CN101901646B - High temperature Y1-xYbxBCO superconducting thin film and preparation method thereof - Google Patents

High temperature Y1-xYbxBCO superconducting thin film and preparation method thereof Download PDF

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CN101901646B
CN101901646B CN2010102285498A CN201010228549A CN101901646B CN 101901646 B CN101901646 B CN 101901646B CN 2010102285498 A CN2010102285498 A CN 2010102285498A CN 201010228549 A CN201010228549 A CN 201010228549A CN 101901646 B CN101901646 B CN 101901646B
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bco
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trifluoroacetic acid
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叶帅
索红莉
吴紫平
刘敏
袁慧萍
吕昭
徐燕
马麟
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Beijing University of Technology
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Abstract

The invention discloses a high temperature Y1-xYbxBCO superconducting thin film and a preparation method thereof, belonging to the technical field of high temperature superconducting material preparation, wherein X is more than 0 and not more than 1. The thickness of the high temperature Y1-xYbxBCO superconducting thin film is about 200nm. The preparation method comprises the following steps: firstly preparing precursor solution of Y1-xYbxBCO; coating the precursor solution on the single crystal substrate; then presintering the obtained product in the wet oxygen at the temperature below 400 DEG C to obtain the precursor amorphous film; and then sintering the precursor amorphous film at 800-850 DEG C for 1-4h, introducing wet Ar/O2 gas mixture in the first 3/4 time slot and introducing dry Ar/O2 gas mixture in the last 1/4 time slot. The method is simple in equipment, low in cost and fast in sedimentation and dispenses with vacuum, most importantly, the film components are easy to control and the dopants and the proportion thereof can be randomly changed, thus the method is more suitable for developing practical high temperature superconducting long strips.

Description

A kind of Y 1-xYb xBCO high-temperature superconducting thin film and preparation method thereof
Technical field
The invention belongs to the high temperature superconducting materia preparing technical field, be specifically related to the technology of preparing of rare-earth barium copper oxides second generation coating superconducting high-temperature superconducting thin film.
Background technology
With YBCO is main rare-earth barium copper oxides second generation coating superconductor, owing to have high irreversible, high current capacity, low A.C. losses, potential price advantage has just received widely since coming to light the end of the eighties in last century always and paying close attention to.Along with progress of research, YBCO coating conductor technology is more and more ripe, and is also more and more nearer apart from the realization of practicability.Up to the present, people adopt pulsed laser deposition technique (PLD) to prepare at 77K lower critical current value (I c) up to the ybco film of 1400A/cm, and adopt the ybco film I of metal organic deposit (MOD) technology preparation cPeak has also reached 795A/cm; Aspect long band, U.S. SuperPower company adopts metal organic salt chemical vapour deposition (CVD) (MOCVD) technology to prepare more than 1000 meter band, and the whole I of band cValue is 220A/cm, can reach practical standard fully.
But, because the decline rapidly along with the increase of externally-applied magnetic field of the Ic value of ybco film under externally-applied magnetic field, must be through artificially introduce some nano level defectives suppress the Ic value of ybco film as pinning center reduction at ybco film.Adopt other rare earth elements partly to replace the Y of the Y element preparation among the YBCO 1-xRE xThe BCO film is because Y 3+Different with the radius of rare earth element ion and cause the inner lattice of film to distort.These defectives can be used as effective pinning center and improve the Ic value of ybco film under magnetic field.In addition, with respect to PLD method and mocvd method, adopt the MOD method to prepare this Y 1-xRE xThe BCO film is not only with low cost, and can control the stoichiometric proportion of Y element and rare earth element neatly, has more wide application prospect.
Summary of the invention
The object of the present invention is to provide a kind of employing chemical solution method to prepare Y 1-xYb xBCO film and preparation method thereof.This method equipment is simple, with low cost, and the Y of preparation 1-xYb xThe surface compact of BCO film is smooth, and the superconductivity under externally-applied magnetic field has obtained good raising.
A kind of Y provided by the present invention 1-xYb xThe BCO film, 0＜X≤1 wherein, thickness is greatly about about 200～250nm.Because Y 3+And Yb 3+This Y of ion 1-xYb xCan exchange according to arbitrary proportion in the BCO film, can be according to different demands to Y 3+And Yb 3+The ratio of ion is regulated.
