CN108179465A - The preparation method of high-temperature superconductor - Google Patents

The preparation method of high-temperature superconductor Download PDF

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Publication number
CN108179465A
CN108179465A CN201611119194.2A CN201611119194A CN108179465A CN 108179465 A CN108179465 A CN 108179465A CN 201611119194 A CN201611119194 A CN 201611119194A CN 108179465 A CN108179465 A CN 108179465A
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China
Prior art keywords
temperature
baco3
powder
cuo
solution
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Pending
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CN201611119194.2A
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Chinese (zh)
Inventor
房毅
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Shandong Yuan Kun Superconducting Mstar Technology Ltd
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Shandong Yuan Kun Superconducting Mstar Technology Ltd
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Priority to CN201611119194.2A priority Critical patent/CN108179465A/en
Publication of CN108179465A publication Critical patent/CN108179465A/en
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B19/00Liquid-phase epitaxial-layer growth
    • C30B19/12Liquid-phase epitaxial-layer growth characterised by the substrate
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • C30B29/225Complex oxides based on rare earth copper oxides, e.g. high T-superconductors

Abstract

The invention discloses a kind of preparation methods of high temperature superconducting film, include the following steps:A) Ba Cu O powder is prepared;B) Ba Cu O pioneers powder is added in the Y2O3 crucibles in crystal growing furnace, is heated to the first temperature and is kept the temperature, obtain Y Ba Cu O solution;C) Ba Cu O pioneer's powder is added in solution, and kept the temperature;D) solution is reduced to second temperature with the first cooling rate;E) solution that step d) obtains is inserted into using the NGO monocrystal substrates for being fixed on connecting rod as seed crystal material, grows the YBCO liquid phase epitaxy films of pure a axis orientation.The present invention, as seed crystal, the amount of Ba Cu O powder and the time of heat preservation is added in by control to realize that epitaxial growth a axis is orientated YBCO superconducting thick-films for the second time using NGO monocrystal substrates.

Description

The preparation method of high-temperature superconductor
Technical field
The present invention relates to a kind of preparation methods of high temperature superconducting materia.
Background technology
High temperature superconducting materia has excellent superconductivity in liquid nitrogen temperature, therefore in superconducting energy storage, superconducting motor, nuclear-magnetism The fields such as resonance, device research and development possess extremely important application value.The base application research of high quality film has attracted large quantities of materials The extensive concern of material neo-confucian.
The structures shape of the material performance of material, and then affect the application of material in practice.In general, by In YBCO Superconducting Crystals lattice constant in both direction a axis and b axis approximately equals, i.e. YBCO crystal structures are being similar to one just Quadrangular.Thus, YBCO superconducting thick-films typically exhibit two kinds of orientations, i.e. a axis orientation and c-axis orientation.The YBCO high of c-axis orientation Temperature superconductive thick film has higher critical current density, thus has important application in terms of electric power transport, and a axis orientation REBCO high temperature superconductive thick films have vital application in terms of Josephson's junction device.
Liquid phase epitaxy(Liquid Phase Epitaxy, LPE)It is generally considered a kind of YBCO superconductions of great potential The preparation method of thick film.During rheotaxial growth YBCO superconducting thick-films, seed crystal is fixed in connecting rod and slowly leans on Near saturated solution surface, the growth as unique nucleation point induction YBCO superconducting thick-films.Since the growth conditions of LPE is close flat Weigh state, and the thick film obtained using the smaller material of lattice mismatch as seed crystal induced growth has low defect, high crystalline energy The features such as.In addition, since LPE is carried out under non-vacuum condition, thus this method has the advantages that manufacturing cost is low etc..And with General film technique is compared, and LPE has the faster speed of growth.
Therefore, those skilled in the art, which is dedicated to seeking, a kind of effectively expands pure a axis liquid phase epitaxy film growth window Method so that it is simple to operation of low cost, for preparing the pure a axis orientation of high-quality needed for the research and development of Josephson's junction device YBCO high temperature superconducting films.
Invention content
In view of the drawbacks described above of the prior art, the technical problems to be solved by the invention are to provide a kind of use gallic acid neodymium (NdGaO3, NGO)Monocrystal substrate is orientated as seed crystal using top seeded solvent growth rheotaxial growth a axis in air The method of YBCO superconducting thick-films, this method can effectively expand pure a axis liquid phase epitaxy film growth window, so as to be conducive to pure a axis The preparation of YBCO superconducting thick-films is orientated, it is simple to operation of low cost.
To achieve the above object, the present invention provides a kind of method for preparing a axis orientation high temperature superconducting film in air, packets Include following steps:
A) BaCO3 powder and CuO powder are subjected to dispensing, obtain BaCO3+CuO powders, the Ba in the BaCO3+CuO powders Molar ratio with Cu is 0.4-0.7;
B) the BaCO3+CuO powders obtained by step a) are pre-processed;
C) Ba-Cu-O powder is made in the pretreated BaCO3+CuO powders of sintering step b);
D) the Ba-Cu-O powder obtained by step c) is added in the crucible of Y2O3 materials and is heated to the first temperature, and after continuation of insurance Temperature obtains Y-Ba-Cu-O solution;
E) after obtaining the Y-Ba-Cu-O solution obtained by step d), 20-30 grams of step c) is added in into the Y-Ba-Cu-O solution The Ba-Cu-O powder of gained, and continue to keep the temperature in the first temperature;
F) the Y-Ba-Cu-O solution obtained by step e) is cooled to second temperature;
G) it is using the indices of crystallographic plane(110)NGO monocrystal substrates as seed crystal, the NGO monocrystal substrates are inserted perpendicularly into step F) the Y-Ba-Cu-O solution obtained by, using top seeded solvent growth rheotaxial growth YBCO superconducting thick-films.
Further, the pretreatment of step b) includes following process:
(i)Wet-milling is carried out to BaCO3+CuO powders to obtain BaCO3+CuO slurries, the wet-milling time is 2-4 hours;
(ii)Baking operation(i)The BaCO3+CuO slurries of gained.
Technique effect:
For the present invention using NGO monocrystal substrates as seed crystal, the YBCO superconducting thick-films of the pure a axis orientation of rheotaxial growth pass through control System adds in the amount of Ba-Cu-O powder and the time of heat preservation to realize that epitaxial growth a axis is orientated YBCO superconducting thick-films for the second time Property.
Achievement in research before inventor's combination, the method that the prior art uses can be attributed to from saturation state to satiety With state and then epitaxial growth high temperature superconducting film.And method provided by the invention, it substantially may be considered through control second The secondary amount for adding in Ba-Cu-O powder and soaking time adjust solution from undersaturated condition to high and state, then utilize seed Brilliant induced growth superconduction epitaxial film.One aspect of the present invention avoids the back dissolving effect of Nd elements in hot conditions lower substrate as a result,; On the other hand, solution will certainly undergo a saturation state between undersaturation to hypersaturated state, be equivalent to saturation state Temperature is lower than previous method, it is meant that degree of supersaturation is lower than previous method.
In addition, the present invention not only eliminates implacable contradiction between back dissolving effect and small degree of supercooling so that growth The a axilemmas gone out are free of other phases, and the growth window for effectively expanding a axilemmas can be prepared highly reliably to 30K The YBCO films of pure a axis orientation.Meanwhile method provided by the invention allows entire growth in air environment, therefore greatly simplifies Preparation process and reduce manufacturing cost.

