CN104217817B - Preparation (Ba/Sr)1-xkxfe2as2superconducting wire or the method for band - Google Patents
Preparation (Ba/Sr)1-xkxfe2as2superconducting wire or the method for band Download PDFInfo
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Abstract
The present invention relates to one and prepare (Ba/Sr)1‑xKxFe2As2Superconducting wire or the method for band, concretely comprise the following steps: (a) uses quartz ampoule sealed-tube method to prepare KAs, the intermediate product of (Ba/Sr) As；B (), by KAs, intermediate product and the Fe powder of (Ba/Sr) As, As powder is according to name component proportion ball milling mix homogeneously, more at high temperature reacts, and synthesizes (Ba/Sr)1‑xKxFe2As2Precursor powder；C () is inserted after being sufficiently mixed by the Sn powder of precursor powder Yu 5wt.% uniformly in silver sleeve pipe, then make wire rod by machining；Take a part of wire rod and become band by flat rolling, finally wire rod or band are carried out high-temperature heat treatment.The inventive method can be effectively improved (Ba/Sr)1‑xKxFe2As2Precursor powder quality, improves purity and the uniformity of superconducting phase, strengthens superconducting core texture degree and consistency, thus improve (Ba/Sr)1‑ xKxFe2As2Wire rod or the critical current density of band.The inventive method technique is simple, with low cost, is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to one (Ba/Sr)1-xKxFe2As2Superconducting wire or the preparation method of band.
Background technology
The development that iron-based superconductor is superconductor applications found for 2008 brings new opportunity.Wherein, FeAs-122 superconductor has Tc max～the superconducting transition temperature of 38K, and anisotropy is little, upper critical field is high so that it has broad application prospects at superconductive power transmission and superconducting magnet field.Iron-based superconducting material belongs to ceramic structure, and fragility is higher, and plastic working is relatively difficult.Therefore, powder-in-tube technique (PIT method) becomes the one preferred technique approach preparing iron-based superconducting wire or band.PIT method is to be seated in after starting powder mix homogeneously in metal tube, then by swaging, drawing, the cold working operation such as rolling metal tube is moulded wire rod or band method, have been widely used for Bi-2223 and MgB2Superconducting wire or the preparation of band.At present, in the world general using Ba/Sr granule, K block, Fe powder and As powder as raw material thing, after being mixed by ball milling, high temperature sintering synthesis (Ba/Sr)1-xKxFe2As2Superconduction precursor powder [Sci.Rep.4,4465 (2014), Supercond.Sci.Tech.26,115007 (2013)].But, owing to Ba/Sr granule is relatively big, quality is harder, and K block quality is softer, and ball-milling method is difficult to be sufficiently mixed by raw material uniformly, causes superconducting phase in precursor powder uneven, is unfavorable for the raising of superconduction critical electric current.Recently, the method repeatedly rolling sintering is used to strengthen Ba1-xKxFe2As2The High-Field current capacity of superconducting tape, cold-press method, pressure sintering are also applied to the preparation [Appl.Phys.Lett.104,202601 (2014)] of FeAs-122 superconducting tape.But, above method or technique are complicated, or depend on high pressure equipment, are not particularly suited for low cost, large-scale industrial production.Accordingly, it would be desirable to develop a kind of technique simple high-performance iron-based superconducting wire or band preparation method, reduce production cost, improve production efficiency.
Summary of the invention
In order to simplify FeAs-122 iron-based superconducting wire or the preparation technology of band, reducing its dependency to high pressure equipment, the present invention proposes one and prepares (Ba/Sr)1-xKxFe2As2Superconducting wire or the method for band.The inventive method can be effectively improved (Ba/Sr)1-xKxFe2As2Precursor powder quality, improves purity and the uniformity of superconducting phase, strengthens superconducting core texture degree and consistency, thus improve (Ba/Sr)1-xKxFe2As2Wire rod or the critical current density of band.The inventive method technique is simple, with low cost, is suitable for large-scale industrial production.
One prepares (Ba/Sr)1-xKxFe2As2Superconducting wire or the method for band, it is characterised in that the processing step of described preparation method is as follows:
1, quartz ampoule sealed-tube method is utilized to prepare (Ba/Sr) As intermediate product and KAs intermediate product:
Ba or Sr granule is uniform according to the mixed in molar ratio of (Ba/Sr): As=1:1 with As powder, more mixed powder is placed in corundum set, it is vacuum-sealed in quartz ampoule and carries out heat treatment, obtaining (Ba/Sr) As intermediate product.K block and As powder is uniform according to the mixed in molar ratio of K:As=1:1, more mixed powder is placed in corundum set, in being vacuum-sealed in quartz ampoule and carry out heat treatment, obtain KAs intermediate product.
