CN1317777C - Thallum-based high-temperature superconductive film material and its preparation method - Google Patents
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Abstract
The present invention relates to a Tl2Ba2CaCu2O8 (Tl-2212) superconducting material film and a preparation method thereof. The superconducting transition temperature of the Tl-2212 superconducting film is higher than 100K, and the critical current density is greater than 10<6>A/cm<2> at the temperature of 77K. The surface resistance is less than 1m ohm at the temperature of 77K in frequency of 10GHz, and the thickness of the Tl-2212 superconducting material film is from 10 nm to 1000 nm. The preparation method of the present invention mainly adopts two steps to prepare the Tl-2212 epitaxial superconducting film that a first step, a Tl-Ba-Ca-Cu-O amorphous precursor film is illuviated on a substrate base sheet; a second step, the Tl-Ba-Ca-Cu-O amorphous precursor film is changed into a superconducting film after high heat treatment. The present invention has the preparation method of the large-area double-face Tl-2212 epitaxial superconducting film. The Tl-2212 epitaxial superconducting film which is prepared by the present invention can be used for preparing microwave passive devices or other superconducting electronic devices.
Description
Technical field
The present invention relates to the high-temperature superconducting thin film preparation methods, it is a thallium system high-temperature superconducting material, particularly relates to the Tl-Ba-Ca-Cu-O superconductor material thin film, relates in particular to Tl
2Ba
2CaCu
2O
8(Tl-2212) preparation method of superconductor material thin film.
Background technology
High-quality high-temperature superconducting thin film, at superconductive electronic device, especially the microwave passive component application facet has great importance.In actual applications, require the superconducting transition temperature of superconductor to be higher than 1/3rd of working temperature at least, and have high critical current density, low microwave surface resistance.In the microwave passive component application facet, require on substrate base, to make high-quality two-side film membrane, and area wants enough big.
Document (Epitaxial Tl
2Ba
2CaCu
2O
8Superconducting thin film on Sr
2(AlTa) O
6Buffer layer, Y.Q.Tang, et al., J.Applied Physics 78 (1995) 6846) and 1: adopt laser deposition Ba
2CaCu
2O
xPioneer's film, 800 ℃ of heat treatments obtained Tl in 8 hours in air
2Ba
2CaCu
2O
8Superconducting thin film, crystalline particulate, critical current density jc (77K) has only 3 * 10
5A/cm
2.
Document (Preparation of Tl
2Ba
2CaCu
2O
8Superconducting thin films on LaAlO
3Substratesfrom metalorganic-chemical-vapor-deposition-prepared precursor films, J.A.Ladd, et al., Appl.Phys.Lett.59 (1991) 1368) 2: adopt MOCVD method deposit Ba-Ca-Cu-O pioneer film, 870 ℃ of heat treatment is 0.1 hour in oxygen atmosphere, the Tl that obtains
2Ba
2CaCu
2O
8The superconducting transition temperature Tc of film has only 98K, and critical current density jc (77K) has only 1 * 10
4A/cm
2.
Document (Superconducting epitaxial Tl
2Ba
2CaCu
2O
8Films on sappire with cerium oxidebuffer layers, W.L.Holstein et al, Applied Physics Letters 61 (1992) 982) 3: at CeO
2Separator Al
2O
3Deposit BaCaCuO film on the substrate base, 870 ℃ of heat treatments in air again, the Tl of making
2Ba
2CaCu
2O
8Film contains impurity B aAl
2O
4, superconducting transition temperature Tc=98K, and critical current density jc (75K, 0T)=2.8 * 10
5A/cm
2
Document (Buffer layer/film interaction in growth of Tl
2Ba
2Ca
1Cu
2O
xFilms on CeO
2Bufferedsapphire, A.P.Bramley, et al.Applied Physics Letters 66 (1995) 517) 4: adopt rf sputtering deposit pioneer film, heat treatment in air, 840-880 ℃, for up to 1 hour, seriously react between film and the separator, generate impurity B aCeO
3, Tc=94K, Jc=8 * 10
4A/cm
2
Document (Influence of substrate and precursor film composition on morphology andsuperconducting transition of Tl-2212 thin films characterized by microwaves, S.Chromik, etal, Physica C 354 (2001) 429) 5: with method deposit BaF on substrate base of thermal evaporation
2, Cu and CaF
2, in 700 ℃ of temperature oxygen atmospheres, remove F then
2, heat treatment 30 minutes under 850 ℃ of temperature in the oxygen atmosphere that flows, superconducting transition temperature Tc=95-100K.
