CN102255040A - Continuous preparation method of double-sided superconducting strip buffer layer - Google Patents
Continuous preparation method of double-sided superconducting strip buffer layer Download PDFInfo
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- CN102255040A CN102255040A CN201110091978XA CN201110091978A CN102255040A CN 102255040 A CN102255040 A CN 102255040A CN 201110091978X A CN201110091978X A CN 201110091978XA CN 201110091978 A CN201110091978 A CN 201110091978A CN 102255040 A CN102255040 A CN 102255040A
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- base band
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- superconducting strip
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 13
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000004544 sputter deposition Methods 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 229910052786 argon Inorganic materials 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 238000012423 maintenance Methods 0.000 claims description 5
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 9
- 238000000151 deposition Methods 0.000 abstract description 6
- 239000007789 gas Substances 0.000 abstract description 5
- 239000013077 target material Substances 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000010408 film Substances 0.000 description 30
- 238000000034 method Methods 0.000 description 9
- 230000007704 transition Effects 0.000 description 9
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 description 9
- 239000002887 superconductor Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 4
- 230000003139 buffering effect Effects 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 230000005668 Josephson effect Effects 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000001652 electrophoretic deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Superconductors And Manufacturing Methods Therefor (AREA)
- Physical Vapour Deposition (AREA)
Abstract
A continuous preparation method of a double-sided superconducting tape buffer layer belongs to the technical field of superconducting materials. The invention comprises the following steps: 1) installing a base band between the two turntables; 2) respectively arranging metal yttrium targets on the opposite targets, wherein the normal of a base band plane between the two rotating discs is vertical to a metal yttrium target connecting line on the opposite targets; 3) the growth chamber (9) is vacuumized to 5.0 x 10-4Heating the base band below Pa to 600-660 deg.C, introducing argon-hydrogen mixed gas into the growth chamber at 2-3 Pa, and introducing 1.2 × 10-3To 2.5X 10-3Pa of water vapor; 4) the stepping motor drives the base band to move at a constant speed through the first turntable or the second turntable; 5) starting glow, sputtering yttrium metal target material, and depositing Y on the substrate2O3A film; 6) sputtering is turned off.The invention adopts off-axis sputtering, the base band and the target material form an included angle of 90 degrees, and the internal and external textures of the double-sided buffer layer are improved.
Description
Technical field
The invention belongs to the superconductor technical field, particularly the preparation method of superconducting tape.
Background technology
The discovery of high-temperature superconductor in 1986 has caused great interest of whole world scientific circles and concern.People have carried out research extensively and profoundly to each side such as its material composition, architectural feature, performance, application.Superconductor has the character of many uniquenesses, as zero resistance, perfect diamganetism (Meisser effect) and superconductive tunnel effect (Josephson effect) etc., utilize these character can in research and production, develop many devices that important value is arranged, as kicker magnet, superconducting quantum interference device (SQUID), high-efficiency electric motor and lossless electric energy transmitting system etc.The discovery of high-temperature superconductor makes the working temperature of superconductor bring up to liquid nitrogen temperature (77K) from liquid helium warm area (4.2K), makes the practical prospect of superconductor more wide.
The application of high temperature superconducting materia on forceful electric power is an important direction always, and national governments have dropped into huge man power and material to the research of belt material of high temperature superconduct.First generation Bi-based high-temperature superconductive strip (BSCCO/2223) has entered the practicality stage, but it is difficult to obtain high critical current density J under high-intensity magnetic field
c, and a large amount of uses of expensive silver also make it be restricted in reduction industrial cost.Therefore, national governments transfer to the emphasis of research and development on a kind of coating conductor (Coated Conductor claims CC conductor or second generation belt material of high temperature superconduct) that is coated with the YBCO/123 film on the base band of flexible metal.The YBCO band is better than superconductivity under the higher level of bi tape current-carrying, the magnetic field, price is more cheap, is a high-tech industry that has application prospect.
The metal base band of second generation belt material of high temperature superconduct employing at present is mainly based on Ni and Ni base alloy.If directly on the Ni base band, deposit ybco film, because the counterdiffusion between Ni and the YBCO easily makes the band electrical property worsen, the mechanical performance variation, use value reduces.And the compatibility between Ni and the YBCO is relatively poor, can not directly prepare well-formed's YBCO rete on the Ni base band.Thereby need on the Ni base band, prepare with the YBCO compatibility preferably the oxide transition zone to improve the performance of ybco film.Because need stop the gentle and lattice mismatch of diffusion, buffer layer thin film should possess certain thickness, this just needs high deposition velocity; In order to satisfy the needs of application facet, the longer the better for the second generation superconducting tape that need prepare simultaneously; Simultaneously, in order to carry bigger current strength, just need the dual-face superconducting strip of preparation two sides high conformity; And for industrialization demands, how preparing two-sided oxide transition layer film on long base band fast continuously becomes the technical problem that urgent need solves.
