CN103498140B - A kind of preparation method of nanometer silver doped cerium oxide coating - Google Patents
A kind of preparation method of nanometer silver doped cerium oxide coating Download PDFInfo
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- CN103498140B CN103498140B CN201310422222.8A CN201310422222A CN103498140B CN 103498140 B CN103498140 B CN 103498140B CN 201310422222 A CN201310422222 A CN 201310422222A CN 103498140 B CN103498140 B CN 103498140B
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Abstract
The invention discloses a kind of preparation method of nanometer silver doped cerium oxide coating, the method is: one, organic cerium salt is dissolved in propionic acid, then adds nano silver particles, preparation precursor liquid; Two, adopt spin-coating method to be coated in substrate by precursor liquid, be placed in tube furnace, under reducing atmosphere, being warming up to in-furnace temperature is 850 DEG C ~ 950 DEG C, and is incubated 0.5h ~ 1h, furnace cooling, obtains nanometer silver doped cerium oxide coating.The present invention by introducing nano silver particles in precursor liquid, the nano silver particles of dispersion can be formed with efficacy release center in cerium oxide, the stress equilibrium release in one-tenth phase thinning process of accelerating oxidation cerium coating, avoid the formation of crackle and hole, reduce the roughness on ceria film surface.The cerium oxide adopting method of the present invention to prepare has sharp keen biaxial texture, and smooth surface is smooth, flawless, is conducive to epitaxy superconducting layer.
Description
Technical field
The invention belongs to high temperature superconducting materia technical field, be specifically related to a kind of preparation method of nanometer silver doped cerium oxide coating.
Background technology
The multilayer materials that YBCO coating conductor is made up of metal base band/buffer layer/superconducting layer/protective layer.Owing to there is very large lattice mismatch (about 8%) and serious atomic diffusion between superconducting layer and metal base band, therefore must buffer layer between, just can reach the effect of transmitting texture and intercepting diffusion, realize the texture growing of YBCO superconducting layer, obtain high current capacity simultaneously.Cerium oxide (CeO
2) owing to having the advantages such as high, little and good with the lattice mismatch of the YBCO chemical compatibility of thermostability, be considered to a kind of extremely important cushioning layer material.
CeO
2belong to cubic fluorite structure, control the YBCO superconducting layer that its oriented growth and surface quality have texture for epitaxy very important.CeO prepared by chemical solution deposition
2coating has the advantages such as technique is simple, low cost, and be the focus of research at present, people pass through at CeO
2adulterate in layer various rare earth element, improves CeO further
2the texture orientation of layer and surface quality.Suo Hong jasmine seminar by introducing the transition metals (CN102173801B, CN101219896B) such as the rare earth elements such as La, Gd (CN101624286B, CN101597162B) and Ta, Zr in cerium oxide precursor liquid, can prepare do not have crackle, surfacing fine and close, there is more highly-textured cerium oxide transition layer.But these methods generally all need to heat-treat oxide coating at higher temperature (1000 DEG C ~ 1200 DEG C), this situation can cause NiW metal substrate grain growth, heat etching grooves deepen, must cause grain boundaries to occur discontinuity zone, and cerium oxide surfaceness increases.Doping simultaneously in these situations, does not have nano dot in cerium oxide cured film, and cured film does not exist effective stress relief center in decomposition with becoming in phase process, is unfavorable for the stress relief of thick film.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method of nanometer silver doped cerium oxide coating.The method by introducing nano silver particles in precursor liquid, the nano silver particles of dispersion can be formed with efficacy release center in cerium oxide, the stress equilibrium release in one-tenth phase thinning process of accelerating oxidation cerium coating, avoid cerium oxide to form crackle and hole in thinning, contraction process, reduce the roughness on ceria film surface; Grown by the induced nucleation of nanometer silver, ceria film can be helped to become phase at lesser temps, reduce conventional high-temperature thermal treatment to the impact of metal base band, avoid metal substrate grain growth and heat etching ditch under high temperature to deepen the destruction to cerium oxide, improve the surface quality of coating.The cerium oxide adopting the method to prepare has sharp keen biaxial texture, and smooth surface is smooth, flawless, is conducive to epitaxy superconducting layer.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of nanometer silver doped cerium oxide coating, and it is characterized in that, the method comprises the following steps:
Step one, organic cerium salt is dissolved in propionic acid, then adds nano silver particles, be mixed with the precursor liquid that cerium ion concentration is 0.2mol/L ~ 1mol/L; In described precursor liquid, the molar weight of nano silver particles is 0.05% ~ 1% of cerium ion molar weight;
Precursor liquid described in step one is coated in substrate by step 2, employing spin-coating method, then the substrate being coated with precursor liquid is placed in tube furnace, under reducing atmosphere, with the temperature rise rate of 20 DEG C/min ~ 100 DEG C/min, in-furnace temperature is risen to 850 DEG C ~ 950 DEG C, and be incubated 0.5h ~ 1h, furnace cooling, obtains nanometer silver doped cerium oxide coating; Described substrate is NiW substrate or NiW/La
2zr
2o
7substrate.
