CN109903927A - A kind of preparation method of the iron-based superconducting line strips of compound jacket - Google Patents
A kind of preparation method of the iron-based superconducting line strips of compound jacket Download PDFInfo
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- CN109903927A CN109903927A CN201910094276.3A CN201910094276A CN109903927A CN 109903927 A CN109903927 A CN 109903927A CN 201910094276 A CN201910094276 A CN 201910094276A CN 109903927 A CN109903927 A CN 109903927A
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Abstract
The present invention relates to iron-based superconductor technical fields, and in particular to a kind of preparation method of the compound iron-based superconducting line strips of jacket.The preparation method of the iron-based superconducting line strips of compound jacket provided by the invention, including under an inert atmosphere, the step of iron-based superconducting precursor powder progress first is heat-treated.The present invention is by under an inert atmosphere, carrying out preposition heat treatment to the iron-based superconducting precursor powder of jacket metal tube in being packed into, can effectively eliminate bulge, promote finished product rate.
Description
Technical field
The present invention relates to iron-based superconductor technical fields, and in particular to a kind of preparation of the compound iron-based superconducting line strips of jacket
Method.
Background technique
Iron-based superconductor is the type found at the beginning of 2008, which causes world superconduction forward position again
Revolutionary progress.At present, highest superconduction critical temperature is 55K.According to the ratio of components of superconduction core compound and crystal knot
Structure, iron-based superconducting material are broadly divided into following four big systems: (1) " 1111 " system, member include LnOFeAs (Ln=La, Ce,
Pr, Nd, Sm, Gd, Tb, Dy, Ho, Y) and DvFeAsF (Dv=Ca, Sr) etc.；(2) " 122 " system, member include AFe2As2(A
=Ba, Sr, K, Ca, Eu) etc.；(3) " 111 " system, member include AFeAs (A=Li, Na) etc.；(4) " 11 " system, member's packet
Include FeSe (Te) etc..
Compared with traditional superconductor, iron-based superconductor is high with transition temperature, upper critical field is big, critical current is big, high
The features such as critical current decaying off field is slow；Compared with other high temperature superconducting materias, the crystal of iron-based superconductor is purer, Xiang Gengjia
It is single, anisotropy is small and at low cost, preparation is simple.Since iron-based superconductor has great potential application foreground, iron
The preparation of base superconductor is by international extensive concern.
Currently, the preparation method of general iron-based superconducting line strips is powder-in-tube technique (PIT method), but this method is applied to
A large amount of bulge can be brought when the certain iron-based superconducting line strips of compound jacket (such as copper silver is compound), substantially reduces superconduction critical electric current
With the sintering finished rate of wire strip, meanwhile, this method needs biggish pressure in the actual production process, such as using hot pressing it is standby
Copper silver band prepares round wires using the quasi- static pressure of heat.Regardless of being to require biggish pressure using hot pressing or the quasi- static pressure of heat, it is
This magnitude of 200MPa needs to use Hot Press or Hot Isostatic Press big so that the technique is essential
Type instrument and equipment considerably increases the production cost of product.
Summary of the invention
When producing iron-based superconducting line strips using powder-in-tube technique in the prior art it is an object of the invention to overcome, easy band
Carry out a large amount of bulges, finished product rate is low, and biggish pressure is needed in actual production process, causes production cost is excessively high to ask
Topic, to provide a kind of preparation method of iron-based superconducting line strips of compound jacket.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of the iron-based superconducting line strips of compound jacket, including, under an inert atmosphere, to iron-based superconduction forerunner
Powder carries out the step of the first heat treatment.
Preferably, the temperature of first heat treatment is 700-900 DEG C, and the time is 1-300 minutes, and pressure is normal pressure.
Preferably, the preparation method of the iron-based superconducting precursor powder, includes the following steps: under an inert atmosphere, to iron-based
Superconduction raw material carry out the first sintering.