In addition, studies show that the intercrystalline crystal boundary angle of YBCO has a significant impact superconductivity, when the crystal boundary angle was greater than 4 ° inside and outside the YBCO face, superconductivity sharply descended.Because YBCO intercrystalline angle epitaxial growth on resilient coating in the superconducting tape, therefore improving the inside and outside texture of buffering aspect is another problem that need solve.
At present, can adopt pulsed laser deposition, magnetron sputtering, electron beam coevaporation equal vacuum method for the preparation of this class film, and antivacuum methods such as sol-gel, deposition of metal organic, electrophoretic deposition, liquid phase epitaxial method.But no matter be from continuity, two sides consistency or above the deposition velocity, all exist deficiency, need to seek for this reason a kind of can solution to the problems described above.
Chinese patent 200610020898.4 discloses a kind of continuous preparation method of two-sided long superconducting strip cushion, its target direction is perpendicular to the base band surface, on the consistency of the two sides of deposit film to some extent the shortcoming, and inside and outside the buffering aspect the also prepared gap to some extent of texture than this patent.
Summary of the invention
Technical problem to be solved by this invention is, a kind of method that is used for preparing at a high speed, continuously two-sided second generation belt material of high temperature superconduct resilient coating is provided, use this method can realize the preparation rapidly, continuously of belt material of high temperature superconduct resilient coating, the film that uses this method to prepare has good two sides consistency, the single face good uniformity, degree of orientation height, the surface smoothness height.
The technical scheme that the present invention solve the technical problem employing is that the continuous preparation method of dual-face superconducting strip cushion comprises the steps:
1, the continuous preparation method of dual-face superconducting strip cushion is characterized in that, comprises the steps:
1) the nickel-base alloy biaxial texture base band with tungstenic 5% is installed between first rotating disk and second rotating disk;
2) the metallic yttrium target is placed in respectively on the target, the normal on the base band plane between two rotating disks is vertical with the relative metallic yttrium target line on the target;
3) growth room is taken out back of the body end vacuum to 5.0 * 10
-4Below the Pa, base band is heated, make temperature finally remain on 600 ℃～660 ℃, in the growth room, charge into argon hydrogen mixture, and make maintenance 2～3Pa argon hydrogen mixture in the growth room, charge into 1.2 * 10 again
-3To 2.5 * 10
-3The steam of Pa;
4) stepping motor drives the base band uniform motion by first rotating disk or second rotating disk;
5) open aura, splash-proofing sputtering metal yttrium target deposits Y on substrate
2O
3Film;
6) close sputter, stop substrate heating, the Y that obtains making
2O
3Film.
Further, the base band direction of motion is vertical with metallic yttrium target line.Described argon hydrogen mixture is 96% Ar and 4% H by mol ratio
2Form.
The temperature of step 3) keeps 620 ℃, keeps the 2.5Pa argon hydrogen mixture in growth room (9).
The invention has the beneficial effects as follows:
1, the present invention has adopted the rotating disk of the base band of can reeling, and can prepare the long superconducting strip cushion of random length continuously;
2, the present invention vertically places base band, allows it travel at the uniform speed up and down, because the base band that the base band that action of gravity produces is crooked and excessive pulling force causes is out of shape, makes the deposit film uniformity higher in the time of can avoiding level run;
3, the present invention adopts target off-axis sputtering deposit film, can realize two-sided deposition simultaneously, has improved operating efficiency, has also guaranteed the two sides consistency of deposit film simultaneously.
4, the present invention adopts off-axis sputtering, and base band becomes 90 degree angles with target, has improved the inside and outside texture of two-sided buffering aspect.
The present invention is further illustrated below in conjunction with accompanying drawing.
Description of drawings
Fig. 1 be used a kind of of the continuous preparation method of a kind of two-sided long superconducting strip cushion of the present invention have upper and lower two rotating disks to target from axle magnetic control sputtering device structural representation.
The 1-lower rotary table; The 2-base band; The 3-resistive heater; 4-is to target; The 5-aura; 6-reacting gas intake valve; 7-working gas intake valve; The 8-top rotary table; The 9-growth room; The 10-thermocouple; The 11-steam vent.
Fig. 2 is the prepared superconducting tape oxide transition zone Y of continuous preparation method that utilizes a kind of two-sided long superconducting strip cushion of the present invention
2O
3The X-ray diffraction of film (XRD) θ-2 θ scanning spectra.Wherein X-axis is represented 2 θ angles (unit degree of being), and Y-axis represents to count intensity (unit is count/second).As shown in Figure 2, the Y that utilizes the present invention to prepare
2O
3It is single-orientated that film has (004).