The preparation method of above-mentioned a kind of nanometer silver doped cerium oxide coating, the salt of organic cerium described in step one is propionic acid cerium or methyl ethyl diketone cerium.
The preparation method of above-mentioned a kind of nanometer silver doped cerium oxide coating, described in step one, nano silver particles is of a size of 5nm ~ 20nm.
The preparation method of above-mentioned a kind of nanometer silver doped cerium oxide coating, in precursor liquid described in step one, the molar weight of nano silver particles is 0.5% of cerium ion molar weight.
The preparation method of above-mentioned a kind of nanometer silver doped cerium oxide coating, the rotating speed of spin coating described in step 2 is 500rpm ~ 4000rpm, and spin-coating time is 30s ~ 180s.
The preparation method of above-mentioned a kind of nanometer silver doped cerium oxide coating, reducing atmosphere described in step 2 is the mixed atmosphere of argon gas and hydrogen, and in mixed atmosphere, the volumn concentration of hydrogen is 2% ~ 8%.
The present invention compared with prior art has the following advantages:
1, the present invention by introducing nano silver particles in precursor liquid, the nano silver particles of dispersion can be formed with efficacy release center in cerium oxide, the stress equilibrium release in one-tenth phase thinning process of accelerating oxidation cerium coating, avoid cerium oxide to form crackle and hole in thinning, contraction process, reduce the roughness on ceria film surface.
2, the present invention is grown by the induced nucleation of nanometer silver, ceria film can be helped to become phase at lesser temps, reduce conventional high-temperature thermal treatment to the impact of NiW metal base band, avoid metal substrate grain growth and heat etching ditch under high temperature to deepen the destruction to cerium oxide, improve the surface quality of coating.
3, the cerium oxide that prepared by the present invention has sharp keen biaxial texture, and smooth surface is smooth, flawless, is conducive to epitaxy superconducting layer.
4, at nanometer silver doped cerium oxide coatingsurface epitaxy YBCO superconducting layer prepared by the present invention, the superconducting layer obtained has good superconductivity, and 77K is greater than 2MA/cm from critical current density after the match
2.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction θ-2 θ scintigram of nanometer silver doped cerium oxide coating prepared by the embodiment of the present invention 1.
Fig. 2 is face interscan (Phi scan) figure at nanometer silver doped cerium oxide coating (111) peak prepared by the embodiment of the present invention 1.
Fig. 3 is atomic force microscope (AFM) figure of nanometer silver doped cerium oxide coating morphology prepared by the embodiment of the present invention 1.
Fig. 4 is X diffraction θ-2 θ scintigram of the YBCO superconducting layer prepared in the nanometer silver doped cerium oxide coating of the embodiment of the present invention 1.
Fig. 5 is scanning electron microscope (SEM) figure of nanometer silver doped cerium oxide coating morphology prepared by the embodiment of the present invention 3.
Fig. 6 is X diffraction θ-2 θ scintigram of the YBCO superconducting layer prepared in the nanometer silver doped cerium oxide coating of the embodiment of the present invention 3.
Fig. 7 is X-ray diffraction θ-2 θ scintigram of nanometer silver doped cerium oxide coating prepared by the embodiment of the present invention 5.
