CN105386020B - A kind of preparation method of yttrium barium copper oxide high-temperature superconductor band - Google Patents
A kind of preparation method of yttrium barium copper oxide high-temperature superconductor band Download PDFInfo
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- CN105386020B CN105386020B CN201510706281.7A CN201510706281A CN105386020B CN 105386020 B CN105386020 B CN 105386020B CN 201510706281 A CN201510706281 A CN 201510706281A CN 105386020 B CN105386020 B CN 105386020B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C20/00—Chemical coating by decomposition of either solid compounds or suspensions of the coating forming compounds, without leaving reaction products of surface material in the coating
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- C23C20/08—Coating with inorganic material, other than metallic material with compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
Abstract
A kind of preparation method of yttrium barium copper oxide high-temperature superconductor band.First barium acetate and butyl titanate according to Ba：Ti=1：1 mixed in molar ratio is dissolved in the mixed solution of ethylene glycol monomethyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione, and the precursor liquid of Ba and the metal ion species total concentrations of Ti two for 0.1 0.3mol/L is made after stirring；Then by precursor liquid coated on NiW alloy base bands；Coated film experience heat treatment obtains the barium titanate (BaTiO with biaxial texture3) film；Then in BaTiO3YBa is prepared using chemical solution method on cushion2Cu3O7‑x(YBCO) superconducting layer, it is NiW/BaTiO to prepare structure3/ YBCO high-temperature superconductor band.
Description
Technical field
The present invention relates to a kind of preparation method of high-temperature superconductor band, more particularly to a kind of system of YBCO high-temperature superconductors band
Preparation Method.
Background technology
With YBa2Cu3O7-x(YBCO) superconducting coating is the second-generation high-temperature superconductor of conductor because its is excellent intrinsic
Can (irreversibility field reaches 7T, critical current density up to 10 under 77K6A/cm2), attract people and constantly explore and study its practicality
Become a useful person technology.Second-generation high-temperature superconductor is the important development direction of current superconductor, have broad application prospects and
Huge market potential, it can be widely used for the energy, war industry, medical treatment, traffic and scientific research etc..Therefore, high temperature surpasses
Lead material and technology of preparing is listed in the forward position skill of National Program for Medium-to Long-term Scientific and Technological Development (2006-2020)
Art.
Second-generation high-temperature superconductor is by metal alloy base band, Seed Layer, barrier layer, cap layer, rare earth barium copper oxide superconducting
Layer, protective layer and stabilized zone etc. are formed, and are a kind of sandwich constructions.In the development of YBCO bands, how to obtain with twin shaft
The YBCO superconducting layers of texturizing properties are one of key technologies.Around the source of texturizing properties, transmission and reinforcement, current domestic profile
Into three main technology paths：What 1. U.S.'s Oak Ridge National Laboratory proposed is gone forward side by side by the rolling processing of aximal deformation value
Row high annealing obtains the Ni alloy base bands with biaxial texture characteristic, i.e. rolling auxiliary biaxial texture base band (RABiTS) road
Line；2. Japanese Fujikura companies Iijima etc. is proposed, and is further developed by Los Alamos National Laboratories of the U.S. etc.
In non-textured base band using ion beam bombardment force deposition sull oriented growth obtain biaxial texture oxidation
The scheme of thing film, i.e. ion beam assisted depositing (IBAD) route；3. Bauer etc. is proposed, developed based on German Theva companies
When sull deposits, non-textured base band is in tilted layout at an angle with sedimentary origin is knitted sull
The method of structure orientation, that is, tilt substrate deposition (ISD) route.It is almost various after biaxial texture characteristic is obtained in base band
Membrane deposition method, such as evaporation, sputtering, pulsed laser deposition, chemical solution deposition, chemical vapor deposition, can succeed
Prepare the oxide transition zone and superconducting layer for continuing biaxial texture characteristic.Which kind of however, prepared at present regardless of above-mentioned method
The technique of YBCO bands is extremely complex, and cushion includes Seed Layer, the film of the three kinds of systems in barrier layer and cap layer, and prepares
Cost is high.
The content of the invention
The shortcomings that purpose of the present invention is the YBCO superconducting tape complex process for overcoming prior art to prepare, there is provided one kind tool
There is the preparation method of YBCO superconducting tapes simple in construction.
