Method of making multi-layer tape nanostructure composite based on superconducting niobium-titanium alloy

FIELD: physics; conductors.

SUBSTANCE: invention relates to making composites with improved current-carrying capacity and can be used, particularly, for making superconducting magnet windings. According to the invention, the method of making multi-layer tape nanostructure composites based on a niobium-titanium alloy for composite superconductors involves multi-cycle rolling, each cycle of which involves assembling a packet from alternating plates of niobium and a niobium-titanium alloy, attaching the plates to each other into a packet through diffusion welding at temperature 800-900°C and pressure 20-40 MPa for 0.5-3 hours, hot vacuum rolling and cold rolling. In the first cycle, the initial plates are components of the composite, and in the second and following cycles - plates, obtained from the previous cycle. To stabilise the superconductor before the last rolling cycle, the welded packet is put into a copper casing. Thickness of the copper casing is 3-25% of the thickness of the packet.

EFFECT: increased critical current density.

2 cl, 2 tbl, 6 ex

 

The invention relates to the field of creation of new functional materials, namely layered nanostructured composite superconducting materials based on alloys of niobium with high current-carrying capacity, and can be used to create the windings of superconducting magnets.

Of great interest are materials containing alloys of Nb-Ti and Nb-Zr. Multilayer planar nanostructured composites on the basis of these alloys are promising for the creation of superconducting materials with high current-carrying capacity. The tape conductor flat parallel superconducting layers, the thickness is 10-100 nm and, therefore, comparable with the coherence length of the superconductor, allow you to use the effect of a long, flat interlayer boundaries parallel to the external magnetic field, pinning (fixing) of Abrikosov vortices and, therefore, the value of the critical current density.

A method of obtaining a superconducting wires based on niobium-titanium alloys, including accommodation in a glass made of copper or an alloy based on copper billets of niobium-titanium alloy, sealing, hot extrusion and cold deformation with receiving a rod, the cutting rod measuring part, the subsequent Assembly in a glass made of copper or an alloy based on copper measuring rods on what I get in the last composite blank of the required number of niobium-titanium fibers, conducting cold deformation, annealing and final deformation, with rods placed in the last composite workpiece, the pre-deformed in the cold with intermediate anneals at temperatures 385-420oC for 10-100 hours, after which the Assembly is deformed at room temperature until the total deformation, sufficient to remove all the existing gaps and no less than 10%, then spend an additional annealing at temperature and time regimes corresponding to the regime of intermediate annealing, and subsequent cold deformation annealing, to obtain a wire of the desired cross-section [RF patent №2159474, MKI H01B 13/00, published. 2000.11.20].

However, this method does not allow to obtain a multilayer composite superconducting material in the form of tapes.

A method of obtaining a multilayer composite [patent US 5,230,748, H01L 39/24, July 19, 1991], in which the superconducting layers of alloys of the system Nb-Ti-Zr-V-Hf-Ta at the final stage of manufacture of a superconductor is produced by diffusion annealing of the composite of alternating layers of these metals or their alloys, and the thickness of the normal and superconducting layers, formed during the annealing must be less than 1000 nm.

However, annealing, which requires a sufficiently high temperature, complicates the process of obtaining superconducting Mat is Rial and in addition, calls into question the compatibility of forming composite metal components.

Famous adopted for the prototype, a method of manufacturing a multilayer tape nanostructured composite based on superconducting alloy of niobium-titanium containing alternating layers of niobium and niobium alloy-titanium with an average thickness of each layer of 2.5 nm [Karpov M.I., Grandchildren, V.I., Volkov KG, Bear, NV, I.I. Khodos, Abrosimova G. "the features of the vacuum rolling as a method of producing a multilayer composites with nanometric thicknesses of the layers. // “Materials”, 2004, №1, p.48-53]. The method includes multicyclic rolling, each cycle of which consists of an Assembly of the package of plates of niobium and niobium alloy, titanium, bond package using rivets, vacuum hot rolling and cold rolling. In the first cycle of the original plates were components of the composite, in the second and subsequent cycles plates obtained in the previous cycle. Vacuum rolling in each cycle was performed for 2 passes heated samples up to 900°C and the total compression of 50%. After rolling all the samples were annealed at 400°C for 3 hours for separation of dispersed particles of α-phase in the alloy layers Nb-50 wt.% Ti.

However, the critical current density of such a superconducting composite does not meet the modern requirements of the technician is.

The present invention solves the problem of creating a method of manufacturing a nanostructured composite material with a high critical current density, capable of carrying a large total shock.

