CN110265191B - SrTiO with atomically flat surface3Multi-crystal-boundary substrate and preparation method thereof - Google Patents

SrTiO with atomically flat surface3Multi-crystal-boundary substrate and preparation method thereof Download PDF

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CN110265191B
CN110265191B CN201910518122.2A CN201910518122A CN110265191B CN 110265191 B CN110265191 B CN 110265191B CN 201910518122 A CN201910518122 A CN 201910518122A CN 110265191 B CN110265191 B CN 110265191B
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srtio
substrate
grain boundary
single crystal
fese
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CN110265191A (en
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王立莉
丁翠
薛其坤
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Tsinghua University
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Tsinghua University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
    • H01B12/02—Superconductive or hyperconductive conductors, cables, or transmission lines characterised by their form
    • H01B12/06—Films or wires on bases or cores
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
    • 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

The invention relates to SrTiO with an atomically flat surface3The preparation method of the multi-grain boundary substrate comprises the following steps: mixing an untreated SrTiO3The multi-grain boundary substrate is placed in a vacuum chamber with a pressure below 10‑9mbar, wherein the untreated SrTiO3The multi-crystal boundary substrate comprises a plurality of SrTiO layers which are arranged in a coplanar splicing mode and have different crystal orientations3Single crystal substrate, adjacent SrTiO3The single crystal substrate has a trench therebetween, and each SrTiO3The surface of the single crystal substrate is non-atomically flat; and subjecting the untreated SrTiO3Heating the polycrystalline boundary substrate to above 1050 deg.C to remove the untreated SrTiO3And annealing the polycrystalline boundary substrate for more than 10 minutes. The invention also relates to SrTiO with an atomically flat surface prepared by the method3A multi-boundary substrate comprising: SrTiO with different crystal orientations and formed by coplanar splicing3Single crystal substrate of, wherein adjacent SrTiO3The grain boundaries between the single crystal substrates are completely healed to form atomic-level contacts, and each SrTiO3The surface of the single crystal substrate is atomically flat.

Description

SrTiO with atomically flat surface3Multi-crystal-boundary substrate and preparation method thereof
Technical Field
The invention relates to the technical field of superconduction, in particular to SrTiO3A multi-grain boundary substrate and a method for manufacturing the same.
Background
High temperature superconductors are a class of unconventional superconductors that cannot be explained by conventional BCS theory. In 1986, copper oxide high temperature superconductors were first discovered by miller and beddenoltz. In 2008, japanese scientists discovered iron-based high temperature superconductors for the first time. Because the highest superconducting transition temperature of the iron-based high-temperature superconductor is far lower than that of the copper oxide high-temperature superconductor, the iron-based high-temperature superconductor is widely concerned by people.
See the Chinese patent application with publication No. CN103184513A, which discloses a method for preparing SrTiO3A method for growing FeSe high-temperature superconducting thin film on the surface of a substrate, wherein SrTiO is used3Before the substrate is placed in an ultrahigh vacuum system to grow the FeSe high-temperature superconducting film, the SrTiO needs to be subjected to annealing3The substrate is respectively boiled in waterTreating with acid and high-temperature annealing in air to obtain single TiO with atomic-level flat step2Terminated SrTiO3A substrate.
See the Chinese patent application with publication No. CN105679647A, which discloses a SrTiO film with an atomically flat surface and capable of growing FeSe high-temperature superconducting thin film3A method of preparing a substrate, the method comprising: providing at least two pre-processed substrates of the same material, wherein each pre-processed substrate is provided with at least one polishing surface; stacking the at least two pre-processing substrates to form a stacked structure body, wherein the polishing surfaces of two adjacent pre-processing substrates are opposite and completely overlapped; and placing the laminated structure in a high-temperature furnace in the air for annealing treatment, and separating the laminated structure. Wherein the pre-treating the substrate comprises a water boiling treatment and an acid treatment.
However, the above-mentioned SrTiO treatment3In the method of the substrate, the SrTiO3The substrate is subjected to water boiling treatment, acid treatment and high-temperature annealing treatment in the air, and special treatment liquid and annealing equipment are needed, so that the process is complicated and the cost is high.
Disclosure of Invention
The invention provides SrTiO with an atomically flat surface3Method for preparing a multiple grain boundary substrate without the need for untreated SrTiO3The substrate is boiled in water, treated with acid and heat treated at high temperature in air to obtain SrTiO with atomically flat surface3A substrate.
SrTiO with atomic-level flat surface3The preparation method of the multi-grain boundary substrate comprises the following steps: mixing an untreated SrTiO3The multi-grain boundary substrate is placed in a vacuum chamber with a pressure below 10-9mbar, wherein the untreated SrTiO3The multi-crystal boundary substrate comprises a plurality of SrTiO layers which are arranged in a coplanar splicing mode and have different crystal orientations3Single crystal substrate, adjacent SrTiO3The single crystal substrate has a trench therebetween, and each SrTiO3The surface of the single crystal substrate is non-atomically flat; and subjecting the untreated SrTiO3Multiple boundary substrate andheating to 1050 deg.C or higher to remove the untreated SrTiO3And annealing the polycrystalline boundary substrate for more than 10 minutes.
SrTiO with atomically flat surface prepared by adopting method3A multi-boundary substrate comprising: SrTiO with different crystal orientations and formed by coplanar splicing3Single crystal substrate of, wherein adjacent SrTiO3The grain boundaries between the single crystal substrates are completely healed to form atomic-level contacts, and each SrTiO3The surface of the single crystal substrate is atomically flat.
