CN114446536A - Improved Nb preparation method3Method for preparing Al superconductive long wire - Google Patents
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Abstract
The invention discloses an improved Nb preparation method3The method for preparing the Al superconducting long wire rod comprises the following steps: firstly, preparing an Nb-Al precursor wire by a winding method; secondly, performing high-temperature heat treatment on the Nb-Al precursor wire by using a rapid-heating rapid-cooling high-temperature heat treatment system; the process adopts a roll-to-roll mode for heat treatment, and the copper wheel of the pay-off end and the synchronous wheel of the take-up end are provided with driving forces with the same linear velocity, so that the tension borne by the wire rod is zero; thirdly, annealing at low temperature to obtain Nb with A15 phase3An Al superconducting long wire. The invention provides an improved method for preparing Nb3The method for preparing the Al superconducting long wire rod solves the problems that the wire rod performance is uneven and even broken due to temperature fluctuation caused by tension of the wire rod in the existing preparation method, the method obviously improves the temperature uniformity of the wire rod in the rapid heating and rapid cooling process, the performance of the wire rod is obviously improved, and the continuous heat treatment is favorable for preparing large-batch high-performance wire rods.
Description
Technical Field
The invention belongs to the technical field of performance improvement of superconducting wires, and particularly relates to an improved Nb preparation method3A method for producing an Al superconducting long wire.
Background
Nb from the fifth and sixty years of the 20 th century3Since the discovery of Al superconducting materials, with the gradual and deep research of scientists, it was discovered that the materials are comparable to those already in commercial use in terms of superconducting transition temperature, upper critical field and stress strainNb3Sn superconducting material has a significant advantage over Sn superconducting material, which also makes Nb3The Al superconducting material can bear larger superconducting current. Scientists have therefore developed a wide variety of manufacturing processes in which the use of a winding process to produce a Nb-Al precursor wire and subsequent heat treatment in conjunction with rapid heat quenching is believed to be the current practice in producing high performance Nb3An optimum method for an Al superconducting wire.
However, in the heat treatment process by the rapid heating and quenching method, the heating current and the tension of the wire have great influence on the performance of the wire. The principle of the used quick-heating quenching equipment is based on direct-current ohmic heating, namely, the wire is heated to about 2000 ℃ in a short time of about 0.3 s; from ohm's law, it is known that the heating power during the heat treatment is proportional to the heating time and the square of the resistance value of the heating interval, and the temperature T at the position l in the heating interval can be expressed as:
where rho is the resistivity of the Nb-Al precursor wire, rhomMass density, c specific heat, R wire radius, I heating current, v wire speed. In the process of rapid-heating and rapid-cooling heat treatment, the wire rod is influenced by tension, so that the wire rod is deformed, and the wire diameter is reduced. From the above formula, T/T2I/I, but T/T-4R/R, means that the relative fluctuation of the heat treatment temperature is twice the relative fluctuation of the heating current, and 4 times the relative fluctuation of the wire radius. Therefore, the small change of the wire diameter can cause the change of the temperature of the wire heating section, especially the high temperature of 2000 ℃ in the heat treatment process, the strength of the wire is reduced, the change of the wire diameter is more obvious, the temperature fluctuation in the heat treatment process is seriously aggravated, the performance of the wire is reduced, even the wire is broken, and the conditions that the mass production cannot be realized and the practical stage is entered are caused.
Therefore, the effect of eliminating the tension in the rapid heating and quenching heat treatment process is improved compared with the effect of stabilizing the heating current on increasing Nb3The performance of the Al superconducting material is more important。
Disclosure of Invention
The object of the present invention is to provide an improved process for the production of Nb3Method for preparing Al superconducting long wire and Nb prepared by the method3The Al superconducting long wire has better superconducting performance, and the problem that the performance of the wire is reduced and even the wire is broken due to the influence of tension is solved to a great extent.
