CN103524131B - Preparation method of rare-earth element doped YxSm(l-x)BCO superconducting thin film - Google Patents
Preparation method of rare-earth element doped YxSm(l-x)BCO superconducting thin film Download PDFInfo
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Abstract
The invention discloses a preparation method of a YBCO coating superconducting thin film. According to the preparation method, a YxSm(l-x)BCO superconducting thin film is prepared on a lanthanum perchlorate LAO substrate modified by a palladium nanometer dot, wherein x is greater than or equal to 0 and is less than or equal to 1. The preparation method comprises the following steps: (1) preparing the Pd palladium nanometer dot; (2) preparing a YBCO precursor solution; (3) preparing a SmBCO precursor solution; (4) preparing a YxSm(l-x)BCO precursor solution, wherein x is greater than or equal to 0 and is less than or equal to 1; and (5) sintering YxSm(l-x)BCO, wherein x is greater than or equal to 0 and is less than or equal to 1. The preparation method disclosed by the invention is simple and practicable and has the advantages that the distribution density of the palladium nanometer dot can be controlled at arbitrary, the raw materials are low in cost and easily available, vacuum equipment is not needed during preparation, and the cost is low; and the prepared thin film has relatively high critical transition temperature and good biaxial texture and field performance.
Description
Technical field:
The present invention relates to the doping modification method of YBCO high-temperature superconducting thin film material, belong to YBCO coating superconducting film preparing technology field.
Technical background:
YBCO superconductor, due to a series of advantages of itself, is considered to most possibly by one of superconductor of large-scale application.But YBCO high temperature superconducting materia has a shortcoming,, along with the increase of externally-applied magnetic field, its critical current density transporting significantly declines.Yet the application of YBCO superconductor, normally under certain externally-applied magnetic field, so will reach practical requirement, not only requires it under zero magnetic field, to have the higher current capacity that transports, and also should have the larger current capacity that transports under High-Field.Research discovery, in ybco film, appropriate some defects of introducing can be used as pinning center, effectively reduce flux creep, improve the field performance of YBCO.Introduce pinning center and comprise the several methods such as substrate surface is modified, nano-particle doped and rare earth element replacement.The present invention innovates substrate surface is modified and rare earth doped combining, a kind of method that provides substrate surface to modify, and on the substrate after modified, prepare rare earth doped Y
xsm
1-xbCO (0≤x≤1) superconducting thin film.
Summary of the invention:
The object of this invention is to provide and a kind ofly on chloric acid langasite single crystal substrate (LAO) surface, prepare palladium (Pd) nano dot, and prepare Y on the substrate after palladium (Pd) nano dot is modified
xsm
1-xthe method of BCO (0≤x≤1) high-temperature superconducting thin film.Mainly comprise the following steps:
Step S100: prepare palladium Pd nano dot, comprise the following steps:
Step S101: palladium acetylacetonate is dissolved in n Propanoic acid, obtains the precursor aqueous solution that palladium ion solubility is 0.001～0.003mol/L;
Step 102: adopt the mode of spin coating to be coated on described chloric acid lanthanum substrate LAO monocrystalline the described precursor aqueous solution in step S101, form precursor film, coating time is 50～70 seconds, and rotating speed is 3000～4000 revs/min;
Step S103: by the sintering 20～120 minutes at the protective atmosphere of inert gas and 1000～1300 ℃ of temperature of the described precursor film in step S102, generate palladium Pd nano dot at substrate surface;
Step S200: prepare Y by low fluorine technique
xsm
1-xbCO (0≤x≤1) precursor aqueous solution, comprises the following steps:
Step S201: by acetic acid yttrium and barium acetate in molar ratio the ratio of 1:2 be dissolved in deionized water, at 30～40 ℃ of temperature fully after stirring and dissolving, the ratio that is 1:3 according to the mol ratio of acetic acid yttrium and trifluoroacetic acid adds trifluoroacetic acid, at 30～40 ℃ of temperature, react after 2～5 hours, rotary evaporation at 40～50 ℃ of temperature, obtain white powder, with absolute methanol, dissolve the precursor aqueous solution that this white powder obtains yttrium Y, barium Ba;
