CN1082231C - Y-Ba-Cu-O high-temp. superconductor double-face epitaxial film - Google Patents

Y-Ba-Cu-O high-temp. superconductor double-face epitaxial film Download PDF

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CN1082231C
CN1082231C CN97107678A CN97107678A CN1082231C CN 1082231 C CN1082231 C CN 1082231C CN 97107678 A CN97107678 A CN 97107678A CN 97107678 A CN97107678 A CN 97107678A CN 1082231 C CN1082231 C CN 1082231C
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substrate
sputter
cavity
temperature
double
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CN1211555A (en
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李言荣
刘兴钊
陶伯万
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

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Abstract

The present invention belongs to the technical field of high-temperature superconducting film technology. Because of the adoption of an inverted barrel type direct current sputtering device which has a basal slice rotating in situ, adjustable speeds and radiation heating and also has double surfaces forming films at the same time and an optimized self-epitaxy preparation method, the present invention has the advantages of enhancing the quality of the films and making the performance of prepared Y1Ba2Cu3O<7-delta> high-temperature superconducting epitaxial films. Tco of the high-temperature superconducting epitaxial films is larger than 90k, and delta Tc is less than 0.3k; properties of double-surface films on both surfaces of the basal slice are consistent, and the difference of Tco is less than 0.5k; the difference of delta Tc is less than 0.5k, so the present invention can completely satisfy requirements for manufacturing microwave devices with high frequencies.

