CN104001913B - Tabletting type sealing device and prepare the method for large-scale molybdenum crucible - Google Patents
Tabletting type sealing device and prepare the method for large-scale molybdenum crucible Download PDFInfo
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Abstract
The method of the large-scale molybdenum crucible of preparation disclosed by the invention comprises chooses molybdenum powder, dress powder, die mould, rubber moulding disengaging, shaping, punching block disengaging and sintering seven steps; Tabletting type sealing device comprises punching block, rubber moulding, mould steel plug, stripper rings, screw etc.The method can successfully produce internal diameter 600 ~ 650mm, the large gauge molybdenum crucible product of height 1300 ~ 1400mm, wall thickness 18 ~ 22mm.Isostatic cool pressing is adopted to suppress in production process, 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 reclaimed can utilize by secondary, greatly reduces production cost.Tabletting type sealing device eliminates the risk because of compacting leakage generation waste material.The use of stripper rings, achieves the automatic demoulding of large-scale molybdenum crucible.Adopt progressively heating in sintering process, make the external diameter out-of-roundness of large-scale molybdenum crucible 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 in various high temperature industrial furnace and heater, and the fusing point of molybdenum is up to 2610 DEG C, and the serviceability temperature of molybdenum crucible is usually within 2000 DEG C.Because its production cost is well below tungsten crucible, therefore, under the hot environment within 2000 DEG C, molybdenum crucible substitutes the trend that tungsten crucible has become inevitable.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 gets more and more.Usually, diameter is called large-scale molybdenum crucible more than the molybdenum crucible of 500mm, the preparation that the powder metallurgic method of the small-sized molybdenum crucible of existing preparation cannot be indiscriminately imitated to large-scale molybdenum crucible comes up, because along with the increase of 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 usual employing splicing method or spraying process produce large-scale molybdenum crucible.
Splicing method is broken the whole up into parts by large-scale molybdenum crucible, first prepares the molybdenum product compared with small dimension, be then stitched together by the molybdenum product of above-mentioned small dimension, but this method machined splicing difficulty is comparatively large, and the stitching portion between two crucibles exists gap.
Spraying process be utilize high temperature, the powder particle through specially treated is ejected into graphite core mould surface by high speed flame stream, powder particle obtains the crucible product of given shape in mandrel surface deposition, but this method exists difficulty of processing is large, yield rate is low, production cost is high problem.
Summary of the invention
The object of the present invention is to provide a kind of method preparing large-scale molybdenum crucible, without the need to splicing, one-shot forming just can produce the large-scale molybdenum crucible of 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, Zhuan Fen district is formed between rubber moulding and punching block, 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 lower end of punching block and the upper end of mould steel plug are respectively arranged with the first extension, the two ends up and down of rubber moulding are respectively arranged with the second extension, first extension of relevant position and the second extension are superimposed with each other and together stretch in snap close, first extension and the second extension are fixed through snap close by lock screw, are provided with intermediate plate between lock screw and the second extension; Punching block bottom outside one week uniform intervals is provided with several stripper rings, and 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: the method preparing large-scale molybdenum crucible, comprises the steps:
The first step, chooses molybdenum powder
Choose that particle mean size is 3.2 μm ~ 3.8 μm, pine is than being 1.05 ~ 1.2g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder first step chosen loads in tabletting type sealing device, and the quality loading molybdenum powder is 750 ~ 850kg;
3rd step, die mould
Cold isostatic press put into by tabletting type sealing device second step being installed molybdenum powder, 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;
4th step, rubber moulding departs from
Separate opening lock catch, slough rubber moulding, expose the molybdenum crucible pressed compact formed at place of Zhuan Fen district;
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, ensures the profile rule impulse-free robustness of molybdenum crucible pressed compact;
6th step, the punching block demoulding
Stripper bolt is inserted in the screw of stripper rings respectively, then hangs stripper bolt with crane, slowly mention, molybdenum crucible pressed compact is separated with punching block;
7th step, sintering
The molybdenum crucible pressed compact 6th step being sloughed punching block drops in intermediate frequency furnace, adopts the method progressively heated to heat molybdenum crucible pressed compact, obtained molybdenum crucible.
Feature of the present invention is also,
The method progressively heated in 7th step is: first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 DEG C from 1840 DEG C, then be incubated 6 hours.
The invention has the beneficial effects as follows: the present invention prepares the method for large-scale molybdenum crucible, powder metallurgic method is adopted to prepare molybdenum crucible, can successfully produce internal diameter 600 ~ 650mm, height 1300 ~ 1400mm, the large gauge molybdenum crucible product of wall thickness 18 ~ 22mm, finished product inwall and outer wall smooth, outward appearance rule, seamless.Isostatic cool pressing is adopted to suppress in production process, 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 reclaimed can utilize by secondary, greatly reduces production cost.Adopt tabletting type sealing device in pressing process, eliminate the risk because of compacting leakage generation waste material.Suppress complete after finishing, use the stripper rings demoulding, achieve the automatic demoulding of large-scale molybdenum crucible, reduce operation easier, saved cost of labor.Adopt two-stage method sintering process in 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 is the structural representation of locking position in tabletting type sealing device of the present invention;
Fig. 3 be the present invention prepare slough rubber moulding in the method for large-scale molybdenum crucible after molybdenum crucible pressed compact be separated with punching block before structural representation.