Fig. 3 is the prepared superconducting tape oxide transition zone Y of continuous preparation method that utilizes a kind of two-sided long superconducting strip cushion of the present invention
2O
3The X-ray diffractometer ω scanning spectra at (002) peak of film.Wherein X-axis is represented θ angle (unit degree of being), and Y-axis represents to count intensity (unit is count/second), and as shown in Figure 3, its halfwidth (FWHM) is 1.4 °, shows to have the outer texture of good face.
Fig. 4 is the prepared superconducting tape oxide transition zone Y of continuous preparation method that utilizes a kind of two-sided long superconducting strip cushion of the present invention
2O
3The X-ray diffractometer of (111) face of film
Scanning spectra.Wherein X-axis is represented Phi angle (unit degree of being), and Y-axis represents to count intensity (unit is count/second), and as shown in Figure 4, its halfwidth is 3.8 °, shows to have texture in the good face.
Fig. 5 is the prepared superconducting tape oxide transition zone Y of continuous preparation method that utilizes a kind of two-sided long superconducting strip cushion of the present invention
2O
3The X-ray diffractometer utmost point figure collection of illustrative plates of (111) face of film.As shown in Figure 4, limit converges to 4 points, and limit is 4 heavy symmetries, shows prepared Y
2O
3Be cubic structure, and have texture in the good face.
Fig. 6 is the prepared superconducting tape oxide transition zone Y of continuous preparation method that utilizes a kind of two-sided long superconducting strip cushion of the present invention
2O
3The plane graph of the atomic force microscope of film (AFM) 2 μ m zone internal surface shape.
Fig. 7 is the prepared superconducting tape oxide transition zone Y of continuous preparation method that utilizes a kind of two-sided long superconducting strip cushion of the present invention
2O
3The 3 dimensional drawing of the atomic force microscope of film (AFM) 2 μ m zone internal surface shape.
By Fig. 6,7 as can be known, the prepared Y of the present invention
2O
3Smooth, the flawless of film surface.
Fig. 8 is Y on 1 meter long base band
2O
3Film ω scanning two sides halfwidth distribution map.As shown in Figure 8, the prepared Y of the present invention
2O
3All suitable good of the uniformity of film two sides consistency and single face.
Fig. 9 is Y on 1 meter long base band
2O
3Film
Scanning two sides halfwidth distribution map.As shown in Figure 9, the prepared Y of the present invention
2O
3All suitable good of the uniformity of film two sides consistency and single face.
Embodiment
Embodiment 1:
The specific embodiment of the invention provides a kind of based on the low temperature depositing metal and carry out the method that the in-situ high temperature oxidation processes prepares second generation belt material of high temperature superconduct oxide transition layer film, and its concrete steps are as follows:
The first step: the nickel-base alloy biaxial texture base band of tungstenic 5% is installed between two rotating disks 1,8, and base band is wide to be 10 millimeters, and thickness is 0.1 millimeter.Drive rotating disk 1 or 8 uniform motion by the stepping motor that has rotational speed governor, drive the base band uniform motion thus.When lower rotary table 1 rotates, can drive base band 2 and at the uniform velocity move downward; When top rotary table 8 rotates, can drive base band 2 at the uniform velocity scroll up around.Base band is in cavity 5 winding process, and the base band surface keeps becoming 90 to spend angles with metal targets.
Second step: metallic yttrium (Y) target (length is 48 millimeters, and wide is 32 millimeters, and thickness is 4 millimeters) is placed on the target 4, and 3 pairs of base band of resistive heater heat, and adopt thermocouple 10 to read temperature in the cavity.Rotating disk 1,8, to target 4, base band 2, resistive heater 3, thermocouple 10 all is placed on growth room 9.Reacting gas air inlet pipe and valve 6 feed the inside of growth room always, and then feeding is near the target 4 for working gas air inlet pipe and valve 7, and the right part opening connects vacuum pump 11 (mechanical pump and molecular pump).
Second step: back of the body end vacuum to 5.0 * 10 are taken out by growth room 9 with vacuum pump 11
-4Below the Pa, utilize 3 pairs of base band 2 of resistive heater to heat, make temperature finally remain on 620 ℃, read temperature, in growth room 9, charge into argon hydrogen mixture (Ar96+H from air inlet pipe 7 then by thermocouple 10
24%), and makes maintenance 2.5Pa argon hydrogen mixture in the growth room 9, charge into 1.2 * 10 from air inlet pipe 6
-3～2.5 * 10
-3The steam of Pa.
The 3rd step: open target 4 aura 5, keep sputtering power 40W～60W, splash-proofing sputtering metal yttrium target makes on the NiW5% twin shaft substrate and deposits Y
2O
3Film.