The present invention uses full chemistry solwution method buffer layer and superconducting layer on metal base band.First on metal base band
One layer of barium titanate film is deposited, then barium titanate film is prepared as cushion on barium titanate film using chemical solution method
YBCO superconducting layers, finally prepare metal base band/BaTiO3The high-temperature superconductor band of/YBCO structures
The specific steps order of the present invention is as follows：
(1) according to Ba：Ti=1：1 mol ratio mixes barium acetate and butyl titanate, is dissolved in glycol first at room temperature
In the mixed solution of ether and glacial acetic acid, the mol ratio of solute and solvent is 1 in the solution：50；
(2) solution for preparing step (1) is through magnetic stirrer 1-3h, then solvent is evaporated off using Rotary Evaporators and obtains
To gel；
(3) gel made from the step (2) is added in glycol methyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione, in this step
The mol ratio of gel and glycol methyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione is 1：50, magnetic agitation under the conditions of being 60~70 DEG C in temperature
Device stirs 0.5-1.5h, and the precursor liquid that two kinds of metal total ion concentrations of Ba and Ti are 0.1-0.3mol/L is made；
(4) precursor liquid made of above-mentioned steps (4) is coated on substrate using spin coating or method of pulling up；
(5) substrate after step (4) coating is placed in high-temperature tubular quartz stove, entered at a temperature of 780 DEG C -850 DEG C
Row 2h heat treatment, obtains barium titanate film；The heating rate of the step is 40 DEG C/h；
(6) chemical solution method depositing thin YBCO films are used on barium titanate film, finally prepare substrate/BaTiO3/
The high-temperature superconductor band of YBCO structures.
Substrate described in the step (4) is the NiW alloy base bands with biaxial texture.
Compared with prior art, the invention has the advantages that：
The present invention prepares cushion and superconducting layer using full chemistry solwution method, with magnetron sputtering, Metallo-Organic Chemical Vapor
Deposition prepares cushion with pulsed laser deposition and needs to use the vacuum system of costliness to compare with superconducting layer, and chemical solution method is not required to
Want vacuum equipment, thus have the advantages that cost than it is relatively low, sedimentation rate is high, composition is easily controlled.This hair of what is more important
It is bright to use individual layer barium titanate film to enormously simplify the structure of YBCO superconducting tapes as cushion, improve preparation efficiency, drop
Low preparation cost.
Brief description of the drawings
Fig. 1 is the field emission scanning electron microscope picture of YBCO bands prepared by embodiment 1；
Fig. 2 is the X-ray diffraction pole figure of YBCO bands prepared by embodiment 2；
Fig. 3 is the X-ray diffraction halfwidth collection of illustrative plates in YBCO bands (005) face prepared by embodiment 3；
Fig. 4 is the critical current density (77K, 0T) of YBCO bands prepared by embodiment 4.
Embodiment
Embodiment 1
(1) 0.005mol barium acetate and 0.005mol butyl titanate are weighed, barium acetate and butyl titanate are mixed
It is dissolved in after conjunction in the mixed solution of 25ml glycol methyl ether and 25ml glacial acetic acid；
(2) solution for preparing step (1) is through magnetic stirrer 1h, then solvent is evaporated off using Rotary Evaporators and obtains
Gel；
(3) gel made from the step (2) is added into 25ml glycol methyl ether, 25ml glacial acetic acid and 50ml acetylacetone,2,4-pentanediones
In, the mol ratio of gel and glycol methyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione in this step is 1：50, under the conditions of temperature is 60 DEG C
Magnetic stirrer 0.5h, the precursor liquid that two kinds of metal total ion concentrations of Ba and Ti are 0.1mol/L is made；
(4) precursor liquid made from step (3) is spin-coated on NiW alloy base bands with 1500 revs/min of speed, spin-coating time
For 90s；
(5) substrate after step (4) coating is placed in high-temperature tubular quartz stove, carries out 2h's at a temperature of 780 DEG C
Heat treatment, obtains barium titanate film；The heating rate of the step is 40 DEG C/h；
Described Low Temperature Heat Treatment is carried out under the Oxygen Condition of moistening, is to pass through 100sccm oxygen equipped with distillation
Vapor is brought into reative cell by the vial of water, and it is 100hPa to make water vapour pressure in reative cell, average with 40 DEG C/h from room temperature
Heating rate be warming up to 780 DEG C, then stove is cooled to room temperature again.
