CN101550009A - Preparation method of iron-base high-temperature superconductor - Google Patents

Preparation method of iron-base high-temperature superconductor Download PDF

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CN101550009A
CN101550009A CNA2009100503974A CN200910050397A CN101550009A CN 101550009 A CN101550009 A CN 101550009A CN A2009100503974 A CNA2009100503974 A CN A2009100503974A CN 200910050397 A CN200910050397 A CN 200910050397A CN 101550009 A CN101550009 A CN 101550009A
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iron
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temperature superconductive
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CN101550009B (en
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黄富强
夏玉娟
方爱华
刘战强
谢晓明
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Shanghai Institute of Ceramics of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention relates to a preparation method of iron-base high-temperature superconductor, in which raw materials depending on a stoichiometric ratio is processed by high energy ball milling refinement and initial reactions, powder obtained from ball milling is formed by pressing, superconductive block or superconductive powder are obtained from formed block or un-formed powder via solid phase heat treatment. The method prepares iron-base high-temperature superconductors fast with low cost.

Description

The adulterated iron-based high-temperature superconductive preparation methods of one class
Technical field
The present invention relates to the adulterated iron-based high-temperature superconductive preparation methods of a class, can prepare the iron-based high-temperature superconductive material low-cost, apace with this method.Belong to the high temperature superconducting materia field.
Background technology
Superconduction is one of phenomenon the most marvellous in the physical world.General superconducting alloy resistance near zero absolute temperature the time is reduced to zero and is entered superconducting state, and high-temperature superconductor is meant that then material is extremely zero at certain higher relatively critical temperature resistor bust, and it has diverse Physical Mechanism and more wide application prospect.1986, the physicist found the copper oxide high-temperature superconductor, and this works in next year and has just obtained Nobel Prize in physics.Since then, scientists just never stopped the exploration of new high temperature superconducting materia, and when constantly pursuing more high-critical temperature, physicists are making great efforts announcement mechanism wherein always.At present, nearly all in the world developed country all has research institution to be engaged in the research of high-temperature superconductor aspect.On the one hand, the exploration of high-temperature superconductor mechanism is being attracted numerous physicists' concern; On the other hand, because the energy and other specific demands, industry member is placed high hopes to superconductor technology, but since the critical temperature of general superconducting alloy near zero absolute temperature, it is heavy that the refrigerating reason causes using obstacle, and high-temperature superconductor then is one of following outlet of expecting of everybody.
In by the end of February, 2008, and the H.Hosono study group of Tokyo polytechnical university has reported La[O on the JASC magazine 1-xF x] research of FeAs material, and find temperature this material performance supraconductivity (JACS 130,2008,3296) when 26K.Iron performance supraconductivity, this result be once the concern that the Chinese scholar occurs promptly being subjected to, and made huge contribution in this field.These iron-based superconductor matrix all comprise [FeAs] or [FeSe] layer, and the crystalline structure of this structural unit is anti-oxidation lead layer structure, and the Fe atom is formed foursquare coplane array.Main iron-based superconductor is at LnFeOX (Ln is rare earth element, Y, and X is As, P), AFe 2X 2Induce superconducting characteristic by doping, room etc. in (A is basic metal, alkaline-earth metal, and X is As, P), the FeQ matrix such as (Q are S, Se, Te).
Yet the preparation of iron-based superconducting material at present is still a difficult problem, and its reason is that sample purity and quantity that the made silica tube about 1cm in laboratory is prepared do not reach application requiring.Therefore, cheapness and reliable preparation seems extremely important, the present invention intends developing a kind of high energy ball mill method and prepares iron-based superconducting material for this reason, to realize the preparation of magnanimity, reduces thermal treatment temp, reduces heat treatment time.
Summary of the invention
The object of the present invention is to provide a class iron-based high-temperature superconductive preparation methods, this method can be prepared the iron-based high-temperature superconductive material low-cost and apace, realizes the magnanimity preparation, reduces the solid state reaction temperature, improves the purity of finished product.Concrete preparation process is:
(1) presses the raw material of stoichiometric ratio through high-energy ball milling refinement and initial reaction;
(2) the powder compression moulding of ball-milling processing;
(3) powder of the block of moulding or not moulding obtains superconducting block or superconduction powder by solid phase thermal treatment.
Method provided by the invention is applicable to LnFeOX (Ln is rare earth element, Y, and X is As, P), AFe 2X 2Induce superconducting characteristic by doping, room etc. in (A is basic metal, alkaline-earth metal, and X is As, P), the FeQ matrix such as (Q are S, Se, Te).
