CN101337828B - Method for preparing pyrochlore type Nd2Mo2O7 cushioning layer - Google Patents
Method for preparing pyrochlore type Nd2Mo2O7 cushioning layer Download PDFInfo
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- CN101337828B CN101337828B CN2008101507412A CN200810150741A CN101337828B CN 101337828 B CN101337828 B CN 101337828B CN 2008101507412 A CN2008101507412 A CN 2008101507412A CN 200810150741 A CN200810150741 A CN 200810150741A CN 101337828 B CN101337828 B CN 101337828B
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Abstract
The invention discloses a method for preparing pyrochlor-type Nd2Mo2O7 buffer layer. In the method, solid neodymium acetylacetonate and molybdenum acetylacetonate of certain mol ratio are added to the mixed solution of propanoic acid and methanol; after the solid neodymium acetylacetonate and molybdenum acetylacetonate are dissolved, precursor solution is prepared; the precursor solution is spin coated on a YSZ single crystal base sheet before the spin coated YSZ single crystal base sheet is dried in air in an oven; subsequently, the YSZ single crystal base sheet is heated at the room temperature in argon gas in a pipe heater; finally, the spin coated single crystal base sheet is cooled to the room temperature at the cooling rate of not less than 2 DEG C per minute, thus preparing the Nd2Mo2O7 buffer layer. The Nd2Mo2O7 prepared has good film texture. The Nd2Mo2O7 buffer layer prepared by adopting the method has the characteristics of small roughness of surface, and good grain orientation of the surface coat. The method is highly repetitive. As the antivacuum chemical solution sediment technology is adopted, the preparation cost can be significantly reduced, and the method is applicable for mass production.
Description
Technical field
The present invention relates to a kind of preparation method of used for coating conductor impact plies, be specifically related to a kind of YBCO used for coating conductor pyrochlore-type Nd
2Mo
2O
7The preparation method of impact plies.
Background technology
Coating conductor has higher critical current density with respect to Bi-2223/Ag first-generation belt material of high temperature superconduct under High-Field, be the unique selection of preparation liquid nitrogen temperature high field magnet, and is therefore more competitive.Various countries are making great efforts to research and develop a kind of coating conductor that on flexible base band, is coated with the YBCO thick film at present.This coating conductor generally is to be made up of metal base band, impact plies, YBCO superconducting layer and resist.Impact plies is wherein being born transmission texture and chemical barrier two main tasks.What research was more at present is non-conductivity type buffer layer.In recent years, the impact plies technology also appears by multilayered structure to single layer structure, by the development trend of multiple deposition technique combination to single deposition technique.
Because Nd
2Mo
2O
7Good with NiW base band and YBCO lattice match, and have electroconductibility preferably, therefore can be used as the oriented growth of a kind of conductivity type buffer layer control YBCO.
At present both at home and abroad about Nd
2Mo
2O
7Research mainly concentrate the extraordinary Hall effect and the resistance of single crystal samples to frustrate the spin structure aspect, adopt the floating region single crystal growing furnace to prepare sample usually.About utilizing antivacuum metal organic deposit (being MOD) technology preparation Nd
2Mo
2O
7Result of study as coating conductor buffer layer is not appeared in the newspapers.
Summary of the invention
The objective of the invention is the deficiency that above-mentioned prior art exists, provide that a kind of cost is low, the pyrochlore-type Nd of good process repeatability
2Mo
2O
7The preparation method of impact plies is to prepare the Nd that texture is good, surfaceness is little and grain orientation is good
2Mo
2O
7Film.
To achieve these goals, the technical scheme of the present invention's employing is: a kind of pyrochlore-type Nd
2Mo
2O
7The preparation method of impact plies is characterized in that the preparation process is:
(1) with methyl ethyl diketone neodymium and acetyl acetone solid according to 1: 1 mixed of mol ratio;
(2) add propionic acid and methanol mixed solution in the mixture of step (1), the mol ratio of propionic acid and methyl alcohol is 2: 3, then the heated and stirred precursor liquid that to process flaxen total cation concentration in 1 hour be the 0.2-0.6 mol;
(3) with centrifugal spin coater the precursor liquid in the step (2) is spun on the YSZ single-crystal substrate with the acetone ultrasonic cleaning, said YSZ representes the zirconium white that yttrium is stable;
(4) the good YSZ single-crystal substrate of spin coating in the step (3) is placed baking oven; Dry in air atmosphere, then dried YSZ single-crystal substrate is placed tube furnace, the temperature rise rate with 7 ℃/minute under argon gas atmosphere begins heating from room temperature; Predecomposition under 550 ℃ of conditions of temperature; Under 900-1150 ℃ temperature constant temperature 1-3 hour then, with the rate of cooling that is not less than 2 ℃/minute the YSZ single-crystal substrate is cooled to room temperature at last, promptly process Nd
2Mo
2O
7Impact plies.
