CN1447451A - Method for preparing high temperature superconductor thick film of Ba/YCu with large area by using electrophoresis technique - Google Patents
Method for preparing high temperature superconductor thick film of Ba/YCu with large area by using electrophoresis technique Download PDFInfo
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- CN1447451A CN1447451A CN02116324.3A CN02116324A CN1447451A CN 1447451 A CN1447451 A CN 1447451A CN 02116324 A CN02116324 A CN 02116324A CN 1447451 A CN1447451 A CN 1447451A
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- yba
- thick film
- film
- large area
- high temperature
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000001962 electrophoresis Methods 0.000 title claims abstract description 11
- 239000002887 superconductor Substances 0.000 title description 2
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims description 58
- BTGZYWWSOPEHMM-UHFFFAOYSA-N [O].[Cu].[Y].[Ba] Chemical compound [O].[Cu].[Y].[Ba] BTGZYWWSOPEHMM-UHFFFAOYSA-N 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims 1
- 238000004062 sedimentation Methods 0.000 claims 1
- 229910003097 YBa2Cu3O7−δ Inorganic materials 0.000 abstract 3
- 239000012530 fluid Substances 0.000 abstract 3
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 52
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 22
- 239000000395 magnesium oxide Substances 0.000 description 11
- 238000004549 pulsed laser deposition Methods 0.000 description 5
- 230000007704 transition Effects 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 239000013590 bulk material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A method includes following steps. (1) A metal layer is vaporized on the MgO monocrystal substrate. Then, the substrate is fixed on the negative electrode for stand by application. (2) YBa2Cu3O7-delta sintered is ground till the granularity of the powder is less than 0.1-10 micros. The powder is mixed with organic solvent in mixing ratio being as 20g/liter. The YBa2Cu3O7 delta electrophoresis fluid is prepared by stirring up the organic solvent making the fluid disperse evenly. (3) The YBa2Cu3O7-delta electrophoresis fluid and the electrode with the motorcrystal substrate are put to the cleaned electrophoresis pool. The even YBa2Cu3O7-delta film is obtained after 20-900V DC current being add to electrodes and 5-1600 seconds deposit time being kept.
Description
Technical field
The present invention relates to the preparation field of high temperature superconducting film, particularly relate to electrophoretic techniques and prepare large area high temperature superconductive barium-yttrium-copper oxide (YBa
2Cu
3O
7-δ) method of thick film.
Background technology
YBa
2Cu
3O
7-δSuperconducting film because its higher superconducting transition temperature, high critical current density are widely used in the microwave and the communications field, has irreplaceable status especially in microwave devices such as filter.Prepare YBa now
2Cu
3O
7-δFilm often adopts pulsed laser deposition (hereinafter to be referred as PLD) and magnetron sputtering method etc.The PLD method can grow the good YBa of superconductivity
2Cu
3O
7-δFilm, but its speed of growth can slow down slowly with the increase of rete area.And the preparation difficulty becomes big with the rete area and thickening increases sharply.In addition, the PLD method also needs expensive high-power excimer laser, as document 1:Preparation of Y-Ba-Cu oxide superconductor thin filmsusing pulsed laser evaporation from high Tc bulk material, Appl.Phys.Lett., 51, introduced in 619,1987.The another kind of magnetron sputtering method that adopts prepares YBa
2Cu
3O
7-δFilm is as document 2:Growth and characterization of a-axisoriented YBa
2Cu
3O
7-δThin films on (100) LaSrGaO
4Substrates, PhysicaC is introduced in 280,167,1997, the YBa of this method preparation
2Cu
3O
7-δThe film surface of film is very smooth, but forms reverse sputtering easily in preparation process, makes YBa
2Cu
3O
7-δThe quality of film descends.In addition, the evaporation rate of each element is different, and the composition of film is departed from.Therefore, through facts have proved that above method is not growth YBa
2Cu
3O
7-δThe Perfected process of superconducting thick-film.
Summary of the invention
Can grow the good YBa of superconductivity though the objective of the invention is to overcome the PLD method
2Cu
3O
7-δFilm, but its speed of growth can increase become slow with the rete area, and also the preparation difficulty is with shortcoming that the rete area becomes greatly and thickening increases sharply and the shortcoming that also needs expensive high-power excimer laser; In addition, also be to overcome the film of magnetron sputtering method in preparation process and form reverse sputtering easily, the quality of film is descended and the evaporation rate of each element different, the shortcoming that the composition of film is departed from; Reach for the area for preparing superconducting film in the size range of 5mm-200mm, realize YBa simultaneously again
2Cu
3O
7-δThe superconduction thickness is to 800nm-20 μ m, thereby provides a kind of employing electrophoretic techniques to prepare large tracts of land YBa
2Cu
3O
7-δThe method of thick film.