Compared with the prior art, the SrTiO with the atomically flat surface provided by the invention3Method for preparing multi-grain boundary substrate without untreated SrTiO3The substrate is boiled in water, treated with acid and heat treated at high temperature in air to obtain SrTiO with atomically flat surface3A substrate. Moreover, the SrTiO with the atomically flat surface provided by the invention3The preparation method of the polycrystalline boundary substrate can enable adjacent SrTiO to be subjected to ultrahigh vacuum annealing treatment3The grain boundaries between the single crystal substrates are completely healed to form atomic level contacts. SrTiO with atomically flat surface prepared by the method3In a polycrystalline boundary substrate, adjacent SrTiO3The grain boundaries between the single crystal substrates are completely healed to form atomic level contacts.
Drawings
FIG. 1 is a diagram of SrTiO treated according to an embodiment of the present invention3A schematic view of a method of a substrate.
FIG. 2 shows SrTiO before and after annealing according to embodiments of the present invention3The structure of the double grain boundary substrate is shown schematically.
Fig. 3 is a schematic structural diagram of an FeSe twin boundary superconductor with grooves and slits according to an embodiment of the present invention.
Fig. 4 is a schematic structural diagram of an FeSe twin boundary superconductor without grooves and slits according to an embodiment of the present invention.
FIG. 5 shows SrTiO with atomically flat surface prepared in example 1 of the present invention3Scanning Tunneling Microscope (STM) photographs of single crystal substrates.
FIG. 6 is a photograph of a film prepared in example 1 of the present inventionSrTiO without oxygen supplementation treatment3Scanning tunnel microscope photo of the result of growing FeSe high temperature superconductive film on the substrate.
FIG. 7 is a scanning tunneling microscope photograph of a FeSe high temperature superconducting thin film prepared in example 2 of the present invention before annealing.
FIG. 8 is a scanning tunneling microscope photograph of the FeSe high temperature superconducting thin film prepared in example 2 of the present invention after annealing.
FIG. 9 shows non-annealed SrTiO provided in example 3 of the present invention3Atomic Force Microscope (AFM) photographs of the double grain boundary substrates.
FIG. 10 shows the annealed SrTiO material provided in example 3 of the present invention3Scanning tunneling microscope photograph of the double grain boundary substrate.
FIG. 11 is a scanning tunneling microscope photograph of a FeSe high temperature superconducting thin film prepared in example 4 of the present invention before annealing.
FIG. 12 is a scanning tunneling microscope photograph of an annealed FeSe high temperature superconducting thin film prepared in example 4 of the present invention.
FIG. 13 shows the annealed SrTiO film obtained in example 5 of the present invention3Scanning tunneling microscope photograph of the double grain boundary substrate.
FIG. 14 is a scanning tunneling microscope photograph of a FeSe high temperature superconducting thin film with a thickness of 1UC prepared in example 6 of the present invention.
FIG. 15 is a scanning tunneling microscope photograph of a 10UC thick FeSe high temperature superconducting thin film prepared in example 6 of the present invention.
FIG. 16 shows the annealed SrTiO film obtained in example 7 of the present invention3Scanning tunneling microscope photograph of the double grain boundary substrate.
FIG. 17 is a scanning tunneling microscope photograph of a FeSe high temperature superconducting thin film prepared in example 8 of the present invention before annealing.
FIG. 18 is a scanning tunneling microscope photograph of an annealed FeSe high temperature superconducting thin film prepared in example 8 of the present invention.
FIG. 19 is a low temperature scanning tunneling microscope photograph of the FeSe high temperature superconducting thin film prepared in example 8 of the present invention at the grain boundary.
FIG. 20 is a low temperature scanning tunneling microscope photograph of the FeSe single crystal layer on the left side of the grain boundary of the FeSe high temperature superconducting thin film prepared in example 8 of the present invention.
Fig. 21 is a low-temperature scanning tunneling microscope photograph of the FeSe single crystal layer on the right side of the grain boundary of the FeSe high-temperature superconducting thin film prepared in example 8 of the present invention.
FIG. 22 is a scanning tunneling microscope photograph of a FeSe high temperature superconducting thin film prepared in example 9 of the present invention before annealing.
FIG. 23 is a scanning tunneling microscope photograph of an annealed FeSe high temperature superconducting thin film prepared in example 9 of the present invention.
FIG. 24 shows an annealed SrTiO film provided in example 10 of the present invention3Scanning tunneling microscope photograph of the double grain boundary substrate.
FIG. 25 is a scanning tunneling microscope photograph of a FeSe high temperature superconducting thin film prepared in example 11 of the present invention before annealing.
FIG. 26 is a scanning tunneling microscope photograph of an annealed FeSe high temperature superconducting thin film prepared in example 11 of the present invention.
FIG. 27 shows annealed SrTiO film provided in example 12 of the present invention3Scanning tunneling microscope photograph of the double grain boundary substrate.
FIG. 28 is a scanning tunneling microscope photograph of a FeSe high temperature superconducting thin film prepared in example 13 of the present invention before annealing.
FIG. 29 is a scanning tunneling microscope photograph of an annealed FeSe high temperature superconducting thin film prepared in example 13 of the present invention.
FIG. 30 shows SrTiO annealed according to comparative example 1 of the present invention3Scanning tunneling microscope photographs of single crystal substrates.
FIG. 31 shows SrTiO annealed according to comparative example 2 of the present invention3Scanning tunneling microscope photograph of the double grain boundary substrate.
FIG. 32 shows SrTiO annealed according to comparative example 3 of the present invention3Atomic force microscope pictures of the double grain boundary substrate.
FIG. 33 shows the results of R-T test of FeSe high temperature superconducting films prepared in example 6 of the present invention.
