CN101178955B - Method for enhancing CeO2 thin film thickness for coatings conductive body - Google Patents
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- CN101178955B CN101178955B CN2007100474737A CN200710047473A CN101178955B CN 101178955 B CN101178955 B CN 101178955B CN 2007100474737 A CN2007100474737 A CN 2007100474737A CN 200710047473 A CN200710047473 A CN 200710047473A CN 101178955 B CN101178955 B CN 101178955B
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Abstract
The invention discloses a method with a low cost for increasing the film thickness by mixing rare earth irons in a CeO<SUB>2</SUB> film. Acetate or acetylacetone salts with corresponding content of illinium, holmium, samarium, zirconium, etc. are mixed into mixed solution of cerium acetate by dissolving, heating and mixing so as to become mixed precursor solution with a stated proportion. The precursor solution is coated on a metal underlay after baking, then the CeO<SUB>2</SUB> film with a biaxial texture, a flat surface and a compact structure which is used for a superconducting coated conductor with high temperature is obtained after heat treatment in the next step.
Description
Technical field
The present invention relates to a kind of by rear-earth-doped to improve used for coating conductor CeO
2The method of film thickness.
Two, background technology
More and more caused the attention of countries in the world governments based on epitaxially grown second generation conductor of high-temperature superconductor coat in the concerned power application prospects with it.Each developed country considers from the technological innovation and the long-term interest of national electric power energy industry one after another, has actively implemented to be intended to promote the commercialization of second generation superconductor and the strategic plan that electric power is used, and international competition also is growing more intense.
Typical coating conductor structure generally includes the protective layer at metal substrate, resilient coating, superconducting layer and top.Wherein the buffer layer thin film technology of preparing of height biaxial texture has become the guardian technique of coating conductor.The effect of resilient coating is as follows: on the one hand, it is the epitaxially grown textured substrate of superconducting layer, also is the barrier layer that overcomes the metallic matrix Elements Diffusion and may react with superconducting layer simultaneously.Its crystal grain of last functional requirement is arranged must have the biaxial texture characteristic, and good with the lattice match of superconducting layer; And the latter requires it to have characteristics such as good chemical stability and high-compactness.Early stage people attempt to adopt noble metals such as Ag, Pt, Pb as resilient coating, but owing to have the problem of lattice mismatch and multiple texture, so they are also unsuccessful.The zirconia that Y is stable (YSZ) once was regarded as a kind of resilient coating of the base band of RABiTS preferably afterwards, its high compactness can stop the diffusion of base metal ion to superconducting layer fully, but shortcoming is bigger with superconducting layer mismatch degree, can reduce the superconductivity even the quench of superconducting layer.[Appl.Phys.Lett, 1991,58 (19): 2165-2167] such as Wu had reported CeO in 1991
2Be the epitaxially grown better resilient coating of YBCO, its YBCO on lattice quite mates, and is chemically also highly stable.Takahashi etc. [IEEE Trans.On Appl.Supercond, 1999.9 (2): 3373-2275] utilize CeO
2As single resilient coating the Ag of texture with on obtained the YBCO of height biaxial texture.Yet CeO
2Individual defective is arranged, and promptly (being about 50nm) just has the micro-crack appearance when its thickness surpasses certain value.Therefore people have been developed YSZ/CeO
2Type compound buffer layer structure, wherein CeO
2Thin (＜50 nm) and YSZ thicker (1 μ m).[Appl.Phys.Lett, 1992,60 (6): 1795-1797] such as Goyal utilized such compound buffer layer structure in 1996, had obtained nearly 1MA/cm first
2The coating conductor of critical current density (77K).Because YSZ and YBCO mate on lattice and not really in good condition, people increase the thin CeO of one deck thereon again afterwards
2, so can very improve the YBCO quality effectively.From then on YBCO/CeO
2/ YSZ/CeO
2/ Ni becomes a normal structure of early stage coating conductor.
