CN114178500A - Preparation device and method of high-performance platinum and platinum-rhodium thermocouple wire - Google Patents
Preparation device and method of high-performance platinum and platinum-rhodium thermocouple wire Download PDFInfo
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- CN114178500A CN114178500A CN202111213003.XA CN202111213003A CN114178500A CN 114178500 A CN114178500 A CN 114178500A CN 202111213003 A CN202111213003 A CN 202111213003A CN 114178500 A CN114178500 A CN 114178500A
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 70
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 44
- 239000000956 alloy Substances 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000003723 Smelting Methods 0.000 claims abstract description 15
- 229910000629 Rh alloy Inorganic materials 0.000 claims abstract description 14
- 239000000498 cooling water Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 46
- 230000006698 induction Effects 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000004744 fabric Substances 0.000 claims description 19
- 239000003365 glass fiber Substances 0.000 claims description 19
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 239000004570 mortar (masonry) Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- DECCZIUVGMLHKQ-UHFFFAOYSA-N rhenium tungsten Chemical compound [W].[Re] DECCZIUVGMLHKQ-UHFFFAOYSA-N 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 230000007547 defect Effects 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 6
- 238000007711 solidification Methods 0.000 abstract description 4
- 230000008023 solidification Effects 0.000 abstract description 4
- 238000005266 casting Methods 0.000 abstract description 2
- 238000005242 forging Methods 0.000 abstract description 2
- 238000005096 rolling process Methods 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000009851 ferrous metallurgy Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/14—Plants for continuous casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/08—Accessories for starting the casting procedure
- B22D11/081—Starter bars
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/12—Accessories for subsequent treating or working cast stock in situ
- B22D11/124—Accessories for subsequent treating or working cast stock in situ for cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/16—Controlling or regulating processes or operations
- B22D11/18—Controlling or regulating processes or operations for pouring
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a preparation device and a preparation method of high-performance platinum and platinum-rhodium thermocouple wires, wherein a smelting device is used for melting platinum-rhodium alloy materials; the crystallizer is used for controlling the position of a solid-liquid interface; the dummy bar is used for pulling the ingot and pulling the ingot out of the crystallizer at a preset speed through the pulling device; the cooling device rapidly cools the ingot casting by spraying cooling water. The one-dimensional gradient heat transfer is realized by combining the heating of the crystallizer and the chilling of cooling water, the dummy bar is skillfully combined with the drawing device, the directional solidification of the platinum-rhodium alloy is realized, and the prepared platinum and platinum-rhodium thermocouple wire has good room-temperature plasticity, good high-temperature plasticity and higher high-temperature strength at the same time, and has no influence on the purity of the thermocouple wire; the cast ingot prepared by the device is in a round rod shape, has a smooth surface, does not need mechanical processing such as forging, rolling and the like, can be directly drawn through a die, simplifies the processing procedure and reduces the processing loss.
Description
Technical Field
The invention relates to a device and a method for preparing a high-performance platinum and platinum-rhodium thermocouple wire, in particular to a device and a method for preparing a platinum and platinum-rhodium thermocouple wire, which are used for improving the stability, plasticity and high-temperature strength of the platinum-rhodium thermocouple wire, and belong to the technical field of metal smelting.
Background
The platinum-rhodium thermocouple wire is widely applied to the industries of aerospace, ferrous metallurgy and the like due to the excellent thermoelectric property. Due to the rising price of raw materials, in order to save cost, the platinum-rhodium thermocouple wire is forced to be thinner, from 0.07-0.08 mm of thin wire before 2005 to 0.04-0.06 mm of thin wire between 2006-2020, and then to the extremely thin wire less than 0.04mm in 2021 at present, the wire diameter of the thermocouple wire is changed in a ground-covering manner.
Along with these changes, a number of new technical problems arise: firstly, the wire drawing and breaking rate is high; the mechanical property of the completely annealed state is poor; and the formation rate of the thermocouple is low. The high wire breakage rate is related to the plasticity variation under the extremely fine wire diameter, and the poor mechanical property in the complete annealing state and the low thermocouple measurement rate are related to the low high-temperature strength.
In the prior art, dispersion strengthening or solid solution and gap strengthening is often adopted as methods for improving the strength of materials, but the methods can reduce the plasticity of the materials while improving the strength, and can affect the purity of the materials, thereby further affecting the thermoelectric force.