This object is achieved by a method of manufacturing a multilayer tape nanostructured composites based alloy niobium-titanium method multicycle rolling, each cycle of which included assembling a package of alternating plates of niobium and niobium alloy, titanium, fastening plates among themselves, vacuum hot rolling and cold rolling. In the first cycle of the original plates were components of the composite, and the second and subsequent cycles plates obtained in the previous cycle. The novelty of the proposed method lies in the fact that bond the plates together in the package is carried out using diffusion welding at a temperature of 800-900aboutC and a pressure of 20-40 MPa for 0.5-3 hours

To stabilize the superconductor before the last cycle of rolling welded package is placed in a copper shell. The thickness of the copper shell is 3-25% of the thickness of the package.

The technical result of the invention is to increase the critical current density multilayer tape nanostructured composites by improving the uniformity of thickness of laminate layers, which is the result of reducing their ox is obraznosti.

In the study of the microstructure of the cross-sections of samples of composites, cut parallel to the rolling direction, it was found that the critical current density was higher, the less were undulating layers of niobium and layers of alloy niobium-titanium. By analogy with oscillatory processes to characterize wolnoobraznosti layered structure were taken as the period length of one wavelength L and amplitude A. it Was also noted that in layers with strongly pronounced wave-like (small L and large And there was a local decrease (down to zero) the thickness of the layers as niobium, and an alloy of niobium-titanium.

Noticeable wave-like patterns manifested in that case, when the rolled package, pre-bonded by means of diffusion welding is carried out in the inventive us intervals.

At this place it before the last cycle rolling in the copper shell, declare our thickness, resulted in stabilization of the multilayer tape nanostructured composites with high critical current density.

Table 1 provides data on the change in critical current density of the composites with different composition of niobium-titanium alloy produced by the present method and the method prototype.

Table 2 provides data on the change in critical current density developed the s composites depending on the modes of fastening plates interconnected by means of diffusion welding.

The following examples illustrate, but not limit the invention.

Example 1.

Samples of multilayer tape nanostructured composite in the form of a tape with a width of 30-40 mm and thickness of 0.3 mm was obtained as in the prototype method multicycle rolling. Each cycle consisted of four successive operations: build the package from source plates, fastening the package by using rivets, vacuum hot rolling, cold rolling. In the first cycle of the original plates were components of the composite, in the second and subsequent cycles plates obtained in the previous cycle.

The first Assembly of the composite Nb/(Nb-50 wt.% Ti) consisted of 20 layers of niobium and 19 layers of alloy. The thickness of the base plates of niobium and an alloy was equal to 0.3 mm Cold rolling in each cycle was finished also on the thickness of 0.3 mm In the third cycle were rolling to achieve a final thickness of 0.15 mm. Vacuum rolling in each cycle was performed for 2 passes heated samples up to 900°C and the total compression of 50%. The result is a composite consisting of 64000 layer with an average layer thickness of 2.5 nm.

After rolling all the samples were annealed at 400°C for 3 hours for separation of dispersed particles of α-phase in the alloy layers Nb-50 wt.% Ti.

The critical current was measured at the liquid helium temperature in an external magnetic field up to 7 T at two Orien is the situation: parallel to the plane of the obtained composite (nanolaminate) and perpendicular to the transport current (in this case the Lorentz force, acting on the Abrikosov vortices, directed perpendicular to the plane of nanolaminate, and pinning on the interlayer surface takes place) and perpendicular to the plane of nanolaminate and transport current (in this case, the pinning on the interlayer surface is absent). The critical current density was determined by the ratio of total transport current to the entire cross-sectional area of the composite.

The structure of the samples was studied by scanning electron and transmission electron microscopy. Plane sections and foils for these studies was parallel to the rolling direction of the composite.

The microstructure of the obtained composite was characterized by such values of parameters wolnoobraznosti: L≈170 µm And≈10 ám.

The critical current density of the obtained composite is 30100 A/cm2in a magnetic field of 6 Tesla.

Example 2.

Same as in example 1, except that the fastening plates between them is carried out by means of diffusion welding. Diffusion welding was performed using a setup with induction heating at 850aboutC and pressure of 25 MPa for 1 hour

The microstructure of the obtained composite was characterized by such values of parameters wolnoobraznosti: amplitude And≈0.5 μm, the period L of more than 300 microns.

The critical current density of the obtained composite is 38000 A/cm2in a magnetic field of 6 Tesla.

Example 3.

Same as in example 1, except that as niobium-titanium alloy took the alloy composition of the Nb-30 wt.% Ti.

The microstructure of the obtained composite was characterized by such values of parameters wolnoobraznosti: L≈170 µm And≈10 ám.

The critical current density of the obtained composite is 40000 A/cm2in a magnetic field of 6 Tesla.

