CN102912332A - Method for preparing RexCe1-xOy/M2Zr2O7 double-layer buffer layer by chemical solution deposition - Google Patents

Method for preparing RexCe1-xOy/M2Zr2O7 double-layer buffer layer by chemical solution deposition Download PDF

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CN102912332A
CN102912332A CN2012103189622A CN201210318962A CN102912332A CN 102912332 A CN102912332 A CN 102912332A CN 2012103189622 A CN2012103189622 A CN 2012103189622A CN 201210318962 A CN201210318962 A CN 201210318962A CN 102912332 A CN102912332 A CN 102912332A
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CN102912332B (en
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雷鸣
赵勇
武伟
蒲明华
张勇
张欣
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Southwest Jiaotong University
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Abstract

The invention discloses a method for preparing an RexCe1-xOy/M2Zr2O7 double-layer buffer layer by chemical solution deposition, which comprises the following steps: a. preparation of M2Zr2O7 film: dissolving M(NO3)3.6H2O and ZrO(NO3)3.2H2O in hydroxyethyl methyl ether according to the ion concentration M+3:Zr+4 ratio of 1:1, and adding an oxidized polyethylene 20000 synthetic colloid; applying the colloid onto an Ni-base alloy baseband, drying, and putting the Ni-base alloy baseband into a heat treatment furnace in an H2/Ar reducing atmosphere to carry out phase decomposition; and b. preparation of RexCe1-xOy film: preparing a rare earth nitrate mixture according to the rare earth ion (Re):cerium ion (Ce) ratio of x:(1-x) (0<=x<=0.5), dissolving the mixture in a high-polymer organic solvent synthetic colloid, applying the colloid onto an M2Zr2O7 substrate, drying, putting the M2Zr2O7 substrate into an atmosphere sintering furnace, and carrying out phase decomposition in the H2/Ar reducing atmosphere. The invention adopts the full-nitrate-system chemical solution deposition method to prepare the RexCe1-xOy/M2Zr2O7 double-layer buffer layer. Compared with the physical method, the preparation method disclosed by the invention is simple and easy to implement, has the advantages of low cost and no pollution, and can implement large-scale industrial production.