The rotating speed of centrifugal spin coater is 3000 rev/mins described in the above-mentioned steps (3), and the said spin coating time was 30 seconds.
Temperature of oven is 60 ℃ described in the above-mentioned steps (4).
Be 48 hours time of drying described in the above-mentioned steps (4).
The time of predecomposition described in the above-mentioned steps (4) is 1 hour.
The present invention has adopted a kind of antivacuum metal organic deposit (MOD) method to prepare Nd
2Mo
2O
7Impact plies.Discover that to of the present invention after employing methyl ethyl diketone neodymium and acetyl acetone solid were mixed with the precursor liquid spin coating as precursor, wet film carried out high-temperature heat treatment after the drying in 60 ℃ baking oven, can prepare the Nd of texture
2Mo
2O
7Film and show no hallrcuts and do not have hole even curface characteristic.
The present invention has the following advantages: the present invention adopts methyl ethyl diketone neodymium and acetyl acetone solid to make precursor, adopt metal organic deposit method with 550 ℃ as the predecomposition temperature, make that precursor decomposes as far as possible simultaneously, crystallization, the Nd for preparing
2Mo
2O
7Film texture is good; Adopt the Nd of this method preparation
2Mo
2O
7Impact plies has the little and good characteristics of upper layer grain orientation of surfaceness, and this method good reproducibility owing to adopt antivacuum chemical solution spin coating technique, therefore can significantly reduce preparation cost.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1
Methyl ethyl diketone neodymium and acetyl acetone solid are packed into after according to 1: 1 mixed of mol ratio in the beaker; In beaker, add propionic acid again: the mol ratio of methyl alcohol is 2: 3 propionic acid and a methanol mixed solution, the precursor liquid that it is 0.2 mol that heated and stirred was processed flaxen total cation concentration in 1 hour.The speed of precursor liquid being changeed with PM 3000 with centrifugal spin coater is spun on the YSZ single-crystal substrate with the acetone ultrasonic cleaning; The spin coating time was 30 seconds, and the substrate that spin coating is good places 60 ℃ baking oven, and drying is 48 hours in air atmosphere; Then dried YSZ single-crystal substrate is placed tube furnace; Under argon gas atmosphere with the heating of 7 ℃/minute temperature rise rate, 550 ℃ of following predecomposition 1 hour, then 1150 ℃ of following constant temperature 3 hours; Last rate of cooling with 2 ℃/minute is cooled to room temperature with the YSZ single-crystal substrate, has just made the Nd with good c axle texture and less surfaceness
2Mo
2O
7Impact plies.
Embodiment 2
With methyl ethyl diketone neodymium and acetyl acetone solid according to 1: 1 mixed of mol ratio; Add propionic acid: the mol ratio of methyl alcohol is 2: 3 propionic acid and a methanol mixed solution, the precursor liquid that it is 0.3 mol that heated and stirred was processed flaxen total cation concentration in 1 hour.The speed of precursor liquid being changeed with PM 3000 with centrifugal spin coater is spun on the YSZ single-crystal substrate with the acetone ultrasonic cleaning; The spin coating time was 30 seconds, and the substrate that spin coating is good places 60 ℃ baking oven, and drying is 48 hours in air atmosphere; Then dried YSZ single-crystal substrate is placed tube furnace; Under argon gas atmosphere with the heating of 7 ℃/minute temperature rise rate, 550 ℃ of following predecomposition 1 hour, then 1000 ℃ of following constant temperature 3 hours; Last rate of cooling with 2 ℃/minute is cooled to room temperature with the YSZ single-crystal substrate, has just made the Nd with good c axle texture and less surfaceness
2Mo
2O
7Impact plies.
Embodiment 3
With methyl ethyl diketone neodymium and acetyl acetone solid according to 1: 1 mixed of mol ratio; Add propionic acid: the mol ratio of methyl alcohol is 2: 3 propionic acid and a methanol mixed solution, the precursor liquid that it is 0.4 mol that heated and stirred was processed flaxen total cation concentration in 1 hour.The speed of precursor liquid being changeed with PM 3000 with centrifugal spin coater is spun on the YSZ single-crystal substrate with the acetone ultrasonic cleaning; The spin coating time was 30 seconds, and the substrate that spin coating is good places 60 ℃ baking oven, and drying is 48 hours in air atmosphere; Then dried YSZ single-crystal substrate is placed tube furnace; Under argon gas atmosphere with the heating of 7 ℃/minute temperature rise rate, 550 ℃ of following predecomposition 1 hour, then 900 ℃ of following constant temperature 3 hours; Last rate of cooling with 2 ℃/minute is cooled to room temperature with the YSZ single-crystal substrate, has just made the Nd with good c axle texture and less surfaceness
2Mo
2O
7Impact plies.