Fig. 34 is an enlarged view of a box portion of fig. 33.
FIG. 35 shows the results of R-T test of FeSe high temperature superconducting films prepared in example 8 of the present invention.
Fig. 36 is an enlarged view of a box portion of fig. 35.
FIG. 37 shows the results of R-T test of FeSe high temperature superconducting films prepared in example 13.
Description of the main elements
FeSe superconductor 10,10A
SrTiO3 Substrate 100
Groove 1002
A first electrode 101
Second electrode 102
Heating element 103
FeSe high-temperature superconducting thin film 104
Gap 1042
Vacuum chamber 20
Detailed Description
The invention will be described in further detail with reference to the following drawings and specific embodiments.
For easy understanding, the present invention first introduces SrTiO provided in the embodiments of the present invention3Method for treating substrate, and SrTiO treated by the method3A method for growing FeSe superconductor on a substrate.
Referring to fig. 1, an embodiment of the present invention provides a method for treating SrTiO3A method of processing a substrate, comprising the steps of:
step S10, mixing SrTiO3The substrate 100 is placed in a vacuum chamber 20, the pressure in the vacuum chamber 20 being lower than 10- 9mbar, the SrTiO3The surface of the substrate 100 is non-atomically flat; and
step S20, the SrTiO is mixed3Heating the substrate 100 to over 900 deg.C to form SrTiO3The substrate 100 is annealed for more than 30 minutes.
In the step S10, the SrTiO3The substrate 100 may be a single crystal substrate or a polycrystalline boundary substrate. The single crystal substrate means that the substrate includes only one single crystal. Referring to fig. 2, the polycrystalline boundary substrate means that the substrate only comprises a plurality of SrTiO with different crystal orientations and arranged in a coplanar splicing manner3Single crystal substrate, adjacent SrTiO3The single crystal substrate has nano-scale trenches 1002 between them.
The SrTiO3The substrate 100 has a layered crystal structure composed of titanium dioxide (TiO)2) The layers are alternately laminated with strontium oxide (SrO) layers. Specifically, the SrTiO3The lattice type of the substrate 100 is a tetragonal lattice. The SrTiO3The lattice constant of the substrate 100 in the (100) crystal plane is 0.3905 nm. The SrTiO3The lattice mismatch degree of the substrate 100 on the (100) crystal plane and the FeSe single crystal layer is about 3%, and the small lattice mismatch degree is beneficial to growing the high-quality FeSe single crystal layer on the (100) crystal plane. The SrTiO3Thickness of the substrate 100And optionally between 0.2 mm and 1.0 mm. The SrTiO3The substrate 100 has a high dielectric constant (10) at low temperatures4). The SrTiO3The substrate 100 has a high dielectric constant, which is advantageous for shielding the interaction between carriers. In order to facilitate observation of the superconducting transition temperature of the high-temperature superconducting thin film 10 by electrical transport measurement, high-resistance insulating SrTiO can be selected3A substrate 100.
The vacuum chamber 20 may be a special vacuum annealing device, or may be a reaction chamber of a device for subsequently growing the FeSe high-temperature superconducting thin film 104. Preferably, the invention adopts equipment for growing the FeSe high-temperature superconducting thin film 104 to directly carry out the preparation of the SrTiO3The substrate 100 is annealed to subsequently directly grow the FeSe high temperature superconducting thin film 104. Preferably, for said SrTiO3The pressure of the vacuum chamber 20 is lower than 10 when the substrate 100 is annealed-10mbar。
In the step S20, the SrTiO is treated3The method of heating the substrate 100 is not limited, and heating may be performed by a heating device provided in the vacuum chamber 20 itself, or a special heating device may be provided. Referring to fig. 1, the SrTiO is first prepared in the present invention3The substrate 100 is disposed on a surface of a heating element 103, and then a voltage is applied to the heating element 103 through a first electrode 101 and a second electrode 102, thereby applying a voltage to the SrTiO3The substrate 100 is heated. Specifically, the heating element 103 may be a metal layer, a silicon carbide layer, or the like, and the first electrode 101 and the second electrode 102 are metal-sandwiched electrodes. The first electrode 101 and the second electrode 102 are formed by mixing the SrTiO at both ends thereof3The substrate 100 and the heating element 103 are fixed. The voltage applied to the heating element 103 may be alternating current or direct current.
The inventors of the present invention have found that the SrTiO can be annealed at 900 ℃ or higher in an ultra-high vacuum for 30 minutes or longer3The surface of the substrate 100 is atomically flat. Thus, the steps of the existing water boiling treatment and acid treatment are omitted, and the impurities caused by the high-temperature annealing treatment in the air in the existing method are avoided.
Further, referring to fig. 2, the inventors of the present application also found that the trenches 1002 of the multi-grain boundary substrate are almost disappeared, i.e., the grain boundaries between adjacent single crystal substrates are completely healed to form atomic-level contacts, by annealing at 1050 ℃ or more in ultra-high vacuum.
However, the inventors of the present application have also found that SrTiO treated by the above method3The substrate 100, however, cannot be used directly for growing the FeSe high temperature superconducting thin film 104, since the ultra-high vacuum heat treatment results in SrTiO3The substrate 100 is substantially deoxygenated. SrTiO treated by the above method3The substrate 100, due to the substantial amount of deoxidation, is electrically conductive and is not suitable for growing and studying the FeSe high temperature superconducting thin film 104.