Preferably, the time of first sintering is 1-200 hours, and the temperature of sintering is 500-900 DEG C, the pressure of sintering
For normal pressure.
Preferably, first heat treatment is carried out after jacket metal tube in being packed into iron-based superconducting precursor powder.
It preferably, further include being inserted in the interior jacket metal tube in outsourcing set metal tube, to form compound jacket metal
Pipe.The compound jacket metal tube is swaged, drawing, rolls processing to form the iron-based superconducting line strips of compound jacket.
Preferably, further include the steps that carrying out the second heat treatment to the compound iron-based superconducting line strips of jacket.Described
Two heat treatment temperatures are 500-950 DEG C, and the pressure of heat treatment is 0.1-300MPa, and heat treatment time is 1-12000 minutes.
Preferably, the metal of the interior jacket metal tube and outer jacket metal tube be selected from gold, silver, copper, iron, niobium, nickel, chromium,
The gold of at least one of tin, vanadium, violent, titanium, zirconium, molybdenum, tungsten, lead, aluminium, zinc or the interior jacket metal tube and outer jacket metal tube
Belong to is monel metal or low-carbon steel or stainless steel or high-carbon steel.When the metal of the interior jacket metal tube and outer jacket metal tube
For various metals composite material when, can be alloy (such as monel metal) or Alloy solid solution or metallic multilayer composite material.
Preferably, the iron-based superconducting precursor powder, composition include Ba1-xKxFe2As2、Sr1-xKxFe2As2、FeSe1- xTex、KFeAs、SmFeAsO1-xFx、LaFeAsO1-xFxAt least one of, wherein doping coefficient x value is 0-1.In the present invention
In, the group of the iron-based superconducting precursor powder is grouped as and is not especially limited, optionally, the iron-based superconducting precursor powder, group
122 set member (Sr in Cheng Kewei iron-based superconducting material1-xKxFe2As2、Ba1-xKxFe2As2), 11 set member (FeSe1-xTex),
111 set members (KFeAs), 1111 set member (SmFeAsO1-xFx/LaFeAsO1-xFx)。
Preferably, the inert atmosphere can be argon atmosphere or helium protective atmosphere.
Preferably, the shape of the iron-based superconducting line strips of compound jacket is strip, and thickness is about 0.2-0.4mm, institute
The cross-sectional shape for stating the iron-based superconducting line strips of compound jacket is rectangle, round or ellipse.Iron-based superconduction of the present invention
The final finished of wire strip can be used as superconductivity wire finished product and come into operation.
Beneficial effects of the present invention:
1) present invention provides a kind of preparation method of iron-based superconducting line strips of compound jacket, including under an inert atmosphere, will
Iron-based superconducting precursor powder carries out the step of the first heat treatment.The present invention by under an inert atmosphere, to iron-based superconducting precursor powder into
Row first is heat-treated, and interval gas and adsorbed gas extra between powder can be effectively removed, and is eliminated extra volatile
Impurity eliminates metal composite stress to effectively eliminate bulge, promotes finished product rate.
Simultaneously by being heat-treated to iron-based superconducting precursor powder, so that entire technique does not need additional air pressure, in normal pressure
Under iron-based superconducting line strips can be prepared, set without Hot Press or Hot Isostatic Press large-scale instrument
Standby, so as to increase production scale, and heating equipment used in the present invention is not necessarily to gas tightness, and plant maintenance facilitates fast
Victory greatly reduces production cost, improves finished product rate.
2) present invention provides a kind of preparation method of iron-based superconducting line strips of compound jacket, and further, the present invention is to iron
It is 800-900 DEG C that base superconducting precursor powder, which carries out the first heat treatment temperature, and the time is 1-300 minutes, and pressure is normal pressure, in the condition
Under, it can be further reduced the bulge of the iron-based superconducting line strips of compound jacket, increase the yield rate of product.