Embodiment 4
With methyl ethyl diketone neodymium and acetyl acetone solid according to 1: 1 mixed of mol ratio; Add propionic acid: the mol ratio of methyl alcohol is 2: 3 propionic acid and a methanol mixed solution, the precursor liquid that it is 0.5 mol that heated and stirred was processed flaxen total cation concentration in 1 hour.The speed of precursor liquid being changeed with PM 3000 with centrifugal spin coater is spun on the YSZ single-crystal substrate with the acetone ultrasonic cleaning; The spin coating time was 30 seconds, and the substrate that spin coating is good places 60 ℃ baking oven, and drying is 48 hours in air atmosphere; Then dried YSZ single-crystal substrate is placed tube furnace; Under argon gas atmosphere with the heating of 7 ℃/minute temperature rise rate, 550 ℃ of following predecomposition 1 hour, then 1000 ℃ of following constant temperature 2 hours; Last rate of cooling with 2 ℃/minute is cooled to room temperature with the YSZ single-crystal substrate, has just made the Nd with good c axle texture and less surfaceness
2Mo
2O
7Impact plies.
Embodiment 5
With methyl ethyl diketone neodymium and acetyl acetone solid according to 1: 1 mixed of mol ratio; Add propionic acid: the mol ratio of methyl alcohol is 2: 3 propionic acid and a methanol mixed solution, the precursor liquid that it is 0.6 mol that heated and stirred was processed flaxen total cation concentration in 1 hour.The speed of precursor liquid being changeed with PM 3000 with centrifugal spin coater is spun on the YSZ single-crystal substrate with the acetone ultrasonic cleaning; The spin coating time was 30 seconds, and the substrate that spin coating is good places 60 ℃ baking oven, and drying is 48 hours in air atmosphere; Then dried YSZ single-crystal substrate is placed tube furnace; Under argon gas atmosphere with the heating of 7 ℃/minute temperature rise rate, 550 ℃ of following predecomposition 1 hour, then 1000 ℃ of following constant temperature 1 hour; Last rate of cooling with 2 ℃/minute is cooled to room temperature with the YSZ single-crystal substrate, has just made the Nd with good c axle texture and less surfaceness
2Mo
2O
7Impact plies.
Explanation of nouns: above-mentioned YSZ representes the zirconium white that yttrium is stable.
Claims (1)
1. pyrochlore-type Nd
2Mo
2O
7The preparation method of impact plies is characterized in that the preparation process is:
(1) with methyl ethyl diketone neodymium and acetyl acetone solid according to 1: 1 mixed of mol ratio;
(2) add propionic acid and methanol mixed solution in the mixture of step (1), the mol ratio of propionic acid and methyl alcohol is 2: 3, then the heated and stirred precursor liquid that to process flaxen total cation concentration in 1 hour be the 0.2-0.6 mol;
(3) with centrifugal spin coater the precursor liquid in the step (2) is spun on the YSZ single-crystal substrate with the acetone ultrasonic cleaning, said YSZ representes the zirconium white that yttrium is stable; The rotating speed of said centrifugal spin coater is 3000 rev/mins, and the said spin coating time was 30 seconds;
(4) the good YSZ single-crystal substrate of spin coating in the step (3) is placed baking oven; Said temperature of oven is 60 ℃; Drying is 48 hours in air atmosphere, then dried YSZ single-crystal substrate is placed tube furnace, and the temperature rise rate with 7 ℃/minute under argon gas atmosphere begins heating from room temperature; Predecomposition is 1 hour under 550 ℃ of conditions of temperature; Under 900-1150 ℃ temperature constant temperature 1-3 hour then, with the rate of cooling that is not less than 2 ℃/minute the YSZ single-crystal substrate is cooled to room temperature at last, promptly process Nd
2Mo
2O
7Impact plies.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101507412A CN101337828B (en) | 2008-08-28 | 2008-08-28 | Method for preparing pyrochlore type Nd2Mo2O7 cushioning layer |
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|---|---|---|---|
| CN2008101507412A CN101337828B (en) | 2008-08-28 | 2008-08-28 | Method for preparing pyrochlore type Nd2Mo2O7 cushioning layer |
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| CN101337828B true CN101337828B (en) | 2012-02-29 |
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