SrTiO treated by the above method is required for growing and researching FeSe high-temperature superconducting thin film 1043The substrate 100 is subjected to an oxygen supplement treatment to thereby make the SrTiO3The substrate 100 is converted to an insulator. Thus, the treated SrTiO3The method of the substrate may further include treating the SrTiO treated by the method3Step S30 of performing the oxygen replenishment process on the substrate 100 is described below.
Referring to fig. 1 and 3-4, embodiments of the present invention further provide a method of making a FeSe superconductor 10, comprising the steps of:
step S10, mixing SrTiO3The substrate 100 is placed in a vacuum chamber 20, the pressure in the vacuum chamber 20 being lower than 10- 9mbar, the SrTiO3The surface of the substrate 100 is non-atomically flat;
step S20, the SrTiO is mixed3Heating the substrate 100 to over 900 deg.C to form SrTiO3Annealing the substrate 100 for more than 30 minutes;
step S30, the temperature of the vacuum chamber 20 is reduced to 650-800 deg.C, and then an oxygen-containing atmosphere is introduced into the vacuum chamber 20 to maintain the pressure of the vacuum chamber 20 at 1 × 10-6mbar～1×10-4mbar, to the annealed SrTiO3The substrate 100 is subjected to oxygen supplement treatment for 10 to 30 minutes; and
step S40, in the SrTiO after the oxygen supplement treatment3The FeSe high temperature superconducting film 104 is grown on the surface of the substrate 100.
In step S30, the oxygen-containing atmosphere may be oxygen or air ozone. The vacuum chamber 20 for annealing and oxygen supplement in the embodiment of the invention is a reaction chamber of the equipment for subsequently growing the FeSe high-temperature superconducting thin film 104. Preferably, the embodiment of the invention uses ozone for oxygen supplementation. This is because the oxygen and air require greater pressure and volume to achieve the same supplemental oxygen effect. On the one hand, this may destroy the vacuum atmosphere of the vacuum chamber 20, resulting in failure of molecular beam epitaxial growth in the chamber. On the other hand, for a multi-grain boundary substrate, the re-cracking of grain boundaries may be caused by the addition of oxygen in oxygen and air at high pressure.
In step S40, the method for growing the FeSe high temperature superconducting thin film 104 is not limited, and may be any conventional method.
Referring to fig. 3, when the SrTiO is used3When the substrate 100 is a polycrystalline boundary substrate with a nano-scale trench 1002, the grown FeSe high-temperature superconducting thin film 104 is a polycrystalline boundary superconducting thin film, which includes a plurality of FeSe single crystal thin films that are spliced in a coplanar manner and have different crystal orientations, and a nano-scale gap 1042 corresponding to the trench 1002 is formed between the plurality of FeSe single crystal thin films. Referring to fig. 4, when the SrTiO is used3When the substrate 100 is a polycrystalline boundary substrate without the trench 1002, grain boundaries between a plurality of FeSe single crystal thin films of the grown FeSe high temperature superconducting thin film 104 are completely healed to form atomic-level contact. That is, there is no gap between the two FeSe single crystal films, thereby forming an integral structure.
The following are specific examples of the present invention.
Example 1
Firstly, SrTiO3The single crystal substrate is placed in a vacuum chamber at a pressure of<10-9mbar, the SrTiO3The surface of the single crystal substrate is non-atomically flat. Next, the SrTiO is mixed3Heating the substrate to 900-1000 deg.C, and heating the SrTiO3The substrate is annealed for more than 30 minutes. Example 1 annealing temperatures were 900 ℃, 950 ℃ and 1000 ℃, respectively. The annealing times were 30 minutes, 60 minutes, 75 minutes and 90 minutes, respectively. As shown in FIG. 1, in this example, a silicon carbide heating layer was used to heat the SrTiO by direct current3A substrate. Referring to fig. 5, the annealed SrTiO3The surface of the substrate is atomically flat. The higher the annealing temperature and the longer the annealing time, the treated SrTiO3The flatter the substrate surface.
However, the SrTiO treated in example 13The substrate cannot be directly used for growing the FeSe high-temperature superconducting film, because the SrTiO is caused by the ultrahigh vacuum heating treatment3The substrate is substantially deoxygenated. Referring to fig. 6, SrTiO treated in the method of example 1 but without oxygen supplementation3When a FeSe high-temperature superconducting thin film is grown on a substrate, a plurality of dispersed clusters are obtained, and a continuous FeSe single crystal layer cannot be obtained. Furthermore, even if SrTiO is reduced3SrTiO not treated with oxygen supplementation in the presence of a substrate growth temperature, increased Se flow, or annealing in a Se atmosphere3The surface of the substrate obtains a continuous FeSe monocrystal layer.
Example 2
Example 2 of the present invention is substantially the same as example 1 except that example 2 further comprises SrTiO 2 on the basis of example 13The substrate is subjected to oxygen supplement treatment, and SrTiO treated by the oxygen supplement treatment is adopted3Growing FeSe high-temperature superconducting film on the substrate.
Specifically, the SrTiO3After annealing the substrate for more than 60 minutes, the temperature of the vacuum chamber is reduced to 750 ℃, and then an oxygen-containing atmosphere is introduced into the vacuum chamber to keep the pressure of the vacuum chamber at 8X 10-6mbar, to the annealed SrTiO3The substrate was subjected to an oxygen replenishment treatment for 10 minutes.