3) present invention provides a kind of preparation method of iron-based superconducting line strips of compound jacket, the present invention under an inert atmosphere,
First heat treatment is carried out after jacket metal tube in being packed into iron-based superconducting precursor powder, is eliminated to metal tube progress
The process of independent preposition heat treatment, while the connectivity to the crystal grain of superconducting core is strengthened, it finally prepares with superior performance
The iron-based superconductivity wire of compound jacket.
4) present invention carries out the second heat treatment to the iron-based superconducting line strips of the compound jacket, when not increasing gas pressure additionally
Qiang Shi, the compound iron-based superconducting line strips of jacket obtained still have preferably performance and yield rate, increase gas pressure intensity when additional
When, obtained properties of product are more excellent.
5) powder can be effectively removed by the first sintering, the first heat treatment, the second heat treatment in preparation method of the present invention
Between extra interval gas and adsorbed gas, eliminate extra volatile impurity, bulge can effectively be eliminated by doing so, and be eliminated
Metal composite stress promotes yield rate.The compound iron-based superconducting wire band of jacket of copper silver being prepared under normal pressure using this method
Material obtains supercurrent performance, critical current JcReach 10000-50000A/cm2。
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the preparation method flow chart of the compound iron-based superconducting line strips of jacket of the present invention；
Fig. 2 is the iron-based superconducting line strips heat treatment cycle curve figure of the compound jacket of embodiment 1；
Fig. 3 is the structural schematic diagram of the 3 iron-based superconducting line strips of compound jacket of embodiment；
Specific embodiment
There is provided following embodiments is to preferably further understand the present invention, it is not limited to the best embodiment party
Formula is not construed as limiting the contents of the present invention and protection scope, anyone under the inspiration of the present invention or by the present invention and its
The feature of his prior art is combined and any and identical or similar product of the present invention for obtaining, all falls within of the invention
Within protection scope.
Specific experiment step or condition person are not specified in embodiment, according to the literature in the art described routine experiment
The operation of step or condition can carry out.Reagents or instruments used without specified manufacturer, being can be by commercially available acquisition
Conventional reagent product.
Embodiment 1
Present embodiments provide a kind of compound LaFeAsO of single copper silver0.76F0.24The preparation method of superconducting line strips, including
Following steps:
1) under Ar gas shielded atmosphere, by iron-based superconduction raw material simple substance La, Fe, As, O, F according to above-mentioned stoichiometric ratio
Precise amounts to 20g, is then packed into load weighted simple substance raw material planetary ball mill ball milling 10 hours, is allowed to become powder.
The powder of milled is packed into Nb pipe, heat treatment sintering is carried out after being shut both ends with copper plug, the sintering time is 1 hour,
Sintering temperature is 900 DEG C, and sintering pressure is normal pressure, finally obtains LaFeAsO0.76F0.24, powder is broken into get iron-based
Superconducting precursor powder；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 700 DEG C, and heat treatment time is 300 minutes, heat
Processing pressure is normal pressure.After heat treatment by equipped with iron-based superconducting precursor powder Ag pipe be inserted in Cu pipe (Cu manage outside, Ag pipe
Inside), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
Under argon atmosphere, temperature is first increased to 500 DEG C, pressure 0.1MPa, and after heat-insulation pressure keeping 12000 minutes and is cooled to room temperature,
The iron-based superconducting line strips of compound jacket are taken out, the compound LaFeAsO of single copper silver is obtained0.76F0.24Superconducting line strips finished product.This reality
It applies a step 2) and 3) heat treatment cycle curve figure is as shown in Figure 2.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 10000A/cm2 (4.2K, 0T), superconducting transition temperature is not less than 53K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 95%.
Embodiment 2
Single copper silver composite S mFeAsO0.76F0.24The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, by iron-based superconduction raw material simple substance Sm, Fe, As, O, F according to above-mentioned stoichiometric ratio
Precise amounts to 20g, is then packed into load weighted simple substance raw material planetary ball mill ball milling 10 hours, is allowed to become powder.