Series of rare earth oxide (RE has also studied in ORNL group
2O
3, RE=Y, Yb, Gd, Eu etc.) and as the possibility of resilient coating, wherein Y
2O
3And Yb
2O
3Be found to be cushioning layer material preferably, this is because them and the close cause of the basic alloy lattice constant of Ni.[Appl.Phys.Lett, 1992,61 (10): 1243-1245] such as Bardal in 1992 and Prusseit had once prepared YBCO/Y by thermal evaporation method on the Si monocrystalline
2O
3/ YSZ/Si structure; [Physica C, 2002,372:810-813] such as nearest Tomov is with at a ternary RABiTS (Ni-Cr-W alloy), do not using reproducibility mixed atmosphere (H
2Successfully obtained high-quality Y under+Ar) the situation
2O
3/ YSZ/CeO
2Type resilient coating (FWHM is about 10 ° in the face, and (111) orientation disappears fully).Y
2O
3Lattice constant between Ni and YBCO, and it is not as CeO
2Exist thickness to induce the phenomenon of crackle like that.Ichinose and Cai etc. [Physica C, 2002,372-376:786-798] had once prepared Y
2O
3The coating conductor of single transition zone, their result is: the lattice texture inside and outside the YBCO face is better, with use Y
2O
3/ YSZ multi-buffering-layer sample is suitable, but superconductivity is unsatisfactory.This may be relevant with the diffusion of Ni, because Y
2O
3Density do not resemble the YSZ highly, under the situation of thickness deficiency, be difficult to stop on the matrix metallic element to the diffusion of superconducting layer, thereby the performance that causes superconducting layer reduces.The single resilient coating of other kind, for example La
0.7Si
0.3MnO
3, SrRuO
3, LaMnO
3, LaNiO
3And NdGaO
3Be studied Deng also, wherein preceding two kinds of conductive characteristics owing to them help the enhancing of whole coating conductor electric stability, thereby are had an optimistic view of especially.Adopt the short sample coating conductor of single resilient coating once to have Jc (77K) to surpass 1MA/cm
2Report, but the result report of long carry sample is not arranged as yet so far.At present, though people will CeO
2/ YSZ/Y
2O
3(CeO
2) be considered as the standard buffer layer structure of RABiTS technology path, and be successfully used to the long band preparation of Reel-to-Reel, but the work of seeking the individual layer cushioning layer material of new function admirable does not stop all always.
It is found that recently by rear-earth-doped CeO
2Can improve the thickness of film significantly, in the hope of obtain the CeO of individual layer by this kind method
2The buffer layer thin film material that mixes.So just can greatly reduce the preparation cost of coating conductor.A.Gauzzi etc. [IEEE Trans.Appl.Superconduct.Vol.17, No.3 June 2007] go out the CeO that thickness reaches 260nm by prepared by heat evaporation
2Doping film, performances such as inside and outside texture of its face and surface roughness also significantly do not reduce simultaneously, and this is the doped Ce O for preparing individual layer
2Buffer layer thin film provides good precedent.And compare with methods such as pulsed laser deposition (PLD), magnetron sputtering and thermal evaporations, chemical solution method (CSD) is not owing to need high-vacuum apparatus, be a kind of the most economic preparation method, be hopeful to be applied to the long band of suitability for industrialized production YBCO conductor of high-temperature superconductor coat most.Along with this technology continuous maturation experimentally, increasing people begins to pay close attention to the full chemical method technology of preparing of resilient coating to superconducting layer, and this has become one of much-talked-about topic of current coating conductor development.Therefore prepare effective single layer barrier CeO by the CSD method
2Rear-earth-doped film finally moves towards commerce to coating conductor and has great practical significance.
Three, summary of the invention
The present invention is directed to the CeO of the individual layer that exists in the prior art
2Can not stop of the diffusion of base metal ion effectively, and the problem that multilayer film is difficult to prepare and cost is high provides a kind of by the rear-earth-doped CeO of raising to superconducting layer
2The method of film quality and thickness.