In order to achieve the purpose, the invention adopts the technical scheme that:
improved Nb preparation method3The method for preparing the Al superconducting long wire rod comprises the following steps:
(1) preparing a precursor wire: winding Nb foil and Al foil by a central Nb rod by adopting a traditional winding method to obtain an Nb-Al precursor wire;
(2) quick-heating, rapid-cooling and high-temperature heat treatment:
firstly, winding a Nb-Al precursor wire on a pay-off wheel, and connecting the wire through a first finishing wheel, a first wire pressing wheel, a copper wheel, a second wire pressing wheel, a gallium pool, a second finishing wheel, a third wire pressing wheel and a take-up wheel;
secondly, vacuumizing the rapid-heating rapid-cooling high-temperature heat treatment system;
setting the copper wheel of the wire releasing end and the synchronous wheel of the wire receiving end to have driving forces with the same linear speed;
setting input current and input voltage, and adjusting the input current and the input voltage to be in a constant current mode or a constant voltage mode;
linkage starting and starting a heating power supply, carrying out rapid heating and rapid cooling heat treatment on the wire, recording output voltage and output current, and observing the light and shade condition of the fire during the heat treatment of the wire;
closing a heating power supply after the wire is treated, stopping the wire in a linkage manner, balancing the air pressure inside and outside the heat treatment furnace chamber, and taking down the heat-treated wire to obtain the wire with the Nb-Al supersaturated solid solution Nb (Al) ss;
(3) low-temperature annealing: the wire rod of Nb (Al) ss after the rapid-heating rapid-cooling high-temperature heat treatment is annealed at low temperature in a tube furnace to obtain Nb with A15 phase3An Al superconducting long wire.
The invention is also characterized in that:
in the step (2), the sizes of the grooves of the arranging wheel and the wire pressing wheel are matched with the diameter of the wire.
In the step (2), the vacuum degree of the rapid-heating rapid-cooling high-temperature heat treatment system is stabilized at 1 multiplied by 10-3-9×10-3Pa。
In the step (2), the linear speed of the copper wheel at the wire releasing end and the synchronous wheel at the wire collecting end is 100-300 mm/s.
In the step (2), the input voltage is 9.5-10.8V, and the input current is 80-300A.
In the step (3), the temperature of the low-temperature annealing is 750-850 ℃, and the time is 1-25 h.
Compared with the prior art, the invention has the beneficial effects that:
1. a zero-tension fast-heating rapid cooling heat treatment system is developed, a copper wheel at a pay-off end and a synchronous wheel at a take-up end are provided with independent driving motors, the copper wheel at the pay-off end and the synchronous wheel at the take-up end can be provided with driving forces with the same linear velocity, the tension borne by a wire rod can be well controlled to be zero, and the problems that the wire rod is uneven in performance and even broken due to temperature fluctuation caused by the fact that the wire rod is subjected to tension in the existing preparation method are solved.
2. The wire diameter of the wire rod is ensured not to change and keep constant in the rapid-heating rapid-cooling heat treatment process, and the fluctuation of the heating temperature is reduced, so that the Nb (Al) ss supersaturated solid solution formed after the heat treatment is more uniform.
3. Due to Nb in the heat treatment process3The uniform performance of the components, the structure and the performance of the Al wire rod can be effectively ensured, and the coil-to-coil rapid-heating rapid-cooling heat treatment equipment can be used for continuously treating the superconducting wire rod with the length of kilometers.
Therefore, Nb prepared by the process of the invention3The Al superconducting long wire has higher current-carrying density, and the high-performance superconducting wire can be prepared in batch continuously under the condition of zero tension, so that the material is favorable for large-scale practicability and has a larger application prospect.
Drawings
FIG. 1 is a schematic view of the production apparatus of the present invention.
FIG. 2 is a pictorial representation of the product prepared in example 1.
Detailed Description
The following examples are intended to illustrate the invention only and are not intended to limit the invention.
Example 1
Improved Nb preparation method3The method for preparing the Al superconducting long wire rod comprises the following steps:
(1) preparing a precursor wire: winding Nb foil and Al foil by a central Nb rod by adopting a traditional winding method to obtain an Nb-Al precursor wire;
(2) quick-heating, rapid-cooling and high-temperature heat treatment:
firstly, winding a Nb-Al precursor wire on a pay-off wheel, wherein a connecting wire passes through a first finishing wheel, a first wire pressing wheel, a copper wheel, a second wire pressing wheel, a gallium pool, a second finishing wheel, a third wire pressing wheel and a take-up wheel, and the size and the wire diameter of a groove of each wheel are 1 mm;
② vacuum pumping the rapid-heating rapid-cooling high-temperature heat treatment system to 9 x 10-3Pa；
Setting the copper wheel of the wire releasing end and the synchronous wheel of the wire receiving end to have the same linear speed which is 100 mm/s;
setting the input voltage to be 10V and the input current to be 100A;
linkage starting and starting a heating power supply, carrying out rapid heating and rapid cooling heat treatment on the wire, recording output voltage and output current, and observing the light and shade condition of the fire during the heat treatment of the wire;
closing a heating power supply after the wire is treated, stopping the wire in a linkage manner, balancing the air pressure inside and outside the heat treatment furnace chamber, and taking down the heat-treated wire to obtain the wire with the Nb-Al supersaturated solid solution Nb (Al) ss;
(3) low-temperature annealing: the wire rod of Nb (Al) ss is put into a tube furnace for annealing at 760 ℃ for 5h to obtain Nb 15 phase3An Al superconducting long wire.