The powder of milled is packed into Nb pipe, heat treatment sintering is carried out after being shut both ends with copper plug, the sintering time is 200 small
When, sintering temperature is 500 DEG C, and sintering pressure is normal pressure, finally obtains SmFeAsO0.76F0.24, powder is broken into get iron
Base superconducting precursor powder；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 900 DEG C, and heat treatment time is 1 minute, at heat
Reason pressure is normal pressure.After heat treatment by equipped with iron-based superconducting precursor powder Ag pipe be inserted in Cu pipe (Cu manage outside, Ag pipe exists
It is interior), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
Under argon atmosphere, temperature is first increased to 950 DEG C, pressure 0.1MPa, and after heat-insulation pressure keeping 1 minute and is cooled to room temperature, is taken out
The compound iron-based superconducting line strips of jacket obtain single copper silver composite S mFeAsO0.76F0.24Superconducting line strips finished product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 11000A/cm2(4.2K, 0T), superconducting transition temperature are not less than 50K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 93%.
Embodiment 3
The compound Ba of single copper silver0.6K0.4Fe2As2The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, iron-based superconduction raw material simple substance Ba, K, Fe, As is quasi- according to above-mentioned stoichiometric ratio
It really weighs and amounts to 20g, then load weighted simple substance raw material is packed into planetary ball mill ball milling 10 hours, is allowed to become powder.It will
The powder of milled is packed into Nb pipe, and heat treatment sintering is carried out after being shut both ends with copper plug, and the sintering time is 35 hours, burns
Junction temperature is 900 DEG C, and sintering pressure is normal pressure, finally obtains Ba0.6K0.4Fe2As2, powder is broken into get iron-based superconduction
Front axle shell；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 800 DEG C, and heat treatment time is 30 minutes, heat
Processing pressure is normal pressure.After heat treatment by equipped with iron-based superconducting precursor powder Ag pipe be inserted in Cu pipe (Cu manage outside, Ag pipe
Inside), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
In argon atmosphere under room temperature, temperature is first increased to cool down to 740 DEG C, pressure 0.1MPa, and after heat-insulation pressure keeping 20 hours
To room temperature, the iron-based superconducting line strips of compound jacket are taken out, obtain the compound Ba of single copper silver0.6K0.4Fe2As2Superconducting line strips at
Product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 20000A/cm2(4.2K, 0T), superconducting transition temperature are not less than 37K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 97%.
Embodiment 4
The compound Ba of single Monel silver0.6K0.4Fe2As2The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, iron-based superconduction raw material simple substance Ba, K, Fe, As is quasi- according to above-mentioned stoichiometric ratio
It really weighs and amounts to 20g, then load weighted simple substance raw material is packed into planetary ball mill ball milling 10 hours, is allowed to become powder.It will
The powder of milled is packed into Nb pipe, and heat treatment sintering is carried out after being shut both ends with copper plug, and the sintering time is 50 hours, burns
Junction temperature is 800 DEG C, and sintering pressure is normal pressure, finally obtains Ba0.6K0.4Fe2As2, powder is broken into get iron-based superconduction
Front axle shell；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 850 DEG C, and heat treatment time is 60 minutes, heat
Processing pressure is normal pressure.The Ag pipe equipped with iron-based superconducting precursor powder is inserted in Monel pipe (Monel pipe after heat treatment
Outside, including Ag pipe), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
In argon atmosphere under room temperature, temperature is first increased to cool down to 750 DEG C, pressure 300MPa, and after heat-insulation pressure keeping 22 hours
To room temperature, the iron-based superconducting line strips of compound jacket are taken out, obtain the compound Ba of single Monel silver0.6K0.4Fe2As2Superconducting wire band
Material finished product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 50000A/cm2(4.2K, 0T), superconducting transition temperature are not less than 37K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 99%.