Document (Dual mode cross slotted filter realized grown with double-sided Tl
2Ba
2CaCu
2O
8Films by MOCVD, A.Cassinese etc., Superconductor Science and Technology 14 (2001) 406) 6: adopt Organometallic Chemistry gas deposition (MOCVD) to make pioneer's film, 10 * 10mm
2LaAlO
3(100) substrate base, two-sided, Tl
2Ba
2CaCu
2O
8The thin film crystallization pattern is bad, a lot of cavities, cause Jc (77K) have only=5 * 10
4A/cm
2
Document (TlBaCaCuO-(2212) thin films on lanthanum aluminate and sapphire substrates formicrowave filters, H Schneidewind etc., Superconductor Science and Technology14 (2001) 200) 7: adopt the Ba-Ca-Cu alloy to make sputtering target, do not mention sputter rate.Two-side film membrane needs film of first sputter, sintering, and then spatter another side, sintering again.
Document (Large area YBa
2Cu
3O
7And Tl
2Ba
2CaCu
2O
8Thin films for microwave and electronicapplications, D.W.Face etc., Physica C 357-360 (2001) 1488-1494) 8: at first make BaCaCuO pioneer's film, again at oxygen and Tl with the off-axis magnetron sputtering
2Heat treatment in the O atmosphere.There is BaCeO in the film
3Impurity.Do not provide concrete manufacturing process, do not provide the specific targets of the Tc and the Jc of film yet.
Document (Method of fabricating thin film superconducting materials, Ying Xin etc., U.S. Pat 5807809) 9: at first make the Ba that contains 10% gold medal of having an appointment: Ca: Cu: O 223 prefabricated membranes, heat-treat then, obtain containing the Tl-2223 superconducting thin film of gold.The Tl-2223 film superconducting transition temperature of invention is greater than or equal to 120K, and critical current density jc (77K) is more than or equal to 10
5A/cm
2
Document (Preparation of superconducting Tl-Ba-Ca-Cu-O thin films by Tl
2O
3Vaporprocessing, Allen M.Hermann, Zhengzhi Sheng, U.S. Pat 5112800) 10: propose to make earlier the Ba-Ca-Cu oxide, heating Tl
2O
3Obtain Tl
2O
3Steam and the reaction of Ba-Ca-Cu oxide generate the thallium series superconducting material.Do not mention Tl
2Ba
2CaCu
2O
8The manufacture method of superconducting thin film is not mentioned structure, the critical current density of Tl-Ba-Ca-Cu-O film and sheet resistance yet.
Summary of the invention
The purpose of this invention is to provide a kind of thallium system high-temperature superconducting thin-film material and preparation method thereof.The present invention can overcome the shortcoming of prior art, and technology is simple, and production cost is low, and the superconducting transition temperature Tc>100K of the superconducting film material (Tl-2212) that the present invention makes can be operated in liquid nitrogen temperature or higher temperature.The area maximum of double sided superconducting film can reach more than the diameter 50mm.
Thallium system high-temperature superconducting thin-film material of the present invention, general formula is Tl
2Ba
2CaCu
2O
8, described Tl
2Ba
2CaCu
2O
8The superconducting transition temperature Tc of film>100K, liquid nitrogen temperature lower critical current density, J c (77K)>1 * 10
6A/cm
2, the surface resistance R s of 10GHz under the liquid nitrogen temperature<1m Ω.Tl
2Ba
2CaCu
2O
8The thickness of superconducting thin film is between 10nm-1000nm.
