CN101797639A - Device for directionally solidifying by locally and forcibly heating with resistance at high gradient - Google Patents
Device for directionally solidifying by locally and forcibly heating with resistance at high gradient Download PDFInfo
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- CN101797639A CN101797639A CN 201010142263 CN201010142263A CN101797639A CN 101797639 A CN101797639 A CN 101797639A CN 201010142263 CN201010142263 CN 201010142263 CN 201010142263 A CN201010142263 A CN 201010142263A CN 101797639 A CN101797639 A CN 101797639A
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Abstract
The invention relates to a device for directionally solidifying by locally and forcibly heating with resistance at high gradient, comprising an upper oven and a lower oven. A crucible, a resistance ring, a tungsten cylinder and a shielding layer are arranged in sequence from the center of the upper oven to the outside of the upper oven, and the crucible, the resistance ring and the tungsten cylinder are arranged in the shielding layer; power leads are respectively connected to the upper surfaces of both the tungsten cylinder and the resistance ring; the power lead of the tungsten cylinder and the power lead of the resistance wire are respectively and independently connected with a power supply and are used for wholly heating the sample in the crucible through the tungsten cylinder and partially and forcibly heating the sample in the crucible through the resistance ring which is arranged on the lower part of the crucible; and two thermocouples are respectively on the upper part and the lower part of the tungsten cylinder and are respectively used for measuring the temperature of the tungsten cylinder and the resistance ring. The device can wholly heat the sample and locally and forcibly heat the sample to ensure that the sample obtains the high-temperature gradient and can be fully melted on the front edge of the solid/liquid interface and can reduce the burning loss of the low melting point elements. In addition, the device can be used for more materials of different size and can eliminate the forced convection of the melt, which is caused by the traditional induction heating.
Description
Technical field
The present invention relates to the unidirectional solidification material preparation field, specifically is a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient.
Background technology
Directional solidification technique can make the material solidification tissue arrange by specific direction, obtains orientation and single crystal organization, improves material property.In the directional solidification process of material, high thermograde is the assurance that obtains ultra-fineization tissue, reduces component segregation, controls microscopic defect and distribute mutually.In addition, high-temperature gradient can improve withdrawing rate when guaranteeing to optimize solidified structure, thereby enhances productivity.Therefore, high thermograde is the target that apparatus for directional solidification is pursued.The developing history of directional solidification technique is exactly the history that improves constantly the apparatus for directional solidification thermograde.And the acquisition of big thermograde can be by strengthening the heating and cooling condition.Therefore, various countries scholar and the engineers and technicians method of having invented a series of raising solid/liquid interfaces temp gradient at front edge along these two thinkings.
At present, the directional freeze method of extensive use mainly contains rapid solidification method (HRS) and liquid metal cooling method (LMC) on industrial production.The HRS method is by induction or resistance heated sample to be carried out whole heat fused, foundry goods is shifted out from stove with certain withdrawing rate finish directional solidification then, and thermograde is 60～100 ℃/cm.The main distinction of LMC method and HRS is that cooling medium adopts low melting point liquid metal to force cooling, and thermograde can reach 100～300 ℃/cm.Yet HRS method and LMC method be because all be that sample is carried out fine melt, therefore, if improve the scaling loss that thermograde will cause low melting point element in the alloy by strengthening heating.Though the molten directional solidification method in high energy beam district can obtain high thermograde, still, only is applicable to the directional solidification of small size sample.For example, people such as the Zhang Jun of Northwestern Polytechnical University's solidification technology National Key Laboratory, Cui Chunjuan utilize the electron-beam floating zone melting directional solidification to prepare Si/TaSi
2The spontaneous compound field emmision material of eutectic, its thermograde is 350～500 ℃/cm.
Solidification technology National Key Laboratory of Northwestern Polytechnical University has developed a kind of novel directional solidification technique on the basis of LMC method---zone melting liquid metal cooling method ((ZMLMC)).The local heat technology makes the solid/liquid interfaces forward position be strengthened heating fully, thereby can obtain the thermograde up to 1300 ℃/cm.But under the withdrawing rate condition with higher, the regional induction heating mode that the ZMLMC method adopts is to the melting capacity hysteresis withdrawing rate of sample, thereby causes full pattern fully not melt, and this has just limited the further raising of cooldown rate.