The present invention is achieved in that employing electrophoretic techniques provided by the invention prepares large tracts of land YBa
2Cu
3O
7-δThe method of thick film may further comprise the steps:
The first step is with the YBa that sinters in advance
2Cu
3O
7-δPowder fully grinds, and reaching granularity less than 0.1-10 μ m, otherwise can cause film inhomogeneous;
Second step, deposit layer of metal film with common evaporation earlier on the MgO single crystal substrates, this metal film comprises: Ag, and perhaps other does not destroy the metal of barium-yttrium-copper oxide superconductivity, for example: Pt, Au, Cu, Ir, Al, the film of materials such as Pd is fixed on this substrate that has plated film on the negative pole, is placed in the clean vessel standby;
In the 3rd step, get the prepared YBa of step 1
2Cu
3O
7-δPowder is pressed YBa
2Cu
3O
7-δPowder mixes with organic solvent, and its mixed proportion is the 2-40 grams per liter, and described organic solvent comprises: acetone, alcohol, chloroform or dichloroethylene, high-purity water or the like, all organic solvents can, stir then and make YBa
2Cu
3O
7-δIn organic solvent, be uniformly dispersed fully, be mixed with YBa
2Cu
3O
7-δElectrophoresis liquid;
The 4th step, the YBa that step 3 is prepared
2Cu
3O
7-δElectrophoresis liquid 4 is put into clean tiselius apparatus, stirs once more and makes it more even; The electrode that substrate is housed for preparing is prevented in the tiselius apparatus that positive and negative electrode connects a high-voltage DC power supply; The energising of the direct current of logical 20-900V on electrode, and maintenance then deposits 5-1600 second, deposition layer of even YBa on substrate
2Cu
3O
7-δFilm;
In the 5th step, step 5 has been deposited YBa
2Cu
3O
7-δFilm is placed in the sintering furnace, furnace temperature with the 300-400 degree/hour programming rate be raised to 1000-1106 ℃, and be incubated 30 minutes, then with 300 the degree/hour cooling rate reduce to 990 ℃, again with 1 the degree/hour speed reduce to 950 ℃, with 300 degree/hour cooling rate cool to room temperature, obtain being deposited on on-chip YBa at last
2Cu
3O
7-δThick film;
In order to obtain high T
C0, high J
cWell-crystallized, fine and close YBa
2Cu
3O
7-δThick film also comprises the 6th step: with YBa
2Cu
3O
7-δThick film is placed in the sintering furnace, and furnace temperature and charges into oxygen under keeping 300 ℃ to 400 ℃, the flow velocity of its oxygen be the 0.1-25 liter/minute, carry out after annealing and handle.
Described tiselius apparatus, as shown in Figure 1; Limit the size of electrode according to the size of required preparation thick film, positive and negative electrode (2,3) is by making with a kind of sheet metal strip, and positive and negative electrode is spaced apart 3-5cm, with negative pole 3 lower ends with the side has bent so that substrate can be fixed on the negative pole, insert in the tiselius apparatus together;
Described organic solvent purity is 99.99%.
Described metal material as electrode requires chemical property highly stable, and has certain pliability, as copper, silver, stainless steel etc.
Advantage of the present invention:
Employing electrophoretic techniques of the present invention prepares the method for large area high temperature superconductive barium-yttrium-copper oxide thick film, since the high deposition rate of electrophoresis, feasible growth YBa
2Cu
3O
7-δThe thickness of film increases rapidly, and the thickness of film controls easily, and the size of film is also unrestricted, so easy growth thick film; This method technology is simple, is particularly suitable for suitability for industrialized production; The thick film quality even compact of being grown, function admirable, cheap.
Description of drawings Fig. 1 is the tiselius apparatus structural representation
Drawing is described as follows: the anodal 3-negative pole of 1-high voltage source 2-4-electrophoresis liquid
Embodiment
Embodiment 1: prepare YBa on the MgO of 10mm * 10mm substrate
2Cu
3O
7-δSuperconducting thick-film.