(6) chemical solution method depositing thin YBCO films are used on barium titanate film, finally prepare substrate/BaTiO3/
The high-temperature superconductor band of YBCO structures.Surface topography observation, YBCO thick film tables have been carried out to the sample with field emission scanning electron microscope
Face is smooth, fine and close, without crackle, as shown in Figure 1.
Embodiment 2
(1) 0.01mol barium acetate and 0.01mol butyl titanate difference are weighed, by barium acetate and butyl titanate
It is dissolved in after mixing in the mixed solution of 25ml glycol methyl ether and 25ml glacial acetic acid；
(2) solution for preparing step (1) is through magnetic stirrer 2h, then solvent is evaporated off using Rotary Evaporators and obtains
Gel；
(3) gel made from the step (2) is added into 25ml glycol methyl ether, 25ml glacial acetic acid and 50ml acetylacetone,2,4-pentanediones
In, the mol ratio of gel and glycol methyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione in this step is 1：50, under the conditions of temperature is 65 DEG C
Magnetic stirrer 1h, the precursor liquid that two kinds of metal total ion concentrations of Ba and Ti are 0.2mol/L is made；
(4) precursor liquid made from step (3) is spin-coated on NiW alloy base bands with 3000 revs/min of speed, spin-coating time
For 90s；
(5) substrate after step (4) coating is placed in high-temperature tubular quartz stove, carries out 2h's at a temperature of 825 DEG C
Heat treatment, obtains barium titanate film；The heating rate of the step is 40 DEG C/h；
Described Low Temperature Heat Treatment is carried out under the Oxygen Condition of moistening, is to pass through 200sccm oxygen equipped with distillation
Vapor is brought into reative cell by the vial of water, and it is 200hPa to make water vapour pressure in reative cell, average with 40 DEG C/h from room temperature
Heating rate be warming up to 825 DEG C, then stove is cooled to room temperature again.
(6) chemical solution method depositing thin YBCO films are used on barium titanate film, finally prepare substrate/BaTiO3/
The high-temperature superconductor band of YBCO structures.(102) face is made to sample used in Philips X ' Pert types X-ray diffractometersSweep
Retouch, YBCO films have good epitaxial orientation, as shown in Figure 2.
Embodiment 3
(1) 0.015mol barium acetate and 0.015mol butyl titanate are weighed, barium acetate and butyl titanate are mixed
It is dissolved in after conjunction in the mixed solution of 25ml glycol methyl ether and 25ml glacial acetic acid；
(2) solution for preparing step (1) is through magnetic stirrer 3h, then solvent is evaporated off using Rotary Evaporators and obtains
Gel；
(3) gel made from the step (2) is added into 25ml glycol methyl ether, 25ml glacial acetic acid and 50ml acetylacetone,2,4-pentanediones
In, the mol ratio of gel and glycol methyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione in this step is 1：50, under the conditions of temperature is 70 DEG C
Magnetic stirrer 1.5h, the precursor liquid that two kinds of metal total ion concentrations of Ba and Ti are 0.3mol/L is made；
(4) precursor liquid made from step (3) is spin-coated on NiW alloy base bands with 4000 revs/min of speed, spin-coating time
For 90s；
(5) substrate after step (4) coating is placed in high-temperature tubular quartz stove, carries out 2h's at a temperature of 850 DEG C
Heat treatment, obtains barium titanate film；The heating rate of the step is 40 DEG C/h；
Described Low Temperature Heat Treatment is carried out under the Oxygen Condition of moistening, is to pass through 300sccm oxygen equipped with distillation
Vapor is brought into reative cell by the vial of water, and it is 300hPa to make water vapour pressure in reative cell, average with 40 DEG C/h from room temperature
Heating rate be warming up to 850 DEG C, then stove is cooled to room temperature again.
(6) chemical solution method depositing thin YBCO films are used on barium titanate film, finally prepare substrate/BaTiO3/
The high-temperature superconductor band of YBCO structures.The ω for having made (005) face to sample used in Philips X ' Pert types X-ray diffractometers is swept
Retouch, as shown in Figure 3.The halfwidth at YBCO (005) peak is only 1.443 °, illustrates that YBCO bands have in good face and is orientated, no
High-angle boundary be present.