For achieving the above object, the present invention adopts following technical scheme:
A kind of raising used for coating conductor CeO
2The method of film thickness is characterized in that the concrete steps of this method are as follows:
A. the cerous acetate after will toasting is dissolved in the mixed solution of propionic acid, isopropyl alcohol and acetylacetone,2,4-pentanedione, and heats and to be stirred to solution even and transparent at 60～80 ℃; Temperature is brought up to 100～120 ℃, continues to add thermal agitation and add to need the Doped Rare Earth metal organic salt, can stop to add thermal agitation to solution is even and transparent; Gained solution was toasted 12 hours under 100 ℃ temperature, promptly obtain precursor aqueous solution; The volume ratio of wherein said propionic acid, isopropyl alcohol and acetylacetone,2,4-pentanedione is 3.5～3: 1: 0.5～1; The mol ratio of institute's Doped Rare Earth metal ion and cerium ion is: 0.25～1: 1; The precursor aqueous solution concentration of gained is 0.1mol/L～0.3mol/L;
B. above-mentioned precursor aqueous solution is coated on the substrate of conductor of high-temperature superconductor coat of pretreated biaxial texture, the method for coating is spin coating or dip-coating; During spin coating, the rotating speed of sol evenning machine is 800～2000 rev/mins, and the time is 20 seconds～1 minute; During dip-coating, substrate stops in colloidal sol after 10～20 seconds and withdraws from 1～4 centimeters/minute;
C. with 50～180 ℃ of bakings 10～20 minutes in baking oven of the above-mentioned substrate that scribbles precursor aqueous solution, put into then and be connected with Ar+5%H
2The vacuum tube furnace of gaseous mixture under 800 ℃～1000 ℃ temperature, annealed 1～8 hour, at last with stove cooling, the conductor of high-temperature superconductor coat that promptly obtains mixing doped Ce O
2Film, its structural formula is: RE
xCe
1-xO
2-δ, wherein RE is rare-earth metal doped ion, and X is 0.2～0.5, and δ is 0～0.25.
Above-mentioned need Doped Rare Earth metal organic salt is: acetic acid samarium, acetic acid holmium, acetic acid yttrium or acetylacetone,2,4-pentanedione zirconium.
The metal substrate of above-mentioned biaxial texture is: the Ni+5%W alloy.
Above-mentioned step a is: it is even and transparent that the mixed solution of propionic acid, isopropyl alcohol and the acetylacetone,2,4-pentanedione of cerous acetate is stirred to solution 60～80 ℃ of heating, after adding needs the Doped Rare Earth metal organic salt, continue to add thermal agitation at 100～120 ℃ again, get evenly and transparent up to solution becomes.
Among the above-mentioned steps c, as formula R E
xCe
1-xO
2-δIn x=0.5 the time, its annealing temperature is 1000 ℃; And when x＜0.5, its annealing temperature is 900 ℃; And 180 ℃ and the 600 ℃ stops that 15 minutes and 30 minutes are arranged respectively, heating rate is 10 ℃/min in the annealing process.
The invention provides and under non-vacuum condition, improve used for coating conductor CeO
2The method of film thickness, this method is with low cost, and the doped Ce O for preparing
2Film thickness can reach 200nm, and the inside and outside texture property of good face is arranged, and film surface is even, smooth and flawless.