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.
Detailed description of the invention
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, Zhuan Fen district 10 is formed between rubber moulding 1 and punching block 2, 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 lower end of punching block 2 and the upper end of mould steel plug 3 are 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, 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, first extension 7 and the second extension 8 are fixed through snap close 5 by lock screw 4, are provided with intermediate plate 6 between lock screw 4 and the second extension 8; Punching block 2 bottom outside one week uniform intervals is provided with stripper rings 11, and stripper rings 11 inside is provided with screw 12;
The wall thickness of rubber moulding 1 is 5 ~ 7mm.
Wherein, the through hole 9 that the sidewall of steel plug 3 and bottom are arranged makes pressure in isostatic cool pressing pressing process act directly on the surface of rubber moulding 1, can not cause mould steel plug 3 displacement and come 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 to stretch and stir in use.
Embodiment 1
Prepare the method for large-scale molybdenum crucible, comprise the steps:
The first step, chooses molybdenum powder
Choose that particle mean size is 3.2 μm, pine is than being 1.05g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder first step chosen loads in the Zhuan Fen district 10 of tabletting type sealing device, and the quality loading molybdenum powder is 750kg;
3rd step, die mould
Cold isostatic press put into by tabletting type sealing device second step being installed molybdenum powder, under the pressure of 180MPa, and pressurize 6 minutes, then release, then tabletting type sealing device is hung out from cold isostatic press;
4th step, rubber moulding departs from
Separate opening lock catch 5, slough rubber moulding 1, expose the molybdenum crucible pressed compact 14 formed at place of Zhuan Fen district 10, as shown in Figure 3;
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, ensures the profile rule impulse-free robustness of molybdenum crucible pressed compact 14;
6th step, the punching block demoulding
Stripper bolt 13 is inserted in the screw 12 of stripper rings 11 respectively, then hangs stripper bolt 13 with crane, slowly mention, molybdenum crucible pressed compact 14 is separated with punching block 2;
7th step, sintering
Drop in intermediate frequency furnace by the molybdenum crucible pressed compact 14 that the 6th step sloughs punching block 2, first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 DEG C from 1840 DEG C, then be incubated 6 hours, obtained molybdenum crucible.
The internal diameter of molybdenum crucible prepared by the present embodiment is 600mm, and yield rate more than 88%, and adopts spraying process to process the crucible of same size, and yield rate is about 50%.
Embodiment 2
Prepare the method for large-scale molybdenum crucible, comprise the steps:
The first step, chooses molybdenum powder
Choose that particle mean size is 3.8 μm, pine is than being 1.2g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder first step chosen loads in the Zhuan Fen district 10 of tabletting type sealing device, and the quality loading molybdenum powder is 850kg;
3rd step, die mould
Cold isostatic press put into by tabletting type sealing device second step being installed molybdenum powder, under the pressure of 200MPa, and pressurize 9 minutes, then release, then tabletting type sealing device is hung out from cold isostatic press;
4th step, rubber moulding departs from
Separate opening lock catch 5, slough rubber moulding 1, expose the molybdenum crucible pressed compact 14 formed at place of Zhuan Fen district 10;
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, ensures the profile rule impulse-free robustness of molybdenum crucible pressed compact 14;
6th step, the punching block demoulding
Stripper bolt 13 is inserted in the screw 12 of stripper rings 11 respectively, then hangs stripper bolt 13 with crane, slowly mention, molybdenum crucible pressed compact 14 is separated with punching block 2;
7th step, sintering
Drop in intermediate frequency furnace by the molybdenum crucible pressed compact 14 that the 6th step sloughs punching block 2, first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 DEG C from 1840 DEG C, then be incubated 6 hours, obtained molybdenum crucible.
The internal diameter of molybdenum crucible prepared by the present embodiment is 650mm, and yield rate more than 85%, and adopts spraying process to process the crucible of same size, and yield rate is about 45%.
Embodiment 3
Prepare the method for large-scale molybdenum crucible, comprise the steps:
The first step, chooses molybdenum powder
Choose that particle mean size is 3.5 μm, pine is than being 1.1g/cm
3molybdenum powder;
Second step, dress powder
The molybdenum powder first step chosen loads in the Zhuan Fen district 10 of tabletting type sealing device, and the quality loading molybdenum powder is 800kg;
3rd step, die mould
Cold isostatic press put into by tabletting type sealing device second step being installed molybdenum powder, under the pressure of 190MPa, and pressurize 8 minutes, then release, then tabletting type sealing device is hung out from cold isostatic press;
4th step, rubber moulding departs from
Separate opening lock catch 5, slough rubber moulding 1, expose the molybdenum crucible pressed compact 14 formed at place of Zhuan Fen district 10;
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, ensures the profile rule impulse-free robustness of molybdenum crucible pressed compact 14;
6th step, the punching block demoulding
Stripper bolt 13 is inserted in the screw 12 of stripper rings 11 respectively, then hangs stripper bolt 13 with crane, slowly mention, molybdenum crucible pressed compact 14 is separated with punching block 2;
7th step, sintering
Drop in intermediate frequency furnace by the molybdenum crucible pressed compact 14 that the 6th step sloughs punching block 2, first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 DEG C from 1840 DEG C, then be incubated 6 hours, obtained molybdenum crucible.