The present invention is directed to the deficiency that LMC method and ZMLMC method exist, proposed a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient.This device combines the LMC method with zone-melting technique, not only can obtain the thermograde up to 600 ℃/cm, and has guaranteed that sample melts and reduced the scaling loss of low melting point element fully.In addition,, make the scope of application expand electrically non-conductive material to, and resistance heated can not cause forced convertion as eddy-current heating, can obtain stable crystal growth, thereby be convenient to solidification theory research owing to adopt resistance heated.
Summary of the invention
For overcome exist in the prior art or sample carried out whole heat fused cause thermograde lower; The deficiency that perhaps regional eddy-current heating can not fully melt sample the present invention proposes a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient.
The present invention includes power line, thermocouple, thermal insulation board, crystallizer, body of heater, liquid metal, pull system, crucible, tungsten tube and screen layer, body of heater comprises upper furnace body and lower furnace body, in lower furnace body, center by lower furnace body is outside, pull system and crystallizer are arranged successively, liquid metal is housed in crystallizer; The furnace bottom of lower furnace body passes in the pull system, links to each other with servomotor; Two cooling water inlets are arranged in the bottom of crystallizer; In upper furnace body, outside by the center of upper furnace body, crucible, tungsten tube and screen layer are arranged successively, crucible one end passes the centre bore of upper furnace body bottom, links to each other with the pull system that is positioned at the lower furnace body center; And the temperature by thermocouple measurement tungsten tube; It is characterized in that described device for directionally solidifying by locally and forcibly heating with resistance at high gradient also comprises resistance ring and tantalum electrode; Resistance ring is positioned at thermal insulation board top tungsten tube, is sleeved on the excircle of crucible; One end of tantalum electrode is connected with water-cooled power line on being fixed on the upper furnace body wall, and is fluted on the end face of the other end, and resistance ring not blind end embeds and constitutes the closed-loop path in this groove; Be connected to thermocouple on the resistance ring.
Described resistance ring is the sleeve that opening is arranged on the circumference.Do not interfere between resistance ring and tungsten tube and the crucible; Gapped between resistance ring and the thermal insulation board; The axis of resistance ring and the central lines of body of heater.
The power line of described tungsten tube independently is connected with power supply respectively with the power line of resistance ring.
The invention has the beneficial effects as follows: the present invention combines the advantage of ZMLMC method and HRS method,, the local strengthening heating is carried out in sample solid liquid interface forward position and is cooled off with liquid metal by resistance ring sample being carried out integral body heating by the tungsten tube.Whole heating guarantees that sample fully melts, even also not molten particle can not occur in sample like this when the high speed pull; The local strengthening heating in solid liquid interface forward position makes equipment that high thermograde can be provided, and therefore, the present invention is guaranteeing can to obtain high thermograde when sample melts fully.Concrete effect as shown in Table 1.Simultaneously the material of resistance ring, highly, thickness and internal diameter all can adjust according to the size and the needed thermograde of sample.
Because adopt resistance heated, this device is not only applicable to conductive material, also is applicable to electrically non-conductive materials such as pottery, semiconductor, ceramic matric composite.In addition, tungsten tube and resistance ring adopt two dc sources to power respectively, and both power can be regulated separately, thereby, convenient integral body heating and the local strengthening heating that realizes sample.Direct current supply has also guaranteed can not form electromagnetic distu in heating process, has reduced flowing of melt in the directional solidification process, is convenient to directional solidification theory research.
The different device for directionally solidifying of table one prepare sample fusing effect and directed situation compares
Description of drawings
Fig. 1 is the schematic diagram of institute of the present invention coupling apparatus.
Fig. 2 is the structural representation of resistance ring calandria of the present invention.
Fig. 3 is the vertical view of resistance ring calandria of the present invention.Wherein:
1. power line 2. thermocouples 3. thermal insulation boards 4. crystallizers 5. liquid metals 6. pull systems
7. lower furnace body 8. cooling water inlets 9. crucibles, 10. tungsten tubes 11. screen layers 12. samples
13. resistance ring 14. upper furnace bodies 15. tantalum electrodes
The specific embodiment
Embodiment one
Present embodiment is a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient, comprises power line 1, thermocouple 2, thermal insulation board 3, crystallizer 4, body of heater, liquid metal 5, pull system 6, crucible 9, tungsten tube 10, screen layer 11, resistance ring 13 and tantalum electrode 15.The alloy of present embodiment heating is the DZ125 directional solidification nickel-base high-temperature alloy, and the local strengthening temperature is 2000 ℃, and whole heating-up temperature is 1500 ℃, in the thermograde that guarantees to obtain on the basis that sample melts fully 600 ℃/cm.