Description

A kind of chemical solution deposition prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer
Technical field
The invention belongs to the conductor of high-temperature superconductor coat research field, specifically relate to a kind of chemical solution deposition preparation Re x Ce 1-x O y / M 2 Zr 2 O 7 The method of double-layer bumper layer.
Background technology
S-generation belt material of high temperature superconduct because its good intrinsic electromagnetic property, especially its current capacity good under the upfield, is gathered around in power system and is had broad application prospects.
Conductor of high-temperature superconductor coat forms and comprises three parts, and substrate, buffer layer, superconducting layer, cushioning layer material serve as again barrier layer therein both as growth templates, act on great.La 2Zr 2O 7Since thermostability and with NiW substrate and the good chemical matching of YBCO, become the focus of coating conductor research.And CeO 2Because it has and the splendid matching degree of superconducting layer and good chemical stability, remains at present first-selected cushioning layer material.But the CeO of chemical method preparation 2There is the less problem of critical thickness in the individual layer buffer layer, is not enough to play iris action.And at La 2Zr 2O 7The upper high performance YBCO superconducting layer of acquisition that is difficult to.So Re x Ce 1-x O y / La 2Zr 2O 7The double-layer bumper layer becomes at present comparatively popular buffer layer frame form.
Summary of the invention
The object of the present invention is to provide a kind of cheaply, be conducive to the preparation of large-scale industrial production Re x Ce 1-x O y / M 2 Zr 2 O 7 The method of double-layer bumper layer, but that this preparation method compares with Physical is simple, cost is low, pollution-free large-scale industrial production.
The technical solution adopted for the present invention to solve the technical problems is a kind of chemical solution deposition preparation Re x Ce 1-x O y / M 2 Zr 2 O 7 The method of double-layer bumper layer is characterized in that: be made of following steps successively:
A, M 2 Zr 2 O 7 Thin film technology:
With M (NO 3) 3.6H 2O and ZrO (NO 3) 3.2H 2O is according to ionic concn M + 3: Zr + 4For 1:1 is dissolved in the hydroxyethyl methyl ether, add oxidic polyethylene 20000 synthetic colloids, colloid is coated on the Ni base alloy baseband, put into after the drying and be connected with H 2Resolve into phase in the heat treatment furnace of/Ar reducing atmosphere.
B, rare earth Re x Ce 1-x O y Thin film technology:
Press rare earth (Re) ion and cerium (Ce) ion ratio x:1-x, 0≤x≤0.5 preparation rare earth nitrate mixture is dissolved in mixture in the polymer organic solvent, and solution is coated on M 2 Zr 2 O 7 In the substrate, put into H after the drying 2In the atmosphere sintering furnace of/Ar protection of reducing atmosphere, resolve into phase.
According to a kind of chemical solution deposition preparation of the present invention Re x Ce 1-x O y / M 2 Zr 2 O 7 The method of double-layer bumper layer is characterized in that: described a is in the step, and rare earth (M) is lanthanum (La) or gadolinium (Gd).
According to a kind of chemical solution deposition preparation of the present invention Re x Ce 1-x O y / M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a is in the step, and the amount ratio of Gadolinium trinitrate, zirconium nitrate and hydroxyethyl methyl ether is: 1 mole of (Gadolinium trinitrate+zirconium nitrate): 0.5-3 rises volume hydroxyethyl methyl ether.
According to a kind of chemical solution deposition preparation of the present invention Re x Ce 1-x O y / M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a is in the step, and the add-on of oxidic polyethylene 20000 is the 3wt. ﹪-5wt. ﹪ of precursor aqueous solution total mass.
According to a kind of chemical solution deposition preparation of the present invention Re x Ce 1-x O y / M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a resolves into the phase process for being warming up to 350 ℃-600 ℃ with 1 ℃/min-5 ℃/min speed first in the step, allow organism and nitrate fully decompose, directly be warming up to afterwards 1100 ℃-1200 ℃ and become the phase temperature, be incubated 1-2 hour, obtain Re x Ce 1-x O y Film.
According to a kind of chemical solution deposition preparation of the present invention Re x Ce 1-x O y / M 2Zr 2O 7The method of double-layer bumper layer, it is characterized in that: described b is in the step, and rare earth is a kind of in yttrium (Y), lanthanum (La), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), the lutetium (Lu).
According to a kind of chemical solution deposition preparation of the present invention Re x Ce 1-x O y / M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described b is in the step, and the polymer organic solvent is the polymkeric substance of polymethyl acrylic acid or vinylformic acid and N-N dimethyl formamide.
According to a kind of chemical solution deposition preparation of the present invention Re x Ce 1-x O y / M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described b is in the step, resolves into the phase process for furnace temperature is risen to 350 with 1 ℃/min-5 ℃/min speed OC-550 OC, guarantee that macromolecule organic and nitrate fully decompose, after be warming up to 1000 oC-1200 oC becomes the phase temperature, is incubated 1-2 hour, Re x Ce 1-x O y Crystallize into phase.
According to a kind of chemical solution deposition preparation of the present invention Re x Ce 1-x O y / M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a step and b are in the step, and coating method can be spin-coating method, crystal pulling method or slit spraying method.
Beneficial effect of the present invention is: compared with prior art, one, the present invention adopts full nitrate system chemical solution deposition, has greatly reduced preparation cost, and the easier large-scale industrial production of chemical method; Its two, the rear-earth-doped CeO that adopts the polymer organic solvent to prepare 2Buffer layer, its critical thickness is greatly improved; Its three, adopt Re x Ce 1-x O y / M 2Zr 2O 7The framework of double-layer bumper layer had both guaranteed effectively that the thickness of buffer layer was enough to play well the barrier layer effect, on it Re x Ce 1-x O y Buffer layer can be guaranteed again the high performance YBCO superconducting layer of follow-up preparation.
 