The present invention adopts MOD chemical method with low cost to prepare Y 1-xYb xThe BCO film at first obtains Y 1-xYb xThe precursor aqueous solution of BCO, again through filming, low temperature and high temperature sintering obtain Y 1-xYb xThe BCO film, concrete steps are following:
1) Y 1-xYb xThe preparation of BCO precursor aqueous solution: with trifluoroacetic acid yttrium, trifluoroacetic acid ytterbium, trifluoroacetic acid barium and trifluoroacetic acid copper or acrylic acid copper by amount of substance than 1-x: x: fully be dissolved in absolute methanol at 2: 3,0＜X≤1 obtains the Y of 1.0-2.0mol/L 1-xYb xThe BCO precursor aqueous solution;
2) coating of film: with Y 1-xYb xThe mode of BCO precursor aqueous solution through spin coating or dip-coating is coated to and obtains precursor film on the single crystal substrates;
3) low temperature presintering: the pre-burning in being lower than 400 ℃ wet oxygen of coated precursor film is obtained forerunner's amorphous film;
4) high temperature sintering: in 800-850 ℃ of following sintering 1-4 hour, in the sintering process, in preceding 3/4 time period, feeding oxygen content was the wet Ar/O of 100-1000ppm with forerunner's amorphous film 2Gaseous mixture, in 1/4 time period of back, feeding oxygen content is the dried Ar/O of 100-1000ppm 2It is the dried Ar/O of 100-1000ppm continuing to feed oxygen content that gaseous mixture, sintering finish the back 2Gaseous mixture is cooling down, when temperature drops to 500 ℃, changes purity oxygen into, and is incubated 2-4 hour, obtains Y with the stove cooling 1-xYb xThe BCO film.
Wherein, the trifluoroacetate that uses in the step 1) obtains through corresponding acetate and trifluoroacetic acid reaction, and acrylic acid copper obtains through Schweinfurt green and acrylic acid reaction;
Step 2) adopt the spin coating mode in Y 1-xYb xThe BCO precursor aqueous solution is coated in lanthanum aluminate (LAO) or strontium titanates (STO) substrate, and the revolution of filming is 3000-6000 rev/min, and the time of filming is 1-2 minute; When adopting the mode of dip-coating, the pull rate of filming is the 5-80 mm/min;
Wet oxygen described in the step 3) is to realize that through the container that distilled water is housed that oxygen is fed water-bath heating bath temperature is 20-50 ℃, oxygen flow be the 0.2-1.0 liter/minute, the temperature range that feeds wet oxygen is between 150～400 ℃;
The sintering process that uses in the step 3) is different and difference to some extent according to the mantoquita that uses: when using trifluoroacetic acid copper; Sintering process is following: the programming rate of room temperature to 200 ℃ is 135 ℃/hour; Programming rate between 200 ℃-250 ℃ is 5-7 ℃/hour; Programming rate between 250 ℃-300 ℃ is 30 ℃/hour, and the programming rate between 300 ℃-400 ℃ is 300 ℃/hour; When using propylene to ache, its sintering process is following: the programming rate of room temperature to 150 ℃ is 400～600 ℃/hour, and 150～400 ℃ programming rate is 100～300 ℃/hour;
Wet Ar/O described in the step 4) 2Gaseous mixture is through with Ar/O 2Gaseous mixture feeds that the container that distilled water is housed of water-bath heating realizes, bath temperature is 30-50 ℃, mixed gas flow be the 0.2-1.5 liter/minute.
Compared with prior art, the present invention has following beneficial effect:
1) compare present widely used PLD method doping techniques, the employed equipment of the inventive method is simple, and cost is low; Needing no vacuum, deposition velocity is fast, the most important thing is that thin film composition controls easily; And can arbitrarily change alloy and proportioning thereof, be more suitable for developing the long band of high-temperature superconductor of practicability.
2) with respect to pure ybco film, Y 1-xYb xThe surface of BCO film is well improved, and more smooth densification becomes; In addition, Y 1-xYb xThe BCO film is inner because Y 3+And Yb 3+The ionic radius difference can cause lattice to distort, and the distortion of this lattice can be used as pinning center, reduces the magnetic field wriggling under the magnetic field, improves the critical current density of ybco film under magnetic field.Under uniform temp, magnetic field is high more, the J of doped samples cBe higher than pure ybco film more.Y 1-xYb xThe BCO film has higher superconductivity under the high temperature High-Field, comparing pure ybco film more has application prospect.
Description of drawings
Fig. 1: the SEM of gained film surface figure in the Comparative Examples 1.