Body of heater comprises upper furnace body 14 and lower furnace body 7, and is outside by the center of lower furnace body in lower furnace body 7, and pull system 6 and crystallizer 4 are arranged successively, and liquid metal 5 is housed in crystallizer 4; The furnace bottom of lower furnace body 7 passes in pull system 6, links to each other with servomotor; Two cooling water inlets 8 are arranged in the bottom of crystallizer 4.
In upper furnace body 14, outside by the center of upper furnace body, crucible 9, resistance ring 13, tungsten tube 10 and screen layer 11 are arranged successively, and crucible 9, resistance ring 13 and tungsten tube 10 all are positioned at screen layer 11.At the upper surface of tungsten tube 10 and resistance ring 13, there is power line 1 to pick out respectively; The power line of the power line of tungsten tube 10 and resistance ring 13 independently is connected with power supply respectively, and is positioned at sample 12 whole heating of crucible 9 by 10 pairs in tungsten tube, and sample 12 local strengthenings of the 13 pairs of crucibles of resistance ring by being positioned at crucible 9 bottoms heat.Crucible 9 one ends pass the centre bore of upper furnace body 14 bottoms, link to each other with the pull system 6 that is positioned at lower furnace body 7 centers.Two thermocouples 2 lay respectively at the bottom of tungsten tube 10 tops and resistance ring 13, are respectively applied for the temperature of measuring tungsten tube 10 and resistance ring 13.
Between upper furnace body 14 and lower furnace body 7, thermal insulation board 3 is arranged.
The resistance ring of making of tantalum 13 is the sleeve that opening is arranged on the circumference.The external diameter of resistance ring 13 is less than the internal diameter of tungsten tube 10, and internal diameter is greater than the external diameter of crucible 9.Resistance ring 13 be positioned at thermal insulation board top tungsten tube 10, be sleeved on the excircle of crucible 9, and do not interfere between resistance ring 13 and tungsten tube 10 and the crucible 9; Gapped between resistance ring and the thermal insulation board; The axis of resistance ring and the central lines of body of heater.The height of resistance ring 13 and thickness determine that according to the thermograde in temperature that is heated and solid/liquid interfaces forward position it determines that principle is that resistance ring 13 does not soften under needed thermograde.In the present embodiment, the height of resistance ring 13 is 10mm; The thickness of resistance ring 13 is 0.5mm.
During use, earlier with crucible 9 clampings in pull system 6, the placement center has the thermal insulation board 3 of through hole again, then alloy sample 12 is put into crucible 9, upper furnace body 14 falls and guarantee upper furnace body and lower furnace body concentric, thereby guarantee that crucible and heater are concentric, again four power lines 1 of heater are received on two dc sources after the last lower furnace body closure, open dc source then, carry out the integral body heating by 10 pairs of samples of tungsten tube 12, after sample reaches desired temperature, the input power of adjusting resistance ring 13 obtains temperature required gradient, then, pull system 6 downwards in immigration liquid metal cooling fluid 5 realizes directional solidification with sample 12 and crucible 9 by pull system 6 with the speed of setting.
According to the experimental design requirement, the alloy sample of a plurality of same compositions is carried out directional solidification according to different speed, obtain the style of organizing under the different growth rates, and further analyze the microstructure Evolution rule.According to final experimental result, the thermograde of this device is up to 600K/cm, and do not find that when withdrawing rate reaches 1mm/s the final sample that obtains does not have the existence of no cofusing particle.
Embodiment two
Present embodiment is a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient, comprises power line 1, thermocouple 2, thermal insulation board 3, crystallizer 4, body of heater, liquid metal 5, pull system 6, crucible 9, tungsten tube 10, screen layer 11, resistance ring 13 and tantalum electrode 15.The alloy of present embodiment heating is an AM3 single crystal super alloy alloy, and the local strengthening temperature is 1650 ℃, and whole heating-up temperature is 1500 ℃, in the thermograde that guarantees to obtain on the basis that sample melts fully 290 ℃/cm.
