 ℃ from 1400 ℃, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 ℃ from 1640 ℃, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 ℃ from 1840 ℃, then be incubated 6 hours.
The invention has the beneficial effects as follows: the present invention prepares the method for large-scale molybdenum crucible, adopt powder metallurgic method to prepare molybdenum crucible, can successfully produce internal diameter 600～650mm, height 1300～1400mm, the large specification molybdenum crucible product of wall thickness 18～22mm, finished product inwall and outer wall are smooth, and outward appearance rule is seamless.In production process, adopt isostatic cool pressing compacting, one-shot forming, pressure-free type waste material, vertical lathe refacing in band steel mold after compacting, yield rate reaches more than 85%, and the rate of recovery reaches more than 95%, and the turning molybdenum powder reclaiming can secondary utilization, greatly reduces production cost.In pressing process, adopt tabletting type sealing device, eliminated the risk that produces waste material because of compacting leakage.Suppress complete through finishing after, use the stripper rings demoulding, realized the automatic demoulding of large-scale molybdenum crucible, reduced operation easier, saved cost of labor.In sintering process, adopt two-stage method sintering process, make the external diameter out-of-roundness of large-scale molybdenum crucible lower than 2%.
Accompanying drawing explanation
Fig. 1 is the structural representation of tabletting type sealing device of the present invention;
Fig. 2 locks the structural representation at position in tabletting type sealing device of the present invention;
Fig. 3 is that the present invention prepares and in the method for large-scale molybdenum crucible, sloughs the structural representation before separated with punching block of molybdenum crucible pressed compact after rubber moulding.
In figure, 1. rubber moulding, 2. punching block, 3. mould steel plug, 4. lock screw, 5. snap close, 6. intermediate plate, 7 first extensions, 8. the second extension, 9. through hole, 10.Zhuan Fen district, 11. stripper rings, 12. screws, 13. stripper bolts, 14. molybdenum crucible pressed compacts.
The specific embodiment
Below in conjunction with the drawings and the specific embodiments, the present invention is described in detail.
Tabletting type sealing device for the preparation of large-scale molybdenum crucible of the present invention, as shown in Figure 1, comprise columniform punching block 2, the arranged outside of punching block 2 has columnar rubber moulding 1, between rubber moulding 1 and punching block 2, form Zhuan Fen district 10, the upper end of rubber moulding 1 is provided with open-topped cylindrical mold steel plug 3, and the sidewall of mould steel plug 3 and bottom are provided with some through holes 9; The upper end of the lower end of punching block 2 and mould steel plug 3 is respectively arranged with the first extension 7, the two ends up and down of rubber moulding 1 are respectively arranged with the second extension 8, the first extension 7 of relevant position and the second extension 8 are superimposed with each other and together stretch in snap close 5, as shown in Figure 2, lock screw 4 is fixing by the first extension 7 and the second extension 8 through snap close 5, between lock screw 4 and the second extension 8, is provided with intermediate plate 6; Along punching block 2 bottom outside, within one week, be evenly arranged at intervals with stripper rings 11, stripper rings 11 inside are provided with screw 12;
The wall thickness of glued membrane 1 is 5～7mm.
Wherein, the through hole 9 that the sidewall of steel plug 3 and bottom arrange is to make pressure in isostatic cool pressing pressing process act directly on the surface of rubber moulding 1, can not cause 3 displacements of mould steel plug and comes off.
The wall thickness of rubber moulding 1 is 5～7cm, is that if too thin, in pressing process, rubber moulding 1 is easily cut and leakage by punching block 2 because this thickness result of use is best, if too thick, rubber moulding 1 is not easy stretch and stir in use.
Embodiment 1
The method of preparing large-scale molybdenum crucible, comprises the steps:
The first step, chooses molybdenum powder
Choosing particle mean size is that 3.2 μ m, pine are than being 1.05g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder that the first step is chosen packs in tabletting type sealing device Zhuan Fen district 10, and the quality that packs molybdenum powder into is 750kg;
The 3rd step, die mould
The tabletting type sealing device that second step is installed to molybdenum powder is put into cold isostatic press, under the pressure of 180MPa, and pressurize 6 minutes, then release, then tabletting type sealing device is hung out from cold isostatic press;
The 4th step, rubber moulding departs from
Separate opening lock catch 5, slough rubber moulding 1, expose the molybdenum crucible pressed compact 14 that 10 places, Zhuan Fen district form, as shown in Figure 3;
The 5th step, shaping
Use lathe to process the molybdenum crucible pressed compact 14 with punching block 2, lathe jaw is clamped in the bottom of punching block 2, guarantees that the profile rule of molybdenum crucible pressed compact 14 is without burr;
The 6th step, the punching block demoulding
Stripper bolt 13 is inserted respectively in the screw 12 of stripper rings 11, then hang stripper bolt 13 with crane, slowly mention, make molybdenum crucible pressed compact 14 separated with punching block 2;
The 7th step, sintering
The molybdenum crucible pressed compact 14 of the 6th step being sloughed to punching block 2 drops in intermediate frequency furnace, first heats and within 6 hours, makes furnace temperature rise to 1000 ℃ from room temperature, then be incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 ℃ from 1000 ℃, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 ℃ from 1200 ℃, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 ℃ from 1400 ℃, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 ℃ from 1640 ℃, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 ℃ from 1840 ℃, then be incubated 6 hours, make molybdenum crucible.