Disclosure of Invention
The invention provides a device and a method for preparing a high-performance platinum and platinum-rhodium thermocouple wire, aiming at overcoming the defects in the prior art, and realizing the preparation of columnar crystal or even single crystal tissue by directional solidification, so that the plasticity and high-temperature mechanical property of the platinum and platinum-rhodium thermocouple wire are improved, the mechanical property of the material can be improved without adding a reinforcer, and the purity and the temperature measurement performance of the material are not influenced.
The technical solution of the invention is as follows: a high-performance platinum and platinum-rhodium thermocouple wire preparation device structurally comprises a reaction furnace, a smelting device, a crystallizer, a dummy bar, a thermocouple, a drawing device, a cooling device and a plug bar, wherein the inner cavity of the reaction furnace is a sealed cavity with a furnace cover, the smelting device is installed in the reaction furnace and comprises a crucible, the crystallizer is arranged under the crucible and communicated with the bottom of the crucible, the upper end of the plug bar is connected with a pull rod, the lower end of the plug bar is positioned at the inner bottom of the crucible, the pull rod movably penetrates through the furnace cover at the top of the reaction furnace in a lifting mode, the upper end of the dummy bar extends into the inner bottom of the crystallizer, the drawing device is connected with the lower end of the dummy bar, the cooling device is arranged on the side face of the dummy bar outside the lower outlet of the crystallizer, and the temperature measuring ends of the thermocouple are respectively positioned at the crystallizer and in the upper end of the dummy bar.
Preferably, the smelting device further comprises an induction coil, glass fiber cloth and refractory mortar, the glass fiber cloth is wrapped outside the crucible, the refractory mortar is filled between the crucible and the glass fiber cloth, and the glass fiber cloth surrounds the inner wall of the induction coil.
Preferably, the crystallizer include heater strip and zirconia pipe, the heater strip evenly twines in the zirconia pipe outside, the zirconia pipe outside also is wrapped up by glass fiber cloth, fills the fire clay between zirconia pipe and the glass fiber cloth.
Preferably, the number of the cooling devices is four, and the cooling devices are water-cooling jet cooling devices and are arranged at positions 10-50 mm away from the lower outlet of the crystallizer and respectively correspond to the front, the rear, the left and the right of the dummy bar.
Preferably, the temperature measuring end of the thermocouple is positioned at the heating wire of the crystallizer.
Preferably, the reaction furnace further comprises a water cooling machine, a vacuum pump and a gas cylinder, wherein the water cooling machine is connected with the induction coil through a pipeline, the vacuum pump is connected with the inner cavity of the reaction furnace through a pipeline, and the gas cylinder is connected with the inner cavity of the reaction furnace through a pipeline.
Preferably, the induction coil is formed by winding a copper tube with a hollow channel, and the hollow channel of the copper tube is communicated with the water cooling machine through a pipeline.
Preferably, the crucible is a zirconia crucible, the diameter of a crucible opening of the crucible is phi 80mm, the diameter of a crucible bottom of the crucible is phi 8mm, the depth of the crucible is 140mm, the crucible is funnel-shaped, an inclined plane of the crucible bottom of the crucible is 63 degrees, the refractory mortar is formed by bonding and mixing alumina powder and water, the plug rod is made of zirconia, the heating wire is a tungsten wire with phi 2.0mm, the thermocouple is a tungsten-rhenium thermocouple, the dummy bar is a round rod with phi 8mm, and the material of the dummy bar is the same as that of a thermocouple wire fused in the crucible.
A preparation method of a preparation device of a high-performance platinum and platinum rhodium thermocouple wire comprises the following steps:
step one, plugging the bottom of a crucible by a plug rod, and then placing a platinum-rhodium alloy material in the crucible 14;
closing a furnace cover of the reaction furnace, starting a water cooling machine, increasing the power of the induction coil to melt the alloy material in the crucible, and simultaneously electrifying a heating wire to heat the crystallizer to the platinum-rhodium alloy melting point temperature;
step three, reducing the power of the induction coil to ensure that the alloy melt is in a heat preservation state and the components are uniform, and simultaneously starting a vacuum pump to vacuumize the inner cavity of the reaction furnace to 1 multiplied by 10-6Pa, then filling protective gas to ensure that the internal pressure is the same as the external pressure;
inserting the dummy bar into the crystallizer, starting a cooling device to spray cooling water towards the dummy bar, then pulling the pull bar upwards, pulling the plug bar out of the crucible, and enabling the alloy melt to flow into the crystallizer;
regulating the temperature of the crystallizer according to the thermocouple display temperature in the dummy bar, regulating the position of a solid-liquid interface and ensuring that the surface of the pulled ingot is bright, flat and free of defects;
sixthly, opening the drawing device to draw the solidified alloy part out of the crucible, and rapidly cooling the solidified alloy part through cooling water;
step seven, immediately closing the current of the induction coil and the heating wire after the ingot is completely pulled out of the crystallizer, and keeping the water cooling machine in an opening state;
and step eight, cutting the cast ingot from the dummy bar after the cast ingot is fully cooled, and closing the water cooling machine after the crucible is fully cooled.