Body of heater comprises upper furnace body 14 and lower furnace body 7, and is outside by the center of lower furnace body in lower furnace body 7, and pull system 6 and crystallizer 4 are arranged successively, and liquid metal 5 is housed in crystallizer 4; The furnace bottom of lower furnace body 7 passes in pull system 6, links to each other with servomotor; Two cooling water inlets 8 are arranged in the bottom of crystallizer 4.
In upper furnace body 14, outside by the center of upper furnace body, crucible 9, resistance ring 13, tungsten tube 10 and screen layer 11 are arranged successively, and crucible 9, resistance ring 13 and tungsten tube 10 all are positioned at screen layer 11.At the upper surface of tungsten tube 10 and resistance ring 13, there is power line 1 to pick out respectively; The power line of the power line of tungsten tube 10 and resistance ring 13 independently is connected with power supply respectively, and is positioned at sample 12 whole heating of crucible 9 by 10 pairs in tungsten tube, and sample 12 local strengthenings of the 13 pairs of crucibles of resistance ring by being positioned at crucible 9 bottoms heat.Crucible 9 one ends pass the centre bore of upper furnace body 14 bottoms, link to each other with the pull system 6 that is positioned at lower furnace body 7 centers.Two thermocouples 2 lay respectively at the bottom of tungsten tube 10 tops and resistance ring 13, are respectively applied for the temperature of measuring tungsten tube 10 and resistance ring 13.
Between upper furnace body 14 and lower furnace body 7, thermal insulation board 3 is arranged.
The resistance ring of making of molybdenum 13 is the sleeve that opening is arranged on the circumference.The external diameter of resistance ring 13 is less than the internal diameter of tungsten tube 10, and internal diameter is greater than the external diameter of crucible 9.Resistance ring 13 be positioned at thermal insulation board top tungsten tube 10, be sleeved on the excircle of crucible 9, and do not interfere between resistance ring 13 and tungsten tube 10 and the crucible 9; Gapped between resistance ring and the thermal insulation board; The axis of resistance ring and the central lines of body of heater.The height of resistance ring 13 and thickness determine that according to the thermograde in temperature that is heated and liquid-solid boundary forward position it determines that principle is that resistance ring 13 does not soften under needed thermograde.In the present embodiment, the height of resistance ring 13 is 5mm; The thickness of resistance ring 13 is 1mm.
During use, earlier with crucible 9 clampings in pull system 6, the placement center has the thermal insulation board 3 of through hole again, then alloy sample is put into crucible 9, upper furnace body 14 falls and guarantee upper furnace body and lower furnace body concentric, thereby guarantee that crucible and heater are concentric, again four power lines 1 of heater are received on two dc sources after the last lower furnace body closure, open dc source then, carry out the integral body heating by 10 pairs of samples of tungsten tube 12, after sample reaches desired temperature, the input power of adjusting resistance ring 13 obtains temperature required gradient, then, pull system 6 downwards in immigration liquid metal cooling fluid 5 realizes directional solidification with sample 12 and crucible 9 by pull system 6 with the speed of setting.
According to the experimental design requirement, the alloy sample of a plurality of same compositions is carried out directional solidification according to different speed, obtain the style of organizing under the different growth rates, and further analyze the microstructure Evolution rule.According to final experimental result, the thermograde of this device is 290K/cm, and does not find that when withdrawing rate reaches 0.9mm/s the final sample that obtains does not have the existence of no cofusing particle.
Embodiment three
Present embodiment is a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient, comprises power line 1, thermocouple 2, thermal insulation board 3, crystallizer 4, body of heater, liquid metal 5, pull system 6, crucible 9, tungsten tube 10, screen layer 11, resistance ring 13 and tantalum electrode 15.The alloy of present embodiment heating is the DZ125 directional solidification nickel-base high-temperature alloy, and the local strengthening temperature is 2000 ℃, and whole heating-up temperature is 1500 ℃, in the thermograde that guarantees to obtain on the basis that sample melts fully 600 ℃/cm.
Body of heater comprises upper furnace body 14 and lower furnace body 7, and is outside by the center of lower furnace body in lower furnace body 7, and pull system 6 and crystallizer 4 are arranged successively, and liquid metal 5 is housed in crystallizer 4; The furnace bottom of lower furnace body 7 passes in pull system 6, links to each other with servomotor; Two cooling water inlets 8 are arranged in the bottom of crystallizer 4.
