CN1211555A - 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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CN1211555A
CN1211555A CN97107678A CN97107678A CN1211555A CN 1211555 A CN1211555 A CN 1211555A CN 97107678 A CN97107678 A CN 97107678A CN 97107678 A CN97107678 A CN 97107678A CN 1211555 A CN1211555 A CN 1211555A
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substrate
sputter
sputtering
cavity
double
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CN1082231C (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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

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Abstract

A double-surface high-temp epitaxial superconducting Y1Ba2Cu3O7-delta membrane used as high-frequency microwave device features that a reverse barrel type of DC sputter that features in-situ rotation of substrate, adjustable speed, radiation heating and double-surface filming at same time is used and optimized self-epitaxy process is implemented to obtain high-quality membrane. Its Tco is higher than 90K and its delta Tc is less than 0.3k. The difference between the films on both surfaces is less than 0.5k for Tco or delta Tc.

Description

Yttrium barium copper oxide high-temperature superconductor double-face epitaxial film
The invention belongs to the high-temperature superconducting thin film technical field, particularly the system of double sided superconducting film is scooped up with a dustpan.
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 wave filter, retarding 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 heating element 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 homogeneity 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 deposition system, 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 synoptic 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 ring-shaped magnet and form, this d.c. sputtering is easier than the operation of common magnetron sputtering, also can improve the utilization ratio of target greatly.This device is made up of sputtering system 1 and heating system 2 two partss.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 pipe 5, its Al 2O 3Symmetry has two holes 6,7 on cavity 5 walls, wherein passes thermopair 8 in 6 holes, and it can test 0 ℃～1000 ℃ temperature, and allows the test cap of thermopair 8 be in Al 2O 3The center of pipe 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, two of substrate fixture 10 with having groove on the limit, and 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, and rotating speed is adjustable, thereby guarantees 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 homogeneity of the superconducting film of substrate two sides institute sputter, for raising the efficiency, at the Al that is wound with heater strip 4 2O 3The outside of pipe 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, are fixed on Al in 1 inch 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 mera of sputter coolings sputter 7 hours again;
Sputter rate is controlled at 1nm～5nm/ branch.
(5) aftertreatment: 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, 77 ° of k, 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 rotation continuously of substrate radiation heating, original position, adjustable-speed, film forming rewinding formula dc sputtering device of two-sided while, 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 excellent property 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 synoptic diagram
Wherein: 1 sputtering system; 2 heating systems; 3 targets; 4 heater strips; 5Al 2O 3Pipe; 6,7 holes; 8 thermopairs; 9 substrate support bars; 10 substrate fixtures; 11 substrates; 12,13,14 heat radiation screening covers.
The typical Y that Fig. 2 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 mask
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 mixed gass, 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 (3)

  1. Yttrium barium copper oxide high-temperature superconductor double-face epitaxial film its wait to levy be adopt the rotation of substrate original position, adjustable-speed, radiation heating, film forming rewinding formula dc sputtering device of two-sided while and optimization from epitaxy technique, make at the two-sided Y that grows good (Tco greater than 90k, Δ Tc less than 0.3k), performance unanimity (Tco of double-side membrane differs less than 0.5k, and Δ Tc differs less than 0.5k) simultaneously of substrate 1Ba 2Cu 3O 7-δThe high-temperature superconductor double-face epitaxial film.
  2. The device of yttrium barium copper oxide high-temperature superconductor double-face epitaxial film rewinding formula d.c. sputtering preparation its wait to levy and be that it is made up of sputtering system (1) and heating system (2) two parts, be fixed with target (3) in the 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 pipe (5), the Al of formation 2O 3Symmetry has two holes (6), (7) on the wall of cavity (5), and the test cap that passes thermopair (8), thermopair 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, and the substrate original position is rotated during sputter, adjustable-speed, substrate (11) is subjected to radiation heating in cavity (5), the while film forming is for raising the efficiency, 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.
  3. 3. the preparation technology of yttrium barium copper oxide high-temperature superconductor double-face epitaxial film is characterized in that adopting getting along alone and prolongs method, and concrete preparation technology is:
    (1) target is Y 1Ba 2Cu 3O 7-δCylinder is fixed on (1) of sputtering system;
    (2) substrate is LaAlO 3(100) monocrystalline, diameter through twin polishing, after the clean, are fixed on Al in 1 inch 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 mera of sputter coolings sputter 7 hours again;
    Sputter rate is controlled at 1nm～5nm/ branch.
    (5) aftertreatment: 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.
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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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102383191A (en) * 2010-08-31 2012-03-21 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
CN104129280A (en) * 2013-03-20 2014-11-05 通用汽车环球科技运作有限责任公司 Actuator element for a motor vehicle cover

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL8701779A (en) * 1987-07-28 1989-02-16 Philips Nv SUPER CONDUCTIVE 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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102383191A (en) * 2010-08-31 2012-03-21 苏州大学 Preparation method of (103) oriented yttrium-barium-copper-oxide (YBa2Cu3O7-delta, YBCO) high-temperature superconductive film
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
CN104129280A (en) * 2013-03-20 2014-11-05 通用汽车环球科技运作有限责任公司 Actuator element for a motor vehicle cover

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