EXAMPLE 2 SrTiO after oxygenating treatment3The substrate is an insulator and can be directly used for growing the FeSe high-temperature superconducting thin film. Specifically, the annealed SrTiO3After the substrate is oxygen-supplemented, the introduction of oxygen-containing atmosphere is stopped to reduce the pressure of the vacuum chamber to 10-9mbar or less, and the vacuum chamber temperature is reduced to 380 ℃ to 420 ℃. Then respectively introducing an Fe source and an Se source into the vacuum chamber, wherein the beam current ratio of the Fe source to the Se source is kept between 1:10 and 1:20, the growth temperature of the Fe source and the growth temperature of the Se source are respectively kept between 1000 ℃ and 1100 ℃ and between 130 ℃ and 150 ℃, and the growth beam current of the FeSe high-temperature superconducting thin film is kept at 025UC/min or so. Further, after the FeSe high-temperature superconducting film is grown, the SrTiO is further processed3The substrate is annealed at a temperature between 450 ℃ and 550 ℃ for 20 hours to 30 hours. The annealing treatment aims to remove the surplus Se and simultaneously improve the FeSe high-temperature superconducting thin film and the SrTiO3The bonding effect between the substrates is more favorable for the iron-based high-temperature superconducting film to obtain stronger interface enhanced superconducting effect.
In this embodiment, the beam current ratio of the Fe source and the Se source is maintained at 1: 10. The SrTiO3The temperature of the substrate was maintained at 400 deg.C and the growth temperatures of the Fe source and Se source were maintained at 1100 deg.C and 150 deg.C, respectively. After the growth is finished, the SrTiO is added3The substrate was annealed at 500 c for 70 minutes. Referring to FIGS. 7-8, the FeSe high temperature superconducting film is a single crystal layer with a thickness of 1.2UC, and the FeSe single crystal layer and SrTiO3The single crystal substrates have an atomically flat interface therebetween.
In this embodiment, the FeSe high temperature superconducting thin film is further away from the SrTiO3And a FeTe single crystal layer is grown on the surface of the substrate and is used as a protective layer. An atomically flat interface is arranged between the FeTe single crystal layer and the FeSe single crystal layer.
Example 3
Example 3 of the present invention is substantially the same as example 1 except that SrTiO of example 3 is used3The substrate is a double grain boundary substrate.
Specifically, first, SrTiO3The double grain boundary substrate is placed in a vacuum chamber with a pressure below 10- 9mbar. Secondly, the vacuum chamber is heated to 950 ℃ to the SrTiO3The double grain boundary substrate was annealed for 60 minutes. Referring to fig. 9, the untreated SrTiO3The double-crystal-boundary substrate comprises two SrTiO layers which are arranged in a coplanar splicing mode and have different crystal orientations3Single crystal substrate, adjacent SrTiO3Grooves with the width of 80 nanometers and the depth of 0.6 nanometers are arranged between the single crystal substrates, and each SrTiO3The surface of the single crystal substrate is non-atomically flat. Referring to fig. 10, the annealed SrTiO3The double crystal boundary substrate surface forms a groove with an atomically flat but adjacent single crystal substratesStill, about 15 nm wide and 1 nm deep. SrTiO treated in the same manner as in example 33The substrate can not be directly used for growing the FeSe high-temperature superconducting thin film.
Example 4
Example 4 of the present invention is substantially the same as example 3, except that example 4 further includes SrTiO in addition to example 33The substrate is subjected to oxygen supplement treatment, and SrTiO treated by the oxygen supplement treatment is adopted3Growing FeSe high-temperature superconducting film on the substrate.
In this example, the SrTiO compound3Annealing the double-grain boundary substrate for more than 60 minutes, reducing the temperature of the vacuum chamber to 750 ℃, and then introducing ozone into the vacuum chamber to keep the pressure of the vacuum chamber at 1 x 10-5mbar, to the annealed SrTiO3And carrying out oxygen supplement treatment on the double-grain boundary substrate for 15 minutes.
EXAMPLE 4 SrTiO after oxygenating treatment3The double-grain boundary substrate is an insulator and can be directly used for growing the FeSe high-temperature superconducting thin film. Specifically, the method of example 2 for growing FeSe high temperature superconducting thin film is adopted in SrTiO3And growing a FeSe high-temperature superconducting film on the surface of the double-crystal boundary substrate. Referring to fig. 11, the FeSe high temperature superconducting thin film grown in this example is a double grain boundary superconducting thin film. The FeSe double-crystal boundary superconducting film comprises two FeSe single crystal films which are spliced in a coplanar mode and have different crystal orientations, and a gap is formed between the two FeSe single crystal films. The FeSe single crystal film and SrTiO3The single crystal substrates have an atomically flat interface therebetween. After FeSe growth is finished, SrTiO3The substrate was annealed at 500 c for 70 minutes. Referring to fig. 12, after annealing the grown FeSe double grain boundary superconducting thin film, a distinct dark domain appears, and the FeSe single crystal thin film is decomposed along the dark domain in the vicinity of the grain boundary.
In this embodiment, the FeSe high temperature superconducting thin film is further away from the SrTiO3And a FeTe single crystal layer is grown on the surface of the substrate and is used as a protective layer. An atomically flat interface is formed between the FeTe single crystal layer and the FeSe single crystal film.
Example 5
Examples 5 and 3 of the present inventionThe process is essentially the same except that the SrTiO is treated3The annealing temperature of the double-grain boundary substrate in the vacuum chamber is 1000 ℃, and the annealing time is 60 minutes. Referring to fig. 13, this example annealed SrTiO3The double grain boundary substrate surface is atomically flat, but the trenches between adjacent single crystal substrates remain.
Example 6
Example 6 of the present invention is substantially the same as example 4 except that SrTiO is used3The annealing temperature of the double-grain boundary substrate in the vacuum chamber is 1000 ℃, and the annealing time is 60 minutes. Referring to fig. 14, the FeSe high temperature superconducting thin film grown in this example is a double grain boundary superconducting thin film, and there is still a significant gap between the two FeSe single crystal thin films. Referring to FIG. 15, in this example, even if FeSe of raw 10UC is annealed at 450 ℃, SrTiO can only be filled3And partial grooves of the double-grain boundary substrate.