In upper furnace body 14, outside by the center of upper furnace body, crucible 9, resistance ring 13, tungsten tube 10 and screen layer 11 are arranged successively, and crucible 9, resistance ring 13 and tungsten tube 10 all are positioned at screen layer 11.At the upper surface of tungsten tube 10 and resistance ring 13, there is power line 1 to pick out respectively; The power line of the power line of tungsten tube 10 and resistance ring 13 independently is connected with power supply respectively, and is positioned at sample 12 whole heating of crucible 9 by 10 pairs in tungsten tube, and sample 12 local strengthenings of the 13 pairs of crucibles of resistance ring by being positioned at crucible 9 bottoms heat.Crucible 9 one ends pass the centre bore of upper furnace body 14 bottoms, link to each other with the pull system 6 that is positioned at lower furnace body 7 centers.Two thermocouples 2 lay respectively at the bottom of tungsten tube 10 tops and resistance ring 13, are respectively applied for the temperature of measuring tungsten tube 10 and resistance ring 13.
Between upper furnace body 14 and lower furnace body 7, thermal insulation board 3 is arranged.
The resistance ring of making of tungsten 13 is the sleeve that opening is arranged on the circumference.The external diameter of resistance ring 13 is less than the internal diameter of tungsten tube 10, and internal diameter is greater than the external diameter of crucible 9.Resistance ring 13 be positioned at thermal insulation board top tungsten tube 10, be sleeved on the excircle of crucible 9, and do not interfere between resistance ring 13 and tungsten tube 10 and the crucible 9; Gapped between resistance ring and the thermal insulation board; The axis of resistance ring and the central lines of body of heater.The height of resistance ring 13 and thickness determine that according to the thermograde in temperature that is heated and solid/liquid interfaces forward position it determines that principle is that resistance ring 13 does not soften under needed thermograde.In the present embodiment, the height of resistance ring 13 is 10mm; The thickness of resistance ring 13 is 0.5mm.
During use, earlier with crucible 9 clampings in pull system 6, the placement center has the thermal insulation board 3 of through hole again, then alloy sample 12 is put into crucible 9, fall upper furnace body 14 and guarantee upper furnace body and thereby lower furnace body guarantees that with one heart crucible and heater are concentric, again four power lines 1 of heater are received on two dc sources after the last lower furnace body closure, open dc source then, carry out the integral body heating by 10 pairs of samples of tungsten tube 12, after sample reaches desired temperature, the input power of adjusting resistance ring 13 obtains temperature required gradient, then, pull system 6 downwards in immigration liquid metal cooling fluid 5 realizes directional solidification with sample 12 and crucible 9 by pull system 6 with the speed of setting.
According to the experimental design requirement, the alloy sample of a plurality of same compositions is carried out directional solidification according to different speed, obtain the style of organizing under the different growth rates, and further analyze the microstructure Evolution rule.According to final experimental result, the thermograde of this device is up to 600K/cm, and do not find that when withdrawing rate reaches 1mm/s the final sample that obtains does not have the existence of no cofusing particle.
Embodiment four
Present embodiment is a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient, comprises power line 1, thermocouple 2, thermal insulation board 3, crystallizer 4, body of heater, liquid metal 5, pull system 6, crucible 9, tungsten tube 10, screen layer 11, resistance ring 13 and tantalum electrode 15.The alloy of present embodiment heating is the DZ125 directional solidification nickel-base high-temperature alloy, and the local strengthening temperature is 1500 ℃, and whole heating-up temperature is 1500 ℃, in the thermograde that guarantees to obtain on the basis that sample melts fully 120 ℃/cm.
Body of heater comprises upper furnace body 14 and lower furnace body 7, and is outside by the center of lower furnace body in lower furnace body 7, and pull system 6 and crystallizer 4 are arranged successively, and liquid metal 5 is housed in crystallizer 4; The furnace bottom of lower furnace body 7 passes in pull system 6, links to each other with servomotor; Two cooling water inlets 8 are arranged in the bottom of crystallizer 4.