Description of drawings
Fig. 1 is the invention process case Sm 0.2Ce 0.8O 1.9/ La 2Zr 2O 7The XRD figure spectrum of/NiW buffer layer;
Fig. 2 is the invention process case Sm 0.2Ce 0.8O 1.9/ La 2Zr 2O 7The SEM collection of illustrative plates of/NiW buffer layer.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is elaborated:
In recent years, relevant chemical solution deposition prepares La 2Zr 2O 7(LZO) report is a lot, but all is that the expensive metal alkoxide of employing is raw material, in order further to reduce production costs, improves the performance of film, adopts nitrate La (NO among the present invention 3) 3.6H 2O and ZrO (NO 3) 3.2H 2O is that precursor prepares high-quality LZO film.There is at present the physical vacuum of employing preparation method to prepare CeO 2/ La 2Zr 2O 7The double-layer bumper layer, and have no the full chemical method of the low-cost nitrate of employing.Gd 2Zr 2O 7And La 2Zr 2O 7Equally be the composite oxide material with pyrochlore constitution, from YBCO and NiW lattice match angle, Gd 2Zr 2O 7Also satisfy the condition as buffer layer.The invention provides a kind of preparation that is conducive to the heavy industrialization development at this Re x Ce 1-x O y / M 2Zr 2O 7Double-layer bumper floor height performance methodology.
Implement in the following manner:
Embodiment one: a kind of chemical solution deposition prepares Sm 0.2Ce 0.8O 1.9/ La 2Zr 2O 7The method of double-layer bumper layer is made of following steps successively:
A, La 2Zr 2O 7(LZO) thin film technology:
With an amount of La (NO 3) 3.6H 2O and ZrO (NO 3) 3.2H 2O is according to ionic concn La + 3: Zr + 4For 1:1 is dissolved in the ethylene glycol monomethyl ether, wherein rise volume ratio according to 1 mole of (Gadolinium trinitrate+zirconium nitrate): 0.5-3 and add the hydroxyethyl methyl ether, add 5wt.% oxidic polyethylene 20000 synthetic colloids.Colloid evenly is spun on the NiW base band, removes moisture content after the wet film drying of acquisition, then put into and be connected with H 2In the heat treatment furnace of/Ar reducing atmosphere, first be warming up to 350 ℃ with 5 ℃/min speed, allow organism and nitrate fully decompose, directly be warming up to 1100 ℃ and become the phase temperature afterwards, be incubated 2 hours, acquisition La 2Zr 2O 7/ NiW film.
B, rare-earth Sm 0.2Ce 0.8O 1.9Thin film technology:
Press rare-earth Sm ion and cerium Ce ion ratio 0.2:0.8 preparation rare earth nitrate and cerous nitrate mixture, the mixture of preparing is dissolved in the polymkeric substance of polyacrylic acid and N-N dimethyl formamide and obtains colloid, colloid is spun on La 2Zr 2O 7In/NiW the substrate, in infrared drying equipment, remove moisture afterwards, then with Sm 0.2Ce 0.8O 1.9/ La 2Zr 2O 7/ NiW puts into atmosphere sintering furnace, at H 2Under/Ar the protection of reducing atmosphere, furnace temperature is risen to 550 with 1 ℃/min speed OC, guarantee that macromolecule organic and nitrate fully decompose, after be warming up to 1100 oC is incubated 1 hour, guarantees Sm 0.2Ce 0.8O 1.9/ La 2Zr 2O 7/ NiW crystallizes into phase.
Embodiment two: a kind of chemical solution deposition prepares Gd 0.3Ce 0.7O 1.85/ Gd 2Zr 2O 7The method of double-layer bumper layer is made of following steps successively:
A, Gd 2Zr 2O 7(GZO) thin film technology:
With an amount of Gd (NO 3) 3.6H 2O and ZrO (NO 3) 3.2H 2O is according to ionic concn Gd + 3: Zr + 4For 1:1 is dissolved in the ethylene glycol monomethyl ether, wherein rise volume ratio according to 1 mole of (Gadolinium trinitrate+zirconium nitrate): 0.5-3 and add the hydroxyethyl methyl ether, add 3wt.% oxidic polyethylene 20000 synthetic colloids.Adopt crystal pulling method to be coated on the NiW base band in colloid, remove moisture content after the wet film drying of acquisition, then put into and be connected with H 2In the heat treatment furnace of/Ar reducing atmosphere, first be warming up to 600 ℃ with 1 ℃/min speed, allow organism and nitrate fully decompose, directly be warming up to 1200 ℃ and become the phase temperature afterwards, be incubated 1 hour, acquisition Gd 2Zr 2O 7/ NiW film.
B, rare-earth Gd 0.3Ce 0.7O 1.85Thin film technology:
Press rare-earth Gd ion and cerium Ce ion ratio 0.3:0.7 preparation rare earth nitrate and cerous nitrate mixture, the mixture of preparing is dissolved in the polymkeric substance of vinylformic acid and N-N dimethyl formamide and synthesizes colloid, adopt crystal pulling method to be coated on Gd in colloid 2Zr 2O 7In/NiW the substrate, in infrared drying equipment, remove moisture afterwards, then with Gd 0.3Ce 0.7O 1.85/ Gd 2Zr 2O 7/ NiW puts into atmosphere sintering furnace, at H 2Under/Ar the protection of reducing atmosphere, furnace temperature is risen to 350 with 5 ℃/min speed oC guarantees that macromolecule organic and nitrate fully decompose, after be warming up to 1200 oC is incubated 0.5 hour, guarantees Gd 0.3Ce 0.7O 1.85/ Gd 2Zr 2O 7/ NiW crystallizes into phase.
Among embodiment 1 and the embodiment 2, implement with rare-earth Sm and rare-earth Gd, wherein rare-earth yttrium (Y), lanthanum (La), praseodymium (Pr), neodymium (Nd), europium (Eu), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu) all can be according to implementing with upper type.
Fig. 1 is the Sm that case study on implementation makes 0.2Ce 0.8O 1.9/ La 2Zr 2O 7The X ray diffracting spectrum of/NiW buffer layer, as seen from the figure, the double-layer bumper layer that the ownership system gets all has good biaxial texture; The Sm that Fig. 2 case study on implementation makes 0.2Ce 0.8O 1.9/ La 2Zr 2O 7The SEM picture of/NiW double-layer bumper layer, the as seen from the figure smooth densification of buffer-layer surface, non-microcracked, have a good surface property.