Step S202: by Schweinfurt green and α-methacrylic acid in molar ratio the ratio of 1:4 be dissolved in absolute methanol, at 60～70 ℃ of temperature, reflux 2～10 hours, rotary evaporation at 40～50 ℃ of temperature, obtain blue gel, with absolute methanol, dissolve this blue gel, obtain the precursor aqueous solution of copper Cu;
Step S203: the precursor aqueous solution of yttrium Y, barium Ba, copper Cu filters respectively rear mixing, obtain blue clear solution, make this blueness clear solution rotary evaporation at 40～50 ℃ obtain blue gel, with absolute methanol, dilute this blue gel again, make and comprise that the total cation concentration of ruthenium ion, barium ions and copper ion is 1.5mol/L, obtain YBCO precursor aqueous solution;
Step S204: change the described acetic acid yttrium in S201 into acetic acid samarium, become SmBCO precursor aqueous solution according to the Process configuration identical with S203 with S201, S202;
Step S205: YBCO, SmBCO precursor aqueous solution are mixed according to the volume ratio of 3:1 or 1:1, obtain Y
xsm
1-xbCO (0≤x≤1) precursor aqueous solution;
Step S300: apply Y on the substrate after palladium Pd nano dot is modified
xsm
1-xbCO (0≤x≤1), comprises the following steps:
By the Y configuring in step S200
xsm
1-xthe method of BCO (0≤x≤1) precursor aqueous solution by spin coating is coated in step S100 on the substrate after palladium Pd nano dot is modified, and obtains Y
xsm
1-xbCO (0≤x≤1) precursor film;
Step S400: low-temperature sintering, comprises the following steps:
At room temperature, precursor film is warming up to 100 ℃ with the programming rate of 600 ℃/h, then is warming up to 400 ℃ with the programming rate of 200 ℃/h, obtain amorphous precursor film, wherein, from room temperature, rise to 150 ℃ of temperature-rise periods, pass into dry oxygen, gas flow is 0.1～0.3 liter/min; In 150 ℃ to 400 ℃ temperature-rise periods, pass into wet oxygen; Wet oxygen is to take the throughput of 0.1～0.3 liter/min to pass into temperature and obtain in the distilled water of 25 ℃～35 ℃;
Step S500: high temperature sintering, comprises the following steps:
Amorphous precursor film in abovementioned steps S400, in 800～850 ℃ of sintering 2-4 hour, wherein, is passed into the wet Ar/O of oxygen content 200～500ppm in front 2/3 time
2gaseous mixture, in rear 1/3 time, passing into oxygen content is the dry Ar/O of 200～500ppm
2gaseous mixture, and passing into the dry Ar/O that oxygen content is 200～500ppm
2under the condition of gaseous mixture, with stove, be cooled to after 450 ℃～500 ℃, in the atmosphere of pure dry oxygen, be incubated 2-4 hour, obtain the Y preparing on the LAO substrate after Pd nano dot is modified
xsm
1-xbCO (0≤x≤1) superconducting thin film; Wet Ar/O
2gaseous mixture is by dry Ar/O
2gaseous mixture passes into the throughput of 0.5～1.0 liter/min and obtains in the distilled water of 40～60 ℃.
The present invention has following income effect:
1. by chemical method with low cost, on LAO substrate, prepare palladium (Pd) nano dot, and adopt Samarium Nitrate (Sm) part to replace the yttrium (Y) in YBCO, substrate surface is modified and rare earth element replacement combines and can, in the inner defect of introducing of superconducting thin film as pinning center, improve Y
xsm
1-xthe field performance of BCO (0≤x≤1) film;
2. the Y preparing on the LAO substrate after palladium (Pd) nano dot is modified
xsm
1-xbCO (0≤x≤1) superconducting thin film, has good c-axis orientation, does not occur Y
xsm
1-xthe diffraction maximum of other crystal faces of BCO (0≤x≤1) and superconducting phase (as shown in Figure 1); Film surface is smooth, fine and close, there is no (as shown in Figure 2) of obvious hole, crackle and a axialite;
3. the Y preparing on the LAO substrate after palladium (Pd) nano dot is modified
xsm
1-xbCO (0≤x≤1) superconducting thin film has higher superconduction critical transition temperature T
c(as shown in Figure 3).
Accompanying drawing explanation:
The XRD figure of Fig. 1 YBCO superconducting thin film that to be embodiment 1 gained prepare on the LAO substrate after palladium (Pd) nano dot is modified;
Fig. 2 is the Y preparing on the LAO substrate after palladium (Pd) nano dot is modified that embodiment 2 obtains
0.75sm
0.25the SEM figure of BCO superconducting thin film;
Fig. 3 is the Y preparing on the LAO substrate after palladium (Pd) nano dot is modified that embodiment 2 obtains
0.5sm
0.5the critical transition temperature T of BCO superconducting thin film
c.