In upper furnace body 14, outside by the center of upper furnace body, crucible 9, resistance ring 13, tungsten tube 10 and screen layer 11 are arranged successively, and crucible 9, resistance ring 13 and tungsten tube 10 all are positioned at screen layer 11.At the upper surface of tungsten tube 10 and resistance ring 13, there is power line 1 to pick out respectively; The power line of the power line of tungsten tube 10 and resistance ring 13 independently is connected with power supply respectively, and is positioned at sample 12 whole heating of crucible 9 by 10 pairs in tungsten tube, and sample 12 local strengthenings of the 13 pairs of crucibles of resistance ring by being positioned at crucible 9 bottoms heat.Crucible 9 one ends pass the centre bore of upper furnace body 14 bottoms, link to each other with the pull system 6 that is positioned at lower furnace body 7 centers.Two thermocouples 2 lay respectively at the bottom of tungsten tube 10 tops and resistance ring 13, are respectively applied for the temperature of measuring tungsten tube 10 and resistance ring 13.
Between upper furnace body 14 and lower furnace body 7, thermal insulation board 3 is arranged.
The resistance ring of making of graphite 13 is the sleeve that opening is arranged on the circumference.The external diameter of resistance ring 13 is less than the internal diameter of tungsten tube 10, and internal diameter is greater than the external diameter of crucible 9.Resistance ring 13 be positioned at thermal insulation board top tungsten tube 10, be sleeved on the excircle of crucible 9, and do not interfere between resistance ring 13 and tungsten tube 10 and the crucible 9; Gapped between resistance ring and the thermal insulation board; The axis of resistance ring and the central lines of body of heater.The height of resistance ring 13 and thickness determine that according to the thermograde in temperature that is heated and liquid-solid boundary forward position it determines that principle is that resistance ring 13 does not soften under needed thermograde.In the present embodiment, the height of resistance ring 13 is 5mm; The thickness of resistance ring 13 is 0.5mm.
During use, earlier with crucible 9 clampings in pull system 6, the placement center has the thermal insulation board 3 of through hole again, then alloy sample is put into crucible 9, upper furnace body 14 falls and guarantee upper furnace body and lower furnace body concentric, thereby guarantee that crucible and heater are concentric, again four power lines 1 of heater are received on two dc sources after the last lower furnace body closure, open dc source then, carry out the integral body heating by 10 pairs of samples of tungsten tube, after sample reaches desired temperature, the input power of adjusting resistance ring 13 obtains temperature required gradient, then, pull system 6 downwards in immigration liquid metal cooling fluid 5 realizes directional solidification with sample 12 and crucible 9 by pull system 6 with the speed of setting.
According to the experimental design requirement, the alloy sample of a plurality of same compositions is carried out directional solidification according to different speed, obtain the style of organizing under the different growth rates, and further analyze the microstructure Evolution rule.According to final experimental result, the thermograde of this device reaches as high as 120 ℃/cm, and does not find that when withdrawing rate reaches 0.8mm/s the final sample that obtains does not have the existence of no cofusing particle.
Embodiment five
Present embodiment is a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient, comprises power line 1, thermocouple 2, thermal insulation board 3, crystallizer 4, body of heater, liquid metal 5, pull system 6, crucible 9, tungsten tube 10, screen layer 11, resistance ring 13 and tantalum electrode 15.The alloy of present embodiment heating is the DZ125 directional solidification nickel-base high-temperature alloy, and the local strengthening temperature is 1500 ℃, and whole heating-up temperature is 1500 ℃, in the thermograde that guarantees to obtain on the basis that sample melts fully 120 ℃/cm.
Body of heater comprises upper furnace body 14 and lower furnace body 7, and is outside by the center of lower furnace body in lower furnace body 7, and pull system 6 and crystallizer 4 are arranged successively, and liquid metal 5 is housed in crystallizer 4; The furnace bottom of lower furnace body 7 passes in pull system 6, links to each other with servomotor; Two cooling water inlets 8 are arranged in the bottom of crystallizer 4.
In upper furnace body 14, outside by the center of upper furnace body, crucible 9, resistance ring 13, tungsten tube 10 and screen layer 11 are arranged successively, and crucible 9, resistance ring 13 and tungsten tube 10 all are positioned at screen layer 11.At the upper surface of tungsten tube 10 and resistance ring 13, there is power line 1 to pick out respectively; The power line of the power line of tungsten tube 10 and resistance ring 13 independently is connected with power supply respectively, and is positioned at sample 12 whole heating of crucible 9 by 10 pairs in tungsten tube, and sample 12 local strengthenings of the 13 pairs of crucibles of resistance ring by being positioned at crucible 9 bottoms heat.Crucible 9 one ends pass the centre bore of upper furnace body 14 bottoms, link to each other with the pull system 6 that is positioned at lower furnace body 7 centers.Two thermocouples 2 lay respectively at the bottom of tungsten tube 10 tops and resistance ring 13, are respectively applied for the temperature of measuring tungsten tube 10 and resistance ring 13.