What present embodiment used is the tiselius apparatus shown in Fig. 1, and the MgO substrate of 10mm * 10mm * 0.5mm is steamed last layer Ag in advance.The first step is with 2.45 gram YBa
2Cu
3O
7-δPowder, fully grinding makes its granularity less than 2 μ m, then with ground YBa
2Cu
3O
7-δPowder mixes with 125-1000 milliliter acetone (purity 99.99%), pours tiselius apparatus into after stirring with glass bar.Second step is with the positive and negative electrode of the argent of the long 5cm of the wide 1.5cm of thick 0.3mm cleaning as tiselius apparatus.The lower end of negative pole and side are bent with fixed substrate, and the MgO substrate that is coated with Ag is fixed on the negative pole.In the 3rd step, on electrode, add 900 volt direct currents and kept 10 minutes.On substrate, just deposited the thick YBa of the about 10 μ m of one deck
2Cu
3O
7-δFilm.In the 4th step, will deposit YBa
2Cu
3O
7-δBeing placed in the sintering furnace of film, furnace temperature with the 300-400 degree/hour programming rate be raised to 1106 ℃, and keep half an hour, then with 300 the degree/hour cooling rate reduce to 990 ℃, again with 1 the degree/hour speed reduce to 950 ℃, with 300 degree/hour cool to room temperature, be deposited on on-chip YBa so at last
2Cu
3O
7-δThe just preliminary preparation of thick film is finished.Also comprised for the 5th step, in oxygen, temperature keeps 400 ℃ to carry out the after annealing processing, and oxygen flow speed is 0.5 liter/minute, the YBa that obtains
2Cu
3O
7-δThe thick film even compact, superconducting transition temperature 91K, critical current density is 1.5 * 10
6A/cm
2Illustrate that this method obtains the large tracts of land YBa of function admirable
2Cu
3O
7-δThick film,, good reproducibility simple through this method of experiment confirm repeatedly.
Embodiment 2: prepare YBa on the big substrate of the MgO of 150mm * 150mm
2Cu
3O
7-δSuperconducting thick-film.
Present embodiment uses is tiselius apparatus among Fig. 1.Method is similar to Example 1, steams one deck Pt at the MgO substrate in advance.Tiselius apparatus is identical with embodiment 1, YBa
2Cu
3O
7-δPowder particle size is less than 0.5 μ m, electrophoresis solvent chloroform.The MgO substrate that is coated with Pt is fixed on the negative pole, is connected with 900 volts of voltages between the both positive and negative polarity, kept 30 minutes.On substrate, just deposited the thick YBa of the about 800nm of one deck
2Cu
3O
7-δFilm.To deposit YBa
2Cu
3O
7-δBeing placed in the sintering furnace of film, furnace temperature with the 300-400 degree/hour programming rate be raised to 1080 ℃, and keep half an hour, then with 300 the degree/hour cooling rate reduce to 990 ℃, again with 1 the degree/hour speed reduce to 950 ℃, at last with 300 degree/hour cool to room temperature, with this YBa
2Cu
3O
7-δThick film carries out after annealing in 350 ℃ of oxygen atmospheres handles, and oxygen flow speed is 20 liters/minute, the YBa that obtains
2Cu
3O
7-δThick film even compact, superconducting transition temperature are distributed between 85K and the 92K.
Embodiment 3: the ybco film of growing on the nickel sheet of texture, MgO makes separator.
The tiselius apparatus of present embodiment among Fig. 1.Method is similar to Example 1, and at first the fine and close magnesia film uniformly of preparation (by Chinese patent application number: NO.01110033.8 makes) steams last layer Al with the MgO substrate.Tiselius apparatus is identical with embodiment 1, YBa
2Cu
3O
7-δPowder particle size is less than 8 μ m.Al/MgO/Ni is fixed on the negative pole, is connected with 900 volts of voltages between the both positive and negative polarity, kept 10 minutes.On substrate, just deposited the thick YBa of the about 17 μ m of one deck
2Cu
3O
7-δTo deposit YBa
2Cu
3O
7-δBeing placed in the sintering furnace of film, furnace temperature with the 300-400 degree/hour programming rate be raised to 1050 ℃, and keep half an hour, then with 300 the degree/hour cooling rate reduce to 990 ℃, again with 1 the degree/hour speed reduce to 950 ℃, at last with 300 degree/hour cool to room temperature, with this YBa
2Cu
3O
7-δThick film carries out after annealing in 350 ℃ of oxygen atmospheres handles, and oxygen flow speed is 10 liters/minute, the YBa that obtains
2Cu
3O
7-δThe thick film even compact, superconducting transition temperature is distributed in 93K.Critical current density is 2.3 * 10
6A/cm
2
Claims (7)
1. adopt electrophoretic techniques to prepare the method for large area high temperature superconductive barium-yttrium-copper oxide thick film, it is characterized in that: may further comprise the steps:
The first step is with YBa
2Cu
3O
7-δPowder fully grinds, and reaches granularity less than 0.1-10 μ m;
Second step deposited layer of metal film with evaporation earlier on the MgO single crystal substrates, this substrate is fixed on the negative pole, was placed in the clean vessel standby;
In the 3rd step, get the prepared YBa of step 1
2Cu
3O
7-δPowder is pressed YBa