Embodiment 4
(1) 0.015mol barium acetate and 0.015mo l butyl titanates are weighed, barium acetate and butyl titanate are mixed
It is dissolved in after conjunction in the mixed solution of 25ml glycol methyl ether and 25ml glacial acetic acid；
(2) solution for preparing step (1) is through magnetic stirrer 3h, then solvent is evaporated off using Rotary Evaporators and obtains
Gel；
(3) gel made from the step (2) is added into 25ml glycol methyl ether, 25ml glacial acetic acid and 50ml acetylacetone,2,4-pentanediones
In, the mol ratio of gel and glycol methyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione in this step is 1：50, under the conditions of temperature is 70 DEG C
Magnetic stirrer 1.5h, the precursor liquid that two kinds of metal total ion concentrations of Ba and Ti are 0.3mol/L is made；
(4) precursor liquid made from step (3) is coated on NiW alloy base bands with the pull rate of 20 centimeters/minutes；
(5) substrate after step (4) coating is placed in high-temperature tubular quartz stove, carries out 2h's at a temperature of 850 DEG C
Heat treatment, obtains barium titanate film；The heating rate of the step is 40 DEG C/h；
Described Low Temperature Heat Treatment is carried out under the Oxygen Condition of moistening, is to pass through 300sccm oxygen equipped with distillation
Vapor is brought into reative cell by the vial of water, and it is 300hPa to make water vapour pressure in reative cell, average with 40 DEG C/h from room temperature
Heating rate be warming up to 850 DEG C, then stove is cooled to room temperature again.
(6) chemical solution method depositing thin YBCO films are used on barium titanate film, finally prepare substrate/BaTiO3/
The high-temperature superconductor band of YBCO structures.The survey of critical current density has been carried out to prepared YBCO bands with Lepi-system
Examination, critical current density jc are up to 5MA/cm2, as shown in Figure 4.
Claims (2)
- A kind of 1. preparation method of yttrium barium copper oxide high-temperature superconductor band, it is characterised in that described preparation YBCO superconducting tape sides Method comprises the following steps：(1) according to Ba：Ti=1：1 mol ratio mixes barium acetate and butyl titanate, be dissolved at room temperature glycol methyl ether and In the mixed solution of glacial acetic acid, the mol ratio of solute and solvent is 1 in the solution：50；(2) the trifluoroacetic acid salting liquid that step (1) is prepared is evaporated off through magnetic stirrer 1-3h, then using Rotary Evaporators Solvent obtains gel；(3) gel made from the step (2) is added in glycol methyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione, the gel in this step Mol ratio with glycol methyl ether, glacial acetic acid and acetylacetone,2,4-pentanedione is 1：50, magnetic stirring apparatus stirs under the conditions of being 60~75 DEG C in temperature 0.5-1.5h is mixed, the precursor liquid that two kinds of metal total ion concentrations of Ba and Ti are 0.1-0.3mol/L is made；(4) precursor liquid made of above-mentioned steps (4) is coated on substrate using spin coating or method of pulling up；(5) substrate after step (4) coating is placed in high-temperature tubular quartz stove, 2h is carried out at a temperature of 780 DEG C -850 DEG C Heat treatment, obtain barium titanate film；The heating rate of the step is 40 DEG C/h；(6) chemical solution method depositing thin YBCO films are used on barium titanate film, finally prepare substrate/BaTiO3/ YBCO structures High-temperature superconductor band.
- 2. the preparation method of YBCO high-temperature superconductors band as claimed in claim 1, it is characterised in that institute in the step (4) It is the NiW alloy base bands with biaxial texture to state substrate.
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| CN104446434A (en) * | 2014-11-17 | 2015-03-25 | 中国科学院电工研究所 | Method for preparing yttrium barium copper oxide high-temperature superconducting film |
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| CN104446434A (en) * | 2014-11-17 | 2015-03-25 | 中国科学院电工研究所 | Method for preparing yttrium barium copper oxide high-temperature superconducting film |
Non-Patent Citations (3)
| Title |
|---|
| Precursor evolution and growth mechanism of BTO/YBCO films by TFA-MoD process;wang hongyan etal.;《Chin.Phys.B》;20141231;第23卷(第10期);第107402-1~107402-5页 * |
| Strongly enhanced pinning force density in YBCO-BaTiO3 nanocomposite superconducror;Alok K.Jha etal.;《Physica C：Superconductivity》;20090518;第469卷(第14期);第810-813页 * |
| 溶胶-凝胶法制备BaTiO3薄膜;梁鸿东等;《山西师范大学学报（自然科学版）》;20060630;第20卷(第2期);第29-31页 * |
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