Wherein in the LnFeOX base iron-based high-temperature superconductive material, Ln is rare earth element, Y, X is As, P, and alkaline-earth metal, alkaline earth metal doping Ln position (doping is 0.02-0.30), Co doped F e position (doping is 0.02-0.50), F doping O (doping is 0.02-0.20) position or oxygen room (room amount 0.02-0.10) all can induce supraconductivity.Its raw material can be Ln, Fe, Co, As, Ln 2O 3, Y 2O 3, FeO, CoO, Fe 3O 4, Co 3O 4, Fe 2O 3, LnX, FeX (X=As, P), Fe 2X (X=As, P), LnF 3, LnOF, FeOF, LnFeOAs be formulated by stoichiometric ratio.
At AFe 2X 2In the base iron-based high-temperature superconductive material, A is basic metal, alkaline-earth metal, X is As, P, and alkaline-earth metal and alkaline-earth metal mix (doping is 0.05-0.95) mutually, rare earth doped A position (doping is 0.05-0.5), Co doped F e position (doping is 0.02-0.50) all can induce supraconductivity.Its raw material can be A, Ln, Fe, Co, As, A 3X 2, LnX, FeX (X=As, P), Fe 2X (X=As, P), AFe 2As 2Formulated by stoichiometric ratio.
In FeQ base iron-based high-temperature superconductive material, Q is S, Se, Te, and Q room or Q position S, Se and Te mix (0-1.00) mutually and can induce supraconductivity, and the room amount is 0.01-0.30.Its raw material can be that Fe, Se, FeSe are formulated by stoichiometric ratio.
Specifically, at first by the raw material high-energy ball milling of stoichiometric ratio 0.5-12 hour, utilize irony wear-resistant medium (ball milling in the ball grinder of attrition resistant mould steel) in mechanical movement to raw material collide, push, broken, mixed, energy exchange causes abundant refinement of raw material and partial reaction; The ball milling time is 0.5-24 hour; Then by moulded section; The solid phase thermal treatment in Ar atmosphere or vacuum sealing system (as silica tube) of the powder of the block of moulding or not moulding obtains superconducting block or superconduction powder.For adulterated LnFeOX base, adulterated AFe 2X 2The heat treated temperature of the solid phase of basic or adulterated FeQ base is respectively 900-1200 ℃, 700-1000 ℃ and 200-700 ℃.
Description of drawings
(annealing conditions is 400 ℃, XRD 24h) after (the ball milling time is 12h) and the thermal treatment behind Fig. 1 (a) Fe-Se simple substance powder high-energy ball milling.
The SEM shape appearance figure of Fig. 2 high-energy ball milling 10h powder.
Fig. 3 α-meterings such as FeSe pure phase vary with temperature than the resistivity of compound, and illustration varies with temperature for the resistivity in the 2-16K scope.
Embodiment
Below by specific embodiment further to illustrate substantive distinguishing features of the present invention and obvious improvement.The present invention only is confined to embodiment by no means.Be better confirmation creativeness of the present invention and invention effect simultaneously, listed two Comparative Examples, more to show creativeness of the present invention from the another side.
Embodiment 1
With Fe and Se simple substance by stoichiometric ratio weighing in 1: 1 (gross weight is 3 grams), (XRD saw the Lower Half of accompanying drawing 1 to ball milling in 12 hours in attrition resistant mould steel ball grinder, pattern is seen accompanying drawing 2), place vacuum-tight silica tube, 400 ℃ of reactions 24 hours, obtain cubic phase FeSe (XRD sees the first half of accompanying drawing 1).Physicals test macro (PPMS) test R-T characteristic is found superconducting characteristic, T C OnsetBe 8.9K (seeing accompanying drawing 3).
Embodiment 2
By stoichiometric ratio weighing in 1: 1 (gross weight is 3 grams), ball milling is 3 hours in attrition resistant mould steel ball grinder, places vacuum-tight silica tube, 500 ℃ of reactions 5 hours, obtains cubic phase FeSe with Fe and Se simple substance.Physicals test macro (PPMS) test R-T characteristic is found superconducting characteristic, T C OnsetBe 8.8K.