Description

Yttrium barium copper oxide high-temperature superconductor double-face epitaxial film preparation method and device
The invention belongs to the high-temperature superconducting thin film technical field, particularly the preparation method of double sided superconducting film and device.
As everyone knows, because the microwave surface resistance Rs very low (only being about 200 μ Ω) of high-temperature superconductor, thereby wide application arranged aspect microwave device, some special microwave devices need be made on double sided superconducting film such as filter, delay line etc., thereby in recent years, research to double sided superconducting film increases, the method of its making is different, laser deposition, sputtering method, MOCVD etc. are arranged, two-sided making is simultaneously arranged, also there is single face to make respectively, can have made yttrium barium copper oxide (YBCO) the high-temperature superconductor double-side membrane of φ 75mm.Because at present heating systems that adopt traditional plane heating type more, its heater is in a plane, this heating system is difficult to accomplish the uniformity of temperature profile on substrate two sides, thereby make the Rs lack of homogeneity (differing from more than 100% approximately) of two facial masks, Tc width of transition not ideal enough (more than the difference 1K), this will reduce the performance of the microwave device that utilizes this dual-face superconducting film production greatly.
The objective of the invention is to manufacture yttrium barium copper oxide (YBCO) double-faced high-temperature superconducting film of good performance unanimity, to satisfy the needs that microwave device is made.
The present invention is through careful research and test, think and to solve the problem that ybco film two sides film properties differs greatly, must at first solve the uniformity of substrate two surface temperature distribution, for this reason, specialized designs of the present invention one cover substrate rotation, radiation heating, two-sided while original position film formation device, and optimize from extension double-side membrane sputtering technology, successfully made the YBCO of good performance unanimity.
Yt-Ba-Cu-O high-temperature superconductive film of the present invention is meant that first three component is fixed as Y 1Ba 2Cu 3, and the 4th component O is the serial high-temperature superconducting thin film of 7-δ.Be preparation Y 1Ba 2Cu 3O 7-δThe high-temperature superconductor two-side film membrane, specialized designs of the present invention one the cover preparation facilities, its schematic diagram as shown in Figure 1, it is a rewinding formula dc sputtering device, on rewinding formula magnetically controlled DC sputtering (ICP) device, take down annular magnet and form, this direct current sputtering is easier than the operation of common magnetron sputtering, also can improve the utilance of target greatly.This device is made up of sputtering system 1 and heating system 2 two large divisions.Be fixed with target 3 in the sputtering system, heating system 2 comprises: with the Al of NiCr heater strip 4 uniform winding at one one end closure 2O 3On the cavity 5, its Al 2O 3Symmetry has two holes 6,7 on cavity 5 walls, wherein passes thermocouple 8 in 6 holes, and it can test 0 ℃～1000 ℃ temperature, and allows the test cap of thermocouple 8 be in Al 2O 3The center of cavity 5 is to test the temperature of this cavity; Pass substrate support bar 9 in 7 holes, be in Al 2O 3Be fixed with substrate fixture 10 on the termination of the substrate support bar 9 in 5 cavitys, have groove on two peripheries of substrate fixture 10, substrate 11 is stuck in the groove of anchor clamps, the other end of substrate support bar 9 links to each other with motor, the substrate original position is rotated, rotating speed adjustable, thus guarantee at Al 2O 3Substrate LaAlO in the cavity 5 3Two faces of 11 are subjected to radiation heating, and its uniformity of temperature profile has guaranteed the uniformity of the superconducting film of substrate two sides institute sputter, and at the Al that is wound with heater strip 4 2O 3The outside of cavity 5 is added with the heating radiation shield 12,13,14 that three layers of stainless steel are manufactured.
The present invention utilizes device shown in Figure 1, and that adopts optimization prepares Y from epitaxy method 1Ba 2Cu 3O 7-δThe high-temperature superconductor double-side membrane makes the quality of film excellent more, and concrete technology is:
(1) target is Y 1Ba 2Cu 3O 7-δCylinder is fixed on the sputtering system 1;
(2) substrate is LaAlO 3(100) monocrystalline, diameter through twin polishing, after the clean, is fixed on Al in 1 inch (being 2.54cm) 2O 3On the substrate fixture 10 in the cavity 5;
(3) adjustment substrate to the distance of target is 5～8cm;
(4) adopt from the epitaxy method sputter:
Sputtering condition: atmosphere: the argon-mixed O of oxygen 2: Ar=1: 2～3.5, stagnation pressure 40～65Pa
Electric current: 0.3～0.7A, voltage: 110～180V
Substrate temperature: 760～820 ℃
Substrate rotates with 5～10 rev/mins of speed during sputter;
10～20 ℃ of 1 hour meron of sputter coolings sputter 7 hours again;
Sputter rate was controlled at 1nm～5nm/ minute.
(5) reprocessing: turn off argon gas, aerating oxygen to 6～8 * 10 4Pa, insulation is 5～10 minutes when being cooled to 370～440 ℃, naturally cools to room temperature then.
The typical Y that utilizes sputter equipment provided by the invention and film-forming process to make 1Ba 2Cu 3O 7-δResistance-the temperature variation curve of high-temperature superconductor double-side membrane as shown in Figure 2, the Tco=91.1K of the 1st facial mask, Δ Tc=0.17K, the Tco=91.2K of the 2nd facial mask, Δ Tc=0.18K; The Rs=2.8m Ω of the 1st facial mask under 18.9GHz, 77K, the Rs=3.2m Ω of the 2nd facial mask.The performance of obvious two facial masks differs very little, is better than prior art greatly.
Because the present invention has adopted the rewinding formula dc sputtering device of the rotation continuously of substrate radiation heating, original position, adjustable-speed, two-sided while film forming, compare whole substrate, the particularly temperature distribution evenness on substrate two sides are greatly improved with the substrate plane heating of prior art, fixed rewinding formula magnetically controlled DC sputtering device; Add employing from the quality that epitaxial optimization preparation technology has improved film, make prepared Y 1Ba 2Cu 3O 7-δThe function admirable of high-temperature superconducting epitaxial thin film, its Tco is all greater than 90K, Δ Tc is all less than 0.3K, the performance unanimity of substrate two-side film membrane, its Tco differs less than 0.5K, Δ Tc differs less than 0.5K, the microwave device that utilizes this film to make to can be used in the satellite communication such as: be operated in 6 path filters of C-band and resonator that operating frequency is 6.2GHz etc., satisfy the requirement of microwave device fully.
Accompanying drawing and description of drawings:
Fig. 1: the present invention manufactures double-faced high-temperature superconducting film sputter equipment schematic diagram
Wherein: 1 sputtering system; 2 heating systems; 3 targets; 4 heater strips; 5 Al 2O 3Cavity; 6,7 holes; 8 thermocouples; 9 substrate support bars; 10 substrate fixtures; 11 substrates; 12,13,14 heat radiation screening covers.
Fig. 2: the Y that the present invention makes 1Ba 2Cu 3O 7-δResistance-the temperature variation curve of double sided superconducting film
Wherein: 1 the 1st facial mask, 2 the 2nd facial masks
Embodiment 1: target is selected Y for use 1Ba 2Cu 3O 7-δ
φ 10 * 10mm 2Twin polishing LaAlO 3Substrate, with 10 rev/mins of rotations, target, cardinal distance are 8cm during sputter;
Base temperature 820 ℃, sputtering atmosphere: O 2: Ar=1: 2 mists, stagnation pressure 65Pa, sputtering current 0.7A, sputtering voltage 120V, sputter after 1 hour with ℃ again sputter 7 hours of basic temperature drop to 805;
After sputter is finished, turn off argon gas, feed 8 * 10 immediately 4The oxygen of Pa, and be cooled to 440 ℃ of insulations 10 minutes, naturally cool to room temperature then.
Prepared Y 1Ba 2Cu 3O 7-δThe high-temperature superconductor double-side membrane, the 1st is Tco=91.1K, Δ Tc=0.17K.The 2nd is Tco=91.2k, Δ Tc=0.18k.
Embodiment 2:
φ 10.5 * 5.8mm 2The twin polishing substrate, with 5 rev/mins of rotations, 780 ℃ of base temperature, sputter are with the argon-mixed (O of oxygen during sputter 2: 2.5), stagnation pressure 50Pa Ar=1:, other sputtering condition is identical with embodiment 1, and sputter is after 1 hour, and with ℃ again sputter 7 hours of basic temperature drop to 770, embodiment 1 is identical for other method.The Y that makes 1Ba 2Cu 3O 7-δThe 1st of high-temperature superconductor double-side membrane is Tco=90.8k, Δ Tc=0.2k; The 2nd is Tco=90.7k, Δ Tc=0.3k.
Embodiment 3:
φ 15 * 15mm 2The twin polishing substrate, with 10 rev/mins of rotations, basic temperature is 820 ℃ during sputter, sputtering atmosphere is O 2: Ar=1: 3, stagnation pressure 60Pa, other sputtering condition is identical with embodiment 1, and sputter is after 1 hour, and with ℃ again sputter 7 hours of basic temperature drop to 800, method is identical with embodiment 1 thereafter.The Y that makes 1Ba 2Cu 3O 7, the high-temperature superconductor double-side membrane, its 1st is Tco=90.9k, Δ Tc=0.2, the 2nd facial mask are Tco=90.7k, Δ Tc=0.25.