The XRD figure of gained film among Fig. 2: the embodiment 1.
(103) face Φ scanning result of gained film among Fig. 3: the embodiment 1.
The critical transition temperature T of gained film among Fig. 4: the embodiment 2 cThe result.
The J of gained film among Fig. 5: the embodiment 2 cValue is with the variation relation in outfield.
The XRD figure of gained film among Fig. 6: the embodiment 3.
The SEM of gained film figure among Fig. 7: the embodiment 3.
The SEM of the section of gained film figure among Fig. 8: the embodiment 4
Below in conjunction with accompanying drawing and embodiment the present invention is explained further details.
Embodiment
Comparative Examples 1
1), in 0.02mol trifluoroacetic acid barium and the 0.03mol trifluoroacetic acid copper dissolution absolute methanol, obtains the YBCO precursor aqueous solution of 1.5mol/L with 0.01mol trifluoroacetic acid yttrium;
2) adopt spin coating method that the YBCO precursor aqueous solution is coated in the LAO substrate and obtain wet film, the revolution of filming is 4000 rev/mins, and the time of filming is 1 minute;
3) wet film low temperature presintering in the wet oxygen below 400 ℃ is obtained forerunner's amorphous film; Wherein, The programming rate of room temperature to 200 ℃ is 135 ℃/hour; Programming rate between 200 ℃-250 ℃ is 5 ℃/hour, and the programming rate between 250 ℃-300 ℃ is 30 ℃/hour, and the programming rate between 300 ℃-400 ℃ is 300 ℃/hour; Wet oxygen is that the container that distilled water is housed of the water-bath heating of 30 ℃ of oxygen feedings is realized that feed since 150 ℃ (inconsistent with summary of the invention), oxygen flow is 0.2 liter/minute;
4) forerunner's amorphous film is incubated 2 hours down at 820 ℃, wherein, the wet Ar/O of feeding in preceding 1.5 hours 2(oxygen content is 200ppm to gaseous mixture, with Ar/O 2The container that distilled water is housed of the water-bath heating that the gaseous mixture feeding is 50 ℃ realizes that mixed gas flow is 0.5 liter/minute), Ar/O is done in feeding in back 0.5 hour 2Gaseous mixture after sintering finishes, is continuing to feed dried Ar/O 2Lower the temperature under the condition of gaseous mixture, when temperature drops to 500 ℃, change purity oxygen into, and be incubated 2 hours, with the stove cooling, obtain ybco film then.
The SEM of this film surface is as shown in Figure 1, can find to exist small hole and spherical particle.
Embodiment 1
1), in 0.0025mol trifluoroacetic acid ytterbium, 0.02mol trifluoroacetic acid barium and the 0.03mol acrylic acid copper dissolution absolute methanol, obtains the Y of 1.5mol/L with 0.0075mol trifluoroacetic acid yttrium 0.75Yb 0.25The BCO precursor aqueous solution;
2) adopt spin coating method with Y 0.75Yb 0.25The BCO precursor aqueous solution is coated in the LAO substrate and obtains wet film, and the revolution of filming is 4000 rev/mins, films 2 minutes time;
3) wet film low temperature presintering in the wet oxygen below 400 ℃ is obtained forerunner's amorphous film, wherein, the programming rate of room temperature to 150 ℃ is 500 ℃/hour, and the programming rate between 150 ℃-400 ℃ is 200 ℃/hour; Identical in the wet oxygen condition that feeds and the Comparative Examples 1;
4) forerunner's amorphous film is incubated 2.0 hours down at 830 ℃, wherein, the wet Ar/O of feeding in preceding 1.5 hours 2(oxygen content is 500ppm to gaseous mixture, with Ar/O 2The container that distilled water is housed of the water-bath heating that the gaseous mixture feeding is 50 ℃ realizes that mixed gas flow is 0.35 liter/minute), Ar/O is done in feeding in back 0.5 hour 2Gaseous mixture after sintering finishes, is continuing to feed dried Ar/O 2Lower the temperature under the condition of gaseous mixture, when temperature drops to 500 ℃, change purity oxygen into, and be incubated 4 hours, with the stove cooling, obtain Y then 0.75Yb 0.25The BCO film.
