CN102851655B - Preparation method for Gd2Zr2O7 buffer layer through chemical solution deposition - Google Patents

Preparation method for Gd2Zr2O7 buffer layer through chemical solution deposition Download PDF

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CN102851655B
CN102851655B CN201210318922.8A CN201210318922A CN102851655B CN 102851655 B CN102851655 B CN 102851655B CN 201210318922 A CN201210318922 A CN 201210318922A CN 102851655 B CN102851655 B CN 102851655B
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film
preparation
wet film
aqueous solution
precursor aqueous
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CN102851655A (en
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雷鸣
赵勇
武伟
蒲明华
张勇
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Southwest Jiaotong University
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Southwest Jiaotong University
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Abstract

The invention provides a preparation method for a Gd2Zr2O7 buffer layer through chemical solution deposition. The preparation method comprises the following concrete steps: A, preparation of a Gd2Zr2O7 precursor solution: a step of dissolving a proper amount of Gd(NO3)3.6H2O and Zr(NO3)3.2H2O according to a ratio of the concentration of Gd<3+> ions to the concentration of Zr<4+> ions of 1: 1 in hydroxyethyl methyl ether and adding oxidized polyethylene 20000 to adjust the viscosity of an obtained solution so as to obtain the precursor solution; B, preparation of a wet film: a step of uniformly coating the precursor solution on a textured substrate so as to obtain the wet film; C, preparation of a dry film: a step of putting the wet film into a drying apparatus to remove moisture in the wet film; and D, decomposition for formation of a phase: a step of putting the dry film into a heat treatment furnace filled with H2Ar reducing atmosphere, heating the film to a temperature of 350 to 600 DEG C at a rate of 1 to 5 DEG C/min at first so as to allow organic matters and nitrate to be fully decomposed, then directly heating the film to allow the film to be in a phase-forming high temperature zone of 1100 to 1200 DEG C and carrying out insulation for 0.5 to 2 h so as to obtain a Gd2Zr2O7 film. The preparation method for the Gd2Zr2O7 buffer layer by using a chemical approach and a nitrate system has the advantages of low cost, a simple process, easily controllable operation and no pollution to the environment and is favorable for large scale industrial production.