This example further tests the R-T characteristics of the prepared FeSe high temperature superconducting thin film. Referring to fig. 33-34, zero resistance R1 and R2 can be observed for both sides of the gap or grain boundary below 10K, but the resistance Rc across the grain boundary is still 2Ohm at 1.8K. The resistance Rc across the grain boundaries is mainly due to the fact that there are still significant gaps between the two FeSe single crystal thin films.
Example 7
Example 7 of the present invention is substantially the same as example 3 except that SrTiO is used3The annealing temperature of the double-grain boundary substrate in the vacuum chamber is above 1050 ℃.
Specifically, first, SrTiO3The double grain boundary substrate is placed in a vacuum chamber with a pressure below 10- 9mbar. Secondly, heating the vacuum chamber to over 1050 ℃ to the SrTiO3The double grain boundary substrate is annealed for more than 10 minutes. Example 7 annealing temperatures were 1050 ℃, 1100 ℃ and 1200 ℃, respectively. The annealing times were 10 minutes, 20 minutes, 30 minutes, 60 minutes and 90 minutes, respectively. Experiments show that the crystal boundary between adjacent single crystal substrates can be completely healed by annealing at 1050 ℃ for more than 10 minutes, atomic-level contact is formed, and the surface of the substrate is atomically flat. Referring to FIG. 16, this example is annealedSrTiO3The double-grain-boundary substrate surface is formed to be atomically flat, and the grooves between the adjacent single crystal substrates are almost disappeared, that is, the grain boundaries between the adjacent single crystal substrates are completely healed to form atomic-level contact. Due to SrTiO3At 1050 ℃, the double-grain boundary substrate gradually loses oxygen, the resistance is reduced, the temperature is increased, and the risk of fracture is easily caused. And the risk of substrate fracture due to overhigh temperature can be reduced by reducing the annealing time at 1050 ℃. Therefore, the annealing time is preferably 60 minutes or less.
Example 8
Example 8 of the present invention is substantially the same as example 7 except that example 8 is performed on SrTiO further on the basis of example 73The substrate is subjected to oxygen supplement treatment, and SrTiO treated by the oxygen supplement treatment is adopted3Growing FeSe high-temperature superconducting film on the substrate.
Specifically, first, SrTiO3The double grain boundary substrate is placed in a vacuum chamber with a pressure below 10- 9mbar. Secondly, the vacuum chamber is heated to 1050 ℃ to the SrTiO3The double grain boundary substrate was annealed for 60 minutes. Then, the method of example 2 was used to perform oxygen replenishment treatment and grow a FeSe high-temperature superconducting thin film. Referring to fig. 17, the FeSe high temperature superconducting thin film grown in this example is a double grain boundary superconducting thin film with a thickness of 1.2UC, and the grain boundary between the two FeSe single crystal thin films is completely healed to form atomic level contact. That is, there is no gap between the two FeSe single crystal films, thereby forming an integral structure. The FeSe single crystal film and SrTiO3The single crystal substrates have an atomically flat interface therebetween. After FeSe growth is finished, SrTiO3The substrate was annealed at 490 c for 60 minutes. Referring to fig. 18, the grown FeSe double grain boundary superconducting thin film, after annealing, appeared a distinct dark domain, and the FeSe single crystal thin film was decomposed along the dark domain in the vicinity of the grain boundary. Referring to fig. 19 to 21, the two FeSe single crystal layers are in contact with each other at a position having a distinct grain boundary, and the FeSe single crystal layers on both sides of the grain boundary have different crystal orientations.
In this embodiment, the FeSe high temperature superconducting thin film is further away from the SrTiO3Growing a FeTe single crystal layer on the surface of the substrate as a protective layerAnd (4) a protective layer. An atomically flat interface is formed between the FeTe single crystal layer and the FeSe single crystal film.
This example further tests the R-T characteristics of the prepared FeSe high temperature superconducting thin film. Referring to fig. 35-36, zero resistance R1 can be observed for gaps or grain boundaries on one side below 12K, but the resistance across grain boundaries Rc is 20mOhm at 1.8K. The resistance Rc across the grain boundary is mainly caused by the decomposition of the two FeSe single crystal thin films along the dark domain in the vicinity of the grain boundary. The resistance Rc across the grain boundaries was significantly reduced for the sample of example 8 compared to the sample of example 6.
Example 9
Inventive example 9 was substantially the same as example 8 except that the oxygen replenishment temperature was 750 ℃ for example 8 and 680 ℃ for example 9. Referring to fig. 22, the FeSe high temperature superconducting thin film grown in this example is a double grain boundary superconducting thin film with a thickness of 1.2UC, and the grain boundary between the two FeSe single crystal thin films is completely healed to form atomic level contact. After FeSe growth is finished, SrTiO3The substrate was annealed at 450 ℃ for 60 minutes. Referring to fig. 23, after annealing the grown FeSe double grain boundary superconducting thin film, no bright/dark domains were observed, but the FeSe single crystal thin film still decomposed along the dark domains in the vicinity of the grain boundaries.