The internal diameter of molybdenum crucible prepared by the present embodiment is 600mm, and yield rate is more than 88%, and the crucible of employing spraying process processing same size, yield rate is in 50% left and right.
Embodiment 2
The method of preparing large-scale molybdenum crucible, comprises the steps:
The first step, chooses molybdenum powder
Choosing particle mean size is that 3.8 μ m, pine are than being 1.2g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder that the first step is chosen packs in tabletting type sealing device Zhuan Fen district 10, and the quality that packs molybdenum powder into is 850kg;
The 3rd step, die mould
The tabletting type sealing device that second step is installed to molybdenum powder is put into cold isostatic press, under the pressure of 200MPa, and pressurize 9 minutes, then release, then tabletting type sealing device is hung out from cold isostatic press;
The 4th step, rubber moulding departs from
Separate opening lock catch 5, slough rubber moulding 1, expose the molybdenum crucible pressed compact 14 that 10 places, Zhuan Fen district form;
The 5th step, shaping
Use lathe to process the molybdenum crucible pressed compact 14 with punching block 2, lathe jaw is clamped in the bottom of punching block 2, guarantees that the profile rule of molybdenum crucible pressed compact 14 is without burr;
The 6th step, the punching block demoulding
Stripper bolt 13 is inserted respectively in the screw 12 of stripper rings 11, then hang stripper bolt 13 with crane, slowly mention, make molybdenum crucible pressed compact 14 separated with punching block 2;
The 7th step, sintering
The molybdenum crucible pressed compact 14 of the 6th step being sloughed to punching block 2 drops in intermediate frequency furnace, first heats and within 6 hours, makes furnace temperature rise to 1000 ℃ from room temperature, then be incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 ℃ from 1000 ℃, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 ℃ from 1200 ℃, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 ℃ from 1400 ℃, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 ℃ from 1640 ℃, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 ℃ from 1840 ℃, then be incubated 6 hours, make molybdenum crucible.
The internal diameter of molybdenum crucible prepared by the present embodiment is 650mm, and yield rate is more than 85%, and the crucible of employing spraying process processing same size, yield rate is in 45% left and right.
Embodiment 3
The method of preparing large-scale molybdenum crucible, comprises the steps:
The first step, chooses molybdenum powder
Choosing particle mean size is that 3.5 μ m, pine are than being 1.1g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder that the first step is chosen packs in tabletting type sealing device Zhuan Fen district 10, and the quality that packs molybdenum powder into is 800kg;
The 3rd step, die mould
The tabletting type sealing device that second step is installed to molybdenum powder is put into cold isostatic press, under the pressure of 190MPa, and pressurize 8 minutes, then release, then tabletting type sealing device is hung out from cold isostatic press;
The 4th step, rubber moulding departs from
Separate opening lock catch 5, slough rubber moulding 1, expose the molybdenum crucible pressed compact 14 that 10 places, Zhuan Fen district form;
The 5th step, shaping
Use lathe to process the molybdenum crucible pressed compact 14 with punching block 2, lathe jaw is clamped in the bottom of punching block 2, guarantees that the profile rule of molybdenum crucible pressed compact 14 is without burr;
The 6th step, the punching block demoulding
Stripper bolt 13 is inserted respectively in the screw 12 of stripper rings 11, then hang stripper bolt 13 with crane, slowly mention, make molybdenum crucible pressed compact 14 separated with punching block 2;
The 7th step, sintering
The molybdenum crucible pressed compact 14 of the 6th step being sloughed to punching block 2 drops in intermediate frequency furnace, first heats and within 6 hours, makes furnace temperature rise to 1000 ℃ from room temperature, then be incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 ℃ from 1000 ℃, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 ℃ from 1200 ℃, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 ℃ from 1400 ℃, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 ℃ from 1640 ℃, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 ℃ from 1840 ℃, then be incubated 6 hours, make molybdenum crucible.