Preferably, the weight of the platinum-rhodium alloy material in the first step is controlled to be 1-4 kg, the protective gas in the third step is argon, helium or nitrogen, the position of a solid-liquid interface in the fifth step is adjusted to be 10-50 mm away from a lower outlet of a crystallizer, and the drawing device in the sixth step draws the solidified alloy part out of the crucible at a preset speed of 1-20 mm/s.
The invention has the advantages that: the structure and the method are reasonable in design, and the smelting device is used for melting the platinum-rhodium alloy material; the crystallizer is used for controlling the position of a solid-liquid interface; the dummy bar is used for pulling the ingot and pulling the ingot out of the crystallizer at a preset speed through the pulling device; the cooling device rapidly cools the ingot casting by spraying cooling water. The one-dimensional gradient heat transfer is realized by combining the heating of the crystallizer and the chilling of cooling water, the dummy bar is skillfully combined with the drawing device, the directional solidification of the platinum-rhodium alloy is realized, and the prepared platinum and platinum-rhodium thermocouple wire has good room-temperature plasticity, good high-temperature plasticity and higher high-temperature strength at the same time, and has no influence on the purity of the thermocouple wire; the cast ingot prepared by the device is in a round rod shape, has a smooth surface, does not need mechanical processing such as forging, rolling and the like, can be directly drawn through a die, simplifies the processing procedure and reduces the processing loss.
Drawings
FIG. 1 is a schematic structural diagram of a high-performance platinum and platinum-rhodium thermocouple wire manufacturing device according to the present invention.
Fig. 2 is a schematic view of the smelting unit and the crystallizer of fig. 1.
FIG. 3 is a graph comparing the performance of a pure platinum couple wire with a diameter of 0.04mm prepared by the present invention and the prior art.
In the figure, 1 is a reaction furnace, 2 is a melting device, 3 is a crystallizer, 4 is a dummy bar, 5 is a thermocouple, 6 is a drawing device, 7 is a cooling device, 8 is a plug bar, 9 is a draw bar, 10 is a water cooler, 11 is a vacuum pump, 12 is a gas cylinder, 13 is an induction coil, 14 is a crucible, 15 is glass fiber cloth, 16 is refractory mortar, 17 is a heating wire, and 18 is a zirconia round tube.
Detailed Description
The present invention will be described in further detail with reference to examples and specific embodiments.
As shown in fig. 1 and 2, a high-performance platinum and platinum rhodium thermocouple wire manufacturing device structurally comprises a reaction furnace 1, a smelting device 2, a crystallizer 3, a dummy bar 4, a thermocouple 5, a drawing device 6, a cooling device 7 and a stopper rod 8.
Wherein the inner cavity of the reaction furnace 1 is a sealed chamber with a furnace cover.
The smelting device 2 is arranged in the reaction furnace 1 and comprises an induction coil 13, a crucible 14, glass fiber cloth 15 and refractory mortar 16, the glass fiber cloth 15 wraps the crucible 14, the refractory mortar 16 is filled between the crucible 14 and the glass fiber cloth 15, the glass fiber cloth 15 surrounds the inner wall of the induction coil 13, and the smelting device 2 is used for smelting platinum-rhodium alloy materials.
The crystallizer 3 is arranged under the crucible 14 and communicated with the bottom of the crucible 14, and comprises a heating wire 17 and a zirconia circular tube 18, the heating wire 17 is uniformly wound on the outer side of the zirconia circular tube 18, the outer side of the zirconia circular tube 18 is also wrapped by glass fiber cloth 15, refractory mortar 16 is filled between the zirconia circular tube 18 and the glass fiber cloth 15, and the crystallizer 3 controls the position of a solid-liquid interface by adjusting the temperature.