2, metal tube sealed-tube method synthesis (Ba/Sr) is used1-xKxFe2As2Precursor powder:
Take (Ba/Sr) As intermediate product and the intermediate product of KAs that step 1 prepares, uniform according to (Ba/Sr) As:KAs:Fe:As=(1-x): the mixed in molar ratio of (x+0.1): 2:0.9 with Fe powder, As powder, x is chemical formula (Ba/Sr)1-xKxFe2As2In x.Being inserted by mixed powder in Nb pipe, Nb pipe two copper plug seals, then is placed in iron pipe by Nb pipe in Ar atmosphere is enclosed, and seals with argon arc welding.Finally iron pipe is thermally treated resulting in (Ba/Sr)1-xKxFe2As2Precursor powder.
3, superconducting wire or band are prepared:
(Ba/Sr) that step 2 is prepared1-xKxFe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares wire rod；Take a part of wire rod and become band by flat rolling.Finally wire rod or vacuum web are sealed in quartz ampoule, are warmed up to 850-950 DEG C and are incubated 0.5 hour.
The heat treatment temperature preparing (Ba/Sr) As intermediate product in described step 1 is 400-900 DEG C, and temperature retention time is 12-48 hour；The heat treatment temperature preparing KAs intermediate product in described step 1 is 300-600 DEG C, and temperature retention time is 3-10 hour.
To iron pipe heat treatment in described step 2, prepare (Ba/Sr)1-xKxFe2As2The temperature of precursor powder is 900 DEG C, and temperature retention time is 35 hours.
In step 1 and step 2, to Ba/Sr granule, K block, As powder, (Ba/Sr) As intermediate product, KAs intermediate product and the weighing of Fe powder, grinding, tubulature operation all complete in the glove box of full Ar gas.
In step 1 and step 2, by ball-milling method, raw material thing is sufficiently mixed uniformly, ball grinder is full of Ar gas.
In step 1 and step 3, the vacuum of vacuum-packed quartz ampoule is better than 10-2Pa。
In step 2, (Ba/Sr)1-xKxFe2As2The span of the x in precursor powder is 0.1-1.
In step 3, (Ba/Sr)1-xKxFe2As2The thickness range of band is 0.1-0.8mm.
The present invention compared with prior art has the advantage that
(1) the precursor powder purity that prepared by the inventive method is high, and uniformity is good, and in wire rod and band, the ratio of superconducting phase is close to 100%.The inventive method can be effectively improved the consistency of band superconducting core, texture degree and critical current density.
(2) the inventive method technique is simple, with low cost, does not relies on high pressure equipment, is suitable for large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is Ba in the embodiment of the present invention 10.6K0.4Fe2As2The X ray diffracting spectrum of precursor powder.
Fig. 2 is Ba in the embodiment of the present invention 10.6K0.4Fe2As2Web Transporting critical current density is with magnetic induction change curve.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
(1) the Ba granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 600 DEG C of insulations 24 hours, obtain BaAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 400 DEG C of insulations 5 hours, obtain KAs intermediate product.
(3) take step (1) prepare BaAs intermediate product and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component Ba0.6K0.5Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain Ba0.6K0.4Fe2As2Precursor powder.
(4) Ba that step (3) is prepared0.6K0.4Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.3mm by flat rolling.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 900 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa,.
Ba prepared by the present embodiment is recorded by the PPMS-9 test system of Quantum Design company0.6K0.4Fe2As2The superconducting transition temperature of superconducting tape is Tc=38K, superconduction ratio reaches 97%.Bruker D8Advance X-ray diffractometer is utilized to record Ba prepared by the present embodiment0.6K0.4Fe2As2The X ray diffracting spectrum of precursor powder, except Ba0.6K0.4Fe2As2The diffraction maximum of other dephasigns is not found outside the diffraction maximum of principal phase.In the X ray diffracting spectrum of the superconducting core of superconducting tape, (00l) peak is remarkably reinforced by force compared with precursor powder, and being calculated F value by Lotgering method is 0.69, is the peak in iron-based superconducting tape, illustrates that it has high texture degree.Micro Vickers hardness tester is utilized to record Ba prepared by the present embodiment0.6K0.4Fe2As2The Vickers hardness of the superconducting core of superconducting tape reaches 136, illustrates that it has high-compactness.The 14T low temperature high-intensity magnetic field test system utilizing northeastern Japan university superconductor high-intensity magnetic field laboratory (HFLSM) records, Ba prepared by the present embodiment0.6K0.4Fe2As2Superconducting tape reaches 5.4 × 10 in 4.2K, 10T magnetic field lower critical electric current density4A/cm2。
Embodiment 2
(1) the Sr granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 400 DEG C of insulations 48 hours, obtain SrAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 300 DEG C of insulations 10 hours, obtain KAs intermediate product.