The Nb-Al precursor wire does not have the disconnection phenomenon in the process of rapid heating and rapid cooling heat treatment, has bright fire light, and finally obtains the Nb3The Al superconducting wire has better plasticity. After the wire is tested, the superconducting transition temperature reaches 17.4K, no magnetic flux jumping phenomenon exists,the critical current measured at 4.2K, 12T reached 400A.
Example 2
Improved Nb preparation method3The method for preparing the Al superconducting long wire rod comprises the following steps:
(1) preparing a precursor wire: winding Nb foil and Al foil by a central Nb rod by adopting a traditional winding method to obtain an Nb-Al precursor wire;
(2) quick-heating, rapid-cooling and high-temperature heat treatment:
firstly, winding a Nb-Al precursor wire on a pay-off wheel, wherein a connecting wire passes through a first finishing wheel, a first wire pressing wheel, a copper wheel, a second wire pressing wheel, a gallium pool, a second finishing wheel, a third wire pressing wheel and a take-up wheel, and the size and the wire diameter of a groove of each wheel are 1 mm;
② vacuum pumping the rapid-heating rapid-cooling high-temperature heat treatment system to 7 x 10-3Pa；
Setting the copper wheel of the wire releasing end and the synchronizing wheel of the wire receiving end to have the same linear speed which is 150 mm/s;
setting the input voltage to be 10.2V and the input current to be 100A;
linkage starting and starting a heating power supply, carrying out rapid heating and rapid cooling heat treatment on the wire, recording output voltage and output current, and observing the light and shade condition of the fire during the heat treatment of the wire;
closing a heating power supply after the wire is treated, stopping the wire in a linkage manner, balancing the air pressure inside and outside the heat treatment furnace chamber, and taking down the heat-treated wire to obtain the wire with the Nb-Al supersaturated solid solution Nb (Al) ss;
(3) low-temperature annealing: placing the Nb (Al) ss wire rod in a tube furnace for annealing at 780 ℃ for 10h to obtain Nb 15 phase3An Al superconducting long wire.
The Nb-Al precursor wire does not have the disconnection phenomenon in the process of rapid heating and rapid cooling heat treatment, has bright fire light, and finally obtains the Nb3The Al superconducting wire has better plasticity. After the wire is tested, the superconducting transition temperature reaches 17.7K, the phenomenon of magnetic flux jumping is avoided, and the critical current measured under 4.2K and 12T reaches 360A.
Example 3
Improved Nb preparation method3The method for preparing the Al superconducting long wire rod comprises the following steps:
(1) preparing a precursor wire: winding Nb foil and Al foil by a central Nb rod by adopting a traditional winding method to obtain an Nb-Al precursor wire;
(2) quick-heating, rapid-cooling and high-temperature heat treatment:
firstly, winding a Nb-Al precursor wire on a pay-off wheel, wherein a connecting wire passes through a first finishing wheel, a first wire pressing wheel, a copper wheel, a second wire pressing wheel, a gallium pool, a second finishing wheel, a third wire pressing wheel and a take-up wheel, and the size and the wire diameter of a groove of each wheel are 1 mm;
② vacuum pumping the rapid-heating quenching high-temperature heat treatment system to 5 x 10-3Pa；
Setting the copper wheel of the wire releasing end and the synchronizing wheel of the wire receiving end to have the same linear speed which is 200 mm/s;
setting the input voltage to be 10.4V and the input current to be 100A;
linkage starting and starting a heating power supply, carrying out rapid heating and rapid cooling heat treatment on the wire, recording output voltage and output current, and observing the light and shade condition of the fire during the heat treatment of the wire;
closing a heating power supply after the wire is treated, stopping the wire in a linkage manner, balancing the air pressure inside and outside the heat treatment furnace chamber, and taking down the heat-treated wire to obtain the wire with the Nb-Al supersaturated solid solution Nb (Al) ss;
(3) low-temperature annealing: the wire rod of Nb (Al) ss is put into a tube furnace for annealing at 800 ℃ for 15h to obtain Nb 15 phase3An Al superconducting long wire.