Embodiment 5
The compound Ba of single iron silver0.6K0.4Fe2As2The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, iron-based superconduction raw material simple substance Ba, K, Fe, As is quasi- according to above-mentioned stoichiometric ratio
It really weighs and amounts to 20g, then load weighted simple substance raw material is packed into planetary ball mill ball milling 10 hours, is allowed to become powder.It will
The powder of milled is packed into Nb pipe, and heat treatment sintering is carried out after being shut both ends with copper plug, and the sintering time is 49 hours, burns
Junction temperature is 860 DEG C, and sintering pressure is normal pressure, finally obtains Ba0.6K0.4Fe2As2, powder is broken into get iron-based superconduction
Front axle shell；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 880 DEG C, and heat treatment time is 30 minutes, heat
Processing pressure is normal pressure.The Ag pipe equipped with iron-based superconducting precursor powder is inserted in iron pipe (iron pipe outside, Ag pipe after heat treatment
Inside), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
In argon atmosphere under room temperature, temperature is first increased to be cooled to 860 DEG C, pressure 20MPa, and after heat-insulation pressure keeping 20 hours
Room temperature takes out the iron-based superconducting line strips of compound jacket, obtains the compound Ba of single iron silver0.6K0.4Fe2As2Superconducting line strips finished product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 20000A/cm2(4.2K, 0T), superconducting transition temperature are not less than 37K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 97%.
Embodiment 6
The compound Ba of single stainless steel silver0.6K0.4Fe2As2The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, iron-based superconduction raw material simple substance Ba, K, Fe, As is quasi- according to above-mentioned stoichiometric ratio
It really weighs and amounts to 20g, then load weighted simple substance raw material is packed into planetary ball mill ball milling 10 hours, is allowed to become powder.It will
The powder of milled is packed into Nb pipe, and heat treatment sintering is carried out after being shut both ends with copper plug, and the sintering time is 35 hours, burns
Junction temperature is 900 DEG C, and sintering pressure is normal pressure, finally obtains Ba0.6K0.4Fe2As2, powder is broken into get iron-based superconduction
Front axle shell；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 820 DEG C, and heat treatment time is 50 minutes, heat
Processing pressure is normal pressure.The Ag pipe equipped with iron-based superconducting precursor powder is inserted in stainless steel tube (stainless steel tube after heat treatment
Outside, including Ag pipe), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
In argon atmosphere under room temperature, temperature is first increased to cool down to 700 DEG C, pressure 0.1MPa, and after heat-insulation pressure keeping 50 hours
To room temperature, the iron-based superconducting line strips of compound jacket are taken out, obtain the compound Ba of single stainless steel silver0.6K0.4Fe2As2Superconducting wire band
Material finished product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 50000A/cm2(4.2K, 0T), superconducting transition temperature are not less than 37K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 99%.
Embodiment 7
The compound Ba of single mild steel silver0.6K0.4Fe2As2The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, iron-based superconduction raw material simple substance Ba, K, Fe, As is quasi- according to above-mentioned stoichiometric ratio
It really weighs and amounts to 20g, then load weighted simple substance raw material is packed into planetary ball mill ball milling 10 hours, is allowed to become powder.It will
The powder of milled is packed into Nb pipe, and heat treatment sintering is carried out after being shut both ends with copper plug, and the sintering time is 35 hours, burns
Junction temperature is 900 DEG C, and sintering pressure is normal pressure, finally obtains Ba0.6K0.4Fe2As2, powder is broken into get iron-based superconduction
Front axle shell；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 840 DEG C, and heat treatment time is 40 minutes, heat
Processing pressure is normal pressure.The Ag pipe equipped with iron-based superconducting precursor powder is inserted in low carbon steel pipe (low carbon steel pipe after heat treatment
Outside, including Ag pipe), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
In argon atmosphere under room temperature, temperature is first increased to cool down to 890 DEG C, pressure 0.1MPa, and after heat-insulation pressure keeping 20 hours
To room temperature, the iron-based superconducting line strips of compound jacket are taken out, obtain the compound Ba of single mild steel silver0.6K0.4Fe2As2Superconducting wire band
Material finished product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 30000A/cm2(4.2K, 0T), superconducting transition temperature are not less than 37K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 99%.