Example 4.

Same as in example 3, only the fastening plates between them is carried out by means of diffusion welding. Diffusion welding was performed using a setup with induction heating at 850aboutC and pressure of 25 MPa for 1 hour

The microstructure of the obtained composite was characterized by such values of parameters wolnoobraznosti: amplitude And≈0.5 μm, the period L over 550 microns.

The critical current density of the obtained composite is 57200 A/cm2in a magnetic field of 6 Tesla.

Data on the change in critical current density of the composites with different composition of niobium-titanium alloy produced by the present method and the method prototype is given in table 1.

As seen from the above examples, the fastening plates between them, carried out by means of diffusion welding by the proposed method reduces the wave-like layers and thereby increases the critical current density.

Example 5.

The same that when the ore 4, only the fastening plates between them is carried out using diffusion welding is carried out under different conditions. Data on the change in critical current density depending on the modes of fastening plates interconnected by means of diffusion welding are shown in table 2.

As can be seen from the table, the optimal modes of diffusion welding are: temperature of 800-900aboutWith the pressure of 20-40 MPa, time of 0.5-3 hours

Example 6.

Samples of multilayer tape nanostructured composite in the form of a tape width of 30-40 mm and a thickness of 0.15 mm was obtained by the method of high-rolling. Each cycle consisted of four successive operations: build the package from source plates, fastening the package by means of diffusion welding, vacuum hot rolling, cold rolling. In the first cycle of the original plates were components of the composite, in the second and subsequent cycles plates obtained in the previous cycle.

The first Assembly of the composite Nb/(Nb-30 wt.% Ti) consisted of 16 layers of niobium and 15 layers of alloy. The thickness of the base plates of niobium and an alloy was equal to 0.3 mm Cold rolling in each cycle was finished also on the thickness of 0.3 mm Before the third cycle rolling welded package was placed in a copper shell, whose thickness is equal to 10% of the thickness of the package and rolling were to achieve a final thickness of 0.3 mm Vacuum rolling in CA is home cycle was performed for 2 passes heated samples up to 900°C and the total compression of 50%. The result is a composite consisting of 28830 layers of niobium and niobium alloy, titanium and two outer layers of copper, in which the thickness of each layer of the alloy was equal to 5.9 nm.

Study of the effect of the thickness of the copper shell to receive the composite showed that the reduction in the thickness of the copper shell is less than 3% of the thickness of the package is impractical, so as not to impair its stabilizing action. Increasing the thickness of the copper shell more than 25% of the thickness of the package leads to an unjustified increase neteconomy cross-sectional area, i.e. to decrease the critical current density.

As seen from the above examples, the manufacture of multilayer tape nanostructured composite based on superconducting alloy of niobium-titanium proposed method leads to the increase of critical current density by lowering settings wolnoobraznosti layers.

Table 1
№ p/pThe composition of the niobium-titanium alloyPrototype method: bond package rivetThe inventive method: the bond package by diffusion welding
Options wolnoobraznosti layers Indicators of critical current density at 6 T, A/cm2Options wolnoobraznosti layersIndicators of critical current density at 6 T, A/cm2
125And≈10 µm
L=170 microns
39700And≈0.5 µm
L>500 μm
56000
230And≈10 µm
L=170 microns
40000And≈0.5 µm
L>500 μm
57200
340And≈10 µm
L=170 microns
40500And≈0.5 µm
L>500 μm
57000
450And≈10 µm
L=170 microns
30120And≈0.5 µm
L>300 μm
38000
555And≈10 µm
L=170 microns
25400And≈0.5 µm
L>300 μm
36000

Table 2
№ p/pModes of fastening plates interconnected by means of diffusion weldingIndicators of critical current density at 6 T, A/cm2
TemperatureaboutPressure, MPaTime, h
1750150,3There is no connection
2800200,557600
3850301,557000
490040356500
5950453,5Mutual diffusion between layers

1. A method of manufacturing megol logo tape nanostructured composite based on superconducting alloy of niobium-titanium, including high-rolling, each cycle of which consists of an Assembly of the package from the plane parallel to the plane of the composite of alternating plates of niobium and niobium alloy, titanium, bond wafers together with subsequent vacuum hot and cold prokatami, and in the first cycle of the source plates are components of the composite, and the second and subsequent cycles plates obtained in the previous cycle, characterized in that the fastening plates between them is carried out using diffusion welding at a temperature of 800-900°C and a pressure of 20-40 MPa for 0.5-3 hours

2. The method according to claim 1, characterized in that before the last cycle of rolling welded package is placed in a copper shell with a wall thickness 3-25% of the thickness of the package.



 

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