The upper end of the plug rod 8 is connected with a pull rod 9, the lower end of the plug rod is positioned at the bottom in the crucible 14, the pull rod 9 penetrates through a furnace cover at the top of the reaction furnace 1 and can move up and down, and the plug rod 8 and the pull rod 9 are combined to control the communication between the crucible 14 and the crystallizer 3.
The upper end of the dummy bar 4 extends into the bottom in the crystallizer 3 and is used for blocking the lower outlet of the crystallizer 3 and drawing the cast ingot.
The drawing device 6 is connected to the lower end of the dummy bar 4, and draws the alloy solidified portion out of the crucible 14 through the dummy bar 4 at a predetermined speed.
Four cooling devices 7 are water-cooling jet cooling devices, are arranged at the positions 10-50 mm away from the lower outlet of the crystallizer 3, are respectively positioned at the front, back, left and right directions of the dummy bar 4, and are used for rapidly cooling the cast ingot by jet cooling pure water.
The temperature measuring ends of the thermocouples 5 are respectively positioned near the heating wire 17 and inside the upper end of the dummy bar 4 and are used for measuring the temperatures of the two positions.
Wherein, the crucible 14 is preferably a zirconia or magnesia crucible, the diameter of the crucible opening is phi 80mm, the diameter of the crucible bottom is phi 8mm, the crucible depth is 140mm, the crucible is funnel-shaped, alloy melt can conveniently flow into the crystallizer 3, and the inclined plane is 63 degrees with the ground. The refractory mortar 16 is formed by bonding and mixing alumina powder and water, the plug rod 8 is made of zirconia, the heating wire 17 is a tungsten filament with the diameter of 2.0mm, the thermocouple 5 is a tungsten-rhenium thermocouple, the dummy bar 4 is a round rod with the diameter of 8mm, and the material of the dummy bar is the same as that of the fused couple filament.
Preferably, the system further comprises a water cooler 10, a vacuum pump 11 and a gas cylinder 12.
The water cooler 10 is connected to a water-cooling jacket layer (not shown) and the induction coil 13 in the reaction furnace 1 through pipes, and cools the water-cooling jacket layer and the induction coil 13 in the reaction furnace 1.
The vacuum pump 11 is connected with the inner cavity of the reaction furnace 1 through a pipeline and is used for vacuumizing the inner cavity of the reaction furnace 1.
The gas cylinder 12 is connected with the inner cavity of the reaction furnace 1 through a pipeline and is used for filling required protective gas into the chamber of the reaction furnace.
As shown in fig. 2, the induction coil 13 is formed by winding a copper tube with a hollow channel, i.e. the copper tube for winding the coil is a water flow pipe. The induction coil 13 can generate a vortex electromagnetic field to heat the platinum-rhodium alloy, and meanwhile, the hollow channel of the copper tube is directly communicated with the water cooler 10 through a pipeline, so that the induction coil can be prevented from being overheated.
A preparation method of a high-performance platinum and platinum-rhodium thermocouple wire comprises the following steps:
step one, plugging the bottom of a crucible 14 by using a plug rod 8, and then placing a platinum-rhodium alloy material in the crucible 14, wherein the weight of the platinum-rhodium alloy is controlled to be 1-4 Kg;
step two, closing a furnace cover of the reaction furnace 1, starting the water cooling machine 10, increasing the power of the induction coil 13 to melt the alloy material in the crucible 14, and simultaneously electrifying the heating wire 17 to heat the crystallizer 3 to the alloy melting point temperature;
step three, reducing the power of the induction coil 13 to ensure that the alloy melt is in a heat preservation state and the components are uniform, and simultaneously starting the vacuum pump 11 to vacuumize the inner cavity of the reaction furnace 1 to 1 multiplied by 10-6Pa, then filling protective gas (argon, helium or nitrogen) to make the internal pressure the same as the external pressure;
step four, inserting the dummy bar 4 into the crystallizer 3, starting the cooling device 7 to spray cooling water towards the dummy bar 4, then pulling the pull rod 9 upwards, pulling the plug rod 8 out of the crucible 14, and enabling the alloy melt to flow into the crystallizer 3;
fifthly, the temperature of the crystallizer 3 is adjusted according to the display of the thermocouple 5 in the dummy bar 4, and the position of a solid-liquid interface is adjusted to be controlled at a position 10-50 mm away from a lower outlet of the crystallizer, so that the surface of the pulled ingot is bright, flat and flawless;
sixthly, starting the drawing device 6, drawing the solidified alloy part out of the crucible 14 at a preset speed of 1-20 mm/s, and rapidly cooling the solidified alloy part by cooling water;
step seven, immediately closing the current of the induction coil 13 and the heating wire 17 after the ingot is completely pulled out of the crystallizer 3, and keeping the water cooling machine 10 in an open state;
and step eight, cutting the cast ingot from the dummy bar 4 after the cast ingot is fully cooled, and closing the water cooler 10 after the crucible 14 is fully cooled.