Example 10
The method of example 10 of the present invention is substantially the same as that of example 3, except that SrTiO is used3After annealing the double grain boundary substrate at 950 ℃ for 40 minutes, the vacuum chamber is heated to 1050 ℃ and then annealed for 20 minutes. That is, example 10 includes two anneals at different temperatures, respectively. Referring to fig. 24, this example shows SrTiO after annealing at 1050 deg.c3The double-crystal-boundary substrate surface is formed into an atomic-level flat surface, and crystal boundaries between adjacent single-crystal substrates are completely healed to form atomic-level contact. Example 10 pre-annealing at 950 ℃ for 40 minutes and then annealing at 1050 ℃ was performed mainly to reduce the difficulty of maintaining ultra-high vacuum by direct heating to 1050 ℃.
Example 11
The method of the invention in example 11 is substantially the same as that of example 10, except that in example 11, SrTi is further added to example 10O3The substrate is subjected to oxygen supplement treatment, and SrTiO treated by the oxygen supplement treatment is adopted3Growing FeSe high-temperature superconducting film on the substrate.
Specifically, the method of example 2 for growing FeSe high temperature superconducting thin film is adopted in SrTiO3And growing a FeSe high-temperature superconducting film on the surface of the double-crystal boundary substrate. Referring to fig. 25, the FeSe high temperature superconducting thin film grown in this example is a double grain boundary superconducting thin film, and the grain boundary between the two FeSe single crystal thin films is completely healed to form atomic level contact. After FeSe growth is finished, SrTiO3The substrate was annealed at 430 ℃ for 60 minutes. Referring to fig. 26, after annealing the grown FeSe double grain boundary superconducting thin film, no bright/dark domains were observed, but the FeSe single crystal thin film still decomposed along the dark domains near the grain boundaries.
Example 12
Inventive example 12 was substantially the same as example 7 except that the SrTiO was heated using alternating current3A double grain boundary substrate. Referring to fig. 27, this example annealed SrTiO3The double grain boundary substrate surface is formed to be atomically flat, and the trenches between adjacent single crystal substrates are almost disappeared.
It was also found experimentally that heating the SrTiO with alternating current3When a substrate, the SrTiO3The substrate is not easily broken. And heating the SrTiO by direct current3When a substrate, the SrTiO3The substrate is easily broken. This is because the SrTiO compound is heated by direct current3Oxygen vacancies generated by deoxidation of the substrate at a high temperature are accumulated on the negative electrode side, resulting in the SrTiO3The substrate has too high local temperature and is easy to break. When AC heating is used, the SrTiO3Oxygen vacancies generated by deoxidation of the substrate at high temperature are uniformly distributed in SrTiO3Within the substrate, therefore, the SrTiO3The temperature distribution of the substrate is also very uniform and is not easy to break.
In addition, SrTiO treated by direct current heating3The oxygen vacancies in the substrate are unevenly distributed and the SrTiO is subjected to a subsequent oxygen supplementation treatment3The distribution of oxygen elements within the substrate is also less uniform. The subsequent FeSe growth process is long, and the high-quality FeSe film cannot be obtained due to excessive oxygen vacancies. WhileIn addition, when the direct current heat treatment is used, SrTiO on the negative electrode side3The substrate still has the possibility of electric conduction after oxygen supplementation, and the subsequent research on the superconducting property of the FeSe film is influenced. However, SrTiO treated with alternating current heat3Oxygen vacancies in the substrate are uniformly distributed, and SrTiO is subjected to the subsequent oxygen supplement treatment process3The substrate can be sufficiently oxygen-supplemented.
Example 13
Example 13 of the present invention is substantially the same as example 12 except that example 13 further employs SrTiO in addition to example 123The substrate is subjected to oxygen supplement treatment, and SrTiO treated by the oxygen supplement treatment is adopted3Growing FeSe high-temperature superconducting film on the substrate.
Specifically, the method of example 2 for growing FeSe high temperature superconducting thin film is adopted in SrTiO3And growing a FeSe high-temperature superconducting film on the surface of the double-crystal boundary substrate. Referring to fig. 28, the FeSe high temperature superconducting thin film grown in this example is a double grain boundary superconducting thin film, and the grain boundary between the two FeSe single crystal thin films is completely healed to form atomic level contact. After FeSe growth is finished, SrTiO3The substrate was annealed at 490 c for 60 minutes. Referring to fig. 29, after annealing the grown FeSe double-grain-boundary superconducting thin film, the FeSe films on both sides of the grain boundary showed bright domains, and the FeSe single-crystal thin film did not show decomposition, but the grain boundary protruded higher than both sides by about 1 nm.
This example further tests the R-T characteristics of the prepared FeSe high temperature superconducting thin film. Referring to fig. 37, the resistances R1 and R2 on both sides of the gap or grain boundary, and the resistance Rc across the grain boundary are below 10K, and a zero resistance phenomenon can be observed. The zero resistance phenomenon can be observed for the resistance Rc across the grain boundary, which is caused by that the FeSe single crystal film is not decomposed after the FeSe double-grain boundary superconducting film is annealed.
Comparative example 1
Comparative example 1 of the present invention was substantially the same as example 1 except that the annealing temperature was 650 ℃. Referring to fig. 30, SrTiO treated by the method of comparative example 13The surface of the substrate is still non-atomically flat, and the SrTiO3The substrate cannot be used for growing the FeSe high-temperature superconducting thin film.
Comparative example 2
Comparative example 2 of the present invention was substantially the same as example 3 except that the annealing temperature was 650 ℃. Referring to fig. 31, SrTiO treated by the method of comparative example 23The surface of the double-crystal boundary substrate is still non-atomically flat, and two single crystals SrTiO3The width of the groove between the substrates is 80 nm, the depth is 1 nm, and the SrTiO is3The double grain boundary substrate cannot be used for growing the FeSe high-temperature superconducting thin film.