Fig. 8 be the embodiment of the present invention 5 prepare nanometer silver doped cerium oxide coating (002) peak face outside scan (Omega scan) figure.
Fig. 9 is scanning electron microscope (SEM) figure of the YBCO superconducting layer surface pattern prepared in the nanometer silver doped cerium oxide coating of the embodiment of the present invention 5.
Embodiment
Embodiment 1
Step one, methyl ethyl diketone cerium (or propionic acid cerium) is dissolved in propionic acid, then adds the nano silver particles being of a size of 5nm, be mixed with the precursor liquid that cerium ion concentration is 0.2mol/L; In described precursor liquid, the molar weight of nano silver particles is 0.5% of cerium ion molar weight;
Step 2, employing spin-coating method, be coated on NiW/La with the rotating speed of 4000rpm by precursor liquid described in step one
2zr
2o
7in substrate, coating time is 30s, is then placed in tube furnace, in the mixed atmosphere of argon gas and hydrogen, with the temperature rise rate of 100 DEG C/min, in-furnace temperature is risen to 950 DEG C, and is incubated 0.5h, furnace cooling, obtain nanometer silver doped cerium oxide coating; In described mixed atmosphere, the volumn concentration of hydrogen is 8%.
Fig. 1 is x diffraction θ-2 θ scintigram of nanometer silver doped cerium oxide coating prepared by the present embodiment, and the nanometer silver doped cerium oxide coating as can be seen from the figure prepared has CeO
2(002) peak, and there is no (111) dephasign peak, show sharp keen cubic texture.Fig. 2 is face interscan (Phi scan) figure at nanometer silver doped cerium oxide coating (111) peak prepared by the present embodiment, as can be seen from the figure, occur 4 peaks in whole sweep limit, and the halfwidth at peak is 6.1 degree, display coating has sharp keen biaxial texture.Fig. 3 is atomic force microscope (AFM) figure of nanometer silver doped cerium oxide coating morphology prepared by the present embodiment, as can be seen from the figure, cerium oxide uniform crystal particles, surfaceness is 3nm, fine and close and the flawless of smooth surface, illustrates that the silver adulterated facilitates homogeneous nucleation and the growth of cerium oxide layer.Fig. 4 be adopt ordinary method to prepare at the present embodiment nanometer silver doped cerium oxide coating on prepare x diffraction θ-2 θ scintigram of YBCO superconducting layer, as can be seen from the figure, YBCO superconducting layer has sharp keen (00l) orientation peak and not assorted peak, display YBCO coating has good extension texture, and the critical current density of this sample at 77K temperature is 2.6MA/cm
2, show good superconductivity.
The cerium oxide of doping 0.5%Ag prepared by the present embodiment has sharp keen biaxial texture, and surfacing and non-microcracked and hole, and heat etching groove can be avoided the destruction of coating, and surfaceness is 3nm; The nano silver particles of doping improves texture orientation and the surface quality of cerium oxide effectively.YBCO superconducting layer prepared by dopen Nano silver particles cerium oxide layer shows excellent superconductivity, significantly improves the critical current density of superconducting layer.
Embodiment 2
The present embodiment is identical with embodiment 1, and wherein difference is: described substrate is NiW substrate.
The cerium oxide of doping 0.5%Ag prepared by the present embodiment has sharp keen biaxial texture, and surfacing and non-microcracked and hole, and heat etching groove can be avoided the destruction of coating, and surfaceness is 3nm; The nano silver particles of doping improves texture orientation and the surface quality of cerium oxide effectively.YBCO superconducting layer prepared by dopen Nano silver particles cerium oxide layer shows excellent superconductivity, significantly improves the critical current density of superconducting layer.
Embodiment 3
Step one, propionic acid cerium (or methyl ethyl diketone cerium) is dissolved in propionic acid, then adds the nano silver particles being of a size of 20nm, be mixed with the precursor liquid that cerium ion concentration is 0.5mol/L; In described precursor liquid, the molar weight of nano silver particles is 0.05% of cerium ion molar weight;
Step 2, employing spin-coating method, be coated on NiW/La with the rotating speed of 2000rpm by precursor liquid described in step one
2zr
2o
7in substrate, coating time is 90s, is then placed in tube furnace, in the mixed atmosphere of argon gas and hydrogen, with the temperature rise rate of 50 DEG C/min, in-furnace temperature is risen to 900 DEG C, and is incubated 0.7h, furnace cooling, obtain nanometer silver doped cerium oxide coating; In described mixed atmosphere, the volumn concentration of hydrogen is 4%.