Examples
1) Blocking the bottom of a zirconia crucible by a zirconia plug rod, and then placing 3kg of prepared pure platinum in the zirconia crucible;
2) closing the furnace cover of the reaction furnace, starting a water cooling machine, increasing the power of an induction coil to 21KW to melt pure platinum in the crucible, and simultaneously electrifying a tungsten heating wire to heat the crystallizer to 1769 ℃;
3) reducing the power of the induction coil to 16KW to keep the pure platinum melt at a heat preservation state, and simultaneously starting a vacuum pump to vacuumize the inner cavity of the reaction furnace to 1 × 10-6Pa, then filling protective gas argon to 1.01 multiplied by 105Pa；
4) Inserting a pure platinum dummy bar into a crystallizer, installing a cooling device at a position 20mm away from a lower outlet of the crystallizer, starting the cooling device to spray cooling water towards the pure platinum dummy bar, then pulling a pull rod upwards, pulling a zirconia plug rod out of a crucible, and enabling alloy melt to flow into the crystallizer;
5) according to the temperature displayed by a tungsten-rhenium thermocouple in a pure platinum dummy bar, the temperature of the crystallizer is adjusted to 1800 ℃, and a solid-liquid interface is controlled to be 20mm away from a lower outlet of the crystallizer;
6) opening a drawing device, and drawing the pure platinum solidification part out of the crucible at a preset speed of 2 mm/s;
7) after pure platinum is completely pulled out of the crystallizer, the current of the induction coil and the heating wire is immediately closed, and the opening state of the water cooling machine is kept;
8) and cutting the pure platinum cast ingot from the dummy bar after the pure platinum cast ingot is fully cooled, and closing the water cooling machine after the crucible is fully cooled.
All the above components are prior art, and those skilled in the art can use any model and existing design that can implement their corresponding functions.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (10)
1. A high-performance platinum and platinum rhodium thermocouple wire preparation device is characterized by comprising a reaction furnace (1), a smelting device (2), a crystallizer (3), a dummy bar (4), a thermocouple (5), a drawing device (6), a cooling device (7) and a plug rod (8), wherein an inner cavity of the reaction furnace (1) is a sealed cavity with a furnace cover, the smelting device (2) is arranged in the reaction furnace (1), the smelting device (2) comprises a crucible (14), the crystallizer (3) is arranged under the crucible (14) and communicated with the bottom of the crucible (14), the upper end of the plug rod (8) is connected with a pull bar (9), the lower end of the plug rod is positioned at the inner bottom of the crucible (14), the pull bar (9) is movably lifted and penetrates through the furnace cover at the top of the reaction furnace (1), the upper end of the dummy bar (4) extends into the inner bottom of the crystallizer (3), the drawing device (6) is connected with the lower end of the dummy bar (4), the cooling device (7) is arranged at the side surface of the dummy bar (4) at the outer side of an outlet below the crystallizer (3), the temperature measuring ends of the thermocouple (5) are respectively positioned at the crystallizer (3) and in the upper end of the dummy bar (4).
2. The preparation device of the high-performance platinum and platinum-rhodium thermocouple wire according to claim 1, wherein the smelting device (2) further comprises an induction coil (13), glass fiber cloth (15) and refractory mortar (16), the glass fiber cloth (15) is wrapped outside the crucible (14), the refractory mortar (16) is filled between the crucible (14) and the glass fiber cloth (15), and the glass fiber cloth (15) surrounds the inner wall of the induction coil (13).
3. The device for preparing the high-performance platinum and platinum-rhodium thermocouple wire according to claim 2, wherein the crystallizer (3) comprises heating wires (17) and a zirconia circular tube (18), the heating wires (17) are uniformly wound on the outer side of the zirconia circular tube (18), the outer side of the zirconia circular tube (18) is also wrapped by glass fiber cloth (15), and fire clay (16) is filled between the zirconia circular tube (18) and the glass fiber cloth (15).