Described superconducting thin film is on the one side of substrate base or on the two sides.More than the area diameter 50mm of described superconducting thin film.The preparation method of thallium system high-temperature superconducting thin-film material of the present invention comprises the steps:
1) deposit Tl-Ba-Ca-Cu-O amorphous pioneer film on substrate base;
2) in argon gas or oxygen or argon oxygen gas mixture atmosphere (~10
5Pa), in containing the earthenware Crucible of thallium source material, carry out high-temperature heat treatment, make Tl-Ba-Ca-Cu-O amorphous pioneer film change superconducting thin film into.
The ratio of the metallic element of described amorphous pioneer film is Tl: Ba: Ca: Cu=1-3: 2: 1: 2.
Described Tl can partly be replaced by Hg, Pb, Cr, and Ba can partly be replaced by Sr.
Described amorphous pioneer thin film deposition is on the one side of substrate base or on the two sides.
Described substrate base material is a crystalline material, the lattice constant of its crystalline material or after these crystalline material surfaces add separator the lattice constant and the described superconductor lattice constant of separator be complementary.Described substrate base material is LaAlO
3, SrTiO
3, NgGaO
3, LSAT[(La, Sr) (Al, Ta) O
3], or on MgO, sapphire, add CeO
2Separator.
Described amorphous pioneer film is to adopt ion sputtering or laser evaporation to be deposited on the substrate base from the Tl-Ba-Ca-Cu-O bulk material.
Described Tl-Ba-Ca-Cu-O bulk material is to use BaO
2Or BaNO
3, CaO or CaCO
3, CuO and Tl
2O
3Make; Use BaO earlier
2Or BaNO
3, CaO or CaCO
3After evenly mixing, grind with CuO, high temperature in oxygen atmosphere (900-950 ℃) calcination is more than 10 hours, then with Tl
2O
3Mixing, grinding and compressing tablet, 800-900 ℃ of calcination is more than 1 hour in sealing earthenware Crucible.
Described thallium source material is through the heat treated Tl of containing, Ba, and Ca, the oxide of Cu, manufacturing process is identical with making Tl-Ba-Ca-Cu-O bulk material, is 2 to make standard with Ba content, and structural formula is Tl
wBa
2Ca
hCu
kO
y, wherein, w=2.5 ± 0.5, h=1.5 ± 1.0, k=2.5 ± 1.0, y=2+h+k+1.5w.
Described high-temperature heat treatment is that amorphous pioneer film and thallium source material are together put into sealing earthenware Crucible, put into the quartz ampoule heating again, temperature is 720-900 ℃, time 0.5-12 hour, make amorphous pioneer film be transformed into the extension superconducting thin film on substrate base, the thickness of superconducting thin film is between 10nm-1000nm.
The gas atmosphere of high-temperature heat treatment of the present invention can flow, and also can seal.Flowing gas filters the back by condensation and dilute acid soln and discharges, to guarantee that environment can be not contaminated.
The invention provides preparation Tl
2Ba
2CaCu
2O
8(Tl-2212) method of superconducting thin film.The Tl-2212 superconducting thin film of preparation has good extension feature and even even curface pattern, and the superconducting transition temperature of film is higher than 100K, and 77K temperature lower critical current density is greater than 10
6A/cm
2, under the 77K temperature, sheet resistance when the 10GHz frequency less than 1m Ω.The present invention can prepare single face Tl-2212 film on substrate base, also can make two-sided Tl-2212 film, and the area maximum gauge of the Tl-2212 film of making is more than 50mm.
The Tl-2212 superconducting thin film that the present invention makes can be used for making microwave passive component, also can be used for making other superconductive devices and carries out scientific research etc.