(3) take step (1) prepare SrAs and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component Sr0.6K0.5Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain Sr0.6K0.4Fe2As2Precursor powder.
(4) Sr that step (3) is prepared0.6K0.4Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.3mm by flat rolling.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 850 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa。
Embodiment 3
(1) the Sr granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 800 DEG C of insulations 12 hours, obtain SrAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 500 DEG C of insulations 3 hours, obtain KAs intermediate product.
(3) take step (1) prepare SrAs and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component Sr0.6K0.5Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain Sr0.6K0.4Fe2As2Precursor powder.
(4) Sr that step (3) is prepared0.6K0.4Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.6mm by flat rolling.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 920 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa。
Embodiment 4
(1) the Ba granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 900 DEG C of insulations 12 hours, obtain BaAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 600 DEG C of insulations 3 hours, obtain KAs intermediate product.
(3) take step (1) prepare BaAs and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component Ba0.6K0.5Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain Ba0.6K0.4Fe2As2Precursor powder.
(4) Ba that step (3) is prepared0.6K0.4Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.1mm by flat rolling.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 950 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa。
Embodiment 5
(1) the Ba granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 600 DEG C of insulations 24 hours, obtain BaAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 400 DEG C of insulations 5 hours, obtain KAs intermediate product.
(3) take step (1) prepare BaAs and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component Ba0.6K0.5Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain Ba0.6K0.4Fe2As2Precursor powder.
(4) Ba that step (3) is prepared0.6K0.4Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.8mm by flat rolling.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 900 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa。
Embodiment 6
(1) the Ba granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 600 DEG C of insulations 24 hours, obtain BaAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 400 DEG C of insulations 5 hours, obtain KAs intermediate product.
(3) take step (1) prepare BaAs and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component Ba0.9K0.2Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain Ba0.9K0.1Fe2As2Precursor powder.
(4) Ba that step (3) is prepared0.9K0.1Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.3mm by flat rolling further.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 900 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa。
Embodiment 7
(1) the Sr granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 600 DEG C of insulations 24 hours, obtain SrAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 400 DEG C of insulations 5 hours, obtain KAs intermediate product.
(3) take step (1) prepare SrAs and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component Sr0.4K0.7Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain Sr0.4K0.6Fe2As2Precursor powder.
(4) Sr that step (3) is prepared0.4K0.6Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.3mm by flat rolling.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 900 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa。
Embodiment 8
(1) the Sr granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 600 DEG C of insulations 24 hours, obtain SrAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 400 DEG C of insulations 5 hours, obtain KAs intermediate product.
(3) take step (1) prepare SrAs and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component Sr0.2K0.9Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain Sr0.2K0.8Fe2As2Precursor powder.
(4) Sr that step (3) is prepared0.2K0.8Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.3mm by flat rolling.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 900 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa。
Embodiment 9
(1) the Sr granule that purity is 99.9% is mixed homogeneously according to the abundant ball milling of the mol ratio of 1:1 with the As powder that purity is 99.95%.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 600 DEG C of insulations 24 hours, obtain SrAs intermediate product.
(2) according to the mol ratio of 1:1, the K block that purity is 99.95% and the As powder that purity is 99.95% are placed in ball grinder fully ball milling to mix homogeneously.Being placed in by the powder mixed in corundum set, then be vacuum-sealed in quartz ampoule by corundum set, the vacuum of quartz ampoule is better than 10-2Pa.Quartz ampoule is placed in Muffle furnace and is warmed up to 400 DEG C of insulations 5 hours, obtain KAs intermediate product.
(3) take step (1) prepare SrAs and step (2) prepare KAs intermediate product, with Fe powder, As powder according to name component K1.1Fe2As2Ball milling mix homogeneously.Being loaded by powder in Nb pipe, Nb pipe two Cu plug seals.Again by the Nb seal of tube in the iron pipe of full Ar gas.Iron pipe is placed in tube furnace and is warmed up to 900 DEG C, be incubated 35 hours, obtain K1.0Fe2As2Precursor powder.