4. The manufacturing device of high performance platinum and platinum rhodium thermocouple wires according to claim 3, characterized in that four cooling devices (7) are water-cooled spray cooling devices, are arranged at the height of 10-50 mm from the lower outlet of the crystallizer (3), and are respectively arranged at the front, back, left and right positions corresponding to the dummy bar (4).
5. The manufacturing device of high performance platinum and platinum rhodium thermocouple wires according to claim 4, characterized in that the temperature measuring end of the thermocouple (5) is located at the heating wire (17) of the crystallizer (3).
6. The preparation device of the high-performance platinum and platinum-rhodium thermocouple wire according to claim 5, which is characterized by further comprising a water cooling machine (10), a vacuum pump (11) and a gas cylinder (12), wherein the water cooling machine (10) is connected with the induction coil (13) through a pipeline, the vacuum pump (11) is connected with an inner cavity of the reaction furnace (1) through a pipeline, and the gas cylinder (12) is connected with the inner cavity of the reaction furnace (1) through a pipeline.
7. The device for preparing the high-performance platinum and platinum-rhodium thermocouple wire according to claim 6, wherein the induction coil (13) is formed by winding a copper tube with a hollow channel, and the hollow channel of the copper tube is communicated with the water cooler (10) through a pipeline.
8. The device for preparing the high-performance platinum and platinum-rhodium thermocouple wire according to claim 7, characterized in that the crucible (14) is a zirconia crucible, the diameter of the opening of the crucible (14) is phi 80mm, the diameter of the bottom of the crucible is phi 8mm, the depth of the crucible is 140mm, the crucible is funnel-shaped, the inclined plane and the ground surface are 63 degrees, the refractory mortar (16) is formed by bonding and mixing alumina powder and water, the material of the plug rod (8) is zirconia, the material of the heating wire (17) is phi 2.0mm tungsten wire, the material of the thermocouple (5) is tungsten-rhenium thermocouple, the material of the dummy bar (4) is 8mm round bar, and the material is the same as the phi thermocouple wire melted in the crucible (14).
9. The method for preparing the high-performance platinum and platinum-rhodium thermocouple wire according to claim 1, which is characterized by comprising the following steps:
step one, plugging the bottom of a crucible (14) by a plug rod (8), and then placing a platinum-rhodium alloy material into the crucible 14;
step two, closing a furnace cover of the reaction furnace (1), starting a water cooling machine (10), increasing the power of an induction coil (13) to melt the alloy material in the crucible (14), and simultaneously electrifying a heating wire (17) to heat the crystallizer (3) to the platinum-rhodium alloy melting point temperature;
step three, reducing the power of the induction coil (13), keeping the alloy melt in a heat preservation state, ensuring the components to be uniform, simultaneously starting a vacuum pump (11), and vacuumizing the inner cavity of the reaction furnace (1) to 1 multiplied by 10-6Pa, then filling protective gas to ensure that the internal pressure is the same as the external pressure;
step four, inserting the dummy bar (4) into the crystallizer (3), starting the cooling device (7) to spray cooling water towards the dummy bar (4), then pulling the pull rod (9) upwards, pulling the plug rod (8) out of the crucible (14), and enabling the alloy melt to flow into the crystallizer (3);
fifthly, the temperature of the crystallizer (3) is adjusted according to the display of the thermocouple (5) in the dummy bar (4), the position of a solid-liquid interface is adjusted, and the surface of the pulled ingot is bright, flat and free of defects;
sixthly, opening the drawing device (6) to draw the solidified alloy part out of the crucible (14), and rapidly cooling the solidified alloy part by cooling water;
step seven, immediately closing the current of the induction coil (13) and the current of the heating wire (17) after the ingot is completely pulled out of the crystallizer (3), and keeping the water cooling machine (10) in an opening state;
and step eight, cutting the cast ingot from the dummy bar (4) after the cast ingot is fully cooled, and closing the water cooler (10) after the crucible (14) is fully cooled.
10. The method for preparing a high-performance platinum and platinum-rhodium thermocouple wire according to claim 1, wherein the weight of the platinum-rhodium alloy material in the first step is controlled to be 1-4 kg, the protective gas in the third step is argon, helium or nitrogen, the solid-liquid interface position in the fifth step is adjusted to be 10-50 mm away from the lower outlet of the crystallizer, and the drawing device (6) in the sixth step draws the solidified alloy part out of the crucible (14) at a predetermined speed of 1-20 mm/s.
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