Description of drawings
Fig. 1: magnetically controlled DC sputtering deposit Tl-Ba-Ca-Cu-O amorphous pioneer film schematic diagram.
Fig. 2: amorphous pioneer film annealing device is thrown the face schematic diagram.
Fig. 3: at LaAlO
3Scanning electron microscopy (SEM) photo of the two-sided Tl-2212 superconducting thin film of (001) making on the single crystalline substrate of 2 inch diameters.
Fig. 4: the Tc of film shown in Figure 3 is the distribution on the film in the 50.8mm scope.
Fig. 5: the Jc of film shown in Figure 3 is the distribution on the film in the 50.8mm scope.
Embodiment
Below in conjunction with case description the present invention, do not represent the present invention is imposed any restrictions.
Embodiment
Preparation Tl-Ba-Ca-Cu-O amorphous pioneer film adopts magnetically controlled DC sputtering.Fig. 1 is the magnetic control sputtering device schematic diagram.Two sputtering target 1 symmetries are placed among the figure.Film-substrate substrate 2 is placed on the rotatable base sheet rack 3.
Sputtering target 1 is to adopt 2 footworks to make.At first use BaO
2, CaO and CuO be according to atomic ratio Ba: Ca: Cu=2: 1: 2 ratio cooperates, evenly behind the mixed grinding, calcination is 10 hours in the oxygen atmosphere that flows and under 900 ℃ of temperature, carefully grinds after the cooling again, the BaCaCuO powder is made in calcination 10 hours again under similarity condition.Then, with BaCaCuO powder and Tl
2O
3Powder is carefully ground the back compressing tablet, with the calcination 1 hour in the oxygen atmosphere that flows and under 850 ℃ of temperature of earthenware Crucible sealing back.Carefully grind again after the cooling, compressing tablet, with similarity condition calcination 1 hour again, make the TlBaCaCuO sputtering target, the metallic atom proportioning is near Tl: Ba: Ca: Cu=2: 2: 1: 2 ratio.
Before the magnetron sputtering, vacuum degree is extracted into 10 at the bottom of the back of the body of vacuum chamber
-3Below the handkerchief, charge into Ar/O then
2Mist, Ar/O
2Ratio be Ar: O
2=4: 1.During sputter, air pressure remains on about 1.5 handkerchiefs.Sputter rate is regulated by direct current, is controlled at per minute 6nm.
Fig. 2 is that annealing device is thrown the face schematic diagram.Thallium source material 5 is to adopt 2 footworks to make.At first use BaO
2, CaO and CuO be according to atomic ratio Ba: Ca: Cu=2: 2: 3 ratio cooperate grind after, calcination is 10 hours in the oxygen atmosphere that flows and under 900 ℃ of temperature, grinds after the cooling again, the BaCaCuO powder is made in calcination 10 hours again under similarity condition.Then, with BaCaCuO powder and Tl
2O
3Powder is ground the back compressing tablet, with the calcination 1 hour in the oxygen atmosphere that flows and under 850 ℃ of temperature of earthenware Crucible sealing back.Grind again after the cooling, compressing tablet, with similarity condition calcination 1 hour again, make thallium source material 5.The metallic atom proportioning of thallium source material 5 is near Tl: Ba: Ca: Cu=3: 2: 2: 3.Amorphous pioneer film and substrate base 4 are placed between two thallium source materials 5, and together put into sealing earthenware Crucible 6.Sealing earthenware Crucible 6 is put into quartz ampoule 7 together with pioneer's film of inside and substrate base 4 and thallium source material 5, quartz ampoule 7 is placed in the tube furnace heats, make amorphous pioneer film 4 change the Tl-2212 superconducting thin film into.