Comparative example 3
Comparative example 3 of the present invention, SrTiO was treated by the method of the Chinese patent application having publication No. CN105679647A3A double grain boundary substrate.
Specifically, two SrTiO materials with polished surfaces are provided3Sequentially placing the double-crystal-boundary substrate in acetone, isopropanol and ultrapure water for ultrasonic cleaning for five minutes respectively, and then cleaning SrTiO3Soaking the double-grain boundary substrate in hot water bath for 1 hour, and soaking the double-grain boundary substrate in hot hydrochloric acid (HCl) with the concentration of 10% for 45 minutes to obtain two pretreated SrTiO3A double grain boundary substrate. Two pretreated SrTiO materials are mixed3Double grain boundary substrate is laminated in pure water with two pretreated SrTiO3And the polished surfaces of the double-grain boundary substrates are opposite and overlapped to obtain a laminated structure. Placing the laminated structure in a high temperature furnace, annealing at 1080 ℃ under an oxygen atmosphere of about one atmosphere, separating for 3 hours to obtain two SrTiO with atomically flat surfaces3A double grain boundary substrate. Referring to FIG. 32, the SrTiO3The double grain boundary substrate has an atomically flat surface, but two single crystal SrTiO3The width of the trench between the substrates was 80 nm and the depth was 10 nm. That is, the method of comparative example 3 cannot make two single crystal SrTiO3The trenches between the substrates disappear, instead deepening the trenches.
Further, the SrTiO with the atomically flat surface is adopted3And growing a FeSe high-temperature superconducting thin film on the double-crystal-boundary substrate. The grown FeSe high-temperature superconducting thin film is two independent FeSe single crystal thin films. That is, the two FeSe single crystal thin films are separated by a gap, and a continuous grain boundary cannot be formed.
In addition, other modifications within the spirit of the invention may occur to those skilled in the art, and such modifications within the spirit of the invention are intended to be included within the scope of the invention as claimed.

Claims (10)

1. SrTiO with atomic-level flat surface3The preparation method of the multi-grain boundary substrate is characterized by comprising the following steps of:
mixing an untreated SrTiO3The multi-grain boundary substrate is placed in a vacuum chamber with a pressure below 10-9mbar, wherein the untreated SrTiO3The multi-crystal boundary substrate comprises a plurality of SrTiO layers which are arranged in a coplanar splicing mode and have different crystal orientations3Single crystal substrate, adjacent SrTiO3The single crystal substrate has a trench therebetween, and each SrTiO3The surface of the single crystal substrate is non-atomically flat; and
the untreated SrTiO3Heating the polycrystalline boundary substrate to above 1050 deg.C to remove the untreated SrTiO3And annealing the polycrystalline boundary substrate for more than 10 minutes.
2. SrTiO with atomically flat surface according to claim 13A method for producing a multi-grain boundary substrate, characterized in that the untreated SrTiO is treated3The method for heating the multi-grain boundary substrate comprises the following steps: subjecting the untreated SrTiO3The multi-grain boundary substrate is disposed on a surface of a heating element, and then a voltage is applied to the heating element via a first electrode and a second electrode.
3. SrTiO with atomically flat surface according to claim 23A method of producing a multi-grain boundary substrate, characterized in that an alternating current is applied to the heating element through a first electrode and a second electrode.
4. SrTiO with atomically flat surface according to claim 23A method for producing a multi-grain boundary substrate, characterized in that a direct current is applied to the heating element through a first electrode and a second electrode.
5. SrTiO with atomically flat surface according to claim 13A method for producing a multi-grain boundary substrate, characterized in that the untreated SrTiO is treated3The multi-grain boundary substrate is annealed at 1050 ℃ or higher for 30 minutes or longer.
6. SrTiO with atomically flat surface according to claim 13A method for producing a multi-grain boundary substrate, characterized in that the untreated SrTiO is3The untreated SrTiO material is heated to above 1050 deg.C before the polycrystalline boundary substrate is heated3Preheating the polycrystal boundary substrate to 900-1000 ℃ and keeping the temperature for more than 30 minutes.
7. SrTiO with atomically flat surface according to claim 13A method for producing a multi-grain boundary substrate, characterized in that the untreated SrTiO is treated3After annealing the multi-boundary substrate for more than 10 minutes, the method further comprises the following steps: the temperature of the vacuum chamber is reduced to 650-800 ℃, then oxygen-containing atmosphere is introduced into the vacuum chamber, and the pressure of the vacuum chamber is kept at 1 x 10-6mbar～1×10-4mbar, to the annealed SrTiO3And carrying out oxygen supplement treatment on the multi-grain boundary substrate for 10-30 minutes.
8. SrTiO with atomically flat surface according to claim 73The preparation method of the multi-grain boundary substrate is characterized in that the oxygen-containing atmosphere is ozone.
9. SrTiO with atomic-level flat surface3The multi-crystalline interface substrate composed of SrTiO with atomically flat surface of any one of claim 1 to claim 83The SrTiO with the atomically flat surface is prepared by a preparation method of a multi-crystal-boundary substrate3The polycrystalline boundary substrate includes: SrTiO with different crystal orientations and formed by coplanar splicing3A single crystal substrate, characterized in that adjacent SrTiO3The grain boundaries between the single crystal substrates are completely healed to form the precursorsSub-level contact, and each SrTiO3The surface of the single crystal substrate is atomically flat.
10. SrTiO with atomically flat surface of claim 93A polycrystalline boundary substrate, wherein each SrTiO3The single crystal substrate includes a plurality of oxygen vacancies such that the SrTiO3The multi-grain boundary substrate is an electric conductor.
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