The 4th step: base band at the uniform velocity by behind the aura zone, is closed sputter, stops air inlet pipe 6,7 is closed in the substrate heating simultaneously, stops molecular pump and mechanical pump, takes out the Y that makes
2O
3Film.
With the above Y that makes
2O
3It is as follows that film carries out the instrument that structural analysis and surface topography analyze:
X-ray diffractometer (XRD), model are Britain Bede D1 System; Atomic force microscope (AFM), model are Japanese SEIKO SPA-300HV.
By above to Y
2O
3The structure of film and surface topography analysis are as can be known, adopt apparatus of the present invention can prepare the good two-sided long band resilient coating of two sides consistency and inner evenness fast continuously, and the buffer layer thin film for preparing has good orientation and high surface smoothness, for the growth of subsequent film provides good growth templates.Owing to possess above advantage, can satisfy the demand that industrialization is produced fast.
The difference of the present invention and embodiment 1 is, in the step 3), base band 2 is heated, and makes temperature finally remain on 660 ℃, charges into argon hydrogen mixture in growth room 9, and makes maintenance 2Pa argon hydrogen mixture in the growth room 9.
Embodiment 3
The difference of the present invention and embodiment 1 is, in the step 3), base band 2 is heated, and makes temperature finally remain on 660 ℃, charges into argon hydrogen mixture in growth room 9, and makes maintenance 3Pa argon hydrogen mixture in the growth room 9.
Claims (4)
1. the continuous preparation method of dual-face superconducting strip cushion is characterized in that, comprises the steps:
1) the nickel-base alloy biaxial texture base band with tungstenic 5% is installed between first rotating disk (1) and second rotating disk (8);
2) the metallic yttrium target is placed in respectively on the target (4), the normal on the base band plane between two rotating disks is vertical with the relative metallic yttrium target line on the target (4);
3) growth room (9) are taken out back of the body end vacuum to 5.0 * 10
-4Below the Pa, base band (2) is heated, make temperature finally remain on 600 ℃～660 ℃, in growth room (9), charge into argon hydrogen mixture, and make maintenance 2～3Pa argon hydrogen mixture in the growth room (9), charge into 1.2 * 10 again
-3To 2.5 * 10
-3The steam of Pa;
4) stepping motor drives the base band uniform motion by first rotating disk (1) or second rotating disk (8);
5) open aura (5), splash-proofing sputtering metal yttrium target deposits Y on substrate
2O
3Film;
6) close sputter, stop substrate heating, the Y that obtains making
2O
3Film.
2. the continuous preparation method of dual-face superconducting strip cushion as claimed in claim 1 is characterized in that, the base band direction of motion is vertical with metallic yttrium target line.
3. the continuous preparation method of dual-face superconducting strip cushion as claimed in claim 1 is characterized in that, described argon hydrogen mixture is 96% Ar and 4% H by mol ratio
2Form.
4. the continuous preparation method of dual-face superconducting strip cushion as claimed in claim 1 is characterized in that, the temperature of step 3) keeps 620 ℃, keeps the 2.5Pa argon hydrogen mixture in growth room (9).
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|---|---|---|---|
| CN 201110091978 CN102255040B (en) | 2011-04-13 | 2011-04-13 | Continuous preparation method of double-sided superconducting strip buffer layer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110091978 CN102255040B (en) | 2011-04-13 | 2011-04-13 | Continuous preparation method of double-sided superconducting strip buffer layer |
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|---|---|
| CN102255040A true CN102255040A (en) | 2011-11-23 |
| CN102255040B CN102255040B (en) | 2013-06-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103276360A (en) * | 2013-06-14 | 2013-09-04 | 电子科技大学 | Magnetic nanowire array thin film and preparation method thereof |
| CN109023276A (en) * | 2018-08-29 | 2018-12-18 | 电子科技大学 | A method of the two-sided MgO film of homoepitaxy is prepared based on mid frequency sputtering |
| CN109518154A (en) * | 2019-01-16 | 2019-03-26 | 上海上创超导科技有限公司 | Superconducting strip cushion double-sided coating device |
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2011
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103276360A (en) * | 2013-06-14 | 2013-09-04 | 电子科技大学 | Magnetic nanowire array thin film and preparation method thereof |
| CN103276360B (en) * | 2013-06-14 | 2015-02-18 | 电子科技大学 | Magnetic nanowire array thin film and preparation method thereof |
| CN109023276A (en) * | 2018-08-29 | 2018-12-18 | 电子科技大学 | A method of the two-sided MgO film of homoepitaxy is prepared based on mid frequency sputtering |
| CN109518154A (en) * | 2019-01-16 | 2019-03-26 | 上海上创超导科技有限公司 | Superconducting strip cushion double-sided coating device |
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|---|---|
| CN102255040B (en) | 2013-06-12 |
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