The Nb-Al precursor wire does not have the disconnection phenomenon in the process of rapid heating and rapid cooling heat treatment, has bright fire light, and finally obtains the Nb3The Al superconducting wire has better plasticity. After the wire is tested, the superconducting transition temperature reaches 17.6K, the phenomenon of magnetic flux jumping is avoided, and the critical current measured under 4.2K and 12T reaches 450A.
Example 4
Improved Nb preparation method3The method for preparing the Al superconducting long wire rod comprises the following steps:
(1) preparing a precursor wire: winding Nb foil and Al foil by a central Nb rod by adopting a traditional winding method to obtain an Nb-Al precursor wire;
(2) quick-heating, rapid-cooling and high-temperature heat treatment:
firstly, winding a Nb-Al precursor wire on a pay-off wheel, wherein a connecting wire passes through a first finishing wheel, a first wire pressing wheel, a copper wheel, a second wire pressing wheel, a gallium pool, a second finishing wheel, a third wire pressing wheel and a take-up wheel, and the size and the wire diameter of a groove of each wheel are 1 mm;
② vacuum pumping the rapid-heating quenching high-temperature heat treatment system to 3 x 10-3Pa；
Setting the copper wheel of the wire releasing end and the synchronizing wheel of the wire receiving end to have the same linear speed of 250 mm/s;
setting the input voltage to be 10.6V and the input current to be 100A;
linkage starting and starting a heating power supply, carrying out rapid heating and rapid cooling heat treatment on the wire, recording output voltage and output current, and observing the light and shade condition of the fire during the heat treatment of the wire;
closing a heating power supply after the wire is treated, stopping the wire in a linkage manner, balancing the air pressure inside and outside the heat treatment furnace chamber, and taking down the heat-treated wire to obtain the wire with the Nb-Al supersaturated solid solution Nb (Al) ss;
(3) low-temperature annealing: the wire rod of Nb (Al) ss is put into a tube furnace for annealing at 820 ℃ for 20h to obtain Nb 15 phase3An Al superconducting long wire.
The Nb-Al precursor wire does not have the disconnection phenomenon in the process of rapid heating and rapid cooling heat treatment, has bright fire light, and finally obtains the Nb3The Al superconducting wire has better plasticity. After the wire is tested, the superconducting transition temperature reaches 17.5K, the phenomenon of magnetic flux jumping is avoided, and the critical current measured under 4.2K and 12T reaches 380A.
Example 5
Improved Nb preparation method3The method for preparing the Al superconducting long wire rod comprises the following steps:
(1) preparing a precursor wire: winding Nb foil and Al foil by a central Nb rod by adopting a traditional winding method to obtain an Nb-Al precursor wire;
(2) quick-heating, rapid-cooling and high-temperature heat treatment:
firstly, winding a Nb-Al precursor wire on a pay-off wheel, wherein a connecting wire passes through a first finishing wheel, a first wire pressing wheel, a copper wheel, a second wire pressing wheel, a gallium pool, a second finishing wheel, a third wire pressing wheel and a take-up wheel, and the size and the wire diameter of a groove of each wheel are 1 mm;
② vacuum pumping the rapid-heating rapid-cooling high-temperature heat treatment system to 1 × 10-3Pa；
Setting the copper wheel of the wire releasing end and the synchronous wheel of the wire receiving end to have the same linear speed which is 300 mm/s;
setting the input voltage to be 10.8V and the input current to be 100A;
linkage starting and starting a heating power supply, carrying out rapid heating and rapid cooling heat treatment on the wire, recording output voltage and output current, and observing the light and shade condition of the fire during the heat treatment of the wire;
closing a heating power supply after the wire is treated, stopping the wire in a linkage manner, balancing the air pressure inside and outside the heat treatment furnace chamber, and taking down the heat-treated wire to obtain the wire with the Nb-Al supersaturated solid solution Nb (Al) ss;
(3) low-temperature annealing: annealing the Nb (Al) ss wire rod in a tube furnace at 840 ℃ for 25h to obtain Nb 15 phase3An Al superconducting long wire.