Fig. 5 is scanning electron microscope (SEM) figure of nanometer silver doped cerium oxide coating morphology prepared by the present embodiment, as can be seen from the figure, and smooth and the non-microcracked and hole of nanometer silver doped cerium oxide coatingsurface, and heat etching groove can be avoided the destruction of coating.Fig. 6 be adopt ordinary method to prepare at the present embodiment nanometer silver doped cerium oxide coating on prepare x diffraction θ-2 θ scintigram of YBCO superconducting layer, as can be seen from the figure, YBCO superconducting layer has sharp keen (00l) orientation peak, have good extension texture, the critical current density of this sample at 77K temperature is 2.3MA/cm
2, show good superconductivity.
The cerium oxide of doping 0.05%Ag prepared by the present embodiment has sharp keen biaxial texture, and surfacing and non-microcracked and hole, and heat etching groove can be avoided the destruction of coating, and surfaceness is less than 5nm; The nano silver particles of doping improves texture orientation and the surface quality of cerium oxide effectively.YBCO superconducting layer prepared by dopen Nano silver particles cerium oxide layer shows excellent superconductivity, significantly improves the critical current density of superconducting layer.
Embodiment 4
The present embodiment is identical with embodiment 3, and wherein difference is: described substrate is NiW substrate.
The cerium oxide of doping 0.05%Ag prepared by the present embodiment has sharp keen biaxial texture, and surfacing and non-microcracked and hole, and heat etching groove can be avoided the destruction of coating, and surfaceness is less than 5nm; The nano silver particles of doping improves texture orientation and the surface quality of cerium oxide effectively.YBCO superconducting layer prepared by dopen Nano silver particles cerium oxide layer shows excellent superconductivity, significantly improves the critical current density of superconducting layer.
Embodiment 5
Step one, methyl ethyl diketone cerium (or propionic acid cerium) is dissolved in propionic acid, then adds the nano silver particles being of a size of 10nm, be mixed with the precursor liquid that cerium ion concentration is 1mol/L; In described precursor liquid, the molar weight of nano silver particles is 1% of cerium ion molar weight;
Step 2, employing spin-coating method, with the rotating speed of 500rpm, precursor liquid described in step one is coated in NiW substrate, coating time is 180s, then tube furnace is placed in, in the mixed atmosphere of argon gas and hydrogen, with the temperature rise rate of 20 DEG C/min, in-furnace temperature is risen to 850 DEG C, and be incubated 1h, furnace cooling, obtains nanometer silver doped cerium oxide coating; In described mixed atmosphere, the volumn concentration of hydrogen is 2%.
Fig. 7 is X-ray diffraction θ-2 θ scintigram of nanometer silver doped cerium oxide coating prepared by the present embodiment.As can be seen from the figure, CeO is only had
2(002) peak, shows sharp keen cubic texture.Fig. 8 be nanometer silver doped cerium oxide coating (002) peak prepared by the present embodiment face outside scan (Omega scan) figure, as can be seen from the figure, scanning halfwidth outside its face is 5.1 degree, display there is good diaxial orientation.Fig. 9 be adopt Typical physical method to prepare at the present embodiment nanometer silver doped cerium oxide coating on prepare scanning electron microscope (SEM) figure of the surface topography of YBCO superconducting layer, as can be seen from the figure, the smooth densification of YBCO superconducting layer surface, the critical current density of this sample at 77K temperature is 2.1MA/cm
2, show good superconductivity.
The cerium oxide of doping 1%Ag prepared by the present embodiment has sharp keen biaxial texture, and surfacing and non-microcracked and hole, and heat etching groove can be avoided the destruction of coating, and surfaceness is less than 5nm; The nano silver particles of doping improves texture orientation and the surface quality of cerium oxide effectively.YBCO superconducting layer prepared by dopen Nano silver particles cerium oxide layer shows excellent superconductivity, significantly improves the critical current density of superconducting layer.