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment
Embodiment 1
Step S100: prepare palladium (Pd) nano dot:
Step S101: a certain amount of palladium acetylacetonate is dissolved in n Propanoic acid, obtains palladium ion (Pd
+) the concentration precursor aqueous solution that is 0.001mol/L;
Step S102: adopt the mode Tu of spin coating on LAO monocrystalline the precursor aqueous solution in step S101, the coating time is 50 seconds, and rotating speed is 3000 revs/min;
Step S103: under argon shield, sintering is 20 minutes in 1000 ℃ by the precursor film of step S102, generates palladium (Pd) nano dot at substrate surface, obtains the LAO substrate that palladium (Pd) nano dot is modified;
Step S200: prepare YBCO precursor aqueous solution by low fluorine technique:
Step S201: by acetic acid yttrium, barium acetate in molar ratio the ratio of 1:2 be dissolved in deionized water, at 30 ℃ fully after stirring and dissolving, according to the mol ratio of acetic acid yttrium and trifluoroacetic acid, be that 1:3 adds trifluoroacetic acid, at 30 ℃, react after 2 hours, rotary evaporation at 40 ℃, obtain white powder, with absolute methanol, dissolve, obtain the precursor liquid of Y, Ba;
Step S202: by Schweinfurt green and α-methacrylic acid in molar ratio the ratio of 1:4 be dissolved in absolute methanol, rotary evaporation at 40 ℃, obtains blue gel, with absolute methanol, dissolves, and obtains the precursor liquid of Cu;
Step S203: the precursor liquid of yttrium (Y), barium (Ba), copper (Cu) is filtered respectively to rear mixing, obtain blue clear solution, rotary evaporation at 40 ℃, obtain blue gel, with absolute methanol, dilute again, controlling total cation concentration (comprising ruthenium ion, barium ions and copper ion) is 1.5mol/L, obtains YBCO precursor liquid;
Step S300: apply YBCO on the substrate after palladium (Pd) nano dot is modified:
Method by the YBCO precursor liquid configuring in step S200 by spin coating is coated in step S100 on the substrate after palladium (Pd) nano dot is modified, and obtains YBCO precursor film.
Step S400: low-temperature sintering: under room temperature, the YBCO precursor film that step S300 is obtained is warming up to 100 ℃ with the programming rate of 600 ℃/h from room temperature, then is warming up to 400 ℃ with the programming rate of 200 ℃/h, obtains amorphous precursor film.Wherein, from room temperature, rise to 150 ℃ of temperature-rise periods, with the gas flow of 0.1 liter/min, pass into dry oxygen; In 150 ℃ to 400 ℃ temperature-rise periods, pass into wet oxygen, wet oxygen is to take the throughput of 0.1 liter/min to pass in the 1000ml distilled water that temperature is 25 ℃ and obtain;
Step S500: high temperature sintering: amorphous precursor film, 800 ℃ of temperature sintering 2 hours, wherein, is passed into the wet Ar/O of oxygen content 200ppm in front 2/3 time
2gaseous mixture, in rear 1/3 time, passing into oxygen content is the dry Ar/O of 200～500ppm
2gaseous mixture, and passing into the dry Ar/O that oxygen content is 200～500ppm
2under the condition of gaseous mixture, with stove, be cooled to after 450 ℃, in the atmosphere of pure dry oxygen, be incubated 2 hours, obtain the YBCO superconducting thin film of preparing on the LAO substrate after palladium (Pd) nano dot is modified; Wet Ar/O
2gaseous mixture is by dry Ar/O
2gaseous mixture passes into the throughput of 0.5 liter/min and obtains in the distilled water of 40 ℃.
Step S600: as can be seen from Figure 1, the YBCO superconducting thin film of preparing on the LAO substrate after palladium (Pd) nano dot is modified has good c-axis orientation, the diffraction maximum of not obvious other orientations of YBCO.