Embodiment 8
The compound Ba of single high-carbon steel silver0.6K0.4Fe2As2The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, iron-based superconduction raw material simple substance Ba, K, Fe, As is quasi- according to above-mentioned stoichiometric ratio
It really weighs and amounts to 20g, then load weighted simple substance raw material is packed into planetary ball mill ball milling 10 hours, is allowed to become powder.It will
The powder of milled is packed into Nb pipe, and heat treatment sintering is carried out after being shut both ends with copper plug, and the sintering time is 35 hours, burns
Junction temperature is 900 DEG C, and sintering pressure is normal pressure, finally obtains Ba0.6K0.4Fe2As2, powder is broken into get iron-based superconduction
Front axle shell；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 850 DEG C, and heat treatment time is 80 minutes, heat
Processing pressure is normal pressure.The Ag pipe equipped with iron-based superconducting precursor powder is inserted in high carbon steel pipe (high carbon steel pipe after heat treatment
Outside, including Ag pipe), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
In argon atmosphere under room temperature, temperature is first increased to cool down to 880 DEG C, pressure 0.1MPa, and after heat-insulation pressure keeping 20 hours
To room temperature, the iron-based superconducting line strips of compound jacket are taken out, obtain the compound Ba of single high-carbon steel silver0.6K0.4Fe2As2Superconducting wire band
Material finished product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 28000A/cm2(4.2K, 0T), superconducting transition temperature are not less than 37K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 98%.
Embodiment 9
The compound Ba of single copper silver0.6K0.4Fe2As2The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, iron-based superconduction raw material simple substance Ba, K, Fe, As is quasi- according to above-mentioned stoichiometric ratio
It really weighs and amounts to 20g, then load weighted simple substance raw material is packed into planetary ball mill ball milling 10 hours, is allowed to become powder.It will
The powder of milled is packed into Nb pipe, and heat treatment sintering is carried out after being shut both ends with copper plug, and the sintering time is 35 hours, burns
Junction temperature is 900 DEG C, and sintering pressure is normal pressure, finally obtains Ba0.6K0.4Fe2As2, powder is broken into get iron-based superconduction
Front axle shell；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, Ag pipe both ends sealing, under argon atmosphere, to dress
There is the Ag pipe of iron-based superconducting precursor powder to be heat-treated, the heat treatment temperature is 800 DEG C, and heat treatment time is 30 minutes, heat
Processing pressure is normal pressure.After heat treatment by equipped with iron-based superconducting precursor powder Ag pipe be inserted in Cu pipe (Cu manage outside, Ag pipe
Inside), by it is a series of swage, drawing, rolling obtain compound iron-based superconducting line strips of jacket；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
In argon atmosphere under room temperature, temperature is first increased to cool down to 740 DEG C, pressure 200MPa, and after heat-insulation pressure keeping 20 hours
To room temperature, the iron-based superconducting line strips of compound jacket are taken out, obtain the compound Ba of single copper silver0.6K0.4Fe2As2Superconducting line strips at
Product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 31000A/cm2(4.2K, 0T), superconducting transition temperature are not less than 37K, and wire strip finished product provided in this embodiment is hardly deposited
In bulge, yield rate 98%.