Description of drawings
Fig. 1. the doped Ce O of the inventive method preparation
2Film H
0.5Ce
0.5O
1.75XRD figure
Fig. 2. the doped Ce O of the inventive method preparation
2Film H
0.5Ce
0.5O
1.75The EDX collection of illustrative plates
Fig. 3. the doped Ce O of the inventive method preparation
2Film H
0.5Ce
0.5O
1.75Utmost point figure
Fig. 4. the doped Ce O of the inventive method preparation
2Film Sm
0.2Ce
0.8O
1.9Utmost point figure
Fig. 5. the doped Ce O of the inventive method preparation
2Film Zr
0.2Ce
0.8O
2Utmost point figure
Fig. 6. the doped Ce O of the inventive method preparation
2Film Y
0.5Ce
0.5O
1.75Utmost point figure
Fig. 7. the doped Ce O of the inventive method preparation
2Film H
0.5Ce
0.5O
1.75SEM figure
Embodiment
Embodiment one: take by weighing acetic acid holmium (Ho[CH
3COO]
31.5H
2O) 0.342g, cerous acetate (Ce[CH
3COO]
31.5H
2O) 0.344g, after the baking cerous acetate is joined in the mixed solution of 6ml propionic acid, 2ml isopropyl alcohol and 2ml acetylacetone,2,4-pentanedione and add thermal agitation 30min at 60 ℃, treat after solution substantially evenly temperature to be brought up to 100 ℃, add the acetic acid holmium simultaneously and add thermal agitation and get homogeneous transparent up to solution becomes and promptly stop to stir, obtain the Ho of 0.2mol/L
0.5Ce
0.5O
1.75Precursor aqueous solution 10ml.Gained solution is put into 100 ℃ of bakings of baking oven to be preserved stand-by after about 12 hours.
The Ni-W substrate of getting 1 * 1cm cleans and dries up with ethanol again with acetone ultrasonic waves for cleaning 20min.With the rotating speed spin coating 30s of 800rpm, put into vacuum tube furnace then and be warmed up to 180 ℃ and 600 ℃ with 10 ℃/min and stop 15min and 30min respectively, again with phase same rate to 1000 ℃ annealing 2h.With the stove cooling, just can obtain the Ho of biaxial texture at last
0.5Ce
0.5O
1.75Film.Can obtain biaxial texture and the uniform and smooth Ho in surface by repeating coating
0.5Ce
0.5O
1.75Thick film.Compose Ho in the visible film by the EDX of Fig. 2
3+And Ce
4+The ratio of ion is close to 1: 1.Its X ray 2 θ scanning and utmost point figure see Fig. 1 and Fig. 3, and the result shows that in the existing good face of this sample be texture property.And it is even, smooth and flawless by the visible gained film surface of the scanning electron microscope diagram of Fig. 7.
Embodiment two: take by weighing acetylacetone,2,4-pentanedione zirconium (Zr[CH
3COCHCOCH
3]
3XH
2O) 0.195g, cerous acetate (Ce[CH
3COO]
31.5H
2O) 0.5504g.Preparation technology under it and the example 1 identical Zr that obtains
0.2Ce
0.8O
2Precursor aqueous solution, different is to adopt dip-coating method, soaks 15s in mixed solution, withdraws from about 2-3cm/min again.Press intensification condition identical in the example 1 and, can obtain the Zr of biaxial texture 900 ℃ of annealing 2 hours
0.2Ce
0.8O
2Film.Its X ray 2 θ scanning and utmost point figure see Fig. 1 and Fig. 5.
Prepare doped Ce O respectively according to said method
2Film Sm
0.2Ce
0.8O
1.9, Y
0.5Ce
0.5O
1.75, their X ray 2 θ scanning and utmost point figure see Fig. 1, Fig. 4, Fig. 6.As can be seen from the figure, it is texture property that the gained sample all has in the good face, and the surface is also evenly smooth.The maximum ga(u)ge of the doping film of process laminated coating can reach more than the 200nm, also can keep the sliding surface of texture property peace lay the grain preferably.