Before the tube furnace heating, quartz ampoule is vacuumized by blast pipe 8 with mechanical pump earlier, vacuum degree reaches<10 handkerchiefs, charges into about 1 atmospheric pressure (10 by air inlet pipe 9 then
5Pa) Ar gas, and keep this air pressure.The speed about 10 ℃ with per minute is heated to 770 ℃ of temperature with quartz ampoule, and keeps 6 hours.Then, turn off the tube furnace power supply and be cooled to room temperature naturally, just form the Tl-2212 superconducting thin film.The scanning electron microscopy of Tl-2212 superconducting thin film (SEM) photo is seen Fig. 3, and superconducting transition temperature Tc sees Fig. 4, and critical current density jc is seen Fig. 5.
Fig. 3 has provided at LaAlO
3Scanning electron microscopy (SEM) photo of the two-sided Tl-2212 superconducting thin film of (001) making on the single crystalline substrate of 2 inch diameters.Film surface is clean, compact crystallization.
The superconducting transition temperature Tc of film and critical current density jc are to adopt the inductance method test.Fig. 4 has provided Tc distribution on the film in 2 inches scopes of film shown in Figure 3, the highest Tc=105.2K, minimum Tc=104.8K.Fig. 5 has provided the critical current density jc of film shown in Figure 3 in the distribution on the film in the 50.8mm scope under the 77K temperature.Remove outmost turns because test problem causes beyond the data that the result forbidden, other results can be expressed as Jc (77K)=(5.08-6.32) * 10
6A/cm
2
Claims (8)
1, a kind of preparation method of thallium system high-temperature superconducting thin-film material, the general formula of this superconducting film material is Tl
2Ba
2CaCu
2O
8Described Tl
2Ba
2CaCu
2O
8The superconducting transition temperature Tc of film>100K, 77K temperature lower critical current density, J c>1 * 10
6A/cm
2, the surface resistance R s of 10GHz under the liquid nitrogen temperature<1m Ω; Described superconducting thin film is on the one side of substrate base or on the two sides; The thickness of described superconducting thin film is between 10nm-1000nm; More than the area diameter 50mm of described superconducting thin film;
It is characterized in that specifically comprising the steps:
1) deposit Tl-Ba-Ca-Cu-O amorphous pioneer film on substrate base;
2) 10
5In the argon gas of Pa or oxygen or the argon oxygen gas mixture atmosphere, in containing the earthenware Crucible of thallium source material, carry out high-temperature heat treatment, make Tl-Ba-Ca-Cu-O amorphous pioneer film change superconducting thin film into.
2, according to the preparation method of the described thallium system high-temperature superconducting of claim 1 thin-film material, it is characterized in that described amorphous pioneer film is to adopt ion sputtering, or the pulse laser evaporation deposition.
3, according to the preparation method of the described thallium system high-temperature superconducting of claim 2 thin-film material, it is characterized in that described ion sputtering, or the used target material of pulse laser evaporation being the Tl-Ba-Ca-Cu-O bulk material, is to use BaO
2Or BaNO
3, CaO or CaCO
3, CuO and Tl
2O
3Make, use BaO earlier
2Or BaNO
3, CaO or CaCO
3After evenly mixing, grind with CuO, 900-950 ℃ of following calcination is more than 10 hours, then with Tl in oxygen atmosphere
2O
3Mixing, grinding and compressing tablet, 800-900 ℃ of calcination is more than 1 hour in sealing earthenware Crucible; The ratio Tl of metallic element: Ba: Ca: Cu=1-3: 2: 1: 2.
4,, it is characterized in that the ratio Tl of the metallic element of described amorphous pioneer film: Ba: Ca: Cu=1-3: 2: 1: 2 according to the preparation method of the described thallium system high-temperature superconducting of claim 1 thin-film material.
5, according to the preparation method of the described thallium system high-temperature superconducting of claim 1 thin-film material, it is characterized in that described substrate base material is a crystalline material, the lattice constant of its crystalline material or after these crystalline material surfaces add separator the lattice constant and the superconductor lattice constant of separator be complementary.