Embodiment 2
Step S100: prepare palladium (Pd) nano dot:
Step S101: a certain amount of palladium acetylacetonate is dissolved in n Propanoic acid, obtains the precursor aqueous solution that palladium ion solubility is 0.002mol/L;
Step S102: adopt the mode Tu of spin coating on LAO monocrystalline the precursor liquid in step S101, the coating time is 60 seconds, and rotating speed is 3500 revs/min;
Step S103: under argon shield, sintering is 60 minutes in 1200 ℃ by the precursor film in step S102, generates palladium (Pd) nano dot at substrate surface, obtains the substrate that palladium (Pd) nano dot is modified;
Step S200: prepare Y by low fluorine technique
0.75sm
0.25bCO precursor aqueous solution:
Step S201: by acetic acid yttrium and barium acetate in molar ratio the ratio of 1:2 be dissolved in deionized water, at 40 ℃ fully after stirring and dissolving, according to the mol ratio of acetic acid yttrium and trifluoroacetic acid, be that 1:3 adds trifluoroacetic acid, at 40 ℃, react after 2 hours, rotary evaporation at 45 ℃, obtain white powder, with absolute methanol, dissolve, obtain the precursor liquid of yttrium (Y), barium (Ba);
Step S202: by Schweinfurt green and α-methacrylic acid in molar ratio the ratio of 1:4 be dissolved in absolute methanol, at 60 ℃, reflux 5 hours, rotary evaporation at 45 ℃, obtains blue gel, with absolute methanol, dissolves, and obtains the precursor liquid of Cu;
Step S203: the precursor liquid of yttrium (Y), barium (Ba), copper (Cu) is filtered respectively to rear mixing, obtain blue clear solution, rotary evaporation at 45 ℃, obtain blue gel, with absolute methanol, dilute again, controlling total cation (ruthenium ion, barium ions and copper ion) concentration is 1.5mol/L, obtains YBCO precursor liquid;
Step S204: change the acetic acid yttrium in step S201 into acetic acid samarium, become SmBCO precursor liquid according to step S201, step S202, Process configuration that step S203 is identical.
Step S205: YBCO, SmBCO precursor aqueous solution are mixed according to the volume ratio of 3:1, obtain Y
0.75sm
0.25bCO precursor liquid.
Step S300: apply Y on the substrate after palladium (Pd) nano dot is modified
0.75sm
0.25bCO:
By the Y configuring in step S200
0.75sm
0.25the method of BCO precursor liquid by spin coating is coated in step 1 on the substrate after palladium (Pd) nano dot is modified, and obtains Y
0.75sm
0.25bCO precursor film.
Step S400: low-temperature sintering: under room temperature, by the Y obtaining in step S300
0.75sm
0.25bCO precursor film is warming up to 100 ℃ with the programming rate of 600 ℃/h, then is warming up to 400 ℃ with the programming rate of 200 ℃/h, obtains amorphous precursor film.Wherein, from room temperature, rise to 150 ℃ of temperature-rise periods, with the gas flow of 0.2 liter/min, pass into dry oxygen; In 150 ℃ to 400 ℃ temperature-rise periods, pass into wet oxygen, wet oxygen is to take the throughput of 0.2 liter/min to pass into temperature and obtain in the distilled water of 30 ℃;
Step S500: high temperature sintering: amorphous precursor film, 820 ℃ of temperature sintering 3 hours, wherein, is passed into the wet Ar/O of oxygen content 300ppm in time of two of first three minute
2gaseous mixture, in rear 1/3 time, passing into oxygen content is the dry Ar/O of 300ppm
2gaseous mixture, and passing into the dry Ar/O that oxygen content is 300ppm
2under the condition of gaseous mixture, with stove, be cooled to after 500 ℃, in the atmosphere of pure dry oxygen, be incubated 3 hours, obtain the Y preparing on the LAO substrate after palladium (Pd) nano dot is modified
0.75sm
0.25bCO superconducting thin film; Wet Ar/O
2gaseous mixture is by dry Ar/O
2gaseous mixture passes into the throughput of 0.7 liter/min and obtains in the distilled water of 50 ℃.