The XRD of this film is as shown in Figure 2, has only occurred the diffraction maximum of (00l) face among the figure, explains that film has good orientation and generates, and in addition, a peak on the diffraction maximum of each (00l) face, only occurred, explains that the film of preparation is pure Y 0.75Yb 0.25BCO, rather than the amalgam of YBCO and YbBCO.Can find out that from the Phi scanning of this film (103) face this film has texture in the good face, as shown in Figure 3.
Embodiment 2
1), in 0.005mol trifluoroacetic acid ytterbium, 0.02mol trifluoroacetic acid barium and the 0.03mol trifluoroacetic acid copper dissolution absolute methanol, obtains the Y of 1.0mol/L with 0.005mol trifluoroacetic acid yttrium 0.5Yb 0.5The BCO precursor aqueous solution;
2) adopt spin coating method with Y 0.5Yb 0.5The BCO precursor aqueous solution is coated in the STO substrate and obtains wet film, and the revolution of filming is 4500 rev/mins, and the time of filming is 2 minutes;
3) sintering process is identical with the step 3) of Comparative Examples 1;
4) sintering process is identical with the step 4) of Comparative Examples 1;
The critical transition temperature T of this film cAs shown in Figure 4, its initial critical transition temperature is 86.5K; Its Jc value is as shown in Figure 5 with the variation relation of externally-applied magnetic field.
Embodiment 3
1) with 0.0025mol trifluoroacetic acid yttrium, 0.0075mol trifluoroacetic acid ytterbium, 0.02mol barium acetate and 0.03mol acrylic acid copper dissolution obtain the Y of 1.3mol/L in absolute methanol 0.25Yb 0.75The BCO precursor aqueous solution;
2) adopt dip-coating method with Y 0.25Yb 0.75The BCO precursor aqueous solution is coated in the LAO substrate and obtains wet film, and pull rate is 20 mm/min;
3) wet film low temperature presintering in oxygen wet below 400 ℃ is obtained forerunner's amorphous film, wherein, the programming rate of room temperature to 150 ℃ is 600 ℃/hour, and the programming rate between 150 ℃-400 ℃ is 300 ℃/hour; Wet oxygen is that the container that distilled water is housed of the water-bath heating of 50 ℃ of oxygen feedings is realized that since 150 ℃ of feedings, oxygen flow is 0.3 liter/minute;
4) forerunner's amorphous film is incubated 2 hours down at 780 ℃, wherein, the wet Ar/O of feeding in preceding 1.5 hours 2(oxygen content is 200ppm to gaseous mixture, with Ar/O 2The container that distilled water is housed of the water-bath heating that the gaseous mixture feeding is 50 ℃ realizes that mixed gas flow is 0.5 liter/minute), Ar/O is done in feeding in back 0.5 hour 2Gaseous mixture after sintering finishes, is continuing to feed dried Ar/O 2Lower the temperature under the condition of gaseous mixture, when temperature drops to 500 ℃, change purity oxygen into, and be incubated 2 hours, with the stove cooling, obtain Y then 0.25Yb 0.75The BCO film.
The XRD of this film is as shown in Figure 6, has only occurred the diffraction maximum of (00l) face among the figure, explain that film has good orientation and generates, and the film of preparation is pure Y 0.25Yb 0.75BCO.Shown in Figure 7 is the SEM figure on the surface of this film, can find out that this film has very even curface.
Embodiment 4
1) with 0.005mol trifluoroacetic acid ytterbium, 0.01mol trifluoroacetic acid barium and 0.015mol trifluoroacetic acid copper dissolution obtain the YbBCO precursor aqueous solution of 1.0mol/L in absolute methanol;
2) adopt dip-coating method that the YbBCO precursor aqueous solution is coated in the LAO substrate and obtain wet film, pull rate is 50 mm/min;
3) wet film low temperature presintering in wet oxygen below 400 ℃ is obtained forerunner's amorphous film; Wherein, The programming rate of room temperature to 200 ℃ is 135 ℃/hour; Programming rate between 200 ℃-250 ℃ is 4 ℃/hour, and the programming rate between 250 ℃-300 ℃ is 30 ℃/hour, and the programming rate between 300 ℃-400 ℃ is 300 ℃/hour;
4) forerunner's amorphous film is incubated 2.5 hours down at 820 ℃, wherein, the wet Ar/O of feeding in preceding 2 hours 2(oxygen content is 500ppm to gaseous mixture, with Ar/O 2The container that distilled water is housed of the water-bath heating that the gaseous mixture feeding is 50 ℃ realizes that mixed gas flow is 0.8 liter/minute), Ar/O is done in feeding in back 0.5 hour 2Gaseous mixture after sintering finishes, is continuing to feed dried Ar/O 2Lower the temperature under the condition of gaseous mixture, when temperature drops to 500 ℃, change purity oxygen into, and be incubated 2 hours, with the stove cooling, obtain the YbBCO film then.