Between upper furnace body 14 and lower furnace body 7, thermal insulation board 3 is arranged.
The resistance ring of making of the silicon molybdenum compound 13 is the sleeve that opening is arranged on the circumference.The external diameter of resistance ring 13 is less than the internal diameter of tungsten tube 10, and internal diameter is greater than the external diameter of crucible 9.Resistance ring 13 be positioned at thermal insulation board top tungsten tube 10, be sleeved on the excircle of crucible 9, and do not interfere between resistance ring 13 and tungsten tube 10 and the crucible 9; Gapped between resistance ring and the thermal insulation board; The axis of resistance ring and the central lines of body of heater.The height of resistance ring 13 and thickness determine that according to the thermograde in temperature that is heated and liquid-solid boundary forward position it determines that principle is that resistance ring 13 does not soften under needed thermograde.In the present embodiment, the height of resistance ring 13 is 5mm; The thickness of resistance ring 13 is 0.5mm.
During use, earlier with crucible 9 clampings in pull system 6, the placement center has the thermal insulation board 3 of through hole again, then alloy sample is put into crucible 9, fall upper furnace body 14 and guarantee upper furnace body and thereby lower furnace body guarantees that with one heart crucible and heater are concentric, again four power lines 1 of heater are received on two dc sources after the last lower furnace body closure, open dc source then, carry out the integral body heating by 10 pairs of samples of tungsten tube, after sample reaches desired temperature, the input power of adjusting resistance ring 13 obtains temperature required gradient, then, pull system 6 downwards in immigration liquid metal cooling fluid 5 realizes directional solidification with sample 12 and crucible 9 by pull system 6 with the speed of setting.
According to the experimental design requirement, the alloy sample of a plurality of same compositions is carried out directional solidification according to different speed, obtain the style of organizing under the different growth rates, and further analyze the microstructure Evolution rule.According to final experimental result, the thermograde of this device reaches as high as 120 ℃/cm, and does not find that when withdrawing rate reaches 0.8mm/s the final sample that obtains does not have the existence of no cofusing particle.
Embodiment six
Present embodiment is a kind of device for directionally solidifying by locally and forcibly heating with resistance at high gradient, comprises power line 1, thermocouple 2, thermal insulation board 3, crystallizer 4, body of heater, liquid metal 5, pull system 6, crucible 9, tungsten tube 10, screen layer 11, resistance ring 13 and tantalum electrode 15.The alloy of present embodiment heating is the DZ125 directional solidification nickel-base high-temperature alloy, and the local strengthening temperature is 1200 ℃, and whole heating-up temperature is 1200 ℃, in the thermograde that guarantees to obtain on the basis that sample melts fully 90 ℃/cm.
Body of heater comprises upper furnace body 14 and lower furnace body 7, and is outside by the center of lower furnace body in lower furnace body 7, and pull system 6 and crystallizer 4 are arranged successively, and liquid metal 5 is housed in crystallizer 4; The furnace bottom of lower furnace body 7 passes in pull system 6, links to each other with servomotor; Two cooling water inlets 8 are arranged in the bottom of crystallizer 4.
In upper furnace body 14, outside by the center of upper furnace body, crucible 9, resistance ring 13, tungsten tube 10 and screen layer 11 are arranged successively, and crucible 9, resistance ring 13 and tungsten tube 10 all are positioned at screen layer 11.At the upper surface of tungsten tube 10 and resistance ring 13, there is power line 1 to pick out respectively; The power line of the power line of tungsten tube 10 and resistance ring 13 independently is connected with power supply respectively, and is positioned at sample 12 whole heating of crucible 9 by 10 pairs in tungsten tube, and sample 12 local strengthenings of the 13 pairs of crucibles of resistance ring by being positioned at crucible 9 bottoms heat.Crucible 9 one ends pass the centre bore of upper furnace body 14 bottoms, link to each other with the pull system 6 that is positioned at lower furnace body 7 centers.Two thermocouples 2 lay respectively at the bottom of tungsten tube 10 tops and resistance ring 13, are respectively applied for the temperature of measuring tungsten tube 10 and resistance ring 13.