Claims (2)

  1. A kind of 1. method for preparing a axis orientation high temperature superconducting film in air, it is characterised in that:Include the following steps:A) will BaCO3 powder and CuO powder carry out dispensing, obtain BaCO3+CuO powders, and the Ba's and Cu in the BaCO3+CuO powders rubs You are than being 0.4-0.7;
    B) the BaCO3+CuO powders obtained by step a) are pre-processed;
    C) Ba-Cu-O powder is made in the pretreated BaCO3+CuO powders of sintering step b);
    D) the Ba-Cu-O powder obtained by step c) is added in the crucible of Y2O3 materials and is heated to the first temperature, and after continuation of insurance Temperature obtains Y-Ba-Cu-O solution;
    E) after obtaining the Y-Ba-Cu-O solution obtained by step d), 20-30 grams of step c) is added in into the Y-Ba-Cu-O solution The Ba-Cu-O powder of gained, and continue to keep the temperature in the first temperature;
    F) the Y-Ba-Cu-O solution obtained by step e) is cooled to second temperature;
    G) it is using the indices of crystallographic plane(110)NGO monocrystal substrates as seed crystal, the NGO monocrystal substrates are inserted perpendicularly into step F) the Y-Ba-Cu-O solution obtained by, using top seeded solvent growth rheotaxial growth YBCO superconducting thick-films.
  2. 2. the method as described in claim 1, it is characterised in that:Pretreatment described in step b) includes following process:(i)It is right The BaCO3+CuO powders carry out wet-milling to obtain BaCO3+CuO slurries, and the wet-milling time is 2-4 hours;
    (ii)Baking operation(i)The BaCO3+CuO slurries of gained.
CN201611119194.2A 2016-12-08 2016-12-08 The preparation method of high-temperature superconductor Pending CN108179465A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611119194.2A CN108179465A (en) 2016-12-08 2016-12-08 The preparation method of high-temperature superconductor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611119194.2A CN108179465A (en) 2016-12-08 2016-12-08 The preparation method of high-temperature superconductor

Publications (1)

Publication Number Publication Date
CN108179465A true CN108179465A (en) 2018-06-19

Family

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CN201611119194.2A Pending CN108179465A (en) 2016-12-08 2016-12-08 The preparation method of high-temperature superconductor

Country Status (1)

Country Link
CN (1) CN108179465A (en)

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