6,, it is characterized in that described substrate base material is LaAlO according to the preparation method of the described thallium system high-temperature superconducting of claim 5 thin-film material
3, SrTiO
3, NgGaO
3, LSAT[(La, Sr) (Al, Ta) O
3] or on MgO, sapphire, add CeO
2Separator.
7, according to the preparation method of the described thallium system high-temperature superconducting of claim 1 thin-film material, it is characterized in that described high-temperature heat treatment is that amorphous pioneer film and thallium source material are together put into sealing earthenware Crucible, put into the quartz ampoule heating again, heating-up temperature is 720-900 ℃, and the time is 0.5-12 hour.
8, according to the preparation method of the described thallium system high-temperature superconducting of claim 7 thin-film material, it is characterized in that described thallium source material is the heat treated Tl that contains, Ba, Ca, the oxide of Cu, thallium source material adopt 2 footworks to make, and are to use BaO
2Or BaNO
3, CaO or CaCO
3, CuO and Tl
2O
3Make, use BaO earlier
2Or BaNO
3, CaO or CaCO
3After evenly mixing, grind with CuO, 900-950 ℃ of following calcination is more than 10 hours, then with Tl in oxygen atmosphere
2O
3Mixing, grinding and compressing tablet, 800-900 ℃ of calcination is more than 1 hour in sealing earthenware Crucible.
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CN102531567B (en) * | 2011-12-02 | 2013-06-05 | 西安理工大学 | Preparation method of high temperature superconductive film adopting modified low fluoride solution method |
CN106544636B (en) * | 2016-11-14 | 2018-10-02 | 南开大学 | The method for preparing thallium system high-temperature superconducting film without roasting target |
CN108677154B (en) * | 2018-04-08 | 2020-04-21 | 南开大学 | Method for preparing Tl-1223 high-temperature superconducting film by using non-roasted Tl source |
Citations (4)
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---|---|---|---|---|
CN1018113B (en) * | 1988-02-25 | 1992-09-02 | 住友电气工业株式会社 | Superconductive material and method mfg. thereof |
US5688383A (en) * | 1996-02-22 | 1997-11-18 | E. I. Du Pont De Nemours And Company | Method for improving the performance of high temperature superconducting thin film wafers |
US5807809A (en) * | 1993-05-17 | 1998-09-15 | Midwest Superconductivity, Inc. | Method of fabricating thin film superconducting materials |
US5939361A (en) * | 1997-03-19 | 1999-08-17 | Sanyo Electric Co., Ltd. | Method of fabricating Tl or Hg-containing oxide superconductor film |
-
2003
- 2003-08-29 CN CNB031442072A patent/CN1317777C/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1018113B (en) * | 1988-02-25 | 1992-09-02 | 住友电气工业株式会社 | Superconductive material and method mfg. thereof |
US5807809A (en) * | 1993-05-17 | 1998-09-15 | Midwest Superconductivity, Inc. | Method of fabricating thin film superconducting materials |
US5688383A (en) * | 1996-02-22 | 1997-11-18 | E. I. Du Pont De Nemours And Company | Method for improving the performance of high temperature superconducting thin film wafers |
US5939361A (en) * | 1997-03-19 | 1999-08-17 | Sanyo Electric Co., Ltd. | Method of fabricating Tl or Hg-containing oxide superconductor film |
Non-Patent Citations (3)
Title |
---|
American Insititute of Physics W.L.Holstein,L.A.Parisi,and D.W.Face,Applied Physics Letter,Vol.61 No.8 1992 * |
American Insititute of Physics W.L.Holstein,L.A.Parisi,and D.W.Face,Applied Physics Letter,Vol.61 No.8 1992;Insititute of Physics Publishing H Schneidewind,M Manzel,G Bruchlos and K kirsch,Superconductor Science and Technology,Vol.14 2001 * |
Insititute of Physics Publishing H Schneidewind,M Manzel,G Bruchlos and K kirsch,Superconductor Science and Technology,Vol.14 2001 * |
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