The internal diameter of molybdenum crucible prepared by the present embodiment is 620mm, and yield rate more than 86%, and adopts spraying process to process the crucible of same size, and yield rate is about 48%.
The method of the large-scale molybdenum crucible of preparation of the present invention, can successfully produce internal diameter 600 ~ 650mm, the large gauge molybdenum crucible product of height 1300 ~ 1400mm, wall thickness 18 ~ 22mm, and finished product inwall and outer wall are smooth, and outward appearance is regular, seamless.Isostatic cool pressing is adopted to suppress in production process, 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 reclaimed can utilize by secondary, greatly reduces production cost.Tabletting type sealing device eliminates the risk because of compacting leakage generation waste material.The use of stripper rings, achieves the automatic demoulding of large-scale molybdenum crucible, reduces operation easier, has saved cost of labor.Adopt progressively heating sintering process in sintering process, make the external diameter out-of-roundness of large-scale molybdenum crucible lower than 2%.
Claims (4)
1. tabletting type sealing device, comprise columniform punching block (2), the arranged outside of described punching block (2) has columnar rubber moulding (1), it is characterized in that, Zhuan Fen district (10) is formed between described rubber moulding (1) and described punching block (2), the upper end of described rubber moulding (1) is provided with open-topped cylindrical mold steel plug (3), and sidewall and the bottom of described mould steel plug (3) are provided with some through holes (9), the lower end of described punching block (2) and the upper end of described mould steel plug (3) are 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), described first extension (7) and the second extension (8) are fixed through described snap close (5) by lock screw (4), intermediate plate (6) is provided with between described lock screw (4) and described second extension (8), described punching block (2) bottom outside one week uniform intervals is provided with several stripper rings (11), and described stripper rings (11) inside is provided with screw (12).
2. tabletting type sealing device as claimed in claim 1, it 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 that particle mean size is 3.2 μm ~ 3.8 μm, pine is than being 1.05 ~ 1.2g/cm
3molybdenum powder;
Second step, dress powder
In tabletting type sealing device described in the molybdenum powder first step chosen loads, the quality loading molybdenum powder is 750 ~ 850kg;
3rd step, die mould
Cold isostatic press put into by tabletting type sealing device second step being installed molybdenum powder, 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;
4th step, rubber moulding departs from
Separate opening lock catch (5), slough rubber moulding (1), expose the molybdenum crucible pressed compact (14) formed at Zhuan Fen district (10) place;
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), ensures the profile rule impulse-free robustness of molybdenum crucible pressed compact (14);
6th step, the punching block demoulding
Stripper bolt (13) is inserted respectively in the screw (12) of stripper rings (11), stripper bolt (13) is hung again with crane, slowly mention, molybdenum crucible pressed compact (14) is separated with punching block (2);
7th step, sintering
The molybdenum crucible pressed compact (14) 6th step being sloughed punching block (2) drops in intermediate frequency furnace, adopts the method progressively heated to heat molybdenum crucible pressed compact (14), obtained molybdenum crucible.
4. the method for the large-scale molybdenum crucible of preparation as claimed in claim 3, it is characterized in that, the method progressively heated described in the 7th step is: first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 DEG C from 1840 DEG C, then be incubated 6 hours.
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| CN104289714A (en) * | 2014-09-30 | 2015-01-21 | 苏州普京真空技术有限公司 | Preparation method of tungsten crucible for rare earth |
| CN106881463B (en) * | 2015-12-21 | 2019-06-28 | 成都虹波实业股份有限公司 | A kind of manufacturing method of tubular or cup-shaped tungsten product |
| 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 |
| CN117680662B (en) * | 2024-02-04 | 2024-04-09 | 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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| CN202490933U (en) * | 2012-03-07 | 2012-10-17 | 金堆城钼业股份有限公司 | Metal powder isostatic cool pressing forming mold |
| CN103170621B (en) * | 2013-03-26 | 2014-12-24 | 金堆城钼业股份有限公司 | Preparation method of large molybdenum rod blank |
| CN103157795B (en) * | 2013-03-26 | 2014-12-24 | 金堆城钼业股份有限公司 | Preparation method of large-scale molybdenum plate blank |
| CN203330400U (en) * | 2013-05-16 | 2013-12-11 | 常州市鼎亨机电设备有限公司 | Pressing device for metal powder |
| CN103277514B (en) * | 2013-05-30 | 2016-02-24 | 无锡市威海达机械制造有限公司 | The manufacturing process of cold isostatic press superhigh pressure sealing device and seal ring thereof |
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