Claims (9)

1. a chemical solution deposition prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: be made of following steps successively:
A, M 2Zr 2O 7Thin film technology:
With M (NO 3) 3.6H 2O and ZrO (NO 3) 3.2H 2O is according to ionic concn M + 3: Zr + 4For 1:1 is dissolved in the hydroxyethyl methyl ether, add oxidic polyethylene 20000 synthetic colloids, colloid is coated on the Ni base alloy baseband, put into H after the drying 2Resolve into phase in the heat treatment furnace of/Ar reducing atmosphere;
B, Re xCe 1-xO yThin film technology:
Press rare earth (Re) ion and cerium (Ce) ion ratio x:1-x, 0≤x≤0.5 preparation rare earth nitrate mixture is dissolved in the synthetic colloid of polymer organic solvent with mixture, and colloid is coated on M 2Zr 2O 7In the substrate, put into H after the drying 2In the sintering oven of/Ar protection of reducing atmosphere.
2. a kind of chemical solution deposition according to claim 1 prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a is in the step, and rare earth (M) is lanthanum (La) or gadolinium (Gd).
3. a kind of chemical solution deposition according to claim 1 prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a is in the step, and the amount ratio of Gadolinium trinitrate, zirconium nitrate and hydroxyethyl methyl ether is: 1 mole of (Gadolinium trinitrate+zirconium nitrate): 0.5-3 rises volume hydroxyethyl methyl ether.
4. a kind of chemical solution deposition according to claim 1 prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a is in the step, and the add-on of oxidic polyethylene 20000 is the 3wt. ﹪-5wt. ﹪ of precursor aqueous solution total mass.
5. a kind of chemical solution deposition according to claim 1 prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a resolves into the phase process for being warming up to 350 ℃-600 ℃ with 1 ℃/min-5 ℃/min speed first in the step, allow organism and nitrate fully decompose, directly be warming up to afterwards 1100 ℃-1200 ℃ and become the phase temperature, be incubated 1-2 hour, obtain M 2Zr 2O 7Film.
6. a kind of chemical solution deposition according to claim 1 prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer, it is characterized in that: described b is in the step, and rare earth is a kind of in yttrium (Y), lanthanum (La), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), the lutetium (Lu).
7. a kind of chemical solution deposition according to claim 1 prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described b is in the step, and the polymer organic solvent is the polymkeric substance of polymethyl acrylic acid or vinylformic acid and N-N dimethyl formamide.
8. a kind of chemical solution deposition according to claim 1 prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described b resolves into the phase process for furnace temperature is risen to 350 with 1 ℃/min-5 ℃/min speed in the step oC-550 oC guarantees that macromolecule organic and nitrate fully decompose, after be warming up to 1000 oC-1200 oC becomes the phase temperature, is incubated 1-2 hour, Re xCe 1-xO yCrystallize into phase.
9. a kind of chemical solution deposition according to claim 1 prepares Re xCe 1-xO y/ M 2Zr 2O 7The method of double-layer bumper layer is characterized in that: described a step and b are in the step, and coating method can be spin-coating method, crystal pulling method or slit spraying method.
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CN110104680A (en) * 2019-05-16 2019-08-09 湖南工学院 One kind having core-shell structure heat barrier coat material and preparation method thereof
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CN111978087B (en) * 2019-05-22 2022-04-15 北京理工大学 Composite material and preparation method and application thereof

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