Embodiment 3
By stoichiometric ratio weighing in 1: 0.9 (gross weight is 3 grams), ball milling is 0.5 hour in attrition resistant mould steel ball grinder, places vacuum-tight silica tube, 600 ℃ of reactions 5 hours, obtains cubic phase FeSe with Fe and Se simple substance 0.9Physicals test macro (PPMS) test R-T characteristic is found superconducting characteristic, T C OnsetBe 8.5K.
Embodiment 4
With SmAs, FeO, SmOF and Fe 2As presses SmFeO 1-xF xAs (x=0.12) stoichiometric ratio weighing (gross weight is 4 grams), ball milling is 2 hours in attrition resistant mould steel ball grinder, places the sealed furnace of Ar gas shiled, 1100 ℃ of reactions 5 hours, obtains SmFeO 0.88F 0.12As.XRD analysis shows that sample is a pure phase; Physicals test macro (PPMS) test R-T characteristic is found superconducting temperature T C OnsetBe 52.3K.
Embodiment 5
With LaAs, La, FeO, Fe 2O 3, LaF 3And Fe 2As presses LaFeO 1-xF xAs (x=0.12) stoichiometric ratio weighing (gross weight is 4 grams), ball milling is 1 hour in attrition resistant mould steel ball grinder, places the sealed furnace of Ar gas shiled, 1000 ℃ of reactions 10 hours, obtains LaFeO 0.88F 0.12As.XRD analysis shows that sample is a pure phase; Physicals test macro (PPMS) test R-T characteristic is found superconducting temperature T C OnsetBe 28.2K.
Embodiment 6
With Y 2O 3, Y, FeAs, FeOF and Fe press YFeO 1-xF xAs (x=0.15) stoichiometric ratio weighing (gross weight is 4 grams), ball milling is 10 hours in attrition resistant mould steel ball grinder, places the sealed furnace of Ar gas shiled, 1200 ℃ of reactions 10 hours, obtains YFeO 0.85F 0.15As.XRD analysis shows that sample is a pure phase; Physicals test macro (PPMS) test R-T characteristic is found superconducting temperature T C OnsetBe 32.1K.
Embodiment 7
NdAs, FeO, Fe are pressed NdFeO 1-x xAs (x=0.10) stoichiometric ratio weighing (gross weight is 4 grams), ball milling is 1 hour in attrition resistant mould steel ball grinder, places the sealed furnace of Ar gas shiled, 1000 ℃ of reactions 10 hours, obtains NdFeO 0.90As.XRD analysis shows that sample is a pure phase; Physicals test macro (PPMS) test R-T characteristic is found superconducting temperature T C OnsetBe 31.7K.
Embodiment 8
BaAs, FeAs and KAs are pressed Ba 1-xK xFe 2As 2(x=0.40) stoichiometric ratio weighing (gross weight is 4 grams), ball milling is 1 hour in attrition resistant mould steel ball grinder, places the sealed furnace of Ar gas shiled, 700 ℃ of reactions 5 hours, obtains Ba 0.6K 0.4Fe 2As 2XRD analysis shows that sample is a pure phase; Physicals test macro (PPMS) test R-T characteristic is found superconducting temperature T C OnsetBe 38.3K.
Embodiment 9
SrAs, FeAs, LaAs and As are pressed Sr 1-xLa xFe 2As 2(x=0.20) stoichiometric ratio weighing (gross weight is 4 grams), ball milling is 0.5 hour in attrition resistant mould steel ball grinder, places the sealed furnace of Ar gas shiled, 900 ℃ of reactions 10 hours, obtains Sr 1.8La 0.2Fe 2As 2XRD analysis shows that sample is a pure phase; Physicals test macro (PPMS) test R-T characteristic is found superconducting temperature T C OnsetBe 26.9K.
Embodiment 10
SrAs, FeAs, CoAs and As are pressed SrFe 2-xCo xAs 2(x=0.20) stoichiometric ratio weighing (gross weight is 4 grams), ball milling is 1 hour in attrition resistant mould steel ball grinder, places the sealed furnace of Ar gas shiled, 600 ℃ of reactions 2 hours, obtains SrFe 1.8Co 0.2As 2XRD analysis shows that sample is a pure phase; Physicals test macro (PPMS) test R-T characteristic is found superconducting temperature T C OnsetBe 19.7K.
Comparative Examples 1
Fe and Se simple substance by stoichiometric ratio weighing in 1: 1 (gross weight is 3 grams), were ground 15 minutes, place vacuum-tight silica tube, reacted 24 hours, obtain six side's phase FeSe at 300 ℃.Physicals test macro (PPMS) test R-T characteristic is not found superconducting characteristic.