The internal diameter of molybdenum crucible prepared by the present embodiment is 620mm, and yield rate is more than 86%, and the crucible of employing spraying process processing same size, yield rate is in 48% left and right.
The method of the large-scale molybdenum crucible of preparation of the present invention, can successfully produce internal diameter 600～650mm, height 1300～1400mm, and the large specification molybdenum crucible product of wall thickness 18～22mm, finished product inwall and outer wall are smooth, and outward appearance rule is seamless.In production process, adopt isostatic cool pressing compacting, one-shot forming, pressure-free type waste material, vertical lathe refacing in band steel mold after compacting, yield rate reaches more than 85%, and the rate of recovery reaches more than 95%, and the turning molybdenum powder reclaiming can secondary utilization, greatly reduces production cost.Tabletting type sealing device has been eliminated the risk that produces waste material because of compacting leakage.The use of stripper rings, has realized the automatic demoulding of large-scale molybdenum crucible, has reduced operation easier, has saved cost of labor.In sintering process, adopt progressively heating sintering process, make the external diameter out-of-roundness of large-scale molybdenum crucible lower than 2%.
Claims (4)
1. tabletting type sealing device, it is characterized in that, comprise columniform punching block (2), the arranged outside of described punching block (2) has columnar rubber moulding (1), between described rubber moulding (1) and described punching block (2), form Zhuan Fen district (10), the upper end of described rubber moulding (1) is provided with open-topped cylindrical mold steel plug (3), and the sidewall of described mould steel plug (3) and bottom are provided with some through holes (9); The upper end of the lower end of described punching block (2) and described mould steel plug (3) is respectively arranged with the first extension (7), the two ends up and down of described rubber moulding (1) are respectively arranged with the second extension (8), described first extension (7) of relevant position and the second extension (8) are superimposed with each other and together stretch in snap close (5), lock screw (4) is fixing by described the first extension (7) and the second extension (8) through described snap close (5), between described lock screw (4) and described the second extension (8), is provided with intermediate plate (6); Along described punching block (2) bottom outside, within one week, be evenly arranged at intervals with several stripper rings (11), described stripper rings (11) inside is provided with screw (12).
2. tabletting type sealing device as claimed in claim 1, is characterized in that, the wall thickness of described rubber moulding (1) is 5～7mm.
3. utilize device as claimed in claim 1 to prepare the method for large-scale molybdenum crucible, it is characterized in that, comprise the steps:
The first step, chooses molybdenum powder
Choose particle mean size and be 3.2 μ m～3.8 μ m, pine than being 1.05～1.2g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder that the first step is chosen packs in described tabletting type sealing device, and the quality that packs molybdenum powder into is 750～850kg;
The 3rd step, die mould
The tabletting type sealing device that second step is installed to molybdenum powder is put into cold isostatic press, under the pressure of 180～200MPa, and pressurize 6～9 minutes, then release, more described tabletting type sealing device is hung out from cold isostatic press;
The 4th step, rubber moulding departs from
Separate opening lock catch (5), slough rubber moulding (1), expose Zhuan Fen district (10) and locate the molybdenum crucible pressed compact (14) forming;
The 5th step, shaping
Use lathe to process the molybdenum crucible pressed compact (14) with punching block (2), lathe jaw is clamped in the bottom of punching block (2), guarantees that the profile rule of molybdenum crucible pressed compact (14) is without burr;
The 6th step, the punching block demoulding
Stripper bolt (13) is inserted respectively in the screw (12) of stripper rings (11), then hang stripper bolt (13) with crane, slowly mention, make molybdenum crucible pressed compact (14) separated with punching block (2);
The 7th step, sintering
The molybdenum crucible pressed compact (14) of the 6th step being sloughed to punching block (2) drops in intermediate frequency furnace, adopts the method for progressively heating to heat molybdenum crucible pressed compact (14), makes molybdenum crucible.
4. the method for the large-scale molybdenum crucible of preparation as claimed in claim 3, is characterized in that, the progressively method of heating described in the 5th step is: first heat and within 6 hours, make furnace temperature rise to 1000 ℃ from room temperature, then be incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 ℃ from 1000 ℃, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 ℃ from 1200 ℃, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 ℃ from 1400 ℃, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 ℃ from 1640 ℃, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 ℃ from 1840 ℃, then be incubated 6 hours.
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| CN107877919A (en) * | 2017-12-20 | 2018-04-06 | 镇江华核装备有限公司 | A kind of structure of steel die of energy-efficient isostatic tooling |
| CN117680662A (en) * | 2024-02-04 | 2024-03-12 | 山西禧佑源民机完工中心有限公司 | Casting equipment for metal turbine blade of aviation aircraft |
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| CN104001913B (en) | 2016-04-20 |
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