Description

A kind of chemical solution deposition prepares Gd 2zr 2o 7the method of buffer layer
Technical field
The invention belongs to conductor of high-temperature superconductor coat research field, relate to a kind of chemical solution deposition and prepare Gd 2zr 2o 7the method of buffer layer.
Background technology
Second-generation high-temperature superconductor, due to the intrinsic electromagnetic property that it is excellent, especially its current capacity excellent under upfield, gathers around and has broad application prospects in power system.
Conductor of high-temperature superconductor coat composition comprises three parts, substrate, buffer layer, superconducting layer, and cushioning layer material both as growth templates, serves as barrier layer again wherein, acts on great.La 2zr 2o 7due to thermostability and with NiW substrate and the good chemical matching of YBCO, become coating conductor research focus.Gd 2zr 2o 7and La 2zr 2o 7equally the composite oxide material with pyrochlore constitution, from YBCO and NiW lattice match angle, Gd 2zr 2o 7also the condition as buffer layer is met.In recent years, major part adopts expensive metal alkoxide to be that raw material is to prepare La 2zr 2o 7(LZO), therefore cost is high, therefore needs to be improved, and in order to reduce costs further, adopts nitrate Gd (NO in this patent 3) 3.6H 2o and ZrO (NO 3) 3.2H 2o is that precursor is to prepare the Gd of high-quality 2zr 2o 7film, replaces La 2zr 2o 7.
Summary of the invention
The object of the present invention is to provide a kind of cheap, be conducive to the preparation Gd of large-scale industrial production 2zr 2o 7the method of buffer layer, the method preparation technology is simple compared with Physical, cost is low, free from environmental pollution, can large-scale industrial production.
The technical solution adopted for the present invention to solve the technical problems is, a kind of chemical solution deposition prepares Gd 2zr 2o 7the method of buffer layer, is characterized in that: be made up of following steps successively:
A, Gd 2zr 2o 7the preparation of precursor aqueous solution:
By 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 hydroxyethyl methyl ether, add the viscosity of oxidic polyethylene 20000 regulator solution, obtain precursor aqueous solution;
The preparation of b, wet film: be evenly coated in by obtained precursor aqueous solution in texture base band, obtains wet film.
The preparation of c, dry film: wet film is entered freeze-day with constant temperature equipment, removes moisture content in film completely.
D, resolve into phase:
Put into and be connected with H 2in the heat treatment furnace of/Ar reducing atmosphere, first with 1 DEG C/min-5 DEG C/min ramp to 350 DEG C-600 DEG C, allow organism and nitrate fully decompose, be directly warming up to into 1100 DEG C-1200 DEG C, phase high-temperature zone afterwards, insulation 0.5-2 hour, obtains Gd 2zr 2o 7film.
2, a kind of chemical solution deposition according to claim 1 prepares Gd 2zr 2o 7the method of buffer layer, is characterized in that: in described a step, 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.
Gd is prepared according to a kind of chemical solution deposition of the present invention 2zr 2o 7the method of buffer layer, is characterized in that: in described a step, the add-on of oxidic polyethylene 20000 is the 3wt. ﹪-5wt. ﹪ of precursor aqueous solution total mass.
Technical solution of the present invention beneficial effect is: compared with prior art, one, adopts nitrate system chemical solution deposition, significantly reduces preparation cost, and the easier large-scale industrial production of chemical method; They are two, the Gd of preparation years old 2zr 2o 7film performance can with La 2zr 2o 7compare favourably.
Accompanying drawing explanation
Fig. 1 is the invention process case Gd 2zr 2o 7the XRD figure spectrum of/NiW buffer layer;
Fig. 2 is the invention process case Gd 2zr 2o 7the SEM collection of illustrative plates of/NiW buffer layer;
Fig. 3 is the invention process case Gd 2zr 2o 7the EDX collection of illustrative plates of/NiW buffer layer;
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further described in detail:
Embodiment one: a kind of chemical solution deposition prepares Gd 2zr 2o 7the method of buffer layer, is made up of following steps successively:
A, Gd 2zr 2o 7the preparation of precursor aqueous solution:
By the Gd (NO of 1 mole 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 0.5 liter of volume hydroxyethyl methyl ether, add the viscosity of oxidic polyethylene 20000 regulator solution of 3wt.%, obtain precursor aqueous solution.
The preparation of b, wet film:
Adopted by precursor aqueous solution spin-coating method to be evenly coated in Ni-5%W base band, obtain wet film.
The preparation of c, dry film:
By wet film by constant temperature 120 oc infrared drying equipment 10 minutes, removes moisture content in film.
D, resolve into phase:
Put into and be connected with H 2in the heat treatment furnace of/Ar reducing atmosphere, first with 1 oc/min is warming up to 350 DEG C, allows organism and nitrate fully decompose, and is directly warming up to into 1100 DEG C, phase high-temperature zone afterwards, is incubated 2 hours, obtains Gd 2zr 2o 7film.
Embodiment two: a kind of chemical solution deposition of the present invention prepares Gd 2zr 2o 7the method of buffer layer, is made up of following steps successively:
A, Gd 2zr 2o 7the preparation of precursor aqueous solution:
By the Gd (NO of 1 mole 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 3 liters of volume hydroxyethyl methyl ethers, add the viscosity of oxidic polyethylene 20000 regulator solution of 5wt.%, obtain precursor aqueous solution.
The preparation of b, wet film:
Adopted by precursor aqueous solution crystal pulling method to be evenly coated in Ni-5%W base band, obtain wet film.
The preparation of c, dry film:
By wet film by constant temperature 100 oc infrared drying equipment 20 minutes, removes moisture content in film.
D, resolve into phase:
Put into and be connected with H 2in the heat treatment furnace of/Ar reducing atmosphere, first with 5 oc/min is warming up to 600 DEG C, allows organism and nitrate fully decompose, and is directly warming up to into 1200 DEG C, phase high-temperature zone afterwards, is incubated 0.5 hour, obtains Gd 2zr 2o 7film.
Embodiment three: a kind of chemical solution deposition prepares Gd 2zr 2o 7the method of buffer layer, is made up of following steps successively:
A, Gd 2zr 2o 7the preparation of precursor aqueous solution:
By the Gd (NO of 1 mole 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 2 liters of volume hydroxyethyl methyl ethers, add the viscosity of oxidic polyethylene 20000 regulator solution of 4wt.%, obtain precursor aqueous solution.
The preparation of b, wet film:
Adopted by precursor aqueous solution slot coated method to be evenly coated in Ni-5%W base band, obtain wet film.
The preparation of c, dry film:
By wet film by constant temperature 110 oc infrared drying equipment 15 minutes, removes moisture content in film.
D, resolve into phase:
Put into and be connected with H 2in the heat treatment furnace of/Ar reducing atmosphere, first with 3 oc/min is warming up to 450 DEG C, allows organism and nitrate fully decompose, and is directly warming up to into 1150 DEG C, phase high-temperature zone afterwards, is incubated 1 hour, obtains Gd 2zr 2o 7film.
Fig. 1 is the Gd that above-mentioned case study on implementation obtains 2zr 2o 7the X ray diffracting spectrum of/NiW buffer layer, as seen from the figure, Gd 2zr 2o 7(400) peak value manifest, the Gd obtained by proving 2zr 2o 7/ NiW buffer layer has good biaxial texture; Fig. 2 is the Gd that case study on implementation obtains 2zr 2o 7the SEM picture of/NiW buffer layer, the smooth densification of buffer-layer surface as seen from the figure, non-microcracked, there is good surface property.Fig. 3 is the Gd that case study on implementation obtains 2zr 2o 7the EDX collection of illustrative plates of/NiW buffer layer, the ratio of Gd, Zr ion and existence thereof, prove really to obtain Gd as seen from the figure 2zr 2o 7film.