That shown in Figure 8 is the SEM figure of the section of this film.Can find out that the thickness of this film is about 200nm.

Claims (7)

1. a kind of Y of claim 1 1-xYb xThe preparation method of BCO film is characterized in that, may further comprise the steps:
(1) Y 1-xYb xThe preparation of BCO precursor aqueous solution: with trifluoroacetic acid yttrium, trifluoroacetic acid ytterbium, trifluoroacetic acid barium and acrylic acid copper by amount of substance than 1-x: x: fully be dissolved in absolute methanol at 2: 3,0＜X≤1 obtains the Y of 1.0-2.0mol/L 1-xYb xThe BCO precursor aqueous solution;
(2) coating of film: with Y 1-xYb xThe mode of BCO precursor aqueous solution through spin coating or dip-coating is coated to and obtains precursor film on the single crystal substrates;
(3) low temperature presintering: the pre-burning in being lower than 400 ℃ wet oxygen of coated precursor film is obtained forerunner's amorphous film;
(4) high temperature sintering: in 800-850 ℃ of following sintering 1-4 hour, in the sintering process, in preceding 3/4 time period, feeding oxygen content was the wet Ar/O of 100-1000ppm with forerunner's amorphous film 2Gaseous mixture, in 1/4 time period of back, feeding oxygen content is the dried Ar/O of 100-1000ppm 2It is the dried Ar/O of 100-1000ppm continuing to feed oxygen content that gaseous mixture, sintering finish the back 2Gaseous mixture is cooling down, when temperature drops to 500 ℃, changes purity oxygen into, and is incubated 2-4 hour, obtains Y with the stove cooling 1-xYb xThe BCO film.
2. a kind of Y of claim 1 1-xYb xThe preparation method of BCO film is characterized in that, the trifluoroacetic acid yttrium that uses in the step (1), trifluoroacetic acid ytterbium, trifluoroacetic acid barium obtain through corresponding acetate and trifluoroacetic acid reaction, and acrylic acid copper obtains through Schweinfurt green and acrylic acid reaction.
3. a kind of Y of claim 1 1-xYb xThe preparation method of BCO film is characterized in that, adopts the spin coating mode with Y in the step (2) 1-xYb xThe BCO precursor aqueous solution is coated in lanthanum aluminate (LAO) or strontium titanates (STO) substrate, and the revolution of filming is 3000-6000 rev/min, and the time of filming is 1-2 minute; When adopting the mode of dip-coating, the pull rate of filming is the 5-80 mm/min.
4. a kind of Y of claim 1 1-xYb xThe preparation method of BCO film; It is characterized in that; Wet oxygen described in the step (3) is to realize through the container that distilled water is housed that oxygen is fed the water-bath heating; Bath temperature is 20-50 ℃, oxygen flow be the 0.2-1.0 liter/minute, the temperature range that feeds wet oxygen is between 150～400 ℃.
5. a kind of Y of claim 1 1-xYb xThe preparation method of BCO film is characterized in that, when using acrylic acid copper, its sintering process is following: the programming rate of room temperature to 150 ℃ is 400～600 ℃/hour, and 150～400 ℃ programming rate is 100～300 ℃/hour.
6. a kind of Y of claim 1 1-xYb xThe preparation method of BCO film is characterized in that, the wet Ar/O described in the step (4) 2Gaseous mixture is through with Ar/O 2Gaseous mixture feeds that the container that distilled water is housed of water-bath heating realizes, bath temperature is 30-50 ℃, mixed gas flow be the 0.2-1.5 liter/minute.
7. according to the prepared a kind of Y of the method for claim 1 1-xYb xThe BCO film, 0＜X≤1.
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CN103274681A (en) * 2013-03-28 2013-09-04 北京工业大学 Nb-doped YxYb1-xBCO superconductive film and preparation method thereof
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CN101694788A (en) * 2009-10-16 2010-04-14 北京工业大学 Gd-doped YBCO superconducting film and preparation process thereof
CN101719399A (en) * 2009-11-06 2010-06-02 北京工业大学 Preparation process for improving production efficiency and film thickness of YBCO superconducting film

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