Embodiment 6
The present embodiment is identical with embodiment 5, and wherein difference is: described substrate is NiW/La
2zr
2o
7substrate.
The cerium oxide of doping 1%Ag prepared by the present embodiment has sharp keen biaxial texture, and surfacing and non-microcracked and hole, and heat etching groove can be avoided the destruction of coating, and surfaceness is less than 5nm; The nano silver particles of doping improves texture orientation and the surface quality of cerium oxide effectively.YBCO superconducting layer prepared by dopen Nano silver particles cerium oxide layer shows excellent superconductivity, significantly improves the critical current density of superconducting layer
The above; it is only preferred embodiment of the present invention; not any restriction is done to the present invention, every above embodiment is done according to invention technical spirit any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (5)
1. a preparation method for nanometer silver doped cerium oxide coating, is characterized in that, the method comprises the following steps:
Step one, organic cerium salt is dissolved in propionic acid, then adds nano silver particles, be mixed with the precursor liquid that cerium ion concentration is 0.2mol/L ~ 1mol/L; In described precursor liquid, the molar weight of nano silver particles is 0.05% ~ 1% of cerium ion molar weight;
Precursor liquid described in step one is coated in substrate by step 2, employing spin-coating method, then the substrate being coated with precursor liquid is placed in tube furnace, under reducing atmosphere, with the temperature rise rate of 20 DEG C/min ~ 100 DEG C/min, in-furnace temperature is risen to 850 DEG C ~ 950 DEG C, and be incubated 0.5h ~ 1h, furnace cooling, obtains nanometer silver doped cerium oxide coating; Described substrate is NiW substrate or NiW/La
2zr
2o
7substrate;
The salt of organic cerium described in step one is propionic acid cerium or methyl ethyl diketone cerium.
2. the preparation method of a kind of nanometer silver doped cerium oxide coating according to claim 1, it is characterized in that, described in step one, nano silver particles is of a size of 5nm ~ 20nm.
3. the preparation method of a kind of nanometer silver doped cerium oxide coating according to claim 1, it is characterized in that, in precursor liquid described in step one, the molar weight of nano silver particles is 0.5% of cerium ion molar weight.
4. the preparation method of a kind of nanometer silver doped cerium oxide coating according to claim 1, is characterized in that, the rotating speed of spin coating described in step 2 is 500rpm ~ 4000rpm, and spin-coating time is 30s ~ 180s.
5. the preparation method of a kind of nanometer silver doped cerium oxide coating according to claim 1, it is characterized in that, reducing atmosphere described in step 2 is the mixed atmosphere of argon gas and hydrogen, and in mixed atmosphere, the volumn concentration of hydrogen is 2% ~ 8%.
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| CN101597162A (en) * | 2009-07-03 | 2009-12-09 | 北京工业大学 | A kind of Gd doped Ce O 2Transition layer film and preparation method thereof |
| CN101624286A (en) * | 2009-07-03 | 2010-01-13 | 北京工业大学 | La -CeO2 doped transition layer film and preparation method thereof |
| CN102173801A (en) * | 2011-01-20 | 2011-09-07 | 北京工业大学 | Ta doped CeO2 depletion layer film and preparation method thereof |
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2013
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597162A (en) * | 2009-07-03 | 2009-12-09 | 北京工业大学 | A kind of Gd doped Ce O 2Transition layer film and preparation method thereof |
| CN101624286A (en) * | 2009-07-03 | 2010-01-13 | 北京工业大学 | La -CeO2 doped transition layer film and preparation method thereof |
| CN102173801A (en) * | 2011-01-20 | 2011-09-07 | 北京工业大学 | Ta doped CeO2 depletion layer film and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| "Use of cerium ethylhexanoate solutions for preparation of CeO2 buffer layers by spin coating";S. Morlens 等;《Materials Science and Engineering》;20031115;第104卷(第3期);第185-191页 * |
| "溶胶-凝胶法制备Y系涂层导体隔离层";刘慧舟 等;《低温物理学报》;20031031;第25卷;第129-133页 * |
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