The Nb-Al precursor wire does not have the disconnection phenomenon in the process of rapid heating and rapid cooling heat treatment, has bright fire light, and finally obtains the Nb3The Al superconducting wire has better plasticity. After the wire is tested, the superconducting transition temperature reaches 17.6K, the phenomenon of magnetic flux jumping is avoided, and the critical current measured under 4.2K and 12T reaches 320A.
Claims (7)
1. Improved Nb preparation method3The method for preparing the Al superconducting long wire is characterized by comprising the following steps:
(1) preparing a precursor wire: winding Nb foil and Al foil by a central Nb rod by adopting a traditional winding method to obtain an Nb-Al precursor wire;
(2) quick-heating, rapid-cooling and high-temperature heat treatment:
firstly, winding a Nb-Al precursor wire on a pay-off wheel, and connecting the wire through a first finishing wheel, a first wire pressing wheel, a copper wheel, a second wire pressing wheel, a gallium pool, a second finishing wheel, a third wire pressing wheel and a take-up wheel;
secondly, vacuumizing the rapid-heating rapid-cooling high-temperature heat treatment system;
setting the copper wheel of the wire releasing end and the synchronous wheel of the wire receiving end to have driving forces with the same linear speed;
setting input current and input voltage, and adjusting the input current and the input voltage to be in a constant current mode or a constant voltage mode;
linkage starting and starting a heating power supply, carrying out rapid heating and rapid cooling heat treatment on the wire, recording output voltage and output current, and observing the light and shade condition of the fire during the heat treatment of the wire;
closing a heating power supply after the wire is treated, stopping the wire in a linkage manner, balancing the air pressure inside and outside the heat treatment furnace chamber, and taking down the heat-treated wire to obtain the wire with the Nb-Al supersaturated solid solution Nb (Al) ss;
(3) low-temperature annealing: the wire rod of Nb (Al) ss is put into a tube furnace for low-temperature annealing to obtain Nb with A15 phase3An Al superconducting long wire.
2. An improved Nb production according to claim 13The method for preparing the Al superconducting long wire is characterized in that in the step (2), the sizes of grooves of the finishing wheel and the wire pressing wheel are matched with the diameter of the wire.
3. An improved Nb production according to claim 13The method for preparing Al superconducting long wire is characterized in that in the step (2), the vacuum degree of a rapid-heating rapid-cooling high-temperature heat treatment system is stabilized at 1 x 10-3-9×10-3 Pa。
4. An improved Nb production according to claim 13The method for the Al superconducting long wire is characterized in that in the step (2), the linear speed of a copper wheel at the wire releasing end and a synchronous wheel at the wire collecting end is 100-300 mm/s.
5. Root of herbaceous plantAn improved method of making Nb in accordance with claim 13The method for preparing the Al superconducting long wire is characterized in that in the step (2), the input voltage is 9.5-10.8V, and the input current is 80-300A.
6. An improved Nb production according to claim 13The method for the Al superconducting long wire is characterized in that in the step (3), the low-temperature annealing temperature is 750-850 ℃, and the time is 1-25 h.
7. Nb obtained by the production method according to any one of claims 1 to 63An Al superconducting long wire.
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Cited By (2)
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| CN116200690A (en) * | 2023-01-29 | 2023-06-02 | 西南交通大学 | Preparation of high-current-carrying Nb by multiple instantaneous high-temperature heat treatments 3 Method of Al superconducting wire |
| CN116884700A (en) * | 2023-07-10 | 2023-10-13 | 西南交通大学 | Niobium-aluminum superconductive wire doped with iodine simple substance, and preparation method and application thereof |
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| CN109609750A (en) * | 2019-01-17 | 2019-04-12 | 西南石油大学 | A kind of zero tension synchronous transmission heat treatment system preparing high performance superconductor wire rod |
| CN110610781A (en) * | 2019-08-28 | 2019-12-24 | 福建师范大学 | Heat treatment device and method for high-performance iron-based superconducting wire |
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| CN116884700B (en) * | 2023-07-10 | 2024-02-06 | 西南交通大学 | Niobium-aluminum superconductive wire doped with iodine simple substance, and preparation method and application thereof |
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