Comparative example 1
The compound Ba of single copper silver0.6K0.4Fe2As2The preparation method of superconducting line strips, includes the following steps:
1) under Ar gas shielded atmosphere, iron-based superconduction raw material simple substance Ba, K, Fe, As is quasi- according to above-mentioned stoichiometric ratio
It really weighs and amounts to 20g, then load weighted simple substance raw material is packed into planetary ball mill ball milling 10 hours, is allowed to become powder.It will
The powder of milled is packed into Nb pipe, and heat treatment sintering is carried out after being shut both ends with copper plug, and the sintering time is 35 hours, burns
Junction temperature is 900 DEG C, and sintering pressure is normal pressure, finally obtains Ba0.6K0.4Fe2As2, powder is broken into get iron-based superconduction
Front axle shell；
2) the iron-based superconducting precursor powder for obtaining step 1) is packed into Ag pipe, and the sealing of Ag pipe both ends will be equipped with before iron-based superconduction
The Ag pipe for driving powder is inserted in Cu pipe (Cu manage outside, including Ag pipe), by it is a series of swage, drawing, rolling obtain compound jacket
Iron-based superconducting line strips；
3) it after the iron-based superconducting line strips both ends sealing of the compound jacket obtained step 2), is put into high-temperature high-pressure apparatus,
In argon atmosphere under room temperature, temperature is first increased to cool down to 740 DEG C, pressure 0.1MPa, and after heat-insulation pressure keeping 20 hours
To room temperature, the iron-based superconducting line strips of compound jacket are taken out, obtain the compound Ba of single copper silver0.6K0.4Fe2As2Superconducting line strips at
Product.
It is tested by comprehensive physical property measuring system (PPMS system) and using northeastern Japan university superconductor high-intensity magnetic field
The 10T low temperature high-intensity magnetic field test macro of room (HFLSM) measures the critical current of wire strip finished product, measures its critical current
For 200A/cm2(4.2K, 0T), superconducting transition temperature are not less than 37K, and the wire strip finished product that this comparative example provides has a large amount of drums
Packet, yield rate is only 25%.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (9)
1. a kind of preparation method of the iron-based superconducting line strips of compound jacket, which is characterized in that including under an inert atmosphere, to iron
Base superconducting precursor powder carries out the step of the first heat treatment.
2. preparation method according to claim 1, which is characterized in that the temperature of first heat treatment is 700-900 DEG C,
Time is 1-300 minutes, and pressure is normal pressure.
3. preparation method according to claim 1 or 2, which is characterized in that the preparation method of the iron-based superconducting precursor powder,
Include the following steps: under an inert atmosphere, the first sintering is carried out to iron-based superconduction raw material.
4. preparation method according to claim 3, which is characterized in that the time of first sintering is 1-200 hours, is burnt
The temperature of knot is 500-900 DEG C, and the pressure of sintering is normal pressure.
5. preparation method according to claim 1, which is characterized in that first heat treatment is by iron-based superconducting precursor powder
It is carried out after jacket metal tube in being packed into.
6. preparation method according to claim 5, which is characterized in that further include that the interior jacket metal tube is inserted in outsourcing
Cover metal tube in, to form compound jacket metal tube, the compound jacket metal tube is swaged, drawing, rolling processing with
Form the iron-based superconducting line strips of compound jacket.
7. preparation method according to claim 6, which is characterized in that further include to the compound iron-based superconducting wire band of jacket
Material carries out the step of the second heat treatment, and second heat treatment temperature is 500-950 DEG C, and the pressure of heat treatment is 0.1-
300MPa, heat treatment time are 1-12000 minutes.
8. preparation method according to claim 1-8, which is characterized in that the interior jacket metal tube and outer jacket
The metal of metal tube is selected from least one of gold, silver, copper, iron, niobium, nickel, chromium, tin, vanadium, violent, titanium, zirconium, molybdenum, tungsten, lead, aluminium, zinc,
Or the metal of the interior jacket metal tube and outer jacket metal tube is monel metal or low-carbon steel or stainless steel or high-carbon steel.
9. preparation method according to claim 1 to 9, which is characterized in that the iron-based superconducting precursor powder,
Composition includes Sr1-xKxFe2As2、Ba1-xKxFe2As2、FeSe1-xTex、KFeAs、SmFeAsO1-xFx、LaFeAsO1-xFxIn extremely
Few one kind, wherein doping coefficient x value is 0-1.
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