Step S600: as can be seen from Figure 2, the Y preparing on the LAO substrate after Pd nano dot is modified
0.75sm
0.25the surfacing of BCO superconducting thin film, densification, does not have obvious hole, the existence of crackle and a axialite.Embodiment 3
Step S100: prepare palladium (Pd) nano dot:
Step S101: a certain amount of palladium acetylacetonate is dissolved in n Propanoic acid, obtains the precursor aqueous solution that palladium ion solubility is 0.003mol/L;
Step S102: adopt the mode of spin coating to be coated on LAO monocrystalline the precursor liquid in step S101, coating time is 70 seconds, and rotating speed is 4000 revs/min;
Step S103: the precursor film in step S102, under high-purity argon gas protection, 1300 ℃ of temperature sintering 120 minutes, is generated to palladium (Pd) nano dot at substrate surface, obtain the substrate that palladium (Pd) nano dot is modified;
Step S200: prepare Y by low fluorine technique
0.5sm
0.5bCO precursor aqueous solution:
Step S201: by acetic acid yttrium, barium acetate in molar ratio the ratio of 1:2 be dissolved in deionized water, at 40 ℃ fully after stirring and dissolving, according to the mol ratio of acetic acid yttrium and trifluoroacetic acid, be that 1:3 adds trifluoroacetic acid, at 40 ℃, react after 2 hours, rotary evaporation at 50 ℃, obtain white powder, with absolute methanol, dissolve, obtain the precursor liquid of yttrium (Y), barium (Ba);
Step S202: by Schweinfurt green and α-methacrylic acid in molar ratio the ratio of 1:4 be dissolved in absolute methanol, at 70 ℃, reflux 3 hours, rotary evaporation at 50 ℃, obtains blue gel, with absolute methanol, dissolves, and obtains the precursor liquid of Cu.
Step S203 filters respectively rear mixing by the precursor liquid of yttrium (Y), barium (Ba), copper (Cu), obtain blue clear solution, rotary evaporation at 50 ℃, obtain blue gel, with absolute methanol, dilute again, controlling total cation (ruthenium ion, barium ions and copper ion) concentration is 1.5mol/L, is YBCO precursor liquid.
Step S204: change the acetic acid yttrium in step S201 into acetic acid samarium, the Process configuration identical with step S203 according to step S201, step S202 becomes SmBCO precursor liquid
Step S205: YBCO, SmBCO precursor aqueous solution are mixed according to the volume ratio of 1:1, obtain Y
0.5sm
0.5bCO precursor liquid.
Step S300: apply Y on the substrate after palladium (Pd) nano dot is modified
0.5sm
0.5bCO:
By the Y configuring in step S200
0.5sm
0.5the method of BCO precursor liquid by spin coating is coated in step S100 on the substrate after palladium (Pd) nano dot is modified, and obtains Y
0.5sm
0.5bCO precursor film.
Step S400: low-temperature sintering: under room temperature, by the Y obtaining in step S300
0.5sm
0.5bCO precursor film is warming up to 100 ℃ with the programming rate of 600 ℃/h, then is warming up to 400 ℃ with the programming rate of 200 ℃/h, obtains amorphous precursor film.Wherein, from room temperature, rise to 150 ℃ of temperature-rise periods, with the gas flow of 0.3 liter/min, pass into dry oxygen; In 150 ℃ to 400 ℃ temperature-rise periods, pass into wet oxygen, wet oxygen is to take the throughput of 0.3 liter/min to pass into temperature and obtain in the distilled water of 35 ℃;
Step S500: high temperature sintering: by amorphous precursor film sintering 4 hours at 850 ℃ of temperature, wherein, pass into the wet Ar/O of oxygen content 500ppm in front 2/3 time
2gaseous mixture, in rear 1/3 time, passing into oxygen content is the dry Ar/O of 500ppm
2gaseous mixture, and passing into the dry Ar/O that oxygen content is 500ppm
2under the condition of gaseous mixture, with stove, be cooled to after 500 ℃, in the atmosphere of pure dry oxygen, be incubated 4 hours, obtain the Y preparing on the LAO substrate after palladium (Pd) nano dot is modified
0.5sm
0.5bCO superconducting thin film; Wet Ar/O
2gaseous mixture is by dry Ar/O
2gaseous mixture passes into the throughput of 1.0 liters/min and obtains in the 1000ml distilled water of 60 ℃.
Step S600: as can be seen from Figure 3, the Y preparing on the LAO substrate after palladium (Pd) nano dot is modified
0.5sm
0.5bCO superconducting thin film has higher critical transition temperature.