Claims (3)

1. a chemical solution deposition prepares Gd 2zr 2o 7the method of buffer layer, is characterized in that: be made up of following steps successively:
A, Gd 2zr 2o 7the preparation of precursor aqueous solution: by the Gd (NO of 1 mole 3) 36H 2o and ZrO (NO 3) 32H 2o is according to ionic concn Gd + 3: Zr + 4for 1:1 is dissolved in 0.5 liter of volume hydroxyethyl methyl ether, add the viscosity of oxidic polyethylene 20000 regulator solution of 3wt.%, obtain precursor aqueous solution;
The preparation of b, wet film: adopted by precursor aqueous solution spin-coating method to be evenly coated in Ni-5%W base band, obtains wet film;
The preparation of c, dry film: by wet film by constant temperature 120 oc infrared drying equipment 10 minutes, removes moisture content in film;
D, resolve into phase: put into and be connected with H 2in the heat treatment furnace of/Ar reducing atmosphere, first with 1 oc/min is warming up to 350 DEG C, allows organism and nitrate fully decompose, and is directly warming up to into 1100 DEG C, phase high-temperature zone afterwards, is incubated 2 hours, obtains Gd 2zr 2o 7film.
2. a chemical solution deposition prepares Gd 2zr 2o 7the method of buffer layer, is characterized in that: be made up of following steps successively:
A, Gd 2zr 2o 7the preparation of precursor aqueous solution: by the Gd (NO of 1 mole 3) 36H 2o and ZrO (NO 3) 32H 2o is according to ionic concn Gd + 3: Zr + 4for 1:1 is dissolved in 3 liters of volume hydroxyethyl methyl ethers, add the viscosity of oxidic polyethylene 20000 regulator solution of 5wt.%, obtain precursor aqueous solution;
The preparation of b, wet film: adopted by precursor aqueous solution crystal pulling method to be evenly coated in Ni-5%W base band, obtains wet film;
The preparation of c, dry film: by wet film by constant temperature 100 oc infrared drying equipment 20 minutes, removes moisture content in film;
D, resolve into phase: put into and be connected with H 2in the heat treatment furnace of/Ar reducing atmosphere, first with 5 oc/min is warming up to 600 DEG C, allows organism and nitrate fully decompose, and is directly warming up to into 1200 DEG C, phase high-temperature zone afterwards, is incubated 0.5 hour, obtains Gd 2zr 2o 7film.
3. a chemical solution deposition prepares Gd 2zr 2o 7the method of buffer layer, is characterized in that: be made up of following steps successively:
A, Gd 2zr 2o 7the preparation of precursor aqueous solution: by the Gd (NO of 1 mole 3) 36H 2o and ZrO (NO 3) 32H 2o is according to ionic concn Gd + 3: Zr + 4for 1:1 is dissolved in 2 liters of volume hydroxyethyl methyl ethers, add the viscosity of oxidic polyethylene 20000 regulator solution of 4wt.%, obtain precursor aqueous solution;
The preparation of b, wet film: adopted by precursor aqueous solution slot coated method to be evenly coated in Ni-5%W base band, obtains wet film;
The preparation of c, dry film: by wet film by constant temperature 110 oc infrared drying equipment 15 minutes, removes moisture content in film;
D, resolve into phase: put into and be connected with H 2in the heat treatment furnace of/Ar reducing atmosphere, first with 3 oc/min is warming up to 450 DEG C, allows organism and nitrate fully decompose, and is directly warming up to into 1150 DEG C, phase high-temperature zone afterwards, is incubated 1 hour, obtains Gd 2zr 2o 7film.
CN201210318922.8A 2012-09-03 2012-09-03 Preparation method for Gd2Zr2O7 buffer layer through chemical solution deposition Expired - Fee Related CN102851655B (en)

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CN102222761A (en) * 2011-04-12 2011-10-19 西南交通大学 Preparation method of high temperature superconductive coating conductor La2Zr2O7 buffer layer film

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102222761A (en) * 2011-04-12 2011-10-19 西南交通大学 Preparation method of high temperature superconductive coating conductor La2Zr2O7 buffer layer film

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* Cited by examiner, † Cited by third party
Title
Highly textured Gd2Zr2O7 films grown on textured Ni-5 at.%W substrates by solution deposition route: Growth, texture evolution, and microstructure dependency;Y. Zhao 等;《Thin Solid Films》;20120101;第520卷(第6期);第1页第2栏第7－9行，第2页第2.1节、2.2节，第4页第2栏第4－6行、第50－53行，第6页第1栏第20－21行、第2栏第2－5行，第8页第2栏第14－19行 *
周志华等.电介质陶瓷.《材料化学》.化学工业出版社、教材出版中心,2006,(第1版),第19页. *
硝酸钆水合物热分解研究;杨祖培;《无机化学学报》;19900930;第6卷(第3期);第2页第8－9行 *

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