Claims (2)

1. the preparation method of a yttrium barium copper oxide high-temperature superconductor double-face epitaxial film comprises:
(1) target is Y 1Ba 2Cu 3O 7-δCylinder is fixed on the sputtering system (1);
(2) substrate is LaAlO 3(100) monocrystalline, diameter through twin polishing, after the clean, are fixed on Al in 2.54cm 2O 3On the substrate fixture (10) in the cavity (5);
(3) adjustment substrate to the distance of target is 5～8cm;
(4) adopt from the epitaxy method sputter:
Sputtering condition: atmosphere: the argon-mixed O of oxygen 2: Ar=1: 2～3.5, stagnation pressure 40～65Pa
Electric current: 0.3～0.7A, voltage: 110～180V
Substrate temperature: 760～820 ℃
Substrate rotates with 5～10 rev/mins of speed during sputter;
10～20 ℃ of 1 hour meron of sputter coolings sputter 7 hours again;
Sputter rate was controlled at 1nm～5nm/ minute,
(5) reprocessing: turn off argon gas, aerating oxygen to 6～8 * 10 4Pa, insulation is 5～10 minutes when being cooled to 370～440 ℃, naturally cools to room temperature then.
2. device of implementing yttrium barium copper oxide high-temperature superconductor double-face epitaxial film preparation method in the claim 1, what adopt is rewinding formula sputter equipment, comprise: sputtering system (1) and heating system (2), be fixed with target (3) in the described sputtering system (1), include the Al of NiCr heater strip (4) uniform winding at one one end closure in heating system (2) 2O 3On the cavity (5), the Al of formation 2O 3Symmetry has two holes (6), (7) on the wall of cavity (5), and the test cap that passes thermocouple (8), thermocouple in its mesopore (6) is in Al 2O 3Substrate support bar (9) is passed at the center of cavity (5) in hole (7), be in Al 2O 3Be fixed with substrate fixture (10) on the termination of the substrate support bar (9) in the cavity, have groove on two peripheries of substrate fixture (10), substrate (11) is stuck in the limit groove of substrate fixture (10), the other end of substrate support bar (9) links to each other with motor, the substrate original position is rotated during sputter, adjustable-speed, and substrate (11) is subjected to radiation heating in cavity (5), the while film forming, and at Al 2O 3The outside of cavity (5) is added with the heating radiation shield (12,13,14) that three layers of stainless steel are made.
CN97107678A 1997-09-15 1997-09-15 Y-Ba-Cu-O high-temp. superconductor double-face epitaxial film Expired - Fee Related CN1082231C (en)

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Publication number Priority date Publication date Assignee Title
CN102383191B (en) * 2010-08-31 2014-05-28 苏州大学 Preparation method of (103) oriented yttrium-barium-copper-oxide (YBa2Cu3O7-delta, YBCO) high-temperature superconductive film
CN102965615A (en) * 2011-08-30 2013-03-13 无锡华润上华科技有限公司 Cavity used in PVD processing and PVD processing method
DE102013004791A1 (en) * 2013-03-20 2014-09-25 GM Global Technology Operations, LLC (n.d. Ges. d. Staates Delaware) Control element for a motor vehicle flap

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1030997A (en) * 1987-07-28 1989-02-08 菲利浦光灯制造公司 Superconductive thin layer
CN1045658A (en) * 1989-03-16 1990-09-26 中国科学院上海冶金研究所 A kind of preparation method of metallic oxide superconduction film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1030997A (en) * 1987-07-28 1989-02-08 菲利浦光灯制造公司 Superconductive thin layer
CN1045658A (en) * 1989-03-16 1990-09-26 中国科学院上海冶金研究所 A kind of preparation method of metallic oxide superconduction film

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