Claims (5)
1. one kind is improved used for coating conductor CeO
2The method of film thickness is characterized in that the concrete steps of this method are as follows:
A. the cerous acetate after will toasting is dissolved in the mixed solution of propionic acid, isopropyl alcohol and acetylacetone,2,4-pentanedione, and it is even and transparent to be stirred to solution 60～80 ℃ of heating; Temperature is brought up to 100～120 ℃, and continuing to add thermal agitation and adding needs the Doped Rare Earth metal organic salt, and is even and transparent to solution; Gained solution was toasted 12 hours under 100 ℃ temperature, promptly obtain precursor aqueous solution; The volume ratio of wherein said propionic acid, isopropyl alcohol and acetylacetone,2,4-pentanedione is 3.5～3: 1: 0.5～1; The mol ratio of institute's Doped Rare Earth metal ion and cerium ion is: 0.25～1: 1; The precursor aqueous solution concentration of gained is 0.1mol/L～0.2mol/L;
B. above-mentioned precursor aqueous solution is coated on the metal substrate of pretreated biaxial texture, the method for coating is spin coating or dip-coating; During spin coating, the rotating speed of sol evenning machine is 800～2000 rev/mins, and the time is 20 seconds～1 minute; During dip-coating, substrate stops in colloidal sol after 10～20 seconds and withdraws from 1～4 centimeters/minute;
C. with 50～180 ℃ of bakings 10～20 minutes in baking oven of the above-mentioned substrate that scribbles precursor aqueous solution, put into then and be connected with Ar+5%H
2The vacuum tube furnace of gaseous mixture under 800 ℃～1000 ℃ temperature, annealed 1～8 hour, at last with stove cooling, the conductor of high-temperature superconductor coat that promptly obtains mixing doped Ce O
2Film, its structural formula is: RE
xCe
1-xO
2-δ, wherein RE is rare-earth metal doped ion, x is 0.2～0.5,6 to be 0～0.25.
2. raising used for coating conductor CeO according to claim 1
2The method of film thickness is characterized in that the described Doped Rare Earth metal organic salt that needs is: acetic acid samarium, acetic acid holmium, acetic acid yttrium or acetylacetone,2,4-pentanedione zirconium.
3. raising used for coating conductor CeO according to claim 1
2The method of film thickness is characterized in that the metal substrate of described biaxial texture is: the Ni+5%W alloy.
4. raising used for coating conductor CeO according to claim 1
2The method of film thickness, it is characterized in that described step a is: it is even and transparent that the mixed solution of propionic acid, isopropyl alcohol and the acetylacetone,2,4-pentanedione of cerous acetate is stirred to solution 60～80 ℃ of heating, after adding needs the Doped Rare Earth metal organic salt, continue to add thermal agitation at 100～120 ℃ again, get evenly and transparent up to solution becomes.
5. raising used for coating conductor CeO according to claim 1
2The method of film thickness is characterized in that among the above-mentioned steps c, as formula R E
xCe
1-xO
2-δIn x=0.5 the time, its annealing temperature is 1000 ℃; And when x＜0.5, its annealing temperature is 900 ℃; And 180 ℃ and the 600 ℃ stops that 15 minutes and 30 minutes are arranged respectively, heating rate is 10 ℃/min in the annealing process.
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|---|---|---|---|---|
| CN101281806B (en) * | 2008-06-04 | 2010-07-28 | 西南交通大学 | Method for preparing high temperature superconduction coating conductor buffer layer using polymer auxiliary deposition |
| CN102241526B (en) * | 2011-03-31 | 2012-09-26 | 西北有色金属研究院 | Preparation method of high temperature superconductive coating conductor buffer layer |
| CN103008210B (en) * | 2012-12-11 | 2014-08-20 | 电子科技大学 | Planarization method for high-temperature superconducting coated conductor substrate |
| CN104538113B (en) * | 2014-12-04 | 2017-12-19 | 江苏亨通光电股份有限公司 | Superconducting coating Y2Ce2O7The preparation method of transition layer film |
| CN105130428B (en) * | 2015-07-13 | 2019-10-25 | 西安理工大学 | A kind of Ce1-xZrxO2Buffer layer and preparation method thereof |
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