(4) K that step (3) is prepared1.0Fe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt.%.Silver sleeve pipe is carried out machining, prepares the wire rod of a diameter of 1.9mm；Take the band that a part of wire rod becomes thickness to be 0.3mm by flat rolling.Finally wire rod or vacuum web being sealed in quartz ampoule, be warmed up to 900 DEG C and be incubated 0.5 hour, the vacuum of quartz ampoule is better than 10-2Pa。
Claims (5)
1. prepare (Ba/Sr) for one kind1-xKxFe2As2Superconducting wire or the method for band, it is characterised in that the processing step of described preparation method is as follows:
(1) quartz ampoule sealed-tube method is utilized to prepare (Ba/Sr) As intermediate product and KAs intermediate product:
Ba or Sr granule is uniform according to the mixed in molar ratio of (Ba/Sr): As=1:1 with As powder, more mixed powder is placed in corundum set, it is vacuum-sealed in quartz ampoule and carries out heat treatment, obtaining (Ba/Sr) As intermediate product；K block is uniform according to the mixed in molar ratio of K:As=1:1 with As powder, more mixed powder is placed in corundum set, it is vacuum-sealed in quartz ampoule and carries out heat treatment, obtaining KAs intermediate product；
(2) metal tube sealed-tube method synthesis (Ba/Sr) is used1-xKxFe2As2Precursor powder:
Take (Ba/Sr) As intermediate product and KAs intermediate product that step (1) prepares, uniform according to (Ba/Sr) As:KAs:Fe:As=(1-x): the mixed in molar ratio of (x+0.1): 2:0.9 with Fe powder, As powder, x is chemical formula (Ba/Sr)1-xKxFe2As2In x, span is 0.1-1；Being inserted by mixed powder in Nb pipe, Nb pipe two copper plug seals, then is placed in iron pipe by Nb pipe in Ar atmosphere is enclosed, and seals with argon arc welding；Finally iron pipe is thermally treated resulting in (Ba/Sr)1-xKxFe2As2Precursor powder；
(3) superconducting wire or band: (Ba/Sr) step (2) prepared is prepared1-xKxFe2As2Precursor powder is inserted in silver-colored sleeve pipe after being sufficiently mixed uniformly with the Sn powder of 5wt%, silver sleeve pipe is carried out machining, prepares wire rod；Take a part of wire rod and become band by flat rolling；Finally wire rod or vacuum web are sealed in quartz ampoule, are warmed up to 850-950 DEG C and are incubated 0.5 hour；
In described step (1), the heat treatment temperature of preparation (Ba/Sr) As intermediate product is 400-900 DEG C, and temperature retention time is 12-48 hour；The heat treatment temperature preparing KAs intermediate product in described step (1) is 300-600 DEG C, and temperature retention time is 3-10 hour；
In described step (2), to iron pipe heat treatment, prepare (Ba/Sr)1-xKxFe2As2The temperature of precursor powder is 900 DEG C, and temperature retention time is 35 hours.
Prepare (Ba/Sr) the most as claimed in claim 11-xKxFe2As2Superconducting wire or the method for band, it is characterized in that, in described step (1) and step (2), to Ba/Sr granule, K block, As powder, (Ba/Sr) As intermediate product, KAs intermediate product, and the weighing of Fe powder, grinding, tubulature operation all complete in the glove box of full Ar gas.
Prepare (Ba/Sr) the most as claimed in claim 11-xKxFe2As2Superconducting wire or the method for band, it is characterised in that in described step (1) and step (2), be sufficiently mixed uniformly by ball-milling method by raw material thing, be full of Ar gas in ball grinder.
Prepare (Ba/Sr) the most as claimed in claim 11-xKxFe2As2Superconducting wire or the method for band, it is characterised in that in described step (1) and step (3), the vacuum of described quartz ampoule is better than 10-2Pa。
Prepare (Ba/Sr) the most as claimed in claim 11-xKxFe2As2Superconducting wire or the method for band, it is characterised in that (Ba/Sr) prepared by described step (3)1-xKxFe2As2The thickness of band is 0.1-0.8mm.
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| CN106601366B (en) * | 2016-12-14 | 2018-07-13 | 中国科学院电工研究所 | A kind of preparation method of 122 type iron-based compound superconducting wire or band |
| CN108962487B (en) * | 2018-06-15 | 2019-09-06 | 中国科学院电工研究所 | A kind of processing technology improving Fe-base compound superconducting tape performance |
| CN111968788A (en) * | 2020-08-17 | 2020-11-20 | 福建师范大学 | Preparation method of high-performance iron-based superconducting precursor powder and superconducting tape |
| CN113643853B (en) * | 2021-08-13 | 2023-03-03 | 中国科学院电工研究所 | Application of KF as raw material in preparation of 122-series iron-based superconductor and preparation method of 122-series iron-based superconductor |
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