Claims (1)
1. on the chloric acid lanthanum substrate LAO after palladium Pd nano dot is modified, prepare Y for one kind
xsm
1-xthe method of BCO (0≤x≤1) superconducting thin film, the method comprises the following steps:
Step S100: prepare palladium Pd nano dot, comprise the following steps:
Step S101: palladium acetylacetonate is dissolved in n Propanoic acid, obtains the precursor aqueous solution that palladium ion solubility is 0.001～0.003mol/L;
Step 102: adopt the mode of spin coating to be coated on described chloric acid lanthanum substrate LAO monocrystalline the described precursor aqueous solution in step S101, form precursor film, coating time is 50～70 seconds, and rotating speed is 3000～4000 revs/min;
Step S103: by the sintering 20～120 minutes at the protective atmosphere of inert gas and 1000～1300 ℃ of temperature of the described precursor film in step S102, generate palladium Pd nano dot at substrate surface;
Step S200: prepare Y by low fluorine technique
xsm
1-xbCO (0≤x≤1) precursor aqueous solution, comprises the following steps:
Step S201: by acetic acid yttrium and barium acetate in molar ratio the ratio of 1:2 be dissolved in deionized water, at 30～40 ℃ of temperature fully after stirring and dissolving, the ratio that is 1:3 according to the mol ratio of acetic acid yttrium and trifluoroacetic acid adds trifluoroacetic acid, at 30～40 ℃ of temperature, react after 2～5 hours, rotary evaporation at 40～50 ℃ of temperature, obtain white powder, with absolute methanol, dissolve the precursor aqueous solution that this white powder obtains yttrium Y, barium Ba;
Step S202: by Schweinfurt green and α-methacrylic acid in molar ratio the ratio of 1:4 be dissolved in absolute methanol, at 60～70 ℃ of temperature, reflux 2～10 hours, rotary evaporation at 40～50 ℃ of temperature, obtain blue gel, with absolute methanol, dissolve this blue gel, obtain the precursor aqueous solution of copper Cu;
Step S203: the precursor aqueous solution of yttrium Y, barium Ba, copper Cu filters respectively rear mixing, obtain blue clear solution, make this blueness clear solution rotary evaporation at 40～50 ℃ obtain blue gel, with absolute methanol, dilute this blue gel again, make and comprise that the total cation concentration of ruthenium ion, barium ions and copper ion is 1.5mol/L, obtain YBCO precursor aqueous solution;
Step S204: change the described acetic acid yttrium in S201 into acetic acid samarium, become SmBCO precursor aqueous solution according to the Process configuration identical with S203 with S201, S202;
Step S205: YBCO, SmBCO precursor aqueous solution are mixed according to the volume ratio of 3:1 or 1:1, obtain Y
xsm
1-xbCO (0≤x≤1) precursor aqueous solution;
Step S300: apply Y on the substrate after palladium Pd nano dot is modified
xsm
1-xbCO (0≤x≤1), comprises the following steps:
By the Y configuring in step S200
xsm
1-xthe method of BCO (0≤x≤1) precursor aqueous solution by spin coating is coated in step S100 on the substrate after palladium Pd nano dot is modified, and obtains Y
xsm
1-xbCO (0≤x≤1) precursor film;
Step S400: low-temperature sintering, comprises the following steps:
At room temperature, precursor film is warming up to 100 ℃ with the programming rate of 600 ℃/h, then is warming up to 400 ℃ with the programming rate of 200 ℃/h, obtain amorphous precursor film, wherein, from room temperature, rise to 150 ℃ of temperature-rise periods, pass into dry oxygen, gas flow is 0.1～0.3 liter/min; In 150 ℃ to 400 ℃ temperature-rise periods, pass into wet oxygen; Wet oxygen is to take the throughput of 0.1～0.3 liter/min to pass into temperature and obtain in the distilled water of 25 ℃～35 ℃;
Step S500: high temperature sintering, comprises the following steps:
Amorphous precursor film in abovementioned steps S400, in 800～850 ℃ of sintering 2-4 hour, wherein, is passed into the wet Ar/O of oxygen content 200～500ppm in front 2/3 time
2gaseous mixture, in rear 1/3 time, passing into oxygen content is the dry Ar/O of 200～500ppm
2gaseous mixture, and passing into the dry Ar/O that oxygen content is 200～500ppm
2under the condition of gaseous mixture, with stove, be cooled to after 450 ℃～500 ℃, in the atmosphere of pure dry oxygen, be incubated 2-4 hour, obtain the Y preparing on the LAO substrate after Pd nano dot is modified
xsm
1-xbCO (0≤x≤1) superconducting thin film; Wet Ar/O
2gaseous mixture is by dry Ar/O
2gaseous mixture passes into the throughput of 0.5～1.0 liter/min and obtains in the distilled water of 40～60 ℃.
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