Between upper furnace body 14 and lower furnace body 7, thermal insulation board 3 is arranged.
The resistance ring of making of nichrome 13 is the sleeve that opening is arranged on the circumference.The external diameter of resistance ring 13 is less than the internal diameter of tungsten tube 10, and internal diameter is greater than the external diameter of crucible 9.Resistance ring 13 be positioned at thermal insulation board top tungsten tube 10, be sleeved on the excircle of crucible 9, and do not interfere between resistance ring 13 and tungsten tube 10 and the crucible 9; Gapped between resistance ring and the thermal insulation board; The axis of resistance ring and the central lines of body of heater.The height of resistance ring 13 and thickness determine that according to the thermograde in temperature that is heated and liquid-solid boundary forward position it determines that principle is that resistance ring 13 does not soften under needed thermograde.In the present embodiment, the height of resistance ring 13 is 5mm; The thickness of resistance ring 13 is 0.5mm.
During use, earlier with crucible 9 clampings in pull system 6, the placement center has the thermal insulation board 3 of through hole again, then alloy sample is put into crucible 9, fall upper furnace body 14 and guarantee upper furnace body and thereby lower furnace body guarantees that with one heart crucible and heater are concentric, again four power lines 1 of heater are received on two dc sources after the last lower furnace body closure, open dc source then, carry out the integral body heating by 10 pairs of samples of tungsten tube, after sample reaches desired temperature, the input power of adjusting resistance ring 13 obtains temperature required gradient, then, pull system 6 downwards in immigration liquid metal cooling fluid 5 realizes directional solidification with sample 12 and crucible 9 by pull system 6 with the speed of setting.
According to the experimental design requirement, the alloy sample of a plurality of same compositions is carried out directional solidification according to different speed, obtain the style of organizing under the different growth rates, and further analyze the microstructure Evolution rule.According to final experimental result, the thermograde of this device reaches as high as 90 ℃/cm, and does not find that when withdrawing rate reaches 0.8mm/s the final sample that obtains does not have the existence of no cofusing particle.
Claims (4)
1. device for directionally solidifying by locally and forcibly heating with resistance at high gradient, comprise power line (1), thermocouple (2), thermal insulation board (3), crystallizer (4), body of heater, liquid metal (5), pull system (6), crucible (9), tungsten tube (10) and screen layer (11), body of heater comprises upper furnace body (14) and lower furnace body (7), in lower furnace body (7), center by lower furnace body is outside, pull system (6) and crystallizer (4) are arranged successively, liquid metal (5) is housed in crystallizer (4); The furnace bottom of lower furnace body (7) passes in pull system (6), links to each other with servomotor; In the bottom of crystallizer (4) two cooling water inlets 8 are arranged; In upper furnace body (14), outside by the center of upper furnace body, crucible (9), tungsten tube (10) and screen layer (11) are arranged successively, crucible (9) one ends pass the centre bore of upper furnace body (14) bottom, link to each other with the pull system (6) that is positioned at lower furnace body (7) center; And measure the temperature of tungsten tube (10) by thermocouple (2); It is characterized in that described device for directionally solidifying by locally and forcibly heating with resistance at high gradient also comprises resistance ring (13) and tantalum electrode (15); Resistance ring (13) is positioned at thermal insulation board (3) top tungsten tube (10), is sleeved on the excircle of crucible (9); One end of tantalum electrode (15) is connected with power line; Fluted on the end face of tantalum electrode (15) other end, resistance ring (13) not blind end embeds formation closed-loop path in this groove; Be connected to thermocouple (2) on the resistance ring (13).
2. a kind of according to claim 1 device for directionally solidifying by locally and forcibly heating with resistance at high gradient is characterized in that, described resistance ring (13) is for there being the sleeve of opening on the circumference.
3. a kind of according to claim 1 device for directionally solidifying by locally and forcibly heating with resistance at high gradient is characterized in that, does not interfere between resistance ring (13) and tungsten tube (10) and the crucible (9); Gapped between resistance ring (13) and the thermal insulation board; The axis of resistance ring (13) and the central lines of body of heater.
4. a kind of according to claim 1 device for directionally solidifying by locally and forcibly heating with resistance at high gradient is characterized in that, the power line of tungsten tube (10) independently is connected with power supply respectively with the power line of resistance ring (13).
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