2Cu
3O
7-δPowder mixes for the 2-40 grams per liter with the organic solvent mixed proportion, mixes the back and stirs, and is mixed with YBa
2Cu
3O
7-δElectrophoresis liquid;
The 4th step, the YBa that step 3 is prepared
2Cu
3O
7-δElectrophoresis liquid 4 is put into clean tiselius apparatus with the electrode that substrate is housed, and stirs once more; The direct current of logical 20-900V deposits on the positive and negative electrode, and keeps energising sedimentation time 5-1600 second, deposition layer of even YBa on substrate
2Cu
3O
7-δFilm;
The 5th step, the YBa that step 4 deposition is good
2Cu
3O
7-δFilm is placed in the sintering furnace, furnace temperature with the 300-400 degree/hour programming rate be raised to 1000-1106 ℃, and be incubated 30 minutes, then with 300 the degree/hour cooling rate reduce to 990 ℃, again with 1 the degree/hour speed reduce to 950 ℃, with 300 degree/hour cool to room temperature, obtain being deposited on on-chip YBa at last
2Cu
3O
7-δThick film;
2. prepare the method for large area high temperature superconductive barium-yttrium-copper oxide thick film by the described employing electrophoretic techniques of claim 1, it is characterized in that: also comprise the YBa that the 5th step is obtained
2Cu
3O
7-δThick film is placed on and carries out after annealing in the sintering furnace and handle, and furnace temperature remains under 300 ℃ to 400 ℃, and charges into oxygen, the flow velocity of its oxygen be the 0.1-25 liter/minute.
3. by claim 1 or 2 described any methods that adopt electrophoretic techniques to prepare large area high temperature superconductive barium-yttrium-copper oxide thick film, it is characterized in that: the metal film that deposits on the described MgO single crystal substrates comprises Ag, Pt, Au, Cu, Ir, Al, Pd.
4. prepare the method for large area high temperature superconductive barium-yttrium-copper oxide thick film by claim 1 or 2 described any described employing electrophoretic techniquess, it is characterized in that: described organic solvent comprises: acetone, alcohol, chloroform, dichloroethylene or high-purity water
5. the method for preparing large area high temperature superconductive barium-yttrium-copper oxide thick film by each described employing electrophoretic techniques in claim 1 or 2, it is characterized in that: the electrode in the described tiselius apparatus limits the size of electrode according to the size of required preparation thick film, positive and negative electrode is by making with a kind of sheet metal strip, and positive and negative electrode is spaced apart 3-5cm.
6. prepare the method for large area high temperature superconductive barium-yttrium-copper oxide thick film by each described employing electrophoretic techniques in claim 1 or 2, it is characterized in that: described organic solvent purity is 99.99%.
7. the method for preparing large area high temperature superconductive barium-yttrium-copper oxide thick film by each described employing electrophoretic techniques in claim 1 or 2, it is characterized in that: it is highly stable that described metal material as electrode has chemical property, and have certain flexible copper, silver, stainless steel material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021163243A CN100373649C (en) | 2002-03-26 | 2002-03-26 | Method for preparing high temperature superconductor thick film of Ba/YCu with large area by using electrophoresis technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021163243A CN100373649C (en) | 2002-03-26 | 2002-03-26 | Method for preparing high temperature superconductor thick film of Ba/YCu with large area by using electrophoresis technique |
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| Publication Number | Publication Date |
|---|---|
| CN1447451A true CN1447451A (en) | 2003-10-08 |
| CN100373649C CN100373649C (en) | 2008-03-05 |
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|---|---|---|---|
| CNB021163243A Expired - Fee Related CN100373649C (en) | 2002-03-26 | 2002-03-26 | Method for preparing high temperature superconductor thick film of Ba/YCu with large area by using electrophoresis technique |
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Cited By (1)
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|---|---|---|---|---|
| CN107978394A (en) * | 2016-10-25 | 2018-05-01 | 上海新昇半导体科技有限公司 | Superconductive tape and its manufacture method |
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| DE3731275A1 (en) * | 1987-09-17 | 1989-04-06 | Interatom | METHOD FOR PRODUCING SUPRAL-CONDUCTING CERAMIC LAYERS |
| DE3903728A1 (en) * | 1989-02-08 | 1990-08-16 | Interatom | ELECTROPHORETIC DEPOSITION OF A SUPRAL-CONDUCTIVE LAYER UNDER THE INFLUENCE OF AN EXTERNAL MAGNETIC FIELD |
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2002
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| CN107978394A (en) * | 2016-10-25 | 2018-05-01 | 上海新昇半导体科技有限公司 | Superconductive tape and its manufacture method |
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