Fe and Se simple substance by stoichiometric ratio weighing in 1: 1 (gross weight is 3 grams), were ground 15 minutes, place vacuum-tight silica tube, reacted 24 hours, obtain six side's phase FeSe at 600 ℃.Physicals test macro (PPMS) test R-T characteristic is not found superconducting characteristic.
Use conventional solid phase synthesis, attempt the cubic phase FeSe that various reaction conditionss can't obtain having supraconductivity.
Comparative Examples 2
With SmAs, FeO, SmOF and Fe 2As presses SmFeO 1-xF xAs (x=0.15) stoichiometric ratio weighing (gross weight is 2 grams), place vacuum-tight silica tube in 900 ℃ of reactions 24 hours, 1050 ℃ of reactions 48 hours, grinding obtained SmFeO evenly 1150 ℃ of reactions 24 hours in glove box once more after grinding evenly in glove box 0.85F 0.15As.XRD analysis contains the diffraction peak of micro-SmOF; Physicals test macro (PPMS) test R-T characteristic is found superconducting temperature T C OnsetBe 45.5K.
Even processing method difference identical from the composition shown in this Comparative Examples 1 visible embodiment 1-3 but that use, the material that can't obtain to have supraconductivity; And Comparative Examples 2 is similar with embodiment 4 compositions shown in the present, but uses preparation method provided by the invention, and the material of being produced has higher superconducting temperature.

Claims (6)

1, the adulterated iron-based high-temperature superconductive preparation methods of a class is characterized in that preparation process is:
(1) presses the raw material of stoichiometric ratio through high-energy ball milling refinement and initial reaction;
(2) the powder compression moulding of ball-milling processing;
(3) powder of the block of moulding or not moulding obtains superconducting block or superconduction powder by solid phase thermal treatment;
Described adulterated iron-based high-temperature superconductive material is any in following three kinds:
(a) described iron-based high-temperature superconductive material is LnFeOX, and in the formula, Ln is rare earth element or Y; X is As or P; The doping of alkaline-earth metal or alkaline earth metal doping Ln position is that the doping of 0.02-0.30, Co doped F e position is that the doping of 0.02-0.50, F doping O is that the room amount in 0.02-0.20 position or oxygen room is 0.02-0.10;
(b) described iron-based high-temperature superconductive material is AFe 2X 2Base, A is basic metal or alkaline-earth metal in the formula; X is As or P; The mutual adulterated doping of alkaline-earth metal and alkaline-earth metal is that the doping of 0-1.00, rare earth doped A position is that the doping of 0.05-0.50, Co doped F e position is 0.02-0.50;
(c) described iron-based high-temperature superconductive material is the FeQ base, and Q is S, Se or Te in the formula; Q is that room or Q position are that the doping that S, Se or Te mix mutually is 0-1.00; The room amount of Q position is 0.01-0.30.
2, by the described adulterated iron-based high-temperature superconductive preparation methods of claim 1, it is characterized in that described high-energy ball milling is to carry out in the ball grinder of attrition resistant mould steel.
3, by claim 1 or 2 described adulterated iron-based high-temperature superconductive preparation methods, the time that it is characterized in that described high-energy ball milling is 0.5-12 hour.
4, by the described adulterated iron-based high-temperature superconductive preparation methods of claim 1, it is characterized in that:
A) the heat treated temperature of solid phase to adulterated LnFeOX iron-based high-temperature superconductive material is 900-1200 ℃;
B) to adulterated AFe 2X 2The solid phase thermal treatment temp of iron-based high-temperature superconductive material is 700-1000 ℃;
C) the solid phase thermal treatment temp to adulterated FeQ base high temperature super conductive material is 200-700 ℃.
5, by claim 1 or 4 described adulterated iron-based high-temperature superconductive preparation methods, it is characterized in that solid phase thermal treatment is to carry out in the closed system of Ar atmosphere or vacuum.
6, by the described adulterated iron-based high-temperature superconductive preparation methods of claim 5, the closed system that it is characterized in that described vacuum is vacuum-tight silica tube.
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CN102082010A (en) * 2010-12-28 2011-06-01 中国科学院电工研究所 Method for preparing iron-based superconductor
CN101707089B (en) * 2009-12-15 2011-08-10 中国科学院电工研究所 Method for improving upper critical field and critical current density of iron-based superconductor
CN103771844A (en) * 2012-10-24 2014-05-07 中国科学院上海硅酸盐研究所 Doping method of iron-based superconducting material
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